VŠB - TECHNICAL UNIVERSITY OF OSTRAVA

FACULTY OF METALLURGY AND MATERIALS ENGINEERING

DEPARTMENT OF MATERIALS ENGINERING

Properties of 34CrMo4 steel before and

after cyclic loading

Author: Bc. Beini He

Supervisor: Prof. Ing. Eva Mazancová, CSc.

Ostrava 2017
 Acknowledgment

I would like to express my sincere gratitude to my supervisor Prof. Ing. Eva Mazancová,
for her patience, motivation, enthusiasm, and immense knowledge to help me through the
researching and writing processes of this master thesis.
This paper was partially created with the project No. L01203 “Regional Materials
Science and Technology Center - Feasibility program” founded by Ministry of Education
Youth and Sports of Czech Republic.
Abstract:
This presented diploma work describes the characteristics of 34CrMo4 material, and
the properties and microstructures before and after cyclic loading. The obtained results
from mechanical properties revealed an increasing of strength of the tested material after
cyclic loading. Detected fracture surface showed typical quasi-cleavage fracture. Directly
under surface of material the structure was ferritic, and that was changed to
ferritic-pearlitic, and then went over to martensite structure. The decarburization and
segregation were also observed under the surface.

Keywords: 34CrMo4 steel; cyclic loading; mechanical properties; microstructure

Abstrakt:
Prezentovaná diplomová práce popisuje charakteristiky materiálu 34CrMo4, jeho
vlastnosti a mikrostruktury před a po cyklickém zatěžování. Získané výsledky
mechanických vlastností odhalily po cyklickém zatěžování zvýšení pevnosti testovaného
materiálu. Detekovanálomováplocha vykazovala typickékvazi- štěpné porušení. Přímo
pod povrchem materiálu byla struktura feritická, ta se měnila na feriticko-perlitickou a pak
přešla do martensitické struktury. Pod povrchem bylo pozorováno oduhličení a segregační
pásy.

Klíčová slova: Ocel 34CrMo4; cyklické zatěžování; mechanické vlastnosti;

mikrostruktura
 Content
1. Introduction ...................................................................................................................... 3

2. Characterization of Material 34CrMo4 ............................................................................ 4

2.1 Standard chemical composition of 34CrMo4 ......................................................... 4

2.1.1 The influence of alloy elements in 34CrMo4 steel ...................................... 4

2.2 Physical properties .................................................................................................. 5

2.3 Heat treatment processes of 34CrMo4 steel ........................................................... 7

2.4 Mechanical properties of 34CrMo4 ........................................................................ 7

2.4.1 Tensile properties ......................................................................................... 7

2.4.2 Elongation .................................................................................................... 8

2.4.3 Hardness ...................................................................................................... 8

2.4.4 Impact toughness ......................................................................................... 8

2.4.5 Standard mechanical properties of 34CrMo4 .............................................. 9

2.5 Sulfide stress cracking corrosion (SSC) resistance of 34CrMo4 steel ................. 10

3. Mechanical properties and metallographic parameters of 34CrMo4 steel before and after
cyclic loading.......................................................................................................................11

3.1 Introduction of fatigue ...........................................................................................11

3.1.1 Fatigue processes ........................................................................................11

3.1.2 Fatigue propagation rate ............................................................................ 15

3.1.3 Fatigue crack propagation curve................................................................ 16

3.1.4 Fatigue testing ........................................................................................... 16

3.2 Fatigue in the presence of surface treatment of material 42CrMo4 ..................... 17

3.3 Fatigue testing of vessel ....................................................................................... 20

3.4 Experimental procedures ...................................................................................... 22

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 3.4.1 Materials of the experiment ....................................................................... 22

3.4.2 Specimens preparation............................................................................... 23

3.5 Technical methods and the standard used in the experiment ................................ 24

4. Results and their analysis ............................................................................................... 26

4.1 Chemical analysis ................................................................................................. 26

4.2 Mechanical properties before and after cyclic loading ......................................... 26

4.3 Analysis of purity and the result ........................................................................... 28

4.4 Micro-structure analysis ....................................................................................... 30

4.5 SEM analysis of fracture surface .......................................................................... 36

Conclusion .......................................................................................................................... 42

References .......................................................................................................................... 43

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 Properties of 34CrMo4 steel before and after cyclic
loading

1. Introduction

The 34CrMo4 steel is one of the representative medium carbon and low alloy steel. It
shows good mechanical properties, and it also has high durability and creep strength, good
balance of strength, toughness, and wear resistance in an extreme working environment.
Steel 34CrMo4 is typical one for high strength applications including some types of high
pressure steel cylinders [1]. Given material is also resistant against sour mediums and that
makes mentioned material more applicable for different possibilities. Desired mechanical
properties can be increased also by different variation of chemical composition, resp. by
addition of different elements as vanadium, titanium, niobium, representing microalloying
elements and/or by nitrogen being able to form different types of precipitates and being
also responsible for refinement and strengthening of basic matrix. Addition of
molybdenum leads to higher hardenability during heat treatment and in presence of
chromium this properties is yet much more intensive 2.
The fatigue behavior of the seamless gas cylinder tube is important during
manufacturing and using period, because the cyclic loading may cause initiation of
cleavage cracks, and it can lead to more serious problems like gas leakage or explosion.
So it’s very important to understand and analyses of this behavior. The aim of presented
diploma work is to analyze the properties of the 34CrMo4 after cyclic loading, and
compare the results with those reached before cyclic loading.

