Materials Science & Engineering A 723 (2018) 134–140

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Materials Science & Engineering A

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

Effects of La2O3 and Nb2O5 dopants on the microstructural development and T

fracture toughness of Al2O3 ceramic
⁎
Wen He, Yunlong Ai , Bingliang Liang, Weihua Chen, Changhong Liu
School of Material Science and Engineering, Nanchang Hangkong University, No.696, South Fenghe Avenue, Nanchang 330063, Jiangxi, PR China

A R T I C LE I N FO A B S T R A C T

Keywords: Previous research has shown that the inherently low fracture toughness of Al2O3 ceramics can be improved by in
Al2O3 composite ceramics situ growth of a small volume fraction of anisotropic grains. In this study, 7.5La2O3-5Nb2O5-87.5Al2O3 (volume
Toughening mechanism percent) composite ceramics were fabricated by microwave sintering, with the intention of tailoring alumina
In situ growth microstructural development to improve fracture toughness. The effects of sintering temperature and holding
Columnar grain
time on density and fracture toughness of the composite were investigated, and the growth and toughening
Microwave sintering
mechanisms of columnar grains were discussed. The optimal sintering conditions for La2O3/Nb2O5 doped Al2O3
ceramics occurred at 1500 °C for 30 min, which is at least 100 °C lower than that of dense Al2O3. The phases
present in the 7.5La2O3-5Nb2O5-87.5Al2O3 included in situ columnar grains of α-Al2O3 and LaAl11O18, and
equiaxed grains of monoclinic LaNbO4. It is shown that a liquid phase induced the growth of columnar grains.
The fracture toughness of the 7.5La2O3-5Nb2O5-87.5Al2O3 composite ceramic was improved by 116% compared
with that of Al2O3, due to the anisotropic grain growth that enabled toughening mechanisms such as grain pull-
out, crack deflection, crack branching, crack bridging, and domain switching.

1. Introduction
Alumina is one of the most widely used ceramics because its raw
materials are abundant and cost-effective, and its properties include
high hardness, excellent wear and corrosion resistance, high thermal
resistance, and excellent thermal and electrical insulation [1]. How-
ever, its low fracture toughness (KIC ~ 3.0 MPa m1/2) [2] restricts its use
in many applications. Much effort has been devoted in order to enhance
the toughness of Al2O3. One of the more common methods is to add a
second reinforcing phase such as particles, whiskers, or fibers to the
Al2O3 matrix [3–6]. However, this processing presents some dis-
advantages, including complex preparation steps, high costs, difficultly
to obtain a uniform dispersion of the second phase, and potential health
hazards associated with the dispersion of whiskers and fibers.
Faber and Evans predicted that an Al2O3 matrix containing more
than 10vol% columnar grains or 20 vol% platy grains would have a
greatly enhanced fracture toughness [7]. In recent years, additives or
seed crystals in Al2O3 ceramics have been used to induce growth of
columnar Al2O3 grains, thereby resulting in in situ toughening [8,9].
These columnar grains, also described as anisotropic grain growth
(AGG), develop an interlocking microstructure which results in in situ
toughening [10]. The columnar grains act much the same as whiskers
and fibers in the matrix, and toughening mechanisms such as grain pull-
out, crack bridging, and crack deflection can toughen an alumina with
AGG [11–14]. In the literature, AGG of Al2O3 ceramics has been ob-
served by introducing the dopants such as TiO2 [15], TiO2-MgO [16],
CaF2 [12], Cr2O3 [17], Na2O-MgO [18], TiO2-SiO2 [19], La2O3 [20–22],
and Nb2O5 [23]. In other case, AGG of Al2O3 ceramics was observed
when seed crystals such as α-Al2O3 abrasive powder [24,25], Al na-
noparticles [26], and α-Fe2O3 [27] were introduced prior to firing. Note
that in these prior studies, only single additions of Nb2O5, La2O3 or
other oxides or fluorides formed AGG in Al2O3 ceramics. The only
published studies on the combined addition of La2O3 and Nb2O5 to
Al2O3 ceramics have been reported by our team [28].
In order to promote the in situ growth of columnar grains and to
create a domain structure (LaNbO4) that results in improved fracture
toughness values, Al2O3 ceramics were doped with 7.5La2O3 + 5Nb2O5
(volume percent) and densified in a microwave sintering technique in
this study. The effects of sintering temperature and holding time on the
density, microstructure, and fracture toughness of 7.5La2O3-5Nb2O5-
87.5Al2O3 ceramics (abbreviated to 7.5L5N) were investigated.
2. Experimental procedure
Commercially available α-Al2O3 powders (LeiPu Ceramic Material Co.
Ltd., Shandong, China) with a purity of 99.6 wt% α-Al2O3 and a mean

