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MATERIALS CHARACTERIZATION 44:291–299 (2000)

© Elsevier Science Inc., 2000. All rights reserved. 1044-5803/00/$–see front matter 655 Avenue of the Americas, New York, NY 10010 PII S1044-5803(99)00060-1

291

M

icrostructural Characterization of Bainitic Steel

Submitted to Torsion Testing and Interrupted

Accelerated Cooling

A. B. Cota* and D. B. Santos

*Federal University of Ouro Preto, Department of Physics, Ouro Preto, M.G., Brazil; and Federal University of Minas Gerais, Department of Metallurgical and Materials Engineering, Belo Horizonte, M.G. Brazil

HSLA low-carbon bainitic steel containing B was submitted to torsion tests to simulate con-trolled rolling, followed by interrupted accelerated cooling. Microstructural characteristics and the mechanisms for the refinement of structure were evaluated using light microscopy, scanning electron microscopy, transmission electron microscopy, and Vickers hardness test-ing. The final microstructure was found to contain complex mixture of granular bainite, small islands of MA constituent, bainitic ferrite, and polygonal ferrite. Increasing the cool-ing rate or decreascool-ing the finish coolcool-ing temperature resulted in a decrease in the volume fraction and average size of the MA islands and the polygonal ferrite. A finish cooling tem-perature of 400⬚C produced a microstructure consisting of fine laths of bainitic ferrite with an interlath MA constituent. A quantitative relationship between the accelerated cooling variables and the ferrite grain size was developed. © Elsevier Science Inc., 2000. All rights reserved.

INTRODUCTION

In the last 2 decades there have been con-siderable advances in the theory and prac-tice of accelerated cooling after controlled rolling. Several investigations have been conducted with the objective of studying the influence of cooling variables on the mi-crostructure and mechanical properties of High-Strength Low-Alloy (HSLA) low-car-bon bainitic steels [1–6]. The study of the microstructural characteristics of these steels has been carried out using the classification system developed for bainitic and ferritic microstrutures by Krauss and Thompson [7]. Most of the bainitic microstructures ob-served in the low-carbon microalloyed steels can be well described as bainitic fer-rite (acicular ferfer-rite) and granular bainite [with discreet islands of MA (martensite andⲐor residual austenite)].

The MA islands formed in granular bain-ite during the continuous cooling of steels have a strong effect on the mechanical properties [8]. This constituent leads to in-creases in the tensile strength but a deterio-ration in the impact toughness. It also has a small effect on the yield strength. For these reasons, it is very important to understand the influence of cooling variables on the formation of MA islands in the granular bainite.

In the present work, an alternative method, based on hot torsion testing to simulate controlled rolling and on gas-accel-erated cooling, was used to study the influ-ence of cooling rate (CR) and finish cooling temperature (TFC) on the microstructure of

HSLA low-carbon bainitic steel recently de-veloped by the metallurgical industry. The microstructure refinement mechanism and the MA islands (granular or equiaxed

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mor-292 A. B. Cota and D. B. Santos

phology) formation mechanism are dis-cussed. A quantitative relationship between these cooling variables and the ferrite grain size was obtained by multiple regression analysis.

EXPERIMENTAL PROCEDURE The chemical composition of the steel used in this investigation is given in Table 1. Tu-bular torsion specimens, having a gauge length of 16.5mm, 6.5mm outer, and 2mm inner diameter, were used to study micro-structural characteristics after interrupted accelerated cooling. A thermocouple, con-nected to an interface card installed in a personal computer, was placed inside the specimen, allowing control of the thermal profiles during thermomechanical process-ing and data collection of the coolprocess-ing curves.

The specimens were deformed using a nine-pass torsion test. They were reheated

to 1200⬚C for 15 min and, while cooling

down at a rate of 1⬚CⲐs, they were submit-ted to five passes at temperatures above the

nonrecrystallization temperature (Tnr ⫽

970⬚C), followed by four passes below this temperature. A strain per pass of ⑀ ⫽ 0.2 and a strain rate of ⫽ 2 s⫺1 were used.