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2. Characterization of Material 34CrMo4

2.1 Standard chemical composition of 34CrMo4

Here in the Table 1 is the standard chemical composition of 34CrMo4 according to ČSN
EN 10083-3: 2007 standard. 34CrMo4 steel contains different alloy elements: C, Mn, Si,
Cr, Mo and so on, and those elements play different roles during the heat treatment.

Table 1 Standard chemical composition of 34CrMo4 (wt. % )

C Mn Si Cr Mo P S

0.30-0.37 0.50-0.80 ≦ 0.35 0.90-1.20 0.15-0.25 ≦ 0.040 ≦ 0.040

2.1.1 The influence of alloy elements in 34CrMo4 steel

Different alloy elements in steel play different roles, they can contribute to change the
material properties, here are the influence of different alloy elements in 34CrMo4 steel.
Carbon: On one side it increases the strength of the steel by the increasing carbon
content; on the other side, with the increasing carbon content, the structural stress will be
increased as well, and it can lead to the resistance of stress on the steel surface. Thus, the
tendency of quenching crack would be increased with the carbon content. The Carbon
comtent of 34CrMo4 is on the level of 0.30-0.37 wt. %, so the structural stress has not
considerable impact a lot.

Cromium: Cr is carbide former, can enhance the hardenability of the steel, and
decreases the critical cooling rate, and makes it quench-hardened in the oil. Cromium also
surpports temper brittleness.

Molybdenum: Mo can dramatically increase the hardenability of the steel, and also
decreases the critical cooling rate, makes it quench-hardened in the oil, which the coiling
capacity is low. The most outstanding characteristics of Mo are able to reduce temper

4
brittleness and to increase the temper resistance. Normally the percentage of Mo in steel is
0.2-0.3 % and it’s enough to reduce the temper brittleness.

Kinsman and Aaronson justified the experimentally detected reduction in ferrite growth
rate in molybdenum containing steels because molybdenum affects the thermodynamic
stability of austenite relative to ferrite. A better knowledge of the effects of molybdenum
on the evolution of the non-isothermal austenite decomposition could enhance the
production of as-forged acicular ferrite microstructures [3].

Molybdenum not only affects the transformation kinetics but also modifies the
morphology of the acicular ferrite.

Molybdenum favors the acicular ferrite formation but increases the amount of
martensite being present in the final microstructure. In Mo containing steel, the formation
of this phase is the main variable limiting the design of useful cooling cycles in order to
get microstructures with enhanced mechanical properties [4].

Manganese: Mn can increase the stability of austenite and also enhance the
hardenability of steel.

Silicumi: Si can also increase the hardenability of steel. But the surface of the
specimen can easily decarburize.

Above all, the 34CrMo4 steel shows small temper brittleness and good hardenability.
It’s enough for quench-hardening in oil [5].

2.2 Physical properties

The normal physical properties of 34CrMo4 are shown in Table 2.

The coefficient of thermal expansion describes how the size of an object changes with a
change in temperature. Specifically, it measures the fractional change in size per degree
change in temperature at a constant pressure [6].

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 Table 2 Standard chemical composition of 34CrMo4 (wt. % )

Mean coefficient of expansion

Density Transition Point:
in m/m °C

between between
Ac 1 Ac 3 Ms
20°C- 100°C 20°C - 700°C
7.8g/cm3

11.4 × 10-6 14.3 × 10-6 ~740 °C ~810°C ~350°C

Fig. 1 34CrMo4 steel tempering curve [7]

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2.3 Heat treatment processes of 34CrMo4 steel

According standard steel 34CrMo is annealed, quenched and tempered. Given steel can
be also forged. Possible heat treatments are described below:
-Annealing of 34CrMo4 Alloy structural steel

Heated is realized to 870 °C, allows enough times, let the steel to be thoroughly
heated, afterwards is cooled slowly in the furnace. The 34CrMo4 alloy steel will get max
250 HB.

-Hardening of DIN Alloy structural steel 34CrMo4

First quenching heated slowly to 880°C, then after adequate soaking at this temperature
quench in oil or water. Tempering follows after tools reach room temperature. Second
quenching heat corresponds to 780-820°C，then quenching in oil or water follows. Next
operation is tempering of 34CrMo4 Alloy described as it follows:

Material is heated to 205-649 °C, afterwards cooled in water or oil. Normal delivery
hardness corresponds to 18-22 HRC. Forging of Alloy Steel 34CrMo4 corresponds to 926
to 1205 °C (1700 to 2200°F) in accord with DIN 34CrMo4 alloy. Fig. 1 depicts 34CrMo4
steel tempering curve [8].

