Effects of Austenite Conditioning on Austenite/Ferrite Phase Transformation of HSLA Steel

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1 Materials Transactions, Vol. 45, No. 1 (2004) pp. 137 to 142 #2004 The Japan Institute of Metals EXPRESS REGULAR ARTICLE Effects of Austenite Conditioning on Austenite/Ferrite Phase Transformation of HSLA Steel Yang H. Bae 1; *, Jae Sang Lee 2, Jong-Kyo Choi 2, Wung-Yong Choo 2 and Soon H. Hong 1 1 Dept. of Materials Science and Engineering, Korea Advanced Institute of Science and Technology, Kusung-dong, Yusung-gu, Daejeon, , Korea 2 Technical Research Laboratories, POSCO, P.O. Box 36, Pohang, , Korea Effects of surface area of prior austenite grain boundaries and deformation bands on austenite/ferrite phase transformation of high strength low alloy (HSLA) steel during hot working were investigated through simulated hot workings using Gleeble Effective surface areas were controlled by applying different austenite conditionings. It was found that the volume fraction of strain induced dynamic transformation (SIDT) ferrites increased with an increase in the effective surface area. The volume fraction of SIDT ferrite nucleated from the elongated prior austenite grains, however, was higher than that nucleated from equi-axed prior austenite grains at the same effective surface area. From the experiment results and discussions, it was concluded that diffusional austenite/ferrite phase transformation of HSLA steel by the interface nucleation and growth mechanism is accelerated by the deformation bands in the non-recrystallization. (Received October 29, 2003; Accepted November 28, 2003) Keywords: austenite conditioning, strain induced dynamic transformation ferrite, phase transformation, deformation band, surface area, grain size refinement 1. Introduction High strength low alloy (HSLA) steels need good toughness, high tensile strength, and low weld cracking susceptibility for structural applications. 1) In order to improve those properties, the refinement of ferrite grain size is a key technology because it is a unique method of increasing both strength and toughness. 2) Therefore, various methods, such as heavy deformation, multi-variant application, and multi axis deformation, have been suggested and studied extensively by many researchers to refine the ferrite grains in HSLA steel. 3 6) Heavy deformation has been reported to be the most effective and practical method for grain size refinement. 6) Grain size refinement is achieved by the ferrites that are nucleated just after hot working because those ferrites are smaller and exhibit lower grain growth rate than the conventional ferrites which are nucleated during cooling in the conventional thermomechanical controlled process (TMCP). These characteristics are explained by the higher nucleation rate due to the stored strain energy and the fine carbides formed during the austenite/ferrite transformation. Therefore, many researches have been conducted on the ferrites nucleated just after hot working and those ferrites are called SIDT (strain induced dynamic transformation) ferrites. 6,7) However, it is difficult to deform the steel plate to a large strain under one pass, and the heat generated by the heavy deformation causes the grain growth of the ferrites. Therefore, a continuous deformation processes with a small strain is required in the process, including both the recrystallization and non-recrystallization. Because the effect of deformation in each on austenite/ferrite phase transformation is different in terms of the nucleation rate or the nucleation site, a systematic analysis is needed on the effect of the prior austenite *Graduate Student, Korea Advanced Institute of Science and Technology microstructure in each process on the austenite/ferrite transformation during the TMCP. In this paper, the effects of surface area of prior austenite grain boundaries and deformation bands on austenite/ferrite phase transformation of Fe-0.15C-0.25Si-1.1Mn-0.04Nb B steel during hot working were investigated. 2. Microstructural Change of HSLA Steels During TMCP A schematic diagram showing the typical thermal and mechanical processes and microstructural change during thermomechanical controlled processes is presented in Fig. 1. Because the grain size of the austenite strongly affects the ferrite grain size refinement, it has been controlled by the thermomechanical treatment. This process is termed austenite conditioning. 8) The austenitizing temperature determines the initial austenite grain size of a slab. 1) In HSLA steels, a slab is austenitized at relatively lower temperatures to keep austenite grains fine. Then, the slab is hot worked at the recrystallization to refine the austenite grains by Temperature T nr A r3 Austenitizing Treatment Recrystallization Region Non recrystallization Region Fig. 1 Schematic diagram of thermal and mechanical processes, and microstructural evolution in TMCP. Time

