Beruflich Dokumente
Kultur Dokumente
To cite this article: M. Azuma, S. Goutianos, N. Hansen, G. Winther & X. Huang (2012) Effect
of hardness of martensite and ferrite on void formation in dual phase steel, Materials Science
and Technology, 28:9-10, 1092-1100, DOI: 10.1179/1743284712Y.0000000006
This paper is part of a special issue on ‘Hardness across the multi-scales of structure and loading rate’
1
Nippon Steel Corporation, 6-1, Marunouchi 2-Chome, Chiyoda-Ku, Tokyo Experimental
100-8071, Japan
2
Materials Research Division, Risø National Laboratory for Sustainable Materials
Energy, Technical University of Denmark, Roskilde DK-4000, Denmark
3
Danish–Chinese Center for Nanometals, Materials Research Division, An alloy was melted as a 20 kg ingot in a vacuum
Risø National Laboratory for Sustainable Energy, Technical University of furnace. The chemical composition is listed in Table 1.
Denmark, Roskilde DK-4000, Denmark Carbon is one of the most important alloying elements
*Corresponding author, email xiaoxu.huang@risoe.dk when producing dual phase steels, as it affects not only
the volume fraction of martensite but also the hardness related to the tensile properties and strain distribution in
of martensite. Dual phase steels of 590 MPa grade have the ferrite grains and the strain partitioning between
,0?1 wt-%C and from 10 to 20 vol.-% martensite,8–11 martensite and ferrite during deformation. In order to
and in the present steel, 0?1 wt-% carbon addition distinguish ferrite grains from martensite particles,
produced ,20 vol.-% martensite. Manganese was added hardness tests were carried out after polishing and
to retard pearlite transformation during cooling, since, etching by nital. In the nanohardness test, the penetra-
in steel without Mn, pearlite transformation occurs very tion depth was 50 nm, and an indenter with Berkovich
rapidly and most austenites transform to pearlites. geometry was used. The indent size by nanohardness test
Sulphur and oxygen often exist as sulphides and oxides was much smaller than the grain/particle size. In the
in steels, and they have a negative effect on the Vickers tests, the load was 10 gf, and the loading time
mechanical properties because of void formation at was 10 s. The indent size in the Vickers hardness test was
inclusions.21,30–32 Then, an electrolytic iron, with a relatively large, and only the hardness of large grains
sulphur content of ,0?001 wt-%, was used to remove and large particles was measured. In addition, the
the influence of sulphides and oxides. The ingot was average hardness of the specimen was measured by
annealed to 1200uC for 1 h in an argon atmosphere, hot loading of 1 kgf, and the values for 10 areas were
rolled from 45 to 3 mm thickness, cooled slowly from averaged.
a hot rolling finishing temperature of 950–650uC to
promote ferrite formation, then water cooling to In situ tensile testing
ambient temperature and transformation of austenite Tensile tests and three point bending tests were carried
into martensite. Samples have been tempered from 300 out in SEM. For in situ tensile testing, 0?1562?8630 mm
to 600uC as such a treatment may change the hardness specimens were machined, and a hole with a diameter of
of martensite without affecting the volume fraction and 1 mm was made in the centre of the specimen. All
size of ferrite and martensite.29 A short holding time specimens were polished and etched before deformation.
of 100 s has been applied to prevent carbides from The sample was clamped at both ends and stretched
coarsening as void formation can be enhanced by under displacement control in a screw driven load cell,
decohesion at the interface between ferrite and large which was installed inside the microscope. The specimen
particle and also by coarsening of such large particles.32 was strained gradually, and the surface structure was
characterised during loading. During the test, a number
Initial microstructure of parameters were determined, as they can underpin an
The initial microstructures were observed in an SEM analysis of nucleation and growth of voids: size of voids
after polishing and etching by nital (96%C2H5OHz and nucleation density and length and area fraction of
4%HNO3), which allows improved identification of voids. These parameters have been related to a strain
martensite particles. Five areas were observed at a parameter, which is defined in the following section. For
magnification of 62000. However, the microstructure more details, see Ref. 33.
