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1 s2.0 S0264127520301064 Main
1 s2.0 S0264127520301064 Main
H I G H L I G H T S G R A P H I C A L A B S T R A C T
a r t i c l e i n f o a b s t r a c t
Article history: Hydrogen-induced cracking behavior in high-strength steel mainly composed of martensite was analyzed by
Received 27 November 2019 acoustic emission (AE) technique and finite element method (FEM) in slow strain-rate tensile (SSRT) tests and
Received in revised form 15 February 2020 welding tests. The crack initiation was detected by the AE signals, and the time evolution of stress concentration
Accepted 17 February 2020
and hydrogen diffusion were calculated by FEM. The effect of hardness and plastic strain on the hydrogen diffu-
Available online 19 February 2020
sion coefficient was explicitly introduced into the governing equation in FEM. The criterion and indicator param-
Keywords:
eter for the crack initiation were derived as a function of maximum principal stress and locally accumulated
Hydrogen embrittlement, high-strength steels hydrogen concentration. The results showed that the cracking criterion derived by AE and FEM is useful for
Welded joints predicting the cold cracking behavior and determining the critical preheat temperature to prevent hydrogen-
Acoustic emission induced cracking.
Finite element analysis © 2020 The Authors. Published by Elsevier Ltd. This is an open access article under the CC BY license (http://
creativecommons.org/licenses/by/4.0/).
1. Introduction can occur in the welded part due to residual stress and hydrogen em-
brittlement after welding. Therefore, hydrogen embrittlement is one
In recent years, the demand for high-strength steels is increasing to of the environmental embrittlement caused by the interaction of hydro-
reduce the weight of steel structures and transportation equipment gen content, residual stress, and microstructure. Since hydrogen-
from the viewpoint of environmental issues such as global warming. induced crack generally occurs at a low temperature, below approxi-
Application of high-strength steels in structures often requires welding mately 100 °C [1], it is also called “cold cracking” to distinguish from a
process. A significant drawback of high-strength steels is that cracking solidification crack or a grain boundary liquation cracking at a high tem-
perature. It is well known that high-strength steels are more susceptible
⁎ Corresponding author. to hydrogen embrittlement than lower strength steels because disloca-
E-mail address: shiraiwa@rme.mm.t.u-tokyo.ac.jp (T. Shiraiwa). tions in martensite act as hydrogen trap sites [2–6]. Since cracks are the
https://doi.org/10.1016/j.matdes.2020.108573
0264-1275/© 2020 The Authors. Published by Elsevier Ltd. This is an open access article under the CC BY license (http://creativecommons.org/licenses/by/4.0/).
2 T. Shiraiwa et al. / Materials and Design 190 (2020) 108573
Table 1
Chemical compositions of base metal and weld metals (mass%, B, N, O: ppm).
C Si Mn P S Cu Ni Cr Mo Nb V Ti Al B N O
Base metal 0.12 0.12 0.93 0.001 0.002 0.25 2.00 0.60 0.60 0.016 0.050 0.001 0.065 10 25 14
LB-116 0.08 0.63 1.5 0.001 0.006 – 1.83 0.28 0.43 – – – – – – –
LB-80UL 0.05 0.56 1.37 0.009 0.005 – 2.77 – 0.76 – – – – – – –
MG-80 0.08 0.38 1.25 0.009 0.011 – 2.22 – 0.63 – – – – – – –
most severe defects in a welded joint, numerous researches have been Experimental measurements on hydrogen embrittlement of welded
conducted to clarify the cracking mechanism and attempt to develop joints include (1) residual stress measurement, (2) diffusible hydrogen
techniques for preventing hydrogen-induced cracking. Various models content measurement, and (3) observation of cracking behavior. The re-
explain the mechanism of hydrogen embrittlement: lattice embrittle- sidual stress distribution can be obtained by mechanical cutting (stress
ment theory [7], hydrogen-enhanced localized plasticity (HELP) mech- release method), X-ray diffraction, and neutron diffraction. Among
anism [8,9] and hydrogen-enhanced strain-induced vacancy (HESIV) them, the neutron diffraction technique allows the mapping of the in-
mechanism [10]. However, due to the complexity of the phenomenon, ternal stress state [20]. The measurement results are consistent with
a unified physical model for a wide range of materials and environments the results of finite element analysis [21,22]. For the diffusible hydrogen
has not yet been established and is still actively discussed. concentration, the total amount of diffusible hydrogen can be measured
Currently, the practical technique to prevent hydrogen-induced by thermal desorption spectroscopy (TDS) analysis. Recently, it has
cracking in welded joints is preheating. By preheating steel plates before been reported that the type of trap sites can be estimated by performing
welding, hydrogen diffusion is promoted during the welding, and the TDS analysis from a low temperature of approximately 70 K and sepa-
locally accumulated diffusible hydrogen is reduced. However, excessive rating the TDS curve into several peaks by the Gaussian distributions
preheating is not preferable from the viewpoint of production cost and [23–25]. At the mesoscopic scale, it has become possible to obtain
undesirable effects on the microstructure. Therefore, it is required to es- localized hydrogen concentration by secondary ion mass spectroscopy
timate the minimum preheat temperature necessary to prevent (SIMS) [26]. For the cracking behavior, the crack paths are observed
hydrogen-induced cracking. Chart methods using carbon equivalents on the cross-sections after welding in almost cases. However,
