metals

Article
Fatigue Crack Growth Behavior of Austempered AISI
4140 Steel with Dissolved Hydrogen
Varun Ramasagara Nagarajan 1 , Susil K. Putatunda 1, * and James Boileau 2
1 Department of Chemical Engineering and Materials Science, Wayne State University, Detroit, MI 48202, USA;
varunblr83@yahoo.com
2 Research and Innovation Center, Ford Motor Company, Dearborn, MI 48121, USA; jboileau@ford.com
* Correspondence: sputa@eng.wayne.edu, Tel.: +1-313-577-3808

Received: 16 August 2017; Accepted: 24 October 2017; Published: 1 November 2017

Abstract: The focus of this investigation was to examine the influence of dissolved hydrogen on the
fatigue crack growth behavior of an austempered low-alloy AISI 4140 steel. The investigation also
examined the influence of dissolved hydrogen on the fatigue threshold in this material. The material
was tested in two conditions, as-received (cold rolled and annealed) and austempered (austenitized
at 882 ◦ C for 1 h and austempered at 332 ◦ C for 1 h). The microstructure of the annealed specimens
consisted of a mix of ferrite and fine pearlite; the microstructure of the austempered specimens was
lower bainite. Tensile and Compact Tension specimens were prepared. To examine the influence
of dissolved hydrogen, two subsets of the CT specimens were charged with hydrogen for three
different time periods between 150 and 250 h. All of the CT samples were then subjected to fatigue
crack growth tests in the threshold and linear regions at room temperature. The test results indicate
that austempering resulted in significant improvement in the yield and tensile strength as well as
the fracture toughness of the material. The test results also show that, in the absence of dissolved
hydrogen, the crack growth rate in the threshold and linear regions was lower in austempered samples
compared to the as-received (annealed) samples. The fatigue threshold was also slightly greater in
the austempered samples. In presence of dissolved hydrogen, the crack growth rate was dependent
√
upon the ∆K value. In the low ∆K region (<30 MPa m), the presence of dissolved hydrogen caused
the crack growth rate to be higher in the austempered samples as compared to annealed samples.
Above this value, the crack growth rate was increasingly greater in the annealed specimens when
compared to the austempered specimens in presence of dissolved hydrogen. It is concluded that
austempering of 4140 steel appears to provide a processing route by which the strength, hardness,
and fracture toughness of the material can be increased with little or no degradation in the ductility
and fatigue crack growth behavior.

Keywords: fatigue crack growth rate; dissolved hydrogen; fracture toughness; austempering

1. Introduction
In recent years, there has been significant interest in austempering [1–5] as an alternative heat
treatment process relative to traditional quenching and tempering processes. Austempering involves
austentizing the steel in the fully austenitic region (above the A1 temperature) followed by a rapid
cooling into the bainitic temperature region. The steel is then held in this region for sufficient time
to allow the completion of the bainitic phase transformation reaction; finally, air cooling to room
temperature is conducted. The absence of a sudden quench to form martensite (as in the case of
traditional quench and tempering processes) significantly reduces the thermal gradients arising in
the material. This results in reduced distortion and minimization of the appearance of quench cracks.
This is especially the case for small parts (like gears, bolts, and clips) used in automotive and naval
structural applications that are exposed to alternating stresses. In addition, austempering can yield

Metals 2017, 7, 466; doi:10.3390/met7110466 www.mdpi.com/journal/metals

Metals 2017, 7, 466 2 of 18

strengths like those created in traditional quench and tempering processes, especially in medium and
Metals 2017, 7, 466 2 of 18
high carbon steels.
Failure under cyclic
yield strengths loading
like those (fatigue)
created is a very serious
in traditional quench problem for structural
and tempering components.
processes, especially inUnder
cyclicmedium
loading,and cracks can arise and
high carbon steels. grow; in this case, if the crack grows from a sub-critical dimension
to a critical flaw under
Failure size, itcyclic
can lead ultimately
loading (fatigue)toisfailure
a veryinserious
service. The critical
problem flaw size
for structural under a given
components.
loading condition
Under is givencracks
cyclic loading, by thecan
fracture toughness
arise and grow; inof thecase,
this material
if the [6].
crackThe fatigue
grows fromcrack growth rate,
a sub-critical
dimension
(da/dN), has been to arelated
critical to
flaw
thesize, it can
stress lead ultimately
intensity to failure
factor range, (∆K),inthrough
service. the
TheParis
critical flaw size
equation [7]:
under a given loading condition is given by the fracture toughness of the material [6]. The fatigue
da to the stress
crack growth rate, (da/dN), has been related intensity factor range, (∆K), through the
= C (∆K )m − (1)
Paris equation [7]: dN
where C and m are material constants, and ∆K = K∆max − − Kmin , which is the difference between (1) the
maximum (K
where C max
) and the minimum
and m are material constants,
(K min and ∆K = Kmax − Kmin, which is the difference between the has
) stress intensity factor in a fatigue cycle. This equation
been maximum
found to be very
(Kmax useful
) and in characterizing
the minimum (Kmin) stresstheintensity
fatigue factor
crack ingrowth
a fatiguebehavior of steels.
cycle. This equation has
As Figure 1 illustrates, when experimentally-measured crack growth
been found to be very useful in characterizing the fatigue crack growth behavior of steels. rate data is plotted against
∆K on a log As scale,
Figurethe graph shows
1 illustrates, whenthree distinct regions. Incrack
experimentally-measured Region I (therate
growth threshold region),
data is plotted the crack
against
growth∆K rate
on a log scale,
is low andthedeviates
graph shows
from three
thedistinct regions. In Region
Paris equation. I (theIIthreshold
In Region (the linear region), the crack
region), the Paris
growth
equation rate isthe
models lowgrowth
and deviates fromIn
rate well. theRegion
Paris equation. In Region
III (the fast II (the
fracture linearthe
region), region),
crackthe Paris rate
growth
equation models the growth rate well. In Region III (the fast fracture region), the crack
accelerates and again deviates from the Paris equation. In addition to these regions, there is a threshold growth rate
accelerates and again deviates from the Paris equation. In addition to these regions, there is a
stress intensity factor (∆Kth ), below which the crack growth rate approaches a zero value. Fatigue
threshold stress intensity factor (∆Kth), below which the crack growth rate approaches a zero value.
threshold is a very important parameter for structural design; structural components designed on the
Fatigue threshold is a very important parameter for structural design; structural components
basis designed
of fatigueonthreshold arefatigue
the basis of expected to survive
threshold in service
are expected under cyclic
to survive loading
in service underconditions without
cyclic loading
undergoing any catastrophic failure.
conditions without undergoing any catastrophic failure.

Figure 1. Fatigue Crack Growth Curve Schematic.

