Materials Science and Engineering A 378 (2004) 304307

Analysis of the martensitic transformation at various scales in TRIP steel

M.R. Berrahmoune a, , S. Berveiller a , K. Inal a , A. Moulin b,1 , E. Patoor a
a

LPMM, UMR CNRS 7554-ENSAM: 4, rue Augustin Fresnel Technop le, 57078 Metz Cedex 3, France o b LEDEPP, 17 Avenue des Tilleuls B.P. 70011, 57191 Florange Cedex, France Received 17 June 2003; received in revised form 29 September 2003

Abstract The mechanical behavior of transformation induced plasticity (TRIP) steels depends on the martensitic transformation of the retained austenite. The studied material is a three-phase TRIP steel with ferrite base containing less than 1% of bainite and 8% of retained austenite. Tensile tests were performed at various temperatures ranging from 60 to +120 C. X-ray diffraction was used to determine the kinetics of transformation at various temperatures. First results show that at low temperatures, the austenite transforms into martensite very rapidly, whereas the kinetics of transformation are much slower at high temperatures. The stress state in the austenite at room temperature was also obtained by X-ray diffraction. After pre-strain, it is noticed that retained austenite is in tension probably due to the carbon content which is more important in austenite than in ferrite. 2004 Elsevier B.V. All rights reserved.
Keywords: TRIP effect; Martensite transformation; X-ray diffraction; Three-phase material; Mechanical behavior

1. Introduction The use of high strength steels with excellent formability becomes a primary objective for economical and safety reasons. In this context, the transformation induced plasticity (TRIP) steels with their high strength and excellent formability compromise can answer to the demand for weight decrease in the automotive industry. Their excellent mechanical properties result from the martensitic transformation of metastable retained austenite, induced by thermomechanical loading. The TRIP steels possess a multi-phase microstructure, consisting typically of ferrite, bainite and retained austenite. The microstructure is obtained after an intercritical annealing and a subsequent isothermal annealing in the bainitic transformation region, called austempering. The carbon content in austenite is increased both during the intercritical annealing and the austempering. The carbon enrichment during austempering is the result of the suppression of the formation of carbides during the bainitic transformation, due to the presence of the alloying elements such as silicon and aluminum. The enrichment of carbon in the austenite
Corresponding author. Tel.: +33-387375430; fax: +33-387375470. E-mail address: reda.berrahmoune@metz.ensam.fr (M.R. Berrahmoune). 1 Tel.: +33-382515241; fax: +33-382514260. 0921-5093/$ see front matter 2004 Elsevier B.V. All rights reserved. doi:10.1016/j.msea.2003.10.372

increases its thermal stability and consequently, the austenite can be retained upon cooling to room temperature [15]. A quantitative determination of the volume fraction of the existing phases, especially the retained austenite, is essential for the evaluation of the TRIP steels properties. Experimental methods that have been reported in the literature include X-ray diffraction (XRD) [16], optical microscopy combined with image analyses [7], scanning electron microscopy [8], dilatometry [9], and magnetic measurements [10]. Among them, the XRD method is the most frequently used as it is a suitable technique. In fact, it allows to study the crystallographic texture of the material, and also to determine the stress state in the material that evolves with the phase transformation. Indeed, internal stresses are generated during phase transformation. These internal stresses come from different sources: The internal stresses resulting from the incompatible transformation strain accompanying martensitic phase transition (shear strain of 0.2 and change in volume of 0.04 for steels) [4]. The internal stresses associated with plastic ow of product and parent phase due to dislocation motion [11]. The present work aims to determine the mechanical behavior of the (commercial) TRIP 600 steel by characterizing the martensitic transformation using XRD.

M.R. Berrahmoune et al. / Materials Science and Engineering A 378 (2004) 304307 Table 1 Chemical composition of the alloy in wt.% (balance iron) Steel TRIP600 C 0.08 Mn 1.70 Si 1.55 P 0.015 Al 0.029

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2. Experimental procedure 2.1. Material and mechanical testing Experiments were performed on thin sheets of rolled TRIP 600 steel (1.5 mm thickness) provided by Arcelor. The chemical composition is given in Table 1. After polishing, specimens were etched with sodium di-sulte and picral solution. The microstructure was investigated using light optical microscopy (LOM). Tensile tests were performed in the rolling direction using at samples with 25mm gauge length and 4mm width. Strain rate of 2.6 103 s1 was used. High temperature tests (80 and 120 C) were done using resistance heated whereas in low temperature tests (0, 30 and 60 C) liquid nitrogen was used. 2.2. Determination of retained austenite content The retained austenite content was measured at the surface of samples by X-ray phase analysis, using Co K radiation. The measuring accuracy of the retained austenite by this method is about 1%. A step scan within the 2 interval between 45 and 150 was done (Fig. 1). The reection intensities were deduced from the pole gures of {2 0 0} and {2 1 1} planes of ferrite/martensite phase, and {2 2 0} and {3 1 1} planes of austenite phase. To compare retained austenite at the surface and in the volume of samples, the magnetic method was used. For magnetic measurements, the full austenite decomposition in the reference sample was obtained by annealing some samples at 600 C for 4 h. 2.3. Determination of residual stresses For stress analysis, we used the classical sin2 method. is the angle between the surface normal and the direc350 300
Intensity (cps)

