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SERGIY KALNAUS, JIXI ZHANG, and YANYAO JIANG
Stress corrosion cracking of the high-strength martensitic steel AISI 4340 (yield
stress = 1503 MPa) in NaCl aqueous solutions of different concentrations was studied exper-
imentally using compact tension specimens in free corroding conditions. The experiments were
conducted under the controls of constant load, constant crack opening displacement (COD),
constant loading rate, and constant COD rate. Despite the differences in controlling conditions,
the experiments yielded similar results for the threshold stress intensity factor and the plateau
velocity in the 3.5 wt pct NaCl solution. Dependence of the plateau velocity on the NaCl
concentration was observed, whereas the values of the threshold stress intensity factors seem to
be independent of the NaCl concentration in distilled water.
DOI: 10.1007/s11661-010-0335-y
The Minerals, Metals & Materials Society and ASM International 2010
1000
1500
Engineering Stress, MPa
1000 600
400
500
200
AISI 4340 AISI 4340
Monotonic Tension Monotonic Torsion
0 0
0.00 0.10 0.20 0.30 0.00 0.10 0.20 0.30 0.40
Engineering Strain γ, Shear Strain
(a) (b)
Fig. 1—Stress–strain curves obtained from experiments for (a) monotonic tension and (b) monotonic torsion.
12.7 mm, and the diameter was 8.0 mm. The stress– R20.64
strain curve obtained from the monotonic tension test is P
Ø8.0
shown in Figure 1(a). Another smooth dog-bone-shaped
specimen was subjected to pure monotonic torsion
loading. The gage length was 25.4 mm, and the diameter
within the gage length was 12.0 mm. The surface strain
was measured by using an extensometer with 3 pct shear
strain range. The extensometer was removed from the
specimen after the surface strain reached its range. The 10.0 17.0
surface shear strain greater than 3 pct was determined by an
the measuring rotational angle of the actuator through a a
relationship between the surface shear strain and the
rotational angle established before the removal of the
extensometer from the specimen. The surface shear stress
was determined following Nadai’s formula.[63] The shear P
stress–shear strain curve obtained from monotonic
torsion is shown in Figure 1(b). All static material W=30.95
properties of the 4340 steel are listed in Table II. It is 39.64
noticed that the monotonic torsion experiment is advan-
tageous to monotonic tension because it eliminates the Thickness=3.8
process of necking and enables the true fracture stress
and strain of the material to be obtained. Fig. 2—CT specimen used in the SCC experiments (all dimensions
Round CT specimens, as shown in Figure 2, were are in millimeters).
machined from commercially obtained 4340 steel round
bar with a diameter of 44.44 mm in the transversal specimens was 3.8 mm. Notches were cut using the
direction (circumferential orientation[21]). The heat- electrodischarge machine process to eliminate cold work
treatment procedure described previously was done to associated with the traditional saw cutting and drilling.
the specimens prior to testing. The thickness of the One side of the specimens was polished to facilitate the
KISCC (MPa m )
This section describes the experimentally obtained
1/2
15
results of the SCC growth of the 4340 steel. The section
is arranged into subsections with an emphasis on a 10
particular phenomenon being investigated. The presen-
3.5wt% NaCl Aqueous Solution
tation of the crack growth curves is made after the 5
COD Rate Control
accepted format of the crack growth rate vs the stress Load Rate Control
intensity factor on a log-log scale. The stress intensity 0
factor was calculated using the following formula[64] for 2 4 6 8
0.001
2 4 6 8
0.01
2 4 6 8
0.1
2
(da/dt)avg, (mm/s)
>
>
: FðaÞ ¼ 4
ð1 aÞ3=2 2
0.001
½1
3.5wt% NaCl Aqueous Solution
4
where a is the crack length measured from the line 2 COD Rate Control
Load Rate Control
of externally applied load P and W and B are the 0.0001
width and the thickness of the specimen, respectively -5
2 3 4 5 6 7 8
-4
2 3 4 5 6 7 8
-3
10 10 10
(Figure 2). Equation [1] was obtained by the boundary dδ/dt (mm/s)
collocation method and has an accuracy of 0.3 pct when
(b)
0.2 £ a £ 1.0.[64]
The primary data collected as a result of the exper-
Fig. 5—Effect of loading rate on (a) threshold stress intensity KISCC
iment were the crack length and the elapsed time. A and (b) average plateau crack growth velocity.