De-tails of the temperature of each pass during of the hot torsion experiments are given in Fig. 1.

The continuous cooling transformation (CCT) diagram of this steel (Fig. 2) was de-termined by thermal analysis of the cooling curves from deformed austenite according to the nine-pass torsion test schedule de-scribed above [9]. This diagram was uti-lized in the selection of the cooling rates and finish cooling temperatures used after the thermomechanical processing, and are

⑀ •

also indicated in Fig. 1. The cooling rates measured correspond to average values for the temperature range of 800 to 500⬚C.

The cooling rate and the finish cooling temperature after deformation were con-trolled by means of a cooling device using helium and a control panel, which permitted close regulation of the helium flow rate [10]. Samples for metallographic observation and Vickers hardness (VH) measurements (4.905N load) were sectioned longitudi-nally, producing a plane tangential to the gauge length to the torsion specimens. Two percent nital and LePera’s etchants [11] were used to examine the microstructures. The samples were observed by light croscopy (LM) and scanning electron mi-croscopy (SEM). Volume fractions and di-mensions analyses of the constituents were performed using computerized image

anal-ysis, IMAGE PRO-PLUSTM, from light

mi-croscopy. More detailed microstructural characterization, for selected cooling rates and finish cooling temperatures, was con-ducted using transmission electron micros-copy (TEM) of thin foils in a bright-field mode.

RESULTS AND DISCUSSION MICROSTRUCTURE

Figure 3 shows the microstructure corre-sponding to a specimen quenched after the last pass of the nine-pass test. Elongated austenite grains are observed, revealing that accumulation of deformation has taken place during hot working in the low-tem-perature range. The elongated grains have, in the plane of observation, an approximate aspect ration of 4:1, given an average value of 40 ␮m.

Table 1 Chemical Composition of the Steel (wt. %)

C Mn Si P Al Nb V Ti Ni B S N

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Bainitic Steel 293

The combined effects of cooling rate and finish cooling temperature on the micro-structure are illustrated in Figs. 4 (LM pho-tomicrographs) and 5 (SEM photomicro-graphs). It can be seen from Figs. 4(a) and 5(a) that the microstructure associated with

the highest finish cooling temperature (TFC ⫽ 650⬚C) exhibits a mixture of fine

polygonal ferrite (with a volume fraction ⬇ 12%), granular bainite, and small islands of the MA constituent. The MA constituent has a granular or equiaxed morphology

(volume fraction ⬇ 4.5% and with islands

FIG. 1. Schematic representation of the controlled rolling and accelerated cooling simulation.

FIG. 2. CCT diagram of the HSLA bainitic steel

deter-mined via thermal analysis of the cooling curves from deformed austenite using nine-pass torsion testing [9].

FIG. 3. Light photomicrograph of the austenitic

micro-structure of sample quenched after the last pass of the nine-pass test.

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294 A. B. Cota and D. B. Santos

of average size less the 2␮m). By contrast, the microstructures associated with the next

lower finish cooling temperature (TFC ⫽

500⬚C) [Figs. 4(b) and 5(b)] consist of granu-lar bainite and bainitic ferrite. A small amount of polygonal ferrite is also in evi-dence in these microstructures.

In the case of the two higher finish cool-ing temperatures (TFC⫽ 650⬚C and TFC ⫽

600⬚C), the MA islands are distributed

practically uniformly throughout the bain-ite matrix (Fig. 6). This figure, a compila-tion of binary images in which the MA is-lands appear white, shows that the increase in cooling rate or decrease in finish cooling temperature implies a decrease in the vol-ume fraction and the average size of the MA islands.