at the centre of the specimen was not examined to avoid
the effect of Mn segregation. The grain size was measured
Strain parameters
in the transverse direction and in the direction normal to During in situ testing, a local strain at the bottom of one
the rolling direction by a linear intercept method, and the hole eh is estimated based on measurement of gauge
average value was defined as the grain size. The aspect length at the bottom.33 The strain in the tensile direction
ratio of the martensite particles was determined as the is defined as a local strain during in situ testing as the
length in the transverse direction divided by the length in deformation localises at the edge of the hole. A gauge at
the normal direction. The volume fraction of each phase this position was defined based on SEM observations. At
was measured by a point counting method. first, a 100 mm gauge was defined by SEM observation, in
which the distance was estimated based on the visible
Mechanical testing microstructure. The length change of the gauge was
Tensile testing directly followed during the in situ tests. If the gauge
length is too small, few grains exist in the gauge, and a
Flat dog bone specimens of dimensions 36356180 mm
strain does not represent an average value of the specimen
were deformed in tension. The gauge length was 50 mm,
because each grain has a different strain due to different
and the gauge width was 25 mm. The tensile direction
crystal orientations and distribution of martensite parti-
was parallel to the transverse direction of the rolled
cles. On the other hand, since deformation concentrates
sheet. The following parameters have been determined:
at the bottom of the hole, a large gauge length might lead
yield stress (YS), ultimate tensile strength (UTS), uni-
to an underestimation of the strain. In addition, strains in
form elongation and total elongation.
martensite eM and ferrite eF are also important para-
Hardness testing meters to underpin an effect during straining of the
The initial microstructure was characterised by nanoin- hardness of the two phases.34–36 The changes in these
dentation (Hysitron, TriboIndenter TI-950) and by parameters were followed during the initial test by
Vickers hardness test (a Struers DuraScan 70 hardness). measuring the length changes of martensite particles
In particular, the hardness of martensite and ferrite in and ferrite grains. Two hundred grains/particles were
the specimens before deformation was measured and measured, and average values are given as eM and eF. An
additional and important parameter is the local strain in
Table 1 Chemical composition/wt-% the necked region of a martensite particle eL, which is
located at a concave part of the particle, which may be
C Si Mn P S N O present before straining or it may form during straining.
During in situ testing, the strains in the necked region of
0.099 0.01 1.63 ,0.001 0.0007 0.0008 ,0.0010 martensite particles were measured directly, and a strain
Table 3 Volume fraction and grain size of dual phase steel studied
Discussion
In situ tensile tests have revealed that most voids formed
in martensite due to (i) plastic deformation of martensite
particles, (ii) crack formation in the particles, (iii) crack
propagation in the particles and (iv) separation of the
particle fragments. The tests have also shown that
softening of martensite through tempering treatments
retards void (crack) formation in dual phase steel and
thereby improves the formability. As plastic deforma-
tion of the martensite particles preceded void formation
in martensite, plastic deformation of martensite has an
important role to play in void formation in martensite.
In this section, the effect of softening of martensite on
the deformation behaviour of martensite and ferrite is
discussed.
Strain distribution in martensite and ferrite
During the processing of dual phase steel, a difference in
thermal contraction between the two phases and the
transformation from austenite to martensite can lead to
a build-up of internal stresses. Such stresses can be
relaxed by the formation and motion of dislocations,
which will be stored in the structure. During plastic
deformation of dual phase steel, the largest stresses are
expected at the interface between ferrite and martensite,
and their magnitude will depend on the hardness
difference between the two phases. A high hardness
difference will create a large stress, which means that a
tempering treatment reducing the difference (Fig. 2) will
reduce the stress at the martensite particle interface. In
general, this stress can be relaxed by generation and
motion of dislocations, but relaxation can also take
place by interfacial decohesion and crack formation in
martensite or ferrite.
