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a r t i c l e i n f o a b s t r a c t
Article history: Al2O3/SiC nanocomposites were synthesized by high-pressure sintering using a-Al2O3 and b-SiC nano-
Received 25 February 2013 powders as the raw materials. Microstructure and mechanical properties of the sintered samples were
Received in revised form 24 April 2013 investigated using X-ray diffraction (XRD), Scanning Electron Microscope (SEM), Atomic Force Micro-
Accepted 2 May 2013
scope (AFM) et al. The results indicate that high-pressure sintering is an effective sintering technique,
Available online 9 May 2013
which can densify Al2O3/SiC nanocomposites at high pressure (4.5 GPa) and relatively low temperature
(1000–1230 °C). Rapid grain growth of Al2O3 is mainly restrained by the separation effect of nanosized
Keywords:
SiC grains. Grain boundary, grain boundary-intragranular and nano-nano structured Al2O3/SiC nanocom-
High-pressure sintering
Nanocomposite
posites can be achieved by controlling the sintering temperature and b-SiC content. The highly densified
Microstructure Al2O3/SiC nanocomposite (AS5-1170) exhibits excellent mechanical properties as 429.9 GPa in elastic
Mechanical property modulus and 30.7 GPa in nano-hardness.
Ó 2013 Elsevier B.V. All rights reserved.
0925-8388/$ - see front matter Ó 2013 Elsevier B.V. All rights reserved.
http://dx.doi.org/10.1016/j.jallcom.2013.05.009
68 Y. Teng et al. / Journal of Alloys and Compounds 578 (2013) 67–71
Table 1 are in relative density of 97.6%, 96.8% and 97.1%, while other sam-
Experimental data of as-prepared samples. ples show relative density higher than 98%. The AS20-1230 speci-
No Composition Sintering Relative density men exhibits the highest relative density of 99.6%, which is very
of samples temperature (°C) of samples (%) close to the theoretical density of Al2O3-20 vol.%SiC composite.
A-1000 Al2O3 1000 97.6 This result demonstrates that high-pressure sintering is a low tem-
A-1230 Al2O3 1230 96.8 perature and rapid densification technique as reported previously
AS0.5-1100 Al2O3-0.5 vol.%SiC 1100 97.1 [3–7]. The ceramic particles or grains are imposed with very high
AS0.5-1230 Al2O3-0.5 vol.%SiC 1230 98.5
AS5-1000 Al2O3-5 vol.%SiC 1000 98.0
shear and compression stress under high-pressure sintering, which
AS5-1100 Al2O3-5 vol.%SiC 1100 98.2 results in grain boundary slipping, tight cohesion and broken of
AS5-1170 Al2O3-5 vol.%SiC 1170 98.3 particles or even grains. Thus, rapid densification of covalent
AS5-1230 Al2O3-5 vol.%SiC 1230 98.0 bonded ceramics can be readily achieved from effective mass
AS10-1230 Al2O3-10 vol.%SiC 1230 98.6
transfer of plastic flow [14].
AS20-1230 Al2O3-20 vol.%SiC 1230 99.6
⁄
Relative density of sample(RD) = density of sample/ theoretic density of sample
3.2. XRD analysis of Al2O3-20 vol.%SiC before and after sintering
(TD) ⁄ 100% TD = (TD of a-Al2O3 + x ⁄ TD of b-SiC)/(1 + x) = (3.987 + 3.239x)/(1 + x)
x: volume fraction of b-SiC in sample.
The nanocomposite powder of Al2O3-20 vol.%SiC and its high-
pressure sintered specimen (AS20-1230) were characterized by X-
ray diffraction to analyse their phase composition (as shown in
Fig. 1). The results indicate that both samples are composed of a-
Al2O3 and b-SiC phases. The X-ray intensity of a-Al2O3 in nanocom-
posite powder is much higher than the as-densified sample.
The grain sizes of a-Al2O3 and b-SiC have been calculated from
X-ray peak broadening using Scherrer’s formula after eliminating
the instrumental contribution:
D ¼ KkB cos h
Fig. 2. SEM images of: (a) A-1000 sample and (b) A-1230 sample.
Y. Teng et al. / Journal of Alloys and Compounds 578 (2013) 67–71 69
Fig. 3. SEM fracture surface images of: (a) AS0.5-1100 sample (inserted picture with magnification 5000, scale bar: 10 lm) and (b) AS0.5-1230 sample.
Fig. 4. SEM fracture surface images of: (a) AS5-1000, (b) AS5-1100, (c) AS5-1170 and (d) AS5-1230 (scale bar: 1 lm).