2 138 Y. H. Bae, J. S. Lee, J. Choi, W.-Y. Choo and S. H. Hong recrystallization. Small austenite grains obtained by the recrystallization in the recrystallization lead to the refinement of ferrite grains. When reductions are applied at temperatures below those critical points for recrystallization (T nr ), the austenite grains are elongated and deformation bands are introduced within the grains. 9) As the amount of deformation in this increases, the nucleation sites at the austenite grain boundaries and within austenite grains increase. It has been reported that transformation from deformed austenite to ferrite produces much finer grain size of ferrite than that from recrystallized, strain-free austenite to ferrite because additional nucleation sites are introduced within the austenite grains. Therefore, it is very important to produce the as-deformed austenite state, which is realized by the suppression and/or retardation of recrystallization after deformation. 3. Experimental Procedures The composition of the HSLA steel used in this study is shown in Table 1. The steel was manufactured by vacuum induction melting (VIM) and followed by the sizing process for the steel plate with a thickness of 15 mm at Pohang Iron and Steel Co. (POSCO). Thermomechanical simulations were carried out by the Gleeble 1500, with which is possible to simulate complete rolling schedules, changing the applied strain, the number of temperatures of individual deformations and the subsequent cooling. The dimension of the specimen was 10 mm 15 mm. In order to change the grain size and shape of the prior austenite grain, austenite conditionings were conducted using three methods as shown in Fig. 2. The first method is to control the initial grain size of austenite by changing the austenitizing temperature from 1100 to 1200 C. The second method is to recrystallize the austenite grains by applying a fixed strain of 0.6 at the different temperatures in the recrystallization. The last method is to cause the austenite grains to become elongated and produce deformation bands within grain by applying the strain from 0.2 to 0.6 Table 1 Chemical composition of vacuum induction melted HSLA steel. Element Fe C Mn Si Nb B mass% bal in the non-recrystallization. The heating rate to the austenitizing temperatures and the cooling rate to the destination temperatures were fixed at 10 C/s and 2 C/s under all conditions, respectively. Because the Ar 3 temperature strongly affects the volume fraction and size of SIDT ferrites, 10) hot workings for formation of the SIDT ferrites in this study were conducted by fixing the hot working temperature at 40 C over Ar 3 temperature in all conditions. The detailed simulation procedures are presented in Fig. 2. Microstructures of the specimens were observed at the center of a central section parallel to the compression direction. The specimens were prepared for optical microscopy (OM) and scanning electron microscopy (SEM) by polishing and etching with 3% oxalic acid aqueous solution to reveal the prior austenite grain boundaries and deformation bands. In addition, 2% natal and 10% metabi-sulfate aqueous solution were used to reveal the mixed phases composed of prior austenite and ferrite phases. 4. Results and Discussion 4.1 Austenite conditioning Austenite conditionings were performed by controlling the austenitizing temperature, or the amount of deformation in the recrystallization or non-recrystallization. Both the recrystallization and the nonrecrystallization are dependent on temperature, strain, and strain rate. The temperature ranges for the recrystallization and the nonrecrystallization were investigated by simulated hot workings using the Gleeble 1500 under a fixed strain of 0.6 and strain rate of 1/sec. The recrystallization, which is defined as the in which the austenite grains are refined by recrystallization, ranges from 1000 Cto the temperature of the austenitizing treatment; the nonrecrystallization, which is