⁎
Corresponding author.
E-mail address: aiyunlong62@163.com (Y. Ai).

https://doi.org/10.1016/j.msea.2018.03.057
Received 8 February 2018; Received in revised form 13 March 2018; Accepted 14 March 2018
Available online 15 March 2018
0921-5093/ © 2018 Elsevier B.V. All rights reserved.
W. He et al.
Fig. 1. MW-L0316V microwave sintering furnace.
Fig. 2. XRD patterns of the 7.5L5N composite powder (a) and ceramics (b) sintered at
1500 °C for 30 min.
particle diameter of ~ 5 µm was used as the matrix raw material and La2O3
and Nb2O5 (99.99 wt%, Sinopharm Chemical Reagent Co. Ltd., Shanghai,
China) were used as the dopant raw materials. Starting powders with a
composition of 7.5La2O3-5Nb2O5-87.5Al2O3 and 5 wt% polyvinyl alcohol
(PVA) were ball milled together in a corundum jar with corundum ball mill
media for 12 h in ethyl alcohol. After drying, the mixed powders were
pressed into pellets or bars at 100 MPa. Next, the pellets and bars were cold
Fig. 3. Influence of sintering process on relative density and fracture toughness of 7.5L5N composite ceramics: (a) density as a function of temperature at a constant sintering time of
30 min (b) density as a function of holding time at a constant sintering temperature of 1500 °C.
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Materials Science & Engineering A 723 (2018) 134–140
isostatically pressed at 200 MPa and then calcined in a muffle furnace at
600 °C for 3 h to eliminate the organic binder. The green compacts were
sintered at various temperatures between 1450 °C and 1550 °C for times up
to 60 min using a 2.45 GHz multimode microwave sintering furnace (MW-
L0316V, shown in Fig. 1) in an air atmosphere.
The densities of the sintered specimens were measured by the
Archimedes method. The phase compositions were identified using an X-ray
diffractometer (XRD, D8ADVANCE, Bruker-AXS) with Cu-Kα radiation. The
microstructural and elemental analyses were carried out on as-heated speci-
mens using a field emission scanning electron microscope (FESEM, Nova
NanoSEM450, FEI) and energy dispersive spectroscopy (EDS, INCA Energy
250 X-max 50, Oxford Instruments), respectively. The crystal structure was
characterized by high resolution transmission electron microscopy (HRTEM,
Tecnai™ G2 F30, FEI). Using GB/T 23806-2009 standards, fracture toughness
(KIC) was measured by a single edge precracked beam (SEPB) method using a
universal testing machine (WDW-50, Jinan Times Instrument Co. LTD.,
China). After the samples were ground and polished to remove microcracks
and defects in the surface layers, the final specimen was a rectangular bar of
2 mm × 4 mm× 36 mm, with edges ground to R0.5 mm. The span and
crosshead speed for fracture toughness tests were 30 mm and 0.5 mm/min,
respectively. In each test, the maximum load prior to fracture was recorded
for the calculation of KIC.
3. Results and discussion
3.1. Phase composition of the 7.5L5N composite ceramics
The XRD patterns of the 7.5L5N composite powder and dense
ceramics sintered at 1500 °C for 30 min are shown in Fig. 2. The dif-
fraction spectrum of the fired 7.5L5N composite ceramic (Fig. 2b) was
composed of α-Al2O3, monoclinic LaNbO4 and LaAl11O18, but there
were no peaks associated with La2O3 and Nb2O5. We deduced that
Nb2O5 reacted with La2O3 to form LaNbO4 at ~ 1000 °C during the
sintering process [29], and then the surplus La2O3 reacted with Al2O3 to
form LaAl11O18 according to the following reactions [30]:
La2O3 + Nb2O5 → 2LaNbO4 (1)
La2O3 + 11Al2O3 → 2LaAl11O18 (2)
3.2. Effect of microwave sintering process on the 7.5L5N composite
ceramics
The effects of microwave sintering temperature and holding time on
the relative density and fracture toughness of the 7.5L5N composite
ceramic are presented in Fig. 3. With the increase of sintering
W. He et al.
Fig. 4. SEM images of the 7.5L5N composite ceramics sintered at different temperature for 30 min (a) 1450 °C, (b) 1475 °C, (c) 1500 °C, (d) 1550 °C.
temperature, the relative density and fracture toughness both increased
at first, then reached maximum values, and finally decreased (Fig. 3a).
At 1500 °C, the relative density and fracture toughness had the highest
values of 99.3% and 6.49 MPa m1/2, respectively, and this optimum
sintering temperature for 7.5L5N composite ceramic was at least 100 °C
lower than that of a pure Al2O3 ceramic (> 1600 °C) [31,32]. Possible
reasons for this improved density at lower sintering temperatures may
be the use of a microwave sintering process and the existence of a liquid
phase from the La and Nb oxides during the sintering process [33].
When holding times were extended from 30 min to 60 min at
1500 °C, the relative density increased slightly, but the fracture
toughness decreased slightly (Fig. 3b). Because no further improve-
ments in fracture toughness and density were made with additional
time at temperature, the optimum sintering conditions for this study
were 1500 °C for 30 min. Comparing Fig. 3a and b, the sintering tem-
perature appeared to have more effect than holding time on the density
of sintered samples.
When the temperature was low (1450 °C), the microstructure was
not fully developed (93.2% of theoretical density) and it contained a
significant amount of closed porosity. With the increase of temperature
from 1450 °C to 1475 °C or 1500 °C, a liquid phase contributed to well-
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Materials Science & Engineering A 723 (2018) 134–140
developed grains and few pores in the sample, and the density at
1500 °C was not sensitive to holding time (Fig. 3b). More micro-
structural details will be discussed in the microstructural analysis pre-
sented in the next section. As the sintering temperature increased above
1500 °C, the density of sintered samples decreased slightly, likely due to
grain growth. Therefore, we concluded that the optimal microwave
sintering process for 7.5L5N composite ceramics was 1500 °C for
