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Abstract
Formation of nanocrystalline structure in a eutectoid steel by severe plastic deformation has been studied by a ‘ball
drop test’. The microstructures and hardness similar to those of nanocrystalline structures produced by ball milling
have been obtained near the surface of specimens. The high strain rate of around 104 s1 is proposed to be an essential
condition to produce nanostructure by deformation. Ó 2002 Acta Materialia Inc. Published by Elsevier Science Ltd. All
rights reserved.
1359-6462/02/$ - see front matter Ó 2002 Acta Materialia Inc. Published by Elsevier Science Ltd. All rights reserved.
PII: S 1 3 5 9 - 6 4 6 2 ( 0 1 ) 0 1 2 5 8 - 1
384 M. Umemoto et al. / Scripta Materialia 46 (2002) 383–388
Fig. 2. SEM images of Fe–0.89C pearlite steel after ball drop of (a) 50 times with a weight of 3 kg, (b) 10 times with a weight of 5 kg.
9.4 GPa, which is much higher than that of the of 4 kg. The dark field image of Fig. 3 (taken using
work-hardened region (4.5 GPa). It was noted that the (1 1 0) ring of the ferrite) shows that the ferrite
the observed microstructures after the ball drop grain size is of the order of 100 nm. All the dif-
test were similar to those observed in ball milled fraction rings correspond to those of the bcc ferrite
powders with pearlite structure. In the ball milled and rings corresponding to cementite are hardly
powder, dark layer was also observed near the detected. This indicates that the cementite is
surface of the powders and the work-hardened mostly dissolved into the ferrite matrix. The dif-
region was observed in the interior of the powder. fraction pattern was obtained from the area of
It was also revealed that the dark layer consists of 2 lm Ø and shows nearly continuous rings, indi-
either equiaxed or elongated grains with an aver- cating the random orientations of ferrite grains.
age size around 20 nm and the microhardness is
around 9.4 GPa [8,11], which agrees with that 3.2. Ball drop test for specimens with spheroidite
observed in the present ball drop test. Therefore, structure
the dark layer observed in the specimen after the
ball drop test is considered to be nanocrystalline Similar microstructural changes with those in
ferrite. the specimen with the pearlite structure were ob-
The dark layer (nanocrystalline ferrite region) served in the specimens with spheroidite structure
was found not only along the surface of the spec- by the ball drop test. Fig. 4(a) shows a micro-
imen but also in the region several tens of mi- structure of a specimen ball dropped 50 times with
crometers below the specimen surface as shown in a weight of 2 kg. The uniform structured layer is
Fig. 2(b). In most cases, the dark nanocrystalline seen along the specimen surface. The microhard-
layer was seen parallel to the specimen surface. It ness of this region is 8.8 GPa which is much higher
was considered that nanocrystalline structure is than the interior work-hardened region (5.5 GPa).
produced in the region where the most severe de- The highest microhardness of the uniform struc-
formation occurred. In the case of the ball drop tured layer in the ball dropped specimen (after
test, the degree of deformation may not be always eight times drops) was 9.6 GPa, which agrees with
the largest at the surface of the specimen because that observed in the ball milled powder (9.5 GPa),
of the friction between the specimen and ball. This in which the average grain size of about 20 nm was
might be the reason why dark layers form in the observed by TEM [11]. It should be noted that
interior of the specimen. cementite particles are hardly observed in the
Fig. 3 shows a dark field image and electron uniform structured layer but remain undeformed
diffraction pattern of a sample with pearlite in the work-hardened region. The uniform struc-
structure after ball dropped 25 times with a weight tured layer was also observed in the interior of the
386 M. Umemoto et al. / Scripta Materialia 46 (2002) 383–388
Fig. 3. A dark field image and electron diffraction pattern of Fe–0.89C pearlite steel after ball drop of 25 times with a weight of 4 kg.
Fig. 4. SEM images of Fe–0.89C spheroidite steel after ball drop of (a) 50 times with a weight of 2 kg, (b) 3 times with a weight of 4 kg.
ball dropped specimen as shown in Fig. 4(b). In formation of a uniform nanocrystalline structure in
the uniform structured layer, many wavy bands the whole particles.
parallel to each other are seen together with sphe-
roidal cementite. The density of wavy bands near
the center is higher and it looks like they coalesce 4. Ball press test
with each other. The observed microstructures are
quite similar to those of corresponding ball milled It was considered that high strain rate is one of
samples [11]. At the initial stage of BM, a submi- the necessary conditions to obtain nanocrystalline
cron wavy band structure forms near the surface of structure by heavy deformation. To confirm this, a
a powder particle. With increasing milling time, ball press test was carried out. The specimens used
volume fraction of the wavy band structure in- for ball press test were compressed using the same
creases and they evolve into a uniform nanocrys- steel ball (Fe–1.0C–1.5Cr, SUJ2) with a diameter
talline ferrite. Longer milling time up to 1800 ks of 6 mm. Similar degree of deformation was ap-
leads to complete dissolution of cementite and the plied by a number of compressions on the speci-
M. Umemoto et al. / Scripta Materialia 46 (2002) 383–388 387
men surface with a load of 2000 kgf. Each com- over the e as 1000e þ 125e2 (106 J m3 ). If all the
pression was carried out for about 1 s (this cor- potential energy of the weight is used for the
responds to the strain rate of about 1 s1 ). The plastic deformation of a sample, 39:2 ¼ ð1000e þ
structure observation and microhardness mea- 125e2 Þ 106 V , where V is the plastically de-
surement revealed that there was no trace of formed volume. If the plastically deformed volume
nanocrystalline structure even after the specimen is assumed to be same with the volume of the
was compressed 50 times. crater produced by a single ball drop test
(V ¼ 108 m3 ), the average plastic strain of 2.5 is
obtained. Consequently, an average strain rate
5. Discussion e_ ¼ e=s ¼ 5 103 s1 . The strain rate in the ball
drop test is about 2000 times higher than that in
Zhang et al. [12] have carried out an experiment the ball press test.
