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Hadfield Steel shows high strain hardening which can be linked to its ability to form twins
during mechanical loading. Twinning in Hadfield Steel is well documented, however, detwinning
in Hadfield Steel is only barely investigated. Detwinning provides an additional contribution to
plastic deformation, therefore it might be an essential effect during cyclic loading. In order to
gain more information regarding the deformation behavior in Hadfield Steel, the present work
concentrates on the twinning and detwinning behavior during interrupted tensile tests. Tensile
tests were conducted in situ within a scanning electron microscope and interrupted at predefined
elongations. To determine the formation of twins during every interruption, the electropolished
tensile test sample was analyzed by electron backscatter diffraction. The first twins appeared
after 5 to 10 pct strain. Conversely, tensile test interruptions at 30 and 40 pct elongation showed
partial detwinning of the twinned regions. Furthermore, the Kernel Average Misorientation of
the twinned and detwinned regions was analyzed. High values of misorientation were found not
only in the twinned but also in the detwinned regions, thus the high level of misorientation can
be linked to the twinning/detwinning process.
https://doi.org/10.1007/s11661-023-06984-3
The Minerals, Metals & Materials Society and ASM International 2023
size for the detail images was 70 nm and for the (see Experimental), however, this assumption leads to an
overview images it was between 0.8 and 2.2 lm uncertainty concerning the quantitative stress values
(before deformation). For EBSD data analysis the which are at the ultimate tensile strength in the range
Software AZtecCrystal 2.1 from Oxford Instruments of ± 200 MPa and at the yield strength in the range
was used. No clean up was carried out. The misori- of ± 200 MPa.
entation within a grain was determined by evaluating The result of the macroscopic conventional tensile test
the averaged orientation difference between a kernel with a round specimen but without any interruption is
point and the neighboring points. This Kernel Aver- shown in Figures 3(a) and (b). The measured yield
age Misorientation (KAM) was evaluated with a strength was 325 MPa. The elongation at fracture was
kernel size of 3 9 3. 45 pct and the strain hardening reached 620 MPa. The
difference in the results of the macroscopic conventional
tensile to the interrupted tensile tests are originated from
III. RESULTS the very thin flat electropolished sample which varies in
thickness used for the interrupted tests. Furthermore,
A. Analysis of Tensile Tests the testing machine and the measurement of the
Interrupted in situ tensile testing with a flat specimen elongation were different and also the interruptions
led to a strain hardening from 360 to 830 MPa and 82 might lead to relaxation and thus to different deforma-
pct elongation before fracture. The resulting plot is tion behavior. Following Hwang et al.[40] the macro-
shown in (Figure 2). However, during the in situ tensile scopic twinning stress was determined by the
test, the recorded elongations refer to the tensile stage conventional tensile tests at the point at which the
movement. Subsequently, the strain values were calcu- strain hardening rate vs. stress curve flattens and shows
lated based on these elongations. The specimen thick- the lowest strain hardening rate before it increases
ness after electropolishing was estimated to be 1 mm again, see insert in Figure 3(b). The twinning stress for
the Hadfield steel was therefore located at 380 MPa at a
strain of 3 pct.
Fig. 4—Overview on selected positions for microstructure analysis on the electropolished in situ tensile test specimen with SEM and EBSD
before deformation and after 5, 10, 20, 30 and 40 pct strain. Details on the sub-images are given in the text.
images of position 1. However, due to straining of the C. Twinning Behavior Between 0 and 10 pct Strain
sample the surface begins to deform, so that a macro- Before deformation, the FS images (Figures 4(a) and
scopic relief is formed. The grain of the upper left side (i)) exhibit no lines due to deformation and the EBSD
moved downwards along the z-direction so that the IPF-X-BC images (Figures 4(e) and (o)) exhibits also no
initially analyzed triple point of position 1 is no longer twins or change of orientation within the grain for both
visible in the images with 20 pct to 40 pct elongation. positions. After the loading/ unloading cycle to 5 pct
Thus, for the analysis after 20 to 40 pct strain another strain, the first topographical effects in form of defor-
position was selected and denoted in the following as mation lines are visible in the detail FS image for
position 2 (columns four to six of Figure 4). Position 2 is position 1 (Figure 4(j)). In the EBSD IPF-X-BC image
marked by green arrows and rectangles. Before defor- (Figure 4(p)) a slight tilt over the whole grain on the
mation (Figures 4(a) and (e)) and after 10 pct upper side left but no twins were observed only by
(Figure 4(b)) strain both positions are visible in the analyzing the IPF mapping. After the loading cycle to 10
overview images.