(Pcm and CEN) and empirical formulas of restraint intensity have been hydrogen-induced cracking is a phenomenon that occurs in a non-
used to determine the critical preheat temperature [11,12]. The chart static state. In order to derive a fracture criterion, it is necessary to cap-
methods are completely based on the empirical results by y-groove ture the crack initiation and propagation together with time evolution
weld cracking tests, and the prediction accuracy and the application of stress concentration and hydrogen diffusion. Acoustic emission (AE)
range of the joint design are limited. Inaccurate predictions may require method is one of the non-destructive evaluation (NDE) techniques
excessively safe designs and increase manufacturing costs. In order to that provide in-situ monitoring of deformation and fracture phenomena
more precisely predict the critical preheat temperature regardless of [27]. There are several attempts to apply the AE method to detect
the loading condition or joint shape, it is essential to derive the critical hydrogen-induced cracking in tensile specimens [28,29] and welded
condition of cracking. It has been proposed to conduct slow strain-rate joints [30–32]. In the previous studies, it has been confirmed that
tensile (SSRT) tests using various hydrogen-charged specimens and ob- hydrogen-induced cracking of weldments can be detected using AE
tain the fracture criterion as a function of maximum principal stress and method [30]. The crack initiation time in the welded joints was esti-
amount of diffusible hydrogen accumulated in the hydrostatic stress mated by AE signal [31]. It was also proposed to determine the occur-
field [13,14]. Basically, it is expected that the prediction of hydrogen- rence of hydrogen-induced cracking from the shape of the cumulative
induced cracking behavior can be realized by calculating the maximum AE energy curve [32]. However, there is a lack of quantitative discussion
principal stress and hydrogen concentration distribution by finite ele- on the relationship between the crack initiation time, hydrogen concen-
ment method (FEM) and substituting them into the fracture criterion. tration and stress distribution. To validate the prediction of hydrogen-
In the specimen scale, the hydrogen susceptibility behavior during the induced cracking using fracture criteria, it is necessary to systematically
crack growth test was well reproduced by combining the stress field investigate the time evolution of stress, hydrogen and cracking behavior
analysis and the hydrogen diffusion analysis [15–18]. More recently, after welding under various welding conditions.
the behavior of cold cracking in welded joints could be explained qual- The empirical methods for determining the preheat temperature,
itatively by using two extreme boundary conditions in FEM [19]. In such as the chart methods, are not accurate with a limited number of ex-
order to achieve quantitative predictions with a broader range of mate- periments and are difficult to apply to various joint types. Hence, the
rials and welded joints, experimental measurements are required to ob- present study aims to examine the combination of the AE method and
tain a fracture criterion and validate the method. numerical analysis of the stress-strain field and hydrogen concentration
Fig. 1. (a) Dimensions (in mm) of circumferentially notched round bar specimen for slow strain rate tensile (SSRT) test, and (b) experimental photo of SSRT test with AE measurement. The
notch root radius (r) and depth (d) is 0.25 mm and 1 mm, respectively.
T. Shiraiwa et al. / Materials and Design 190 (2020) 108573 3
Table 2 are measured in oblique y-groove weld cracking tests. The time evolu-
Conditions of heat treatment and hydrogen charging, and diffusible hydrogen concentra- tions of the stress field and hydrogen concentration field in complex-
tion in SSRT specimen.
shaped specimens are calculated by FEM. By changing the initial hydro-
Specimen Cooling Current Diffusible hydrogen gen content and preheat temperature in the y-groove weld cracking
number rate/°C/s density/A/m2 concentration / tests, the validity of the hydrogen cracking criterion derived by the AE
ppm
method is examined.
S1 1 0.05 0.06
S2 0.10 0.11
2. Material and experimental procedure
S3 0.50 0.55
S4 30 0.05 0.08
S5 0.10 0.16 2.1. Materials and SSRT specimens
S6 0.50 0.82
Chemical compositions of materials used in SSRT tests and y-groove
weld cracking tests are shown in Table 1. The chemical composition of
field as a tool to estimate the critical condition for hydrogen-induced the base material was determined with reference to HT980 high tensile
cracking of high-strength steels. Although the criterion for hydrogen- strength steel [33]. Blocks with a dimension of 12 mm × 13 mm × 120 mm
induced cracking is usually derived using the maximum stress during were cut out from 35 mm thick plate of the base metal. To simulate the
the SSRT test, it is desirable to use the stress at the crack initiation to en- thermal process in the heat-affected zone in the y-groove welded joint
sure reliability. The crack formation in the SSRT tests is detected by the described later, heat treatments were performed on the block pieces
AE method. Finite element analysis is performed to calculate stress with a high-frequency induction heating device. The high frequency in-
distribution and hydrogen concentration distribution, and derive the duction heating method applies high frequent magnetic field (around
formation criterion of hydrogen-induced cracking. Also, the AE signals 10 kHz) and heats up the specimen by causing eddy current. In this
Fig. 2. (a) Dimension (in mm) of y-groove weld cracking test joint, and (b) experimental photo of AE measurement.