defined as the in which the austenite grains cannot be recrystallized any further, ranges from the Ar 3 temperature to 900 C. Figure 3 shows the microstructures after austenite conditioning by changing the austenitizing temperature from 1100 to 1200 C for 1 min. as shown in Fig. 2. As the austenitizing temperature increases, the average size of austenite grains increases. It is found that the average size of prior austenite grains drastically increased between 1150 C (Fig. 3) and 1200 C (Fig. 3) because Nb Temperature T nr Ar 3 Controlling the austenitizing temperature 1100 C~1200 C/1min Recrystallization Non Recrystallization 2 C/sec 650~660 C/ ε =0.6 W.Q. W.Q C/1min Recrystallization Non Recrystallization Hot working at recrystallization 1050~1150 C/ ε =0.6 2 C/sec W.Q. W.Q. 605~635 C/ ε = C/1min Hot working at Recrystallization non recrystallization 900 C/ ε =0.2,0.4,0.6 Non Recrystallization 2 C/sec W.Q. W.Q. 650 C/ ε = C/sec 10 C/sec 10 C/sec Fig. 2 The thermomechanical process routes, composed of austenitizing treatment and hot working, performed for Fe-0.15C-0.25Si- 1.1Mn-0.04Nb-0.002B steel. Austenite conditionings of controlling the austenitizing temperature, hot working in recrystallization and hot working in non-recrystallization were conducted. Time

3 Effects of Austenite Conditioning on Austenite/Ferrite Phase Transformation of HSLA Steel 139 Fig. 3 Optical micrographs of Fe-0.15C-1.1Mn-0.25Si-0.04Nb-0.002B steel quenched before hot working near the Ar 3 temperature. Austenite conditioning of those micrographs was conducted by controlling the austenitizing temperature. Austenitizing temperatures are 1100 C, 1150 C and 1200 C, and Ar 3 temperatures are 620 C, 615 C and 610 C. Fig. 4 Optical micrographs of Fe-0.15C-1.1Mn-0.25Si-0.04Nb-0.002B steel quenched before hot working near the Ar 3 temperature. Austenite conditioning of those micrographs was conducted by the hot working in the recrystallization. Hot workings with a fixed strain of 0.6 in recrystallization were conducted at 1050 C, 1100 C and 1150 C, and Ar 3 temperature are 565 C, 580 C and 590 C. precipitates are dissolved over 1150 C and, then, cannot suppress the growth of austenite grains. 1) Figure 4 shows the microstructures after austenite conditioning by recrystallization through applying a fixed strain of 0.6 from 1050 to 1150 C in recrystallization as shown in Fig. 2. As the temperature decreases and the amount of strain increases, grain size of recrystallized austenite becomes finer. Although the average sizes of austenite grains just after recrystallization in this study range from 10 to 20 mm, the average sizes before hot working near the Ar 3 temperature range from 50 to 100 mm due to grain growth during cooling. Figure 5 shows the microstructures after austenite conditioning by applying the strain from 0.2 to 0.6 at 900 Cin the non-recrystallization as shown in Fig. 2. Deforming the austenite in the non-recrystallization produces elongated grains, the shape of which depends on the amount of strain. The grain boundaries increase with an increase in the amount of strain. Unlike the recrystallized grains, the deformed austenite grains did not grow. Therefore, although the austenitizing temperature is 1200 C, there are more grain boundaries in the case of the austenite conditioning in the non-recrystallization than in any of the other cases, as shown in Figs. 3, 4 and 5. The advantages of austenite conditioning by deformation in the non-recrystallization are explained by the increase in the grain boundaries and the introduction of the deformation bands inside grains according to several authors. 9) However, it may need to be considered that suppressing the grain growth by the deformation in the non-recrystallization also plays an important role in grain size refinement. Austenite conditionings by controlling the austenitizing temperature and recrystallization change only the size of the austenite grains. Austenite conditionings by deformation in the nonrecrystallization, on the other hand, change the shape of grains from equi-axed to elongated and introduce the Fig. 5 Optical micrographs of Fe-0.15C-1.1Mn-0.25Si-0.04Nb-0.002B steel quenched before hot working near the Ar 3 temperature. Austenite conditionings of those micrographs were conducted by the hot working in non-recrystallization. Amount of strains at 900 C are 0.2, 0.4 and 0.6. Ar 3 temperatures are 610 C in all conditions. Arrows indicate the deformation bands.

