Journal of Alloys and Compounds 783 (2019) 806e812

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Journal of Alloys and Compounds

journal homepage: http://www.elsevier.com/locate/jalcom

Low-temperature preparation of Al2O3-ZrO2 nanoceramics via

pressureless sintering assisted by amorphous powders
Xiqing Xu a, Yan Yang b, Xingang Wang a, Xinghua Su a, Jiachen Liu c, *
a
School of Materials Science & Engineering, Chang'an University, Xi'an, 710061, People's Republic of China
b
College of Communication Engineering, Chengdu University of Information Technology, Chengdu, 610225, People's Republic of China
c
Key Laboratory for Advanced Ceramics and Machining Technology of Ministry of Education, School of Materials Science and Engineering, Tianjin
University, Tianjin 300072, People's Republic of China

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

Article history: In present work, Al2O3 nanoceramics toughened with 5 mol% ZrO2 and 10 mol% ZrO2 were prepared by
Received 3 June 2018 pressureless sintering; polycrystalline ZrO2 powders and Al2O3-ZrO2 amorphous powders were used as
Received in revised form dopants in conventional sintering and amorphous-phase-assisted sintering, respectively. In amorphous-
9 December 2018
phase-assisted sintering, the densification of Al2O3-ZrO2 nanoceramics was highly promoted, and
Accepted 31 December 2018
Available online 2 January 2019
nanoceramics with composition of Al2O3-5 mol% ZrO2 and Al2O3-10 mol% ZrO2 were almost fully
densified at temperature as low as 1350
C. The easy densification was attributed to the metastable state
and phase transition of amorphous powders, which acted as sintering aids. The nanoceramics exhibited
Keywords:
Pressureless sintering
dense and homogenous mixture of Al2O3 and ZrO2 particles with fine grain size, and the microstructure
Amorphous powders refinement further contributed to superior mechanical properties with high Vickers hardness, bending
Densification behavior Al2O3-ZrO2 strength and Weibull modulus values. This work may provide new guidance for low temperature
nanoceramics fabrication of nanoceramics by employing amorphous powders as sintering aids.
Phase transition © 2019 Elsevier B.V. All rights reserved.

1. Introduction techniques are presented to manage pressureless sintering at low

temperatures, e.g., liquid-phase sintering [15,16], two-step sinter-
Low-temperature sintering has received distinct technological ing [17,18], sintering assisted by sintering aids or dopants [19,20],
and scientific attentions in the fields of ceramics and powder and phase-transition-assisted sintering [21e23].
metallurgy. One of the most important advantages of low- Sintering assisted by phase transition is an effective technique of
temperature sintering is refined microstructure, which leads to low temperature sintering. The phase transition from metastable to
superior mechanical properties [1e3]. There are some other ben- stable phase can easily occur in sintering and improve the atomic
efits, including low cost for heating apparatus and consumable diffusion as well as particle rearrangement, and this is beneficial to
items, avoidance of melting at high temperature [4], preventing the efficient densification into full dense structure at low temper-
unwanted reactions of constituents in sintering [5], attainment of ature without serious grain growth. Recently, various ceramic
demanded functional properties [6,7]. In this regard, several tech- materials have been prepared taking advantages of this technique,
niques have been proposed to achieve sintering at low temperature, which was accompanied by transformation from metastable to
which include spark plasma sintering [8,9], hot pressing [10], hot stable phase, including transition of TiO2 from anatase to rutile
isostatic pressing [11], pulsed electric current sintering [12]. How- phase [21], Al2O3 transforming from gamma to alpha [22], transi-
ever, these methods require applications of simultaneous pressure tion from cubic to monoclinic Y2O3 [23].
during sintering, and the products are generally limited by the In our previous work, Al2O3-ZrO2 nanocomposites were fabri-
molds both in shape and size. Actually, pressureless sintering is cated by hot pressing [24] and pressureless sintering [25] of Al2O3-
more attractive in preparing ceramic products due to its lower cost, ZrO2 amorphous powders, which were benefited from amorphous
controllable shape and simplicity [13,14]. Fortunately, some to crystalline phase transition of the Al2O3 and ZrO2. However,
attributed to the strong tendency in crystallization of the Al2O3-
ZrO2 system, only powders near eutectic composition could be
* Corresponding author. obtained in amorphous state, a condition highly constraining the
E-mail address: [email protected] (J. Liu). constituent ratio in products. In fact, Al2O3-ZrO2, as one of the most

