Journal of Minerals and Materials Characterization and Engineering, 2014, 2, 428-469

Published Online September 2014 in SciRes. http://www.scirp.org/journal/jmmce

http://dx.doi.org/10.4236/jmmce.2014.25047

Recent Trends in Producing Ultrafine

Grained Steels
Hossam Halfa
Steel Technology Department, Central Metallurgical Research and Development Institute (CMRDI), Helwan,
Egypt
Email: hossamhalfa@cmrdi.sci.eg, hossamhalfa@gmail.com

Received 3 May 2014; revised 23 June 2014; accepted 3 July 2014

Copyright © 2014 by author and Scientific Research Publishing Inc.

This work is licensed under the Creative Commons Attribution International License (CC BY).
http://creativecommons.org/licenses/by/4.0/

Abstract
Ultrafine grained steels with grain sizes below about 1 µm offer the prospect of high strength and
high toughness with traditional steel compositions. These materials are currently the subject of
extensive research efforts worldwide. Alloy design is one of the first considered issues, while de-
signing new steel with targeted mechanical properties. However, the alloying content of steel does
not fully determine the mechanical properties, but manufacturing procedure, hot rolling and
cooling parameters, heat treatment parameters etc. are also of vital importance. For instance,
same steel with different processing conditions can exhibit rather large variations in properties.
To be precise, chemical composition with the processing parameters determines the microstruc-
ture, which in turn determines the properties of the steel. Steel is defined as an iron alloy con-
taining C, Mn and Si that are generally used as alloying elements in steel. Micro-alloying elements
such as Nb, Ti V, and B, are considered to be effective, causing strengthening as well as micro-
structural refinement in small quantities below 0.1 wt% (therefore these are called micro-alloy
elements) and are quite generally used in ultrafine grain steel. Substitution alloying elements,
such as Mo, Ni, Cr and Cu are alloyed to suppress phase transformation temperatures, i.e. for
reaching certain level of strengthening, since the strength of steel structures strongly depends on
the phase transformation temperature. Accordingly, the alloy design of ultrafine grains steels with
different structures generally relies on: i) carbon levels, ii) sufficient alloying to obtain the desired
transformation temperature and iii) micro-alloying technology in conjunction with Thermo Me-
chanical Controlled Processes (TMCP). Also, both advanced thermo-mechanical processes and se-
vere plastic deformation strategies are used to produce ultrafine grained steels. Both approaches
are suited to produce submicron grain structures with attractive mechanical properties. This
overview describes the various techniques to fabricate ultrafine grained steels.

Keywords
Ultrafine, Thermomechanical, Severe Plastic Deformation, Structure

How to cite this paper: Halfa, H. (2014) Recent Trends in Producing Ultrafine Grained Steels. Journal of Minerals and Mate-
rials Characterization and Engineering, 2, 428-469. http://dx.doi.org/10.4236/jmmce.2014.25047
 H. Halfa

1. Strengthening Mechanisms of Steel

In principle, the strength of steel is contributed by a number of strengthening mechanisms as follows [1] [2]:
–Intrinsic strength of ferritic iron;
–Solid solution strengthening;
–Precipitation strengthening;
–Grain size strengthening;
–Dislocation strengthening.
The yield strength (Δσy) can then be expressed as:
σ y = ∆σ Fe + ∆σ ss + ∆σ gs + ∆σ dis + ∆σ ppt (1)
In Equation (1), the strength has been expressed as a simple linear sum of individual strengthening mechan-
isms and has been applied in many cases extracting the different strengthening mechanisms in steels with bai-
nitic microstructures [2].
Charleux et al. [3] have discussed the validity of the summing of the strengthening components in expressing
the degree of strengthening in the case of Nb-Ti low carbon bainitic (LCB) steels. According to them, it is ne-
cessary to consider the relative length scales and strength of the strengthening obstacles. If they are significantly
different, a linear addition would be appropriate. For instance, strength of ferrous alloys is derived from the solid
solution strengthening (including base strength of iron) and grain size strengthening. On the other hand, precipi-
tation and dislocation strengthening arise from a similar density and strength of obstacles, which dislocate sam-
ple on the glide plane. For example, Foreman and Makin [4] obtained a Pythagorean flow stress addition law for
discrete obstacles on the slip plane in the case where a similar density of relatively strong discrete obstacles (i.e.
forest dislocations) and relatively weak obstacles (i.e. precipitates) are present. Therefore an alternative way to
express the yield strength as a function of individual strengthening mechanisms is a sum equation where preci-
pitation and dislocation strengthening obey a Pythagorean law:

σ y = ∆σ Fe + ∆σ ss + ∆σ gs + ( ∆σ 2 dis + ∆σ 2 ppt )
1/ 2
(2)

In the following sections different strengthening mechanism will be presented and discussed in detail.

1.1. Intrinsic Strength of Iron

The strength of ferritic iron without significant impurities has been estimated to be 85 - 88 MPa [5] in a low
carbon ferritic steel and this can be considered as the base strength to which the other components will be added
to estimate the overall yield strength.

1.2. Solid Solution Strengthening

Solid solution strengthening arises because the size differences between the solute and solvent atoms and the
strain field that interferes with the dislocations as they move through the lattice causing plastic flow. The most
significant factor behind the solid solution seems to be the size difference between solvent (in steels, Fe) and
solute atoms, but there are also evidences that differences in shear modulus and the relative chemical differences
contribute to solid solution strengthening. Although many of the factors, which contribute to the energetics of
dislocation movement, are known and have been assessed in experimental studies, there is, as yet, no complete
theory and, therefore it is not yet possible to predict the strengthening effect for a particular element from the
first principles [6].
Most practical approach to assess the solid solution strengthening is to use empirical relationships between
alloying additions and tensile properties of steels. These equations are in form:
∆σ ss =ΣAi ∗ wt% (3)
where Ai = factor for strengthening resulting from 1.0 wt% addition of element i. Table 1 shows Ai values for
some alloying elements generally used in LCB steels [2] [5] [7].
A reasonable assumption for aforementioned elements is that a major portion of these element is in solid solu-
tion and available for solid solution strengthening, since with exception of Mo, these elements do not have a
great tendency to precipitate out of solid solution as carbides, nitrides or other complex precipitates in steels. In

429
H. Halfa

Table 1. Values Ai for some alloying elements generally used in LCB steels [2] [5] [7].

Element Cr Si Ni Al Man Cu Mo
Amount/MPa/1 Weight% 0 84 33 30 32 38 11

the case of Mo, the possible precipitation of MoC does not cause significant underestimation of solid solution
strengthening, since the Mo content of investigated steels and the factor of Mo are both low. The very signifi-
cant solid solution strengthening of N that is often reported in the literature is assumed to be zero, since the
presence of strong nitride formers renders it unlikely that any significant levels of N will remain in solid solution.
Carbon in solid solution would also be expected to provide a high level of solid solution strengthening with
coefficient of a similar order to that of nitrogen. However, the solubility of carbon in ferrite and steels contain
strong carbide formers, such as Nb, Mo and Ti at ambient temperatures is very low, so that the contribution from
carbon to solid solution strengthening is assumed to be negligible. In the B treated steels, Ti is added to bind N,
so that the B addition can remain in solid solution and be in the form such that it can be effective for the trans-
formation hardening. However, any significant contribution from solid solution strengthening from B, although
being an interstitial atom, is not expectable since it tends to occupy the sites on prior austenite boundaries rather
than interstitial sites in grain interiors [2]. Solid solution strengthening can be obtained from Si, Mn, Mo and Ni
alloying. Siwecki et al. [8] observed the increase of strength by 30 MPa due to addition of 0.2 wt% of Mo in
microalloyed steels, and also the change of yielding from discontinuous to continuous and improved heat af-
fected zone toughness in Ti-V steels. According to Misra et al. [9], simultaneous additions of 0.3% Cu and
0.15% Ni can further enhance yield strength by 32.4 MPa in a 690 MPa grade steel.

1.3. Precipitation Strengthening

Strengthening effect by the precipitates relies on their interaction with dislocations. Essentially, precipitation
strengthening is achieved by producing a particulate dispersion of obstacles to dislocation movement, which are
produced by the second phase precipitation process. The degree of strengthening is not only dependent upon the
nature of the interaction of precipitates with dislocations, but also on the volume fraction and the size of par-
ticles. In general, there are several mechanisms that can contribute to increase in strength by the precipitation.
These mechanisms include chemical hardening arising from the development of antiphase boundaries, when
dislocation cuts through a particle, coherency strengthening, which relates to coherency strains developed in the
matrix around a coherent precipitate and dispersion hardening due to looping of dislocations around the precipi-
tates in so-called Orowan manner [10].

Strengthening of Steels by Microalloy Precipitates

Three microalloy elements, namely Ti, Nb and V, are widely used as combinations to improve the mechanical
properties of steels. A common feature of aforementioned microalloy elements is their tendency to react with C
and N to form microalloy carbides, nitrides and carbonitrides, which can contribute to precipitation strengthen-
ing. Ti forms an extremely stable nitride, which is virtually insoluble in austenite and may be used for restricting
grain grow growth during processing and removing nitrogen. Excess Ti can precipitate at lower temperatures as
carbides, which contribute to precipitation strengthening [11]. Nb forms carbonitrides, which can precipitate
quite readily in austenite under deformation (so called strain-induced precipitation) and resist recrystallization of
austenite. Further precipitation of the remaining Nb in ferrite gives rise to precipitation strengthening [12]. V is
the most soluble of the three microalloying and does not readily precipitate in austenite. VN is considerably sta-
ble compared to its carbides, so that their precipitation hardening is markedly enhanced with increasing N con-
tent in steel [12]. When precipitation of TiC, NbC or V(C, N) takes place during cooling after the hot rolling it
may occur in two different ways. During the inter-phase precipitation, where nucleation occurs on the auste-
nite-ferrite phase boundary, producing a particle-rich sheet at the location, where the boundary is temporarily
halted. Alternatively, homogeneous nucleation and growth of carbonitrides may occur in the newly formed fer-
rite [13]. Classically, it was believed that total C in steel could not influence homogenous precipitation in ferrite
due to low equilibrium solubility.

1.4. Grain Size Refinement Strengthening

Grain size refinement is one of the best-established strengthening methods in steels, as well as in other metals.

430
 H. Halfa

The well-known Hall-Petch equation describes the relation between ferrite grain size and the yield strength.
σ=
y σ o + k y d −1/ 2 (4)
where σy = yield strength, σo = friction stress, ky = grain boundary resistance and d = grain size.
According to Equation (4) the yield strength is dependent on the reciprocal of square root of the grain size.
This type of relationship has been shown to be valid for grain sizes down to about 1 μm [14].

1.5. Dislocation Strengthening

An increase in dislocation density results in a strength increment, because further motion and production of dis-
locations becomes more difficult. Bainitic ferrite contains a higher dislocation density than polygonal ferrite, for
a part of the dislocation substructure of the deformed parent austenite can be inherited by bainite (plastic relaxa-
tion) and the growth of bainite may be accompanied by the formation of dislocations in and around bainite
(plastic accommodation) leading to additional strengthening [15]. The relationship between dislocation density
and strength increment can be described by:
∆σ =β Gb ( ρ )
1/ 2
(5)
where Δσ = the increase in yield strength, β = a constant, b = Burgers vector, G = shear modulus and ρ = dislo-
cation strengthening.
According to Takahashi and Bhadeshia [16], it might be assumed that for low alloy steels the dislocation den-
sity depends mainly on transformation temperature via the influence of latter on the strength of the parent and
product phases. It should then be possible to treat all of the displacive transformations, such as martensite, bai-
nite and Widmanstätten ferrite together. They have derived an empirical equation between the phase transforma-
tion and dislocation density (in m−2), which is valid over the range 570 - 920 K:
log ρ =9.2880 + 6880 T − 1780360 T 2 (6)
where T = temperature in Kelvin.
Transmission electron microscopy has revealed a dislocation density of about 4 × 1014 m−2 for an alloy with
bainite starting temperature, Bs around 650˚C. This compares with allotriomorphic ferrite obtained in same steel
at 800˚C with a dislocation density of about 0.5 × 1014 m−2. Edmonds and Cochrane [17] reported a value of 1014
m−2 for the dislocation density, attributing to the yield strength by approximately 145 MPa. Hulka and Heister-
kamp [18] gave a value of about 1.5 × 1014 m−2. The dislocation density seems to increase with decreasing trans-
formation temperature. Irregular nature and high dislocation density are typical of low temperature transforma-
tion products (bainitic ferrite, acicular ferrite) formed under continuous cooling.

1.6. Total Strengthening

In total, the contributions of five strengthening mechanisms on yield strength (YS) level of 700 MPa strip are
shown in Figure 1 [19]. However, even higher yield strengths of the order of 1030 MPa may be possible in
HSLA steels with a fully bainitic structure. Simple summation is a simplistic case, marked deviations of the li-
nearity in strengthening have been observed for mixtures of lower bainite/martensite [15] [20].

2. Grain Refinement as a Unique Mechanism for Improving Strength and

Toughness
2.1. Strength
The yield stress for bcc steels processed by different methods is plotted in Figure 2 as a function of the inverse
square root of the grain size for grain sizes ranging from 45 to 0.2 µm. The ultrafine microstructures (grain size
less than 2 µm) were produced by various techniques: the open symbols display the results from the severe plas-
tic deformation (SPD) methods; the full symbols in gray represent the results from the advanced thermome-
chanical process routes (ATP); the full symbols in black show the results from the conventional route (Conv).
The lower yield strength of the 0.13C-0.67Mn-0.14Si (wt%) steel sheet produced by cold rolling and anneal-
ing [21] is shown by the solid diamond in Figure 2 where the grain size varied from 1.6 to 30 µm. The friction
stress σi is about 100 MPa and the grain boundary resistance ky is 551 MPa µm1/2 [21], according to the

431
H. Halfa

Figure 1. Strengthening mechanisms yielding to the YS

level of 700 MPa [19].

Figure 2. Hall-Petch relationship in ultrafine grained bcc steels [22]-[26]. The open symbols
display the results from the SPD methods; the full symbols in gray represent the results from
the advanced thermomechanical process routes (ATP); the full symbols in black show the re-
sults from the conventional route (Conv). The straight lines show the Hall-Petch relation for
different steels.

work of Morrison. Equal-channel angular pressing (ECAP) (at 623 K) followed by annealing at temperatures
between 373 and 873 K produced steels with grain sizes ranging from about 0.23 to 10 µm in a low carbon
(0.15C-1.1Mn-0.25Si, wt%) and a low alloy steel (0.15C-1.1Mn-0.25Si-0.06V, wt%) [22]. The ky value in Fig-
ure 2 (slope of bold line) is smaller in the steel processed by ECAP compared with the results of Morrison
(dashed bold line). The yield stress for a grain size of 30 µm before ECAP is above the value predicted by Mor-
rison, while the yield stress after ECAP is below the line. This phenomenon also reappears in other studies from
both SPD and advanced thermomechanical processes [23]-[29]. That is, while the Hall-Petch relationship in
steels may extend to the submicron range, the parameter ky may decrease. For steels with submicron grain sizes
produced by ECAP, the yield stress for steels with a carbon content less than 0.1 wt% [23] [26] is notably
smaller than for the steels with 0.15 wt% carbon [22] for a given grain size. The reason for this behavior is not
fully understood, but could result from differences in grain size measurement. The data for samples with a dual
phase microstructure (displayed by the sun symbol in Figure 2) [24] do not follow the line predicted by the
Hall-Petch relationship as mentioned above. It seems that a smaller increment in stress is achieved in the dual

432
 H. Halfa

phase steel when the ferrite grain size is refined from 19.4 to 0.8 µm. It is not clear whether this is related to
some variation in the amount and morphology of the second phase after grain refinement.
It should be stressed that in early investigations by Morrison [21], as shown in Figure 2, the different grain
sizes were produced by cold rolling and subsequent annealing at different temperatures. This offered the advan-
tage to alter only one parameter—the grain size. In the investigation by Song [29], (where the initial motivation
was not to measure the value of ky and σi in the Hall-Petch equation), the coarse microstructure consisted of
conventional ferrite and pearlite. When refined into the ultrafine microstructure, however, it comprised ferrite
and fine spheroidized cementite. A smaller ky value was found by Shin et al. [27], which might also be attributed
to the change in overall microstructure (along with grain size) in their study. By use of the ECAP technique, the
initial coarse grained ferrite-pearlite microstructure was severely deformed. After four deformation passes, a
microstructure with finer ferrite and a partially spheroidized pearlite was obtained. Thus, the smaller ky value in
some studies on ultrafine ferrite might be the result of a reduction in the yield strength by replacing harder pear-
lite with softer ferrite and spheroidized cementite in the ultrafine microstructure. The presence of low misorien-
tations between some grains in the ultrafine ferrite may also contribute to the reduced ky value in comparison to
conventional “coarse” ferrite with high misorientations. It should be mentioned that most of the submicron mi-
crostructures measured for the SPD technique consist of large quantities of low-angle grain boundaries, and
grain dimensions measured refer to the thickness of stretched microbands, which is not the same as average
grain diameter. Further consideration of grain morphologies and appropriate characterization methods may be
worthwhile to define the Hall-Petch relationship more accurately.
Unfortunately, the estimation of the contribution of the grain size in bainitic structures is more complicated
than in simple ferritic steels. The nature of bainite, lath size and shape as well as carbide size and distribution,
vary systematically with the temperature of transformation. All features are refined at low transformation tem-
peratures. Furthermore, situation becomes far more complicated due to the fact that in bainitic structures, boun-
daries can be present with both low and high angle misorientations [2]. However in lath type, rather than poly-
gonal structures, several publications suggest that the strength is related to reciprocal of some characteristic
scale in microstructures, rather than d−1/2 type relationship in the Hall-Petch equation [2] [15] [28]. Hence, yield
strength can be expressed as:
σ=
y σ o + k y d −1 (7)
where σy, σo and ky have identical meanings to Equation (4), but these have different values. The microstructural
factor relating to grain size d in Equation (7) is not completely clear. Brozzo et al. [30], in their studies on the
low C bainitic steels, found a clear relationship between lath width and strength but only a weak correlation with
packet size. This would indicate that slip across laths is the controlling factor.

2.2. Impact Toughness

Steel is still one of the traditional engineering materials widely used in industry. The high strength and high
toughness steel is the most desirable product. However, in fact, strength and toughness are normally contrary. If
the strength of steel increase its toughness normally decreases and vice versa. The composition and microstruc-
ture of the steel are primary factors controlling the strength and the toughness. Thus the grain refinement is a
highly effective method to improve both the strength and the toughness [31]-[33].
Toughness is conveniently characterized by the Charpy impact test [34]-[36] in terms of (i) the Charpy Tran-
sition Temperature (CTT), and (ii) the ductile-to-brittle transition appearance temperature, DBTT. CTT is eva-
luated, from the Charpy absorbed energy transition curve, as the absorbed energy corresponding to half the val-
ue of the upper shelf energy. The DBTT is defined as the temperature for 50% cleavage on the fracture surfaces
of the Charpy impact specimens [37] [38]. Conventional coarse grain ferrite/pearlite (CGF/P) steels often show
a close similarity of these two measures of transition temperature, that is CTT-DBTT. The high absorbed energy
in the upper shelf region is associated with ductile fracture by micro-void coalescence (i.e. dimple rupture)
whereas the low absorbed energy in the lower shelf region is associated with brittle cleavage fracture. In contrast,
UGF/C steels had a DBTT was much lower than the CTT, attributed to the fact that the fracture mechanism of
the ductile to brittle transition was caused by a different fracture mechanism: the decreased energy absorption by
ductile fracture [38].
For conventionally processed low carbon steels with ferrite grain sizes greater than 10 µm, Pickering’s clas-

433
H. Halfa

sical work indicated that the ductile-to-brittle transition temperature (DBTT) is a function of strengthening me-
chanism [38]. For a yield strength increase of 9.8 MPa, if the strengthening is by dislocation, the DBTT will in-
crease by 6 K; if by dispersion strengthening, the DBTT will increase by 4 K; if by grain-size refinement, how-
ever, the DBTT will decrease by 10 K. The effect of grain size on DBTT is characterized by Hall-Petch style
formula:
DBTT= A − kd −1/ 2 (8)
and
DBTT= A − kln d −1/ 2 (9)
where constants A and K depend on metallurgical factors other than the grain size, and d is grain size. With these
relationships, it is expected that ultrafine grained steels would have improved impact toughness.
The reported impact toughness data from ultrafine grained steels are still limited, partly due to the difficulty in
obtaining large enough specimens from the laboratory-scale samples. Figure 3 shows a set of recent results,
comparing the DBTT of two steels with ferrite sizes of 6.8 and 1.3 µm, respectively. The upper shelf energy of
the ultrafine grained steel is lower, and the transition region occurs over a wider range of temperature, compared
with the coarser grained steel. The DBTT for the ultrafine grained steel is lower than the coarser grained steel. A
detailed explanation of the DBTT curves is provided in references [39] [40].
The DBTT results reported by Hanamura et al. [38] also confirm that the low-carbon steel with ultrafine
grained ferrite/cementite microstructure has a much lower DBTT than that of the conventional ferrite/pearlite,
quench/tempered, or quenched microstructure. Unlike results of Song et al., results of Hanamura et al. show the
upper shelf energy of the ultrafine grained microstructure is as high as that of the coarser grained ferrite/pearlite
microstructure for the same steel (Figure 4).
The effective grain size (deff) is a useful measurement to characterize the effect of grain size on impact tough-
ness. Instead of using the directly measured grain size, Hanamura et al. [38] have proposed to use the effective
grain size as the variable to measure the impact toughness. The deff is defined as the unit crack path in which a
cleavage crack goes through in a straight fashion to form a facet, corresponding to the microstructural unit hav-
ing a specific crystallographic orientation and bounded by large-angle grain boundaries. The deff can be experi-
mentally measured from the fractography. Using the deff concept, the four types of microstructure are ranked as
deff = 8 µm for the ultrafine grained ferrite/cementite (UF-F/C) microstructure, 20 µm for the ferrite/pearlite (F/P)
microstructure, 25 µm for the quenched and tempered (Q/T) microstructure, and 100 µm for the as-quenched (Q)
microstructure. This ranking is the same as the DBTT ranking, with smaller deff having a lower DBTT. Further,

Figure 3. Effect of test temperature on Charpy impact energy

of two steels with different ferrite grain sizes [40]. The sym-
bol dα indicates the average ferrite grain diameter. DBTT sub-
size refers to ductile-to-brittle transition temperature meas-
ured with sub-sized specimen (ligament size of 3 × 4 mm2).