IV. DISCUSSION
A. Twinning
Fig. 5—Pole figure analysis of the selected region after 5 pct strain. In the present work, an interrupted in situ tensile test
(a) IPF-X-BC image after 5 pct strain with a marked position was carried out in SEM coupled with EBSD analysis
(yellow rectangle) at a deformation line. (b) The marked region is and for comparison a conventional tensile test without
magnified. The IPF-X image shows blue pixels which have a
different orientation with respect to the matrix. In (c) it is illustrated interruption was conducted. The findings of the con-
by the pole figure analysis of the marked region that the blue pixels ventional tensile test showed that according to the
within the deformation line exhibit a R3 coincidence and correspond analysis of the macroscopic twinning stress,[40] the first
to twins that are rotated by 60 deg with respect to the {111}-plane twins form at 380 MPa which is reached after about 3
(Color figure online).
Fig. 7—Pole figures of the overview images after 20 to 40 pct strain. In (a) the position within the twinned grain after 20 pct strain is marked
for pole figure analysis of the twin in (b). In (c) the position within the twinned grain after 30 pct strain is marked for pole figure analysis of the
twin in (d). In (e) the position within the twinned grain after 40 pct strain is marked for pole figure analysis of the twin in (f). The positions were
selected within the grain to avoid effects from the grain boundaries. The {111}-pole figure analysis showed R3 twins.
pct strain. The results of the interrupted tensile test in first deformation twin that forms exhibits a thickness of
SEM suggest that twins have formed after 5 to 10 pct about 10 to 40 nm. Upon further straining further twins
strain. These twins were determined in form of single form near the first one with a similar thickness extending
pixels at deformation lines with a R3 coincidence. the twin to a thicker twin bundle. In this work, the
Especially, after 5 pct strain only very few pixels with thickness of analyzable twin bundles is estimated to be
twinning orientation at deformation lines are present larger than 70 to 100 nm, as the step size for EBSD
(Figure 5). Thus, it was checked if these pixels belong to measurements was 70 nm and the accompanying image
pseudo-symmetries (according to[44]), resulting that resolution would be at or above 70 nm. Thus, due to the
pseudo-symmetries can be excluded for the pixels after limited EBSD image resolution and the characterization
the loading and unloading cycles to 5 and 10 pct strain of only a few grains an exact determination of the start
(Figures 5 and 6). Previous works[14,28,29] determined of twinning is not possible as smaller twins or twins
that deformation twins form as a bundle of twins. The formed at lower strain amplitudes in differently
orientated grains might be undetected by the used The EBSD analysis done during the interruption of
experimental setup in this work. However, a contribu- the tensile test after the loading/unloading cycle to 20
tion to the knowledge on the early stages of twin pct strain indicates that a massive twin formation has
formation in TWIP steel can be given, confirming the already occurred. The thickness of twin bundles
results of works.[41,43,45] Twin formation is described via increased to 7 lm (Figures 4(c), (f), (l) and (r)). Within
the formation of stacking faults by the dissociation of a the formed twin bundles the KAM shows higher values
perfect < 110 > dislocation on an {111} plane into compared to the untwinned matrix (see Figure 8).
two < 112 > Shockey partial dislocations. Adjacent Higher KAM values can be linked to a higher disloca-
stacking faults on {111} planes form twin embryos with tion density. Wu and Bei[42] also analyzed that in the
a critical width.[45] Others describe that twins are formed twinned regions, especially at the interfaces between
after the Shockley partial interacts with a Lomer-Cotrell twin and untwinned matrix a lot of dislocations accu-
lock.[41,43] mulate as formation of twins is accompanied by
However, Barbier et al.[29] found twin bundles after 2 dislocation generation. Furthermore, Idrissi et al.[41]
pct strain in a Fe-22Mn-0.6C steel with TEM experi- revealed that twins are formed according to the pole
ments, whereas EBSD measurements reveal the first mechanism with deviation initially proposed by Cohen
twins bundles between 10 to 20 pct strain. This is in and Weertman[43]: A perfect dislocation on the primary
relatively good coincidence with this work, as the plane dissociates into a sessile Frank partial and a
analysis of the macroscopic twinning stress according glissile Shockley partial dislocation after passing a
to Hwang[40] showed that twins formed at 380 MPa Lomer-Cotrell barrier. The Shockley partial glides away
which is reached after about 3 pct strain and the first from the sessile dislocation on the conjugate twinning
traces of twins were found with EBSD after 5 to 10 pct plane and by this the starting point for the formation of
strain at deformation lines. Thus, it can be deduced that a twin is set. Irdissi et al.[41] determined a lot of sessile
twins may even be present at low strain values (around 3 dislocations in twins, which leads to a strengthening
pct), but the image resolution of EBSD is not sufficient effect and also to an increase of KAM within twin
for displaying the small twin bundles. By increasing the bundles as found in this work.