4 T. Shiraiwa et al. / Materials and Design 190 (2020) 108573
Table 3
Welding conditions in y-groove cracking tests. In the AE measurement column, “o” indicates that AE measurement was performed.
work, we used the induction heating device of Fuji Electric Industrial Co. The conditions of heat treatment and hydrogen charging are summa-
Ltd. The block pieces were heated up to a maximum temperature of rized in Table 2. In total, six SSRT specimens were prepared with two
1400 °C at a heating rate of 50 °C/s and held for 5 s, then cooled at con- heat treatment conditions and three hydrogen charging conditions. To
trolled cooling rates. The cooling rate between the maximum tempera- measure the diffusible hydrogen content (HD) by TDS analysis, the
ture and 1000 °C was fixed to 50 °C/s, and two cooling rates of 30 °C/s hydrogen-charged specimens without zinc electroplating were also
and 1 °C/s were assigned between 1000 °C to 250 °C. The cooling rate prepared under the conditions of S3 and S6 in Table 2. In the TDS anal-
30 °C/s was selected because the microstructure of the specimen is con- ysis, the specimens were heated in an argon atmosphere at a heating
sidered similar to that of the heat-affected zone (HAZ) of the y groove rate of 100 °C/h, and the hydrogen released from room temperature to
weld cracking test. The cooling rate 1 °C/s was selected to change the 400 °C was measured by a gas chromatograph (JTF-20A, J-Science lab).
microstructure and to investigate its effect. After the heat treatments,
the blocks were machined to cylindrical specimens with a circumferen- 2.2. Acoustic emission (AE) measurement in slow strain rate tensile (SSRT)
tial notch. The dimension of the specimen was determined from the lit- tests
erature [34], as shown in Fig. 1(a).
Hydrogen charging was conducted by cathodic electrolysis with 3% The SSRT tests were conducted with AE measurements to detect
NaCl +3 g/l NH4SCN at room temperature for 24 h. The current density crack initiation. After roughening both ends of the specimen with
was assigned to 0.05, 0.1, and 0.5 A/m2. Following the hydrogen emery paper, two AE sensors (M304A, Fuji ceramics) were fixed on
charging, zinc electroplating was performed on the specimens to pre- both ends using cyanoacrylate-based adhesive (Aron Alpha, Toagosei)
vent hydrogen desorption from the surface. The thickness of zinc as shown in Fig. 1(b). The resonance frequency of the AE sensor was
electroplating is estimated to be 10 μm. Suzuki et al. kept the specimens 300 kHz. The specimen was clamped with wedge grips at a length of ap-
of 8 and 16 μm zinc electroplating in the atmosphere for 5 months and proximately 20 mm on both ends. The SSRT tests were conducted at a
investigated the hydrogen content [35]. From their results, we consider displacement rate of 5.0 × 10−3 mm/min at room temperature by uni-
the present zinc thickness is sufficient for the present purpose. After the versal testing machines (AG-5000C and AG-100kNX, Shimadzu). During
zinc electroplating, the specimens were kept at room temperature for the SSRT tests, the AE signals were amplified by approximately 55 dB
24 h to homogenize the hydrogen distribution inside the specimen. through a preamplifier (A1001, Fuji ceramics) and recorded by
Fig. 3. Flowchart of finite element simulations for (a) SSRT test and (b) y-groove weld cracking test.
T. Shiraiwa et al. / Materials and Design 190 (2020) 108573 5
Fig. 4. Finite element models and boundary conditions for (a) SSRT and (b) y-groove welding simulations.
continuous wave memory (CWM) system, which continuously records 3. Numerical method
the whole AE waveforms at a sampling rate of 10 MHz [36]. A high pass
filter of 100 kHz was applied to reduce the noise due to mechanical vi- 3.1. Governing equation of hydrogen diffusion
bration, and the AE events were detected by the threshold level of 40 dB.
Also, to exclude the noise from the outside of the specimen, one- In order to calculate local stress and locally accumulated hydrogen
dimensional AE source location was performed with the sound velocity content, elastic-plastic analysis, and hydrogen diffusion analysis were
of 5900 m/s, and the AE events within ±10 mm from the center of the performed by FEM. Assuming that the driving force for hydrogen diffu-
specimen were extracted. In the AE location analysis, the arrival time sion is the gradient of the chemical potential (μ), the flux of hydrogen
of the AE signal was defined by two-step Akaike's information criterion concentration (J) is expressed by the following equation [41]:
(AIC) [37]. After the SSRT tests, the fracture surfaces were observed with
a scanning electron microscope (SEM, JCM-6000, JEOL). Dc∂μ
J¼− ð1Þ
RT ∂x
2.3. AE measurement in y-groove weld cracking test where D is a hydrogen diffusion coefficient, c is hydrogen concentration,
R is the gas constant (8.3142 J/mol), and T is absolute temperature. The
The y-groove weld cracking test is widely used to investigate the chemical potential is defined by the following equation:
necessary preheat temperature to avoid cold cracking [38]. In this
μ ¼ μ 0 þ RT ln ϕ þ pV H ð2Þ
study, to examine the validity of the crack initiation criterion derived
from AE measurements during the SSRT tests, y-groove weld cracking
where μ0 is the standard chemical potential, ϕ is a normalized concen-
tests were conducted under various preheat temperatures and diffus-
tration of hydrogen (=c/s, s: solubility), p is hydrostatic stress (=
ible hydrogen contents induced by welding. The chemical compositions
of the base metal and the weld metal used in the experiment are shown − trace(σ)/3) and V H is a partial molar volume of hydrogen in iron-
in Table 1. The dimension of the y-grooved specimen is shown in Fig. 2 based alloys. Thus, the following equation is derived from Eqs. (1) and
(a). The restraints at both ends of the y-grooved specimen were pre- (2):
pared by conducting semi-automatic CO2 arc welding. Three types of ( )
weld metal (LB-116, LB-80UL, and MG-80) were used to change the ∂ϕ ∂ ln T ϕV H ∂p
J ¼ −sD þ ϕ lnϕ þ ð3Þ
amount of diffusible hydrogen introduced during welding. Also, the pre- ∂x ∂x RT ∂x
heat temperature was changed between 20 °C and 125 °C. The testing
atmosphere was kept at a temperature of 20 °C and humidity of 60%
RH. The welding conditions are listed in Table 3. The diffusible hydrogen
content of the weld metal under each condition was measured by a gas
chromatograph according to JIS Z3118 [39]. The measured hydrogen
contents are also listed in Table 3.