2.4 Mechanical properties of 34CrMo4

2.4.1 Tensile properties

·Yield point.

In case the stress is too large, the strain deviates from being proportional to the stress.
The point at which this happens is the yield point because there the material yields,
deforming permanently (plastically).

·Yield stress.

Hooke's law is not valid beyond the yield point. The stress at the yield point is called
yield stress, and is an important measure of the mechanical properties of materials. In
practice, the yield stress is chosen as that causing a permanent strain of 0.002. The yield
7
stress measures the resistance to plastic deformation. The reason for plastic deformation,
in normal materials, is not that the atomic bond is stretched beyond repair, but the motion
of dislocations, which involves breaking and reforming bonds. Plastic deformation is
caused by the motion of dislocations.

·Tensile strength.

When stress continues in the plastic regime, the stress-strain passes through a maximum,
called the tensile strength (σTS), and then falls as the material starts to develop a neck and
it finally breaks at the fracture point.

2.4.2 Elongation

Elongation at break, also known as fracture strain, is the ratio between changed length
and initial length after breakage of the test specimen. It expresses the capability of a
material to resist changes of shape without crack formation. The elongation at break is
determined by tensile testing in accordance with EN ISO 527.

2.4.3 Hardness

Hardness is the mechanical resistance which a material asserts against the mechanical
penetration of a harder test body. The definition of hardness differs from strength, which
represents the resistance of a material to deformation. Hardness is also a measure of the
abrasion properties of materials. Harder materials generally demonstrate better abrasion
behaviour than others [9].

2.4.4 Impact toughness

The impact strength describes the ability of a material to absorb shock and impact
energy without breaking. The impact strength is calculated as the ratio of impact
absorption to test specimen cross-section. Toughness is dependent upon temperature and
the shape of the test specimen.

Two different methods of determining impact strength may be used here. Unlike impact
strength, notch impact strength is determined using a notched test specimen, which
increases the sensitivity of the test method.
8
 One of the most popular impact tests is the Charpy Test, schematically presented in the
Fig. 2 below. The hammer striking energy in the Charpy test is 220 ft*lbf (300 J). And the
diameters of the specimen are 5mm×10mm×55mm [10].

(a)

(b)

Fig. 2 Specimen diameters of Charpy Test (a), Charpy test processes (b) [11]

2.4.5 Standard mechanical properties of 34CrMo4

In Table 3 is the standard mechanical properties of 34CrMo4 in different size according

to ČSN EN 10083-3: 2007 standard.

9
 Table 3 Standard for mechanical properties of 34CrMo4 [12]

2.5 Sulfide stress cracking corrosion (SSC) resistance of 34CrMo4 steel

Steel 34CrMo4 has higher carbon content and also presence of some other segregated
elements, after primary material production and especially after reverse extrusion and
broaching microstructure shows strong segregation banding that is detrimental for the SSC
resistance representing ideal located trapping position on the interphase of matrix and
segregation band.
There are two ways for steel 34CrMo4 achieving the high SSC resistance. First way is
to ensure the homogeneous dispersion of very fine inclusions and precipitates as the
uniform hydrogen traps. And the second way is to reduce the inclusions presence to its
minimal possible levels and to refine the grain-size by the more aggressive forming
process to create conditions of maximal redistribution of hydrogen ions and/or atoms on
numerous grain boundaries and dislocations [13].

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3. Mechanical properties and metallographic parameters of 34CrMo4

steel before and after cyclic loading

3.1 Introduction of fatigue

3.1.1 Fatigue processes

Fatigue is an important potential cause of mechanical failure, as most engineering

components or structures are or can be subjected to varying loads during their lifetime.
Fatigue failure of engineering components and structures results from progressive
fracture caused by cyclic or fluctuating loads. The magnitude of each individual load event
is too small to cause complete fracture of the undamaged component, but the cumulative
action of numerous load cycles, often numbering in the hundreds of thousands and
millions, results in initiation and gradual propagation of a crack or cracks. Complete
fracture ensues when the crack reaches critical size. Fatigue fractures are caused by the
simultaneous action of cyclic stress, tensile stress, and plastic strain. If any one of these
three is not present, fatigue cracks will not initiate and propagate. The cyclic stress and
strain starts the crack; the tensile stress produces crack growth (propagation).

Fig. 3 Schematic showing test parameters for cyclic-stress testing

The test parameters for cyclic stress test are shown in Fig. 3. Here are several important
parameters of loading stress:
Sr : the range of stress. Sr = Smax - Smin

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 Sa : the stress amplitude, which means one half of the range stress. Sa = (Smax - Smin) / 2

Sm: the mean stress, is the algebraic average of the maximun and minimun stress in
cycle. Sm = (Smax + Smin) / 2

R : ratio of the minimum stress to the maximum stress. R = Smax / Smin

A : ratio of the alternating stress amplitude to the mean stress. A = Sa / Sm

If the applied ratio is fully reserved, that is Smax = - Smin, and R = -1. That condition is
normally considered the reference fatigue testing condition [14].

