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The material used in this study is AISI 4340 steel, received in the 35
Dr. P. Zhang, Prof. Z.-F. Zhang, Dr. H.-F. Li, Dr. Q.-Q. Duan fully annealed condition, with chemical composition: Fe–0.42C– 36
Materials Fatigue and Fracture Division
Institute of Metal Research
0.25Si–0.66Mn–1.41Ni–0.17Mo–0.74Cr–0.11Cu (in wt%). The 37
Chinese Academy of Sciences specimens were firstly austenitized at 860 C for 30 min followed 38
Shenyang 110016, P. R. China by oil quenching. The as-quenched (AQ) steel was tempered at 39
E-mail: pengzhang@imr.ac.cn; zhfzhang@imr.ac.cn 180, 240, 350, and 420 C for 2 h, respectively, and cooled in air. 40
Dr. H.-F. Li, Prof. Z.-F. Zhang Tensile properties were determined on ASTM-E8 standard 41
School of Materials Science and Engineering specimens with a gauge length/diameter of 25/5 mm. The 42
University of Science and Technology of China
Shenyang 110016, P. R. China
tensile tests were performed on a Servo-hydraulic Instron8801 43
tester at tensile rate of 1 10 3 mm s 1. The Charpy V-notched 44
The ORCID identification number(s) for the author(s) of this article specimens (size: 55 10 10 mm3) were tested at room 45
can be found under https://doi.org/10.1002/adem.201801116.
temperature by a Zwick impact tester (RKP 450, Zwick, 46
DOI: 10.1002/adem.201801116 Germany) of 450 J capacity. The fracture toughness specimens 47
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Figure 1. SEM micrographs of AISI 4340 steel tempered at different temperatures, a) AQ, b) 240 C, c) 420 C.
1 were standard single-edge-notch bended specimens with a martensite morphology with AQ steel, as revealed in Figure 1b. 1
2 width/thickness of 24/12 mm (25 mm thick specimen for the Additionally, Figure 1c marks the presence of carbides 2
3 steel tempered at 420 C). Firstly, the fatigue crack tests were (confirmed by EDS) dispersed between lath tempered martensite 3
4 conducted to induce a fatigue pre-crack and crack length was matrix, as indicated by white circle. It is noted that the prior 4
5 between 0.45 and 0.55 W, where W is the specimen width. The austenite grain size of steels in this study is unchanged 5
6 fracture toughness tests were carried out on a Servo-hydraulic (d ¼ 25 5 mm, through measurement). 6
7 Instron8801 tester according to ASTM E399-12. In our study, The fine microstructure of AISI 4340 steel can be observed by 7
8 three specimens were tested for each condition. The fracture TEM, as shown in Figure 2a–c. Significant variation is observed 8
9 surface morphologies of the specimens after Charpy impact in the specimens, depending upon the tempering process. 9
10 and fracture toughness tests were examined using a LEO Supra Figure 2a demonstrates that the morphology of AQ steel is 10
11 35 scanning electron microscopic (SEM). The TEM microstruc- dislocated martensite laths, and the martensite laths generally 11
12 ture was categorized in an FEI F20 Tecnai instrument operating exhibited a high dislocation density (as high as 1012 cm 2[19]), 12
13 at 200 kV. During the observation, energy dispersive spectrome- resulting from the lattice invariant deformation component of 13
14 ter (EDS) was also utilized to analyze the corresponding the diffusionless martensitic phase transformation.[20] Addition- 14
15 compositions. ally, it can be mentioned that plenty of twinned martensite (red 15
circle)[19] occurs as well. With increasing the tempering 16
temperature, the number of twinned martensite and dislocation 17
density reduce markedly, as displayed in Figure 2b. It is found in 18
16 3. Results
Figure 2c that the large amount of carbide particles precipitated 19
17 3.1. Microstructure Evolution inside the lath, which is confirmed as cementite by EDS.[21] The 20
length of precipitated carbides ranging from 100 to 200 nm, and 21
18 The SEM observations of microstructure in AQ state and the width is about 20–50 nm. There is no significant discrepancy 22
19 tempered at 240 C, 420 C are displayed in Figure 1a–c. It can be in the martensite lath width of tempered steels, the dislocation 23
20 noted in Figure 1a that the morphology of AQ steel is typical density reduction and coarse carbide precipitation in martensite 24
21 martensite laths (yellow arrows) with hundreds of nanometers lath would be the most obvious microstructure variation during 25
22 wide. When tempered at 240 C, there is no obvious difference in tempering. 26
Figure 2. TEM micrographs of AISI 4340 steel tempered at different temperatures, a) AQ, b) 240 C, c) 420 C.