The temperature was measured at three locations on the specimen
using thermocouples. The temperature inside the weld metal was mea-
sured by a C-type thermocouple inserted into the weld metal during
welding. The AE measurements were performed under the conditions
indicated by “o” in Table 3. Two AE sensors (AE254SMH177, Fuji Ce-
ramics) were fixed on the side surface of the y-groove specimen using
magnets. The positions of the AE sensors and experimental photo are
shown in Fig. 2 (a) and (b), respectively. The AE signals were amplified
by 20 dB with a preamplifier (NF9913, NF Circuit Block) and recorded
with the CWM system. Since multiple wave modes can be detected in
the y-grooved specimen, the arrival time was determined by applying
the multi-step AIC picker [40]. Under the assumption that the AE events
occurred on the weld line, the one-dimensional AE source location was
carried out with a sound velocity of 5900 m/s. The AE measurement was
continued for 48 h from the end of welding. After the AE measurements,
cracks in the welded joint were observed on the five cross-sections Fig. 5. Stress-strain curves used in finite element simulation for SSRT test (CR: cooling
shown in Fig. 2(a). rate).
6 T. Shiraiwa et al. / Materials and Design 190 (2020) 108573
Fig. 6. Thermophysical and mechanical properties of base metal used in y-groove welding.
Fig. 7. Microstructure of base metal after heat treatment at cooling rate of (a) 30 °C/s and (b) 1 °C/s.
T. Shiraiwa et al. / Materials and Design 190 (2020) 108573 7
pffiffiffi
3440
s ¼ 0:00185 P exp − ð4Þ
T
828
D ¼ 0:20 exp − ð5Þ
T
Here, the units of s and D are atomic fraction and mm2/s, respec-
tively. P is the pressure of hydrogen gas, and its unit is atm. From
Fig. 8. Hydrogen desorption curves of hydrogen charged specimen with a current density
Eqs. (4) and (5),
of 0.5 A/m2 (CR: cooling rate).
pffiffiffi
4300
Ds ≈ 0:00037 P exp − ð6Þ
T to austenitic microstructures at temperatures higher than austenite
transformation temperature (Ac3). The details of Eq. (10) will be
The temperature dependence of Ds in Eq. (6) is exp(−4300/T), shown elsewhere [49]. To conduct numerical calculations by Abaqus,
which is in fairly good agreement with the experimental result of we selected the pressure of 1 N/mm2 as a reference pressure.
Kumnick and Johnson [45].
We would like to change the unit to [mass ppm] of hydrogen con- 21 4300
s¼ exp − ð11Þ
centration and [N/mm2] of pressure. Since hydrogen concentration is di- Dapp T
lute, when an atomic fraction of hydrogen is x, the hydrogen
concentration [mass ppm] is, The units of s in Eq. (11) is ppm·mm·N−1/2.
x x 106 3.2. Finite element analysis of slow strain rate testing (SSRT)
106 ≈ ð7Þ
x þ ð1−xÞ 55:845 55:845
The overview of the finite element simulation for the SSRT test is
Hence, depicted in Fig. 3(a). In the first step, an elastic-plastic analysis was per-
formed to calculate the distribution of maximum principal stress, equiv-
Ds ¼ 0:00037 alent plastic strain, and hydrostatic stress, which is the driving force for
pffiffiffiffiffiffiffiffiffi pffiffiffi
106 4300 4300 hydrogen diffusion. In the simulation, a two-dimensional axisymmetric
10P exp − ≈ 21 P exp − ð8Þ
55:845 T T finite element model near the notch of the SSRT specimen was used
(Fig. 4(a)). The stress-strain curves were obtained by tensile tests of
Eq. (8) is for the case without trapping sites. But, assuming that Ds smooth round bar specimens using a non-contact extensometer, and
does not depend on a type of site, the solubility for the case with trap- used in the simulation (Fig. 5). The top surface of the model was sub-
ping sites is calculated as follows: jected to tensile stress up to the experimentally obtained crack initiation
pffiffiffi stress (σAE) and maximum stress (σNB). The loading rate was
21 P expð−4300=T Þ
s¼ ð9Þ
Dapp
where Hv is Vickers hardness, and εp is an equivalent plastic strain. In Fig. 9. Stress-time curve and AE event location in SSRT test of hydrogen charged specimen
Eq. (10), Vickers hardness Hv is used as a representative of the micro- (CR = 30 °C/s, c = 0.11 ppm). The arrow represents the AE event corresponding to crack
structures. We would like to emphasize that Eq. (10) cannot be applied initiation.