4 140 Y. H. Bae, J. S. Lee, J. Choi, W.-Y. Choo and S. H. Hong deformation bands denoted by the arrows in Fig Surface area before hot working near the Ar 3 temperature / phase transformation in steel takes place in prior austenite grain boundaries, annealing twin boundaries, and deformation bands, and areas near the precipitates within the grains. 9) Capacity to occur the phase transformation is expressed as the surface area of the boundaries, S v, which is defined as the surface-to-volume ratio. 11) Especially in HSLA steel, the surface area is confined to grain boundaries and deformation bands because the nucleation in twin boundaries and areas near the precipitates within the grains were not observed. The surface area is a sum of the area of grain boundaries, S g.b., and the area of deformation bands, S d.b., which is defined as the effective surface area, S eff. The value of S g.b. in equi-axed grain can be described through eq. (1). S g.b. is very value of effective surface area for equi-axed grains because there is no deformation band. S eff ¼ S g.b. ¼ 2N L ð1þ where, N L is number of intersections with random oriented lines per their length. 11) When the prior austenite grains are deformed, the surface area can be calculated by eq. (2) considering both the elongated grains and the deformation bands. 12) S eff ¼ S g.b. þ S d.b. ¼ 2 ðn LÞ k þ 2 ðn L Þ? þ A" 2 2 where ðn L Þ k is the number of the intersections per unit length of a line parallel to the compression direction, ðn L Þ? is the number of the intersections per unit length of a line normal to the compression direction, and the constant A was reported as about 30 over 0.2 of strain in the 0.03 mass% Nb steel. 9) The surface area of the grain boundaries in each process were measured by means of eqs. (1) and (2), and shown in Fig. 6. As the average grain size of austenite after austenite conditioning increases for the equi-axed grains, the surface area of grain boundaries decreases and is inversely proportional to the average grain size of austenite as shown in Fig. 6. As the amount of strain increases during the hot working in the non-recrystallization, the surface area of grain boundaries increases as shown in Fig. 6. ð2þ Surface area of grain boundary, S g.b. /mm Grain Size, d/µm Fig. 6 The variation of surface areas of grain boundary with varying average grain size for euqi-axed grains and with varying strain for elongated grains are presented. 4.3 Formation of strain induced dynamic transformation (SIDT) ferrite Figure 7 shows the microstructures quenched after hot working near the Ar 3 temperature as shown in Fig. 2. Austenite conditionings of those micrographs were conducted by controlling the austenitizing temperature from 1100 to 1200 C. Figure 8 shows the microstructures quenched after hot working near the Ar 3 temperature as shown in Fig. 2. Austenite conditionings of those micrographs were conducted by the hot working in the recrystallization. Hot workings with a fixed strain of 0.6 in recrystallization were conducted from 1050 to 1150 C. Figure 9 shows the microstructures quenched after hot working near the Ar 3 temperature as shown in Fig. 2. Austenite conditionings of those micrographs were conducted by the hot working in the non-recrystallization. Hot workings at 900 C were conducted with amount of strain from 0.2 to 0.6. When the shape of prior austenite grains is equi-axed, SIDT ferrites are nucleated mainly at the prior austenite grain boundaries as shown in Fig. 7 and Fig. 8. When the prior austenite grains are elongated, SIDT ferrites are nucleated at both grain boundaries and deformation bands as shown in Fig. 9. In Fig. 9, SIDT ferrite nucleated mainly at the prior austenite grain boundaries because the applied strain in the non-recrystallization is 0.2, enough small to be neglected. However, at over 0.2 of strain, SIDT ferrites are nucleated at both grain boundaries and deformation bands which are denoted by arrows in Figs. 9 and. The relationship between the volume fraction of SIDT ferrite and effective surface area, which is analyzed quanti- Surface area of grain boundary, S g.b. /mm Strain Fig. 7 Optical micrographs of Fe-0.15C-1.1Mn-0.25Si-0.04Nb-0.002B steel quenched after hot working near the Ar 3 temperature. Austenite conditionings of those micrographs were conducted by controlling the austenitizing temperature. Austenitizing temperatures are 1100 C, 1150 C and 1200 C, and hot working temperatures are 660 C, 655 C and 650 C. Black lines indicate SIDT ferrites nucleated at the grain boundaries.