Many service failures still occur by fatigue, despite the well-defined characterization of
fatigue properties in the laboratory. In part, the difficulty is that fatigue behavior is
influenced by a great number of variables such as the magnitude and frequency of
application of the fluctuating stress, the presence of a mean stress, temperature,
environment, specimen size and shape, the presence of residual stresses, stress
concentration, surface condition, and material imperfections or discontinuities. These
factors complicate laboratory simulation of actual application conditions. The problem of
fatigue, as a progressive form of damage, also can be sensitive to small imperfections or
variations that accumulate into a critical form. Thus, due to its complex and varied
conditions, prevention of fatigue failure requires education and awareness in all stages in
the life of a part from design and manufacturing to anticipated service, operation
inspection, and maintenance.

The crack propagates under the applied stress through the material until complete
fracture results. On the microscopic scale, the most important feature of the fatigue
process is the nucleation of one or more cracks under the influence of reversed stresses
that exceed the flow stress, followed by the development of cracks at persistent slip bands
or at grain boundaries. Subsequently, fatigue cracks propagate by a series of opening and
closing motions at the tip of the crack that produce, within the grains, striations that are
parallel to the crack front.

The process of fatigue consists of three stages:

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·Stage I: Initial fatigue damage leading to crack nucleation and crack initiation

·Stage II: Progressive cyclic growth of a crack (crack propagation) until the remaining
uncracked cross section of a part becomes too weak to sustain the loads imposed

·Stage III: Final, sudden fracture of the remaining cross section

As illustrated in Fig. 4, fatigue failures have one or more fatigue origins (initiation sites),
a region of progressive fatigue crack propagation, and a final fast overload fracture zone.
Identification of the location and nature of origin sites is important in failure analysis of
fatigue, as fatigue crack initiation is frequently the life-controlling step in the failure
process. Discontinuities introduced during processing or manufacture (e.g., abnormally
large inclusions, weld discontinuities, grinding cracks) or service (e.g., corrosion pits,
impact damage) can result in fatigue crack initiation under circumstances where an
unflawed component would have had acceptable fatigue life. Conversely, inadequate
design, excessive load, or low material strength in fatigue can result in fatigue failure in
the absence of a particular “defect” at the origin site. Fractography provides the basis for
identifying the fatigue fracture mode and for locating origin sites from examination of
fracture surfaces.

Fig. 4 General features of fatigue fractures [15]

Fatigue crack propagation has been historically divided into two parts, designated stage
I and stage II. Stage I propagation occurs on specific crystallographic planes with greatest

13
resolved fluctuating shear stress. Stage II propagation occurs on planes normal to the
fluctuating tensile stress.

The stage I propagation mechanism is favored in materials that exhibit planar slip and in
some alloys strengthened by coherent precipitates (such as age hardened aluminum) and
under fluctuating loads low enough that the cyclic fracture process zone is small relative to
a characteristic microstructural scale parameter. Hence, stage I propagation is often
favored by large grain size. Stage II propagation is favored in materials with easy
cross-slip (wavy slip). In this article, fatigue propagation appearance is described in terms
of morphology rather than the didactic separation into stages I and II.

Final fracture occurs when the crack has grown to the critical size for overload failure.
The size of the final-fracture zone depends on the magnitude of the loads, and its shape
depends on the shape, size, and direction of loading of the fractured part. The
final-fracture zone of a fatigue-fracture surface is often fibrous, resembling the fracture
surfaces of impact or fracture-toughness test specimens of the same material.

Two features of the final-fracture zone aid in determining the origin of fracture. First,
fatigue usually originates at the surface, and therefore the fatigue origin is not included in
the shear-lip zones of the overload region. In tough materials, with thick or round sections,
the final-fracture zone will consist of a fracture by two distinct modes: (a) tensile fracture
(plane-strain mode) extending from the fatigue zone and in the same plane; and (b) shear
fracture (plane-stress mode) at 45°to the surface of the part bordering the tensile fracture.
In thin sheet-metal pieces having sufficient toughness, final fracture occurs somewhat
differently. The second characteristic of a fast-fracture zone is chevron marks that point
back to the origin of fracture [15].

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 Fig. 5 Fracture planes that are 45°to the direction of loading.

(a) Single-shear plane. (b)Double-shear plane [15]

3.1.2 Fatigue propagation rate

The fatigue crack propagation rate is defined as an increased crack length a in the
direction of the crack propagation during one loading cycle. Generally, the crack
propagation rate can be varied within a board interval. The highest crack rate can be
observed just before the fracture.
A typical crack growth in a cracked body under load amplitude cycling is shown in Fig.
6. If the applied cyclic loading is constant, the growth of crack is always an accelerating
process. The crack length increases rapidly with the increasing number of loading cycles.