Figure 1. Fatigue Crack Growth Curve Schematic.
AISI 4140 is an extensively used commercial-grade medium-carbon, low alloy steel. It contains
AISI 4140 ismolybdenum,
chromium, an extensivelyand used commercial-grade
manganese medium-carbon,
as the principal low alloy
alloying elements steel.
and hasIt high
contains
chromium, molybdenum,
hardenability and good and manganese
fatigue resistanceas [1,2].
the principal
This steelalloying elements
has many and has
applications high hardenability
in mission-critical
structural
and good components
fatigue [8] because
resistance of its steel
[1,2]. This high strength
has many andapplications
toughness. Thisinsteel can be hardened
mission-critical by
structural
a variety of common heat-treatment processes to yield a wide variety of mechanical
components [8] because of its high strength and toughness. This steel can be hardened by a variety of properties.
While in service in critical applications, the 4140 steel can be exposed to hydrogen-bearing
common heat-treatment processes to yield a wide variety of mechanical properties. While in service
environments. Therefore, hydrogen-induced fatigue crack growth data for this material is needed
in critical applications, the 4140 steel can be exposed to hydrogen-bearing environments. Therefore,
for safe life prediction and failure-safe design of components. Although a significant number of
hydrogen-induced fatigue crack growth data for this material is needed for safe life prediction and
studies have been carried out on fatigue and corrosion fatigue behavior of high strength steels, most
failure-safe design of components.
of these studies were carried out Although
in 3.5% NaCl a significant number of studies have been carried out on
solutions [9–14].
fatigue and corrosion fatigue behavior of high strength steels, most of these studies were carried out in
3.5% NaCl solutions [9–14].
Metals 2017, 7, 466 3 of 18

Little information is available in literature on the influence of dissolved hydrogen on the fatigue
crack growth behavior of AISI 4140 steel, especially in the austempered condition. One study [15]
compared a quenched and tempered structure to an austempered structure in a gaseous hydrogen
environment. This study found that the austempered samples had lower fatigue crack growth rates
and higher impact toughness in the hydrogen environment. A second study [14] was conducted
on a 4140-type steel that was charged with approximately 0.58 ppm hydrogen. At low ∆K values,
the presence of hydrogen increased the fatigue crack growth rates up to 30×. When the ∆K values
√
exceeded 30 MPa m, the fatigue crack growth rates were comparable regardless of whether hydrogen
was present or not. Similar results were also observed in [16].
Previous research has shown that bainitic microstructures improve the fracture toughness in
ferrous alloys [4,5,17]. This indicates that bainitic microstructures can possibly improve the fatigue
crack growth resistance both in ambient and corrosive environments. Therefore, an investigation was
undertaken to examine the influence of an austempering process on the microstructure, mechanical
properties, fatigue crack growth rate, and fatigue threshold of AISI 4140 steel with dissolved hydrogen.
In a previous investigation [18], the fatigue crack growth behavior of AISI 4140 steel austempered in
the upper bainitic region was examined in the presence of dissolved hydrogen. This investigation is the
continuation of that study; in this paper, the fatigue crack growth of AISI 4140 steel, austempered in the
lower bainitic temperature region, was examined in presence of dissolved hydrogen. The testing was
designed to simulate what the 4140 steel might see following a hydrogen-containing manufacturing
operation and an ambient-air operating environment.

2. Experimental Procedure

2.1. Material
The material used in this investigation is the AISI 4140 steel alloy. The material was available
in the form of cold-rolled and annealed plate with an identifiable rolling direction. The chemical
composition of the material is reported in Table 1.

Table 1. Chemical Composition of the 4140 Alloy Steel.

Element Composition (wt %)

C 0.40
Cr 1.12
Mo 0.18
Mn 0.93
Si 0.33
S 0.031
P 0.025
Cu 0.02
Ni 0.17
Fe Balance

From this steel plate, tensile specimens were prepared as per ASTM E-8 [19]. Compact Tension
(CT) specimens were also manufactured with a TL orientation as per ASTM standard E-647 [20]. In the
CT specimens, the width (W) was 50.8 mm, the thickness ranged between 3 and 4 mm, and the notch
length (as measured from the centerline of the loading holes to the tip of the machined notch) was
15.24 mm. Additional compact tension samples were prepared for fracture toughness testing as per
ASTM standard E-399 [6]; for these samples, the width was 40 mm and the thickness was 20 mm.

2.2. Heat Treatment and Tensile Testing

To understand the effect of austempering, all of the test samples (tensile and CT) were divided into
two batches. The first batch of samples was left in the annealed (as-received) condition. The second
Metals 2017, 7, 466 4 of 18

batch of samples were heat-treated to produce an austempered condition. This was accomplished by
initially austenitizing these samples at 882 ◦ C for 1 h. The samples were then immediately transferred
to a molten salt bath at 332 ◦ C, where they were held for 1 h. The austempering in this 332 ◦ C
temperature region produced the desired lower bainitic structure. The specimens were then removed
from the salt bath and were allowed to air cool to room temperature.
All of the tensile samples (annealed as well as heat-treated) were tested as per ASTM E-8 [19].
The tests were performed at a constant engineering strain rate of 4 × 10−4 s−1 on a servo-hydraulic
Material Test System (MTS) 810 test machine. All of the samples were tested at room temperature and
ambient atmosphere. Load and displacement plots were obtained on an X–Y recorder; from these
load-displacement diagrams, the yield strength, ultimate tensile strength, and % elongation values
were calculated. Four samples were tested in each condition.

2.3. Pre-Cracking of CT Specimens

To minimize the amount of time between hydrogen charging and testing, all of the CT specimens were
pre-cracked before charging occurred. Pre-cracking was performed in the MTS 810 servo-hydraulic
test machine in the load control mode at room temperature and ambient atmosphere. For the fatigue
threshold specimens, a cyclic loading frequency of five cycles per second (5 Hz) was used to produce a
2-mm sharp crack front in accordance with ASTM standard E-647 [20]. The CT samples for the fracture
√
toughness tests were pre-cracked in fatigue at a ∆K level of 10 MPa m with a load ratio of R = 0.10.
This produced a 2-mm sharp crack in accordance with the ASTM standard E-399 [6].

2.4. External Hydrogen Charging

To understand the effect of hydrogen and austempering, all of the pre-cracked Compact Tension
(CT) specimens were divided into one of the four sets listed in Table 2.

Table 2. Matrix of Material Conditions for the 4140 Alloy CT Specimens.

Set Material Externally Charged with Hydrogen?

“A” Annealed No
“B” Annealed Yes
“C” Austempered (332 ◦ C/1 h) No
“D” Austempered (332 ◦ C/1 h) Yes

As detailed in Table 2, two of the sets were set aside; these are referred to as the “Uncharged”
specimens. The other two sets were externally charged with hydrogen (“Charged” specimens).
Charging was accomplished using two DC power supplies (Agilent E3616A and Sorensen XPL-30-2D)
that were capable of providing a steady source of electric current of about 1–1.5 A and a 4-mm
stainless steel bar as the anode; the stainless steel bar was chosen as it was an effective, low-cost
alternative to platinum. The samples to be charged with hydrogen were used as the cathode
(Figure 2). Deionized water, obtained from Barnstead Nanopure Diamond D11911, having a resistivity
of about 16.5 ± 0.5 MΩ-cm, was used to dissolve sodium hydroxide so that a 1 N solution was
obtained. Dissolution was done to avoid the uptake of deleterious ions during the external hydrogen
charging [21]. This 1 N solution was used as the electrolyte for charging hydrogen into the samples.
The current density was maintained steady at 300 A/m2 . The samples were charged with hydrogen
for 150, 200, and 250 h at room temperature. A minimum of three samples were charged from each set
for each of the given exposure times; in each case, the sample was tested within 15 min after charging
was complete.
In addition, six special CT samples were created for the purpose of measuring the hydrogen
concentration in the annealed and austempered conditions. These samples were prepared in the
manner detailed previously.
Metals 2017, 7, 466 5 of 18

In addition, six special CT samples were created for the purpose of measuring the hydrogen
concentration
Metals 2017, 7, 466 in
the annealed and austempered conditions. These samples were prepared in 5 ofthe
18
manner detailed previously.