5 Effects of Austenite Conditioning on Austenite/Ferrite Phase Transformation of HSLA Steel 141 Fig. 8 Optical micrographs of Fe-0.15C-1.1Mn-0.25Si-0.04Nb-0.002B steel quenched after hot working near the Ar 3 temperature. Austenite conditionings of those micrographs were conducted by the hot working in the recrystallization. Hot workings with a fixed strain of 0.6 in recrystallization were conducted at 1050 C, 1100 C and 1150 C, and temperatures of hot working near the Ar 3 temperature are 605 C, 620 C and 630 C. Black lines indicate SIDT ferrites nucleated at the grain boundaries. Fig. 9 Optical micrographs of Fe-0.15C-1.1Mn-0.25Si-0.04Nb-0.002B steel quenched after hot working near the Ar 3 temperature. Austenite conditionings of those micrographs were conducted by the hot working in the non-recrystallization. Hot workings at 900 C were conducted with amount of strain of 0.2, 0.4 and 0.6, and temperatures of hot working near the Ar 3 temperature are 650 C in all conditions. SIDT Ferrite Volume Fraction, vol% Controlling the austenitizing temperature Hot working at the recrystallization Hot working at the non-recrystallization Effective Surface Area, S eff /mm -1 Fig. 10 Relationship between the effective surface area and the volume fraction of SIDT ferrites is presented. tatively, is shown in Fig. 10. Although there are some deviations in each condition, the volume fraction of SIDT ferrite increases with increases in the effective surface area. Even though the surface area of deformation bands is considered in the calculation of the effective surface area, the volume fraction of SIDT ferrite nucleated from the elongated prior austenite grains is higher than that nucleated from equiaxed prior austenite grains at a fixed value of the effective surface area. This indicates that nucleation of SIDT ferrite is much enhanced by the deformation bands. 4.4 Potential for the nucleation of SIDT ferrites The documented advantages of hot working in the nonrecrystallization are that, with increasing amount of reduction, the austenite grain boundary area increases gradually, while the deformation band density increases rapidly, indicating that the ferrite grain refinement resulting from deformation in the non-recrystallization is due mainly to an increase in the deformation band. 9,13) In addition, Kozasu et al. mentioned that not all deformation bands act as the nucleation sites of SIDT ferrites with the same potential for the nucleation as grain boundaries. Furthermore, some bands make only very thin and straight bands of ferrite, implying poor nucleation capacity. 12) If so, there is no explanation for the fact that volume fraction of SIDT ferrite nucleated from the elongated prior austenite grain is higher than that nucleated from the equi-axed prior austenite grain at the same effective surface area. Figure 11 shows that the SIDT ferrites are nucleated at the boundary nucleated from the elongated and equi-axed austenite grains with mono layer. However, SIDT ferrites are nucleated along the deformation band with a few layers in Fig. 11. This shows that the deformation bands act as more effective nucleation sites than the prior austenite grain boundaries. The surface area has been measured and calculated with the assumption that potentials for the nucleation of SIDT ferrites are the same between grain boundaries and deformation bands. 11,13) As shown in Fig. 11, the potential of deformation bands for the nucleation of SIDT ferrite is higher than that of grain boundaries. Potential for phase transformation strongly depends on the nucleation rate