30 min.
3.3. In-situ growth of columnar grains
Fig. 4 shows SEM images of the 7.5L5N composites sintered at dif-
ferent temperatures for 30 min. The phases in the 7.5L5N composites
were identified by combining the results of XRD shown in Fig. 2b and
EDS shown in Fig. 5 which indicate the presence of Al2O3, LaAl11O18
and monoclinic LaNbO4 (marked by points B, D, C in Fig. 5a, respec-
tively). These three phases were also specified in Fig. 4c (the lower
magnification of Fig. 5a). In the SEM micrographs, black grains were
Al2O3, gray grains were LaAl11O18, and white grains were LaNbO4. In
some cases, the black Al2O3 grains grew into columnar grains, while the
gray LaAl11O18 grains were both platy and columnar. The white
W. He et al.
Fig. 5. EDS results of the 7.5L5N composite ceramics sintered at 1500 °C for 30 min.
LaNbO4 appeared to be distributed on the grain boundaries of Al2O3
and LaAl11O18.
High purity alumina typically does not exhibit AGG. Adding dopants
to alumina can generate AGG by means of introducing a liquid phase
during sintering, by solute drag, by adsorption on grain boundary dis-
locations, etc., but presence of a liquid phase is often the most common
mechanism for AGG [15–19]. The distribution of white LaNbO4 on the
grain boundaries of columnar grains in the long axis direction suggests
that LaNbO4 plays a role in the columnar growth of Al2O3 and
LaAl11O18 during the sintering process. The sample sintered at 1450 °C
had a few columnar grains (Fig. 4a), which suggests that a liquid phase
was generated at this temperature. The reported melting point of
LaNbO4 is 1670 °C ± 20 °C [34], but this work demonstrated that mi-
crowave sintering decreased the sintering temperature by about 200 °C,
most likely because the thermal vibration between the molecules was
intensified. As the temperature in our study was increased (1475 °C or
1500 °C), there
was more liquid phase available to promote a greater number of
columnar grains (Fig. 4b and c). When the temperature was increased to
1550 °C, some grains coarsened and the grains became more equiaxed,
probably due to the excessive liquid phase (Fig. 4d).
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Materials Science & Engineering A 723 (2018) 134–140
TEM images and electron diffraction patterns of the 7.5L5N com-
posites are shown in Fig. 6. A particularly large anisotropic Al2O3 grain,
a smaller columnar LaAl11O18 grain, and a monoclinic LaNbO4 phase
exhibiting domain structure and ferroelasticity were detected in Fig. 6a.
The selected area electron diffraction (SAED) patterns of the columnar
LaAl11O18 and the monoclinic LaNbO4 grains are shown in Fig. 6b and
Fig. 6c, respectively. The LaAl11O18 protruded into the grain boundary
between two LaNbO4 grains, which further illustrates the in situ growth
of columnar grains. Theoretically, when liquid phase LaNbO4 wets the
surface of an Al2O3 or LaAl11O18
grain, the surface energy decreases and allows to in situ growth of
columnar grains. This mechanism was evident in Fig. 6d, where a liquid
phase of LaNbO4 likely migrated to the grain boundaries, resulting in
several Al2O3 columnar grains.
3.4. Toughening mechanism of 7.5L5N composite ceramics
Our measured values for fracture toughness at room temperature
were higher (Fig. 2) than previously reported values for Al2O3 com-
posites [35], and our highest fracture toughness was 116% greater than
that of pure, dense Al2O3 [2]. This improvement in fracture toughness is
W. He et al.
Fig. 6. TEM images and electron diffraction patterns of the 7.5L5N composite ceramics.
attributed to the in-situ growth of the columnar grains of Al2O3 and
LaAl11O18. Fig. 7 shows SEM images of the crack propagation paths in
the 7.5L5N composites sintered at 1450 °C for 60 min. When the cracks
encountered columnar grains within the matrix, their propagation
paths were changed, likely due to typical toughening mechanisms of
grain pull-out (Fig. 7a), crack deflection (Fig. 7a and b), crack
branching (Fig. 7b) and crack bridging (Fig. 7c).
Besides toughening mechanisms that are related to the elongation of
crack path, domain structure switching of ferroelastic LaNbO4 grains
may also have an impact on improved fracture toughness in 7.5L5N
composite ceramics. The domain structure of ferroelastic LaNbO4 grains
in the 7.5L5N composites sintered at 1475 °C and then immediately
cooled is presented in Fig. 8. In this image, the domain appeared as a
flat sheet arranged in parallel at equal widths, where the domain widths
ranged from 18.5 nm to 27 nm, depending on the orientation of the
grain with respect to the image. A ferroelastic crystal has two or more
states (orientations) in the condition without mechanical stress and can
be transformed from one to another of these states when it is submitted
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Materials Science & Engineering A 723 (2018) 134–140
to mechanical stress [36]. Tsunekawa and Takei directly confirmed
domain switching of LaNbO4 by measurements for hysteresis in its
stress-strain curves [37]. It is likely that LaNbO4 may release the stress
concentration ahead of a crack tip via domain switching, resulting in
improved fracture toughness. Domain switching in ceramic has also
reported in other studies [38,39].
It is important to mention that there were likely multiple tough-
ening mechanisms occurring simultaneously in these 7.5L5N compo-
sites, including grain pull-out, crack deflection, crack branching, crack
bridging and domain structure switching. Each of these toughening
mechanisms may not have significantly enhanced toughening alone,
but synergistically toughened the composite by their interactions with
each other.
4. Conclusions
We fabricated 7.5La2O3-5Nb2O5-87.5Al2O3 composite ceramics by
microwave sintering at 1450–1550 °C for hold times up to 60 min, and
W. He et al. Materials Science & Engineering A 723 (2018) 134–140

