Effect of reheating rate on microstructure and properties of high-strength-toughness steel Z. J. Xie1†, Y. P. Fang1†, Y. Cui2, X. M. Wang1, C. J. Shang∗ 1 and R. D. K. Misra3 Effects of reheating rate and holding time during tempering on microstructure and properties of a 960-MPa-grade low-alloy steel were investigated. Different reheating rates from 1 to 300 K s−1 and holding time from 5 to 1200 s on tempering at 823 K were carried out. The combination of high reheating rate and short holding time is obviously beneficial forgetting more uniformly distributed and refined carbides, which are believed to contribute to the high strength and high toughness. Yield strength of 960 MPa with elongation of ∼16% and impact toughness of 76 J (half size specimen) at 233 K was obtained by induction reheating tempering at 823 K for 5 s at a rate of 373 K s−1. Keywords: High-strength low-alloy steel, Nano-scale carbides, Reheating rate, Induction tempering Introduction High-strength low-alloy (HSLA) steels are widely used in energy field, such as off-shore drilling platforms, pipelines and other fossil fuel industries, because of their outstanding mechanical properties, good weldability and low cost. To meet the requirements, especially for the severe service environment, a superior combination of high-strength and low-temperature toughness steel is the primary aim in engineering.1 In consideration of the weldability and toughness, the carbon content of HSLA steels is usually controlled at a lower level. As a result, adjusting the microstructure by heat treatment becomes a main route for obtaining desired strength and toughness combination in a given steel. One of the most effective heat treatments is quenching and tempering. During quenching and tempering, matrix recovery and carbide precipitation usually occur. However, the extent of the recovery and the size and morphology of carbides, especially cementite carbides, depend significantly on the appropriate selection of heat treatment parameters, such as reheating rate, holding time and tempering temperature, which are important to obtain desired properties.2 Quenching process inclusive of on-line quenching directly after finishing rolling and off-line quenching after reheating the hot-rolled steel plates to re-austenitisation temperature is the common practical way to obtain high strength in HSLA steel.3 Toughness could be improved by the subsequent tempering with the cost of strength, because of the reciprocal relationship between high-strength and low-temperature toughness. † Contributed equally to this work. School of Materials Science and Engineering, University of Science and Technology Beijing, Beijing, China 2 Shougang Research Institute of Technology, Beijing, China 3 Department of Metallurgical and Materials Engineering, University of Texas at El Paso, El Paso, TX 79968, USA 1 ∗ Corresponding author, email cjshang@ustb.edu.cn © 2016 Institute of Materials, Minerals and Mining Received 1 October 2015; accepted 30 December 2015 DOI 10.1080/02670836.2015.1138044 It is widely reported that the coarse carbide precipitates and brittle particles result in cleavage fracture and are harmful for low-temperature toughness.4–6 In the case of HSLA steels, the conventional tempering (CT) process with slow reheating rate and long holding time would create coarse carbides and particles inhomogeneous distribution, which do harm to toughness.7 However, with the advantage of rapid reheating rate and high efficiency, induction reheating tempering (IT) is favourable to obtain fine microstructure and dispersed precipitates.8 Thus, selection of appropriate tempering parameters is the key factor in controlling carbide precipitation and in obtaining good combination of high-strength and low-temperature toughness.9,10 The aim of the present study is to elucidate the relationship between microstructure and mechanical properties of 960-MPa-grade HSLA steel by altering tempering parameters, with particular attention to reheating rate and holding time on carbide size and distribution, and their relationship to mechanical properties. Experimental methods The chemical composition of experimental steel in weight percent (wt-%) was Fe–0.12C–0.22Si–1.44Mn, <1.0(Cr + Mo + Nb + Ti + V+B). The experimental steel plates were melted in a vacuum induction furnace, cast and were hot rolled to a strip of 8-mm thickness. The experimental steel plates were austenitised at 1173 K for 30 min and water quenched to room temperature at a cooling rate of ∼40 K s−1.Two aspects of experimental test were carried out to investigate the influence of tempering parameter on the