434
 H. Halfa

Figure 4. Charpy impact energy as a function of test tempera-

ture for ferrite/pearlite (F/P), ultrafine ferrite/cementite (UF-F/C),
as quenched (Q), and quench and tempered (Q/T) steels [38].

it is found that the deff number is determined by the ferrite grain size for F/P, by the prior austenite grain size for
Q, by the martensite packet size for Q/T, and by the ferrite grain size for UF-F/C microstructure. With such
knowledge, the impact toughness can be tailored by the microstructure design. Statistically, the impact tough-
ness for low-alloy steels follows an inverse trend against the yield strength, as shown in Figure 5, in which the
shaded region on the left side of figure indicates the data distribution. Conventional quench and tempering (QT)
can significantly increase the yield strength, but greatly decreases the impact energy. Ultrafine grained steels, as
processed with the “tempforming” (TF) process, however, can have 16 times higher impact toughness than the
conventional quench and tempered steel.
The extremely high impact toughness for this “tempformed” steel is owing to the ultrafine, elongated, fibrous
ferrite grains with <110> crystalline orientation along the rolling direction, interspersed with nanometer-sized
carbides. With such a microstructure, the fractured specimens showed fibrous delamination that is thought to re-
lax the triaxial stress conditions ahead of the advancing crack tip, thus leading to high impact energy [41].

3. Grain Refinement for Saving Materials and Saving Energy

Nowadays, the structural materials for aerospace, shipbuilding and offshore steels, pressure vessels and automo-
tive applications and any other applications that are tied to power consumption are increasingly required to be
energy efficient. The development of high-strength steel is an important way of reducing vehicle weight, amount
of material used (reducing material cost) and achieving the purpose of energy saving and emission reduction.
The demand to produce automobiles which fulfill the requirements like, passenger safety, vehicle perfor-
mance and fuel efficiency, has been the biggest challenge faced by the steel industry for the last couple of dec-
ades [42] [43]. In response the steel industry has developed advanced high strength steels (AHSS) including dual
phase (DP), transformation induced plasticity (TRIP), complex phase (CP) and martensitic steels (MART).
These steels are characterized by improved formability and crash worthiness compared to conventional steel
grades, such as pearlitic steels. Currently, advanced high strength steels (AHSS) are extensively used in the auto
industry and the projections are that the weight percentage of AHSS steel will increase to 35% by 2015, here as
mild steel decrease from 55% to 29% in bodies and closures of light vehicles [44]. The rationales for increased
use of the AHSS in the automotive industry are as follows: (1) the reduction of the car weight resulting from the
use of high strength thinner gauge sheet steel, reducing the fuel consumption; (2) Increased passenger safety by
an improved crash worthiness; (3) The strong competition from the light-weight materials, such as Al and Mg
alloys and plastics. Figure 6 is a schematic of Volvo-2009 model [45], showing the different classes of materials
used for designing the car body.
Riding the trend, there is considerable effort to develop nanostructured steels that will meet such demands.
But current effort has been focused on ultrafine-grain (UFG) ferrite single-phase steels, multi-phase steels, and
nanostructured Bainite steels. Among various methods of strengthening steel, grain refinement is a method that
can enhance strength with no deterioration in toughness [46]. In recent years, a variety of methods have been

435
H. Halfa

Figure 5. Charpy V-notch impact energy absorption of the

low-alloy steel as a function of yield strength at room temper-
ature [41]. The steel that was “tempformed” at 500˚C (TF)
shows large impact energy as compared to that of the steel
that was conventionally quenched and tempered (QT), also at
500˚C. Annealing of TF steel at 700˚C degraded the impact
energy to conventionally processed steels.

Figure 6. A schematic of Volvo-2009 model, showing the dif-

ferent class of materials used for designing the car body [45].

developed to produce ultrafine-grained steels, including strain-induced ferrite transformation, large-strain warm
deformation, intercritical hot rolling, multi-directional rolling and cold-rolling plus annealing of martensitic steel.
The grain size is refined to 1 - 3 µm [47]-[49]. But in commercial hot-rolled Nb-Ti and Ti-Mo microalloyed
strip steel, the grain size could be controlled within only 5 - 10 µm [1] [50].

4. Methods of Producing Ultrafine Grained Steels

4.1. Production Ultrafine Grained Steels by Micro-Alloying
High-strength low-alloy (HSLA) steels are a class of steels developed to achieve properties superior to those of
the ferritic + pearlitic steel and comparable to those of low alloy quenched and tempered martensitic steels.
HSLA steels are designed to achieve their desired mechanical properties by the development of microstructures
through controlled thermomechanical processing (TMP) and the steel is produced in its final form by a conti-
nuous hot deformation process, rolling, or forging, which comprise the TMP. Most HSLA steels are microal-
loyed with small additions (0.1 wt%) of niobium, vanadium, and titanium which control microstructural evolu-

436
 H. Halfa

tion during TMP through the formation of carbonitride precipitates.

With the development of the micro-alloying technology the elements of Nb, Ti, and V are used widely in the
production to produce ultrafine grain steels (UFG-steels). During solidification from melt, they combine with C
and/or N to form carbide, nitride and/or carbonitride precipitates. Figure 7 shows the correlation between the
micro-alloying content and the solubility temperature for the precipitate present in steel 16 MnNi4 [51]. The so-
lubility temperatures for the precipitates present in the steel are 1045˚C for the VC, 1130˚C for the VN, 1168˚C
for the TiC, 1682˚C for the TiN, 1338˚C for the NbC and 1073˚C for the NbN [51].
These fine precipitates play an effective role by retarding recrystallization (and therefore, increasing the re-
crystallization stop temperature) that usually follows deformation and thus, helps to retain the accumulated
strain and deformed structures of austenite grains. There have been several studies on the recrystallization of
carbon steels and Nb microalloyed steel [52]-[55], and various models have been proposed for predicting the re-
crystallization of austenite.

4.2. Role of V Micro-Alloying

In high strength low alloy steels (HSLA), it is common practice to make additions of elements such as Ti, Nb, V
for austenite grain size control [56] [57]. These elements have a high chemical affinity for N and C and form
compounds, carbonitrides, which can control austenite grain growth. Special attention has to be paid to vana-
dium microalloying addition. Vanadium is a useful microalloying element which improves the mechanical
properties of HSLA steels. In quenched and tempered steels, vanadium increases their hardenability and me-
chanical properties after tempering [58]. It can be used in dual role. Because of the high chemical affinity to ni-
trogen and carbon it forms carbonitrides V(C, N) which controls the austenite grain size. Dissolved vanadium
decreases the rate of austenite decomposition and thus increases the hardenability. In high strength low alloy
steels, an increase of hardenability at low austenite grain size was observed contrary to the effect of austenite
grain size on the hardenability of common steels. This effect is explained by the Garbarz and Pickering hypothe-
sis [59] that pinning the austenite grain boundaries by undissolved carbonitrides particles creates the possibility
for segregation of dissolved alloying element atoms on immobile grain boundaries. The resulting decrease in the
grain boundary energy reduces their potential for the nucleation of non-martensitic products as was observed in
boron steels [60].

4.3. Role of Nb Micro-Alloying

The use of niobium as microalloy element in steel for grain refinement is widespread. NbC usually precipitates
after deformation of austenite, can pin dislocations so that recovery and recrystallization of deformed austenite
can be intensively retarded [60]-[62].

Figure 7. Correlation between the micro-alloying contents (M%) and

the solubility temperature for the precipitates present in the steel 16
MnNi4 [51].

437
H. Halfa

Nowadays, most of ferritic-perlitic precipitation hardening steel grades are microalloyed steel. These steels
after rolling or forging process would be cooled as completely controlled. The properties of these steel grades
would be affected by solidification microstructures, thermomechanical process and cooling process after rolling
[60]. Niobium has a three-fold influence on the mechanical properties of steel which are as grain size refinement
during thermomechanical hot forming, precipitation hardening and lowering the γ to α transition temperature.
Grain refinement is the only mechanism that simultaneously increases strength, toughness and ductility. Nio-
bium-microalloyed steel has become a standard material in plate and strip for line pipe, automotive and con-
struction use. Until now, the high potential of microalloyed high strength steel has not been used to the same
extent in long products.
Nb(C, N) precipitates that have formed and grown at high temperature and in austenite phase prevent from
grain coarsening in the subsequent stage of hot deformation. Other diffusion controlled process that occur with
solution of niobium in austenite are retarding of austenite (γ) to ferrite (α) transformation that cause to increase
nucleation of ferrite and reduce grain growth rate, forming of quasi-equivalence structures like bainite and fi-
nally appearance very fine Nb(C, N) precipitates during transformation that being coherent interface cause to
increase strength with precipitation hardening mechanism [61] [62].

4.4. Role of Ti Micro-Alloying

In modern industry, obtaining excellent combination of high strength and high toughness is a target for steel. It
is well known that Nb, V and Ti microalloying elements play important roles in it [63]-[65]. While the microal-
loying elements precipitate as carbides or nitrides in austenite, the precipitates can lower the grain growth rate
by pinning the grain boundaries [66] [67]. The obtained fine grain microstructure can enhance the strength and
toughness of steels obviously [68]-[70]. Due to the high price of niobium and vanadium, the development of ti-
tanium microalloyed steels are attracted much more attention recently [71]-[74]. There are some researches of
precipitation effects on microstructure and mechanical properties in Ti-bearing steels [74]-[76]. But steel alloyed
with titanium alone is seldom studied especially in low carbon medium manganese martensitic steel. According
to the thermodynamic analyses [77] [78], the main forms of titanium precipitate are TiN, Ti4C2S2 and TiC or
Ti(C, N) composite particles. The role of TiN particles in austenite grain size control is well known and the me-
chanism by which they exert this influence may be explained by Zener and Gladman’s expressions for pinning
forces [1] [79], which relate the size and fraction of precipitates. However, the precipitation temperatures for
TiN, Ti4C2S2 and TiC particles are above 1500˚C, 1200˚C and 1000˚C, respectively. Due to the higher precipita-
tion temperatures of TiN and Ti4C2S2 particle, they tend to grow to larger particles, and this is disadvantageous
for the mechanical properties. Consequently, TiCs may have the most important effect on steel properties for
their smaller size.

4.5. Role of Nb-Ti Micro-Alloying

The use of niobium and titanium as microalloy elements in steel for grain refinement is widespread. TiN preci-
pitates, forming during solidification, can powerfully inhibit motion of austenite grain boundaries while NbC,
which usually precipitates after deformation of austenite, can pin dislocations so that recovery and recrystalliza-
tion of deformed austenite can be intensively retarded [80] [81]. It is generally believed that, when steels are
heated up to austenite region, the TiN precipitates are the most stable and are known to have a dissolution tem-
perature above the iron liquidus temperature but NbC precipitates dissolve away rapidly [82] [83]. However,
when Nb and Ti co-existed in the same microalloyed steel, the effect of their interaction of formation and ther-
mo-stability of precipitates, especially during solidification and austenization, was frequently neglected. The
approximately solubility temperatures for the precipitates present in the produced steels are shown in Figure 7.
The different precipitates present in the steel due to Ti-Nb micro-alloying were analyzed in terms of size,
morphology, and chemistry. They can be classified into types I - IV based on the size and morphology of the
precipitates, and are summarized in Table 2. Type I are rod-like intergranular (Fe, Mn)3C precipitates. The type
II precipitates are TiN containing small amounts of Nb and are of the size range 120 - 500 nm. The type III pre-
cipitates identified as (Nb, Ti)C are ≈10 - 200 nm size and randomly distributed in the matrix, and type IV are
spherical or needle-shaped (Nb, Ti)C precipitates (3 - 5 nm) that nucleated preferentially on sub-boundaries and
dislocations in ferrite. Type I and II are generally undesirable from the viewpoint of toughness since they are
known to promote cleavage fracture, while type III and IV are strengthening precipitates.

438
 H. Halfa

Table 2. Precipitate observed in 770 MPa Nb-Ti hot rolled steels [1].

Type Size Morphology Precipitate

I 1 - 1.5 µm in length Intergranular rod-like (Fe, Mn)3C

II 120 - 400 nm Cuboid, round, oblong, ellipsoidal (Ti, Nb)N

III 10 - 120 nm Spherical, plate (Nb, Ti)C

IV 3 - 5 nm Needle-like (Ni, Ti)C

4.6. Role of Boron

Boron (B) can be an effective element in enhancing the hardenability of the steel and in obtaining a bainite
and/or martensite dominant structure. As a typical feature of B is its alloying of trace amounts; the controlled
concentration of B is ranging from 10 ppm to 30 ppm. B alloying is not indispensable in low carbon bainitic
(LCB) steels and it is not always used in steels with yield strength from 500 MPa to700 MPa [84]. On the other
hand, for the LCB steels with yield strengths above 700 MPa [85], such as X120 line-pipe steels, B alloying is
found to be crucial in order to promote required lower bainitic microstructures for high strength and toughness,
besides improving the weldability and maintaining alloying cost at low levels. The hardenability-enhanced ef-
fect of B is based on its non-equilibrium segregation at grain boundaries. There are several explanations, how
this type of segregation improves the hardenability of steels [86]:
—The non-equilibrium segregation to austenite grain boundaries reduces the grain boundary energy and pre-
vents nucleation of ferrite.
—B can reduce the coefficient of self-diffusion of iron at grain boundaries, thereby reducing the nucleation
sites for ferrite. Since the grain boundaries are preferential nucleation sites for ferrite, when B segregates to
grain boundaries, these sites will become ineffective.
—Fine borides form along the grain boundaries. Being coherent with the matrix, ferrite is difficult to nucleate
at the interface between boride and matrix. (This explanation contradicts with the assumption of atomistic B be-
ing effective in enhancing the hardenability).
In general, low carbon micro-alloyed steels have 0.05 wt% C and 1.5 wt% Mn and utilize micro-alloying
concepts to attain a fine-grained microstructure. The fundamental basis for the development of ultra-high
strength 770 MPa hot rolled steel is to obtain ferrite-bainite microstructure in the hot rolled product through
controlled rolling and alloy design. The two main elements considered for obtaining a bainitic microstructure
were boron and molybdenum. Boron retards the nucleation of ferrite by segregating to austenite-ferrite bounda-
ries, where it inhibits ferrite nucleation through strong interaction with lattice defects such as dislocations and
vacancies [87] [89]. Thus, boron effectively moves the ferrite C-curve to longer times.

4.7. Role of Vanadium-Nitrogen Micro-Alloying

The mechanism of grain refinement caused by addition of nitrogen has been extensively investigated. Ochi et al.
[90] suggested that N promote the formation of intragranular ferrite, and refine the grain in vanadium steel.
Wang et al. [91] further confirmed that the addition of N to V microalloyed steel could make more vanadium-
containing precipitates in the form of carbonitrides which acted as nucleus of ferrite formation, and raised the
nucleation rate of ferrite, as well as resulted in grain refinement of ferrite. It well known that, vanadium carbides
did not take part in pinning process. On the contrary, vanadium carbonitrides can be assumed to have a higher
solution temperature than pure vanadium carbides, between 1000˚C and 1200˚C, depending on the vanadium
and nitrogen content [57].
Zhao et al. [92] indicated that, in ferritic-pearlitic microalloyed steel, the area fraction of ferrite increased
from 21% to 38%, and the averaged grain size decreased from 10.3 µm to 6.2 µm, when the nitrogen content
was enhanced from 30 ppm to 210 ppm and normalization was performed at 930˚C. An increase in reheating
temperature brought elevated strength at an expense of toughness. Improved combination of yielding strength in
650 MPa and toughness in 48 J at −20˚C can be obtained in 33 Mn2V stee1 with nitrogen content of 140 ppm at
reheating temperature of around 930’C [92].
On the other hand, the higher silicon contents in SiV and SiVN steels increase the activity of carbon in these

439
H. Halfa

alloys thus stabilizing carbides and carbonitrides [93]. Therefore, the austenitizing temperature of 1200˚C (heat
treatment temperature of investigated HSLA steels) is necessarily not high enough to dissolve all VN or V(C, N)
particles and some of them likely restricted the austenite grain growth during the heat treatment. This was, fur-
ther, confirmed by IDS calculation which gave the following temperatures for the start of precipitation of VN:
1085˚C for 38 MnSiV5, 1120˚C for SiV and 1265˚C for SiVN, respectively [93]. Another explanation for the
finer ferritic grain size in vanadium containing steels is the inter-phase precipitation of vanadium carbonitrides
which slows down the austenite-ferrite transformation giving more time for ferrite nucleation [94] [95]. Ac-
cording to the results of this study it is not excluded that also a high silicon (Si > 1%) causes a smaller ferritic
grain size, e.g. through higher AR3 temperature since the nucleation of ferrite starts earlier.

4.8. Summary
In practice, more than one microalloying element is often added, each for a different purpose. Hence, the low
solubility of TiN makes it a good choice to restrain grain growth during reheating. Nb(C, N) is only sparingly
soluble below 1000˚C, and it is a good choice if one wishes either to restrain grain growth below this tempera-
ture or more importantly to precipitate in deformed austenite. Excess Ti, Nb can precipitate at lower tempera-
tures as carbides, which contribute to precipitation strengthening. VC, on the other hand, is much more soluble
and is added so that it can remain in solution and precipitate later, forming a fine hardening dispersion in the fer-
rite. The presence of more than one alloying element can result in the precipitation of complex multi-component
carbonitrides such as (Nb, V) (C, N) or (Nb, Ti) (C, N). The solubility of those complex carbonitrides can be
found to a first approximation from the solubility of the individual carbides and nitrides. Finally, Nb and Ti can
be added to low alloy steels to form carbides and nitrides with a totally different purpose. In the “interstitial free”
steels, Nb and Ti are added to act as “scavengers” for C and N. They form low-solubility precipitates that result
in an almost interstitial free ferrite.

4.9. Production Ultrafine Grained Steels by Heat Treatment

Grain refinement is an effective way to improve both strength and toughness. Since the grain size of austenite
decomposition products decreases with decreasing austenite grain size, many efforts have been made to refine
austenite grains. In the Thermo Mechanical Controlled Processes (TMCP), recrystallization andnon-recrystalli-
zation rolling are used to refine austenite grain, of which the minimum size or thickness is 10 - 20 µm in C-Mn
steels and 5 - 10 µm in steels microalloyed with Ti and Nb [96]. Controlled austenitization is another effective
way to obtain ultrafine grained austenite in heat treatment steels, such as rapid cyclic transformation, reversion
from tempered and cold rolled martensite. The former, which includes 2 - 4 cycles of rapid austenite-martensite
transformation, was employed to obtain austenite grain of 1 - 10 µm [97]-[99]. The latter including tempering
and further heavily cold rolling was attempted to refine austenite grain size to 1 - 5 µm [100] [101].