Figure 2. Experimental setup of external hydrogen charging.

Figure 2. Experimental setup of external hydrogen charging.

2.5. Hydrogen Concentration Analysis

2.5. Hydrogen Concentration Analysis
The six special analysis samples were analyzed for the hydrogen concentration via a Vacuum
The six special analysis samples were analyzed for the hydrogen concentration via a Vacuum Hot
Hot Extraction method using an NRC Model 917 unit. The testing was conducted at Luvak
Extraction method using an NRC Model 917 unit. The testing was conducted at Luvak Laboratories
Laboratories (Boylston, MA, USA) within 24 h of charging. Each charged sample was first weighed
(Boylston, MA, USA) within 24 h of charging. Each charged sample was first weighed and cleaned
and cleaned with ether to remove surface contaminants. Each sample was then placed into an
with ether to remove surface contaminants. Each sample was then placed into an evacuated chamber
evacuated chamber surrounded by induction heating coil. Each sample was heated to a point below
surrounded by induction heating coil. Each sample was heated to a point below the melting point of
the melting point of the sample (approximately 1150 °C) to degas hydrogen from the sample. The
the sample (approximately 1150 ◦ C) to degas hydrogen from the sample. The hydrogen was collected
hydrogen was collected in a separate chamber in the system, and was measured by a McLeod gauge.
in a separate chamber in the system, and was measured by a McLeod gauge. All of the measurements
All of the measurements were accurate to ±0.1 ppm.
were accurate to ±0.1 ppm.
2.6. Fatigue Testing
2.6. Fatigue Testing
Within 15 min after completion of charging, each fatigue sample was tested on a MTS 810
Within 15 min after completion of charging, each fatigue sample was tested on a MTS 810
servo-hydraulic test machine in the load control mode at room temperature and in ambient
servo-hydraulic test machine in the load control mode at room temperature and in ambient atmosphere.
atmosphere. All of the fatigue testing was carried out at a cyclic loading frequency of five cycles per
All of the fatigue testing was carried out at a cyclic loading frequency of five cycles per second
second (5 Hz). A constant amplitude sinusoidal waveform was applied and the tests were carried
(5 Hz). A constant amplitude sinusoidal waveform was applied and the tests were carried out at a
out at a load ratio R = Kmin/Kmax = 0.10. Crack lengths were measured on the specimen surface using
load ratio R = Kmin /Kmax = 0.10. Crack lengths were measured on the specimen surface using an
an optical microscope without interrupting the test; at the same time, the number of fatigue cycles
optical microscope without interrupting the test; at the same time, the number of fatigue cycles was
was also recorded. The crack growth rate, da/dN, was determined as per ASTM standard E-647 [20].
also recorded. The crack growth rate, da/dN, was determined as per ASTM standard E-647 [20].
Four samples from each material condition, as listed in Table 2, were tested and averaged for the
Four samples from each material condition, as listed in Table 2, were tested and averaged for the
values reported in this paper.
values reported in this paper.
The threshold was obtained using the load-shedding, decreasing ∆K procedure detailed in
The threshold was obtained using the load-shedding, decreasing ∆K procedure detailed in
ASTM E-647 [20]; the load was periodically decreased until the crack growth rate reached a level of
ASTM E-647 [20]; the load was periodically decreased until the crack growth rate reached a level of
10−−10 m/cycle. The reduction of load at a given ∆K level was done in such a way that no more than
10 10 m/cycle. The reduction of load at a given ∆K level was done in such a way that no more than
10% of the load was reduced for that ∆K level. This load shedding was also done after the crack has
10% of the load was reduced for that ∆K level. This load shedding was also done after the crack has
grown at least 0.5 mm at the previous ∆K level. In this way, any retardation effect (due to a previous
grown at least 0.5 mm at the previous ∆K level. In this way, any retardation effect (due to a previous
higher ∆K level) was avoided.
higher ∆K level) was avoided.
2.7. Fracture
2.7. Toughness Test
Fracture Toughness Test
Within 15
Within 15 min
min after
after completion
completion of
of charging,
charging, each
each fracture
fracture toughness
toughness specimen
specimen was
was loaded
loaded in
in
tension in
tension in aa servo-hydraulic
servo-hydraulicMTS
MTStest
testmachine;
machine;the
theload-displacement
load-displacementdiagrams
diagramswere
wereobtained
obtained using
using a
a clip gauge in the knife edge attachment on the specimen. From these load-displacement
clip gauge in the knife edge attachment on the specimen. From these load-displacement diagrams,diagrams,
PQ values
P were calculated using the 5% secant deviation technique. From these PQ values, the KQ
Q values were calculated using the 5% secant deviation technique. From these PQ values, the KQ
values were determined using the standard stress intensity factor calibration function for the CT
Metals 2017,
Metals 2017, 7,
7, 466
466 66 of
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18

values were determined using the standard stress intensity factor calibration function for the CT
specimens. Since
Since these
these K KQQ values
values satisfied
satisfied all
all of
of the
the requirements
requirements for a valid KIC IC as per ASTM

standard E-399
standard E-399[6],
[6],they
they
werewere judged
judged to betovalid
be valid KIC values.
KIC values. Four samples
Four samples from eachfrom eachcondition
material material
condition
listed listed
in Table in Table
2 were 2 were
tested and tested
averagedandfor
averaged for the
the values valuesinreported
reported in this paper.
this paper.

3. Results and Discussion

3.1. Microstructure
3.1. Microstructure
The microstructureofofthe
The microstructure the 4140
4140 steel
steel alloyalloy inannealed
in the the annealed condition
condition showedshowed
a mixedaferrite
mixed+
ferrite
pearlite+ pearlite structure;
structure; very finevery fine needles
needles of pearlite
of pearlite werewere observed
observed in in
thethe matrix(Figure
matrix (Figure3)
3) X-ray
X-ray
diffraction [18] as well as transmission electron microscopy (TEM) examinations were
diffraction [18] as well as transmission electron microscopy (TEM) examinations were carried out.carried out.
Both techniques detected only body-centered cubic (BCC) phases in the material. No
Both techniques detected only body-centered cubic (BCC) phases in the material. No retainedretained austenite
was detected
austenite was(via XRD or
detected (viaTEM)
XRDor orobserved
TEM) or in prepared
observed in metallographic specimens.specimens.
prepared metallographic

Figure
Figure 3.
3. Fine Pearlite Observed in the Annealed AISI 4140 Steel Alloy (Sodium Bisulfate etch).