6 142 Y. H. Bae, J. S. Lee, J. Choi, W.-Y. Choo and S. H. Hong Fig. 11 Micrographs show the nucleation of SIDT ferrite at grain boundary and deformation band. Fig. 12 A SEM micrograph shows the deformation band in the prior deformed austenite grain. and the nucleation site. Figure 12 shows the microstructure of the deformation band formed during hot working in the nonrecrystallization. Thickness of deformation bands is about a few micrometers, while that of grain boundaries is reported to be a few nanometers. 14) This means that the different thicknesses between deformation bands and grain boundaries result in different potentials for the phase transformation. Therefore, it is found that not only the surface area but also the thickness of nucleation sites is important during the phase transformation of HSLA steel. Although an increase in S eff causes ferrite grain refinement, for a fixed S eff value, deformation in the nonrecrystallization refines ferrite grains more effectively than that in the recrystallization due to the different thickness in the nucleation sites between deformation bands and grain boundaries. In a sense, general diffusional transformation of HSLA steel controlled by the interface nucleation growth mechanism is accelerated by the deformation bands formed during hot working in the non-recrystallization. 5. Conclusions From the microstructural observation and analysis of austenite/ferrite phase transformation of fine grained Fe- 0.15C-1.1Mn-0.25Si-0.04Nb-0.002B steel during heavy deformation, the following conclusions were drawn: (1) Surface area of grain boundaries is inversely proportional to the grain size for the equi-axed prior austenite grains, while, it increases with increasing the applied strain in the non-recrystallization for the elongated prior austenite grains. In addition, surface area of deformation bands is proportional to the square of strain. (2) Volume fraction of SIDT ferrites increases with an increase in the effective surface area of grain boundaries and deformation bands. The volume fraction of SIDT ferrite nucleated from the elongated prior austenite grains is higher than that nucleated from equi-axed prior austenite grains at the same effective surface area. (3) Although it has been known that only the effective surface area plays an important role in ferrite nucleation, the thickness of nucleation site is also important for the nucleation. Because deformation bands are thicker than the prior austenite grain boundary, the potential of the deformation band for ferrite nucleation is higher than that of prior austenite grain boundaries. (4) Diffusional austenite/ferrite phase transformation of HSLA steel by the interface nucleation and growth mechanism is accelerated by the deformation bands in the nonrecrystallization. REFERENCES 1) F. B. Pickering: Material Science and Technology, 7, ed. by R. W Cahn, P. Haasen and E. J. Krammer, (VCH, 1991) pp ) F. B. Pickering: Physical Metallurgy and Design of Steels, (Applied Science Publishers Ltd., 1978) p ) R. Z. Valiev, N. A. Kransilnikov and N. K. Tsenev: Mater. Sci. Eng. A137 (1991) ) F. Ishikawa and T. Ouch: CAMP-ISIJ 8 (1995) ) J. Choi, H. Ohtsuka, Y. Xu and W. Choo: Scr. Mater. 43 (2000) ) W. Choo: J. Kor. Inst. Met. & Mater. 36 (1998) ) C. Li, H. Yada and H. Yamagata: Scr. Mater. 39 (1998) ) P. D. Hodgson, M. R. Hockson and R. K. Gibs: Scr. Mater. 40 (1999) ) I. Tamura, H. Sekine, T. Tanaka and C. Ouchi: Thermomechanical Processing of High-strength Low-alloy Steels, (Butterworth & Co. Ltd., 1988) pp ) Y. Matsumura and H. Yada: Testu-To-Hange 69 (1983) S ) K. J. Kurzydlowski and B. Ralph: The Quantitative Description of the Microstructure of Materials, (CRC Press, 1995) pp ) I. Kozasu, C. Ouchi, T. Sanpei and T. Okita: Microalloying 75, (Union Carbide Corp., 1977) pp ) K. Tibor and M. Ilija: ISIJ Int. 38 (1998) ) R. M. German: Powder Metallurgy, 2nd ed., (Metal Powder Industries Federation, 1994) p. 152.

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