4.9.1. Phase Transformation through Cyclic Heat Treatment

Grain size refinement of steel, by temperature cycling can be done by repeated alpha-gamma phase transforma-
tions [102] [103]. One of the effective methods of the previous austenite refinement is refinement by tempera-
ture cycling, i.e., by cyclical repeated heating and cooling of steel. Refinement of steel microstructure by tem-
perature cycling can be achieved by a cooling rate that provide diffusional transformations of austenite to pear-
lite, or by rates that provide transformations of austenite to bainite, or diffusion-less transformation to martensite
[104]-[106].

4.9.2. Cyclic Quenching Method (Repetitive Rapid Heating and Quenching)

In previous works, the effect of heating rate on the refinement of steel austenite using a mixture of bainitic fer-
rite and retained austenite as the starting material were studied. During conventional continuous heating rate, as
ranged from 2˚C/s to 100˚C/s which is related to a moderate superheating, would allow the austenite grains to
direct grow from the previous retained austenite present in the initial microstructure, along the ferrite plate. In
this case, the austenite will inevitably grow in an acicular morphology until the original austenite grain structure
is recovered without request for nucleation of new austenite grain, resulting in the so-called memory effect and
little grain refinement [107]. Some other early works [108] [109] also reported the similar observations. Howev-
er, when a very slow continuous heating is imposed and correspondingly a limited superheating achieved though,

440
 H. Halfa

the retained austenite decomposition into the cementite or carbide can occur in an initial bainitic or martensitic
steel, as in the 2.25Cr-1Mo steel for example [110], on early heating stage. This will destroy the memory effect
and lead to new austenite nucleation at prior austenite grain boundaries and the precipitates on the following
austenitization heating.
On the other hand, a high degree of superheating, as a result of extremely rapid heating to an elevated austeni-
tisation temperature, will significantly increase both the driving force for reverse α → γ reaction and atom mo-
bility. This make it possible for some new austenite grains to nucleate at all possible sites, including the prior
austenite grain boundaries, the adjacent ferrite plate interfaces and even inside the plates, even if the retained
austenite film will thicken simultaneously. The austenite will then grow at a high nucleation ratio and develop
an equiaxed and ultrafine-grained morphology. This suggests that the austenite grain can be effectively refined
when extremely rapid cyclic α → γ → α phase transformation occurs in a mixture of bainitic ferrite and retained
austenite under a high superheating situation.
In earlier work done by Wang et al. [110], they were studied the effect of extremely high degree of super
heating on the refinement of steel austenite. They stated that, An extremely high degree of superheating for the
reverse α → γ transformation, which was successfully performed in a initial microstructure composed of bainitic
ferrite and retained austenite as a result of extremely rapid resistance heating up to an elevated austenitization
temperature, can prevent restoration of the previous coarse-grained austenite and lead to the formation of an ul-
trafine structure during the subsequent rapid cooling.

4.10. Production Ultrafine Steels by Advanced Thermomechanical Processes

Recent researches involving metallic materials can lead to technological innovations [111]. Both advanced
thermomechanical processes and severe plastic deformation strategies have been developed to obtain ultrafine
ferrite grain with size close to 1 μm in low-carbon low-alloy steels [37]. Advanced thermomechanical processes
involving modification to conventional large-scale processes can be optimized to operate in deformation condi-
tions where they beneficially exploit solid-solid reactions such as recrystallization, precipitation, and phase
transformation. Ultrafine grain size has been obtained in steels through deformation near or in the intercritical
region by exploiting strain-induced dynamic transformation [112]-[114]. Ferrite dynamic recrystallization can
be exploited straining in warm condition inside the ferrite domain [115] [116]. Also, ultrafine or nanocrystalline
structures has been achieved by warm or cold deformation of martensite starting microstructure [117]-[119].
Two types of procedures are used to deform austenite: conventional or controlled thermomechanical pro-
cessing [120]. The former consists of multi-deformation schedules aimed at changing the shape, while the
second also aims to control the microstructural evolution. Controlled thermomechanical processing has been
successfully industrialized in modern steel mills and can be defined as disciplined deformation schedules under
continuous cooling and controlled conditions, aimed at attaining fine-grained microstructures [121]-[123]. This
kind of processing can be separated in four different stages, as the temperature decreases. Figure 8 is a sche-

Figure 8. Schematic representation of the thermomechanical treat-

ment for microalloyed steel, indicating the critical temperatures
[126].

441
H. Halfa

matic representation of the thermomechanical treatment for microalloyed steel, indicating the critical tempera-
tures (Ts, Tnr, AR3, and AR1). In the first stage, grains coarsened by soaking at temperatures above Ts are refined
by the repetition of deformations and recrystallizations at high temperatures. The second stage takes place under
conditions in which recrystallization is no longer completed during inter pass times due to strain-induced preci-
pitation [124] [125], i.e., below the non recrystallization temperature (Tnr). Grains in this stage have a pan-
cake-like shape and dislocation substructures are created inside the grains.
In the third stage, deformation takes place in the phase transition region, i.e., in the temperature range be-
tween the start of ferrite formation (AR3) and the end of ferrite transformation (AR1). Ferrite nucleates within and
at grain boundaries. In this stage, austenite continues to deform and the transformed ferrite begins to be strained.
In the fourth stage, a variety of microstructures can be obtained during cooling, depending on the cooling rate
and the stage in which the deformation was interrupted. After the first deformation stage, when the material is
air-cooled, the ferrite grains are relatively large due to grain growth during cooling. After the second stage, the
grains are smaller. In the third stage, increasing the cooling rate causes the grains to become finer and sub-
structural dislocation occurs inside the strained ferrite grains. During conventional thermomechanical processing,
the multi-deformation schedule is similar to that of the first stage, where the recrystallization kinetics is very fast.
Thus, static recrystallization occurs during inter pass times and no strain accumulates from one pass to another.
It is well-established that the start temperature of ferrite formation (AR3) and the end temperature of this trans-
formation (AR1) depend on the cooling rate. These temperatures decrease as the cooling rate is increased. When
higher cooling rates are imposed, austenite is present at temperatures below that of equilibrium between the
phases (Ae3 and Ae1). Thus, it is possible to deform unstable austenite [37]-[116]. Upon deformation, strain-in-
duced dynamic phase transformation (austenite to ferrite) can take place. New ferrite grains and transformed
ferrite during cooling are strained together with austenite and continuous dynamic recrystallization of ferrite can
occur. This technique has been used to produce ferrite grain sizes as fine as 2 - 5 µm via recrystallization-con-
trolled rolling or by conventional rolling followed by accelerated cooling [127].

4.10.1. Recrystallization of Austenite during Hot Deformation

An important mechanism that is widely used for grain refinement in steels is dynamic recrystallization during
hot deformation [128]. This technique has been used to produce ferrite grain sizes as fine as 2 - 5 µm via recrys-
tallization-controlled rolling or by conventional rolling followed by accelerated cooling. In recrystallization-
controlled rolling fine precipitates restrict austenite grain growth after deformation. Recrystallization controlled
rolling is often used in conjunction with accelerated cooling and micro-alloying in order to effectively refine the
grain size. Accelerated cooling is used to increase the cooling rate through the transformation zone in order to
decrease the transformation temperature. In principle, a lower transformation temperature results in a higher fer-
rite nucleation rate due to a higher under cooling, and a decreased growth rate. Conventional controlled rolling
has been implemented in many commercial operations through the addition of microalloying elements especially
strong carbide/nitride formers elements. The addition of small amounts (>0.1 wt%) of strong carbide/nitride
formers elements such as Nb, Ti, V, and Zr, with Al also normally present, to the austenite (‘‘microalloying’’) is
extremely important in commercial low alloy steels. Their main role is to precipitate from austenite-forming
carbides/nitrides or complex carbonitrides. The solubility of these elements is small, so that high austenitizing
temperatures in excess of 1100˚C are usually required. This increases the density of sites for ferrite nucleation.
The lowest solubility product is that of TiN followed by NbC, TiC, and VN, with VC being by far the most so-
luble carbide. Precipitation processes from the austenite can be divided in three groups:
1) Precipitation from undeformed austenite: this can happen after reheating of the steel or during cooling from
a high soaking temperature. The carbides/nitrides formed in this way, with size = 20 nm, are intended to restrain
grain growth by pinning the grain boundaries.
2) Precipitation from deformed austenite: it is normally accepted that deformation significantly accelerates
precipitation. In turn, this precipitation can delay the onset of austenite recrystallization that is invaluable for the
controlled rolling of the austenite.
3) Precipitation during austenite-ferrite transformation: if enough alloying element remains in solid solution
after high-temperature processing, carbide/nitride precipitation can occur during the austenite-ferrite transforma-
tion. These precipitates form at the austenite-ferrite transformation front resulting in precipitates arranged in pa-
rallel planes, which is often called interphase precipitation.

442
 H. Halfa

4.10.2. The Martensite Thermomechanical Treatment

Martensite treatment is one of the known thermo-mechanical processes that can be used for the grain refinement
of metastable austenitic stainless steels [129]. The as-cast specimens were first homogenized and then hot forged
in order to prepare a suitable microstructure for the subsequent martensite treatment. This treatment may be
consisted of single [130] [131] or repetitive [132] [134] stages of cold rolling followed by reversion annealing.
In single stage, cold rolling was carried out with the reductions of 10% - 95% followed by annealing at temper-
ature of 850˚C for 15 - 1800 s, as shown in Figure 9. This process results indicated that the specimen was rever-
sion-annealed at 850˚C for 30 s exhibited the smallest average austenite grain size of 65 nm with more than 86%
austenite [130]. In repetitive martensite thermomechanical treatment, the first stage was consisted of cold rolling
to 70% thickness reduction followed by annealing at 850˚C for short annealing durations (60 second), while the
second stage was comprised of cold rolling to 60% thickness reduction followed by annealing at 850˚C up to 60
second, as shown in Figure 10. The smallest grain size of 80 ± 10 nm with a microstructure consisted of auste-
nite and small amount of retained martensite was achieved by secondary annealing for 30 s. Increasing the an-
nealing time to 60 second led to the formation of fully austenitic microstructure but the grain size of about 260 ±
40 nm. This microstructure possessed the yield strength of 1 GPa and the total elongation of 30% [132]. Table 3
and Table 4 show the single/ repetitive martensite thermomechanical treatment for different ultrafine grain aus-
tenitic stainless steel.

Table 3. Effects of different processing parameters on mechanical properties of 301 nano-ultrafine steel [133].
Average UTS Yield strength Elongation Hardness
Processing conditions Steel Structure εc
grain size (MPa) (MPa) (%) (HV)
35% CR at −10˚C + 750˚C/10min + 60 CR
301 95% γ 70 nm - 1970 - 603 0.5
at −10˚C + 850˚C/1min
62% CR at 25˚C + 800˚C/1s 301LN α+γ 520 nm - 850 45 260 -

90% CR 600˚C/30min 301 15% γ 280 nm - 1209 - 370 -

90% CR 750˚C/30min 301 95% γ 1.7 µm - 539 - 165 -

90% CR 900˚C/30min 301 80% γ 5.8 µm - 490 - 150 -

90% CR at −196˚C + 750˚C/3min 301 95% γ 2.5 µm - - - 330 0.9

Coarse grained 301 γ 15 µm - - - 220 -

63% CR + 800˚C/1s 301LN 93% γ 540 nm 1070 700 35 215 -

63% CR + 800˚C/10s 301LN 93% γ 1 µm 1027 630 40 192 -

60% CR + 800˚C/1s 301 α+γ 570 nm 1042 704 35 216 1

95% CR at −10˚C + 800˚C/10s 301 95% γ 250 nm 1470 966 36 422 0.5

Table 4. Mechanical properties of 201L stainless steel at different stages of the repetitive thermo-mechanical
process at room temperature [130].

Processing conditionsa Average grain size UTS (MPa) Yield strength (MPa) Elongation (%) Hardness (HV)

SA at 1100˚C for 150 min 27 µm 1030 330 48 230

95% CR - 1950 - 4 546

95% CR + 850˚C/30s 65 nm 1780 1485 33 393

95% CR + 850˚C/180s 140 nm 1710 1075 37 291

95% CR + 850˚C/600s 810 nm 1420 870 34 262

95% CR + 850˚C/1800s 1.4 µm 1160 780 25 241

a
SA: solution annealing; CR: cold rolling.

443
H. Halfa

Figure 9. Schematic illustration of the thermomechanical pro-

cess to obtain the nano grained structure in a 201L stainless
steel, As and Ar are the reverse transformation start and finish
temperatures, respectively [130].

Figure 10. Schematic illustration of the repetitive thermomechan-

ical process used to obtain nan/ultrafine grain structure in 201
stainless steel [132].

4.10.3. Strain-Induced Ferrite Transformation

Refinement of ferrite grains is a promising way to simultaneously improve both the tensile strength and tough-
ness of steels [135]. Up to now, several different thermomechanical controlled processing (TMCP) routes have
been conducted in steel industry to refine ferrite grains [136]-[141]. However, the grain refinement during
TMCP is limited to 5 µm [142] [143]. In the last decade, researchers have developed new thermo-mechanical
processes to produce fine ferrite grains in the range of 1 - 3 µm [144]-[146]. Among these approaches, ultra fine
ferrite (UFF) formation through dynamic strain induced transformation of austenite to ferrite (DSIT) is a simple
and most effective way [143] [144]. DSIT includes transformation of austenite to ferrite during rather than after
deformation. It has been found that plastic strain increases the austenite to ferrite transformation temperature
(AR3) [147]. Therefore, if steel is deformed at temperatures just above AR3, the transformation temperature in-
creases and reaches to deformation temperature provided that the sufficient amount of plastic strain can be im-
posed on austenite phase. In these conditions, ferrite phase is dynamically formed during deformation process.
The critical strain in the range of 0.1 to 0.8 is required for initiation of DSIT [147]. The principles of DSIT are
shown in Figure 11. The critical temperature for DSIT is usually just above the AR3 temperature. It has also been
demonstrated that DSIT can occur if deformation applied in the austenite meta-stable temperature range between
Ae3 and AR3 [148]. All the dynamic evolving behaviors of microstructure at lower deformation temperature
range between Ae3 and AR3 were similar to that at AR3. The volume fraction of ferrite increased with increasing
the amount of deformation, and most of the strain-induced ferrite were found to nucleate on the boundaries of
ultrafine austenite grains, including a lot of them preferentially selected the corner as their nucleation sites. The
reason should be mostly attributed to the change of carbon diffusion behavior due to the refinement of austenite
grains.

444
 H. Halfa

Figure 11. Principles of dynamic strain induced transforma-

tion during deformation at constant temperature [148].

4.10.4. Large-Strain Warm Deformation

In recent years, a variety of methods have been developed to produce ultrafine-grained (UFG) materials with a
ferrite grain size of around 1 µm [149] [150]. Many investigators [37] [38] [96] used large-strain warm defor-
mation as most important thermomechanical technique to produce ultrafine grained steel.
Large-strain deformation processing schedules for production ultrafine grained steel are outlined in Figure 12.
It consists of 3 min of reaustenitization at 912˚C and a single-pass deformation at 860˚C applying a logarithmic
strain of ε = 0.3 at a strain rate of 10 s−1 above the recrystallization temperature. In the conventional hot rolling
route (Figure 12(a)), the sample is then air cooled to room temperature to obtain a conventional ferrite-pearlite
starting microstructure with ferrite grain size around 12 µm. Grain refinement is achieved by subsequent large-
strain warm deformation at 700˚C (the fine grained (FG) route, Figure 12(b)) and at 550˚C (the UFG route,
Figure 12(c)), respectively. A total strain of 1.6 is realized by a four-step flat compression series, each step ex-
erting a strain of 0.4 at a strain rate of 10 s−1. The deformation temperature controls the degree of grain refine-
ment. At 700˚C, a fine polygonal ferrite matrix with globular cementite and fine pearlite colonies is formed. At
550˚C, continuous grain subdivision and pronounced recovery lead to slightly elongated ferrite grains with a
grain size of around 1 µm [151]. After warm deformation, specimens were annealed for 2 h at the respective
deformation temperature to simulate coiling at elevated temperatures, and then air cooled to room temperature.
On the other hand, previous works illustrate that; to control the finished microstructure, large-strain induced
deformation process may be followed by inter-critical annealing to produce dual phase steel [25]. To obtain the
final dual-phase microstructure, all specimens were subjected to inter-critical annealing followed by quenching
in order to transform all austenite into martensite/bainite/pearlite depend on cooling rate of quenching media.
Plain carbon-manganese steel was subjected under the previous treatment by Calcagnotto et al. [152]. They
concluded that, after inter-critical annealing at 730˚C followed by water quenching, the microstructure obtained
in case of hot deformation consists of a ferrite matrix with a grain size of 12.4 µm and 31.3 vol% martensite, the
latter occurring partly as isolated islands, partly as aligned bands. By applying multi-pass warm deformation at
700˚C (fine grained route) and at 550˚C (ultrafine grained route) between hot deformation and intercritical an-
nealing, the ferrite grain size is reduced to 2.4 and 1.2 µm, respectively. The martensite fraction is 30.1 vol% in
the fine grained steel and 29.8 vol% in the ultrafine grained steel. Exemplary micrographs are shown in Figure
13.

4.10.5. Multistage and Single-Stage High-Speed Compression

Figure 14 shows the thermal processing history in the multistage and single-stage high-speed compression tests,
which were based on the Super Short interval Multi-pass Rolling (SSMR) process. The work pieces were gradu-
ally heated at a rate of 10˚C/s from room temperature to 1000˚C, maintained at the this temperature for 120 s,

445
H. Halfa

(a) (b) (c)

Figure 12. thermomechanical processing routes to produce different grain size in a hot deformation
simulator. All treatment are followed by an intercritical annealing at 730˚C for 3 min and subsequent
quenching to obtain the final ferrite/martensite daul-phase microstructur. Ar3: non-equilbruim trans-
formation start temperature; Pf: pearlite transformation finish temperature; ε: logarithmic starin [152].
(a) Coarse grain (CG) route; (b) Fine grain (FG) route; (c) Ultrafine grain (UFG) route.

Figure 13. Microstructures of the (a) Conventional material (12.4 µm ferrite grain size); (b) Fine grained ma-
terial (2.4 µm ferrite grain size) and (c) ultrafine grained material (1.2 µm ferrite grain size) produced by the
processing routes illustrated in Figure 10 plus intercritical annealing for 3 min at 730˚C in a salt bath, fol-
lowed by water quenching [152].

Figure 14. Thermal processing history in multistage and single-stage compression

tests [154].

and then cooled at a rate of 50˚C/s to the testing temperature of 800˚C or 850˚C. The austenite grain size before
compression was about 30 µm [153]. Before compression, there was a holding time of 5 second at the testing
temperature to minimize the temperature distribution inside the work piece. The axial reductions of the different
stages were 50%, 40%, and 50% and the corresponding strain rates of the different stages were 75/s, 150/s, and
300/s, respectively. Severe plastic deformation at a temperature of approximately Ae3 is effective for producing
ultrafine-grained plain steel because the accumulated strain can immediately induce a ferrite transformation.
However, owing to the heat generation associated with severe deformation, the processing temperature easily

446
 H. Halfa

rises to above Ae3. Consequently, it was necessary to remove the heat, and in the test process, the test pieces
were cooled by mist spray between stages. A single-stage high speed compression test was also conducted. The
heating pattern in the single-stage test was almost the same as that in the multistage compression test, but the
testing temperature was slightly reduced to 760˚C. The axial reduction was 78% and the strain rate was 300/s.
This is because severe single stage compression generates considerable heat, and thus the test must be started
earlier at a lower temperature to produce a stable ferrite structure.

4.10.6. Rapid Cooling and Short Interval Multi-Pass Hot Rolling

Toshiro et al. [155] discover a noble grain refinement method to attain ferrite grain size of 1 µm in plain C-Mn
steel by multi-pass hot rolling in a stable austenite temperature region. 0.1%C-1%Mn and 0.16%C-0.7%Mn
steels were finish-rolled at about Ae3 and then rapidly cooled. Special emphases have been placed on the inter-
val, Δt, between the finish of rolling and the start of water spray cooling of more than 1000˚C∙s−1 in cooling rate
and the interval between the last two rolling passes. By reducing Δt from 0.5 to 0.05 s alone, the grain sizes near
the sheet surface and in the central region were markedly reduced to 1.3 and 2.2 µm respectively. By reducing
Δt and the rolling pass interval together, a further reduction in grain size was then achieved. Consequently, the
steel sheet in which the ultrafine grain structure of about 1 µm in grain size penetrated from the sheet surface to
the depth of a quarter of the sheet thickness and the grain size in the central region was well below 2 µm was
obtained. The transformation to the ultrafine ferrite is considered to be static and from deformed austenite (γ).
The principal of rapid cooling and short interval multi-pass hot rolling is schematically represented in Figure
15. It consists of three rolling stands designated as F1 to F3 and water-cooling devices. The cooling device after
F3 was designed to attain a large cooling rate over 1000˚C∙s−1 for the samples under investigation and to control
the intervening time period Δt between the last rolling pass and the beginning of the rapid cooling. The Δt in this
experiment is specifically defined as the period between the instance of the exit from the last rolling and the in-
stance at which high-pressure water jets first make contact with samples. The cooling devices between the roll-
ing stands were used to suppress adiabatic deformation heating when it was necessary to maintain sample tem-
perature.

