Surface & Coatings Technology 213 (2012) 221228

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Surface & Coatings Technology

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Effect of surface mechanical attrition treatment (SMAT) on boronizing of EN8 steel

T. Balusamy a, c, T.S.N. Sankara Narayanan a, b,, K. Ravichandran c
a
CSIR-National Metallurgical Laboratory, Madras Centre, CSIR Complex, Taramani, Chennai-600 113, India
b
Department of Dental Biomaterials, School of Dentistry, Chonbuk National University, Jeonju 561-756, South Korea
c
Department of Analytical Chemistry, University of Madras, Maraimalai (Guindy) Campus, Chennai-600 025, India

a r t i c l e i n f o a b s t r a c t

Article history: The effect of SMAT on pack boronizing of EN8 steel is addressed. SMAT induced plastic deformation, enabled
Received 2 July 2012 nanocrystallization at the surface, reduced the grain size and increased the volume fraction of non-
Accepted in revised form 21 October 2012 equilibrium gain boundaries, accumulation of defects and dislocations at the grain boundaries and within
Available online 27 October 2012
the grains. These features helped to promote the diffusion of boron. The present study demonstrates for
the rst time that SMAT treated EN8 steel can be boronized with a reasonable case depth at 923 K for 7 h.
Keywords:
Surface mechanical attrition treatment
It also addresses the benets of duplex treatment methodology to achieve the desired case depth and a
(SMAT) dense boronized layer. Formation of an FeB phase along with an Fe2B phase for SMAT treated EN8 steel has
Boronizing also been reported for the rst time. The ndings of the study recommend that SMAT can be used as a
Iron borides pretreatment for boronizing of steel, provided necessary precautions are made on boron concentration, to
Diffusion control the volume fraction of the deleterious FeB phase.
Kinetics 2012 Elsevier B.V. All rights reserved.
Duplex treatment

1. Introduction Surface mechanical attrition treatment (SMAT) is a surface severe

plastic deformation method that enables nanocrystallization at the
Boronizing is a thermo-chemical process, which involves diffusion surface of various metallic materials [1623]. Tong et al. [24] have
of boron atoms into the surface of metal/alloy to produce a layer of shown that surface nanocrystallization promotes chemical reactivity
borides of the corresponding metal/alloying elements [1,2]. Surface and diffusion of nitrogen so that gaseous nitriding of an iron plate
modication by boronizing is widely employed to improve the hard- could be performed even at 573 K instead of ~ 823 K, which is com-
ness, tribological properties and corrosion resistance of ferrous alloys monly practised in conventional gaseous nitriding processes. Similar-
[39]. Various types of boronizing, namely, pack, paste, electrolytic, ly, SMAT enabled the formation of a nitrided layer on pure iron, which
laser, etc., have been developed to meet the challenging needs of var- is two times thicker than those formed on its course-grained counter-
ious industries [1015]. Irrespective of the type of boronizing used, part, under similar gaseous nitriding conditions (773 K for 2 h) [25].
the case depth, phase contents, hardness and tribological properties It has been reported that SMAT of low carbon steel promoted the dif-
of the resultant boronized layers are primarily determined by the sur- fusion of aluminium so that the resultant aluminized layers were
face reactions and the kinetics of boron diffusion. Among the various three times thicker than those that were formed on coarse-grained
types of boronizing, pack boronizing assumes signicance following ones, when subjected to pack aluminizing at 873 K for 8 h [26].
its easy adaptability in process industries. Pack boronizing is usually SMAT of AISI H13 tool steel enhanced the diffusion of chromium up
performed using a boronizing mixture consisting of the active ingre- to ~ 5.2 m when chromizing was performed at 873 K for 2 h whereas
dient (usually B4C), an activating agent (usually KBF4) and a diluent coarse-grained H13 tool steel fails to show the diffusion of chromium
(usually SiC) at 11731273 K for a few hours depending on the de- under similar conditions [27]. Wang et al. [28] have studied the reac-
sired case depth. The major concerns in using such operating condi- tive diffusion kinetics of zinc on coarse-grained and SMAT treated
tions are material distortion, carbide precipitation, grain growth and iron samples after electrodepositing them with zinc and subsequently
the associated degradation in mechanical properties of materials. Im- subjecting them to diffusion treatment. According to them, the for-
proving the surface reactivity and accelerating the diffusion of boron mation of a large number of grain boundaries in the nanostructured
at relatively lower temperatures are always challenging. iron by SMAT decreased the activation energy for the growth of Fe
Zn compound layer from ~ 167.1 kJ mol 1 (for the GC sample) to
~ 108.0 kJ mol 1 and enabled an increased diffusion of zinc. The en-
hanced nitriding, aluminizing, chromizing and zinc diffusion kinetics
Corresponding author at: Department of Dental Biomaterials, School of Dentistry,
Chonbuk National University, Jeonju 561-756, South Korea. Tel.: +82 632704042;
observed in these studies are due to the increased diffusion of the cor-
fax: +82 632704040. responding atoms along the numerous non-equilibrium grain bound-
E-mail address: tsnsn@rediffmail.com (T.S.N. Sankara Narayanan). aries generated by SMAT. Aluminizing, nitriding, chromizing and zinc