Figures 4(c)–(d) and 5(c)–(d) show that, for the lowest finish cooling temperature, TFC ⫽ 400⬚C, the microstructure is

essen-tially bainitic, with fine laths of bainitic

fer-rite and interlath MA constituent. It can be seen from Fig. 5(c), CR ⫽ 6.3⬚CⲐs, that the microstructure contains a small amount of polygonal ferrite. Figure 7(a)–(d), TEM mi-crographs of samples cooled at rates of 6.3⬚CⲐs and 33⬚CⲐs for TFC⫽ 400⬚C, shows

that the width of the bainitic ferrite laths decreases with increasing cooling rate, and that the widths can be as narrow as 0.2␮m. No evident interlath carbides were ob-served in this steel under present condi-tions. The refinement of bainitic ferrite by increasing the cooling rate could be due to the following: when the cooling rate in-creases, the reduction in the bainite trans-formation start temperature, Bs, leads to an

increase in the driving force (the difference in free energy between the austenite phase and the ferrite phase) for the nucleation rate of subunits of ferrite and, conse-quently, to a decrease in the width of the bainitic ferrite laths. The increase in the

FIG. 4. Light photomicrographs of samples cooled at different rates and with different finish cooling

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Bainitic Steel 295

cooling rate leads to a continuous increase inthe Vickers hardness from 262 to 320.

The analysis of the optical, SEM, and TEM photomicrographs reveals that the cooling variable of greater influence on the bainite morphology is the finish cooling temperature. When the finish cooling tem-perature decreases from 650 to 400⬚C, it can be observed that the ferrite crystals change from their granular morphology with the presence MA islands (by default, these is-lands have granular or equiaxed shapes re-solvable in light micrographs) to finer fer-rite crystals with laths morphology (MA constituent is retained between the ferrite laths with acicular morphology).

Figures 8(a)–(b) and 9(a)–(b) show the in-fluence of the cooling rate on the volume fraction and average size of the MA islands and the polygonal ferrite, associated with the various finish cooling temperatures, re-spectively. The results show that the

in-crease in the cooling rate or the dein-crease in the finish temperature leads to a decrease in the volume fraction and the average size of the MA islands and the polygonal ferrite. For TFC ⫽ 400⬚C no MA islands were

de-tected.

FERRITE GRAIN SIZE

A quantitative relationship between the cooling variables and the ferrite grain size was obtained by means of multiple regres-sion analysis. The statistical treatment was carried out by taking the cooling rate and the finish cooling temperature as indepen-dent variables. The following equation was obtained:

(1) where R is the multiple correlation coeffi-cient, d␣ is ferrite grain size. The values

en-closed in the parentheses indicate 95% of dα = 0.12 CR( )–0.27(TFC)0.67 R= 97.2%

FIG. 5. SEM photomicrographs of samples cooled at different rates and with different finish cooling temperatures:

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296 A. B. Cota and D. B. Santos

confidence level. Figure 10 shows that the correspondence between measured and pre-dicted [Eq. (1)] ferrite grain size is quite close, and discrepancies observed are very small.

The effectiveness of cooling rate on the ferrite grain size appears to be reduced as the finish cooling temperature is decreased. The grain size is reduced from 5.6 to 3.7␮m for an increase in the cooling rate from 6.3 to 33⬚CⲐs for TFC ⫽ 650⬚C. Under the same

conditions for TFC ⫽ 500⬚C, d␣ is reduced

from 4.6 to 3.2␮m. From Eq. (1), when the cooling rate increases tenfold, the ferrite grain size is reduced to almost half (0.54).

MA CONSTITUENT

The formation of MA islands is a process controlled by carbon diffusion. Therefore, it

FIG. 6. Binary images of samples cooled at different rates and with different finish cooling temperatures: (a) 6.3⬚CⲐs,

650⬚C; (b) 13.0⬚CⲐs, 650⬚C; (c) 33⬚CⲐs, 650⬚C; (d) 6.3⬚CⲐs, 500⬚C; (e) 13.3⬚CⲐs, 500⬚C; (f) 33⬚CⲐs, 500⬚C. LePera’s etchant; MA constituent is white.