mechanical properties and carbide evaluation. One part of the quenched specimens were machined to cylindrical specimens that were 10 mm in length and 4 mm in diameter with the axis parallel to the rolling direction, and heat treated as illustrated in Fig. 1 using a DIL 805a-type dilatometer for tempering simulation. The Materials Science and Technology 2016 1 Xie et al. Reheating rate and high-strength-toughness steel Results and discussion Influence of tempering parameters on the Vickers hardness 1 Schematic illustration of the quenching and tempering cycle treatment cylindrical specimens were tempered at 823 K for periods of 5, 40, 150 and 1200 s at reheating rates of 1, 20, 100 and 300 K s−1, respectively. After tempering, the specimens were cooled at ∼40 K s−1 to room temperature. The simulated specimens were prepared for the Vickers hardness and microstructure evaluation. The average Vickers hardness was obtained from 12 test points, with a load of 9.8 N using HVS-1000ZDT. The microstructure of specimens were characterised via combination of a scanning electron microscope (ZEISS ULTRA-55 field SEM) and a transmission electron microscope (TEM; JEM-2100F) at 200 kV. Transmission electron microscope foils were prepared by mechanical polishing and twin-jet polishing in a 5% perchloric acid solution using a twin-jet polisher. The second part of the quenched samples were induction reheated at a heating rate of ∼100 K s−1 to 823 K using an induction heating furnace, followed by air cooling to room temperature. These samples were designated as Q-IT. For comparing with the CT process, the quenched specimens were reheated at a reheating rate of ∼1 K s−1 to 823 K and held for 20 min by conventional furnace, followed by air cooling to room temperature. These samples were designated as Q-CT (Fig. 2). The tempered Q-IT and Q-CT samples were machined to the tensile and the Charpy impact tests according to the ASTM standard. Tensile tests were carried out at a strain rate of 2.5 × 10–3 s−1 at room temperature to determine the yield strength, tensile strength and elongation. Impact toughness was determined using the Charpy V-notch specimen of dimensions 5 mm × 10 mm × 55 mm prepared from the longitudinal orientation and tested at 233 K. 2 Schematic illustration of the tempering treatment of quenched specimens with different reheating rates 2 Materials Science and Technology 2016 With regard to tempering, the reheating rate and holding time are the key factors to attain good combination of high-strength and low-temperature toughness.8 By induction tempering, a reheating rate range of 1–300 K s−1 can be obtained and the holding time varied from 5 to 1200 s. The correlation of tempering parameter, microstructure and hardness can be revealed from Fig. 3. It shows the mean hardness obtained after tempering at 823 K by different reheating rates and holding times. The hardness of the as-quenched specimen was 388 HV. Compared with the as-quenched sample, tempering process led to a decrease in the hardness. For holding of specimens for 5 s, the Vickers hardness of tempered specimens increased from 330 to 347 HV with an increase in the reheating rate from 1 to 300 K s−1. There was no significant difference in hardness between the rapid reheating rate and the slow reheating rate on tempering for 1200 s. In addition, when the reheating rate was 300 K s−1, the Vickers hardness decreased from 347 to 309 HV on holding from 5 to 1200 s. It can be concluded that increasing reheating rate and decreasing holding time significantly contributed to higher Vickers hardness after tempering. Meanwhile, prolonging the holding time decreased the contribution of the rapid heating rate on the hardness. Microstructure characterisation Bright-field TEM micrographs showing carbides in quenched and tempered samples with different reheating rates are presented in Fig. 4. It can be seen that the quenched microstructure comprised lath martensite and lower bainite. Owing to the diffusionless, shear mechanism of martensite transformation, there was no carbide precipitation within martensitic lath.11 However, needleshaped carbides were observed in the bainitic ferrite matrix. The average length of the long axis of carbide was approximately 200 nm (Fig. 4b). The previous result confirmed the carbides as cementite precipitation on the basis of selected area diffraction pattern.12 Figure 4c–h shows the bright-field TEM micrographs of as-quenched samples tempered at 823 K for 5 s at a 3 Evolution of the Vickers hardness as a function of heating rate and holding time at the 823 K tempering treatment Xie et al. Reheating rate