4.11. Concept of “SSMR” Process

To make the short interval multi-pass rolling process function well, reduction per pass, inter-pass time, number
of passes and rolling temperature should be optimized. Rolling temperature affects the rolling load as well as the
reduction per pass. The lower the material temperature is, the larger the rolling load becomes. In addition, if the
temperature falls below the ferrite transformation temperature before the final pass, the microstructure of the
rolled strip is supposed to contain deformed ferrite grains or abnormally grown grains, which are not preferable
for mechanical properties of the strip. Therefore the rolling in the stable austenite temperature region was
searched for the new process. In order to shorten the inter-pass time, the rolling stands must be placed close each
other and rolling speed must be fast. However, when the rolling speed increases, the heat generation in rolling
becomes large. For the purpose of the effective strain accumulation, excessive temperature rise should be
avoided because the restoration of the strain proceeds fast in high temperature. Therefore the rapid cooling right
after each rolling pass is necessary to compensate the generated heat. Immediate cooling after rolling is also re-
quired for inducing ferrite transformation and for restraining the grain growth after the transformation. The basic

Figure 15. Schematic representation of experimental hot-rolling simulator [156].

447
H. Halfa

concept of the newly proposed process is as follows. In downstream stands of hot finishing mill, more than two
stands including the final one are equipped at extremely short distance. At those stands high speed and mod-
erately large reduction rolling of 40% - 50% per pass is performed. Strip temperature is controlled around Ae3,
the para-equilibrium transformation temperature from austenite to ferrite, by inter-pass cooling. Then the strip is
cooled down to appropriate temperature immediately. Authors named this process “Super Short interval Multi-
pass Rolling (SSMR) process”.

4.12. Production Ultrafine Steels by Severe Plastic Deformation Techniques

Severe plastic deformation (SPD) techniques [157]-[159] impose large accumulated plastic strains at room or
elevated temperatures, e.g. mainly in the temperature regime of warm deformation. Many different severe plas-
tic deformation (SPD) processing techniques have been proposed, developed and evaluated. These techniques
include equal-channel angular pressing (ECAP) [160]-[162], high-pressure torsion (HPT) [163]-[165], mul-
ti-directional forging [166]-[168], twist extrusion [169] [170], cyclic-extrusion-compression [171] [172], reci-
procating extrusion [173] [174], repetitive corrugation and straightening (RCS) [175] [176], constrained groove
pressing (CGP) [177], cylinder covered compression (CCC) [178], accumulative roll-bonding (ARB) [179]
[180], friction stir processing (FSP) [181] [182] and submerged friction stir processing (SFSP) [183]. All of
these procedures are capable of introducing large plastic straining and significant microstructural refinement in
bulk crystalline solids. Some of these techniques, such as ECAP, HPT, multi-directional forging and ARB, are
already well-established methods for producing UFG materials where, depending upon the crystal structure, the
processed microstructures have grain sizes lying typically within the range of ≈70 - 500 nm. The other tech-
niques are currently under development for this purpose.

4.12.1. Equal-Channel Angular Pressing

Equal-channel angular pressing imposes large plastic strains on massive billets via a pure shear strain state. The
approach was developed by Segal et al. in the early 1980s [184]. Its goal was to introduce intense plastic strain
into materials without changing the cross-sectional area of the deformed billets. Owing to this characteristic, re-
peated deformation is possible. At the beginning of the 1990s this method was further developed and applied as
a severe plastic deformation method for the processing of microstructures with submicron grain sizes [185]. The
equal channel angular pressing method was mainly applied for nonferrous alloys (e.g. Al and Mg alloys) and
some low carbon steels. The finest ferrite grain size obtained by use of this method is reportedly about 0.2 µm
[186] [187].
The ECAP technique was invented as a method for the shape-maintaining plastic deformation of bulk mate-
rials in [188] and for the first time has been shown to be applicable for the formation of an ultra-fine grained
structure in metals and alloys in [189]. The method utilizes a die containing two channels of equal cross sections
intersecting at an angle 2Φ, which normally varies in the range 90˚ - 135˚ (Figure 16). In the vicinity of the
plane of intersection of these channels material undergoes severe plastic deformation, which is mainly of simple
shear character. On passing the two channels a sample maintains its shape except for small portions at the ends
(Figure 3). There have been done many analyses of the mechanics of deformation during ECAP to understand

(a) (b)

Figure 16. Schematic view of equal channel angular pressing [190].

448
 H. Halfa

the exact character of plastic strain during ECAP, its dependence on the location of material elements with re-
spect to the channel walls and to evaluate the accumulated strain [190]-[193]. The simplest approximation is the
model of simple shear according to which materials is subject to simple shear strain of ε = 2/√3cot(Φ/2) singu-
larly at the plane of channels’ intersection [190]. For 2Φ = 90˚ the highest strain per pass equal to ε = 1.15 is
achieved. Dies with such an angle are used for pure metals and easily deformable alloys. For hard-to-deform
materials strain is imposed at elevated temperatures and/or with the channels' intersection angle 2Φ > 90˚.
To accumulate very large strains sample can be forced to pass through the die several times. Strain path can
be easily changed by turning the sample around its longitudinal axis between subsequent passes. Four standard
routes have been established referred to as A, BA, BC, and C [190] [193] [194]. A sample is rotated around its
axis to an angle of 0˚, 90˚, and 180˚ for the routes A, B, and C, respectively. When using route BA, consecutive
90˚ rotations have opposite senses, while in route BC the sample is rotated in the same direction.
Parameters of the die and deformation route can be chosen for any material to meet the following main re-
quirements: Formation of an UFG structure with mainly high-angle grain boundaries, the absence of macros-
copic damages and cracks in the samples, Microstructural homogeneity in the most volume of the samples, and
Formation of equiaxed grains. In some cases using back pressure helps to meet these requirements.
The original ECAP is a discontinuous process and as such has a low production efficiency and high cost. It is
considered as a basic way to understand the principles of SPD fabrication of nano-materials that then can be
used in further developments aimed at scaling up of the process and production of low-cost nanomaterials in
large quantities.
One of numerous ECAP-based continuous SPD methods is the ECAP-Conform process developed at IPAM
[195]. The ECAP-Conform set up is schematically illustrated in Figure 17. A rotating shaft in the center con-
tains a groove, into which the work-piece is fed. The work-piece is driven forward by frictional forces on the
three contact interfaces with the groove, which makes the work-piece rotate with the shaft. The work-piece is
constrained to the groove by a stationary constraint die. The stationary constraint die also stops the work-piece
and forces it to turn an angle by shear as in a regular ECAP process. The angle is about 90˚, which is the most
commonly used channel intersection angle in ECAP. This set up effectively makes ECAP continuous. Other
ECAP parameters (die angle, strain rate, etc.) can also be used. Our preliminary results have shown that the
ECAP-Conform process can effectively refine grains of coarse-grained Al and improve its mechanical properties
in a way similar to the conventional ECAP.

4.12.2. Accumulative Roll Bonding

Accumulative roll bonding essentially involves repeated application of conventional rolling. This approach has
been suggested to possess the potential for mass production [196] [197]. While rolling is an attractive deforma-
tion process for continuous production of bulk sheets, the total reduction in thickness, i.e. the accumulated strain,

Figure 17. Schematic view of ECAP-Conform set-up [195].

449
H. Halfa

which can be achieved by this method, is limited because of the decrease in the strip thickness with increasing
rolling reduction. In order to obtain bulk material, rolled sheets are stacked and then bonded together during
rolling [198]. Hence, the process involves simultaneous bonding and deformation. In the accumulative roll
bonding method, the rolled material is cut, stacked to the initial thickness and rolled again. Owing to this ap-
proach, multiple repetitions are possible to achieve huge strains as shown in Figure 18. A natural limit of this
approach lies in the increase in strength and the gradually reduced surface quality of the roll-bonded sheets.

4.12.3. High Pressure Torsion

High pressure torsion (HPT) technique is based on the use of Bridgeman anvil-type device. The possibility of
the formation of a nano-crystalline structure by this method was first demonstrated in [200] [201]. A disk-
shaped sample is put between two anvils and subjected to a high pressure of 2.5 GPa (Figure 19). Rotation of
one of the anvils forces the sample to deform by torsion. Up to five rotations of the anvil are usually enough to
form a homogeneous microstructure with the grain size typically about 100 nm, in some metals and alloys with
high melting temperature as small as 50 nm. This method enables the preparation of disc-shaped samples with
diameter up to 20 mm and thickness about 0.2 mm, which are good for fundamental studies of the struc-
ture-property relationships for nano-materials.

4.12.4. Bi-Directional Large Strain Deformation

Bi-directional compression can be used to introduce large plastic strains in steels. It combines severe plastic de-
formation (large strain) and thermomechanical processing (phase transformation and controlled cooling can be
exploited). Compression is realized by alternate forging in two perpendicular directions. Elongation in the third
direction is usually not restricted.

(a) (b)

Figure 18. Schematic diagram showing ARB process [199]. (a) Two dimensions; (b) Three dimensions.

Figure 19. Schematic rendering of high pressure

torsion [201].

450
 H. Halfa

4.12.5. Multi-Axially Forged Austenite

In the multidirectional forging (MDF) method, the samples were compressed with a changing loading direction
of 90˚ pass-by-pass (i.e., z to y to x to z.) (Figure 20). The aspect ratio of the samples was almost unchanged
during repeated MDF with a pass strain of Δε = 0.4.
1) Dynamic Recrystallization (DRX)
Production of ultrafine grained or nano-grained steel by multiaxially forged austenite was reported by Hauang
et al. [203] by means of deformation at temperature which dynamic recrystallization (DRX) was dominated
(below 0.5 melting temperature of the material). However, it was recently reported that continuous dynamic re-
crystallization (DRX) could take place and the ultra grain refinement to submicro-size or nano-size level was
achieved [204]-[206] within a lower temperature range of austenite state under a severe plastic deformation such
as Equal Channal Angular Pressing, Accumulative Roll Bonding, etc.
The main thrust of Huang et al. [203] work, is principally concerned with elucidating the microstructural
evolution and the continuous dynamic recrystallization (DRX) mechanism of multi-axially forged austenite.
The evolution of continuous DRX during multiaxial forging can be summarized as a process in Figure 21.
When initial grains are deformed in some direction, deformed bands will be produced along a certain direction
in deformed grains by slip shear. Once the deformation direction changes, other deformed bands will also
formed along other directions, in this way, deformed bands will cross each other, by which an austenite grain

Figure 20. Schematic illustration of the process of multidirec-

tional forging (MDF) with loading stress σ. The indexed num-
bers give the aspect ratio of the sample [202].

(a) (b) (c) (d)

Figure 21. The evolution mechanism of continuous dynamic recrystallization

during multiaxial forging (a) initial grain; (b) after the first pass; (c) after the
second pass with deformation direction rotated 90˚; (d) subgrains angled in
the subsequent passes [203].

451
H. Halfa

can be subdivided into several subgrains. And these subgrains will be gradually angled to new independent
grains and its boundaries transformed into big angle boundaries in subsequent deformation passes.
2) Static Recrystallization
Multi-axial forging or multidirectional forging (MDF) is an effective method to produce ultrafine grained
steel. The ultrafine ferrite grains with sizes of about 1.2 µm obtained (from initial ferrite grains with sizes of
about 38 µm) via MDF at room temperature followed by post deformation annealing at 500˚C for 1 min as pro-
posed by Soleymani et al. [207].
The main feature of the microstructure changed during MDF at room temperature is the ferrite grains pan-
caking. After MDF up to strain of 0.8, the grains are elongated along the transverse press direction. With in-
creasing accumulative strain, more work hardened grains were formed after 4th pass of MDF and the grains as-
pect ratio (the ratio of the grains dimension in the longitudinal direction to that in the transverse direction) in-
creased. The microstructure was completely replaced by highly pan-caked grains when the accumulative strain
was 2.6. Multidirectional deformation can develop the micro-shear bands in various directions due to the change
of deformation axes from pass to pass [208]. At the temperature of 500˚C, the grain refinement mechanism rec-
ognized as static recrystallization. The microstructure evolution process is that the new grains are formed by
nucleating within deformed grains. Then they grow and consume the deformed microstructure until the material
is completely recrystallized.

4.12.6. Constrained Groove Pressing

In terms of using severe plastic deformation to produce nanostructure sheets [209]-[211], two major severe plas-
tic deformation techniques, which are mostly employed, are accumulative roll bonding [212] [213] and con-
strained groove pressing [214]. The constrained groove pressing, introduced by Shin et al. [214], involves repe-
titive corrugating and flattening stages. During constrained groove pressing, the work piece is subjected to cyclic
shear deformation by utilizing asymmetrically grooved dies and flat dies. The constrained groove pressing
process is schematically shown in Figure 22. In this technique, the gap between the upper die and lower die is
identical to the sample thickness and therefore the inclined part of the sample, located in the groove, is subjected
to pure shear deformation [215]. By imposing more constrained groove pressing passes, the higher strains are
introduced to the work piece. The work piece subjected to severe plastic deformation by applying three passes of
constrained groove pressing which resulted in the total strain of 3.48. This led to ultrafine grain low carbon steel
having the grains of 260 - 270 nm. Recently, many works are carried out to study the mechanical properties and
microstructural evolutions of different materials such as low carbon steel, aluminum and copper subjected to
constrained groove pressing. According to these studies [216] [217], it is reported that the constrained groove
pressing can effectively enhance the mechanical properties of sheet metals. The treatments applied to ultra-fine
grain steel is summarized in Table 5.
In order to produce the ultra-fine grain samples, the constrained groove pressing was used. The work piece
was subjected to severe plastic deformation by applying three passes of constrained groove pressing which re-
sulted in the total strain of 3.48. This led to ultrafine grain low carbon steel having the grains of 260 - 270 nm.
According to the past works [213] [216] [217], each constrained groove pressing pass imposes the strain of
about 1.16. In the first step, the flat sheet becomes corrugated which results in a 0.58 effective strain in de-
formed regions. Whereas, in the second step, the flat dies are used to flatten the corrugated sheet by imposing an
extra 0.58 strain to the previously deformed sections [215]-[217]. This is defined as one cycle of constrained

Table 5. The treatments applied to ultrafine grain and coarse samples [218].

Steps Coarse grain specimen Ultrafine grain specimen

1 Solid solution traetment (850˚C/1h) Solid solution traetment (850˚C/1h)

2 Water quenching Water quenching

3 Pre-straining (4%, 6%, and 8%) Producing UFG microstructure by CGP

4 Baking (250˚C and 250˚C for 20 min) Pre-straining (4%, 6%, and 8%)

5 Tensile testing at room temperature Baking (250˚C and 250˚C for 20 min)

6 - Tensile testing at room temperature

452
 H. Halfa

(a)

(b)

Figure 22. The schematic of dies used in constrained groove pressing process [218] [219]. (a) Two dimen-
sions; (b) three dimensions.

groove pressing. After straightening, the specimen is rotated 180˚ around the axis perpendicular to the plane of
the sheet and then the second cycle is employed. After the second pass, another effective strain of 1.16 is intro-
duced in the specimen [213]-[218].

4.12.7. Warm Caliber Rolling

Warm caliber rolling process is shown schematically in Figure 23. Shiro et al. [219] proposed that, caliber roll-
ing has been used with relatively successful for UFG production. Earlier work done by Shiro et al. [219] for
C-Mn steels (C15 and C60 steels) were heated up to 823 K and subsequently rolled by 12 passes from 40 mm
square to a final of 13 mm square. The material of the C30 steel also was heated up to 823 K and subsequently
rolled by 21 passes from 80 mm square to a final of 18 mm square. All calibers except the second last one were
square type caliber and the second last one was oval type one. Immediately after rolling, rolled rods were water
quenched [220] [221].
Kimura et al. [223] [224] have recently developed a warm caliber rolling process of tempered martensitic
structures for medium-carbon low-alloy steels as a method to obtain ultrafine elongated grain (UFEG) structures,
and found out enhanced impact toughness of the low-alloy steels at a yield strength (σy) of 1400 MPa or more.
Kimura et al. [225] concern especially for production ultrafine steel with following chemical composition,
0.39%C, 1.98%Si, 1.04%Cr, 1.05%Mo, 0.21%Mn, 0.001%P, <0.001%S, 0.041%Al, 0.002%N, <0.005%O and
the balance Fe was used in this study. A 100 kg ingot was prepared by vacuum melting and casting, homoge-
nized at 1200˚C, and then hot-rolled to a plate with a thickness of 4 cm. A 12 cm × 4 cm × 4 cm block was cut

453
H. Halfa

Figure 23. Schematic drawing of warm multi-pass caliber

rolling to obtain ultrafine grained structure [222].

out of the plate, solution-treated at 1200˚C for 1 h and then hot-rolled to a squared bar with a cross section area
of 9 cm2, followed by water quenching. The quenched bars were tempered at 500˚C for 1 h and then subjected to
multi-pass caliber rolling to squared bars with a cross section of 2 cm2, followed by air cooling (temp-formed
(TF) samples). The total reduction in area through the multi-pass rolling was 77% in 9 passes. Note that the
samples were held for 5 min in a furnace after every three passes during the rolling and passed through twice for
the final groove to control the cross sectional shape of the bars. For reference, parts of the quenched bars were
tempered at 500˚C for 1 h and then air cooled (QT sample).
Table 6 summarizes the common techniques to produce ultrafine grained steels and the ferrite grain sizes ob-
tained. To obtain ultrafine grains using SPD methods, the accumulated plastic strains are required to be of the
order of 3 - 4 for ECAP and be of the order of 5 - 6 for ARB process. To obtain ultrafine grains using advanced
thermomechanical process methods, the accumulated plastic strain is required to be of the order of 1 - 3.6.
Compared with SPD methods, the advanced thermomechanical process methods are generally less effective in
producing ultrafine grains, but ATP methods are more adaptable to large scale production.

5. Application of Ultrafine Grained Steels

One of many advantages claimed for small grain size is that of dynamic deformation at high strain rate which
are very important for the passengers’ safety in the case of car collisions. However, ultrafine-grained (UFG)
steels [198] [226] are expected to be used in the future as structural materials, including automobile body appli-
cations, because of their superior mechanical properties.
It is important to note also that the grain size has a strong influence on the local flow behavior during mi-
cro-forming and it is believed to be the limiting factor that dictates the minimum size for the production of geo-
metrical features [227]. This means in practice that nano-crystalline materials exhibit the best formability in mi-
cro-imprinting and the use of ultrafine-grained materials may improve the flow behavior and the filling quality
since size effects, such as process scatter and uneven shape evolution, are significantly reduced in comparison
with the conventional coarse-grained materials. Processing by SPD has been used successfully for processing in
micro-forming applications such as production of micro-gears and for production of net-shaped micro-elec-
tro-mechanical system (MEMS) components [228].
Ultrahigh strength wire can have many applications that demand exceptional tensile strength. In terms of
quantity, two most important applications for ultrahigh strength steel wire are in the automotive tire reinforce-
ment [229] and in the cable wire for suspension bridges [230]. In addition to the application in tires and bridges,
ultrahigh strength wire can serve as springs, wire rope, and reinforcement in a wide range of composite struc-
tures, such as pre-stressed concrete structures. The application of ultrahigh strength wire in the composite indus-
try is largely un-explored because the wire was not available before, but the application potential is expected to
be enormous. It is highly recommended to conduct exploratory studies to verify the physical-mechanical proper-
ties, manufacturing procedural, and cost-saving advantages of ultrahigh strength wire reinforced composites.
There is a continued and increasing demand to transport oil and gas by pipelines at high operating pressures in
the attempt to increase the capacity. This requires the use of ultrahigh strength steels. Furthermore, increasing
the strength of the pipeline steel allows wall thickness to be significantly reduced with consequent reduction in
weight. Thus, a major goal within the steel industry is to develop ultrahigh strength microalloyed pipeline steels

454
 H. Halfa

Table 6. Summary of different techniques reported to produce ultrafine grained steels [37].