https://doi.org/10.1016/j.jallcom.2018.12.372
0925-8388/© 2019 Elsevier B.V. All rights reserved.
 X. Xu et al. / Journal of Alloys and Compounds 783 (2019) 806e812 807

important ceramic systems, generally exhibits microstructures and 50 MPa, followed by cold isostatic pressing at 200 MPa. To estimate
properties strongly dependent on the constituent ratio in a wide the densification behavior of the Al2O3-ZrO2 samples, the green
range [26,27]. We propose that, the Al2O3-ZrO2 amorphous pow- bodies were first sintered in a dilatometer (Netzsch DIL402C) in air
ders with eutectic composition might be doped into polycrystalline atmosphere, using a constant heating rate of 5
C/min. Sintering
powders having a single phase, and employed as sintering aids, to was carried out on the green bodies in air under ambient pressure
obtain Al2O3-ZrO2 nanoceramics distinct from eutectic using a muffle furnace, during which the samples were heated at
composition. the heating rate of 5
C/min, up to temperatures of 1200e1400
C,
To explore the possibility of employing amorphous powders as and 2 h were maintained before cooling in the furnace.
sintering aids, polycrystalline ZrO2 powders and Al2O3-ZrO2 Bulk densities of Al2O3-ZrO2 nanoceramics after sintering were
amorphous powders were added into Al2O3 powders and they measured in terms of Archimedes' method (ASTM C373), and each
acted as dopants, respectively; the effect of different dopants on result was obtained through the mean value of 10 samples.
pressureless sintering was investigated. It was confirmed that, the Microstructural investigations of the sintered nanoceramics
doping of amorphous powders highly promote the densification, were carried out using SEM (Model S4800, Hitachi, Japan). The SEM
which was mainly attributed to the phase transition of metastable samples were polished after sintering, followed by thermal etching
amorphous powders. By means of pressureless sintering assisted by for 30 min at temperatures 300
C lower than the sintering tem-
amorphous powders, near full dense Al2O3- 5 mol% ZrO2 and Al2O3- peratures to reveal the grain boundaries. Based on the SEM images,
10 mol% ZrO2 nanoceramics were obtained, and the microstruc- the particle size was determined using the Nano Measurer.
tures and mechanical properties were characterized. Vickers hardness were determined by the of indentation
method using a microhardness indentation equipment (HXD-
2. Experimental details 1000TM, Shanghai). 10 N was loaded on the polished surface and
held for 15 s, and 20 indentations were made on each sample and
2.1. Raw powders the mean values of these measurements were taken as the hard-
ness value. Vickers hardness (HV) values were calculated based on
Al2O3 powders (Sumitomo, Japan) were utilized as the matrix measurements of the diagonal lengths of an indentation, seen in a
phase, and amorphous Al2O3-ZrO2 powders were used as dopants, SEM image using the formula [28].
to provide the toughening phase and act as sintering aids. The
amorphous powders with composition of Al2O3-40 mol% ZrO2 P
HV ¼ 1:854 (1)
(doped by 3 mol% Y2O3), were prepared via sol-gel method fol- d2
lowed by calcination at 800
C for 2 h, and detailed procedures
were reported in our earlier work [24]. To investigate the effect of where P is the load and d is the mean value of the diagonal length.
different dopants on pressureless sintering, polycrystalline ZrO2 Three-point bending measurements were carried out using an
powders (doped by 3 mol% Y2O3, Tosoh, Japan) were also added electron mechanical universal material testing machine
into Al2O3 powders as a comparison. The sintering with additive of (Instron5500R, USA). The dimension of the as-sintered bars was
amorphous Al2O3-ZrO2 powders are defined hereafter as 1.5  2  30 mm, and the loading rate was 1 mm/min using a span
amorphous-phase-assisted sintering (AM), and the other with of 20 mm. The flexure strength (s) was calculated based on the
polycrystal ZrO2 powders was marked as conventional sintering equation [29],
(CS), hereafter. To obtain Al2O3-5 mol% ZrO2 or Al2O3-10 mol% ZrO2
3PL
nanoceramics via different sintering methods, the detailed molar s¼ (2)
fractions of different raw powders are listed in Table 1. The nano- 2bd2
ceramics prepared by conventional sintering are hereafter labeled where, P is the load at which the bars broke down, L is the support
as A5Z-CS and A10Z-CS. Similarly, the samples via amorphous- span, b is the specimen width, and d is the specimen thickness.
phase-assisted sintering are labeled as A5Z-AM and A10Z-AM. Each measurement was tested on 8 specimens, and the mean
In order to disperse the additives of polycrystalline ZrO2 pow- values of these measurements were taken as the three-point
ders or amorphous Al2O3-ZrO2 powders into the Al2O3 powders, bending values.
and obtain homogenous distribution of the mixed powders, the
raw powders were ball milled for 24 h using ethanol as solvent.
After ball milling, the mixture was dried in air and sieved through 3. Results
80-mesh. The resultant powder mixture was quite uniform.
To characterize the morphology and particle size of the raw 3.1. Powders characterization
powders, scanning electron microscope investigations (SEM, Model
S4800, Hitachi, Japan) was carried out. Particle sizes were SEM tests were carried out on the raw powders, and the mi-
measured from the SEM images using the software Nano Measurer. crographs were shown in Fig. 1. Both spherically and nonspherically
shaped particles were exhibited in the a-Al2O3 powders (Fig. 1a),
2.2. Green bodies and sintering and these sharp edges suggested the low surface energy in the
Al2O3 particles. In Fig. 1b, the primary particles in the ZrO2 powders
The raw powders were uniaxially pressed into green bodies at were round in shape with soft particle contacts, and quite fine in