The microstructure of the austempered 4140 samples is shown in the Figure 4. It shows the
The microstructure of the austempered 4140 samples is shown in the Figure 4. It shows the
presence of lower bainite (blue-colored phase) and a limited number of isolated pockets of
presence of lower bainite (blue-colored phase) and a limited number of isolated pockets of martensite
martensite (brown-colored phase) in the microstructure. These arose even though the samples were
(brown-colored phase) in the microstructure. These arose even though the samples were austempered
austempered at a temperature above the Ms (Martensite Start) temperature of the material. This was
at a temperature above the Ms (Martensite Start) temperature of the material. This was attributed to
attributed to segregation effects from the alloying elements present in the steel. The carbides of
segregation effects from the alloying elements present in the steel. The carbides of alloying elements
alloying elements like Cr, Mo, and Mn tend to segregate to the intercellular regions. In these
like Cr, Mo, and Mn tend to segregate to the intercellular regions. In these segregated regions, the
segregated regions, the bainitic reaction associated with the austenite decomposing into ferrite and
bainitic reaction associated with the austenite decomposing into ferrite and carbide becomes sluggish;
carbide becomes sluggish; therefore, complete transformation does not take place during the
therefore, complete transformation does not take place during the processing time. Upon cooling,
processing time. Upon cooling, these untransformed regions can form martensitic structures.
these untransformed regions can form martensitic structures. Optically, a very small amount (<1%) of
Optically, a very small amount (<1%) of retained austenite (white phase) was also observed in the
retained austenite (white phase) was also observed in the material; however, no retained austenite
material; however, no retained austenite was detected using either XRD or TEM. Therefore, it is
was detected using either XRD or TEM. Therefore, it is concluded that the amount of austenite
concluded that the amount of austenite present is so small as to have no effect upon the resultant
present is so small as to have no effect upon the resultant hydrogen concentration or properties in the
hydrogen concentration or properties in the austempered material.
austempered material.
Metals 2017, 7, 466 7 of 18
Metals 2017, 7, 466 7 of 18

Figure 4.
Figure 4. The
The Microstructure of the
Microstructure of the Austempered
Austempered AISI
AISI 4140
4140 Steel
Steel Alloy
Alloy (Sodium
(Sodium Bisulfate
Bisulfate etch).
etch).

3.2. Mechanical
3.2. Mechanical Properties
Properties
The mechanical
The mechanicalproperties
propertiesofofthe
the4140
4140 steel
steel areare reported
reported in Table
in Table 3. Statistical
3. Statistical analysis
analysis ofdata
of this this
data showed
showed thataustempering
that the the austempering
processprocess had significantly
had significantly increased
increased the hardness,
the hardness, as well
as well as both
as both the
the yield and tensile strengths, without any significant reduction in the ductility. In addition,
yield and tensile strengths, without any significant reduction in the ductility. In addition, the fracture the
fracture toughness
toughness shows a slight
shows a statistically statistically slight improvement
improvement as austempered
as well. Thus, the well. Thus, the austempered
microstructure of
lower bainite with a limited amount of martensite has increased the strength, hardness,the
microstructure of lower bainite with a limited amount of martensite has increased andstrength,
fracture
hardness, and
toughness fracture
without toughness
any loss without
of ductility in theany loss
AISI of ductility
4140 in the AISIthe
steel. Furthermore, 4140 steel. and
strength Furthermore,
hardness
the strength and hardness of the material was comparable to that obtained
of the material was comparable to that obtained by a traditional quenching and tempering process in by a traditional
quenching
AISI and[22].
4140 steel tempering process in AISI 4140 steel [22].

Table 3. Mechanical
Table 3. Mechanical Properties
Properties of
of AISI
AISI 4140
4140 Alloy.
Alloy.

Material Yield Strength Ultimate Tensile Fracture Toughness

Material Yield Strength Ultimate Tensile% Elongation
% Hardness
Hardness
(HRc) Fracture Toughness
√
Condition
Condition (MPa)
(MPa) Strength (MPa)
Strength (MPa) Elongation (HRc ) (MPa√m)
(MPa m)
Annealed
Annealed 757±±2020
757 ±5 ±5
10311031 5.6 5.6 28±±
28 11 6565±± 22
Austempered
Austempered 1481 ± 12 1646 ± 9 5.5 45 ± 1 72 ± 6
(332 ◦ C/1 h) 1481 ± 12 1646 ± 9 5.5 45 ± 1 72 ± 6
(332 °C/1 h)

3.3. Hydrogen Concentration

3.3. Hydrogen Concentration
Table 4 shows the effect of charging times on the concentration of dissolved monoatomic hydrogen
Table 4 shows the effect of charging times on the concentration of dissolved monoatomic
in the 4140 steel alloy. As this table shows, the amount of dissolved hydrogen increases as the charging
hydrogen in the 4140 steel alloy. As this table shows, the amount of dissolved hydrogen increases as
time increases for both the annealed and austempered conditions.
the charging time increases for both the annealed and austempered conditions.
Table 4. The Effect of Charging Time on the Dissolved Hydrogen Content of the 4140 Steel.
Table 4. The Effect of Charging Time on the Dissolved Hydrogen Content of the 4140 Steel.
Material Condition Hydrogen Charging Time (Hours) Measured Hydrogen Content (ppm)
Material Condition Hydrogen Charging Time (Hours) Measured Hydrogen Content (ppm)
150 0.7
150 0.7
Annealed 200 1.5
Annealed 200
250 1.5
2.9
250
150 2.9
1.6
Austempered (332 ◦ C/1 h) 200
150 3.6
1.6
250 8.1
Austempered (332 °C/1 h) 200 3.6
250 8.1
Metals 2017, 7, 466 8 of 18
Metals 2017, 7, 466 8 of 18

Additionally,
Additionally, the the table
table shows
shows that
that the
the austempered
austempered samples
samples were
were found
found toto have
have over
over aa two-fold
two-fold
increase in the amount of dissolved hydrogen compared to the
increase in the amount of dissolved hydrogen compared to the annealed samples annealed samples for a given
for charging
a given
time. This
charging can This
time. be attributed to the small
can be attributed to theamount of martensite
small amount present
of martensite in the in
present microstructure
the microstructureafter
austempering. Martensitic structures are known to have a higher dislocation
after austempering. Martensitic structures are known to have a higher dislocation density when density when compared
to other phases
compared to otherlike ferrite,
phases likepearlite,
ferrite, or bainiteor[1,2].
pearlite, These
bainite [1,2].dislocations can actcan
These dislocations as hydrogen traps
act as hydrogen
in thein
traps material [16,23,24].
the material The presence
[16,23,24]. of these
The presence trapstraps
of these also reduces the diffusivity
also reduces of hydrogen
the diffusivity of hydrogento a
lower value than what was estimated by equations based upon the concentration
to a lower value than what was estimated by equations based upon the concentration [25]. One [25]. One previous
investigation [16] also concluded
previous investigation [16] also that that thethat
concluded diffusivity
that theofdiffusivity
hydrogen in ofsteel cannotin
hydrogen besteel
determined
cannot by be
application of Fick’s law in the presence of traps in the material.
determined by application of Fick’s law in the presence of traps in the material.
In
In addition
addition to to dislocation
dislocation density
density effects,
effects, the
the diffusion
diffusion coefficient
coefficient of
of hydrogen
hydrogen appears
appears toto be
be
affected
affected by
by the
the presence
presence of of martensite
martensite as as well.
well. An
An earlier
earlier investigation
investigation on on Cr-Mo
Cr-Mo steels
steels [26]
[26] showed
showed
that
that the
the diffusion
diffusion coefficient
coefficient of of hydrogen
hydrogen in in martensite
martensite was was marginally
marginally lower
lower than
than that
that in
in bainite.
bainite.
Further, a recent study on hydrogen-induced cracking in steels [15] showed
Further, a recent study on hydrogen-induced cracking in steels [15] showed that the diffusionthat the diffusion coefficient
decreases
coefficientas the strength
decreases as theof strength
the alloyof increased.
the alloy increased.
Thus,
Thus, it can be concluded that the presence
it can be concluded that the presence ofof martensite
martensite in in the
the austempered
austempered alloyalloy resulted
resulted inin aa
larger
larger number
number of of dislocations,
dislocations, which
which created a large
large number
number of of hydrogen
hydrogen traps
traps in
in the
the material.
material. This,
in turn, resulted in higher concentration of dissolved hydrogen content in the austempered samples
compared to the annealed sample. sample.