8 T. Shiraiwa et al. / Materials and Design 190 (2020) 108573
using Sysweld and Abaqus. The overall flow of the simulation is shown
in Fig. 3(b). The series of calculations is divided into four steps: (i) heat-
transfer and phase-transformation analysis, (ii) elastic-plastic analysis,
(iii) calculation of hydrogen diffusion coefficient, and (iv) hydrogen dif-
fusion analysis. A two-dimensional finite element model composed of
three regions (base metal, heat-affected zone, and weld metal) was cre-
ated with four-node plane strain elements by Abaqus/CAE, as shown in
Fig. 4(b). The structured meshing method is adopted around the weld
root. The effect of element size on the stress field was investigated by
changing the minimum mesh size between 0.05 mm–0.9 mm. The re-
sults confirmed that the stress field can be calculated with sufficient ac-
curacy using the model with the minimum mesh size of 0.23 mm shown
in the figure. The thermophysical and mechanical properties of the base
metal and the three weld metals were derived from the chemical com-
positions using JMatPro. These properties were assigned to elements
belonging to each corresponding part of the finite element model
shown in Fig. 4. As an example, the properties of the base metal are
shown in Fig. 6. The properties of the other three types of welding ma-
Fig. 10. Notch tensile strength (σNB) and crack initiation stress detected by AE (σAE) as a
function of diffusible hydrogen content. terials were also derived by JMatPro. The continuous cooling transfor-
mation (CCT) diagrams calculated from JMatPro were imported into
Sysweld to take into account the phase transformation. In the heat-
determined so that the crack initiation time or the maximum load time transfer and phase-transformation analysis, a double ellipse heat input
coincided with the experimental results. The hydrogen diffusion coeffi- model [50] with a length of 16 mm, a width of 16 mm, a thickness of
cient (D) and solubility of hydrogen (s) in each element were then de- 4 mm, and conversion efficiency of 0.9 were utilized to reproduce tem-
termined by substituting room temperature of 293 K, experimentally perature distribution during welding. Using the results of temperature
obtained Vickers hardness and the equivalent plastic strain distribution history and phase transformation, the elastic-plastic analysis was then
obtained by the above finite element simulation into Eqs. (10) and (11). performed with Sysweld to calculate the residual stress. The boundary
In the hydrogen diffusion analysis, the boundary condition that the hy- conditions are shown in Fig. 4(b). The right edge of the model was
drogen does not release from the surface (dc/dx = 0) was assigned constrained by elastic support with an elastic modulus of 20.6 GPa.
since the surface of the specimen was coated with zinc electroplating The elastic modulus was determined by the plate thickness according
in the experiment. to the literature equation [51]. The hydrogen diffusion coefficient was
then calculated by Eqs. (10) and (11) based on the temperature field
3.3. Finite element analysis of y-groove weld cracking test and equivalent plastic strain distribution obtained in Sysweld for each
element and each time step. Since the hydrogen diffusion rate in austen-
To evaluate the distribution of stress, strain, and hydrogen content in ite is significantly lower than that in ferrite, the calculation of hydrogen
the y-groove weld cracking test, finite element analysis was performed diffusion started after the temperature dropped below 800 °C. In the
Fig. 11. Fracture surfaces of hydrogen charged specimens with different cooling rates (CR) and diffusible hydrogen contents (HD): (a) CR = 1 °C/s, HD = 0.06 ppm, (b) CR = 1 °C/s, HD =
0.55 ppm, (c) CR = 30 °C/s, HD = 0.08 ppm and (d) CR = 30 °C/s, HD = 0.82 ppm.
T. Shiraiwa et al. / Materials and Design 190 (2020) 108573 9
Fig. 12. Distribution of maximum principal stress at crack initiated stress and maximum stress in SSRT specimens of (a) CR = 1 °C/s and (b) CR = 30 °C/s.
initial state of hydrogen diffusion analysis, the diffusible hydrogen con- contained more trap sites such as dislocations, vacancies, and grain
centration measured according to JIS Z 3118 [39] was uniformly boundaries [52,53].
assigned to the weld metal under each condition. Finally, the time evo-
lution of stress and hydrogen distributions in the y-grooved specimen 4.2. Mechanical and AE behaviors during SSRT test
was obtained.
Examples of the stress-time curve and AE event location during the
SSRT test of the hydrogen-charged specimen are shown in Fig. 9.