parabolic curve was adopted to best fit a set of seven
successive data points in the experimentally obtained
relationship between the crack length and the time. The
K, Stress Intensity Factor(MPa m )
50 2X10
-5
-4
40 10
-4
2X10
30
A. Effect of Loading Rate
20
The effect of the loading rate on SCC for the 4340
steel was investigated in 3.5 pct NaCl aqueous solution. 10
COD (mm)
0.20 2.0
Load (kN)
0.15 1.5 2
crack growth curve within one experiment. Figure 7 K, Stress Intensity Factor, MPa m
shows the variation of the applied load and the
corresponding COD as a function of time in a load Fig. 8—SCC experiments in aqueous NaCl solution of different con-
centrations.
rate-controlled experiment. The experiment was per-
formed at a constant loading rate (linearly increasing
load) of dP/dt = 0.1 N/s and produced a complete crack
growth curve for the material. It is shown in Figure 7 values of the stress intensity factor and the near-
that although the load is changing linearly with time, the threshold crack growth. At the same time, it is shown
COD-vs-time relationship is similar to a parabolic curve. that an addition of NaCl to the solution slows the
Therefore, to obtain the results corresponding to a plateau crack growth as observed earlier.[22,62] The
constant loading rate experiment, the COD rate should highest values of da/dt are reached in pure distilled
not be constant. water. With the addition of sodium and chloride ions,
the crack growth rate within the plateau region
decreases. It should be noticed that the crack growth
B. Effect of NaCl Concentration rate curve in pure water is distinguishable from the SCC
Nine different concentrations of sodium chloride growth curves in saline solutions by the absence of the
(NaCl) in water solution were used in the current pronounced plateau in stage II. In other words, the
investigation. The NaCl concentration ranged from velocity of crack extension in pure water is dependent on
0 pct (distilled water) to 3.5 pct (simulated seawater). the stress intensity in all three stages of crack growth.
The values of the threshold stress intensity factors were One particular phenomenon in regard to plateau
determined from the load rate-controlled experiments crack propagation velocity can be observed in Figure 8.
and correspond to a first observed crack extension of A decrease in the plateau crack growth rate does not
0.01 mm from the crack tip formed by fatigue precrack- occur continuously with an increasing NaCl concentra-
ing prior to the SCC test. All results for the effect of tion. Two groups of crack growth curves, one corre-
NaCl concentration are shown in Figure 8. Experiments sponding to the NaCl concentration lower than
were conducted with constant load, constant COD, and 0.011 pct and one with the NaCl concentrations higher
constant load rate controls. All experiments were than 0.011 pct can be distinguished in Figure 8. A
performed at free potential and at room temperature further illustration of this phenomenon is shown in
without aeration. Figure 9, which depicts the average plateau velocity of
The crack growth results in Figure 8 display typical crack growth as a function of the NaCl concentration. It
SCC behavior with the crack growth curve consisting of is shown in Figure 9 that the NaCl concentration of
three stages, as depicted schematically in the insert in 0.011 pct can be viewed as a ‘‘critical concentration’’
Figure 4. Stage I is the near threshold (subcritical) crack that separates two groups of crack growth curves
growth where the velocity of crack propagation strongly (dashed vertical line in Figure 9). The first group with
depends on the stress intensity factor K . Stage II often is NaCl concentrations lower than the critical number
called a plateau crack growth, and within this range, the behaves close to the SCC in pure water. If the NaCl
rate of crack extension is nearly independent of K. content is increased by 1.5 9 103 wt pct, then the
Finally, the third stage represents the catastrophic plateau velocity decreases to the values characteristic for
failure of the specimen and is not represented in the SCC in the 3.5 pct saline solution.
Figure 8 because most specimens in the current inves- Figure 10 is a plot of KISCC vs the NaCl concentration
tigation were not loaded until complete separation. in the distilled water solution. As was stated earlier, the
It is shown in Figure 8 that the change in the NaCl NaCl concentration has no practical influence on the
concentration has practically no effect on the threshold threshold stress intensity factor. The KISCC values are
0.001
-5 -4 -3 -2 -1 0
10 10 10 10 10 10
NaCl Concentration (wt%)
Fig. 11—SEM photograph illustrating intergranular SCC in AISI
Fig. 9—Average plateau crack growth velocity as function of NaCl 4340 steel.
concentration.