3.4. Influence of
3.4. Influence of Austempering
Austempering on
on the
the Crack
Crack Growth
Growth Behavior
Behavior of
of Uncharged
Uncharged 4140
4140 Steel
Steel
Figure
Figure 55 compares
compares thethefatigue
fatiguecrack
crackgrowth
growthbehavior
behavior in in
thethe threshold
threshold region
region (Region
(Region I) the
I) for for
the annealed and austempered conditions; this data is for the samples without dissolved
annealed and austempered conditions; this data is for the samples without dissolved hydrogen (Sets hydrogen
(Sets “A”“C”
“A” and and in“C” in Table
Table 2). Table
2). Table 5 details
5 details the threshold
the threshold stress
stress intensity
intensity values
values for these
for these materials.
materials. As
As this figure and table illustrate, the fatigue crack growth rate of the annealed
this figure and table illustrate, the fatigue crack growth rate of the annealed samples in samples in the
the
near-threshold
near-thresholdregion
regionwas
washigher thanthan
higher the austempered samples;
the austempered additionally,
samples; the ∆Kththe
additionally, of the
∆Kannealed
th of the
samples was lower than that of the austempered samples in this region as
annealed samples was lower than that of the austempered samples in this region as well.well.

Figure 5. The Effect of Austempering on the Fatigue Crack Growth Rate of Uncharged 4140 Steel in
Figure 5. The Effect of Austempering on the Fatigue Crack Growth Rate of Uncharged 4140 Steel in the
the Threshold Region.
Threshold Region.
Metals 2017, 7, 466 9 of 18

Table 5. Experimentally-Determined Values of ∆Kth for the Uncharged 4140 Steel Alloy.

√
Material Condition ∆Kth (MPa m)
Annealed 6.68
Austempered (332 ◦ C/1 h) 8.12

The lower crack growth rate in the austempered samples was an interesting result and cannot be
attributed to the lower crack closure stress intensity factor (Kop ) in this material. During cyclic loading,
the compressive stress in the crack tip region will cause the crack to remain partially closed during the
unloading part of the fatigue cycle. This stress intensity factor (for crack closure) is often defined as
Kop . Thus, the effective stress intensity factor, ∆Keff , is a measure of crack driving force and is given by
∆Keff = Kmax − Kop . This crack-opening stress intensity factor depends on the cyclic plastic zone size,
which is inversely proportional to the yield strength of the material. Thus, the Kop value decreases as
the material strength increases.
In this study, the cyclic plastic zone size was calculated using Rice’s formula [27] for each set
of specimens at the different charging conditions, based upon where the maximum transgranular
(or intergranular) feature was observed. However, these calculations yielded identical results for all of
the materials; the cyclic plastic zone sizes were approximately 14–22 µm. Further, the austempered
samples had a significantly higher yield strength than the annealed samples (Table 3). This means
that the Kop value will be lower in the austempered samples as compared to the annealed samples.
Therefore, it would be expected that a higher crack driving force (∆Keff ) would be present in the
austempered samples. Consequently, a higher near-threshold fatigue crack growth rate and lower
fatigue threshold (∆Kth ) would also be expected for the austempered samples.
However, the opposite was observed in the samples in this study: a lower crack growth rate and
higher ∆Kth were found for the austempered samples. This unique behavior is hypothesized to be due
to the following two factors:

• First, the austempering process has increased the fracture toughness of the material due to the
presence of a microstructure containing a large amount of lower bainite. The lower bainitic
microstructure increases the fracture toughness of the material [3–5]. The higher fracture
toughness is indicative of a greater crack growth resistance in this material. This, in turn, causes a
lower fatigue crack growth rate and a higher fatigue threshold in the material.
• Secondly, the austempered samples had a very fine-scale microstructure consisting of lower
bainite with a limited amount of tempered martensite. A lower bainitic structure has a much finer
grain size than upper bainite or pearlite. This creates additional resistance to crack growth since
the crack tip encounters large number of fine scale grain boundaries. This, in turn, reduces the
crack propagation rate because the crack grows along a longer, more torturous path.

Figure 6 shows the fatigue crack growth behavior of the uncharged annealed and austempered
specimens in the linear region (Region II). This is further shown by the data in Table 6. The austempered
material had a much lower value of the Paris constant “C” and a slightly higher “m” value. It is
evident from the plot that the austempered specimens have a lower crack growth rate than the annealed
specimens. Again, the general expected trend is that the fatigue crack growth rate increases with a
higher strength and hardness. However, the austempered samples in the present study again have a
lower crack growth rate despite the higher hardness and strength; this behavior is similar to what was
seen previously in the threshold region. The behavior is also attributed to the increased crack growth
resistance provided by the lower bainitic microstructure.
Metals 2017, 7, 466 10 of 18

Table 6. Comparison of Paris Constants for the Uncharged 4140 Steel Alloy.
Metals 2017, 7, 466 10 of 18
Paris Law Constant
Material
Hence, upon comparing theCondition
fatigue crack growth rates in the linear region (Figure 6), as well as
C m
in the threshold region (Figure 5), it can be concluded that−the
10
lower bainitic microstructure provides
Annealed 1 × 10 2.08
an improved fatigue crack growth resistance in 4140 steels when dissolved hydrogen is not present.
Austempered (332 ◦ C/1 h) 5 × 10−11 2.14
Similar results have been reported for a series of low alloy steels [28].

Figure 6. The Effect of Austempering on the Fatigue Crack Growth Rate of Uncharged 4140 Steel in
Figure 6. The Effect of Austempering on the Fatigue Crack Growth Rate of Uncharged 4140 Steel in the
the Linear Region.
Linear Region.