Ferrite grain Log, strain Deformation Heat treatment

Technique Steels Steel composition (wt%) size achieved imposed temperature after
(%) (%) (K) deformation
Plain low carbon
0.08C-0.42Mn-0.18Si 0.2 3.0 293 AC
steel
Plain low carbon
0.15C-1.1Mn-0.25Si 0.3 in thickness 4.0 623 AC
steel
ECAP
Ti-V low carbon
0.1C-1.59Mn-0.29Si-0.02Ti-0.05V ~0.3 thickness 1.0 573 AC
steel
Ferrite-austenite 1003 K ×
0.15C-1.06Mn-0.25Si 0.8 4.0 773
dual phase steel 10 min WQ
ARB Ti-added IF steel 0.003C-0.15Mn < 0.01Si-0.049Ti 0.4 5.6 773 WC
Plain low carbon Shear than 300,
HPT ~0.7C~1.0Mn~0.3 Si 0.01 293 AC
steel log strain 0.45
DRX* during hot Final rolling
Micro-alloyed steel 0.11C-1.45Mn-0.34Si-0.068Nb 2-5 1153 - 1033 AC
deformation 2.3 - 3.6
Strain-induced Plain low carbon 1.0
0.06C-0.59Mn 0.36 1053 AC
ferrite transformation steel (strip surface)
Deformation in the Plain low carbon
0.17C-1.32Mn-0.44Si-0.15Nb 2.1 2.3 973 WQ
inter-critical region steel
Warm rolling in the Final rolling
Ti-added IF steel 0.003C-0.15Mn-0.025Si-0.065Ti 1-3 Below A*r1 WQ
ferrite region ~0.55 × 5
DRX* of ferrite 723 - 823
Ultra-low carbon
during warm 0.0016C-0.1Si-0.03Mn - 4.0 (lower than WQ
steel
deformation A*c1) 823
Pronounced
recovery of ferrite
Plain medium 1.6 at strain 823 K ×
during warm 0.22C-0.21Si-0.74Mn 1.3 823
carbon steel rate of 0.01 s−1 120 min
deformation
and annealing

Cold deformation
773 K ×
and annealing of Martensitic steel 0.13C-0.37Mn-0.01Si 0.18 0.8 293
30 min
martensitic steel

Abbreviation: DRX*, dynamic recrystallization; A*r1, austenite to pearlite transformation temperature during cooling; A*C1, pearlite to austenite
transformation temperature during heating; ECAP, equal channel angular pressing; ARB, accumulative roll bonding; HPT, high pressure torsion; AC,
air cooling; WC, water cooling; WQ, water quench.

with high toughness and formability. High toughness is important to reduce stress-induced cracking, while for-
mability is important from the view point of pipe-bowing. Thus, high strength in conjunction with high tough-
ness and formability are important requirements of the pipeline industry for transporting natural gas and crude
oil over a long distance at high pressures [231]-[233]. Other characteristics that are required include resistance to
hydrogen induced blister cracking in sour service environment [234] [235], stress corrosion cracking resistance,
especially in H2S environment [236], and fatigue resistance [237] [238]. In the aforementioned regard, it is im-
portant that the microstructure of the pipeline steel provides a combination of aforementioned properties.
Finally, it should be noted that considerable attention is now focused on the development of ultrafine-grained
materials for use in specific applications [239]. For example, magnesium alloys are under consideration for use
in hydrogen storage and ultrafine-grained titanium is an excellent candidate material for use in dental and sur-
gical implants [240]. Descriptions of these developments are beyond the scope of this review, but nevertheless
these topics provide exciting challenges for new and meaningful research that will have scientific rigor and yet
provide valuable information for the future use of these materials in technological applications.

6. Contribution of Steel Technology Department

Steel Technology Department, CMRDI staff makes a great effort for studying the strengthening of steel through
different methods such as microalloying [241]-[248], strengthening by solid solution elements [249] [250] for

455
H. Halfa

example N, C and Mn, interrupted accelerated cooling [251], cold drawing [252] [253], well design rolling
schedule [254], reheating and finishing temperature [255] [256], and heat treatment [257].
Steel Technology Department staff published a lot of publications in role of microalloying in carbon manga-
nese steel to produce high strength low alloy steels. In previous work [237]-[244], they studied the contribution
of V, V + N, V + Ti combined with extra C and/or Mn in strengthening of such steel. The results of these works
demonstrated that, the strengthening potential of vanadium seems to be due to precipitation strengthening rather
than grain refinement effect. Both carbon and manganese in combination with vanadium showed a significant
effect on increasing the precipitation strengthening. By study effect of vanadium as alloying element combined
with nitrogen [246] [249] on microstructure and strength of low carbon steels with different manganese contents
the results show that, vanadium microalloying effectively increased the strength of steels through solely precipi-
tation strengthening or both precipitation strengthening and grain refining effect. The effectiveness of vanadium
was greatly enhanced by increasing the nitrogen content. The grain refinement of vanadium-nitrogen microal-
loying seems to be due to inhibition of austenite grain growth as a result of precipitation of vanadium nitride in
austenite during forging. Precipitation strengthening of these steels is achieved by precipitation of vanadium
carbide and nitride in ferrite or bainite. Nitrogen enhanced the precipitation strengthening of vanadium microal-
loyed steels which could be attributed to the finer vanadium nitride dispersion precipitates compared with vana-
dium carbide. Up to 70% of the total nitrogen content of steel precipitates as vanadium nitride which could be
achieved with V/N ratio of about 6 - 7. Microalloying of low carbon-manganese steels (0.1%C and 1.8%Mn)
with 0.15% vanadium and 0.025% nitrogen was found to be effective in attaining high levels of yield and ulti-
mate tensile strengths of 835 and 940 MPa, respectively in the forging condition. On other work [252] [253],
Ultra-high strength high-carbon wire rod steels have been produced using vanadium-microalloying technique
instead of the conventional expensive and environment polluting lead patenting treatment. The experimental re-
sults show that, the strength increment attained in the hot rolled steels due to vanadium additions is maintained
in the cold drawn wire. By using this technique, high tensile strength levels of 1550 - 1600 MPa were attained
either by cold drawing of 0.17%V microalloyed high-carbon steel to 45% - 47% reduction or by cold drawing of
0.20%V microalloyed high-carbon steel to 25% - 30% reduction. They concluded that, a combination of vana-
dium microalloying and accelerated cooling [251], resulted in additional strength increment due to refining of
microstructure and increasing the precipitation strengthening component. In spite of the decrease in the amount
of vanadium precipitates due to the increase in cooling rate, it is suggested that an increase in precipitation
strengthening due to refining of these precipitates by accelerated cooling more than offsets the loss of precipita-
tion strengthening due to decreasing the precipitates fraction. It was concluded that microalloying addition in-
crease the strength of steel through different methods such as grain refinement, solid solution strengthening and
precipitation strengthening [241]-[243]. Also the previous work demonstrate that microalloying addition im-
prove both strength and toughness of steels [241] [258]-[260]. Investigation done by steel technology staff found
that [261], in hot rolled V-and Ti-microalloyed steels, transmission electron microscopy revealed several types
of non-metallic inclusions and precipitates, the most effective on grain refinement and strength increment are the
very fine precipitates.

7. Future Prospects of Ultrafine Grained Steels

The following suggestions can be made for future work:
1) To complete the study the effect of mircro-alloying elements on refining the microstructure;
2) To study the effect of rare earth metal on refining the microstructure of special steel e.g. high speed tool
steel, maraging steel and so on;
3) To use mechanical vibration and ultrasound for production of high speed tool steel with ultrafine and well
distributed carbides;
4) To use mechanical vibration and ultrasound for production ultra-fine C-Mn steel with and without micro-
alloying additions;
5) To use electroslag refining technology for production ultrafine steel single phase with micro-alloying addi-
tions;
6) To use electroslag refining technology equipped with electrical magnetic field for production ultrafine sin-
gle phase steel;
7) To use severe plastic deformation methods for production ultrafine maraging steels;
8) To use severe plastic deformation combined with thermomechanical treatment for production high nitrogen
steel especially meta-stable austenitic steels.

456
 H. Halfa

8. Conclusion
The review reveals that the grain refinement by different strategies of ultrafine grained structure can lead to a
unique combination of strength and ductility in different kinds of advanced steels. Such superior mechanical
properties are highly desirable in the development of advanced steel for the next generation. However, the
achievement of these properties is associated with further treatment to create specific microstructure that is re-
sponsible to improve the ductility of the advanced steel. Depending on the process boundary conditions, either a
change of chemical composition, i.e. microalloying, or change of process, i.e. from conventional heat treatment
to thermomechanical treatment, severe plastic deformation or a combination of any two processes can be se-
lected. Thus, higher strength with equivalent or higher ductility can be obtained.

Acknowledgements
May ALLAH shower his mercy and forgiveness on the souls of my teachers and supervisors: My father Ahmed
Mohamed Halfa, Prof. Dr. Kamal Mohamed Abd-Rabu El-Fawakhry, Mahmoud Farag El-Demerdash. I
am indebted to Prof. Dr. Mamdouh Mahmoud Eissa, for his supervision and continuous guidance through all
my work. I would like to express my thanks and gratitude to Prof. Dr. Taha Mohamed Taha Mattar, Head of
Metal division, CMRDI, and Prof. Hoda Salama El–Faramawy, Head of Steel Technology Department. I
gratefully acknowledge the pleasant atmosphere and support from all of my colleagues at the metal Division,
Steel Technology Department of CMRDI.

References
[1] Misra, R., Nathani, H., Hartmann, J. and Siciliano, F. (2005) Microstructural Evolution in a New 770 MPa Hot Rolled
Nb-Ti Microalloyed Steel. Materials Science and Engineering A, 394, 339-352.
http://dx.doi.org/10.1016/j.msea.2004.11.041
[2] Zajac, S., Komenda, J., Morris, P., Matera, S. and Penalba Diaz, F. (2003) Quantitative Structure-Property Relation-
ships for Complex Bainitic Microstructure. RFCS Final Report, European Commission, Luxembourg.
[3] Charleux, M., Poole,WJ., Militzer, M. and Deschamps, A.(2001) Precipitation Behavior and Its Effect on Strengthen-
ing of an HSLA-Nb/Ti Steel. Metallurgical and Materials Transactions A, 32, 1635-1647.
http://dx.doi.org/10.1007/s11661-001-0142-6
[4] Foreman, J.E. and Makin, A.J. (1967) Dislocation Movement through Random Arrays of Obstacles. Canadian Journal
of Physics, 45, 7-12. http://dx.doi.org/10.1139/p67-044
[5] Thermo-Calc, Ver, P. and Thermo-Calc, A.B. (2002) article. Royal Institute of Technology, Stockholm.
[6] Gladman, T. (1997) The Physical Metallurgy of Microalloyed Steels. The Institute of Materials, London, United King-
dom.
[7] Syarif, J., Nakashima, K., Tsuchiyama, T. and Setsuo, T. (2007) Effect of Solute Copper on Yield Strength in Disloca-
tion-Strengthened Steels. Iron and Steel Institute of Japan (ISIJ) International, 47, 340-345.
http://dx.doi.org/10.2355/isijinternational.47.340
[8] Siwecki, T., Blaz, L. and Petterson, S. (2000) Improving Properties in V-Nb Microalloyed Steels Modified with Mo.
HSLA Steels 2000, Xi’an, China, 30 October-2 November, 2000, Beijing, 504-510.
[9] Misra, R., Weatherley, G., Hartmann, J. and Boucek, A. (2001) Ultrahigh Strength Hot Rolled Microalloyed Steels:
Microstructural Aspects of Development. Materials Science Technology, 17, 1119-1129.
http://dx.doi.org/10.1179/026708301101511040
[10] Kelly, A. and Nicholson, R.B. (1971) Strengthening Methods in Crystals. Applied Science Publishers Ltd., London,
United Kingdom.
[11] Zajac, S., Lagneborg, R. and Siwecki, T. (1995) The Role of Nitrogen in Microalloyed Steels. Proceedings of the In-
ternational Conference on “Microalloying 95”, Pittsburgh, 11-14 June 1995, 321-340.
[12] Lagneborg, R., Siwecki, T., Zajac, S. and Hutchinson, B. (1999) The Role of Vanadium in Microalloyed Steel. Scan-
dinavian Journal of Metallurgy, 28, 186-241.
[13] Baker, R.G. and Nutting, J. (1969) The Tempering of Cr-Mo-V-W and Mo-V Steel Precipitation Processes in Steels.
ISI Report, 64, 1-12.
[14] Kunitake, T. (1967) On the Yield Strength of Quenched and Tempered Structures of Low-Carbon, Low Alloy Steels.
Transaction of the Iron and Steel Institute of Japan, 7, 254-262.

457
H. Halfa

[15] Bhadeshi, H. (2001) Bainite in Steels. IOM Communication Ltd., London.

[16] Takahashi, M. and Bhadeshia, H. (1990) Model for Transition from Upper to Lower Bainite. Materials Science and
Technology, 6, 592-603. http://dx.doi.org/10.1179/mst.1990.6.7.592
[17] Wang, J. and Zwaag, S. (1990) Stabilization Mechanisms of Retained Austenite in Transformation-Induced Plasticity
Steel. Metallurgical and Materials Transactions A, 21, 1527-1539.
[18] Hulka, K. and Heisterkamp, F. (1993) Low Carbon Steels the Key to Economic Constructions. International Sympo-
sium on Low-Carbon Steels for the 90’s, Pittsburgh, 18-21 October 1993, 211-218.
[19] Morrison, W. (2000) Past and Future Development of HSLA Steels. HSLA Steels 2000, Xi’an, China, Beijing, 30 Oc-
tober-2 November 2000, 11-19.
[20] ssKrauss, G. and Thompson, S. (1995) Ferritic Microstructures in Continuously Cooled Low- and Ultralow-Carbon
Steels. Iron and Steel Institute of Japan (ISIJ) International, 35, 937-945.
http://dx.doi.org/10.2355/isijinternational.35.937
[21] Morrison, W. (1996) The Effect of Grain Size on the Stress-strain Relationship in Low Carbon Steel. Transactions of
American Society for Metals, 59, 824-846.
[22] Shin, D., Park, J., Chang, S., Lee, Y. and Park, K. (2002) Ultrafine Grained Low Carbon Steels Fabricated by Equal
Channel Angular Pressing. Iron and Steel Institute of Japan (ISIJ) International, 42, 1490-1496.
http://dx.doi.org/10.2355/isijinternational.42.1490
[23] Fukuda, Y., Oh-Ishi, K., Horita, Z. and Langdon, T. (2002) Processing of a Low-Carbon Steel by Equal-Channel An-
gular Pressing. Acta Materialia, 50, 1359-1368. http://dx.doi.org/10.1016/S1359-6454(01)00441-4
[24] Son,Y., Lee, Y., Park, K., Lee, C. and Shin, D. (2005) Ultrafine Grained Ferrite-Martensite Dual Phase Steels Fabri-
cated via Equal Channel Angular Pressing: Micro-Structure and Tensile Properties. Acta Materialia, 53, 3125-3134.
http://dx.doi.org/10.1016/j.actamat.2005.02.015
[25] Park, K., Han, S., Ahn, B., Shin, D., Lee, Y. and Um, K. (2004) Ultrafine Grained Dual Phase Steel Fabricated by
Equal Channel Angular Pressing and Subsequent Intercritical Annealing. Scripta Materialia, 51, 909-913.
http://dx.doi.org/10.1016/j.scriptamat.2004.06.017
[26] Kim, W., Kim, J., Choo, W., Hong, S. and Lee, J. (2001) Large Strain Hardening in Ti-V Carbon Steel Processed by
Equal Channel Angular Pressing. Materials Letters, 51, 177-182.
http://dx.doi.org/10.1016/S0167-577X(01)00320-2
[27] Shin, D., Seo, C., Kim, J., Park, K. and Choo, W. (2000) Microstructures and Mechanical Properties of Equal-Channel
Angular Pressed Low Carbon Steel. Scripta Materialia, 42, 695-699.
http://dx.doi.org/10.1016/S1359-6462(99)00422-4
[28] Liu, M., Shi, B., Wang, C., Ji, S., Cai, X. and Song, H. (2003) Normal Hall-Petch Behavior of Mild Steel with Submi-
cron Grains. Materials Letters, 57, 2798-2802. http://dx.doi.org/10.1016/S0167-577X(02)01377-0
[29] Song, R. (2005) Microstructure and Mechanical Properties of Ultrafine Grained C-Mn Steels. Shaker Verlag GmbH,
Aachen.
[30] Brozzo, P., Buzzichelli, A., Mascanzoni, A. and Mirabile, G. (1977) Microstructure and Cleavage Resistance of Low
Carbon Bainitic Steels. Metal Science, 11, 123-130. http://dx.doi.org/10.1179/msc.1977.11.4.123
[31] Tomita, Y. and Okabayashi, K. (1986) Effect of Microstructure on Strength and Toughness of Heat-Treated Low Alloy
Structural Steels. Metallurgical Transactions A, 17, 1203-1209. http://dx.doi.org/10.1007/BF02665319
[32] Lazarova, R., Petrov, R.H., Gaydarova, V., Davidkov, A., Alexeev, A. and Manchev, M. (2011) Microstructure and
Mechanical Properties of P265GH Cast Steel after Modification with TiCN Particles. Materials & Design, 32, 2734-
2741. http://dx.doi.org/10.1016/j.matdes.2011.01.024
[33] Rasouli, D., Khameneh Asl, S., Akbarzadeh, A. and Daneshi, G. (2009) Optimization of Mechanical Properties of a
Micro Alloyed Steel. Materials & Design, 30, 2167-2172. http://dx.doi.org/10.1016/j.matdes.2008.08.024
[34] Zhao, M., Yang, K. and Shan, Y. (2003) Comparison on Strength and Toughness Behaviors of Microalloyed Pipeline
Steels with Acicular Ferrite and Ultrafine Ferrite. Material Letters, 57, 1496-1500.
http://dx.doi.org/10.1016/S0167-577X(02)01013-3
[35] Zhao, M., Shan, Y. and Yang, K. (2004) Effect of Aging Treatment on Mechanical Property and H2S Resistant Beha-
vior of Acicular Ferrite Pipeline Steels. Acta Metallurgica Sinica, 40, 948-954.
http://www.ams.org.cn/CN/Y2004/V40/I9/948
[36] Tóth, L., Rossmanith , H.P. and Siewert, T.A. (2002) Historical Background and Development of the Charpy Test.
European Structural Integrity Society: From Charpy To Present Impact Testing, 30, 3-19.
http://dx.doi.org/10.1016/S1566-1369(02)80002-4