0257-8972/$ see front matter 2012 Elsevier B.V. All rights reserved.
http://dx.doi.org/10.1016/j.surfcoat.2012.10.051
222 T. Balusamy et al. / Surface & Coatings Technology 213 (2012) 221228

(a) (b)

(c) (d)

Fig. 1. Microstructure taken at the surface (ac) and cross section (d) of EN8 steel: (a) untreated; (b) after SMAT using 8 mm 316L SS balls for 45 min; (c) dark eld image of (b);
(d) deformed region after SMAT (dark eld image).

diffusion are relatively low temperature processes when compared to enables a decrease in the activation energy for the growth of borided
boronizing. Hence, materials subjected to SMAT could maintain their layer from 213.92 to 144.83 kJ mol1 and boronizing of H13 steel can
nanostructured surface layer. In addition, the increase in grain size is be achieved at 973 K for 8 h. Hence, it is imperative to conrm the bene-
rather limited to cause any signicant inuence on the diffusion ki- ts of using SMAT as a pretreatment for boronizing when the treatment is
netics. Lu et al. [27] have conrmed that the nanostructured surface performed at 11731273 K (usually employed for pack boronizing of
generated on H13 tool steel by SMAT could maintain its grain size many ferrous alloys). The present study aims to explore the same with
up to 873 K. The temperature employed for boronizing of most fer- the following issues: (i) whether surface nanocrystallization of steels by
rous alloys is 11731273 K for a few hours and it is very difcult to SMAT would be benecial when boronizing is performed at 1173 and
realize the benets of nanostructuring at such conditions. Studies on 1223 K; (ii) whether SMAT could help achieve boronizing of steels at
the effect of SMAT on boronizing of steel are rather limited. Xu et al. 923 K; (iii) the possible methodologies and conditions of boronizing so
[29] have studied the effect of SMAT on pack boronizing of AISI H13 that the benets of nanostructuring by SMAT could be realized and; (iv)
tool steel at 9731123 K for 1 to 8 h. According to them, SMAT limitations, if any.

160
Fe (110)

140
y = 15.279x + 32.229
Relative intensity

SMATed R 2 = 0.9963
120
Case depth ( m)

100 smatted
Fe (110)

y = 13.921x + 29.121
untreated R 2 = 0.9949
80

60
Untreated
40

43.0 43.5 44.0 44.5 45.0 45.5 46.0 20

0 2 4 6 8
Diffraction angle (2 ) Treatment time (h)