4. Results and discussion High-amplitude AE events were detected in the vicinity of the circum-
ferential notch in the later stage of the SSRT test. The AE events with
4.1. Microstructure and hydrogen desorption small amplitudes were scattered around the center of the specimen,
which is probably due to cracks in the zinc coating layer. In the current
The microstructures of base metal after heat treatment at a cooling study, the first AE event with an amplitude exceeding 75 dB and loca-
rate (CR) of 30 °C/s and 1 °C/s are shown in Fig. 7. The microstructures tion within ±3 mm from the center of the specimen were considered
were mainly composed of martensite and bainite, and the prior austen- to be due to crack initiation. The example of the AE event determined
ite grain size was approximately 500 μm in both microstructures. The to be due to a crack initiation is indicated by the arrow in the figure,
Vickers hardness (Hv) measured at five points with 98 N (10 kgf) and the corresponding stress was defined as crack initiation stress
load. The average values were Hv 287 for CR = 1 °C/s, and Hv 380 for (σAE). The maximum load divided by the initial cross-sectional area at
CR = 30 °C/s, respectively. the circumferential notch is defined as the notch tensile strength
The hydrogen desorption curves of hydrogen-charged specimens (σNB). Also, testing time corresponding to σAE and σNB were recorded
with a current density of 0.5 A/m2 (S3 and S6 in Table 2) are shown in and utilized to define the loading rate in finite element simulation.
Fig. 8. A peak was observed around 360 K in both cases, which was con- The crack initiation stress and notch tensile strength in all specimens
sidered to be due to hydrogen trapped in dislocations and vacancies are plotted as a function of diffusible hydrogen content in Fig. 10. To
[24]. The total amount of hydrogen released from room temperature evaluate the overall trend, the notch tensile strength (σNB) of the SSRT
to 473 K (200 °C) was defined as diffusible hydrogen content in the tests without AE measurements were also plotted. The SSRT specimens
specimen. The diffusible hydrogen contents in the specimens other without AE measurement were prepared with no hydrogen charge and
than S3 and S6 were estimated by assuming a linear relationship be- charge current densities of 1, 2, and 4 A/m2 for each cooling rate. In the
tween the charge current density and the introduced hydrogen content. condition without hydrogen charge, the specimen with a cooling rate of
The measured and estimated diffusible hydrogen contents in the SSRT 30 °C/s showed higher notch strength. In the hydrogen-charged speci-
specimens are summarized in Table 2 of Section 2.1. Under the same mens, it was confirmed that both crack initiation stress and notch ten-
charge current conditions, the specimen with a cooling rate of 30 °C/s sile strength decreased with increasing the diffusible hydrogen
showed a higher hydrogen concentration than that with a cooling rate content. Under the conditions that the diffusible hydrogen content
of 1 °C/s. This suggests that specimens with higher cooling rates was lower than 0.2 ppm, no apparent decrease in strength was
Fig. 13. Distribution of diffusible hydrogen concentration at crack initiated stress and maximum stress in SSRT specimens of (a) CR = 1 °C/s and (b) CR = 30 °C/s.
10 T. Shiraiwa et al. / Materials and Design 190 (2020) 108573
observed. Overall, the crack initiation stress was slightly smaller than
the notch strength, and the difference was larger for the specimen
with a cooling rate of 30 °C/s than those with a cooling rate of 1 °C/s.
The fracture surface in the vicinity of the notch root was observed by
SEM, as shown in Fig. 11. A characteristic fracture surface was observed
in the specimen with large diffusible hydrogen content (Fig. 11(b) and
(d)). It seems to be a quasi-cleavage surface, which is one of the charac-
teristic fracture surfaces of hydrogen embrittlement [2]. In the
literature, observations using transmission electron microscopy (TEM)
have shown that hydrogen-induced cracks initiate from the boundaries
of lath, packet, and prior austenite grains [54]. On the other hand, dim-
ple patterns are observed throughout the fracture surface of the speci-
men with small diffusible hydrogen content (Fig. 11(a) and (c)). It is
considered that these specimens were less affected by hydrogen
Fig. 14. Limit curves based on locally accumulated hydrogen concentration and local
embrittlement. maximum principal stress.
Fig. 15. (a) Cross-sectional observation and (b) hardness distribution of y-groove welded joint with weld metal of LB-116 and preheat temperature of 125 °C (W5 in Table 1).