Fig. 7. SEM images of the crack propagation paths in the 7.5L5N composite ceramics (1450 °C, 60 min).

Fig. 8. Domain structure of LaNbO4 in the 7.5L5N composite ceramics heated to 1475 °C and immediately cooled.

the optimal microwave sintering conditions were 1500 °C for 30 min.
The microwave sintering temperature of our Al2O3 ceramics doped with
La2O3/Nb2O5 was at least 100 °C lower than sintering temperatures for
pure Al2O3 ceramics. The phases present in the 7.5L5N composite
ceramics consisted of α-Al2O3, LaNbO4, and LaAl11O18. During the
sintering process, LaNbO4 and the columnar grains of Al2O3 and
LaAl11O18 were formed in situ. TEM, SEM, and EDS results indicated
that a liquid phase was responsible for in situ growth of columnar
grains. The fracture toughness of the composite ceramics was 116%
higher than the fracture toughness of pure Al2O3 ceramic due to the

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W. He et al.
toughening mechanisms of grain pull-out, crack deflection, crack
branching, crack bridging and domain structure switching.
Acknowledgements
This work is financially supported by the National Natural Science
Foundation of China (Grant No.51064022), Aeronautical Science
Foundation of China (Grant No.2010ZF56020) and the Jiangxi
Provincial Department of Education Science and Technology Project
(DB201601012, DA201701375). The authors gratefully acknowledge
the Instrumental Analysis Centre of Northwestern Polytechnical
University for the TEM experimental assistance.
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