Dislocations are generated and stored in the structure
3 Shape of indent after the hardness tests: a SEM image both during the processing of dual phase steel and
of an indent in the martensite phase and b SEM image during plastic deformation. These dislocations can be
of an indent in the ferrite phase by the Vickers hard- classified41 as (i) statistically stored dislocations with a
ness tests, and c Scanning probe microscopy image of density that is proportional to the applied stress and
indents by the nanohardness test. In the Vickers hard- inversely proportional to the slip length and (ii)
ness test the load was 10gf and in the nanohardness geometrically necessary dislocations caused by a local
test penetration depth was 50nm. The indents are non-uniform strain at a hard phase. The density of these
marked in the figure and the indent sizes in the nano- dislocations is proportional to the strain and increases
hardness test are much smaller than the particle/grain with an increasing volume concentration and a decreas-
size ing size of the hard phase. However, the density of
a in martensite; b in ferrite
6 Influence of tempering treatments on void number den-
sity in dual phase steel during in situ tensile test
7 Strain distribution, which is represented by deviation of Euler angle at each point from average vale, in ferrite at strain
of 0?05: initial microstructures a without tempering, b tempered at 300uC and c 500uC and deformed microstructure d
without tempering treatments, e tempered at 300 and 500uC. In contour maps, black regions are martensite and yellow,
blue and green regions are ferrite. In yellow regions, deviation was 0u; in blue region, deviation is larger, and in green
regions, deviation is over 7u
reduced by tempering. Finally, it can be observed that implies that the shape of the martensite particles is one of
green regions were often aligned across some ferrite the most important factors affecting void formation in
grains and martensite particles in the 30–60u direction dual phase steels. As strain is also observed to be localised
from the tensile direction. The strain distribution was at the tip of the martensite particles, void formation at
observed in more detail, and Fig. 8 exemplifies typical such positions must also be expected.
misorientation change at the martensite/ferrite interface The present study illustrated the use of EBSD as a
in the marked area in Fig. 7d. Accumulated misorienta- powerful technique to estimate the local deformation
tion profiles were measured at the concave interface (C-F/ behaviour in dual phase steel. However, one limitation is
M) and the flat interface (F-F/M) between martensite and that a poor image quality makes it difficult to analyse
ferrite, and the ferrite/ferrite grain boundary (F/F). the magnitude and distribution of the strain near the
Figure 8a is an inverse pole figure, and Fig. 8b is a band concave part of the martensite particles due to a very
contrast map (an image quality map). In the map, high dislocation density. This may also be an inherent
martensite is dark due to a large dislocation density. difficulty when replacing EBSD with TEM. This means
Figure 8c shows the accumulated misorientation profiles that nanoindentation has a potential as a complemen-
along each line in Fig. 8a. The misorientation increased at tary technique to further elucidate strain and stress
the interface between martensite and ferrite. In particular, distribution in dual phase steel. Figure 8 illustrates in
the change at the concave interface (8u/1 mm) was larger non-tempered dual phase steel that the accumulated
than the flat interface of the martensite particle (2?7u/ misorientation is much more pronounced at the concave
1 mm). On the other hand, the misorientation changed part of martensite than at the flat part. It also shows that
less at the ferrite/ferrite grain boundary (,1u/1 mm). As this effect appears to extend 2–3 mm from the particle
dislocations lead to lattice rotation, Fig. 8 shows that a interface. Note also that there is a relatively small build-
large number of dislocations are present at the concave up of accumulated misorientation near the ferrite
interface, and consequently, a high stress might lead to boundaries.
local plastic deformation at the concave part of marten- It appears that the effect of tempering (Fig. 9) is to
site. As shown in Fig. 5, slip band formation around the make martensite more deformable and ferrite less
concave part of the martensite particles and necking of deformable due to a different stress and strain partition-
the martensite particles supplement that deformation is ing between the two phases. This effect of softening of
localised at this part of the martensite particles. It is reinforcements leads to more deformation in the reinfor-
apparent that the strain localisation at the concave part of cements but less deformation in a matrix in dual phase
martensite accelerated void formation in martensite. This steels and a ferrite–pearlite steel.34,35,43,44 Tasan et al.43
Conclusions
In dual phase steel, the influence of softening of
martensite through tempering treatments at 300–600uC
on void formation in martensite and ferrite has been
8 Electron backscatter diffraction maps of dual phase steel
without tempering after tensile deformation to strain of
0?05: a inverse pole figure and b band contrast map of
martensite containing concave parts and ferrite grains
and c accumulated misorientation profiles from concave
interface between ferrite and martensite (C-F/M), flat inter-
face between ferrite and martensite (F-F/M) and ferrite/fer-
rite grain boundary (F/F) to another interface. In band
contrast map, dark contrast is related to martensite and
due to large dislocation density. Tensile direction is hori-
zontal. Step size is 50 nm
investigated by tensile testing of bulk specimens and by 9. S. K. Han and H. Margolin: Mater. Sci. Eng. A, 1989, A112, 133–
141.
in situ tensile tests in SEM. Martensite and ferrite have
10. X. J. He, N. Terao and A. Berghezan: J. Mater. Sci., 1984, 18, 367–
been characterised by nano- and microhardness tests. 373.