studies, the occurrence of cracking was determined from the shape of weld metal. At the bottom of the weld metal, the HAZ/weld metal bound-
the cumulative AE energy curve [32]. In the present study, to quantify ary on the left side showed higher plastic strain than the right side. In the
the crack initiation time, the cumulative AE energy and AE energy rate contour plot of the diffusible hydrogen concentration, the hydrogen accu-
in y-groove weld cracking tests were calculated by the following proce- mulation was observed in the vicinity of the boundary between the left
dure. The AE energy was defined by the square of AE amplitude, and the HAZ and the weld zone (position A in Fig. 21(c)), which is consistent
AE energy rate was calculated by differentiating the cumulative AE en- with the position where the crack initiation was observed in the experi-
ergy with the testing time using the general least-squares differentia- ment. The time evolution of maximum principal stress and hydrogen
tion method [57]. The results are shown in Fig. 18. In the cracked concentration at the position A is shown in Fig. 22. A qualitative explana-
specimens (W1–3 and W6), a clear peak was observed in the AE energy tion of the change in maximum principal stress is indicated by arrows in
rate plot, which was regarded as the crack initiation time. The relation- the figure. The mechanism can be explained as follows: (i) increasing by
ship between cracking ratio and total AE energy in y-groove weld crack- thermal tensile stress after welding, (ii) sudden decrease by expansion
ing tests is shown in Fig. 19. The total energy increased with the due to martensitic transformation, (iii) gradual increase until the entire
cracking ratio. This result indicates that the detected AE signals were joint is cooled to room temperature and (iv) no change after cooling to
generated by crack initiation and growth in the y-grooved specimen. room temperature. As the preheat temperature increased, the maximum
principal stress at the final calculation step was higher since the temper-
4.6. Hydrogen diffusion and stress concentration in y-groove weld cracking ature difference between the preheat temperature and room tempera-
tests ture increased. The hydrogen concentration at the position A rapidly
increased after welding due to diffusion from the weld zone, and after
The calculation results of the temperature histories at the thermocou- that, decreased due to diffusion into the base material. Under the low pre-
ple positions were in good agreement with the experimental results. An heat temperature conditions, the hydrogen began to accumulate around
example of the temperature history calculation is shown in Fig. 20. The 100 s because the diffusion coefficient at position A became smaller than
distribution of the maximum principal stress, equivalent plastic strain that at the other positions due to the effects of plastic strain and stress
and diffusible hydrogen concentration 2 h after welding in the specimen concentration according to Eqs. (10) and (11). In the case of higher pre-
W1 is depicted in Fig. 21. In the plot of maximum principal stress distri- heat temperature, the diffusion into the base metal was accelerated,
bution, maximum points were located at the weld root. The equivalent and the locally accumulated diffusible hydrogen concentration became
plastic strain was distributed approximately symmetrically around the lower. Compared to the case that the change of the diffusion coefficient
Fig. 16. (a) Cross-sectional observation of y-groove welded joint with weld metal of LB-116 and preheat temperature of 20 °C (W1 in Table 1), and (b) relationship between preheat
temperature and cracking ratio in y-groove weld cracking test.
12 T. Shiraiwa et al. / Materials and Design 190 (2020) 108573
due to plastic strain was not taken into account [19], the peak of the hy- induced cracking is predicted to occur when the hydrogen concentra-
drogen concentration around 104 s was more significant, which leads to tion and maximum principal stress exceed the limit curve. In Fig. 23
safer evaluation. (a), the initial hydrogen concentration was kept at 4.5 ppm under all
four conditions to examine the effect of the preheat temperature. The
4.7. Validation of criterion for hydrogen-induced cracking stress-hydrogen curves exceeded the limit curve of σAE under the
three conditions of W1–3 (preheat temperatures of 20, 50 and 75 °C)
To examine the validity of the hydrogen-induced crack formation among the four conditions. These results are in good agreement with
criterion derived by the AE method, the time-series data of hydrogen the cross-sectional crack observations. In the cross-sectional observa-
concentration and maximum principal stress at the position A are plot- tions, the cracks were observed under these three conditions, and no
ted with the limit curve derived from the SSRT test (cooling rate of cracks were observed at a preheating temperature of 100 °C as de-
30 °C/s) in Fig. 23. In the plots, the cracking time estimated from the scribed in Section 4.5. In contrast, when the conventional limit curve
peak of AE energy rate is marked as “x.” In the conditions without the of σNB is used, cracking is not predicted under the preheat temperature
mark “x”, no crack was found in the cross-sectional observations. The of 75 °C. Therefore, it was suggested that the crack formation criterion
arrows in the figure correspond to those in Fig. 22(a). The hydrogen- derived by the AE method provides a more accurate prediction for
Fig. 17. AE events and location along the weld line in y-groove weld cracking tests of (a)-(d) W1–4, (e) W6, and (f) W9.
T. Shiraiwa et al. / Materials and Design 190 (2020) 108573 13
hydrogen-induced cracking. Under the condition of W3, the time when occurrence and initiation time of hydrogen-induced cracking, it will be
the stress-hydrogen curve passed the limit curve of crack formation was necessary for future studies to reflect the effect of the detailed bead ge-
in good agreement with the cracking time detected by the AE signal. ometries in finite element models.
Under the conditions of W1–2, the time of crossing the limit curve did In the above method, since the two state quantities (hydrogen and
not coincide with the cracking time. The possible reason is that the stress) were plotted in one figure, the cracking time and the degree of
stress at position A was overestimated in FEM calculations because the hydrogen-induced cracking are visually unclear in the figures. Here, it
curvatures at the HAZ/weld metal boundaries were not taken into ac- is examined that the risk of hydrogen-induced cracking is expressed
count in the finite element models. The element types and meshing with a single parameter. Since hydrogen-induced cracking is predicted
methods can also affect analysis results. In Fig. 23(b), the preheat tem- when the power law of Eq. (12) is satisfied, we defined the following
perature was kept constant at 20 °C, and the initial hydrogen concentra- hydrogen-induced cracking (HIC) parameter, F, as an indicator of
tion was changed by using various weld metals. In the condition of W6, hydrogen-induced damage:
although the calculation result approached the limit curve at the crack
initiation time, the stress‑hydrogen curve did not exceed the limit σ 1;loc H loc m
F¼ ð13Þ
curves. In this condition, a short crack was observed only in one of the k
five cross-sections, and the cracking ratio was very limited (6.9%) as
shown in Fig. 16. Therefore, the crack may have occurred due to local where k and m are the coefficient and exponent of the limit curve of σAE
stress concentration that was not considered in the finite element anal- obtained from the SSRT specimens with a cooling rate of 30 °C/s. The
ysis, such as the weld defects and the local geometry of the bead. Thus, values are presented in Table 4, Section 4.3. It is expected that
under the current conditions, the occurrence of hydrogen-induced hydrogen-induced crack initiates when the HIC parameter exceeds
cracking was well predicted by the derived criterion and FEM calcula- unity. The distribution of the HIC parameter 2 h after welding under
tions with this exception. To achieve more accurate predictions for the the condition of W1 is displayed in Fig. 24. It can be seen that the HIC
Fig. 18. Cumulative AE energy and AE energy rate in y-groove weld cracking tests of (a)-(d) W1–4, (e) W6, and (f) W9.