458
 H. Halfa

[37] Zhao, M., Li, J., Zeng, T., Hunag, X., Zhao, Y. and Atrens, A. (2011) The Ductile to Brittle Transition for C-Mn Steel
with an Ultrafine Grain Ferrite/Cementite Microstructure. Materials Science and Engineering A, 528, 7228-7237.
http://dx.doi.org/10.1016/j.msea.2011.06.005
[38] Hanamura, T., Yin, F.X. and Nagai, K. (2004) Ductile-Brittle Transition Temperature of Ultrafine Ferrite/Cementite
Microstructure in a Low Carbon Steel Controlled by Effective Grain Size. Iron and Steel Institute of Japan (ISIJ) In-
ternational, 44, 610-617. http://dx.doi.org/10.2355/isijinternational.44.610
[39] Song, R., Ponge, D., Raabe, D., Speer, J. and Matlock, D. (2006) Overview of Processing, Microstructure and Me-
chanical Properties of Ultrafine Grained bcc Steels. Materials Science and Engineering A, 441, 1-17.
http://dx.doi.org/10.1016/j.msea.2006.08.095
[40] Song, R., Ponge, D. and Raabe, D. (2005) Mechanical Properties of an Ultrafine Grained C-Mn Steel Processed by
Warm Deformation and Annealing. Acta Materialia, 53, 4881-4892. http://dx.doi.org/10.1016/j.actamat.2005.07.009
[41] Kimura, Y., Inoue, T., Yin, F. and Tsuzaki. K. (2008) Inverse Temperature Dependence of Toughness in an Ultrafine
Grain-Structure Steel. Science, 320, 1057-1060. http://dx.doi.org/10.1126/science.1156084
[42] National Highway Traffic Safety Administration (2007) DOT HS 810 863. www.nhtsa.gov .
[43] Euro NCAP (1998) Development of the European New Car Assessment.
http://www.euroncap.com/files/Development-of-Euro-NCAP-1998---0-7498ffa2-36b6-4328-8b6e-f44fe5d35563.pdf
[44] Kim, S., Kim, G. and Chin, K. (2008) Development of High Manganese TWIP Steel with 980 MPa Tensile Strength.
Proceeding of the International. Conference on New Developments in Advanced High-Strength Sheet Steels, AIST. Or-
lando, 15-18 June 2008, 249-256.
[45] Boron Extrication (2009) XC60 Body Structure. http://boronextrication.com/2009/08/2009-xc60-body-structure/.
[46] Shim, J., Cho, H., Chung, S., Shim, J. and Lee, D. (1999) Nucleation of Intragranular Ferrite at Ti2O3 Particle in Low
Carbon Steel. Acta Materialia, 47, 2751-2760. http://dx.doi.org/10.1016/S1359-6454(99)00114-7
[47] Calcagnotto, M., Adachi,Y. Ronge, D. and Raabe, D. (2011) Deformation and Fracture Mechanisms in Fine- and Ul-
trafine-Grained Ferrite/Martensite Dual-Phase Steels and the Effect of Aging. Acta Materialia, 59, 658-670.
http://dx.doi.org/10.1016/j.actamat.2010.10.002
[48] Song, R., Ponge, D., Raabe, D. Speer, J. and Matlock, D. (2006) Overview of Processing, Microstructure and Mechan-
ical Properties of Ultrafine Grained BCC Steels. Materials Science and Engineering A, 441, 1-17.
http://dx.doi.org/10.1016/j.msea.2006.08.095
[49] Song, R., Ponge, D. and Raabe, D. (2005) Mechanical Properties of an Ultrafine Grained C-Mn Steel Processed by
Warm Deformation and Annealing. Acta Materialia, 53, 4881-4892.
http://dx.doi.org/10.1016/j.actamat.2005.07.009
[50] Funakawa, Y., Shiozaki, T., Tomita, K., Yamamoto, T. and Maeda, E. (2004) Development of High Strength Hot-
Rolled Sheet Steel Consisting of Ferrite and Nanometer-Sized Carbides. Iron and Steel Institute of Japan (ISIJ) Inter-
national, 44, 1945-1951. http://dx.doi.org/10.2355/isijinternational.44.1945
[51] Fernández, J., Illescas, S. and Guilemany, J. (2007) Effect of Microalloying Elements on the Austenitic Grain Growth
in a Low Carbon HSLA steel. Materials Letters, 61, 2389-2392. http://dx.doi.org/10.1016/j.matlet.2006.09.021
[52] Medina, S. and Hernanden, C. (1995) Static Recrystallization of Austenite and Strain Induced Precipitation Kinetics in
Titanium Microalloyed Steels. Acta Metallurgica, 42, 3945-3951. http://dx.doi.org/10.1016/0956-7151(94)90172-4
[53] Elwazri, A., Wanjara, P. and Yue, S. (2003) Dynamic Recrystallization of Austenite in Microalloyed High Carbon
Steels. Materials Science and Engineering A, 339, 209-215. http://dx.doi.org/10.1016/S0921-5093(02)00164-8
[54] Fernández, A., Uranga, P., López, B. and Rodriguez-Ibabe, J. (2003) Dynamic Recrystallization Behavior Covering a
Wide Austenite Grain Size Range in Nb and Nb-Ti Microalloyed Steels. Materials Science and Engineering A, 361,
367-376. http://dx.doi.org/10.1016/S0921-5093(03)00562-8
[55] Liang. X., Sun, X. and Liu. Q. (2006) Study of Dynamic Recrystallization of Low Carbon Steel in Thin Slab Conti-
nuous Rolling Process. Acta Metallurgica Sinica, 19, 265-270. http://dx.doi.org/10.1016/S1006-7191(06)60054-9
[56] Pickering, F. (1990) Some Beneficial Effects of Nitrogen in Steel. In: Korchynsky, M., Gorczyca, S. and Blicharski,
M., Eds., Proceedings of International Symposium Microalloyed Vanadium Steels, Cracow, 24-26 April 1990, 33-62.
[57] Korczynsky, M. (1988) Microalloying and Thermo-Mechanical Treatment. In: DeArdo, A.J., Ed., Proceedings of In-
ternational Symposium Processing, Microstructure and Properties of HSLA Steels, Pittsburgh, 1-3 September 1988,
169-201.
[58] Pickering, F. (1985) Vanadium as a Hardenability and Temperability Additive in Quenched and Tempered Steels. In:
Gray, J.M., et al., Eds., Proceedings of an International Conference on HSLA Steels 85, Beijing, 4-8 November 1985,
305-324.

459
H. Halfa

[59] Renata, S., Henryk, A. and Anna, A. (2006) Effect of Nitrogen and Vanadium on Austenite Grain Growth Kinetics of a
Low Alloy Steel. Materials Characterization, 56, 340-347. http://dx.doi.org/10.1016/j.matchar.2005.09.012
[60] Melloy, G., Slimmon, P. and Podgursky, P. (1973) Optimization the Boron Effect. Metallurgical and Materials Tran-
sactions A, 4, 2279-2289. http://dx.doi.org/10.1007/BF02669367
[61] Matlock, D., Krauss, G. and Speer, J. (2005) New Microalloyed Steel Applications for the Automotive Sector. Mate-
rials Science Forum, 500-501, 87-96. http://dx.doi.org/10.4028/www.scientific.net/MSF.500-501.87
[62] Klinkenberg, C. and Jansto, J. (2006) International Conference on New Development in Ferrous and Forged Products.
TMS, Winter Park, CO., Colorado.
[63] Ebrahimi, G., Javdani, M. and Arabshahi, H. (2010) Effect of Thermo-Mechanical Parameters on Microstructure and
Mechanical Properties of Microalloyed Steels. Brazilian Journal of Physics, 40, 454-458.
http://dx.doi.org/10.1590/S0103-97332010000400017
[64] Ghosh, P., Ray, R.K., Ghosh, C. and Bhattacharjee, D. (2008) Comparative Study of Precipitation Behavior and Tex-
ture Formation in Continuously Annealed Ti and Ti + Nb Added Interstitial-Free High-Strength Steels. Scripta Mate-
rialia, 58, 939-942. http://dx.doi.org/10.1016/j.scriptamat.2008.01.056
[65] Hong, S., Jun, H., Kang, K. and Park, C. (2003) Evolution of Precipitates in the Nb-Ti-V Microalloyed HSLA Steels
during Reheating. Scripta Materialia, 48, 1201-1206. http://dx.doi.org/10.1016/S1359-6462(02)00567-5
[66] Ghosh, P., Ghosh, C., Ray, R. and Bhattacharjee, D. (2008) Precipitation Behavior and Texture Formation at Different
Stages of Processing in an Interstitial Free High Strength Steel. Scripta Materialia, 59, 276-268.
http://dx.doi.org/10.1016/j.scriptamat.2008.03.044
[67] Adamczyk, J., Kalinowska-Ozgowicz, E., Ozgowicz, W. and Wusatowski, R. (1995) Interaction of Carbonitrides V(C,
N) Undissolved in Austenite on the Structure and Mechanical Properties of Microalloyed V-N Steels. Journal of Mate-
rials Processing Technology, 53, 23-32. http://dx.doi.org/10.1016/0924-0136(95)01958-H
[68] Matsuo, S., Ando, T. and Grant, N. (2000) Grain Refinement and Stabilization in Spray-Formed AISI 1020 Steel. Ma-
terials Science and Engineering A, 288, 34-41. http://dx.doi.org/10.1016/S0921-5093(00)00881-9
[69] Tomita, Y. and Okabayashi, K. (1986) Effect of Microstructure on Strength and Toughness of Heat-Treated Low Alloy
Structural Steels, Metallurgical and Materials Transactions A, 17, 1203-1209.
[70] Lazarova, R., Petrov, R.H., Gaydarova, V., Davidkov, A., Alexeev, A., Manchev, M., and Manolov, M. (2011) Micro-
structure and Mechanical Properties of P265GH Cast Steel after Modification with TiCN Particles. Materials & Design,
32, 2734-2741. http://dx.doi.org/10.1016/j.matdes.2011.01.024
[71] Rasouli, D., Khameneh Asl, S.H., Akbarzadeh, A. and Daneshi, G.H. (2009) Optimization of Mechanical Properties of
a Microalloyed Steel. Materials & Design, 30, 2167-2172. http://dx.doi.org/10.1016/j.matdes.2008.08.024
[72] Andrade, H., Akben, M. and Jonas, J. (1983) Effect of Molybdenum, Niobium, and Vanadium on Static Recovery and
Recrystallization and on Solute Strengthening in Microalloyed Steels. Metallurgical and Materials Transactions A, 14,
1967-1977. http://dx.doi.org/10.1007/BF02662364
[73] Craven, A., He, K., Garvie, L. and Baker, T. (2000) Complex Heterogeneous Precipitation in Titanium-Niobium Mi-
croalloyed Al-Killed HSLA Steels—I. (Ti, Nb) (C, N) Particles. Acta Materialia, 48, 3857-3868.
http://dx.doi.org/10.1016/S1359-6454(00)00194-4
[74] Charleux, M., Poole, W., Militzer, M. and Deschamps, A. (2001) Precipitation Behavior and Its Effect on Strengthen-
ing of an HSLA-Nb/Ti Steel. Metallurgical and Materials Transactions A, 32, 1635-1647.
http://dx.doi.org/10.1007/s11661-001-0142-6
[75] Xu, G., Gan, X., Ma, G., Luo, F. and Zou, H. (2010) The Development of Ti-Alloyed High Strength Microalloy Steel.
Materials & Design, 31, 2891-2896. http://dx.doi.org/10.1016/j.matdes.2009.12.032
[76] Jia, Z., Misra,R., O’Malley, R. and Jansto, SJ. (2011) Fine-Scale Precipitation and Mechanical Properties of Thin Slab
Processed Titanium-Niobium Bearing High Strength Steels. Materials Science and Engineering A, 528, 7077-7083.
http://dx.doi.org/10.1016/j.msea.2011.05.073
[77] Farahat, A. and El-Bitar, T. (2010) Effect of Nb, Ti and Cold Deformation on Microstructure and Mechanical Proper-
ties of Austenitic Stainless Steels. Materials Science and Engineering A, 527, 3662-3669.
http://dx.doi.org/10.1016/j.msea.2010.02.064
[78] Soto, R., Saikaly, W., Bano, X., Issartel, C., Rigaut, G. and Charai, A. (1999) Statistical and Theoretical Analysis of
Precipitates in Dual-Phase Steels Microalloyed with Titanium and Their Effect on Mechanical Properties. Acta Mate-
rialia, 47, 3475-3481. http://dx.doi.org/10.1016/S1359-6454(99)00190-1
[79] Regone, W., Jorge, A. and Balancin, O. (2003) Evidence of Strain-Induced Precipitation of Ti4C2S2 during Hot Defor-
mation of Ti-Only Stabilized IF Steel. Scripta Materialia, 48, 773-778.
http://dx.doi.org/10.1016/S1359-6462(02)00532-8

460
 H. Halfa

[80] Zener, C. and Smith, C. (1948) Grains, Phases and Interfaces: Interpretation of Microstructures. Transaction metallur-
gy Society of AIME, 175, 15-51.
[81] He, K. and Baker, T. (1993) The Effects of Small Ti Additions on the Mechanical Properties and the Microstructures
of Controlled Niobium-Bearing HSLA Plate. Materials Science and Engineering A, 169, 53-65.
http://dx.doi.org/10.1016/0921-5093(93)90598-9
[82] Moon, J., Kim, S., Lee, J. and Lee, C. (2007) Limiting Austenite Grain Size of TiN-Containing Steel Considering the
Critical Particle Size. Scripta Materialia, 56, 1083-1086. http://dx.doi.org/10.1016/j.scriptamat.2007.02.025
[83] Wu, K., Zhang, L., He, X., Shang, C., Yang, S. and Wang, X. (2006) Micro Mechanical Properties and Stability of
Acicular Ferrite in a Low Carbon Microalloyed Steel. Acta Metallurgica Sinica, 42, 19-22.
[84] Poths, R., Higginson, R. and Palmiere, E. (2001) Complex Precipitation Behaviour in a Microalloyed Plate Steel.
Scripta Materialia, 44, 147-151. http://dx.doi.org/10.1016/S1359-6462(00)00617-5
[85] Suikkanen, P., Kömi, J. and Karjalainen, L. (2005) Processing Low and Ultra-Low Carbon Bainitic Steels with Excel-
lent Property Combinations. Proceedings of the International Conference on Microalloying for New Steel Processes
and Applications. Donostia-San Sebastian, 7-9 September, 2005, 535-542.
[86] Asahi, H., Hara, T. and Sugiyama, M. (2004) Metallurgical Design of Ultra-High Strength Steels for Gas Pipelines. In-
ternational Journal of Offshore and Polar Engineering, 14, 11-17.
[87] Wang, M. and He, X. (2002) Effect of Boron Addition on Structure and Properties of. Low Carbon Bainitic Steels.
Iron and Steel Institute of Japan (ISIJ) International, 42, S38-S46.
[88] Misra, R., Tenneti, K., Weatherly, G. and Tither, G. (2003) Microstructure and Texture of Hot-Rolled Cb-Ti and V-Cb
Microalloyed Steels with Differences in Formability and Toughness. Metallurgical and Materials Transactions A, 34,
2341-2351. http://dx.doi.org/10.1007/s11661-003-0297-4
[89] Babbit, M., Valette, P. and Riguat, G. (1991) Development of a New Bainitic Steel With Very High Yield Strength at
SOLLAC. In: DeArdo, A.J. (Ed.), Processing Microstructure and Properties of Microalloyed and Other Modern High
Strength Low Alloy Steels. Iron and Steel Society, 3-6 June 1991, Pittsburgh, 281-288.
[90] Ochi, T., Takahashi, T. and Takada, H. (1988) Improvement of the Toughness of Hot Forged Products through Intra-
granular Ferrite Formation. Proceedings of 30th Mecahnical Working and Steel Proceing Conference, 23-27 October
1988, Dearborn, 65-72.
[91] Wang, K., Wang, L. and Cui, W. (2006) Effect of V and V-N Microalloying on Deformation-Induced Ferrite Trans-
formation in Low Carbon Steels. Journal of Materials Science & Technology, 22, 159-163. (in Chinese).
http://www.jmst.org/EN/Y2006/V22/I02/159
[92] Zhao, S., Wang, Q., Pant, U., Zhang, C., Su, H., Yang, C., Yan, Z. and Zhang, Y. (2007) Fundamental Evaluations on
Microstructure and Mechanical Properties of On-Line Normalizing Processed V-N Microalloyed N80 Class Oil Cas-
ings. Journal of Iron and Steel Research International, 14, 227-233.
http://dx.doi.org/10.1016/S1006-706X(08)60084-9
[93] Ollilainen, V., Kasprzak, W. and Holappa, L. (2003) The Effect of Silicon, Vanadium and Nitrogen on the Microstruc-
ture and Hardness of Air Cooled Medium Carbon Low Alloy Steels. Journal of Materials Processing Technology, 134,
405-412. http://dx.doi.org/10.1016/S0924-0136(02)01131-7
[94] Adamczyk, J. (2006) Development of the Microalloyed Constructional Steels. Journal of Achievements in Materials
and Manufacturing Engineering, 14, 9-20
[95] Wei, H., Liu, G., Zhao, H. and Zhang, M. (2014) Effect of Carbon Content on Hot Deformation Behaviors of Vana-
dium Microalloyed Steels. Materials Science and Engineering A, 596, 112-120.
http://dx.doi.org/10.1016/j.msea.2013.12.063
[96] Sellars, C. and Whiteman, J. (1979) Recrystallization and Grain Growth in Hot Rolling. Metal Science, 13, 187-194.
http://dx.doi.org/10.1179/msc.1979.13.3-4.187
[97] Grange, RG. (1971) The Rapid Heat Treatment of Steel. Metallurgical Transactions, 2, 65-78.
http://dx.doi.org/10.1007/BF02662639
[98] Kolesnik, B.P. (1964) Rapid Heat Treatment of Mn-Si Pipe Steel. Metal Science and Heat Treatment, 6, 100-104.
http://dx.doi.org/10.1007/BF00655386
[99] Yao, J., Du, X. and Liu, X. (2009) Isothermal Growth Kinetics of Ultra-fine Austenite Grains in a Nb-V-Ti Microal-
loyed Steel. Journal of Materials Science & Technology, 25, 615-618.
[100] Tokizane, M., Ameyama, K. and Takao, K. (1988) Ultra-Fine Austenite Grain Steel Produced by Thermomechanical
Processing. Scripta Metallurgica, 22, 697-701. http://dx.doi.org/10.1016/S0036-9748(88)80185-6
[101] Furuhara, T., Kikumoto, K., Saito, H., Sekine, T., Ogawa, T., Morito, S. and Maki, T. (2008) Phase Transformation
from Fine-Grained Austenite. Iron and Steel Institute of Japan (ISIJ) International, 48, 1038-1045.

461
H. Halfa

[102] Grange, R. (1966) Strengthening by Austenite Grain Refinement. Transaction of the American Society Metals, 1, 26-
29.
[103] Anashkin, A., Belov, A., Sokolov, A., Bogatov, A. and Smirnov, S. (1987) Heat Cycling of Carbon Steel Wire. Metal
Science and Heat Treatment, 30, 93-97.
[104] Fedyukin, V. (1984) Thermal Cycling Treatment of Steels and Cast Irons. Leningrad State University, Leningrad.
[105] Koppehaal, T. (1972) A Thermal Processing for TRIP Steel. Metallurgical and Materials Transactions A, 3, 1549-
1554. http://dx.doi.org/10.1007/BF02643045
[106] Konopleva, E., Éntin, R., Bayazitov, V. and Okoemov, Y. (1988) Thermal Cycling Treatment of Low-Carbon Steel
with Hardening from Intercritical Temperature Range. Metal Science and Heat Treatment, 8, 617-620.
http://dx.doi.org/10.1007/BF00778269
[107] Bhadeshia, H. (1992) Bainite in Steel. The Institute of Materials 1 Carlton House Terrace, London.
[108] Wada, T. and Eldis, G. (1982) Transformation Characteristic of 2.25Cr-1Mo Steel, Application of 2.25Cr-1Mo Steel
for Thick-Wall Pressure Vessels. ASTM STP 755, American Society for Testing Materials, Philadelphia, 343-362.
[109] Kimmins, S. and Gooch, D. (1983) Austenite Memory Effect in 1Cr-1Mo-0.75 V (Ti, B) Steel. Materials Science and
Technology, 17, 519-532.
[110] Wang, Q., Zhang, C., Xu, W., Zhao, J., Zhao, S. and Yanz, S. (2007) Refinement of Steel Austenite Grain Under an
Extremely High Degree of Superheating. Journal of Iron and Steel Research International, 14, 161-166.
http://dx.doi.org/10.1016/S1006-706X(08)60072-2
[111] Howe, A. (2009) Industry Perspective on Ultrafine Grained Steels. Journal of Materials Science & Technology, 24,
815-819. http://dx.doi.org/10.1179/174328409X441247
[112] Niikura, N., Fujioka, M., Adachi, A., Matsukura, A., Yokota, T. and Shirota, Y. (2001) New Concepts for Ultrarefine-
ment of Grain Size in Super Metal Project. JMPT 2001, 117, 141-146.
[113] Beladi, H., Kelly, G., Shokouhi, A. and Hodgson, P. (2004) The Evolution of Ultrafine Ferrite Formation through Dy-
namic Strain-Induced Transformation. Materials Science and Engineering A, 371, 343-352.
http://dx.doi.org/10.1016/j.msea.2003.12.024
[114] Abdollah-Zadeh, A. and Eghbali, B (2007) Mechanism of Ferrite Grain Refinement during Warm Deformation of a
Low Carbon Nb-Microalloyed Steel. Materials Science and Engineering A, 457, 219-225.
http://dx.doi.org/10.1016/j.msea.2006.12.022
[115] Najafi-Zadeh, A., Jonas, J. and Yue, S. (1992) Grain Refinement by Dynamic Recrystallization during the Simulated
Warm-Rolling of Interstitial Free Steels. Metallurgical and Materials Transactions A, 23, 2607-2617.
http://dx.doi.org/10.1007/BF02658064
[116] Murty, S., Torizuka, S. and Nagai, K. (2005) Ferrite Grain Size Formed by Large Strain-High Deformation in a 0.15C
Steel. Materials Transactions, 46, 2454-2460. http://dx.doi.org/10.2320/matertrans.46.2454
[117] Ueji, R., Tsuji, N., Minamino, Y. and Koizumi, Y. (2002) Ultra-Grain Refinement of Plain Low Carbon Steel by Cold-
Rolling and Annealing of Martensite. Acta Materialia, 50, 4177-4189.
http://dx.doi.org/10.1016/S1359-6454(02)00260-4
[118] Tsuji, N. and Maki, T. (2009) Enhanced Structural Refinement by Combining Phase Transformation and Plastic De-
formation in Steels. Scripta Materialia, 60, 1044-1049. http://dx.doi.org/10.1016/j.scriptamat.2009.02.028
[119] Hase, K. and Tsuji, N. (2011) Effect of Initial Microstructure on Ultrafine Grain Formation through Warm Deforma-
tion in Medium-Carbon Steels. Scripta Materialia, 65, 404-407. http://dx.doi.org/10.1016/j.scriptamat.2011.05.018
[120] DeArdo, A. (1995) Modern Thermomechanical Processing of Microalloyed Steel: A Physical Metallurgy Perspective.
Proceedings of Microalloying 95 Conference, Pittsburgh, 11-14 June 1995, 15-33.
[121] Tanaka, T. (1981) Controlled Rolling of Steel Plate and Strip. International Metals Revision, 26, 185-212.
http://dx.doi.org/10.1179/imr.1981.26.1.185
[122] Jonas, J. and Sellars, C. (1992) Thermomechanical Processing. In: Charles, J.A., Greenwood, G.W. and Smith, G.S.
Eds., Future Development of Metals and Ceramics, Woodhead Publishing Limited, Cambridge.
[123] Jonas, J. and Yue, S. (1990) Microstructural Evolution during Hot Rolling. Proceedings of the International Sympo-
sium on Mathematical Modeling of Hot Rolling of Steel, Hamilton, 26-29 August 1990, 99-118.
[124] Dutta, B., Palmiere, E.J. and Sellars, C.M. (2001) Modelling the Kinetics of Strain Induced Precipitation in Nb Micro-
alloyed Steels. Acta Materialia, 49, 785-794. http://dx.doi.org/10.1016/S1359-6454(00)00389-X
[125] Dutta, B. and Palmiere, E.J. (2003) Effect of Prestrain and Deformation Temperature on the Recrystallization Behavior
of Steels Microalloyed with Niobium. Metallurgical and Materials Transactions A, 34, 1237-1247.
http://dx.doi.org/10.1007/s11661-003-0234-6