3.5. Influence of Hydrogen on the Fatigue Crack Gowth Behavior of 4140 Steel
Hence, upon comparing the fatigue crack growth rates in the linear region (Figure 6), as well as in
Figure 7 shows
the threshold region the fatigue
(Figure crack
5), it can growth behavior
be concluded thatofthe
thelower
annealed samples
bainitic in the linear
microstructure region
provides
in presence of dissolved hydrogen; for comparison, the crack growth behavior of
an improved fatigue crack growth resistance in 4140 steels when dissolved hydrogen is not present. the annealed
samplesresults
Similar without dissolved
have hydrogen
been reported for aisseries
also plotted in thesteels
of low alloy same[28].
figure. The data in Figure 7 shows
that the presence of dissolved hydrogen causes a large amount of variation in the crack growth rate
data.Influence
3.5. In addition, the presence
of Hydrogen of hydrogen
on the Fatigue Crack appears to increase
Gowth Behavior theSteel
of 4140 average crack growth rate at ∆K
values that are greater than 60 MPa√m. Figure 7 also shows that the hydrogen charging time does
Figure 7 shows the fatigue crack growth behavior of the annealed samples in the linear region in
not have any significant effect on the crack growth rate, given the high degree of variation in the
presence of dissolved hydrogen; for comparison, the crack growth behavior of the annealed samples
data.
without dissolved hydrogen is also plotted in the same figure. The data in Figure 7 shows that the
presence of dissolved hydrogen causes a large amount of variation in the crack growth rate data.
In addition, the presence of hydrogen appears to increase the average crack growth rate at ∆K values
√
that are greater than 60 MPa m. Figure 7 also shows that the hydrogen charging time does not have
any significant effect on the crack growth rate, given the high degree of variation in the data.
Metals 2017, 7, 466 11 of 18
Metals 2017, 7, 466 11 of 18

Figure 7. The Effect of Hydrogen Charging Time on the Fatigue Crack Growth Rate in the Linear
Figure 7. The Effect of Hydrogen Charging Time on the Fatigue Crack Growth Rate in the Linear
Region for the Annealed 4140 Steel Samples.
Region for the Annealed 4140 Steel Samples.

Figure 8 shows the fatigue crack growth behavior of the austempered samples in the linear
Figure
region in the 8 shows
presence the fatigue crack growth
of dissolved hydrogen;behavior
again,offorthecomparison
austemperedpurposes,
samples inthe thecrack
lineargrowth
region
in the presence
behavior of the of dissolved hydrogen;
austempered again, for
samples without comparison
dissolved purposes,
hydrogen theplotted
is also crack growth
in the samebehavior of
figure.
the austempered samples without dissolved hydrogen is also plotted
Similar to that seen in Figure 7, Figure 8 shows that the hydrogen charging time does not have any in the same figure. Similar to
that seen ineffect
significant Figure on7,the
Figure
crack8 growth
shows that ratethe hydrogen
of the charging
austempered time does
samples. not have
However, in any significant
contrast to the
effect on the crack growth rate of the austempered samples. However,
data in Figure 7, Figure 8 shows that the presence of dissolved hydrogen does not cause a large in contrast to the data in
Figure 7, Figure 8 shows that the presence of dissolved hydrogen does
amount of variation in the crack growth rate data. In addition, Figure 8 shows that the presence of not cause a large amount of
variation in
dissolved the crackincreases
hydrogen growth rate the data.
crack In addition,
growth rate Figure 8 shows
significantly at that the presence
∆K values of dissolved
√below 30 MPa√m.
hydrogen increases the crack growth rate significantly at ∆K values below
Thus, the effect of hydrogen is relatively important when the contribution of other mechanisms 30 MPa m. Thus, the effectis
of hydrogen is relatively important when the contribution of other mechanisms
small. When ∆K is low, there is little stress built up at the crack tip; the effect of hydrogen on crack is small. When ∆K is
low, there
growth is little stress
is increased sincebuilt up is
there at little
the crack
stresstip;
to the effectincreased
provide of hydrogen on crack
energy for the growth is increased
propagation of a
since
crack. there is little stress to provide increased energy for the propagation of a crack.
The results
The results in in Figures
Figures 77 andand 8 8 agree
agree with
with those
those from
from twotwo published research studies
published research [14,16] on
studies [14,16] on
4100-series steel alloys charged with hydrogen and tested in laboratory
4100-series steel alloys charged with hydrogen and tested in laboratory air. They found that the air. They found that the crack
growth
crack rates inrates
growth the range 10−5 to
in theofrange of 10
−7
10−5 m/cycle were increased
to 10−7 m/cycle in the hydrogen-charged
were increased in the hydrogen-charged samples
when
samples compared
when compared to the uncharged samples. samples.
to the uncharged
Table 7 details the fatigue
Table 7 details the fatigue threshold threshold of both the annealed
of both and austempered
the annealed and austempered 4140 alloy 4140as alloy
a function
as a
of dissolved
function hydrogen hydrogen
of dissolved content. The data inThe
content. thisdata
tableinshows that there
this table shows arethat
onlythere
minor aredifferences
only minor in
the threshold values of the annealed and austempered samples; in addition,
differences in the threshold values of the annealed and austempered samples; in addition, all these all these values are low
regardless
values are of lowhydrogen
regardless content. This is ancontent.
of hydrogen important Thisresult,
is anasimportant
it shows that austempering
result, as it shows canthat
be
used to providecan
austempering improved
be usedstrength
to provide properties
improvedwhile avoiding
strength a significant
properties reduction
while avoiding in fatigue crack
a significant
resistance; this combination is not usually observed in most materials.
reduction in fatigue crack resistance; this combination is not usually observed in most materials.
Metals 2017, 7, 466 12 of 18
Metals 2017, 7, 466 12 of 18

Figure 8. The Effect of Hydrogen Charging Time on the Fatigue Crack Growth Rate in the Linear
Figure 8. The Effect of Hydrogen Charging Time on the Fatigue Crack Growth Rate in the Linear
Region for the Austempered 4140 Steel Samples.
Region for the Austempered 4140 Steel Samples.

Table 7. The Effect of Hydrogen-Charging Time on the ∆Kth for the 4140 Steel Alloy.
Table 7. The Effect of Hydrogen-Charging Time on the ∆Kth for the 4140 Steel Alloy.
Material Condition Hydrogen Charging Time (Hours) Hydrogen Concentration (ppm) ∆Kth (MPa√m)
Hydrogen Charging Hydrogen ∆Kth
Material Condition 0 √
Time (Hours) Concentration---
(ppm) (MPa m) 6.68
150 0 — 0.7 6.68 5.58
Annealed
Annealed 200 150 0.7 1.5 5.58 5.49
200 1.5 5.49
250 250 2.9 2.9 7.85 7.85
0 0 — --- 8.12 8.12
◦ C/1 150 150 1.6 1.6 6.59 6.59
Austempered (332 h)
Austempered (332 °C/1 h) 200 3.6 6.17
200 250 8.1 3.6 6.01 6.17
250 8.1 6.01