Fig. 6 Increase of fatigue length with the creasing of loading cycles 14
15
3.1.3 Fatigue crack propagation curve

The fatigue crack growth is mostly depended on the fatigue growth rate on the crack tip
and intensity factor amplitude Ka. This dependence is called fatigue crack propagation
curve. It can be considered as a material characteristic, since it depends on the stress
intensity parameters and it is not affected by geometrical parameters.
A schematic illustration of fatigue crack propagation curve is shown in Fig. 7. In the
middle part of the curve, the dependence can be seen as a straight line. This part is often
called the Price range on the crack growth curve, because Paris and Erdogan for the first
time came up with the relationship between the stress intensity factor and fatigue crack
growth rate.

Fig. 7 crack propagation curve [14]

The middle part of the curve can be described in the form:

da / dN = CKac [m.cycle-1] (1)

where C and c are material constants.

3.1.4 Fatigue testing

One important parameter in fatigue testing is the relationship between the amplitude of
stress and the cycles to failure. The basis of the Stress-Life method is the Wöhler S-N

16
diagram, shown in Fig. 8. The S-N diagram plots nominal stress amplitude S versus cycles
to failure N. There are numerous testing procedures to generate the required data for a
proper S-N diagram. S-N test data are usually displayed on a log-log plot, with the actual
S-N line representing the mean of the data from several tests.

Fig.8 Scheme of a S-N fatigue response [14]

Each material has its fatigue limit or endurance limit which represents a stress level (Sf)
below which the material does not fail and can be cycled infinitely. If the applied stress
level is below the endurance limit of the material, the structure is said to have an infinite
life. If the number of cycles to failure is 105 or above, it will be defined as high-cycle
fatigue, if the number of cycles to failure is 104 or less, it will be low-cycle fatigue.

3.2 Fatigue in the presence of surface treatment of material 42CrMo4

Material 42CrMo4 and 34CrMo4 have practically the same chemical composition, only
the carbon content of 42CrMo4 is 0.42 % while the 34CrMo4 shows about 0.34 %.
Therefore, these two materials have almost the same properties and structures. Here are
the mechanical and fatigue data in different surface treatment environments of 42CrMo4,
which would be similar in material 34CrMo4.

17
 Generally, fatigue properties are very sensitive to surface conditions. The surface
treatment can change the characteristics of the material therefore it will greatly influence
the fatigue properties.
It is not possible to predict quantitatively the fatigue limit of hardened steel specimen, it
depends on a lot of factors, such as the methods of stressing, the hardness of the surface,
the magnitude of the induced compressive residual stresses, the ratio of the case depth to
specimen diameter. Four different surface treatment of 42CrMo4 could be considered as
follows: a) plasma nitriding , b) gas nitriding, c) gas nitrocarburizing and d) plasma
nitrocarburizing – see Fig. 9 number 9, 10, 11 and 12 being mentioned in consequence..
The microhardness results vs. depth profiles on the cross-sections are shown in Fig. 9. It
shows that the treatment in plasma resulted in a slightly lower hardness with respect to the
gas environment.

Fig. 9 Microhardness profiles for 4 different surface treatments 14]

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 Fig. 10 Fatigue data and S-N curve. a) plasma nitriding and gas nitriding, b) plasma
nitrocarburizing and gas nitrocarburizing 14

In Fig. 10 are summarized data about fatigue and S-N curves for nitroburizing and
nitriding in plasma and gas environment which were shown by Bokůvka et al in work [14,
where number 8 represents material after quenching and tempering and the other numbers
are the same like those were described in frame of Fig. 10. It is shown that the highest
increments in the fatigue performance are obtained with the nitriding treatments although
ferritic nitrocarburizing also brings a significant increase in the fatigue resistance. For the
surface treatment in gas environment, still allows the highest increment among the

19
treatments. The S-N curves of the surface treatment materials are also observed to flatten
out very gradually to a fatigue limit when compared to the untreated material.

3.3 Fatigue testing of vessel

For the testing of numbers of cycles, the acoustic emission sensor is R15I (PAC) with
the resonance frequency of 150 kHz and cable of RG58A/U (10m) is put on the middle of
shell using the vacuum grease.

The detected AE signal is put into the DiSP-52 Acoustic emission workstation (PAC)
for processing. In addition, the water was used as medium for burst test. The threshold
value of test was set at 45dB. The source of simulated sound was the destruction of the 2H
Pentel pencil lead. The average sensitivity of sensor was 98dB within 1 inch from sensor.

Fig. 11 Testing method of number of cyclic loading 16]

The burst pressure was estimated to be 600 bar under the pressured conditions. By
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raising the pressure to 30 %, 50 %, 60 %, 70 %, 80 % and 90 % of estimated burst
pressure and keeping each pressure stage for 10 minutes as in Fig. 11(a), we acquired the
AE signal from each stage. As can be seen in the figure, pressure was put on the vessel
with a pump to control the pressure and acoustic emission signals were detected using
acoustic emission sensors attached to the vessel. And the signal were processed and
analyzed after fed into AE equipment. The fatigue test repeated 20000 cycles between 0
and 207 bar, afterwards which has a used pressure of 0 and afterwards, the pressure was
continuously increased and the burst test was carried out. Fig. 11(b) shows the conditions
for pressurization [16].