Fig. 2. XRD patterns of the Fe (110) plane of untreated EN8 steel and those subjected to Fig. 3. Variation in case depth (average layer thickness) of an EN8 steel pack boronized
SMAT using 8 mm 316L SS balls for 45 min. at 1173 K as a function of treatment time.
 T. Balusamy et al. / Surface & Coatings Technology 213 (2012) 221228 223

proles by using pseudo-Voigt function (XD-D1, Shimadzu, Japan with

(a) Cu K radiation). Untreated and SMAT treated EN8 steel samples having
a dimension of 1734 mm3 were packed along with a powder mixture
of boron carbide (5%), potassium tetrauoborate (5%) and silicon carbide
(90%) in an Inconel box and subjected to boronizing at various conditions
in a mufe furnace. The effect of SMAT on boronizing of EN8 steel was
studied using different experimental conditions. In the rst set of experi-
ments, the samples were packed along with the boronizing mixture and
placed inside the furnace maintained at 1173 K and the treatment was
performed for 17 h. In the second set of experiments, the samples
along with the boronizing mixture were placed inside the furnace at
1223 K to study the boron diffusion behaviour at austenitizing tempera-
ture. The third set of experiments; samples along with the boronizing
mixture were placed inside the furnace at ~303 K. Subsequently, the
temperature of the furnace was increased to 1173 K and the samples
were soaked at this temperature for 30 min. The fourth set of experi-
ments involves pack boronizing of EN8 steels at 923 K for 7 h. The
fth set of experiments involves a duplex treatment. In the rst stage,
the temperature was increased from 303 to 923 K and the samples
were soaked at 923 K for 30 min. Subsequently, in the second stage,
(b) the temperature was increased from 923 to 1173 K and the samples
were soaked at 1173 K for 30 min. In all these experiments, the rate
of heating was kept constant at 5 K/min. After thermal treatment at var-
ious temperatures and time duration, the boronized samples were
quenched in air for 5 h to 303 K. For microstructural analysis and
microhardness measurement, the boronized samples were embedded
in a phenolic resin mould, ground using successive grades of SiC coated
abrasive papers, polished using 3 m diamond paste, rinsed with deion-
ized water and dried. The microstructure and case depth of the
untreated and SMAT treated EN8 steel samples were assessed using a
Leica DMLM metallurgical microscope. Scanning electron microscopy
(SEM) was used to assess the uniformity and compactness of the coat-
ing. The microhardness of the boronized layer was measured using a
Leica VMHT (MOT) microhardness tester with a 50 gf load for 15 s.
The phase content of the boronized EN8 steel samples was identied
by X-ray diffraction measurement (XD-D1, Shimadzu, Japan with Cu
K radiation).

3. Results and discussion

3.1. Characteristics of SMAT treated EN8 steel

Temperature (K)

1223 K During SMAT, impingement of the SS balls on the surface of EN8

steel induces plastic deformation with a high strain rate during each im-
pact. The microstructures of untreated EN8 steel and those subjected to
Air Quenching
SMAT using 8 mm 316L SS balls for 45 min are shown in Fig. 1(a) and
(b), respectively. The contrast image (dark eld image) of the SMAT
treated sample surface (Fig. 1(c)) clearly reveals the formation of a
1h 5h 303 K large number of non-equilibrium grain boundaries. The optical micro-
graph (dark eld image) of SMAT treated EN8 steel taken at the cross
Time section (Fig. 1(d)) shows that the deformation depth is ~3540 m in
which heavy deformation is observed for ~30 m from the surface
Fig. 4. Optical micrographs taken at the cross section of an EN 8 steel pack boronized at
1223 K for 1 h: (a) untreated; and (b) after SMAT using 8 mm 316L SS balls for
while the extent of deformation is moderate/small for another ~5
45 min (the process sequence employed is shown in the scheme). 10 m. SMAT increased the average surface roughness of EN8 steel
from 0.21 0.039 m to 1.41 0.065 m. The increase in surface
roughness is due to the formation of craters and dimples following
2. Experimental details the impingement of the SS balls on the surface of EN8 steel. The XRD
patterns of the Fe (110) plane of untreated EN8 steel and those
EN8 steel (chemical composition (in wt.%): C: 0.04; Si: 0.20; Mn: 0.65; subjected to SMAT using 8 mm 316L SS balls for 45 min are shown
P: 0.026; S: 0.015; Cr: 0.01; Ni: 0.01; Fe: balance) discs having a dimen- in Fig. 2. Broadening of the Bragg diffraction peaks exhibited by SMATed
sion of 65 mm and 8 mm thickness were used as substrates. They samples is attributed to the reduction in crystallite size and increases in
were degreased using acetone and subjected to SMAT using 8 mm microstrain. The crystallite size calculated from the XRD data using a
316L stainless steel (SS) balls for 45 min. All experiments were performed pseudo-Voigt function is about 61 nm. The decrease in crystallite size
at a xed frequency of 50 Hz and under vacuum. The schematic and de- following SMAT is due to the progressive renement of coarse grains
tails of SMAT has already been described elsewhere [16,22]. The average to ner grains induced by the mechanical impact. The renement in
crystallite size was calculated from the broadening of Bragg diffraction grain size, increase in grain boundary area and dislocation density are
224 T. Balusamy et al. / Surface & Coatings Technology 213 (2012) 221228