Table 7 also illustrates that, as the hydrogen concentration increases, the fatigue threshold
Table slightly
decreases 7 also illustrates that, as thesample.
in the austempered hydrogen This concentration
is the expectedincreases,
result, the
andfatigue threshold
it is believed to
decreases slightly in the austempered sample. This is the expected result,
be due to the increased amount of hydrogen that will cause lattice dilation in the steel. This, and it is believed toin beturn,
due
to the increased
increases the strainamount
fields andof internal
hydrogen that resulting
energy, will cause in alattice
greaterdilation
drivingin thefor
force steel.
crackThis, in turn,
propagation;
increases
this resultsthe
in astrain
lower fields
thresholdandstress
internal energy,
that must resulting toingrow
be achieved a greater
the crack.driving force for crack
propagation; this results in a lower threshold stress that must
Table 7 also shows that, in the annealed samples, the dissolved hydrogen be achieved to grow the crack.
content did not have
any significant effect. The reason for this has not been conclusively determined. It could did
Table 7 also shows that, in the annealed samples, the dissolved hydrogen content be anot have
result of
any significant effect. The reason for this has not been conclusively determined.
the large variation in the experimental data. Or, it may be due to a threshold limit, above which the It could be a result
of the large
presence variation could
of hydrogen in the beexperimental
beneficial todata.
certainOr,microstructures.
it may be due to a threshold
Further limit, above
investigation which
is necessary
theunderstand
to presence of hydrogen
these could
results and be progress.
is in beneficial to certain microstructures. Further investigation is
necessary to understand these results
Figures 9–11 compare the fatigue crack and isgrowth
in progress.
behavior in the linear region for the annealed and
Figures 9–11 compare the fatigue
austempered specimens as a function of the chargingcrack growthtime behavior in thehydrogen
(dissolved linear region for the
content.) annealed
Interestingly,
andof austempered specimens √
all these figures show that, in as
thealowfunction
(<30 MPa of the
m) ∆Kcharging
region,time (dissolved
the annealed hydrogen
specimens havecontent.)
a lower
Interestingly, all of these figures show that, in the low (<30 MPa√m)
crack growth rate than the austempered specimens. As the ∆K values increase beyond approximately ∆K region, the annealed
specimens√
30 MPa m,have a lower stress
a transition crack growth
intensityrate than
factor the austempered
range exists where the specimens.
annealed Asspecimens
the ∆K values have
an increasingly higher crack growth rate than austempered specimen. This observationwhere
increase beyond approximately 30 MPa√m, a transition stress intensity factor range exists the
indicates
annealed specimens have an increasingly higher crack growth rate than austempered
that, in the higher ∆K regions, the austempered specimens are more resistant to crack growth in specimen. This
observation indicates
hydrogen-charged that, in theThis
atmospheres. higherwas∆K regions, the
unexpected, asaustempered specimens
several investigators are more
[28,29] resistant
have reported
to crack growth in hydrogen-charged atmospheres. This was unexpected, as several investigators
[28,29] have reported that the embrittlement effects of hydrogen are more severe in the case of high
 Metals 2017, 7, 466 13 of 18

Metals 2017, 7, 466 13 of 18

Metals 2017, 7, 466 13 of 18
that the embrittlement effects of hydrogen are more severe in the case of high strength steels. Due to
strength
the highersteels. Due to the
strength higher strength and austempered
hardness of the alloy in austempered conditions,
strength steels. Due and hardness
to the higher of the alloy
strength andinhardness conditions,
of the hydrogen embrittlement
alloy in austempered conditions,
hydrogen embrittlement
would be embrittlement
expected to have would be
a stronger expected to have
effect. Ittoishave a stronger
hypothesized effect.
that It
the loweris hypothesized that the
bainitic microstructure
hydrogen would be expected a stronger effect. It is hypothesized that the
lower bainitic
developed microstructure
during developed
the austempering during
process the austempering
is counteracting process is counteracting
this embrittling this
lower bainitic microstructure developed during the austempering process is effect; the increased
counteracting this
embrittling
tortuosity of effect;
the the increased
crack path is tortuosity
believed to ofkey.
be the crack path is believed to be key.
embrittling effect; the increased tortuosity of the crack path is believed to be key.

Figure 9. The Effect of Austempering on the Fatigue Crack Growth Rate of the 4140 Steel
Figure
Figure 9.9. The
TheEffect
EffectofofAustempering
Austemperingononthe
theFatigue
FatigueCrack
CrackGrowth
GrowthRate
Rateofofthe
the4140
4140 Steel
Steel
Hydrogen-Charged for 150 h.
Hydrogen-Charged
Hydrogen-Chargedfor for150
150h.h.

Figure 10. The Effect of Austempering on the Fatigue Crack Growth Rate of the 4140 Steel
Figure 10. The Effect of Austempering on the Fatigue Crack Growth Rate of the 4140 Steel
Figure 10. The Effect
Hydrogen-Charged of h.
for 200 Austempering on the Fatigue Crack Growth Rate of the 4140 Steel
Hydrogen-Charged for 200 h.
Hydrogen-Charged for 200 h.
 Metals 2017, 7, 466 14 of 18
Metals 2017, 7, 466 14 of 18

Figure 11. The Effect of Austempering on the Fatigue Crack Growth Rate of the 4140 Steel
Figure 11. The Effect of Austempering on the Fatigue Crack Growth Rate of the 4140 Steel
Hydrogen-Charged for 250 h.
Hydrogen-Charged for 250 h.

3.6. Fractography
3.6. Fractography
The fracture surfaces that are associated with the annealed 4140 alloy samples are shown in
The fracture surfaces that are associated with the annealed 4140 alloy samples are shown in
Figure 12. As this figure shows, charging with hydrogen only slightly changes the fracture surface
Figure 12. As this figure shows, charging with hydrogen only slightly changes the fracture surface
morphology. The fracture surfaces of the hydrogen-charged samples (Figure 12b) appear to have
morphology. The fracture surfaces of the hydrogen-charged samples (Figure 12b) appear to have
limited ductile tearing with a more flat-like appearance as compared to the uncharged samples
limited ductile tearing with a more flat-like appearance as compared to the uncharged samples
(Figure 12a). This correlates well with experimentally-determined fatigue crack growth rate data
(Figure 12a). This correlates well with experimentally-determined fatigue crack growth rate data
shown in Figures 6 and 7, which show the relative closeness of the fatigue curves to one another
shown in Figures 6 and 7, which show the relative closeness of the fatigue curves to one another
regardless of the charging condition.
regardless of the charging condition.
Figure 13 shows the fracture surfaces associated with the austempered 4140 alloy samples at
Figure 13 shows the fracture surfaces associated with the austempered 4140 alloy samples at
low ∆K values. Several interesting characteristics were observed. Similar to that seen in Figure 12a,
low ∆K values. Several interesting characteristics were observed. Similar to that seen in Figure 12a,
the fracture surface in the uncharged samples (Figure 13a) have little ductile tearing and are
the fracture surface in the uncharged samples (Figure 13a) have little ductile tearing and are relatively
relatively flat in morphology. However, in contrast to those seen in Figure 12b, Figure 13b shows
flat in morphology. However, in contrast to those seen in Figure 12b, Figure 13b shows that the
that the hydrogen-charged austempered samples are characterized by both intergranular and
hydrogen-charged austempered samples are characterized by both intergranular and transgranular
transgranular features. Intergranular features appear increasingly prominently as the ∆K values
features. Intergranular features appear increasingly prominently as the ∆K values decrease in the
decrease in the charged austempered samples. This also agrees well with the experimental fatigue
charged austempered samples. This also agrees well with the experimental fatigue crack growth data,
crack growth data, which shows that the austempered samples that are charged with hydrogen
which shows that the austempered samples that are charged with hydrogen have fatigue crack growth
have fatigue crack growth rates that are faster and fatigue thresholds that are lower when
rates that are faster and fatigue thresholds that are lower when compared to those in the annealed
compared to those in the annealed material at low ∆K values.
material at low ∆K values.
Figure 14 shows the fracture surfaces associated with the austempered 4140 alloy samples at
Figure 14 shows the fracture surfaces associated with the austempered 4140 alloy samples at high
high ∆K values. As this figure details, the fracture surface in the uncharged samples (Figure 14a) are
∆K values. As this figure details, the fracture surface in the uncharged samples (Figure 14a) are very
very similar to those in the charged samples (Figure 14b). Both fracture surfaces are characterized
similar to those in the charged samples (Figure 14b). Both fracture surfaces are characterized by a large
by a large number of transgranular features. Once again, this agrees well with the experimental
number of transgranular features. Once again, this agrees well with the experimental fatigue crack
fatigue crack growth data for high ∆K values, which show that the fatigue crack growth rates for
growth data for high ∆K values, which show that the fatigue crack growth rates for the charged and
the charged and uncharged austempered material are similar at high ∆K values.
uncharged austempered material are similar at high ∆K values.
Metals 2017, 7, 466 15 of 18
Metals 2017, 7, 466 15 of 18
Metals 2017, 7, 466 15 of 18