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3.4 Experimental procedures

3.4.1 Materials of the experiment

Two samples of 34CrMo4 steel were supplied. Those were described as A and B and
both are depicted in Fig. 12 (A1, A2, B1 and B2), where cracks in bottom of vessel can be
observed. A1 , A2 represent the inter surface and outer surface of sample A. The B1 , B2 is
the inter surface and outer surface of sample B. Material A was after final production
while the material B was after final production and after cycling. Realized cycles
corresponded to 29472 and 31945 cycles when cracks were detected.

A1 A2

B1 B2

Fig. 12 Two samples of fatigue fracture of 34CrMo4 steel.

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3.4.2 Specimens preparation

The two samples in Fig. 13 were cut to 7 parts for the observation of macro and micro
structure.

Sample A (without crack):

Point 1 : Traverse direction ATD

Point 2 : Longitudinal direction ALD

Sample B (with crack):

Point 3: Initiation of crack in transverse direction BTD

Point 4: Initiation of crack in longitudinal direction BLD

Point 5: Longitudinal direction of deformation B3

Point 6: Center of crack B4

SEM: Micro observation of fracture surface by scanning electron microscope

23
 B

Fig. 13 Two samples of 34CrMo4 steel with fracture

3.5 Technical methods and the standard used in the experiment

Chemical analysis was carried out using a Thermo ARL 3460 optical emission
analyzer according to ASTM E 415-08 standard. For macro observations a Leica M125
stereo microscope was used.

Metallographic analyses were performed using light optical microscope (LOM) and
scanning electron microscope (SEM). Metallographic specimens were taken from each
fragment to examine bulk material and fracture surface. The cutting was performed by a
precision saw (Buehler Isomet 4000). Specimens were mounted in an automatic mounting
press (Buehler Simplimet 1000) and carefully grinded by grand machine with grit papers
from 120×,240× to 1200×, then using an automatic grinder–polisher system (Buehler
Phoenix Beta) , finished by diamond polishing down to 1 lm. Afterwards, polished areas
were etched with a ferric chloride aqueous solution, according to ASTM E 407-07
standard [17] and examined first under a Nikon Eclipse ME600 optical microscope. Some
samples were examined in un-etched conditions too. Then, SEM analysis was carried out
with a Fegsem Zeiss Ultra Plus instrument.

Destructive tensile tests and KV Charpy tests were conducted on specimens machined
from both the fractured and non-fractured steel, and the Charpy test was applied from

24
transverse direction. Specimens from the exploded cylinder were cut away from the
fractures. Tensile tests were carried out in a W+B 60 ton capacity test machine, at room
temperature, according to EN ISO 6892-1 standard; hardness tests were carried out on a
Wolpert durometer according to HBW-EN ISO 06506-1 standard and Charpy tests were
performed using a 300 J impact test machine Zwick/Roll according to ISO 148-1, cyclic
loading were tested according to standard ISO 9809-1-2010.

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4. Results and their analysis

4.1 Chemical analysis

The results of chemical analysis, reported in Table 4, are in full agreement with the
nominal chemical composition fixed by the standard in force when the supplied materials
were built [1]. Moreover, no significant differences between the standard and test material
have been found.

Table 4 Chemical composition of tested 34CrMo4 steel

C Mn Si Cr Mo P S Ni

0.38 0.71 0.33 1.12 0.233 0.009 0.004 0.024

Cu Sn Al H(in ppm)

0.013 0.001 0.030 1600

4.2 Mechanical properties before and after cyclic loading

The results of tensile tests, KV Charpy tests, and fatigue tests results are reported in
Table 5 and Table 6. Results of specimen 1 and 2 represent are the results of material
before cyclic loading, for specimen 3, 4 and 5 are the results of tested vessel after cyclic
loading.

Table 5 Mechanical properties of tested 34CrMo4 steel before cyclic loading

Specimen 1 (2007/03) 1(Ø) 2 (2007/03) 2(Ø) Ø

Rm(MPa) 1021 1021 1023 1023 1022

26
 Re(MPa) 957 957 956 956 956.5

A(%) 15.6 15.6 16.4 16.4 16

KCV(J/cm2) 76/71/71 73 76/80/71 76 74.5

Destroy(bar) 584 584 578 578 581

Table 6 Mechanical properties of tested 34CrMo4 steel after cyclic loading

Specime 5
3 (2017/2) 3(Ø) 4 (2017/2) 4(Ø) 5(Ø) Ø
n (2017/2)

Rm
1070/1059/1054 1061 1064/1075/1075 1071 1064 1064 1065
(MPa)

Re(MPa) 998/973/968 980 973/998/1003 991 947 947 972

A(%) 16.4/21.2/17.6 18.4 22.1/17.6/17.2 19.0 15.6 15.6 17.7

KCV
69/78/73 73 72/72/74 73 72/70/76 73 73
2
(J/cm )

Cycles 29472 29472 31945 31945 31945 31945 31121

After cycling, loading of tested material was without damage in range from 29 472 to
31 945 cycles, resp. 31 121 cycles on average.