tion of the strain being measured. In the sin2 method, lattice strains are measured at each -tilt of the specimen. For isotropic materials, macroscopic diffracting plane strain values are linearly dependent on sin2 . The slope of the curve leads to the value of the stress . X-ray measurements were carried out on {3 1 1} crystallographic planes of austenite using Co K radiation. A step width of 0.1 and measuring time of 60 s at 2 angles between 108 and 113 , for each of the 13 angles are chosen. The center of gravity method was used for the determination of the peak positions. Then, corresponding strains were computed and the stresses were calculated by linear analysis regression.

3. Results and discussion 3.1. Microstructure Fig. 2 shows the initial microstructure of the three-phase steel which consists in ferrite base with grains of various sizes from 15 to 20 m, containing bainite islands (dark) located on the grain boundaries and retained austenite islands (white) being inside ferrite grains and also on the grain boundaries. An optical phase proportioning gives 8% of retained austenite and less than 1% of bainite content. The low content of retained austenite makes observation of the martensite formed after pre-strain more difcult. The Ms temperature was measured using differential scanning calorimetry and is about 65 C. 3.2. Mechanical properties The stressstrain curves of the TRIP 600 steel at various temperatures ranging from 60 to +120 C are presented in Fig. 3. At low temperatures (T = 0 C), the curves present a plateau in the beginning of plastic range. This phenomenon can be explained by the fact that at low temperatures, retained austenite is less stable than at high temperatures and transforms to martensite easily. It corresponds to GreenwoodJohnson effect that results in plastic accommodation carried out at constant stress [12]. At higher temperatures (T 20 C), the plateau disappears. The Fig. 4

{1 1 0}

250 200 150 100 50 0 45 65 85 2 105 125 145

{2 1 1}

{2 0 0} {2 2 0} {3 1 1} {2 2 0}g

Fig. 1. 2-scan showing peaks of each phase after a pre strain of 0.5% at 20 C.

Fig. 2. Optical micrograph of TRIP 600 steel. F: ferrite; B: bainite; RA: retained austenite.

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800 700

M.R. Berrahmoune et al. / Materials Science and Engineering A 378 (2004) 304307
30

3 4

uniform elongation A %

25 20 15 10 5 0 -100 -50 0 50 100 150

Stress ( MPa)

600 500 400 300 200 100 0 0 20 40

5 1 --- T = 2 --- T = 3 --- T = 4 --- T = 5 --- T =

60

- 60C - 30C + 20C + 80C + 120C

80

Temperature (C)
Fig. 6. The evolution of uniform elongation as function of temperature.

Strain ( %)
Fig. 3. Tensile stressstrain curves of the TRIP 600 at various temperatures.
460

Yield strentgh (MPa)

450 440 430 420 410 400 390 380 370 -100 -50 0 50 100 150

temperatures above Ms at increasingly higher stresses for increasing temperatures until Ms (point C). Above Ms new nucleation sites are introduced by the plastic strain. So the yield strength of austenite decreases with increasing temperatures. Near Ms both modes will operate [13]. The Fig. 6 represents the evolution of the uniform elongation as a function of the temperature. The elongation increases with temperature until T = 70 C, temperature at which the TRIP effect is maximum. The increase of elongation corresponds to the additional strain which due to GreenwoodJohnson and the Magee effect [12,13]. 3.3. Volume fraction of retained austenite From the Fig. 7, it can be seen that the rate of the transformation is zero at the beginning and gradually increases to a maximum after a considerable amount of strain. After this the rate gradually decreases until no further transformation occurs upon further straining and a limiting value for the martensite content is reached. In the other hand, at low temperatures (60 up to 0 C), the austenite transforms into martensite very rapidly: for = 5% at T = 30 C, the fraction of retained austenite has decreased from 6 to 2%, and it is about 1% at failure. On the contrary, the kinetics of transformation at high temperatures are much slower at

temperature (C)
Fig. 4. The evolution of yield strength as function of temperature.

presents the evolution of yield strength as a function of the temperature. It can be seen that the yield strength decreases with temperature. However, a peak is observed around T = 20 C. This could correspond to Ms temperature that is the transition temperature between the stress-assisted transformation and strain induced transformation domains. Indeed, from the Fig. 5, it can be seen that the mechanism of the transformation depends on the temperature. Spontaneous transformation at pre-existing nucleation sites occurs on cooling to below the Ms temperature (point A). Stress-assisted nucleation on the same sites will occur at

Strain induced nucleation Yield strength of austenite

Stress assisted nucleation A

10 9 8 7 6 5 4 3 2 1 0 0

retained austenite (%)

1- T = -60C 2- T = -30C 3- T = 0C 4- T = 20C 5- T = 80C 6- T = 120C

6 5 4 1 2 3

Stress

MS

MS

Temperature

Md

10

15

20

25

Strain(%)
Fig. 7. The volume fraction of retained austenite as function of strain at various temperatures.