Adv. Eng. Mater. 2019, 1801116 1801116 (2 of 6) © 2019 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim
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Table 1. The mechanical properties of AISI 4340 steel tempered at which would be attributed to the TME.[16] However, contradicted 1
different temperatures. to the impact toughness results, the fracture toughness increases 2
markedly with improving the tempering temperature, even at 3
Tempering KIC 350 C. To analysis more intuitively, the two types of toughness 4
temperature σy [MPa] σb [MPa] e [%] A [%] [MPa m1/2] CVN [J] results would be normalized, as illustrated in Figure 3b. The 5
AQ (25 C) 1355 2061 10.29 51 41.07 0.61 14.8 1.2 result shows that there is a trade-off relation between the 6
180 C 1550 1933 10.75 75 55.00 3.07 17.9 0.9 strength and fracture toughness, while an approximately 7
240 C 1473 1810 9.31 78 58.58 1.87 18.5 1.7
invariable trend between the strength and impact toughness. 8
Consequently, the difference of the two strength-toughness 9
350 C 1430 1606 9.40 79 75.64 0.71 16.6 0.3
relations would be elaborated in detail in the discussion part. 10
420 C 1320 1452 9.63 77 91.73 3.34 19.8 0.8
Figure 3. a) The plane strain fracture toughness and impact toughness as a function of tempering temperature for AISI 4340 steel; b) the relationship
between the tensile strength and normalized toughness.
Figure 4. The SEM images of fracture surface morphologies of Charpy impact specimens tempered at different temperatures, a) AQ, b) 240 C,
c) 420 C.
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Figure 5. The SEM images of fracture surface morphologies of KIC specimens tempered at different temperatures, a) AQ, b) 240 C, c) 420 C.
1 fracture morphology generally shows a cleavage pattern (yellow easily reach the critical fracture strength, resulting in the crack 1
2 circles) corresponding to a brittle fracture mode. When initiation. Especially in steel tempered at low temperature 2
3 tempered at 240 C (Figure 5b), the number of cleavage planes (200–400 C), the coarse carbides precipitated in and along 3
4 (yellow circles) significantly reduces while the amount of the martensite lath would reduce the bond strength with the 4
5 dimples increases. Furthermore, the micrographs of steel matrix.[24] Although the dislocation density reduction in the 5
6 tempered at 420 C (Figure 5c) show different size dimples martensite lath could promote the mobile dislocations glide and 6
7 without the cleavage surface, illustrating the enhancement of proliferation, the stress field near the notch root would 7
8 toughness. preferentially reach the critical fracture strength,[6] leading to 8
the initiation of micro-cracks at numerous carbides. Conse- 9
quently, the coarse carbides around the rounded notch would 10
9 4. Discussion reduce the crack initiation energy in tempered steel.[10] The 11
energy consumed by the dislocation motion in the matrix is just 12
10 It is believed that the embrittlement of tempered steel might be enough to offset the reduced crack initiation energy by the 13
11 caused by the combination of several mechanisms,[10,12,15] occurrence of coarse carbides. This is explanation that the TME 14
12 mainly indicating the coarse carbide precipitation, decomposi- occurs in the Charpy impact toughness test, leading to the 15
13 tion of retained austenite or impurity separation. However, the invariable trend between the strength and impact toughness in 16
14 retained austenite does not occur in the AQ steel, and the AQ/QT steels. It should be mentioned here that the slightly 17
15 intergranular fracture morphology has not yet been observed in higher impact energy in tempered steel than AQ steel might be 18
16 impact specimen. Therefore, the carbide precipitation would be attributed to the increased resistance of martensite matrix to the 19
17 the major factor in promoting TME in this study. Lee and crack propagation. 20
18 Takebayashi[22,23] reported a linear relation between the carbide However, the fracture toughness of materials illustrates the 21
19 size and the critical distance for cleavage crack initiation, resistance ability (energy absorption) to stable crack propagation, 22
20 revealing that the coarse carbides are detrimental to the impact as revealed by the R curve[31,32] in Figure 6c. The R curve 23
21 toughness. Several researchers[16,24,25] thought that the distribu- represents the energy for the formation of plastic deformation 24
22 tion of carbides along the martensite lath and prior austenite zone ahead of the crack tip, initiation and growth-coalescence of 25
23 grain boundaries causes embrittlement of materials, promoting micro-cracks. When the energy release rate is equal to the crack 26