14 T. Shiraiwa et al. / Materials and Design 190 (2020) 108573
could be estimated by using the HIC parameter defined based on the cri-
where t is time. The relationship between the average HIC parameter terion. The optimal preheat temperature can be selected by the average
and cracking ratio is shown in Fig. 26. Overall, the cracking ratio in- HIC parameter. Unlike the conventional chart methods, the calculation
creased with the average HIC parameter. Under the conditions where procedure proposed in this study can be applied to different joint
the average HIC parameter exceeded unity, the cracking ratio was types because it uses local parameters considering joint geometries. In
more than 50%. These results showed that the amount of hydrogen- the present study, the criterion (limit curve) was derived from the sim-
induced cracks can be estimated by the average HIC parameter, even ulated HAZ specimens. A more accurate limit curve would be obtained
with the variation in the detailed shape of the weld bead. Focusing on
the minimum value of A with hydrogen-induced cracking, it was sug-
gested that the cracking ratio would be zero when the average HIC pa-
rameter is less than approximately 0.6. Therefore, by selecting the
preheat temperature so that the average HIC parameter does not exceed
this threshold value, the critical preheat temperature to prevent
hydrogen-induced cracking can be determined for arbitrary initial hy-
drogen content. To ensure adequate reproducibility of the threshold
value, it is required to increase the number of weld cracking tests. Be-
sides, other grades of steel with different susceptibility to hydrogen-
induced cracking are expected to have different thresholds of the aver-
age HIC parameter.
As described above, the criterion for hydrogen-induced crack forma-
tion derived by the AE method was validated by y-groove welding tests.
The results showed that the cracking ratio in the y-groove welding tests
Fig. 21. Distribution of (a) maximum principal stress, (b) equivalent plastic strain, and
Fig. 19. Relationship between cracking ratio and total AE energy in y-groove weld cracking (c) diffusible hydrogen concentration 2 h after welding with weld metal of LB-116 and
tests. preheat temperature of 20 °C (W1).
T. Shiraiwa et al. / Materials and Design 190 (2020) 108573 15
5. Conclusions
(1) In SSRT testing, the AE signals due to the crack initiation were de- Fig. 23. Local maximum principal stress and locally accumulated diffusible hydrogen
concentration in y-groove welding crack tests with (a) initial hydrogen concentration of
tected around the circumferential notch before the maximum
4.5 ppm (W1–4) and (b) preheat temperature of 20 °C (W1, W6, W9). The cross
stress. The crack initiation stress estimated by the AE signals de- symbols represent the crack initiation points detected by the AE method.
creased with increasing the initial diffusible hydrogen content.
(2) The stress field and hydrogen concentration field at the crack ini-
tiation time in the SSRT specimens were calculated by finite ele- equivalent plastic strain distribution in FEM. The limit curve for
ment analysis. The hydrogen diffusion coefficient and solubility the hydrogen-induced crack formation was derived as a power
of hydrogen were determined by Vickers hardness and the law of local maximum principal stress and locally accumulated
hydrogen concentration.
(3) In y-groove weld cracking tests, the AE signals were detected
after welding. There was a clear correlation between the total
AE energy and the cracking ratio in the cracked specimens. This
result indicates that the amount of cold cracking in high-
strength steels could be estimated from the total AE energy.
(4) The occurrence of hydrogen-induced cracking and the time of
cracking were successfully predicted by the proposed method.
On the other hand, it was suggested that a numerical analysis
considering a more detailed geometry is necessary to predict
the cracking behavior under partially cracked conditions.
(5) To quantitatively evaluate the risk of hydrogen-induced cracking,
an indicator parameter was defined as a function of the local
maximum principal stress and locally accumulated hydrogen
concentration. It was shown that the proposed indicator
Fig. 22. Time evolution of (a) local maximum principal stress and (b) locally accumulated
diffusible hydrogen concentration at the position A of Fig. 21 in y-grooved welding joints Fig. 24. Distribution of hydrogen-induced cracking parameter 2 h after welding with weld
with initial hydrogen concentration of 4.5 ppm (W1–4). metal of LB-116 and preheat temperature of 20 °C (W1).
16 T. Shiraiwa et al. / Materials and Design 190 (2020) 108573
Fig. 25. Hydrogen-induced cracking parameter histories at position A in y-groove welding crack tests with (a) initial hydrogen concentration of 4.5 ppm (W1–4) and (b) preheat
temperature of 20 °C (W1, W6, W9). The cross symbols represent the crack initiation time detected by AE method.
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