After cyclic loading, the average value of strength and elongation of the material has

27
slightly increased. The KCV properties are almost the same before and after cyclic loading.
The increasing of strength after cyclic loading accompany with the loss of ductility.

The tensile strength Rm has increased by 4.2 %, the yield strength Re has increased by
1.6 %, the elongation has increased by 10.6 %. The cyclic loading has small impact on
KVC results.

4.3 Analysis of purity and the result

After the preparation of 6 specimens, using the grand machine with sandpaper from
120×, 240× to 1200×，and then use the polish machine polish the specimen until the
surface looks like a mirror. After polishing, it’s available to use the optical microscope to
observe the purity of supplied material under the surfaces positions and in central areas
Level of purity in all cut of material was practically the same.

ALD ATD
D 0.5 ------

a b

BLD BTD
D 1.5 D 1.5

c d
28
 B3 B4
D1 D 0.5

e f

BTD

Fig. 14 a-f Light microscopy – Image of observed inclusions and defects - 6 samples
which are polished but unetched showing the oxide inclusions. The BTD represents
situation close the crack and the ALD outside of crack

There are several black “points” on the surface of each specimen. Based on the standard:
ČSN ISO 4967, the black “points” represent oxide inclusions, showing typical globular
form in shape [18, 19].
The grade of purity is part of each presented figure as it Fig. 14(a-f) shows. The grade
was from D 0 to D 1.5. The best purity was detected in case of sample ATD and the worse
was in sample BLD and BTD, which are closer to the fracture area.
Observation area near the general crack as it Fig. 14(g) demonstrates, resp. sample BTD
shows. It demonstrates general crack with the small normal cracks in the end of the

29
general crack. It was not possible to detect the crack propagation directly from the figure.

4.4 Micro-structure analysis

Here are the results from light optical microscope analysis after etching of samples.

Sample - ATD:

a b 50µm

500µm 100µm

c d

500µm 100µm

100µm

Fig. 15 a. Decarburization of the internal surface; b. detail of decarburization;

c. represents segregation in center; d. is detail of segregation; e. detail of oxidation.

30
 Fig. 15(a-e) represents microstructure of the inner surface of the vessel. Normally, there
is no access of the quenching medium to the internal surface, this causes the internal
surface and the area which is slightly under the internal surface traps the gases for longer
time than outer surface during the heating, but the cooling rate is lower than the outer
surface during the quenching. This results in more noticeable segregation banding in the
under inner surface area, and also leads to the decarburization under the inner surface [20].

The Fig. 15(a-b) shows the decarburization area under the internal surface, which is
much brighter than the outer area. Fig. 15(b) shows the detail of decarburization area, the
depth was about 50 µm under the internal surface.

The structure directly under the surface was ferritic, and that was changed to
ferritic-pearlitic, and it was going to martensite or bainite structure, respectively to the
structure of the studied vessel.

In material could be also seen segregation bands as Fig. 15(a) and Fig. 15(c) in detail
show. The microstructure of vessel is martensitic structure, as it can be seen in Fig. 15(d),

in which also 2 sulfides can be observed being approximately 45 µm in length. In Fig.

15(e) an oxide can be also seen.

Microhardness analysis of sample ATD

Fig. 16 demonstrates results of microhardness of sanple ATD in decarburizatin area.

Eleven points were chosen from the cross section of the studied vessel as showed in Fig.
15 (a), from the internal surface to the outer area in each 0.05 mm, the total depth was 0.5
mm under the surface decarburization area.

31
 Fig. 16 Microhardness results of sample ATD

The level of measured microhardness was between 279-376 HV0.2, the average value
corresponded to 337 HV0.2. The value of microhardness in carburized area is slightly
higher than the decarburized area just under the crack surface.

Sample - ALD:

a b c

500µm 100µm 100µm

Fig. 17. a. decarburization ; b. segregation in center;

c. detail of segregation

In Fig. 17microstructure of internal surface is seen where again the decarburization can
be observed in Fig. 17(a). The maximum decarburization depth corresponded to 160 µm,
and minimum depth was 100 µm. In Fig. 17(b) and Fig. 17(c), basic martensitic structure
can be seen as well as the segregation bandings as Fig. 17(c) clearly represents.

32
Sample - BLD:

a b

500µm 100µm

Fig. 18 a. fine segregation; b. general structure

Sample BLD Fig. 8(a) and Fig. 18(b) was taken off in vicinity of crack, and
microstructure shows slight segregation and microsructure is again martensitic one. In
vicinity of crack, none important changes in microstructure were observed.

Sample - B3:

a b

500µm 100µm

Fig. 19 a. decarburization of the internal surface;

b. detail of decarburization

33
 Sample B3 was cut from the longitudinal direction of fracture deformation and from
outside of the crack. The similar microstructure was mentioned above. The maximum
decarburization depth corresponded to 200 µm, and minimum depth was 100 µm showed
in Fig. 19(a).

