Materials Science and Engineering A 502 (2009) 126–130

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Materials Science and Engineering A

journal homepage: www.elsevier.com/locate/msea

Microstructures and fracture features of cold-rolled low carbon steel sheet

after annealing and mechanical stress concurrently loaded
Kun Yang a,b , Huiyang Gou a,b , Bo Zhang a,b , Rui Huang a,b , Hui Li a,b , Manman Lu a,b ,
Xiangyi Zhang a,b , Jingwu Zhang a,b,∗
a
College of Materials Science and Engineering, Yanshan University, Qinhuangdao 066004, PR China
b
State Key Laboratory of Metastable Materials Science and Technology, Yanshan University, Qinhuangdao 066004, PR China

a r t i c l e i n f o a b s t r a c t

Article history: The microstructure and fracture feature of a cold-rolled low carbon steel sheet after annealing under
Received 26 May 2008 a stress were investigated by using the optical microscope (OM), scanning-electron microscopy (SEM)
Received in revised form 7 October 2008 and transmission electron microscopy (TEM). It was found that a commixed grain structure was formed
Accepted 7 October 2008
when concurrently stressed and annealed at 650 ◦ C, and that both the tensile strength and hardness of
the steel are still higher while the elongation is increased markedly. The dimple like fracture feature with
Keywords:
delamination cracks was observed after tensile deformation. These superior mechanical properties were
Cold-rolled low carbon steel
derived from the commixed grain structure composing of cold-rolled lamellar grains, fine equiaxed grains,
Anneal
Mechanical stress
and sub-grains as well as ultrafine carbide precipitates.
Commixed grain structure © 2008 Elsevier B.V. All rights reserved.
Delamination crack

1. Introduction rate of steel materials owing to the accumulation of geometrically

necessary dislocations around the rigid particles [12,13].
In order to obtain superior mechanical properties of metal mate- Recently, the studies by Winning [14,15] have indicated that the
rials, development of techniques, such as controlled rolling (CR) applied mechanical stresses can slow down the motion of grain
and controlled cooling (CC) [1], deformation-induced phase trans- boundaries in the process of annealing to obtain the ultrafine grains
formation (DIT) [2,3], equal channel angular pressing (ECAP) [4], of a cold-rolled Al–Mg alloy, when the applied load is below the
deformation enhanced transformation (DET) [5], and severe plas- critical stress for activation of dynamic recrystallization. However,
tic deformation (SPD) of a martensite starting structure [6,7] as in the study by Winning the mechanical properties of the samples
well as severe plastic deformation plus static recrystallization [8], after annealing under a mechanical stress have not been explored.
has been made to produce the ultrafine grained (UFG) materials In the present paper, the annealing under a mechanical stress was
based on the Hall-Petch relationship between strength and grain applied to the cold-rolled low carbon steel sheet. The mechani-
size. The grain size of 1–2 ␮m [2,3], or even in the nanometer scale cal properties, microstructure and fracture features of the material
[8], in metallic materials can be achieved by above these novel were investigated. The effect of microstructures on the fracture
techniques. However, cases contradictory to the Hall-Petch rela- mechanisms was also analyzed and discussed.
tion has been discovered in some single-phased nanocrystalline
materials [9], i.e. the strength of the materials increased with grain
size increasing from 2 to 30 nm. Subsequently, in some studies the 2. Materials and experimental
commixed structures which comprise of multiphase and fine grains
with different sizes and shapes also exhibit the superior mechanical In this study, the chemical composition of the experimental
properties [10,11]. For example, fine dispersed second phase parti- steel sheet used is Fe–0.17C–0.32Si–0.40Mn–0.015P–0.045S (wt.%).
cles can effectively enhance strength and improve work hardening The experimental steel sheet with 7.5 mm thickness was heated
up to 900 ◦ C prior to cold rolling, and then quenched in the 10%
sodium chloride ice water in order to obtain the microstructure
∗ Corresponding author at: State Key Laboratory of Metastable Materials Science
of lath martensite. The martensite steel sheet was rolled with
and Technology, College of Materials Science and Engineering, Yanshan University,
80% reduction to 1.5 mm final thickness at room temperature and
Qinhuangdao 066004, PR China. Tel.: +86 139 33617469; fax: +86 335 8074545. subsequently cut along rolling direction according to the tensile
E-mail address: [email protected] (J. Zhang). direction. The sample geometry is shown in Fig. 1. Then, the sam-

0921-5093/$ – see front matter © 2008 Elsevier B.V. All rights reserved.
doi:10.1016/j.msea.2008.10.006
 K. Yang et al. / Materials Science and Engineering A 502 (2009) 126–130 127

Fig. 1. Schematic of a tensile sample of the annealed steel sheet.