24 rapid fracture. Cao et al.[3] pointed out that the local fracture resistance (G ¼ R), the fracture instability occurs. According to 27
25 stresses for cleavage fracture were determined by the morphol- the fracture mechanics, GIC and KIC have the following relation: 28
26 ogy and size of the grain and carbide particles, illustrating that
27 the coarse carbide and grain result in the inferior impact K 2IC
28 toughness. Duan et al.[26] proposed that the energy for crack GIC ¼ ; ð1Þ
E
29 initiation approaches to 75% of the Charpy impact energy
30 through the quasi-situ impact fracture test. Figure 6a presents a where GIC is the maximum energy release rate and E is Young’s 29
31 typical load-time trace (P-t) of instrumented impact test revealing modulus. It is found that the notch root radius in the KIC 30
32 the energy consumed by crack initiation (EI) and crack specimen is approach to 0 (ρ ¼ 0) due to the fatigue pre-crack. At 31
33 propagation (EP).[27] Additionally, the notch root radius (ρ) of the beginning of crack extension, the plastic zone radius ahead of 32
34 specimen would affect the toughness through the variation of the crack tip is approximately equivalent to the prior austenite 33
35 the stress field around the notch tip.[28,29] For the Charpy impact grain size (25 5 mm) of AISI 4340 steel by calculation 34
36 test, the plastic zone radius ahead of the notch root is much (Figure 6d). The micro-cracks also preferentially initiated at 35
37 larger than the prior austenite grain size under the effect of high- the coarse carbides around the crack tip in tempered steel. 36
38 rate stress, as displayed (yellow curve) in Figure 6b, which has While, the amount of the micro-cracks is much lower than that 37
39 been verified by the previous experimental study[6,26,30] and finite in the Charpy impact specimen, demonstrating that the energy 38
40 element analysis.[29] Hence, the stress around the notch tip can for crack initiation would not be the major part. Additionally, the 39
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Figure 6. a) Schematic illustration of load–time trace from an instrumented impact test, energy consumed for crack initiation (EI) and crack propagation
(EP); b) schematic illustration of the stress field (yellow curve) ahead of the rounded notch tip for Charpy impact specimen; c) R curve for ductile metal
material; d) schematic illustration of the stress field (yellow curve) ahead of the sharp crack tip for KIC specimen.
1 micro-cracks are difficult to grow alone owing to the existence of the dislocation density reduction in the martensite laths would 1
2 the main crack. The dislocation density inside the martensite promote the dislocation movement, enhancing the crack 2
3 lath decreases sharply with increasing the tempering tempera- propagation resistance. 3
4 ture, promoting the number of mobile dislocation ahead of
5 the crack tip. Numerous movable dislocations are emitted
6 from the surface of the voids under plastic strain controlled, Acknowledgement 4
7 which are beneficial for stress relaxation.[33,34] Therefore, the
This work was financially supported by the National Natural Science 5
8 sharp crack would be blunted by the emission of mobile Foundation of China (NSFC) under grant Nos. 51331007, 51771208, 6
9 dislocations[35,36] and prevent the crack growth. The micro- U1664253 and the Strategic Priority Research Program of the Chinese 7
10 cracks initiated at the carbides are connected to the main crack Academy of Sciences under grant No. XDB22020202. 8
11 through void growth/coalescence, which could consume more
12 energy. It is seen that the substructure inside the martensite lath
13 in tempered steel plays a significant role in the crack growth, Conflict of Interest 9
14 illustrating the fracture toughness would increase with the
The authors declare no conflict of interest. 10
15 tempering temperature.
Keywords
16 5. Conclusions
crack initiation and growth, fracture toughness, impact toughness,
17 In summary, the strength-toughness relations in AISI 4340 strength-toughness relationship, tempered martensite embrittlement
18 tempered steel were systematically investigated. The results
11
19 show that there is a trade-off relation between strength-fracture Received: October 21, 2018 12
20 toughness and the approximately invariable relationship Revised: December 11, 2018 13
21 between strength-impact toughness. The effect of microstruc- Published online:
22 ture on the materials toughness is related to the manner of
23 energy consumption, which should be attributed to the notch
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