Sample - B4:

a b

500µm 100µm

c d

50µm 50µm

Fig.20 a. structure around crack; b. detail of the structure

c. structure around crack I; d. structure around crack II

Sample B4 wat cut from the central area of crack but out of crack. It also can be seen
the microstructure outside of general crack, and the microstructure can be defined as
martensitic structure with thin segregation bands and also with numerals carbides being
observed especially in Fig. 20(a) and (d). Microstructure here looks even without
anomalies.
34
Sample - BTD：

a b

500µm 100µm

c e d

100µm 100µm 100µm

Fig. 21 a. Shape of crack; b. details of crack;

c. structure around crack; d. structure out of crack

Fig. 21(a-d) shows the microstructure close the general crack. Fig. 21(a) represents the
ending of crack, Fig. 21(b) shows the detail of initiation of crack, Fig. 21(c) and Fig. 21(d)
represent the microstructure in detail.
In vicinity of crack plastic deformation was observed, the gain size close to the crack
edge is finer than the others. The crack was partially propagated intergranularly or
intragranularly.

The presented general crack is branched into finer cracks as it Fig. 21(a) demonstrates
and general crack is approximately 500 µm in length in initiation state, and in the end is
the secondary crack about other 500 µm in length.

35
 a b

Fig. 22 SEM analysis of: a. crack view; b. microstruction around crack;

c. detail of crack ending

Especially, in Fig. 22(a) and Fig. 22(c) was used SEM analysis. Some inclusions in the
end of crack were observed and it can be seen the crack was also propagated through the
inclusions.

In detail it can be seen the microstructure in etched state in Fig. 22 (c). Microstructure
in close vicinity is again martensitic structure with numerals carbides.

4.5 SEM analysis of fracture surface

Fracture surface of studied material after cyclic loading Fig. 23 depicts. From this
figure can be seen initiation from the internal surface of vessel and as well as propagation
of fatigue crack to its outdoor surface. In details, fracture surface is presented in Fig. 24,

36
which was observed from the top to the bottom, which is parallel to the direction of crack
growth. Test samples exhibited typical characteristic of fatigue fracture propagation.

Fig. 23 Studied fracture surface

Crack growth direction

37
 b

Fig. 24 a.crack surface view-beginning (internal surfacre) b.crack surface

view-middle c.crack surface view-eding (outer surface)

In Fig. 24 the typical quasi-cleavage fracture surface was observed, which is a fracture
mode that combines the characteristics of cleavage fracture and dimpled rupture fracture
[21]. Quasi-cleavage occurs where the crack initiates (the stresses are highest), and the
fracture changes to intergranular as the crack grows and relieves e.g. the hydrogen
pressure. For further observation, 10 points (see red marking in Fig. 24) were chosen from
the top to the bottom of the fracture surface to observe under higher magnification.

38
0 1

2 3

4 5

6 7

39
 8 9

10

Fig. 25(1-10) SEM analysis of fracture surface under greater magnification

The SEM images with higher magnification of the specimen revealing the topography
of the fracture surface in different zones of crack growth are shown in Fig. 25. The Fig.
25(1-3) shows the initiation part of the crack, the surface was seen as quasi-cleavage
fracture. Several pores - holes in Fig. 25 (3) can be observed which may correspond to
oxides or inclusions generally.

In Fig. 25 (5) more pores/holes can be observed, that might because it was the crack
propagation area, the crack propagated radially from the pores and was dominated by a
transgranular mode of cracking [22].

In Fig. 25 (6) and (7), the fracture topography was mainly characterized by typical
fatigue striations and secondary cracks, and also the segregation bands. Fig. 25 (8) and (9)
show the same fracture as mentioned above, in addition a significant crack can be
observed in Fig. 25 (8), and also two small cracks can be seen in Fig. 25(9). It would be
the further crack propagation to the outer surface.
40
 Fig. 25 (10) shows a total different structure compared to other figures. It represents the
ending of the crack in the cross section near the outer surface of the tested vessel.

41
Conclusion

This paper summarizes the character of 34CrMo4 alloy steel, and analysis of the results
of mechanical properties, metallographic and fractographic observations of 34CrMo4
material before and after cyclic loading.
- The 34CrMo4 steel is one of the representative medium carbon and low alloy steel. It
shows good mechanical properties, and it also has high durability and creep strength, good
balance of strength, toughness, and wear resistance in an extreme working environment.
- The average value of strength properties of the material has slightly increased after
cyclic loading. The tensile strength Rm has increased by 4.2 %, the yield strength Re has
increased by 1.6 % and the elongation was by 10.6 % higher. The cyclic loading had small
impact in KVC results. After cycling KCV values showed fall by 1.5 J.cm-2 representing
insignificant decrease on average, even when individual difference of maximal and
minimal value before and after cycling amounted to 11 J.cm-2.
- Decarburization can be observed under the internal surface after cyclic loading. The
structure directly under the surface was ferritic, and that was changed to ferritic-pearlitic,
and it was going over to martensite structure, respectively to the structure of the studied
vessel.

- The microstructure of fracture surface revealed typical quasi-cleavage fracture, and

also the fatigue striations and segregation bands can be observed under SEM analysis.

42
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