ples in a bath furnace were annealed in temperature ranging from

350 to 750 ◦ C at an interval of 50 ◦ C, respectively, and soaked for
90 min, finally cooled down to the room temperature in air. The
recrystallization temperature was determined by use of the optical
microscope (OM) and transmission electron microscopy (TEM). In
addition, another set of samples were annealed after meet mechan-
ical pressure of 10 MPa on the rolling surface. Comparing with above
work, the same annealing schedule was used.
The mechanical properties of all samples along rolling direction
were measured in tensile test, and the hardness was also tested in a
HR-150A Rockwell hardness tester. In order to determine recrystal-
lization temperature, the observation of metallographic structure
was carried out by using a NEOPHOT21 OM. After cleaning in ace-
tone by ultrasonic, the tensile fracture regions were observed by
using a KYKY-2800 scanning electron microscopy. The TEM studies
were conducted with a JEM-2010 transmission electron micro-
scope. To obtain the foil samples used for TEM work, the samples
from above two processes were first sliced into ∼0.3 mm in thick-
ness, and then mechanically thinned to ∼30 ␮m in thickness by use
of sand paper. Finally TEM samples with thin area utilized were
obtained by use of a twin jet electro-polishing technique in an
alcohol solution with 10% perchloric acid.

3. Results and discussion

3.1. The initial cold-rolled microstructure

Fig. 3. The effect of annealing temperature on tensile strength (a), hardness (b) and
elongation (c).
As result from TEM observation, the three-dimensional
microstructure of the cold-rolled specimen with 80% cold reduction
in thickness is shown in Fig. 2. It can be seen, from the microstruc- grains with laminated arrangement [16]. A larger number of inter-
ture in longitudinal cross-section of steel sheet, that the martensite faces and high-density dislocations appeared after cold-rolling, and
lathes were obtained after quenching and paralleled approximately provided a great lot of perfect nuclear sites for annealing recrystal-
to the rolling plane. In general, size of the martensite laths in thick- lization of the steel sheet [17].
ness of the steel sheet is less than 100 nm.
The grain size in rolling plane is relatively larger than that 3.2. Mechanical properties
in cross-sections and the regions with high-density dislocation
appear in the grain interiors. The water wave pattern with different The relationships between the mechanical properties and
spacings can be seen due to the thin grains overlapping. This indi- annealing temperature of the specimens in the two different pro-
cates that low-carbon martensite steel formed into the pancaked cessing routes (with and without stress) are shown in Fig. 3. On
the condition of annealing at different temperatures, the mechan-
ical stress loaded of the specimens is 1014.33 MPa, which is close
to the tensile strength after the cold rolling specimen. With the
annealing temperature changed from 350 to 650 ◦ C, the tensile
strength of specimens with and without stress normally decreased
(Fig. 3(a)). However, the drop of tensile strength of specimens with
the mechanical stress is far smaller than that without the stress.
Also, it can be seen that the hardness change of specimens with
and without stress shows a very similar phenomenon with tensile
Fig. 2. Schematic of a TEM micrograph of the cold-rolled steel sheet in three dimen-
strength (Fig. 3(b)). Without loading stress, annealing can result
sions. in a large elongation with temperature increasing (Fig. 3(c)), but
128 K. Yang et al. / Materials Science and Engineering A 502 (2009) 126–130

Fig. 4. OM microstructures of steel sheet annealed at 650 ◦ C with stress (a) and without stress (b), respectively.

the tensile strength and hardness dropped quickly. Under stress ultrafine carbides. Using secant measuring method of grain size,
loaded condition, the tensile strength of the specimen annealed at the mean diameter of the equiaxed grains is about 0.31 ␮m and
650 ◦ C can still reach at 882.90 MPa and the hardness is HRC28.45, the average sub-grain size is about 0.15 ␮m in the specimen with
meanwhile the elongation is close to 7.69% and the value is greater stress-annealed at 650 ◦ C. In addition, the carbides distributed at
comparatively. So it should be suggested that to obtain the good the interior of grains and in grain boundaries and the sizes of the
balance between strength and toughness, namely, annealing plus carbides were in the range from 15 to 50 nm. It was also seen that
stress can make the material simultaneously having high strength the partial sub-grains retain the morphology of the lamellar grain
and perfect toughness. paralleling to rolling plane, which formed during the process of
cold-rolling, and the weak interfaces still exist between parallel
3.3. Analysis of microstructure from anneal plus stress sub-grains.
The commixed grain structure, including the ultrafine carbide
Fig. 4(a) and (b) shows the OM microstructure of specimens precipitates and the ferrite with the different shape and size, was
annealed at 650 ◦ C with and without stress, respectively. In the obtained in the specimen annealed at 650 ◦ C with stress loaded.
specimen annealed without stress, ferrite and a small amount of The existence of the equiaxed grains, the sub-grains and the cold-
pearlite can be seen (see Fig. 4(a)). It was found from Fig. 4(b) rolling lamellar grains results from incomplete recrystallization,
fine carbides and ferrite appear in the stress-annealed speci- but at the same temperature, the full recrystallization happened
men and the grain size is too fine to be difficultly distinguished. in the annealed specimen without stress. It is indicated that the
Fig. 5(a) and (b) shows the TEM images of specimens annealed at recrystalline temperature rise due to the mechanical stress during
650 ◦ C with and without stress, respectively. Note that the fully annealing [17,18]. Because the shear stress, parallel to grain bound-
recrystallization took place in the specimen unstress-annealed ary, can pick up motion speed of grain boundary, which leads to
at 650 ◦ C (see Fig. 5(a)), which microstructure correspond with recrystallization of grain [14], whereas for the lamellar grains after
the OM microstructure (see Fig. 4(a)). The average value of grain cold-rolling, a majority of the grain boundaries does not parallel
size is about 2.10 ␮m, and a small amount of dislocations emerge with the shear stress. In this case, the motion of the grain bound-
inside the grains. The microstructure of the specimen from anneal aries slow down and the recrystallization is inhibited. The grain
plus stress is more complex (see Fig. 5(b)), containing cold-rolled size of the stress-annealed specimen is obviously smaller com-
lamellar grains, fine equiaxed grains, and sub-grains as well as pared to the unstress-annealed specimen. Moreover, the dispersed