Table 1
Molar constituents of starting powders prepared via conventional sintering and amorphous-phase- assisted sintering.

Method Label Al2O3 powder ZrO2 powder amorphous powder

conventional sintering A5Z 95 mol% 5 mol% 0

A10Z 90 mol% 10 mol% 0
amorphous-phase-assisted sintering A5Z 87.5 mol% 0 12.5 mol%
A10Z 75 mol% 0 25 mol%
808 X. Xu et al. / Journal of Alloys and Compounds 783 (2019) 806e812

Fig. 1. SEM images of the raw powders before mixing: (a) a-Al2O3 powders, (b) t-ZrO2 powders, and (c) amorphous Al2O3-ZrO2 powders.

nature with a uniform size distribution. In Fig. 1c, the morphology

of the amorphous powders was similar to that of ZrO2 powders, the
small particles were mostly spherically and slightly agglomerated
due to the high-energy surfaces. Based on the SEM images, the
average particle size of the Al2O3 powders was about 190 nm, and
the mean values of ZrO2 powders and amorphous powders were
30 nm and 25 nm, respectively.

3.2. Densification behavior

Fig. 2 exhibited the comparison on shrinkage behaviors between

A5Z nanoceramics prepared by conventional sintering and
amorphous-phase-assisted sintering at the constant heating rate of
5
C/min. In conventional sintering, the shrinkage started at about
1150
C, and it was accelerated with increasing temperature.
Apparently, the linear shrinkage was attributed to the densification
of the bulk ceramic due to the particle rearrangement and mass
diffusion. Shrinkage rate versus temperature was also plotted in
Fig. 2, and the maximum shrinkage rate was recorded in the vicinity
of 1370
C for the sample A5Z-CS. After heating to 1420
C without
soaking time, the sample exhibited a final linear shrinkage of 25%.
In amorphous-phase-assisted sintering, the shrinkage curve was
similar to that in conventional sintering; however, the shrinkage
rate exhibited two local maximal values at 920
C and 1213
C.
Detailed crystallization pathways of amorphous Al2O3-ZrO2 were
studied in a previous work [31], and the peaks of shrinkage rate at
920
C and 1213
C could be attributed to the crystallization of t-
ZrO2 and g-Al2O3 from amorphous phase, respectively. Further-
more, the amorphous-phase-assisted sintering highly promoted
the shrinkage or densification of the A5Z sample. Compared to
Fig. 2. Linear shrinkage and shrinkage rate versus temperature for Al2O3- 5 mol% ZrO2
conventional sintering, the maximal shrinkage rate in A5Z-AM
samples prepared via conventional sintering and amorphous-phase- assisted sintering.
sample was shifted to a lower temperature of 1323
C; the final
linear shrinkage was also increased to 36%.
Fig. 3 shows the shrinkage behaviors of A10Z nanoceramics shrinkage rate was exhibited at 1357
C, and the final linear
conventionally sintered and that sintered via the amorphous- shrinkage was 28% after heating, slightly higher than that in the
phase-assisted sintering. In conventional sintering, the maximum A5Z-CS sample. The A10Z-AM sample exhibited a shrinkage curve
 X. Xu et al. / Journal of Alloys and Compounds 783 (2019) 806e812 809