20
1/2
15
KISCC, MPa m
10
Distilled Water
5
0
-5 -4 -3 -2 -1 0
10 10 10 10 10 10
NaCl Concentration (wt%)
Fig. 12—Photograph of a propagating SCC crack (specimen HT-43,
Fig. 10—Dependence of KISCC on NaCl concentration. dP/dt = 0.1 N/s).
pffiffiffiffi
confined within the range of 9:4 13:0 MPa m; as dependent on the segregation of impurities, which
indicated by the dashed lines in Figure 10. The KISCC serves as hydrogen-trapping sites, along the grain
distribution has no correlation with the NaCl concen-
pffiffiffiffi boundaries.[15] At the same time, experimental observa-
tration. The average KISCC value was 11:07 MPa m tions point to a connection between hydrogen-induced
(thick blue line in Figure 10). cracking and plastic deformation by slip on the {110}
planes.[4,15] Such a deformation mechanism leads to
transgranular cracking induced by a local process of
C. Microscopic Observations and Crack Morphology plastic strain as a result of the motion of dislocations.
An examination of the fracture surfaces under the Both mechanisms can be activated during the SCC, and
scanning electron microscope (SEM) revealed the inter- the final fracture mode depends on the hydrogen
granular cracking mechanism typical for heat-treated distribution among the trapping sites.
4340 steel[65,66] in all specimens subjected to environ- In the current investigation, in situ observation of the
mentally assisted cracking (Figure 11). The mechanism SCC crack extension through the optical microscope
is not influenced by the loading rate or the NaCl allowed for the acquisition of rather peculiar cracking
concentration and no significant differences were behavior of AISI 4340. Figure 12 shows the photograph
observed in fracture morphologies of the specimens of a growing SCC crack captured with the CCD camera
tested under different loading conditions. attached to the microscope. It is shown that the crack
It has been generally accepted that the yield strength propagation consists of several small steps (‘‘cells’’) in
influences the threshold value of the stress corrosion which the crack is separated in two branches that later
and hydrogen-assisted cracking,[4,7,25,62] whereas the tend to merge together. Although the overall plateau
plateau velocity is not significantly dependent on the velocity remains constant, the crack propagation is
strength of an alloy.[25] The particular microstructural slower when the new ‘‘cell’’ is being formed by crack
cracking mechanism, however, is a function of a rate- deviation in two branches. Once the ‘‘cell’’ has started to
limiting process (i.e., anodic dissolution or hydrogen form, the crack extension becomes faster until the
embrittlement). For hydrogen-assisted cracking, the branches come together, and the new step is starting to
transgranular or intergranular path of a crack is emerge. The schematic representation of the crack
0.001
8
6
4
0.0001 8 9 2 3 4 5 6 7 8 9
10 100
1/2
K, Stress Intensity Factor, MPa m
4 -2 Present Work
KISCC, MPa m
10
2 -3
10
-4
10 10
8
6 -5
10
1000 1200 1400 1600 1800 2000
-6
σy, Yield Stress, MPa 10
1000 1200 1400 1600 1800
σy, Yield Stress, MPa
Fig. 15—KISCC as a function of yield stress for AISI 4340 steel.
Fig. 16—Plateau velocity as a function of yield stress for AISI 4340
steel.
pffiffiffiffi
showed values
pffiffiffiffi of KISCC ranging from 23:3 MPa m to
26:8 MPa m: Experiments conducted by the researchers
employing the WOL and CTpspecimensffiffiffiffi later yielded the precracking is done with a low Kmax and crack growth is
range of K ffiffiffiffi from 9:7 MPa m[74]
pISCC (ry = 1682 MPa)[73] to observed directly at a microscopic level (Table AI).