(a) (c)

18 m I

(b) (d)

27 m

I
Temperature (K)

1173 K

Air Quenching

303 K 2.9 h 30 min 5h 303 K

Time

Fig. 5. Optical and scanning electron micrographs taken at the cross section of an EN8 steel pack boronized at 1173 K for 30 min: (a, c) untreated; and (b, d) after SMAT using 8 mm
316L SS balls for 45 min (the process sequence employed is shown in the scheme).

expected to promote the diffusion of boron. The ability of the nano- of boron at the austenitizing temperature, the second set of experi-
structures generated by SMAT to store a large excess energy in the ments were performed at 1223 K for 1 h. The optical micrographs of
grain boundaries as well as within each grain (non-equilibrium defects) untreated EN8 steel and SMATed samples after pack boronizing at
could provide the driving force for faster diffusion of boron atoms. 1223 K for 1 h are shown in Fig. 4. It is evident from Figs. 3 and 4
that SMAT enables an increase in case depth of borided layer. Howev-
3.2. Role of SMAT on boronizing of EN8 steel er, the extent of increase in case depth is rather limited. In the third
set of experiments, the samples along with the boronizing mixture
The effect of SMAT on boronizing of EN8 steel is studied using dif- were placed inside the furnace at ~ 303 K. Subsequently, the temper-
ferent experimental conditions. In the rst set of experiments, the ature of the furnace was increased to 1173 K and the samples were
samples were packed along with the boronizing mixture and placed soaked at this temperature for 30 min. The corresponding optical
inside the furnace maintained at 1173 K and the treatment was and scanning electron micrographs of these samples are shown in
performed for 17 h. The variation in case depth of untreated and Fig. 5. It is evident from Fig. 5(a) and (b) that compared to untreated
SMAT treated samples measured as a function of treatment time at steel, a moderate increase in case depth (from 18 to 27 m) is ob-
1173 K is shown in Fig. 3. In order to study the diffusion behaviour served after SMAT. The increase in case depth of the borided layer
 T. Balusamy et al. / Surface & Coatings Technology 213 (2012) 221228 225

(a) boride layers with a marginal increase in the kinetics of boron diffusion.
This is due to the temperature employed (1173 and 1223 K) for
boronizing, which would promote grain growth and the benecial effect
of surface nanocrystallization by SMAT could not be fully realized. Si et
al. [26] have demonstrated that SMAT can increase the case depth of alu-
minized layer from 2.40.5 (for coarse-grained sample) to 10.91.8 m
(surface nanocrystallized by SMAT) when the treatment was performed
at 773 K for 8 h. However, irrespective of an increase in case depth, the
ratio of the mean growth rate on SMAT treated to the coarse-grained
one is decreased by ~50% when the treatment was performed at 873 K
for 8 h. Similarly, severe plastic deformation of 9Cr1Mo (P92) alloy
steel by shot peening exhibits an improvement in the diffusion kinetics
of aluminide coatings only when the treatment was performed at temper-
atures below 948 K whereas further increase in temperature progressive-
ly diminishes the kinetics of the coating formation [30]. These inferences
lead to the question whether SMAT would enable an increase in kinetics
of boron diffusion at lower temperatures. In order to verify this phenom-
enon, additional experiments were performed.
The fourth set of experiment involves pack boronizing of EN8
steels at 923 K. At this temperature, the case depth of the borided
(b) layer becomes appreciable only after 7 h. The optical micrographs of
untreated EN8 steel and those subjected to SMAT using 8 mm
316L SS balls for 45 min after pack boronizing at 923 K for 7 h are
shown in Fig. 6. It is evident from Fig. 6 that SMAT has the ability to
promote the formation of a compact and uniform boride layer even
at 923 K whereas the layer formed on untreated EN8 steel lacks this
attribute. Xu et al. [29] have reported that SMAT of H13 steel enables
the formation of a borided layer when treated at 973 K for 8 h where-
as its untreated counterpart fails in this respect. The results of the
present study conrm that boronizing of EN8 steel can be performed
at temperatures as low as 923 K. However, to develop a reasonable
case depth of the boronized layer on SMAT treated EN8 steel at this
temperature, the treatment has to be performed for a long duration
and the ability of the material to maintain its nanostructure becomes
the key factor to achieve an improvement in the kinetics of boron dif-
fusion. Xu et al. [29] have reported that there is no signicant grain
growth of H13 steel and it can maintain the nanostructure at 973 K
for 30 min. However, 30 min is not sufcient to achieve a reasonably
good case depth for all types of steels when they are boronized at
923 K. Hence, the treatment conditions have to be suitably changed
and it calls for further modications.
The fth set of experiments involves a duplex treatment. In the rst
Temperature (K)