462
 H. Halfa

[126] Alberto, M., Luiz, H. and Oscar, B. (2012) Ultra Grain Refinement during the Simulated Thermo-Mechanical
Processing of Low Carbon Steel, The Journal of Materials Research and Technology, 1, 141-147.
http://dx.doi.org/10.1016/S2238-7854(12)70025-X
[127] Speich, G., Demarest, V. and Miller, R. (1981) Formation of Austenite during Intercritical Annealing of Dual-Phase
Steels. Metallurgical and Materials Transactions A, 12, 1419-1428. http://dx.doi.org/10.1007/BF02643686
[128] Oliveira, M., Jorge, J. and Balancin, O. (2004) Influence of Strain-Induced Nucleation on the Kinetics of Phase Trans-
formation in a Forging Steel during Warm Working. Scripta Materialia, 50, 1157-1162.
http://dx.doi.org/10.1016/j.scriptamat.2004.01.011
[129] Rezaee, A., Kermanpur, A., Najafizadeh, A. and Moallemi, M. (2011) Production of Nano/Ultrafine Grained AISI
201L Stainless Steel through Advanced Thermo-Mechanical Treatment. Materials Science and Engineering A, 528,
5025-5029. http://dx.doi.org/10.1016/j.msea.2011.02.093
[130] Farnoosh, F., Abbas, N., Kermanpur, K., Ali, H. and Roohallah. S. (2010) Production of Nano/Submicron Grained
AISI 304L Stainless Steel through the Martensite Reversion Process. Materials Science and Engineering A, 527, 7334-
7339. http://dx.doi.org/10.1016/j.msea.2010.08.002
[131] Moallemi, M., Kermanpur, A., Najafizadeh, A., Rezaee, A. and Samaei baghbadorani, H. (2012) Formation of Na-
no/Ultrafine Grain Structure in a 201 Stainless Steel Through the Repetitive Martensite Thermomechanical Treatment.
Materials Letters, 89, 22-24. http://dx.doi.org/10.1016/j.matlet.2012.08.058
[132] Eskandari, M., Najafizadeh, A., Kermanpur, A. and Karimi, M. (2009) Potential Application of Nanocrystalline 301
Austenitic Stainless Steel in Lightweight Vehicle Structures. Materials and Design, 30, 3869-3872.
http://dx.doi.org/10.1016/j.matdes.2009.03.043
[133] Momeni, A. and Abbasi, S. (2011) Repetitive Thermomechanical Processing towards Ultra Fine Grain Structure in 301,
304 and 304L Stainless Steels. The Journal of Materials Research and Technology, 27, 338-343.
http://dx.doi.org/10.1016/S1005-0302(11)60071-6
[134] Pickering, F. (1978) Physical Metallurgy and the Design of Steels. Applied Science Publishers, London.
[135] Al-Hajeri, K. (2005) The Grain Coarsening and Subsequent Transformation of Austenite in the HSLA Steel during
High Temperature Thermomechanical Processing. University of Pittsburgh, Pittsburgh, 15-16.
[136] Tanaka, T. (1995) Science and Technology of Hot Rolling Process of Steel. Proceedings of the International Confe-
rence on “Microalloying 95”, Pittsburgh, 11-14 June 1995, 165-181.
[137] Llewellyn, D. (1992) Steels: Metallurgy and Applications. Butterworth-Heinemann Reading, London.
[138] Cohen, C. and Hansen, S. (1985) On the Fundamentals of HSLA Steels, HSLA Steels. Metallurgy and Applications,
Conference Proceeding, ASM International, Beijing, 4-8 November 1985, 61-71.
[139] Gray, J. and DeArdo, A. (1985) Austenite Conditioning Alternatives for Microalloyed Steels Products. HSLA Steels,
Metallurgy and Applications, Conference Proceeding, ASM International, Beijing, 4-8 November 1985, 83-96.
[140] Palmiere, E., Garcia, C. and DeArdo, A. (1994) Compositional and Microstructural Changes Which Attend Reheating
and Grain Coarsening in Steels Containing Niobium. Metallurgical and Materials Transactions A, 25, 277-286.
http://dx.doi.org/10.1007/BF02647973
[141] Priestner, R. and Hodgson, P.D. (1992) Ferrite Grain Coarsening during Transformation of Thermomechanically
Processed C-Mn-Nb Austenite. The Journal of Materials Research and Technology, 8, 849-854.
http://dx.doi.org/10.1179/mst.1992.8.10.849
[142] Hodgson, P.D., Hickson, M.R. and Gibbs, R.K. (1998) The Production and Mechanical Properties of Ultrafine Ferrite.
Materials Science Forum, 284-286, 63-72. http://dx.doi.org/10.4028/www.scientific.net/MSF.284-286.63
[143] Hurley, P.J., Muddle, B.C. and Hodgson, P.D. (2002) The Production of Ultrafine Ferrite during Hot Torsion Testing
of a 0.11 wt pct C Steel. Metallurgical and Materials Transactions A, 33, 2985-2993.
http://dx.doi.org/10.1007/s11661-002-0283-2
[144] Beladi, H., Kelly, G., Shokouhi, A. and Hodgson, P.D. (2004) The Evolution of Ultrafine Ferrite Formation through
Dynamic Strain-Induced Transformation. Materials Science and Engineering A, 371, 343-352.
http://dx.doi.org/10.1016/j.msea.2003.12.024
[145] Priestner, R. and Ibraheem, A.K. (2000) Processing of Steel for Ultrafine Ferrite Grain Structures. Journal of Materials
Science & Technology, 16, 1267-1272. http://dx.doi.org/10.1179/026708300101507497
[146] Azevedo, G., Barbosa, R., Pereloma, E.V. and Santos, D. B. (2005) Development of an Ultrafine Grained Ferrite in a
Low C-Mn and Nb-Ti Microalloyed Steels after Warm Torsion and Intercritical Annealing. Materials Science and En-
gineering A, 402, 98-108. http://dx.doi.org/10.1016/j.msea.2005.04.026
[147] Beladi, H., Kelly, G., Shokouhi, A. and Hodgson, P. (2004) Effect of Thermomechanical Parameters on the Critical
Strain for Ultrafine Ferrite Formation through Hot Torsion Testing. Materials Science and Engineering A, 367, 152-

463
H. Halfa

161. http://dx.doi.org/10.1016/j.msea.2003.09.095
[148] Yada, H., Li, C.M. and Yamagata, H. (2000) Dynamic γ → α Transformation during Hot Deformation in Iron-Nickel-
Carbon Alloys. Iron and Steel Institute of Japan (ISIJ) International, 40, 200-206.
http://dx.doi.org/10.2355/isijinternational.40.200
[149] Chang, y., Kim, N. and Lee, C. (2007) Deformation Induced Ferrite Transformation in Microalloyed Steels: Theory
and Application. Materials Science Forum, 561-565, 2491-2508.
[150] Matsumura, H. and Yada, Y. (1987) Evolution of Ultrafine-Grained Ferrite in Hot Successive Deformation. Transac-
tions of the Iron and Steel Institute of Japan, 27, 492-498. http://dx.doi.org/10.2355/isijinternational1966.27.492
[151] Calcagnotto, M., Ponge, D. and Raabe, D. (2008) Ultrafine Grained Ferrite/Martensite Dual Phase Steel Fabricated by
Large Strain Warm Deformation and Subsequent Intercritical Annealing. Iron and Steel Institute of Japan (ISIJ) Inter-
national, 48, 1096-1101. http://dx.doi.org/10.2355/isijinternational.48.1096
[152] Calcagnotto, M., Ponge, D. and Raabe, D. (2010) Effect of Grain Refinement to 1 µm on Strength and Toughness of
Dual-phase Steels. Materials Science and Engineering A, 527, 7832-7840.
http://dx.doi.org/10.1016/j.msea.2010.08.062
[153] Eduardo D., Akira, Y. and Jun, Y. (2014) Modeling Static and Dynamic Kinetics of Microstructure Evolution in Type
316 Stainless Steel. Steel Research International, 85, 1099-1108. http://dx.doi.org/10.1002/srin.201300173
[154] Akira, Y., Mamoru, I., Hisanao, K. and Jun, Y. (2012) Multistage and High-speed Compression Testing Machine for
Obtaining Flow Stress and Microstructure Evolution in Hot Forming of Steels. Iron and Steel Institute of Japan (ISIJ)
International, 52, 574-581. http://dx.doi.org/10.2355/isijinternational.52.574
[155] Toshiro, T., Norio, I. Kaori, M., Suguhiro, F., Mitsuru, Y., Masayuki, W., Manabu, E., Tamotsu, S., Youichi, H. and
Yasutaka, O. (2008) Grain Refinement of C-Mn Steel to 1 μm by Rapid Cooling and Short Interval Multi-Pass Hot
Rolling in Stable Austenite Region. Iron and Steel Institute of Japan (ISIJ) International, 48, 1148-1157.
[156] Manabu, E., Suguhiro, F., Tamotsu, S., Youichi, H., Kaori, M., Masayuki, W., Toshiro, T., Norio, I., Mitsuru, Y. and
Yasutaka, O. (2008) Super Short Interval Multi-Pass Rolling Process for Ultrafine-Grained Hot Strip. Iron and Steel
Institute of Japan (ISIJ) International, 48, 1142-1147.
[157] Valiev, R., Sergueeva, A. and Mukherjee, A. (2003) The Effect of Annealing on Tensile Deformation Behavior of Na-
nostructure SPD Titanium. Scripta Materialia, 49, 669-674. http://dx.doi.org/10.1016/S1359-6462(03)00395-6
[158] Alexandrov, I. and Valiev, R. (2001) Developing of SPD Processing and Enhanced Properties in Bulk Nanostructured
Metals. Scripta Materialia, 44, 1605-1608. http://dx.doi.org/10.1016/S1359-6462(01)00783-7
[159] Stolyarov, V., Zhu, Y., Lowe, T., Islamgaliev, R. and Valiev, R. (1999) A Two Step SPD Processing of Ultrafine-
Grained Titanium. Nanostructred Materials, 11, 947-954. http://dx.doi.org/10.1016/S0965-9773(99)00384-0
[160] Valiev, R., Krasilnikov, N. and Tsenev, N. (1991) Plastic Deformation of Alloys with Submicro-Grained Structure.
Materials Science and Engineering A, 137, 35-40. http://dx.doi.org/10.1016/0921-5093(91)90316-F
[161] Segal, V., Dobatkin, S. and Valiev, R. (editors) (2004) Equal-Channel Angular Pressing of Metallic Materials: Achie-
vements and Trends. Thematic Issue, Part 1, Russian Metall, 1, 1-102. (translated from Metally 2004, no. 1, pp. 3-119).
[162] Brandon, D.G. (1966) The Structure of High-Angle Grain Boundaries Structure de Joints de Grains a Grands Angles.
Acta Metallurgica, 14, 1479-1484. http://dx.doi.org/10.1016/0001-6160(66)90168-4
[163] Zhilyaev, A. and Langdon, T. (2008) Using High-Pressure Torsion for Metal Processing: Fundamentals and Applica-
tions. Progress in Materials Science, 53, 893-979. http://dx.doi.org/10.1016/j.pmatsci.2008.03.002
[164] Mishra, R.S. Valiev, R.Z. and A.K. Mukherjee, A.K. (1997) The Observation of Tensile Superplasticity in Nanocrys-
talline Materials. Nanostructured Materials, 9, 473-476. http://dx.doi.org/10.1016/S0965-9773(97)00103-7
[165] Zhilyaev, A., Nurislamova, G., Kim, B., Baro, M., Szpunar, J. and Langdon, T. (2003) Experimental Parameters In-
fluencing Grain Refinement and Microstructural Evolution During High-Pressure Torsion. Acta Materialia, 51, 753-
765. http://dx.doi.org/10.1016/S1359-6454(02)00466-4
[166] Salishchev, G., Valiahmetov, O. and Galeev, R. (1993) Formation of Submicrocrystalline Structure in Titanium Alloy
VT8 and Its Influence on Mechanical Properties. Journal of Materials Science, 28, 2898-2902.
http://dx.doi.org/10.1007/BF00354692
[167] Sevillano, J., Houtte, P. and Aernoudt, E. (1980) Large Strain Work Hardening and Textures. Progress in Materials
Science, 25, 69134. http://dx.doi.org/10.1016/0079-6425(80)90001-8
[168] Sitdikov, O., Sakai, T., Goloborodko, A., Miura, H. and Kaibyshev, R. (2004) Effect of Pass Strain on Grain Refine-
ment in 7475 Al Alloy during Hot Multidirectional Forging. Materials Transactions, 45, 2232-2238.
http://dx.doi.org/10.2320/matertrans.45.2232
[169] Beygelzimer, Y., Varyukhin, V., Orlov, D., Synkov, S., Spuskanyuk, A. and Pashinska,Y. (2004) Severe Plastic De-

464
 H. Halfa

formation by Twist Extrusion. In: Zehetbauer, M.J. and Valiev, R.Z., Eds., Nanomaterials by Severe Plastic Deforma-
tion. Wiley-VCH Verlag, Weinheim, 511-516.
[170] Varyutkhin, V., Beygelzimer, Y., Synkov, S. and Orlov. D. (2006) Application of Twist Extrusion. Materials Science
Forum, 503-504, 335-340.
[171] Bay, B., Hansen, N., Hughes, D.A. and Kuhlmann-Wilsdorf, D. (192) Overview No. 96 Evolution of f.c.c. Deforma-
tion Structures in Polyslip. Acta Metallurgica et Materialia, 40, 205-219.
http://dx.doi.org/10.1016/0956-7151(92)90296-Q
[172] Richert, M., Liu, Q. and Hansen, N. (1999) Microstructural Evolution over a Large Strain Range in Aluminum De-
formed by Cyclic-Extrusion Compression. Materials Science and Engineering A, 260, 275-283.
http://dx.doi.org/10.1016/S0921-5093(98)00988-5
[173] Chu, H., Liu, K. and Yeh, J. (2000) Study of 6061-Al2O3p Composites Produced by Reciprocating Extrusion. Metal-
lurgical and Materials Transactions A, 31, 2587-2596. http://dx.doi.org/10.1007/s11661-000-0203-2
[174] Chu, H., Liu, K. and Yeh, J. (2001) Aging Behavior and Tensile Properties of 6061Al-0.3 μm Al2O3p Particle Com-
posites Produced by Reciprocating Extrusion, Scripta Materialia, 45, 541-546.
http://dx.doi.org/10.1016/S1359-6462(01)01055-7
[175] Huang, I., Zhu, Y., Jiang, H. and Lowe, T. (2001) Microstructures and Dislocation Configurations in Nanostructured
Cu Processed by Repetitive Corrugation and Straightening, Acta Materialia, 49, 1497-1505.
http://dx.doi.org/10.1016/S1359-6454(01)00069-6
[176] Zhu, Y., Jiang, H., Huang, J. and Lowe, T. (2001) A New Route to Bulk Nanostructured Metals. Metallurgical and
Materials Transactions A, 32, 1559-1562. http://dx.doi.org/10.1007/s11661-001-0245-0
[177] Shin, D., Park, J., Kim, Y. and Park, K. (2002) Constrained Groove Pressing and Its Application to Grain Refinement
of Aluminum. Materials Science and Engineering A, 328, 98-103. http://dx.doi.org/10.1016/S0921-5093(01)01665-3
[178] Zhao, X., Jing, T.F., Gao, Y.W., Zhou, J.F. and Wang, W. (2004) A New SPD Process for Spheroidal Cast Iron. Mate-
rials Letters, 58, 2335-2339. http://dx.doi.org/10.1016/j.matlet.2004.01.034
[179] Saito, Y., Tsuji, N., Utsunomiya, H., Sakai, T. and Hong, R.G. (1998) Ultra-Fine Grained Bulk Aluminum Produced
by Accumulative Roll-Bonding (ARB) Process. Scripta Materialia, 39, 1221-1227.
http://dx.doi.org/10.1016/S1359-6462(98)00302-9
[180] Saito, Y., Utsunomiya, H., Tsuji, N. and Sakai, T. (1999) Novel Ultra-High Straining Process for Bulk Materials—
Development of the Accumulative Roll-bonding (ARB) Process. Acta Materialia, 47, 579-583.
http://dx.doi.org/10.1016/S1359-6454(98)00365-6
[181] Rhodes, C., Mahoney, M., Bingel, W., Spurling, R. and Bampton, C. (1997) Effects of Friction Stir Welding on Mi-
crostructure of 7075 Aluminum. Scripta Materialia, 36, 69-75. http://dx.doi.org/10.1016/S1359-6462(96)00344-2
[182] Mishra, R., Ma, Z. and Charit, I. (2003) Friction Stir Processing: A Novel Technique for Fabrication of Surface Com-
posite. Materials Science and Engineering A, 341, 307-310. http://dx.doi.org/10.1016/S0921-5093(02)00199-5
[183] Hofmann, D. and Vecchio, K. (2005) Submerged Friction Stir Processing (SFSP): An Improved Method for Creating
Ultra-fine-grained Bulk Materials. Materials Science and Engineering A, 402, 234-241.
http://dx.doi.org/10.1016/j.msea.2005.04.032
[184] Hofmann, D. and Vecchio, K. (2007) Thermal History Analysis of Friction Stir Processed and Submerged Friction Stir
Processed Aluminum, Materials Science and Engineering A, 465, 165-175.
http://dx.doi.org/10.1016/j.msea.2007.02.056
[185] Valiev, R., Krasilnikov, N. and Tsenev, N. (1991) Plastic Deformation of Alloys with Submicron-Grained Structure.
Materials Science and Engineering A, 137, 35-40. http://dx.doi.org/10.1016/0921-5093(91)90316-F
[186] Fukuda, Y., Oh-Ishi, K., Horita, Z. and Langdon, T.G. (2002) Processing of a Low-Carbon Steel by Equal-channel
Angular Pressing. Acta Materialia, 50, 1359-1368. http://dx.doi.org/10.1016/S1359-6454(01)00441-4
[187] Shin, D., Kim, B., Kim, Y. and Park, K. (2000) Microstructural Evolution in a Commercial Low Carbon Steel by Equal
Channel Angular Pressing. Acta Materialia, 48, 2247-2256. http://dx.doi.org/10.1016/S1359-6454(00)00028-8
[188] Tóth, L. (2005) Modelling of Strain Hardening and Microstructural Evolution in Equal Channel Angular Extrusion.
Computational Materials Science, 32, 568-576. http://dx.doi.org/10.1016/j.commatsci.2004.09.007
[189] Hansen, N. and Barlow, C.Y. (2014) 17—Plastic Deformation of Metals and Alloys. Physical Metallurgy (Fifth Edi-
tion), II, 1681-1764. http://dx.doi.org/10.1016/B978-0-444-53770-6.00017-4
[190] Segal, V. (1995) Equal Channel Angular Extrusion: From Macromechanics to Structure Formation. Materials Science
and Engineering A, 271, 322-333. http://dx.doi.org/10.1016/S0921-5093(99)00248-8
[191] Tóth, I., Massion, R., Germain, L., Baik, S. and Suwas, S. (2003) Analysis of Texture Evolution in Equal Channel