116 MPa m (ry = 985 MPa). Resent research by Previous investigations on 4340 steel with yield strength
Raman et al.[75,76] using circumferential notch tensile ry = 1654 MPa,[66] however, demonstrated the exis-
(CNT) specimens as a substitute for traditional p CT
ffiffiffiffi tence of rather prolonged incubation times (from
geometry produced values of KISCC close to 15 MPa m 11 minutes to 3000 minutes) even when the fatigue
(ry ¼ 1470 MPa). In the current work, the average value precracking was done with maximum stress intensities
of KISCC for AISI 4340 with pffiffiffiffiry = 1503 MPa was lower than the initial values of K in stress corrosion
determined to bep11:07 ffiffiffiffi MPa m; which is close to cracking. The difference most likely can be explained by
KISCC ¼ 11:9 MPa m determined by Hirose et al. for different definitions of the incubation time concept.
the AISI 4340 steel with the yield stress equal to Although in the current investigation, the incubation
1530 MPa.[46] The values of threshold stress intensity time is defined as a time required for a crack to extend
and plateau crack growth velocity available from the by 0.01 mm, the incubation time in Reference 66 was
research results reported in the literature are arranged in treated as time when the crack growth rate reaches the
Table AVI. In addition to yield stress values, the plateau regime.
controlling conditions during the experiment and the The constant COD experiments used for the threshold
specimen types are specified in Table AVI. The values of intensity factor determination can take a very long time
threshold stress intensity factors obtained in the current (up to 7000 hours) when the low initial values of K are
investigation are compared with the data from the applied.[20] Therefore, efforts were directed toward
literature in Figure 15. The results taken from the developing techniques to accelerate the determination
literature are represented by open circles, and the results of the threshold.[52–55] Three fracture-mechanics-based
of the current experiments are shown with filled mark- testing approaches (constant load, constant displace-
ers. The solid line represents the reference exponential fit ment, and constant displacement rate) were applied and
of the data, and the dashed lines show the 100 pct compared by Dietzel et al.[56] in the experiments on 2024
spread from the reference line. A significant amount of aluminum alloy. The resulted values of KISCC and the
scatter can be observed in Figure 15 and a rather large plateau crack growth velocities were very similar in all
variation is noted in KISCC values for an identical yield three applied testing techniques.[56] The applicability of
stress. An overall tendency of decreasing threshold rising COD control to the SCC experiments was
stress intensity with increase in ry can be observed despite investigated further with other metallic materials includ-
the scatter. It is shown that the data obtained in the ing AISI 4340,[16,27,54,57,58] and the results confirmed
current investigation fall within the scattering band in that the experiments with faster constant displacement
Figure 15. rates can be used in place of time-consuming constant
The average plateau velocity as a function of the yield load tests. It should be mentioned that the degree of
stress is shown in Figure 16 for the 4340 steel. The influence of the loading rate on the threshold stress
detailed values of the plateau velocities are listed in intensity, however, depends on the manufacturing pro-
Table AVI under the column Vavg. The open circles cess applied to the material. Research on Ti alloys[77,78]
represent the results from the literature, and the solid demonstrated that within the same range of dK/dt, age-
markers are the results obtained from the current study. hardened and cold-worked materials exhibit different
It is clear that, as a general tendency, a higher yield behavior of KISCC as a function of loading rate.
stress results in a higher plateau velocity. In the current investigation, independence of both the
In addition to the threshold values, the constant load threshold stress intensity factor and the plateau velocity
experiments provide information in regard to the crack of AISI 4340 of the testing technique was confirmed
incubation time. In the current investigation, the exper- with the experiments in the 3.5 wt pct NaCl solution.
iments under constant load control revealed that the It was observed, however, that the linearly increas-
incubation time is practically zero when K > KISCC if ing COD-controlled experiments may not provide a
Crack Initiation
possible physical explanation. 10
Although the plateau velocity depends on the chloride
concentration, the intergranular fracture mechanism
5
was observed to be independent of both the NaCl
content and the loading mode. It is known that the high- 0 2000 4000 6000 8000
strength steels are susceptible to hydrogen-assisted Time, sec
cracking.[6–10,15,80] The following possible mechanisms
of hydrogen embrittlement have been suggested: the Fig. 17—Crack length measured during the experiment and obtained
influence of hydrogen on crack-tip plasticity and grain from Eq. [2].