Fig. 5. SEM fracture surface images of: (a) AS10-1230 and (b) AS20-1230 (scale bar: 1 lm).
grains are coarsened dramatically to about 5 lm. This phenome- 1100 sample (Fig. 3a) contains many small grains with grain size
non is totally different from tranditional theory that slow grain less than 1 lm. The doped b-SiC nanoparticles impede the grain
growth takes place at relatively low temperature (<1300 °C). The boundary movement of a-Al2O3 under high-pressure sintering,
mechanism of rapid grain growth for a-Al2O3 under high-pressure which leads grain coarsening significantly be depressed and small
sintering will be investigated in our future research. grains can be maintained. The sub-microsized grains are located at
Compared with pure a-Al2O3, samples with b-SiC nanoparticle grain boundaries or be enclosed by large grains, resulting in grain-
addition exhibit much different microstructure with inhomoge- boundary typed nanocomposite structure. The amount of sub-
neous and refined grains after high-pressure sintering. The AS0.5- microsized grains decreases obviously as the sintering temperature
70 Y. Teng et al. / Journal of Alloys and Compounds 578 (2013) 67–71
Fig. 6. 2-D top-view and 3-D AFM images in 500 nm 500 nm region of AS5-1170 sample.
increases to 1230 °C (Fig. 3b). The grain boundary movement is Al2O3 based nanostructured ceramics will be distinctly impacted
accelerated as the sintering temperature be elevated, which makes as well. It can be concluded that grain-boundary typed, grain
Al2O3 grain boundary capable to move across the doped SiC parti- boundary-intragranular typed and nano–nano typed Al2O3/SiC
cles and grain growth of Al2O3 is promoted. The grain growth takes nanocomposite ceramics can be obtained from high-pressure sin-
place rapidly along with the decrement of small grains. Nanosized tering under the controlling of SiC content and sintering
b-SiC grains are partly enclosed by large Al2O3 grains and grain- temperature.
boundary typed nanocomposite structure transforms to grain
boundary-intragranular typed nanocomposite morphology. 3.4. AFM analysis of AS5-1170 sample
The 5 vol% b-SiC doped sample were sintered at 1000, 1100,
1170 and 1230 °C with fracture surface images presented in The microstructure of AS5-1170 sample was characterized by
Fig. 4. All samples exhibit similar morphology with high relative AFM with the images illustrated in Fig. 6. It can be observed in
density, no obvious pores and nanosized grains. Integrated grains the microzone (200 nm 200 nm) that the sample surface is
and clear grain boundaries can hardly be observed in these sam- highly densified with low roughness. The grains are in irregular
ples, which is much different from normal-pressure sintered shape with grain size smaller than 100 nm. The nanosized grains
microsized ceramics. Grain boundary movement and grain growth are densely cohered with indistinct morphology and boundary,
are greatly restrained as more b-SiC nanoparticles are located which is in agreement with XRD and SEM results.
among the Al2O3 grain matrix with 5 vol.% b-SiC addition. Thus,
the composite transforms to nano–nano typed microstructure as
3.5. Mechanical properties of AS5-1170 sample
SiC content increases from 0.5 vol.% to 5 vol.%.
Higher SiC addition, such as 10 vol.% and 20 vol.% in AS10-1230
The relationship curves of elastic modulous and hardness ver-
and AS20-1230 (Fig. 5a and b), also results in nano–nano structured
sus surface displacement for AS5-1170 sample are presented in
composites with similar microstructure as AS5-1000, AS5-1100,
Fig. 7a and b. Elastic modulous and nano-hardness exhibit high
AS5-1170 and AS5-1230. The AS10-1230 specimen exhibits very
uniformity for AS5-1170 in the surface displacement range of sta-
uniform morphology with mean grain size lower than 100 nm,
ble measurement. The sample exhibits high elastic modulous and
which is in agreement with the previous result calculated from
hardness from the microzone analysis. The mean elastic modulous
Scherrer’s formula. However, tetragonal grains with particle size
of AS5-1170 reaches 429.9 GPa and the mean nano-hardness
of about 200–500 nm precipitate from the nanostructured matrix
achieves 30.7 GPa, which reveals this sample possesses excellent
in the AS20-1230 specimen. This phenomenon reveals that grain
mechanical properties. The high mechanical properties of AS5-
growth of Al2O3 is restrained effectively with high SiC addition
1170 sample can be related with its high relative density and
(P5 vol.%). The microstructure and grain size distribution of
nano–nanocomposite structure.
Fig. 7. Nanoindenter measurement of AS5-1170 sample: (a) modulus vs. displacement to surface and (b) hardness vs. displacement to surface.
Y. Teng et al. / Journal of Alloys and Compounds 578 (2013) 67–71 71
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