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Bainitic Steel 297

was expected that both the cooling rate and finish cooling temperature would influence the average size and volume fraction of the MA islands. The displacive model has been proposed and accepted [12–15] for the ki-netics of bainite transformation. In this model the nucleation of ferrite occurs by a diffusional mechanism, and longitudinal

growth takes place by a displacive mecha-nism. The growth of ferrite laths (or plates) is controlled by the repeated nucleation of subunits (individual ferrite laths), and its nucleation rate strongly depends on the driving force for the phase transformation reaction. Diffusionless growth requires that transformation occurs at a temperature

be-FIG. 7. TEM photomicrographs of samples cooled at different rates but with the same finish cooling temperature:

(a) 6.3⬚CⲐs, 400⬚C; (b) 33⬚CⲐs, 400⬚C.

FIG. 8. Influence of cooling rate on: (a) the volume

fraction of the MA islands (fMA); (b) the average size of

the MA islands (dMA).

FIG. 9. Influence of cooling rate on: (a) the volume

fraction of the polygonal ferrite (fPF); (b) the average

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298 A. B. Cota and D. B. Santos

low To, when the free energy of bainite

be-comes less than that of austenite of the

same composition. The To curve defines

temperatures at which austenite and ferrite of the same composition have equal free energy (Fig. 11). While the austenite–bain-ite transformation proceeds, any excess car-bon is rejected into the residual austenite. When carbon-enriched residual austenite is continuously cooled to a temperature be-low the martensite transformation start temperature (Ms), it will transform to an

MA constituent.

An increase in the cooling rate causes a decrease in the bainite transformation start temperature (Bs) (Fig. 2) and, consequently,

an increase in the difference of free energy between austenite and bainite, as shown in Fig. 11. The free energy of the austenite will rise from ␥1 to ␥2, and the To curve shifts

from To1 to To2. This results in an increased

amount of bainite and in a smaller amount of retained austenite, which subsequently transform into MA islands. This can ex-plain why the amount of the MA islands decreases when the cooling rate increases.

The finish cooling temperature also influ-ences the dimensions and volume fraction of MA islands. For a given cooling rate and for a higher finish cooling temperatures (e.g., 600⬚C), bainite has not yet started to

form, or is only in the very initial stages of development. During the subsequent slow cooling in air (1⬚CⲐs), the sample remains for a long enough time at temperatures where diffusion of carbon atoms over long distances is still possible. The bainite trans-formation, already initiated during acceler-ated cooling, can then continue until zones of stable carbon-enriched austenite are formed, which will become lower tempera-ture MA islands. When the finish cooling temperature is smaller, the formation of bainite is already at an advanced stage at the point of interruption of the accelerated cooling, and is brought to completion dur-ing the subsequent air cooldur-ing. In this case, the sample remains a very small time at temperatures where diffusion of carbon at-oms over long distances is still possible. During the austenite–bainite transforma-tion the carbon is rejected into the adjacent residual austenite, reducing the volume fraction and the size of the MA islands.

CONCLUSIONS

The effects of interrupted accelerated cool-ing on the microstructural characteristics of the HSLA low-carbon bainitic steel were FIG. 10. Correlation between measured and predicted

ferrite grain size (d␣).

FIG. 11. Schematic dependence of carbon

concentra-tion vs. free energy of austenite (␥, and bainite (␣B)

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Bainitic Steel 299 studied, and the following conclusions

were reached.

For the conditions of accelerated cooling applied in the present work, the final mi-crostructure consists of a complex mixture of granular bainite, small MA islands, bai-nitic ferrite, and polygonal ferrite. For TFC⫽

400⬚C, the microstructure is essentially bai-nitic, with fine laths of bainitic ferrite with an interlath MA constituent. No evident in-terlath carbides could be observed in this steel.

The increase in the cooling rate or the de-crease in the finish cooling temperature re-sults in decreasing volume fraction and average size of the MA islands and the poly-gonal ferrite.

A quantitative relationship between the cooling variables and ferrite grain size is proposed. The empirical equation shows that the cooling rate has a stronger influ-ence than the finish cooling temperature on the ferrite grain size.