V. CONCLUSIONS
Based on the experimental results of the SCC exper-
iments on the AISI 4340 steel (yield stress = 1503 ACKNOWLEDGMENTS
MPa), the following conclusions can be drawn:
The work was supported financially by the Office of
1. KISCC and the plateau velocity are not significantly Naval Research (N00014-08-1-0646). The authors
influenced by the loading rate. gratefully acknowledge the inspiring suggestions made
2. Stage I crack growth can be obtained only when by Dr. Asuri K. Vasudevan in the course of the
the loading rate is low. research.
3. Constant COD rate control does not provide an
avenue for the experimental determination of a
complete stress corrosion (da/dt K) curve. APPENDIX
4. For 4340 steel, a load-control experiment can pro-
vide reasonable stress corrosion results. Tables AI through AVI
Spec. Number NaCl Pct Step Number P kN Kpr MPa m1/2 Kin MPa m1/2 Kf MPa m1/2 ai mm af mm tinc s
HT-24 0 — 3.40 25.70 25.70 90.80 8.004 19.846 203
HT-26 0 — 3.00 25.80 22.80 76.13 8.006 19.473 631
HT-36 3.5 1 2.80 4.91 18.00 19.90 6.276 7.338 180
HT-27 3.5 1 1.80 5.48 15.00 15.70 9.140 10.153 83
3 1.00 — 14.20 61.13 14.562 24.277 —
HT-33 0 1 2.97 5.22 20.00 22.70 6.807 7.818 127
3 0.80 — 14.80 72.60 16.952 25.700 —
HT-34 0.35 1 2.36 5.48 18.00 19.00 7.996 8.559 246
3 1.10 — 16.80 59.27 15.187 23.755 —
HT-40 0.0035 1 2.25 5.98 14.20 15.08 6.245 6.826 159
3 1.00 — 12.60 58.77 13.405 24.125 —
HT-39 0.0105 1 2.20 5.25 13.60 21.37 6.064 10.154 171
3 1.10 — 24.80 42.90 18.621 22.163 —
ABBREVIATIONS: P – Applied load; Kpr – Maximum stress intensity factor at the end of fatigue precracking; Kin – Stress intensity factor at the
beginning of the experiment; Kf – Stress intensity factor at the termination of the experiment; ai – Crack length at the beginning of the experiment
measured from the line of applied load; af – Crack length at the termination of the experiment measured from the line of applied load; tinc – Crack
incubation time based on 0.5 mm crack length.
Spec. Number NaCl Pct Step Number d mm Kin MPa m1/2 Kf MPa m1/2 ai mm af mm
HT-27 3.5 2 0.042 15.70 11.80 10.153 14.325
HT-33 0 2 0.062 23.90 13.40 7.994 16.953
HT-34 0.35 2 0.070 18.33 12.39 8.586 15.188
HT-40 0.0035 2 0.051 16.93 11.12 7.223 13.267
HT-39 0.0105 2 0.063 21.38 11.83 10.155 18.517
HT-37 0.015 2 0.240 39.17 17.29 18.881 28.138
ABBREVIATION: d – Displacement of the notch flanks at the edge of the specimen (COD displacement).
Spec. Number NaCl Pct Step Number D mm Kpr MPa m1/2 Kin MPa m1/2 Kf MPa m1/2 ai mm af mm tinc s
HT-29 0 — 0.191 26.2 26.20 14.58 8.048 28.557 245
HT-30 3.5 — 0.141 19.75 21.60 13.50 8.000 26.753 265
HT-31 3.5 — 0.122 19.82 18.05 14.96 8.009 27.659 288
HT-28 3.5 5 0.121 — 17.44 11.85 9.715 26.272 —
HT-36 3.5 2 0.150 — 16.02 12.30 8.041 25.231 —
ABBREVIATION: D – Displacement of the actuator at the point of load application.
Spec. Number NaCl Pct dd/dt mm/s Kpr MPa m1/2 Kin MPa m1/2 Kf MPa m1/2 ai mm af mm KISCC MPa m1/2
HT-45 3.5 1E-04 4.90 6.97 51.49 5.9245 14.009 9.96
HT-48 3.5 2E-05 4.36 4.37 19.56 6.0055 18.2445 12.06
HT-49 3.5 2E-04 3.56 1.94 53.94 6.4110 7.6110 12.91
HT-50 3.5 1E-05 4.49 4.49 13.89 6.321 16.244 11.54
ABBREVIATION: dd/dt – Rate of crack opening displacement.
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