and high-strength-toughness steel reheating rate of 1–300 K s−1. There are two types of carbides forming in the microstructure: one is needle-like within the bainitic ferrite lath, and the other one is spherical along the lath boundary or prior austenite boundary. With an increase in the reheating rate, the distribution of carbides became homogenous and the carbides were finer (Fig. 4c–f). With an increase in the reheating rate from 1 to 300 K s−1, the morphology of carbides precipitated within bainitic ferrite lath changed from needle to rod-like, and the dimension of the long axis was decreased from 200 to 80 nm. Figure 4g–h reveals the changes in spherical-type carbides at different reheating rates. The diameter of spherical-type carbides was ∼200 nm at a reheating rate of 1 K s−1, while their size decreased to less than 100 nm at a reheating rate of 100 K s−1. This clearly gives evidence 4 Bright-field TEM micrographs showing cementite carbides of as-quenched specimens and tempered with different reheating rates a and b as-quenched, c and g reheating rate 1 K s−1, d 20 K s−1, e and h 100 K s−1 and f 300 K s−1, respectively Materials Science and Technology 2016 3 Xie et al. Reheating rate and high-strength-toughness steel to support that increasing the reheating rate significantly contributes to refining carbides. Influence of tempering parameter on refinement of carbides’ size Generally, during the precipitation process, carbides preferentially choose the prior austenite boundaries, packet boundaries (high-angle boundaries), lath boundaries and dislocation within laths (low-angle boundaries) to nucleate in the microstructure.8 Considering the difference between prior austenite boundaries and martensitic or bainitic lath boundaries, it is important to analyse the evolution of carbides. As mentioned above, needle- type carbides precipitated primarily within the lath and spherical carbides precipitated along the lath boundary or prior austenite boundaries. Figure 5 shows the effect of tempering parameters on the size distribution of carbides during tempering. The results indicate that after holding for 5 s(short time), the length of long and short axes of the carbides was significantly decreased irrespective of the locations of the precipitates for reheating rates of 1–300 K s−1 (Fig. 5a–b). By increasing the reheating rate from 1 to 300 K s−1 during tempering, the length of the long axis of carbides precipitated at the prior austenite boundaries decreased from 300 to 100 nm, while, for carbides those precipitated within lath, the length of the long axis decreased from 210 to 80 nm. On the 5 The relationship between long axis, short axis and axis ratio of the carbides with different tempering parameters at 823 K with different reheating rates and holding times a and b 1 to 300 K s−1 for 5 s; c and d 1 K s−1 for 5 to 1200 s; e and f 100 K s−1 for 5 to 1200 s at prior austenite boundaries a, c and e and within the lath b, d and f 4 Materials Science and Technology 2016 Xie et al. Reheating rate and high-strength-toughness steel holding times, it can be found that the holding time makes a significant effect on the size of carbides coarsening at a rapid reheating rate. During tempering process, rapid reheating rate retards the recovery of dislocations.8,13 On the other hand, the time–temperature–precipitation diagram for high reheating rate is expected to be different from the normal reheating rate.14–17 The rapid reheating rate reduces the incubation time of carbides, resulting in acceleration of precipitation kinetics of carbides. From this aspect, the rapid nucleation rate of carbides and short holding time are basic parameters to obtain fine carbides. Figure 5 further confirmed that tempering parameters such as reheating rate and holding time are important to regulate the size and distribution of secondary precipitation. When the tempering temperature was 823 K, increasing the reheating rate to 100 K s−1 and decreasing the holding time is an ideal approach to obtain nano-scale carbides in the experimental steel. Relationship between the size of carbides and the Vickers hardness 6 Relationship between mean carbides’ size and hardness in 1 and 100 K s−1 with different holding times a at prior austenite boundaries and b within the lath other hand, the morphology of carbides changed from needle-like to short rod-like with a decrease in the long/ short axis and axis ratio. To analyse the effect of holding time on the size and distribution of carbides, Fig. 5c–f summarises carbides’ size distribution obtained for specimens reheated at 1 and 100 K s−1, held for 5–1200 