Fig. 4. Relative densities of A5Z and A10Z nanoceramics versus temperature in con-
ventional sintering and amorphous-phase-assisted sintering.

sintering temperature reached 1350
C. Almost full dense was

achieved in A5Z and A10Z nanoceramics during amorphous-phase-
assisted sintering, inferring that the additive of amorphous Al2O3-
ZrO2 powders highly promoted the densification of Al2O3-ZrO2
nanoceramics, compared to the doping of polycrystal ZrO2 pow-
ders. In our previous work [24], Al2O3-ZrO2 nearly full dense
nanoceramics were prepared by hot pressing of nanocrystalline or
amorphous powders, and the amorphous powders were easily
Fig. 3. Linear shrinkage and shrinkage rate versus temperature for Al2O3- 10 mol% shaped into dense bulk nanoceramics, compared to nanocrystalline
ZrO2 samples prepared via conventional sintering and amorphous-phase- assisted
powders. Therefore, it can be stated that, the contribution of the
sintering.
amorphous state to densification should be attributed to the
smaller particle size, plastic deformation, and phase transformation
similar to that of A5Z-AM, i.e., two local maximum shrinkages in amorphous powders. In another work [25], Al2O3-ZrO2 nano-
occurred at 918
C and 1216
C in the shrinkage rate curve of the ceramics were obtained from powders sintered at different degrees
A10Z-AM sample (Fig. 3b) due to the crystallization of t- ZrO2 and of crystallinity. Powders with crystallinity of 25 vol% exhibited the
g-Al2O3. Compared to the A5Z-AM sample, the A10Z-AM sample best sinterability due to the crystallization of amorphous phase
exhibited distinct shrinkage and densification values. As a result, promoted by the nanocrystalline phase as nucleation seeds. In the
the maximum shrinkage rate in A10Z-AM sample was lowered to present investigation, the easier densification in amorphous-
1296
C and the final linear shrinkage was further elevated to 43%. phase-assisted sintering can also be attributed to the metastable
Following the sintering of nanoceramics at different tempera- state of amorphous phase. Due to the high-energy state, surface
tures for 2 h, the bulk densities were evaluated using the Archi- and bulk diffusion was faster in amorphous powders than in
medes' method, and the relative densities were calculated and polycrystal ones, which acted as sintering aids. Moreover, the phase
plotted in Fig. 4. During conventional sintering of A5Z sample, the transition from amorphous to crystalline phase took place easily,
nanoceramic exhibited a monotonic increase in relative density with large decrease in free energy. Similarly, as reported in various
from 79.8% at 1200
C to 96.0% to 1400
C. The conventionally studies [21e23], the phase transition highly promoted the atomic
sintered A10Z sample, showed similar variation tendency in mobility, mass diffusion, and the particle rearrangement, and
densification behavior, and the relative density increased from speeded up the densification as a result.
81.3% to 96.2% with increasing temperature, slightly higher than
that for the sample A5Z-CS. A similar behavior was reported in Ye's 3.3. Microstructure
work [32], who stated that the uniform dispersion of ZrO2 nano-
powders were beneficial to the densification of Al2O3 ceramics, and Fig. 5 shows the SEM micrographs of the A5Z and A10Z nano-
effectively restrained the severe grain growth. Ma et al. [33] ceramics sintered at 1350
C for 2 h via conventional sintering and
investigated the effects of ZrO2 doping on the sintering densifica- amorphous-phase-assisted sintering. The microstructure of the
tion of the Al2O3 matrix composites and confirmed that the relative A5Z-CS (Fig. 5a) and A10Z-CS (Fig. 5b) are not dense with quite a
density increased with increasing ZrO2 content when it was below few of porosities around the grains, confirming with the relative
15 vol% and decreased when the doping was higher than 15 vol%. density of about 95% and in Fig. 5. However, the samples A5Z-AM
However, after conventional sintering at temperatures below and A10Z-AM in Fig. 5c, d reveal dense microstructures with
1400
C, the A5Z and A10Z nanoceramics could not be sintered to almost no pores, suggesting that full dense was achieved after
full density due to insufficient free energy for particle rearrange- amorphous-phase-assisted sintering at 1350
C, in agreement with
ment and mass diffusion at these temperatures. the relative density of higher than 99%. In this dense microstruc-
In amorphous-phase-assisted sintering, the A5Z and A10Z ture, the light ZrO2 particles and dark Al2O3 grains are homoge-
nanoceramics displayed much higher relative densities than those neously and tightly mixed. Based on the image-forming
in conventional sintering, and the values were close to 100% as the mechanisms, the dark particles were Al2O3 phase and the light ones
810 X. Xu et al. / Journal of Alloys and Compounds 783 (2019) 806e812