(a)
(a)

(b)
(b)
Figure 12.
Figure Typical Fatigue
Typical
12.Typical Fracture
Fatigue Surface
Fracture Features
Surface Present
Features in the Annealed
Present 4140 Samples.
in the Annealed (∆K = 12
4140 Samples.
Figure 12. √ Fatigue Fracture Surface Features Present in the Annealed 4140 Samples. (∆K = 12
MPa√m; crack
(∆K = 12crack growth
MPagrowth direction
m; crack was
growth from top to bottom of photos). (a) Uncharged (No Hydrogen);
MPa√m; direction wasdirection
from topwas from top
to bottom to bottom
of photos). (a) of photos). (No
Uncharged (a) Hydrogen);
Uncharged
(b) Hydrogen-Charged.
(NoHydrogen-Charged.
Hydrogen); (b) Hydrogen-Charged.
(b)

(a)
(a)

Figure 13. Cont.

Metals 2017, 7, 466 16 of 18
Metals 2017, 7, 466 16 of 18

Metals 2017, 7, 466 16 of 18

(b)
(b)
Figure 13. Typical
Figure 13. TypicalFatigue
FatigueFracture
FractureSurface
SurfaceFeatures
Features Present
Present in the
in the Austempered
Austempered 41404140 Samples
Samples at
at low
Figure
low ∆K 13. Typical
Values. (∆K = √MPa√m;
Fatigue
19 Fracturecrack
Surface Features
growth Present
direction in the
was fromAustempered
top to 4140ofSamples
bottom at(a)
photos).
∆K Values. (∆K = 19 MPa m; crack growth direction was from top to bottom of photos). (a) Uncharged
low ∆K Values.
Uncharged (∆K = 19 MPa√m;
(No Hydrogen); crack growth direction was from top to bottom of photos). (a)
(b) Hydrogen-Charged.
(No Hydrogen); (b) Hydrogen-Charged.
Uncharged (No Hydrogen); (b) Hydrogen-Charged.

(a)

(b)
(b)
Figure
Figure 14.14. Typical
Typical Fatigue
Fatigue Fracture
Fracture Surface
Surface Features
Features Present
Present in in
thethe Austempered
Austempered 4140
4140 Samples
Samples at
at high
Figure
high 14.
∆K Typical Fatigue
Values. (∆K =√ 50 Fracture
MPa√m; Surface Features
crack growth Present
direction wasinfrom
the Austempered
top to bottom 4140 Samples
of photos). (a) at
∆K Values. (∆K = 50 MPa m; crack growth direction was from top to bottom of photos). (a) Uncharged
high ∆K Values.
Uncharged (No (∆K = 50 MPa√m;
Hydrogen); crack growth direction was from top to bottom of photos). (a)
(b) Hydrogen-Charged.
(No Hydrogen); (b) Hydrogen-Charged.
Uncharged (No Hydrogen); (b) Hydrogen-Charged.
4. Conclusions and Future Work
4. Conclusions
4. Conclusions andand Future
Future Work
Work
To better understand the effect of hydrogen upon the mechanical properties and fatigue crack
To better
growth
To better understand
understand the
of austempered 4140effect
the steel,of
effect hydrogen
ofthe present upon
hydrogen the
the mechanical
research
upon study properties
was conducted.
mechanical and
The fatigue
properties and crack
study was
fatigue crack
growth
growth ofofaustempered
conducted ex-situ to 4140
austempered steel,
simulate
4140 the exposure
the
steel, present research study
of aresearch
the present 4140 was
alloy toconducted.
study hydrogen The study
during
was conducted. wasstudy
conducted
manufacturing
The was
conducted ex-situ to simulate the exposure of a 4140 alloy to hydrogen during manufacturing
Metals 2017, 7, 466 17 of 18

ex-situ to simulate the exposure of a 4140 alloy to hydrogen during manufacturing followed by usage
in an ambient environment. From the data obtained in this study, the following conclusions can
be drawn:

1. Austempering in the lower bainitic temperature range has significantly increased the mechanical
properties and the fracture toughness of AISI 4140 steel as compared to the as-received
(annealed) condition.
2. In the absence of any charged hydrogen, the austempered samples had a much lower average
crack growth rate and higher fatigue threshold than the as-received (annealed) samples.
3. The presence of dissolved hydrogen increased the average crack growth rate in the austempered
as well as in the as-received (annealed) samples.
√
4. There is a transition stress intensity factor value of approximately 40–50 MPa m; below this
value, the presence of dissolved hydrogen causes the crack growth rate to be higher in the
austempered samples when compared to annealed samples.
5. In presence of dissolved hydrogen, above the transition stress intensity factor value, the crack
growth rate was increasingly greater in the annealed specimens as compared to the austempered
specimens.
6. When compared to the as-received (annealed) condition, austempering of 4140 steel appears to
provide a processing route by which the strength, hardness, and fracture toughness of the material
can be increased with little or no degradation in the ductility and fatigue crack growth behavior.

The results from this study also highlight the need for three future investigations. First, it is
recommended that a study be conducted to better define the effect of austempering temperature on the
fatigue crack growth resistance. This study would also need to more closely characterize crack closure
effects and the effects of microstructural grains on the rate of crack propagation. Second, a study
examining the effect of hydrogen concentration on the fatigue crack growth resistance in austempered
4140 should be conducted. This study should include hydrogen content measurements before and after
the fatigue test in order to understand the effect of hydrogen diffusion, ingress, and outgassing during
the testing process. Third, the study needs to be repeated for a quenched and tempered 4140 steel
alloy that was exposed to hydrogen charging like that done in the current study. This will allow for
an evaluation of the degree of commercial improvement yielded by austempering compared to the
current commonly used heat treatment process.

Author Contributions: This research study was performed in fulfillment of a PhD Thesis by Varun Ramasagara
Nagarajan. Susil K. Putatunda and Varun Ramasagara Nagarajan conceived and designed the experiments;
James Boileau provided the material for this study; Varun Ramasagara Nagarajan performed the experiments;
Varun Ramasagara Nagarajan, Susil K. Putatunda and James Boileau analyzed the data and wrote the paper.
Conflicts of Interest: The authors declare no conflict of interest.

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