Based on the microstructural observation, deformation 11. G. Avramovic-Cingara, C. H. A. R. Saleh, M. K. Jain and D. S.
and void formation behaviour have been related to the Wilkinson: Metall. Mater. Trans. A: Phys. Metall. Mater. Sci.,
structure and properties of martensite and ferrite. 2010, 40A, 3117–3127.
12. G. Avramovic-Cingara, Y. Ososkov, M. K. Jain and D. S.
1. Softening of martensite through tempering treat- Wilkinson: Mater. Sci. Eng. A, 2009, A516, 7–16.
ments at 300–600uC significantly increases the elonga- 13. Y. Toji, S. Takagi, K. Yoshino, K. Hasegawa and Y. Tanaka:
tion, counterbalanced by a reduction in strength. In Tetsu-to-Hagane, 2009, 95, 81.
particular, post-uniform elongation was increased sig- 14. A. F. Szewczyk and J. Gurland: Metall. Trans. A, 1982, 13A, 1821–
1826.
nificantly. The tempering introduced a yield point effect
15. C. Landron, O. Bouaziz, E. Maire and J. Adrien: Scr. Metall.,
followed by an increase in yield stress. On the other 2010, 63, 973–976.
hand, the tempering treatments affect less the hardness 16. E. Maire, O. Bouaziz, M. Di Michiel and C. Verdu: Acta Metall.,
of ferrite and the grain size, shape and volume fraction 2008, 56, 4954–4964.
of martensite. 17. R. K. Ray: Scr. Metall., 1984, 18, 1205–1209.
18. M. Sarwar and R. Priestner: J. Mater. Sci., 1996, 31, 2091–2095.
2. Cracks and voids have been observed at different 19. E. Ahmad, T. Manzoor and N. Hussain: Mater. Sci. Eng. A, 2009,
sites in the martensite phase, in the ferrite phase and at A508, 259–265.
inclusions both before and after tempering. At a given 20. D. L. Steinbrunner, D. K. Matlock and G. Krauss: Metall. Trans.
strain, the majority of voids formed in the martensite. A, 1988, 19A, 579–589.
21. E. Erdogan: J. Mater. Sci., 2002, 37, 3623–3630.
3. The voids in martensite evolve in four steps: plastic
22. M. Calcagnotto, Y. Adachi, D. Ponge and D. Raabe: Acta Metall.,
deformation of martensite, crack initiation at the 2011, 59, 658–670.
martensite/ferrite interface, crack propagation leading 23. J. Kadkhodapour, A. Butz, S. Z. Rad and S. Schmauder: Int.
to fracture of martensite particles and void formation by J. Plast., 2011, 59, 2575–2588.
separation of particle fragments. 24. X. Fang, Z. Fan, B. Ralph, P. Evans and R. Underhill: J. Mater.
Process. Technol., 2003, 132, 215–218.
4. Void formation in martensite depends on a critical 25. F. H. Samuel: Metall. Trans., 1985, 75, 51–66.
strain for void formation in martensite and local strain 26. A. Joarder, J. N. Jha, S. N. Ojha and D. S. Sarma: Mater. Charact.,
at the concave part of martensite. Softening of mar- 1990, 25, 199–209.
tensite through tempering treatments improves the 27. K. Hasegawa, K. Kawamura, T. Urabe and Y. Hosoya: ISIJ Int.,
2004, 44, 603–609.
critical strain and decreases the local strain at the 28. Y. Tomota, H. Yoshino and K. Kuroki: Scr. Metall., 1977, 11,
concave parts; midland increases strain partitioning 853–856.
between martensite and ferrite. Therefore, the tempering 29. O. R. Jardim, W. P. Longo and K. K. Chawla: Metallography,
treatments retard void formation in martensite and 1984, 17, 123–130.
thereby improve the formability. 30. S. B. Hosseini, C. Temmel, B. Karlsson and N.-G. Ingesten:
Metall. Mater. Trans. A: Phys. Metall. Mater. Sci., 2007, 38A, 982–
989.