Fig. 5. TEM images of the cold-rolled steel annealed at 650 ◦ C with stress (a) and without stress (b), respectively.
 K. Yang et al. / Materials Science and Engineering A 502 (2009) 126–130 129

Fig. 6. SEM images of the tensile sample (a), the cold-rolled sample (b), the sample annealed at 650 ◦ C without stress (c), and the sample annealed at 650 ◦ C with stress (d).

carbides distribute in grains and the grain growth is markedly hin- The typical fracture morphology of the initial cold-rolled sam-
dered. Therefore, the mechanical stress should promote nucleation ple is represented in Fig. 6(a). A long delamination crack appears
of the ferrite and carbides, and simultaneously inhibit the growth in the middle of the sample, which is deeper and penetrates the
of grains based on the alloy thermodynamic theory [19]. It can be whole fracture region along transverse direction. At both sides of
explained that the samples with stress can hold high strength and delamination crack, the retuse dimples are clearly seen at high mag-
hardness during annealing, even at a relative higher temperature, nification. After cold rolling, the fracture region delaminated due
owing to the effect of grain/sub-grain boundaries of fine grain and to laminated arrangement of pancake-shaped grains, namely, the
lamellar structure on dislocation motion. Especially, the dispersed traversed crack corresponds to lamellar microstructure.
nano-carbides play a more important role in keeping high-hardness Fig. 6(b) is SEM image of the specimen after unstress-annealed
of the steel sheet. at 650 ◦ C, the fracture feature shows a typical ductile fracture with
dimples. Without stress, full recrystallization can be completed in
the specimen. Microstructure of the ferrite including a small quan-
3.4. Fracture features tity of pearlite was obtained, which leads to the deeper dimple in
the fracture region.
As shown in Fig. 6 from the SEM images in the two different Both Fig. 6(c) and (d) shows the fracture region of the specimen
processing routes, the commixed microstructures can give rise to a stress-annealed at 650 ◦ C, the shorter delamination cracks substi-
typical fracture feature during tensile deformation. tuted for the penetrated longer and approximately paralleled cracks

Fig. 7. Sketch of fracture process of the commixed grains.

130 K. Yang et al. / Materials Science and Engineering A 502 (2009) 126–130

superior mechanical properties. The tensile strength can reach to

882.90 MPa and the hardness is HRC28.45 with elongation of 7.69%.
Comparing with annealed without stress, at the same tempera-
ture, the sample retain high strength and hardness and elongation
increased markedly. This results from the commixed microstruc-
ture after annealing with stress loading, which is composed of the
cold-rolled lamellar grains, the fine equiaxed grains, and the sub-
grains as well as the ultrafine carbides.
Fig. 8. Dimples and delamination cracks on the fracture region of the commixed The fracture mechanisms of the commixed microstructure
grain structure. which was obtained after annealing at 650 ◦ C and with stress
concurrently loading, firstly form micro-cracks along the weak
at relative low magnification (as indicated by arrow in Fig. 6(c)). The interface and some orientations, and finally the micro-cracks
typical dimple is seen between delamination cracks, and the frac- change into local and short delamination cracks in the fracture
ture feature has obviously changed (Fig. 6(d)). Under the stress, the region in the process of tensile deformation, and the formation of
commixed microstructure appeared in the specimen, as a result of the dimple fracture regions is due to micro-crack expansion into
incomplete recrystallization (Fig. 4). In the process of tensile defor- fine grains and sub-grains.
mation, the commixed microstructure gives rise to another typical
fracture feature with short delamination cracks and dimples. Acknowledgment
Fig. 7 demonstrates the formation and development of the typ-
ical fracture feature with short cracks corresponding to the above The authors acknowledge the financial support from the
microstructures. For most of sub-grains retaining parallel lami- National Natural Science Foundation of China (No. 50371073).
nated arrangement, micro-cracks firstly formed along transverse
direction (T.D.) in the laminated weak interface during tensile References
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4. Conclusions

The cold-rolled low-carbon martensite steel sheet, which was

annealed at 650 ◦ C and concurrently stress was applied, exhibits the