using the falling-ball impact wear tester to simu- Dissipation of the potential energy leads to a
late the deformation conditions of BM. A cast iron temperature rise in plastically deformed region.
ball of 4 kg (100 mm in diameter) was dropped 30 For the presentpexperiment,
ffiffiffiffiffiffiffi the thermal diffusion
times from a height of 3.5 m on a tempered low distance R (¼ Dt s, where the thermal diffusion
alloy 0.4 mass% C steel sample with the angle of coefficient Dt ¼ 4 106 m2 s1 for steel and the
45°. They reported that a white layer with fine collision time s ¼ 5 104 s) is estimated to be 50
subgrains was observed on the surface and interior lm. This is much smaller than the plastically de-
of sample. The structures they observed are similar formed thickness (1 mm). Thus thermal diffusion
to those obtained in the present study. However, can be neglected for the maximum temperature
they did not examine the deformation conditions reached. If all the potential energy of the weight is
in their experiment, such as the degree of defor- converted into heat, average temperature rise is:
mation or strain rate. The present deformation mgH
condition is analyzed as follows. DT ¼ ;
vqm
When a ball of 6 mm in diameter with a weight
of 4 kg was dropped from the height of 1 m onto a where v is the heat capacity, q is the density. The
flat bulk specimen surface, the potential energy E average temperature rise of 1140 K (v ¼ 444
of the weight (¼ mgH , where m is the mass of J kg1 K1 and q ¼ 7:85 g cm3 ) can be obtained.
weight and H is the height) is 39.2 J. The velocity
pffiffiffiffiffiffiffiffiffi This is considered to be the maximum temperature
of the ball when it hits the specimen v0 (¼ 2gH ) rise that can be reached. A part of the potential
is 4.4 m s1 . The collision time s (¼ S=v, where S energy of the weight will be used for the bouncing
is the collision depth (measured as 1.1 mm) and back of the weight, kinetic energy of the specimen
v is the average velocity (0.5v0 ) of the ball dur- and specimen holder, sound, elastic energy of the
ing collision) is 5 104 s. The collision load P weight, and specimen, etc. Thus the actual tem-
(¼ ma ¼ mv0 =s) is obtained as 3:6 103 kgf. The perature rise may be about half of the above esti-
average collision stress r (¼ P =A, where the con- mated maximum temperature rise. However, the
tact area A was measured as 21 mm2 ) is 1.7 GPa. It possibility of local temperature raise above the
should be noted that the collision time of 5 104 austenite transformation temperature (1000 K)
s is much shorter than that of the ball press test still remains. This means that there is a possibility
(1 s) and the collision load of 3:6 103 kgf is 1.8 that the layered nanocrystalline ferrite is the mar-
times larger than the load (2000 kgf) applied in the tensite produced during cooling from the austenite
ball press test. The strain rate by ball drop test can state. At present, there is no clear evidence to
be estimated as follows. For the 0.89C pearlite support the occurrence of the transformation to
steel, the measured relationship between the stress austenite by deformation induced heating.
(r) and plastic strain (e) is rðMPaÞ ¼ 1000 þ 250e. Lee and Lam [13] have studied the deformation
Therefore, the energy per volume necessary to give behavior of high strength steels under various high
true strain e is obtained by integrating r and de strain rates (103 to 5 103 s1 ). They have found
388 M. Umemoto et al. / Scripta Materialia 46 (2002) 383–388
that the strain rate has an effect both on disloca- can induce nanocrystallization if the strain rate is
tion arrangement and cell size. They also found high around 104 s1 .
that the dislocation density at a given degree of
deformation increases with increasing strain rate.
With increasing the strain rate, dislocation cell size
Acknowledgements
decreases and fraction of cells with large misori-
entation increases [13]. From this experiment, it
One of the authors (B. Huang) would like to
can be inferred that when the strain rate is higher
thank Heiwa Nakajima foundation for supplying
than a certain value, the dislocation density can
the scholarship to carry out this work in Japan.
reach a critical value to induce the transition from
This study is financially supported in part by the
dislocation cellular structure to granular struc-
Grant-in-Aid by the Japan Society for the Pro-
ture (dynamic continuous recrystallization [14]). It
motion of Science.
seems that high strain rate raises local temperature
and thermally assisted process may occur in some
extent. This might be the reason for that a high
strain rate is a necessary condition to produce References
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