s, respectively. When the reheating rate was 1 K s−1, prolonging the holding time led to coarsening of carbides, consequently, the length of long and short axes was increased dramatically (Fig. 5c and d ). The ratio of long/short axis of carbides was decreased from ∼5.0 to 4.0, implying that the morphology of carbides was changed to spherical type. As the reheating rate increased to 100 K s−1, with an increase in the holding time, the length of long and short axes behaved in the same manner as that at a low reheating rate (Fig. 5e and f ). However, comparing the size distribution of carbides at a constant reheating rate with different Table 1 Figure 6 shows the relationship between the mean size of carbides and the Vickers hardness. It was clearly noted that tempering parameters make a big difference in the Vickers hardness. Irrespective of precipitation at prior austenite boundaries (Fig. 6a) or within the lath (Fig. 6b), the general behaviour of plot is similar. The hardness decreased with the increasing holding time from 5 to 1200 s. In other words, the coarsening of carbide is the main reason for the lower hardness. While combining rapid reheating rate with short holding time, fine precipitates were obtained, the hardness was higher. This is because the fine and dispersed precipitates contribute more to strengthening the matrix.18,19 The lower hardness can be explained from two aspects: the first one is the coarsening of carbides caused by the slow reheating rate and long holding time; the other one is the dramatical decrease in the dislocation density due to the recovery process. Mechanical properties Table 1 shows mechanical properties of experimental steel quenched and tempered by two different tempering procedures, namely conventional furnace reheating and induction reheating. After IT and CT at 823 K as described in the experimental procedure, the yield strength of both samples was greater than 960 MPa, and the tensile strength was greater than 1000 MPa. The Charpy impact energy of the conventional tempered specimen (half thickness) was 35 J at 233 K, and that of the induction tempered sample is 76 J at 233 K. The latter is twice as much as the former. This suggests that rapid reheating rate significantly contributes to improve the low-temperature impact toughness. As mentioned above, Fig. 4e and h shows short rod-like carbides Mechanical properties of the studied steel after tempering at 823 K with different reheating rates Processing Q-CT550 (1 K s−1) Q-IT550 (100 K s−1) Yield strength/MPa Tensile strength/MPa Total elongation/% Charpy impact energy at 233 K (half thickness specimen)/J 988 997 1000 1026 15.5 16.7 35 76 Materials Science and Technology 2016 5 Xie et al. Reheating rate and high-strength-toughness steel precipitated within the lath and finer spherical carbides located at the prior austenite boundaries or lath boundaries during the induction rapid reheating tempering, consistent with the underlying reason for improvement in toughness reported in previous literatures.20,21 Comparing the mechanical properties and microstructure of the experiment steel tempered by different reheating methods, it can be concluded that IT is an excellent approach to achieve good combination of high strength and excellent toughness. Rapid reheating tempering is an effective heat treatment to obtain high strength and toughness in HSLA steel. Conclusions This study focused on the heat treatment of a low-carbon HSLA steel with particular emphasis on the effect of reheating rate and holding time of tempering process on the size distribution of carbides. It was observed that increasing reheating rate and decreasing holding time are conducive to reduce the size of carbides and alter their morphology to short rod-like or spherical type. Prolonging the holding time led to coarsening of carbides whether the reheating rate is rapid or slow. Dispersed fine carbides and high density of dislocations were the reasons for yield strength greater than 960 MPa and low-temperature toughness (half thickness) at 233 K of ∼76 J, which was two times as high as that by the CT process. Acknowledgements This work was financially supported by the National Basic Research Program of China (973 Program) through the Contract No. 2010CB630801 and the Natural Science Foundation of China through the Contract No. 51371001. Z. J.X.thanks the China Scholarship Council for the award of a scholarship for studying at McMaster University, Canada. R.D.K.M gratefully acknowledges the support from the University of Texas at El Paso, USA. References 1. X. C. Li, Z. J. 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