Acknowledgements 31. W. Roberts, B. Lehtinen and K. E. Easterling: Acta Metall., 1976,
24, 745–758.
The authors thank Nippon Steel Corporation for the 32. J. Gurland: Acta Metall., 1972, 20, 735–741.
financial support and for producing the steel sheets used 33. M. Azuma, S. Goutianos, N. Hansen, G. Winther and X. Huang:
in the present study, and the Danish National Research Proc. 31th Risø Int. Symp. on ‘Material science’, Roskilde,
Denmark, September 2010, Risø National Laboratory, 243–250.
Foundation and the National Natural Science Found- 34. Y. L. Su and J. Gurland: Mater. Sci. Eng., 1987, 95, 151–165.
ation of China (grant no. 50911130230) for supporting 35. H. P. Shen, T. C. Lei and J. Z. Liu: Mater. Sci. Technol., 1986, 2,
the Danish–Chinese Center for Nanometals, within 28–33.
which part of the present work was performed. 36. F. B. Pickering: in ‘Hardenability concepts with applications to
steel’, (ed. D. V. Daone and J. S. Kirkaldy), 229; 1978, Warrendale,
PA, AIME.
References 37. S. Nishijima, A. Ishii, K. Kanazawa, S. Matsuoka and C. Masuda:
‘Fundamental fatigue properties of JIS steels for machine structural
1. R. G. Davies: in ‘Formable HSLA and dual phase steels’, (ed. A. T. use’, 77; 1989, Ibaraki, National Research Institute for Metals.
Davenport), 25–39; 1977, Warrendale, PA, TMS-AIME. 38. J. Lian, Z. Jiang and J. Liu: Mater. Sci. Eng. A, 1991, A147, 55–65.
2. A. R. Marder and B. L. Bramfitt: in ‘Structure and properties of 39. Z. Jiang, Z. Guan and J. Lian: Mater. Sci. Eng. A, 1995, A190, 55–
dual-phase steels’, (ed. R. A. Kot and J. W. Morris), 145–82; 1979, 64.
Warrendale, PA, TMS-AIME. 40. N. A. Stelmashenko, M. G. Walls, L. M. Brown and Y. V. Milman:
3. M. Mazinani and W. J. Poole: Metall. Mater. Trans. A: Phys. Acta Metall. Mater., 1993, 41, 2855–2865.
Metall. Mater. Sci., 2007, 38A, 328–39. 41. M. F. Ashby: Philos. Mag., 1970, 21, 399.
4. O. Akisue and M. Usuda: Nippon Steel Technical Report no. 57, 42. C. Y. Barlow and N. Hansen: Acta Metall. Mater., 1991, 39, 1971–
11–15, Nippon Steel Corporation, Tokyo, Japan, 1993. 1979.
5. S. Matsuoka, K. Hasegawa and K. Tanaka: JFE Technical Report 43. C. C. Tasan, J. P. M. Hoefnagels and M. G. D. Geers: Scr. Metall.,
no. 10, 13–18, JFE Steel Corporation, Tokyo, Japan, 2007. 2010, 62, 835–838.
6. K. Kishida: Nippon Steel Technical Report no. 81, 12–16, Nippon 44. H. Ghadbeigi, C. Pinna, S. Celotto and J. R. Yates: Mater. Sci.
Steel Corporation, Tokyo, Japan, 2000. Eng. A, 2010, A527, 5026–5032.
7. M. Delincé, Y. Bréchet, J. D. Embury, M. G. D. Geers, P. J. 45. A. Melander and J. Steninger: Mater. Sci. Eng., 1982, 52, 239–248.
Jacques and T. Pardoen: Acta Metall., 2007, 55, 2337–2350. 46. T. Gladman, B. Holmes and I. D. Mclvor: ‘Effect of second-phase
8. V. Uthaisangsuk, U. Prahl, S. Munstermann and W. Bleck: particles on the mechanical properties of steel’; 1971, London, ISI
Comput. Mater. Sci., 2008, 43, 43–50. Publication.