465
H. Halfa

Angular Extrusion of Copper Using a New Flow Field. Acta Materialia, 52, 1885-1898.
http://dx.doi.org/10.1016/j.actamat.2003.12.027
[192] Beyerlein, I. and Tome, C. (2004) Analytical Modeling of Material Flow in Equal Channel Angular Extrusion (ECAE).
Materials Science and Engineering A, 380, 171-190. http://dx.doi.org/10.1016/j.msea.2004.03.063
[193] Valiev, R., Islamgaliev, R. and Alexandrov, I. (2000) Bulk Nanostructured Materials from Severe Plastic Deformation.
Progress in Materials Science, 45, 103-189. http://dx.doi.org/10.1016/S0079-6425(99)00007-9
[194] Zhu, Y. and Langdon, T. (2004) Fundamentals of Nanostructured Materials by Severe Plastic Deformation. The Jour-
nal of the Minerals, Metals & Materials Society (TMS), 56, 58-63. http://dx.doi.org/10.1007/s11837-004-0294-0
[195] Raab, G., Valiev, R., Lowe, T. and Zhu, Y. (2004) Continuous Processing of Ultrafine Grained Al by ECAP-Conform.
Materials Science and Engineering A, 382, 30-34. http://dx.doi.org/10.1016/j.msea.2004.04.021
[196] Tsuji, N., Saito, Y., Lee, S. and Minamino, Y. (2003) ARB (Accumulative Roll-Bonding) and Other New Techniques
to Produce Bulk Ultrafine Grained Materials. Advanced Engineering Materials, 5, 338-344.
http://dx.doi.org/10.1002/adem.200310077
[197] Saito, Y., Utsunomiya, H., Tsuji, N. and Sakai, T. (1999) Novel Ultra-High Straining Process for Bulk Materials—
Development of the Accumulative Roll-bonding (ARB) Process. Acta Materialia, 47, 579-583.
http://dx.doi.org/10.1016/S1359-6454(98)00365-6
[198] Tsuji, I., Ito, Y., Saito, Y. and Minamino, Y. (2002) Strength and Ductility of Ultrafine Grained Aluminum and Iron
Produced by ARB and Annealing, Scripta Materialia, 47, 893-899. http://dx.doi.org/10.1016/S1359-6462(02)00282-8
[199] Costa, A., Reis, L., Kestens, M. and Andrade, A. (2005) Ultra Grain Refinement and Hardening of IF-Steel during
Accumulative Roll-bonding. Materials Science and Engineering A, 406, 279-285.
http://dx.doi.org/10.1016/j.msea.2005.06.058
[200] Cao, Y., Wang, Y., Liao, X. Kawasaki, M., Ringer, S., Langdon, T.G. and Zhu. Y.T. (2014) Concurrent Microstructur-
al Evolution of Ferrite and Austenite in a Duplex Stainless Steel Processed by High-Pressure Torsion. Acta Materialia,
63, 16-29. http://dx.doi.org/10.1016/j.actamat.2013.09.030
[201] Valiev, R., Korznikov, A. and Mulyukov, R. (1993) Structure and Properties of Ultrafine-Grained Materials Produced
by Severe Plastic Deformation, Materials Science and Engineering A, 186, 141-148.
http://dx.doi.org/10.1016/0921-5093(93)90717-S
[202] Nakao, Y. and Miura, H. (2011) Nano-Grain Evolution in Austenitic Stainless Steel during Multi-Directional Forging.
Materials Science and Engineering A, 528, 1310-1317. http://dx.doi.org/10.1016/j.msea.2010.10.018
[203] Huang, J. and Xu, Z. (2006) Evolution Mechanism of Grain Refinement Based on Dynamic Recrystallization in Mul-
tiaxially Forged Austenite. Materials Letters, 60, 1854-1858.http://dx.doi.org/10.1016/j.matlet.2005.12.110
[204] Tsuji, N., Kitahara, H., Ueji, R. and Ueda, M. (2005) Crystallographic Analysis of Martensite in Steels by Means of
EBSD. Proceedings of International Conference on Martensitic Transformations (ICOMAT 05), 14-17 June 2005,
Shanghai. KEYNOTE lecture in the session E.
[205] Guthrie, R. and Jonas, J. (1993) ASM Handbook. 10th Edition, Vol. 1, American Society for Metals, Metals Park,
288-292.
[206] Tsuji, I., Ueji, R., Minamino, Y. and Saito, Y. (2002) A New and Simple Process to Obtain Nano-structured Bulk Low-
Carbon Steel with Superior Mechanical Property. Scrpita Materiala, 46, 305-310.
http://dx.doi.org/10.1016/S1359-6462(01)01243-X
[207] Soleymani, V. and Eghbali, B. (2012) Grain Refinement in a Low Carbon Steel through Multidirectional Forging.
Journal of Iron and Steel Research International, 19, 74-78. http://dx.doi.org/10.1016/S1006-706X(12)60155-1
[208] Shiro, T., Akio, O., Narayana, M., Murty, S.V.S. and Kotobu, N. (2006) Effect of Strain on the Microstructure and
Mechanical Properties of Multi-Pass Warm Caliber Rolled Low Carbon Steel. Scripta Materialia, 54, 563-568.
http://dx.doi.org/10.1016/j.scriptamat.2005.10.055
[209] Valiev, R. and Langdon, T. (2006) Principles of Equal-Channel Angular Pressing as a Processing Tool for Grain Re-
finement. Progress in Materials Science, 51, 881-981. http://dx.doi.org/10.1016/j.pmatsci.2006.02.003
[210] Ji, Y. and Park, J. (2009) Development of Severe Plastic Deformation by Various Asymmetric Rolling Processes. Ma-
terials Science and Engineering A, 499, 14-17. http://dx.doi.org/10.1016/j.msea.2007.11.099
[211] Alihosseini, H., Asle Zaeem, M. and Dehghani, K. (2012) A Cyclic Forward-Backward Extrusion Process as a Novel
Severe Plastic Deformation for Production of Ultrafine Grains Materials. Materials Letters, 68, 204-208.
http://dx.doi.org/10.1016/j.matlet.2011.10.037
[212] Saito, Y., Tsuji, N., Utsunomiya, H., Sakai, T. and Hong, R.G. (1998) Ultra-Fine Grained Bulk Aluminum Produced
by Accumulative Roll-bonding (ARB) Process. Scripta Materialia, 39, 1221-1227.

466
 H. Halfa

http://dx.doi.org/10.1016/S1359-6462(98)00302-9
[213] Shin, D., Park, J., Kim, Y. and Park, K. (2002) Constrained Groove Pressing and Its Application to Grain Refinement
of Aluminum. Materials Science and Engineering A, 328, 98-103. http://dx.doi.org/10.1016/S0921-5093(01)01665-3
[214] Tsuji, I., Saito, Y., Utsunomiya, H. and Tanigawa, S. (1999) Ultra-Fine Grained Bulk Steel Produced by Accumulative
Roll-Bonding (ARB) Process. Scripta Materialia, 40, 795-800. http://dx.doi.org/10.1016/S1359-6462(99)00015-9
[215] Krishnaiah, I., Chakkingal, U. and Venugopal, P. (2005) Production of Ultrafine Grain Sizes in Aluminium Sheets by
Severe Plastic Deformation Using the Technique of Groove Pressing. Scripta Materialia, 52, 1229-1233.
http://dx.doi.org/10.1016/j.scriptamat.2005.03.001
[216] Khodabakhshi, F., Kazeminezhad, M. and Kokabi, A.H. (2010) Constrained Groove Pressing of Low Carbon Steel:
Nano-Structure and Mechanical Properties. Materials Science and Engineering A, 527, 4043-4049.
http://dx.doi.org/10.1016/j.msea.2010.03.005
[217] Alihosseini, H. and Dehghani, K. (2012) Bake Hardening of Ultra-Fine Grained Low Carbon Steel Produced by Con-
strained Groove Pressing. Materials Science and Engineering A, 549, 157-162.
http://dx.doi.org/10.1016/j.msea.2012.04.024
[218] Khodabakhshi, F., Kazeminezhad, M. and Kokabi, A.H. (2012) Resistance Spot Welding of Ultra-Fine Grained Steel
Sheets Produced by Constrained Groove Pressing: Optimization and Characterization. Material Characterization, 69,
71-83. http://dx.doi.org/10.1016/j.matchar.2012.04.011
[219] Shiro, T., Matthias, K., Yoshiyuki, F. and Manfred, B. (2012) Effect of Tensile Strength and Microstructure on Notch-
Fatigue Properties of Ultrafine-Grained Steels. Iron and Steel Institute of Japan (ISIJ) International, 52, 910-914.
http://dx.doi.org/10.2355/isijinternational.52.910
[220] Ohmori, I., Torizuka, S., Nagai, K., Koseki N. and Kogo, Y. (2003) Transformations and Microstructures -Evolution of
Ultrafine-Grained Ferrite Structure through Multi-Pass Warm Caliber-Rolling. Tetsu-To-Hagane/Journal of the Iron
and Steel Institute of Japan, 89, 781-788.
[221] Murty, S. and Torizuka, S. (2008) Microstructure-Mechanical Properties Correlation in Ultrafine Grained Steels Pro-
cessed by Large Strain Warm Deformation. Iron and Steel Institute of Japan (ISIJ) International, 48, 1088-1095.
http://dx.doi.org/10.2355/isijinternational.48.1088
[222] Torizuka, S., Muramatsu, E., Murty, S. and Nagai, K. (2006) Microstructure Evolution and Strength-Reduction in Area
Balance of Ultrafine-Grained Steels Processed by Warm Caliber Rolling. Scrpita Materiala, 55, 751-754.
http://dx.doi.org/10.1016/j.scriptamat.2006.03.067
[223] Kimura, Y., Inoue, T., Yin, F. and Tsuzaki, K. (2008) Inverse Temperature Dependence of Toughness in an Ultrafine
Grain-Structure Steel. Science, 320, 1057-1060.
[224] Kimura, Y., Inoue, T., Yin, F. and Tsuzaki, K. (2010) Delamination Toughening of Ultrafine Grain Structure Steels
Processed through Tempforming at Elevated Temperatures. Iron and Steel Institute of Japan (ISIJ) International, 50,
152-161. http://dx.doi.org/10.2355/isijinternational.50.152
[225] Kimura, Y., Inoue, T. and Tsuzaki, K. (2013) Tempforming in Medium-Carbon Low-Alloy Steel. Journal of Alloys
and Compounds, 577, S538-S542. http://dx.doi.org/10.1016/j.jallcom.2011.12.123
[226] Wu, Z., Ding, H., Li, H., Huang, M. and Cao, F. (2013) Microstructural Evolution and Strain Hardening Behavior dur-
ing Plastic Deformation of Fe-12Mn-8Al-0.8C Steel. Materials Science and Engineering A, 584, 150-155.
http://dx.doi.org/10.1016/j.msea.2013.07.023
[227] Kang, S., Na, Y., Park, K., Jeon, J., Son, S. and Lee, J. (2007) A Study on the Micro-Formability of Al 5083 Super-
plastic Alloy Using Micro-Forging Method. Materials Science and Engineering A, 449-451, 338-342.
http://dx.doi.org/10.1016/j.msea.2006.01.166
[228] Langdon. T. (2013) Twenty-Five Years of Ultrafine-Grained Materials: Achieving Exceptional Properties through
Grain Refinement, Acta Materialia, 61, 7035-7059. http://dx.doi.org/10.1016/j.actamat.2013.08.018
[229] Lesuer, D., Syn, C. and Sherby, O. (1996) Ultrahigh Carbon Steel for Automotive Applications. 1996 SAE Interna-
tional Congress & Exposition, Detroit, 26-29 February 1996, 26-29.
[230] Elices, M. (2004) Influence of Residual Stresses in the Performance of Cold Drawing Pearlitic Wires. Journal of Mate-
rials Science, 39, 3889-3899. http://dx.doi.org/10.1023/B:JMSC.0000031470.31354.b5
[231] Zhao, M., Yang, K. and Shan, Y. (2002) The Effects of Thermo-Mechanical Control Process on Microstructures and
Mechanical Properties of a Commercial Pipeline Steel. Materials Science and Engineering A, 335, 14-20.
http://dx.doi.org/10.1016/S0921-5093(01)01904-9
[232] Bott, I., Teixeira, L. and Rios, R. (2005) High-Strength Steel Development for Pipelines. Metallurgical and Materials
Transactions A, 36, 443-454.http://dx.doi.org/10.1007/s11661-005-0315-9
[233] Hillenbrand, I., Graf, I. and Kalwa, I. (2001) Development and Production of High Strength Pipeline Steels. Proceed-

467
H. Halfa

ings of the Conference Niobium, Orlando, 2-5, December 2001.

[234] Takahashi, I. and Iino, M. (1996) Thermomechanical Control Process as a Tool to Grain Refine the Low Manganese-
containing Steel for Sour Service Line Pipe. Iron and Steel Institute of Japan (ISIJ) International, 36, 235-240.
http://dx.doi.org/10.2355/isijinternational.36.235
[235] Takahashi, A. and Iino, M. (1996) Microstructure Refinement by Cu Addition and Its Effect on Strengthening and
Toughening of Sour Service Line Pipe. Iron and Steel Institute of Japan (ISIJ) International, 36, 241-245.
http://dx.doi.org/10.2355/isijinternational.36.241
[236] Contreras, A., Albiter, A., Salazar, M. and Perez, R. (2005) Slow Strain Rate Corrosion and Fracture Characteristics of
X-52 and X-70 Pipeline Steels. Materials Science and Engineering A, 407, 45-52.
http://dx.doi.org/10.1016/j.msea.2005.07.028
[237] Kim, Y., Kim, S., Lim, Y. and Kim, N. (2002) Effect of Microstructure on the Yield Ratio and Low Temperature
Toughness of Line-Pipe Steels. Iron and Steel Institute of Japan (ISIJ) International, 42, 1571-1577.
http://dx.doi.org/10.2355/isijinternational.42.1571
[238] Zhong, Y., Xiao,F., Zhang, J., Shan, Y., Wang, W. and Yang, K. (2006) In Situ TEM Study of the Effect of M/A Films
at Grain Boundaries on Crack Propagation in an Ultra-fine Acicular Ferrite Pipeline Steel. Acta Materialia, 54, 435-
443. http://dx.doi.org/10.1016/j.actamat.2005.09.015
[239] Skripnyuk, V., Rabkin, E., Estrin, Y. and Lapovok, R. (2004) The Effect of Ball Milling and Equal Channel Angular
Pressing on the Hydrogen Absorption/Desorption Properties of Mg-4.95 wt% Zn-0.71 wt% Zr (ZK60) Alloy. Acta
Materialia, 52, 405-414. http://dx.doi.org/10.1016/j.actamat.2003.09.025
[240] Latysh, V., Krallics, G.Y., Alexandrov, I. and Fodor. A. (2006) Application of Bulk Nanostructured Materials in Med-
icine. Current Applied Physics, 6, 262-266.http://dx.doi.org/10.1016/j.cap.2005.07.053
[241] Eissa, M. (1988) The Effect of Microalloying Additions and Hot Rolling Condition on the Mechanical Properties of
High Strength Low Alloy Steels. Ph.D. Thesis, Faculty of Engineering, Cairo University, Egypt.
[242] Baraka, I., El-Fawakhry, K., Mishreky, M.L., Eissa, M. and Lamei, M.M. (1989) Effect of Titanium as Microalloying
Element on the Mechanical Properties of High Strength Low Alloy Steel. 2nd International Conference on Mining and
Metallurgical Engineering, Suez Canal University, 20-22 March 1989, 580-588.
[243] El-Fawakhry, K., Mishreky, M.L. and Eissa, M. (1990) Secondary Hardening of Vanadium and Titanium Microalloyed
Steels. Scandinavian Journal of Metallurgy, 19, 33-38.
[244] Mekkawy, M.F., El-Fawakhry, K., Mishreky, M.L. and Eissa, M. (1990) Effect of Rolling Schedule on Mechanical
Properties and Structure of V- and Ti-Microalloyed Steels. Scandinavian Journal of Metallurgy, 19, 82-84.
[245] Mekkawy, M.F., El-Fawakhry, K., Mishreky, M.L. and Eissa, M. (1990) Effect of Reheating Temperature on Micro-
structure and Strength of V- and Ti-microalloyed Steels. Scandinavian Journal of Metallurgy, 19, 236-245.
[246] Mekkawy, M.F., El-Fawakhry, K., Mishreky, M.L. and Eissa, M. (1990) Effect of Finish-rolling Temperature on Mi-
crostructure and Strength of V- and Ti-Microalloyed Steels. Scandinavian Journal of Metallurgy, 19, 246-256.
[247] Mekkawy, M.F., El-Fawakhry, K., Mishreky, M.L. and Eissa, M. (1990) Direct Quenching of Low Manganese Steels
Microalloyed with Vanadium or Titanium. Transactions of the Iron and Steel Society (ISS), Iron and Steelmaker, Oc-
tober (1990), 75-83.
[248] Mekkawy, M.F., El-Fawakhry, K., Mishreky, M.L. and Eissa, M. (1990) Effect of Interrupted Accelerated Cooling on
Mechanical Properties and Structure of V- and Ti-Microalloyed Steel Bars. Materials Science and Technology, 7, 28-
36. http://dx.doi.org/10.1179/mst.1991.7.1.28
[249] Eissa, M., El-Fawakhry, K., Mishreky, M.L. and Abd ElKarim, O. (1993) Production of Titanium Microalloyed Rein-
forcing Steel Bars in Open Hearth Furnaces. AMSE Transactions, 34, 1-15.
[250] Lamei, M.M. (1993) The Effect of Microalloying Elements on the Mechanical Properties of Low Carbon-Manganese
Steel. Ph.D. Thesis, Faculty of Science, Cairo University, Egypt.
[251] Tawfik, I. (1993) Effect of Vanadium and Nitrogen on Mechanical Properties of Low Carbon Steels. M.Sc. Thesis,
Faculty of Engineering, Cairo University, Egypt.
[252] Fathi, A. (1994) Microalloyed High Carbon Steel. M.Sc. Thesis, Faculty of Science, Helwan University, Egypt.
[253] Eissa, M., El-Fawakhry, K., El-Faramawy, H. and Fathy, A. (1996) Production of Ultra High Strength Wire Rod Steels
by Vanadium Microalloying. Steel Research, 67, 100-105.
[254] Eissa, M., El-Fawakhry, K., El-Faramawy, H. and Fathy, A. (1996) Vanadium-Microalloyed High Carbon Steel.
Transactions of Iron and Steel Society (ISS), Iron and Steelmaker, 23, 73-81
[255] Eissa, M., El-Fawakhry, K., Ahmed, M., El-Zommor, M. and Lamei, M.M. (1997) Development of Superior High
Strength Low Impact Transition Temperature Steels Microalloyed with Vanadium and Nitrogen. Journal of Materials

468
 H. Halfa

Science and Technology, 5, 3-19.

[256] Eissa, M., El-Fawakhry, K., Mishreky, M.L. Hussein, A.H. and Tawfik, A. (1998) Low Carbon Manganese Steels Mi-
croalloyed with Vanadium and Nitrogen. Steel Research, 69, 334-342.
[257] El-Fawakhry, K., Eissa, M. and Mishreky, M.L. (1998) Production of High Strength Steel for Prestressed Concrete
Using Microalloying Technology. AISU 2nd International Symposium on “Electric Furnace”, Damascus, 18-20 Oc-
torber 1998.
[258] Eissa, M. (1998) Influence of Base Composition on the Strength of Vanadium-Microalloyed Steel Bars. Steel Research,
69, 438-445.
[259] Eissa, M. and Mattar, T. (2002) Mechanical Properties Relationships in V- and Ti-Microalloyed Steels. Steel Research,
73, 403-408.
[260] Eissa, M., Abd El-Aziz, A., Ghaly, S., Halfa, H. and Saber, S. (2011) Effect of Microalloying Additions on the Micro-
structure and Mechanical Properties of Low Carbon Steel. Journal of Iron and Steel Research International, 18, 246-
251.
[261] Eissa, M., Mekkawy, F., El-Fawakhry, K. and Mishreky, M.L. (1991) Characterization of Precipitates in Vanadium
and Titanium Microalloyed Steels. Iron and Steel Institute of Japan (ISIJ) International, 31, 1020-1025.
http://dx.doi.org/10.2355/isijinternational.31.1020

469