Fig. 5. SEM images of Al2O3-ZrO2 samples sintered at 1350
C by conventional sintering and amorphous-phase-assisted sintering: (a) A5Z-CS, (b) A10Z-CS, (c) A5Z-AM, (a) A10Z-
AM.

were ZrO2, as marked in Fig. 6c. amorphous powders, which were much finer than those from Al2O3
The average sizes of Al2O3 or ZrO2 particles in different samples raw powders. In sample A5Z-AM, the mean grain sizes were
are displayed in Fig. 6. In each of the sintered samples, Al2O3 grains 350 nm and 96 nm for the Al2O3 and ZrO2 particles, respectively;
were significantly larger than ZrO2 grains, due to the large particle these values were 320 nm and 103 nm for sample A10Z-AM. In the
size of Al2O3 raw powders. Regardless of the sintering methods, work of Ma [33], Al2O3-10 vol% ZrO2 ceramics with nearly full dense
A10Z samples exhibited smaller Al2O3 grains and larger ZrO2 grains were prepared by conventional sintering at 1550
C for 1.5 h, and
than A5Z nanoceramics. It was suggested that, ZrO2 particles as the the average particle size was larger than 0.9 mm. According to
second phase, could hinder the grain boundary motion of Al2O3 Chinelatto [36], Al2O3-5 vol% ZrO2 ceramics were fabricated
matrix and suppress the grain growth, and similar behaviors have through two-step sintering of T1 ¼1450
C/5 min and T2 ¼ 1400
C/
been reported and explained by Meng [34] and Sternitzke [35]. 8 h and relative density of 98.5 was achieved with a mean grain size
Whatever molar fraction of ZrO2 in the sintered nanoceramics, of about 540 nm. As reported by Meng [34], full dense Al2O3
the samples prepared by amorphous-phase-assisted sintering had composites containing 5 and 10 wt% of ZrO2 were obtained via
much smaller grain sizes of both Al2O3 and ZrO2 particles than spark plasma sintering under 100 MPa and their mean grain sizes
those via conventional sintering. In Al2O3-ZrO2 nanoceramics sin- were about 800 nm and 650 nm, respectively. It was suggested that,
tered via amorphous-phase-assisted sintering, quite a few of the the additive of amorphous powders highly promoted the densifi-
Al2O3 particles were developed from Al2O3-40 mol% ZrO2 cation of Al2O3-ZrO2 nanoceramics, and significantly decreased the
sintering temperature for full dense in this work, which further
contributed to the microstructure with fine grain size.

3.4. Mechanical properties

Vickers microhardness (HV) and bending strength (s) of the A5Z

and A10Z ceramics prepared by conventional sintering and
amorphous-phase-assisted sintering are listed in Table 2, and the
Weibull modulus extracted from the Weibull plot of the bending
strength are shown in Fig. 7. It is given evident that, either A5Z or

Table 2
Summary of the measured mechanical properties of Al2O3-ZrO2 samples prepared
via conventional sintering and amorphous-phase-assisted sintering.

Mechanical Vickers Hardness Bending Strength Weibull

Property (GPa) (MPa) Modulus

A5Z-CS 13.6 ± 0.9 760 ± 140 6.0

A5Z-AM 17.8 ± 0.7 990 ± 70 10.2
A10Z-CS 14.2 ± 0.8 820 ± 120 6.3
A10Z-AM 16.9 ± 0.5 1030 ± 60 11.3
Fig. 6. The average size of Al2O3 or ZrO2 particles in different samples.
 X. Xu et al. / Journal of Alloys and Compounds 783 (2019) 806e812 811

2018JM5170).

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