Fig. 5. Schematic representation of stress-assisted and strain-induced regimes of mechanically induced transformation.

M.R. Berrahmoune et al. / Materials Science and Engineering A 378 (2004) 304307 Table 2 Stress values in austenite at different pre-strain determinated by X-ray diffraction Pre-strain (%) 0 0.5 1 Phase Austenite Austenite Austenite Plane {3 1 1} {3 1 1} {3 1 1} Stress (MPa) 75 5 +130 15 +275 5 Remark In compression In tension In tension

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carbon content which is greater in austenite than in ferrite phase. 4. Conclusion Mechanical properties of the TRIP 600 steel were determined using tensile tests at various temperatures ranging from 60 to 120 C. The TRIP effect is maximum for T = 70 C. The temperature Ms was deduced from the yield strength vs. temperature curves, it is about 20 C. The kinetics of transformation are high at low temperatures whereas the transformation is much slower at high temperatures. Stress distribution, determined by X-ray diffraction, shows that after unloading, the austenite phase is in tension. However, measurement on martensite could not be done because of the difculty to distinguish martensite from ferrite peaks. The next step in this work is to distinguish these peaks using deconvolution method. On the other hand, in situ tests will be performed for the determination of stress distribution during the loading. References
[1] H.C. Chen, H. Era, M. Shimizu, Metall. Trans. 20A (1989) 437. [2] W.C. Jeong, D.K. Matlock, G. Krauss, Mater. Sci. Eng. A 165 (1993) 9. [3] O. Matsumura, Y. Sakuma, H. Takechi, Trans. ISIJ Int. 32 (9) (1992) 1014. [4] I.B. Timokhina, P.D. Hodgson, E.V. Pereloma, in: Proceedings of the International Conference on TRIP-Aided High Strength Ferrous Alloys, Ghent, June 2001, p. 153. [5] K. Sugimoto, N. Usui, M. Kobayashi, S. Hashimoto, Trans. ISIJ Int. 32 (1992) 1311. [6] L. Zhao, J. Sietsma, S. Van der Zwaag, P. Neumann, Steels and Materials for Power Plants, vol. 7, Wiley, Weinheim, 2000, p. 77. [7] A. Basuki, E. Aernoudt, Scripta Mater. 40 (1999) 1003. [8] P. Jacques, X. Cornet, P. Harlet, J. Ladrire, F. Delannay, Metall. Mater. Trans. 29A (1998) 2383. [9] A. Ali, M. Ahmed, F.H. Hashimi, A.Q. Khan, Metall. Trans. 24A (1993) 2145. [10] W. Bleck, K. Hulka, K. Papamentellos, Mater. Sci. Forum 284286 (1998) 327. [11] M. Cherkaoui, M. Berveiller, X. Lemoine, Int. J. Plast. 16 (2000) 1215. [12] G.W. Greenwood, R.H. Johnson, Proc. R. Soc. 283A (1965) 403. [13] L. Barb, M. De Meyer, B.C. Cooman, in: Proceedings of the International Conference on Trip-Aided High Strength Ferrous Alloys, Ghent, June 2001, p. 65. [14] Q. Furnmont, P.J. Jacques, T. Pardoen, F. Lani, S. Godet, P. Harlet, K. Conlon, F. Delannay, in: Proceedings of the International Conference on Trip-Aided High Strength Ferrous Alloys, Ghent, June 2001, p. 39.

the beginning. Moreover, the fraction of retained austenite at failure is about 34%. The high rate of transformation at low temperatures is due to the fact that these temperatures are close to Ms and the martensitic transformation is stress assisted. At this stage, the martensitic transformation occurs before the plastic deformation of austenite. At high temperatures, the low kinetics of transformation is due to the high stability of retained austenite. In addition, by XRD analyses (curves 13, 5, and 6) the initial volume fraction of retained austenite is about 6% whereas it is about 8% by magnetic (curve 4) and optical measurements. This can be explained by the fact that during polishing, the retained austenite at the surface of the samples transforms to martensite, and X-ray diffraction measurements are carried out at the surface. To avoid that, it would be necessary to etch samples with electrochemical etching on the depth of 100 m. 3.4. Residual stresses distribution The strain measurements were done only for the austenitic phase only. Measurement on martensite could not be done because it is difcult to distinguish the peak of martensite phase from the peak of the ferrite. Stress values with their uncertainty at different pre-strain in austenite are given in Table 2. It is noticed that the austenite phase is in tension and the stress values increase with increasing pre-strain except at the initial state where the stress value is negative due to surface preparation. However, the fact that austenite phase is in tenI sion ( > 0) shows that this phase is not the softest one. Indeed, the positive residual stresses value in austenite after unloading corresponds to the fact that during the loading, the local behavior of the austenite will be above the macroscopic behavior and then the austenite phase is harder than the ferrite phase. This result is in agreement with nanoindentation tests carried out by Furnmont et al. [14] on different TRIP steels which show that the hardness values increases in the following order: ferrite, bainite, austenite, and martensite. The high value of the austenite hardness is due to the