The authors are grateful for the financial support of CNPq and FAPEMIG. The authors also thank Usiminas S.A. for supplying the material used in this work.

References

1. P. Bufalini, M. Prontemolli, M. Chersi, A. Aprile, and C. Jannone: Optimizing the Microstructure and

the Strengthening Factors in High Strength Plates Produced by Accelerated Cooling. Proc. Int. Conf. on

Accelerated Cooling of Steels, Pittsburgh, PA, pp. 387–400 (1985).

2. L. E. Collins, G. E. Ruddle, A. F. Crawley, and J. D. Boyd: Accelerated Cooling of a Nb-V Microalloyed

Plate Steel. Proc. Int. Conf. on Accelerated Cooling

of Rolled Steels, Winnipeg, Canada, pp. 57–70 (1987).

3. M. Pontremoli, P. Bufalini, A. Aprile, and C. Jan-none: Development of grade APIX80 pipeline steel plates produced by controlled rolling. Metals

Tech-nol. 11:504–514 (1984).

4. P. C. Rodrigues, A. B. Cota, and D. B. Santos: Effect

of Cooling Conditions on the Microstructure and Me-chanical Properties of a HSLA Bainitic Steel. Proc. Int.

Conf. on Thermomechanical Processing of Steel and Other Materials, THERMEC’97, Wollongong, Australia, pp. 787–792 (1997).

5. E. V. Perolama and P. D. Hodgson: Microstructural

Characterization of Strip Steel after Simulated Thermo-mechanical Processing and Accelerated Cooling. Proc.

Int. Conf on Thermomechanical Processing of Steel and Other Materials, THERMEC’97, Wollon-gong, Australia, pp. 803–809 (1997).

6. J. G. Willians, C. R. Killmore, P. D. Edwards, and P. G. Kelly: Thermomechanical Processing of Mo-Nb

High Strength Steels for Application to X70 and X80 ERW Linepipe. Proc. Int. Conf. on

Thermomechani-cal Processing of Steel and Other Materials, THERMEC’97, Wollongong, Australia, pp. 475– 482 (1997).

7. G. Krauss and S. W. Thompson: Ferritic micro-structures in continuously cooled low and ultra-low carbon steels. ISIJ Int. 35:937–945 (1995). 8. S. W. Thompson and G. Krauss: Structure and

Properties of Continuously Cooled Bainitic Ferrite– Austenite–Martensite Microstructures. Proc. Int.

Conf. on Mechanical Working and Steel Process-ing, Chicago, IL, pp. 467–481 (October 1989). 9. A. B. Cota, P. J. Modenesi, R. Barbosa, and D. B.

Santos: Determination of CCT diagrams by ther-mal analysis of a HSLA bainitic steel. Scripta

Mater. 40:165–169 (1999).

10. A. B. Cota: Simulação da Laminação Controlada e Resfriamento Acelerado em um Aço ARBL Bainit-ico de Baixo Carbono atrevés de Ensaios de Torção, Ph.D. Thesis, Federal University of Minas Gerais, Brazil (1998).

11. F. S. LePera: Improved etching technique to em-phasize martensite and bainite in high-strength dual-phase steel. J. Metals 38–39 (1980).

12. H. K. D. H. Bhadeshia and J. W. Christian: Bainite of steels. Metall. Trans. A 21A:767–797 (1990). 13. R. W. K. Honeycombe and H. K. D. H. Bhadeshia:

Steels: Microstructure and Properties. Edward

Ar-nold Ltd., London, pp. 115–139 (1995).

14. E. Mazancová and K. Mazanec: Physical metal-lurgy characteristics of the MA constituent forma-tion in bainite granular. J. Mater. Process. Technol. 64:287–292 (1997).

15. S. Yamamoto et al.: Effects of the austenite grain size and deformation in the unrecrystallized aus-tenite region on bainite transformation behavior and microstructure. ISIJ Int. 35:1020–1026 (1995).

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