923 K stage, the temperature was increased from 303 K to 923 K and the sam-
ples were soaked at 923 K for 30 min. Subsequently, in the second
stage, the temperature was increased from 923 to 1173 K and the sam-
Air Quenching ples were soaked at 1173 K for 30 min followed by air quenching for
5 h. The optical micrographs of untreated EN8 steel and those subjected
to SMAT using 8 mm 316L SS balls for 45 min after pack boronizing
7h 5h 303 K by duplex treatment are shown in Fig. 7. It is evident that the duplex
treatment is effective in increasing the case depth and promoting the
Time formation of a uniform and compact layer on EN8 steel samples
subjected to SMAT. Boronizing of EN8 steel performed at 1173 K in a
Fig. 6. Optical micrographs taken at the cross section of an EN8 steel pack boronized at
single stage promotes grain growth before the effective formation of bo-
923 K for 7 h: (a) untreated; and (b) after SMAT using 8 mm 316L SS balls for
45 min (the process sequence employed is shown in the scheme). ride layers. Hence, the effectiveness of surface nanocrystallization by
SMAT could not be fully realized. In duplex treatment, the rst stage
treatment at 923 K for 30 min promotes the diffusivity of boron and en-
following SMAT observed in the present study is comparable with the ables the formation of iron boride layers since no signicant grain
results of Xu et al. [29]. Scanning electron micrographs show that the growth is expected at this condition [27] whereas the second stage
boronized layers formed on EN8 steel after SMAT appear to be compact treatment at 1173 K for 30 min promotes the kinetics of formation of
and uniform (region marked as I) than those formed over untreated iron borides. A similar trend has been observed earlier for chromizing
steel (Fig. 5(c) and (d)). The renement in grain size, increase in volume of SMAT treated low carbon steel by duplex treatment [31].
fraction of grain boundaries and, accumulation of high density of disloca- The XRD patterns of untreated EN8 steel and those subjected to
tions at the grain boundaries as well as in large grains are considered SMAT using 8 mm 316L SS balls for 45 min after pack boronizing
responsible for this behaviour. The results of the rst three sets of exper- at 1173 K for 30 min are shown in Fig. 8(a). It is evident that
iments of the present study reveal that SMAT of EN8 steel using 8 mm untreated EN8 steel exhibits the formation of an Fe2B phase only.
316L SS balls for 45 min enabled the formation of compact and uniform Conversely, samples subjected to SMAT exhibit the formation of
226 T. Balusamy et al. / Surface & Coatings Technology 213 (2012) 221228

(a)

(b)
Temperature (K)

1173K

923K Air Quenching

303K 2.06 h 30 min 0.83 h 30 min 5h 303 K

Time

Fig. 7. Optical micrographs taken at the cross section of an EN8 steel pack boronized by duplex treatment performed in two stages (923 K for 30 min and 1173 K for 30 min): (a) untreated; and
(b) after SMAT using 8 mm 316L SS balls for 45 min (the process sequence employed is shown in the scheme).