strain to 5 pct the twin bundles become thicker and can
be analyzed by EBSD. It is to mention that the
B. Detwinning
deformation lines, which may indicate twins have
formed already after about 0.75 pct strain, as depicted After the loading/unloading cycle to 30 pct strain the
in Figure 9. thickness of twin bundles decreases to 4 lm and the
amount of twin bundles is reduced (Figures 4(g), (m) by Szczerba et al.[36,37] that only one detwinning system
and (s)). A further cycle to 40 pct strain results in further out of three possible is reversible (transforms to initial
reduction of deformation twins and the thickness of matrix orientation with initial dislocation structure), the
twin bundles was reduced to 2 lm (Figures 4(d), (h), (n) other two lead to pseudo reverse detwinning and the
and (t)). The reduction of deformation twins upon introduction of shear strains and thus, to a raise of
further loading/unloading cycles is linked to detwinning. dislocations, which increase the KAM (transformation
On the nm scale detwinning can be explained by to initial orientation with increased dislocation density).
dislocation reaction with twin interfaces—e.g. a partial Therefore, it is possible that at some positions the higher
dislocation which reacts with the twin boundary and by KAM after detwinning persists where pseudo reverse
that reaction with dislocations the twin thickness is detwinning takes place, where at other positions where
reduced atom layer by atom layer.[34,46] Detwinning was reversible detwinning occurs the KAM decreases as
also reported in former studies after load rever- twins have vanished. However, also low KAM values in
sal.[14,36,37] However, in the present work it is the first twinned regions were found after the loading/unloading
time that detwinning is observed for Hadfield Steel after cycle to 20 pct strain (black arrows in Figures 8(d), (e),
unloading by EBSD. Detwinning is explained by (j), (k), (n) and (r)). In these twinned regions with low
McCormack et al.[14] by backstresses introduced during KAM larger twins with up to 5 lm (measured from
twin formation, which enable detwinning when reaching figure) might be located. Maybe one should see this area
the critical detwinning stress during load reversal. In this as single twin and not as bundle. As it is a single twin no
work no load reversal was applied but straining to 30 pct interfaces are present as in case of the bundle and
elongation leads to plastic deformation. Some grain therefore also a lower amount of dislocations would be
orientation might be strained even more than others present resulting in low KAM values. It is interesting to
which is dependent on the orientation dependent elastic see that the twinned region with low KAM from the
and plastic properties.[47] It is assumed that during detail image of position 2 (Figures 8(d) through (f)) does
unloading, some of the intensively plastically deformed not untwin even after the loading/unloading cycle to 30
regions in tension might be under compressive stresses, pct and 40 pct strain. According to McCormack and Ni
which are high enough to promote detwinning. Detwin- et al.[14,34] detwinning mechanism is based on a disloca-
ning upon unloading was also shown by Hu et al.[48] by tion interaction which removes the twinned area sequen-
phase field modeling. Furthermore, as it is indicated that tially atom layer by atom layer. Consequently, a thick
detwinning occurs during unloading owing to internal twin needs more strain cycles than the smaller ones to
local stress fields, it is suggested that detwining is a result untwin.
of the frequency and setup of loading/unloading cycles.
Additionally, as twins have vanished after 40 pct strain
detwinning gets more favorable than twinning during V. CONCLUSION
cyclic loading. Thus, also plastic deformation by dislo-
cations is favored during cyclic loading compared to In the present work, the behavior of the Hadfield steel
twinning during static loading. during interrupted tensile testing coupled with EBSD
It was also found that the KAM generally increases and SEM analysis was characterized. The results show:
with increasing strain, even in the regions, where no
twinning took place (see Figure 8). This is due to the The analysis of the macroscopic twinning stress
raise of dislocation density due to straining. At the showed, that twinning starts at about 3 pct strain but
twinned regions a high KAM is observable. Detwinning single twins are too thin for EBSD image resolution.
leads to reduction of the KAM but some detwinned After 5 to 10 pct strain, the first traces of small twin
regions with higher KAM values also exist (white bundles in the size of the EBSD image resolution
arrows in Figures 8(d), (e), (j) and (k)). It is described (above 70 to 100 nm) were found by the detection of
single pixels in twinning orientation.