both Fe2B and FeB phases with Fe2B as the predominant phase. Kartal treatment time simultaneously promoted the growth of both Fe2B
et al. [14] have studied the phase homogenization in electrochemical and FeB phases. Dybkov et al. [32] have also observed a similar
boriding (PHEB) of steel. According to them, during PHEB of steel, the trend of increase in volume fraction of both Fe2B and FeB phases
top FeB layer serves as the source of boron and with increase in treat- with increase in treatment time during boriding of Fe25% Cr alloy
ment time the resultant coating consists of a single Fe2B phase. To at 1223 K. However, untreated EN8 steel exhibits the formation of
verify such an occurrence and to have a better understanding of the Fe2B phase only even after the treatment time is increased from
formation of an FeB phase, the treatment time is increased from 30 min to 3 h. Hence, the promotion of FeB phase in SMATed samples
30 min to 3 h. The XRD patterns of untreated EN8 steel and those could be attributed to the higher amount of boron accumulation near
subjected to SMAT using 8 mm 316L SS balls for 45 min after the surface due to a higher number of grain boundaries. The forma-
pack boronizing at 1173 K for 3 h are shown in Fig. 8(b). Increase in tion of FeB phases along with Fe2B phase after boriding for 30 min
 T. Balusamy et al. / Surface & Coatings Technology 213 (2012) 221228 227

(a) FeB
(a)
Fe 2B
Relative intensity

SMATed

Untreated

10 20 30 40 50 60 70 80 90 100
Diffraction angle (2)

(b) FeB
Fe 2B
(b)
Relative intensity

SMATed

Untreated

10 20 30 40 50 60 70 80 90 100
Diffraction angle (2)

Fig. 8. X-ray diffraction patterns of untreated and SMATed EN8 steels after pack
boronized at 1173 K for (a) 30 min; and (b) 3 h.

(Fig. 8(a)) and the increase in volume fraction of Fe2B and FeB phases
when the treatment time is increased from 30 min to 3 h (Fig. 8(b))
conrm the ability of SMAT to increase the kinetics of boron diffusion
on steel. The XRD pattern of the EN8 steel pack boronized by duplex 1800 (c) Untreated
treatment also resembles the pattern of the one treated at 1173 K for 1600 SMATed
30 min (shown in Fig. 8(a)). The optical micrographs showing the in-
Microhardness (VHN)50 gf

dentation marks formed on the EN8 steel after pack boronizing at 1400
1173 K for 2 h clearly show that they are relatively small on samples
subjected to SMAT (Fig. 9(a) and (b)). The hardness proles of the 1200
untreated and SMATed EN8 steels after boronizing exhibit a similar 1000
trend (Fig. 9(c)). However, the hardness values are relatively higher
for the SMATed samples. The ndings of this study indicate that 800
SMAT of EN8 steel helps to promote the diffusion of boron and the for-
600
mation of an FeB phase in addition to the Fe2B phase. It has been
established that among the iron boride phases, the FeB phase is very 400
hard and brittle and it may chip-off during service [33]. According to
the FeB phase diagram, the boron potential is the main factor for the 200
formation of an FeB phase than increase in temperature or treatment
10 20 30 40 50 60 70 80 90 100 110 120 130 140
time [1]. Hence, the concentration of free boron at the steel's surface
Distance from the surface (m)
dictates the type of iron boride phase. If the concentration of boron at
the exterior of the initially formed Fe2B layer is maintained at around Fig. 9. Optical micrographs taken at the cross section showing the indentation
9%, then the Fe2B phase continues to grow. On the other hand, if it marks (a and b) and hardness prole (c) of EN8 steel pack boronized at 1173 K
reaches approximately 16%, then FeB forms and grows on top of the for 2 h: (a) untreated; (b) after SMAT using 8 mm 316L SS balls for 45 min.
Fe2B layer resulting in a two-phase iron boride layer. Since SMAT pro-
motes the formation of an FeB phase, it is suggested that a decrease in
boron potential (concentration) would help to reduce the volume
228 T. Balusamy et al. / Surface & Coatings Technology 213 (2012) 221228

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encouragement and support.