International Journal of Refractory Metals & Hard Materials 69 (2017) 60–65

Contents lists available at ScienceDirect

International Journal of Refractory Metals

& Hard Materials
journal homepage: www.elsevier.com/locate/IJRMHM

Hardness and toughness enhancement of CeO2 addition to ZTA ceramics MARK

through HIPping technique
Nik Akmar Rejab, Wei Kean Lee , Zhwan Dilshad Ibrahim Sktani, Zainal Arifin Ahmad⁎
Structural Materials Niche Area, School of Materials and Mineral Resources Engineering, Engineering Campus, Universiti Sains Malaysia, 14300 Nibong Tebal, Penang,
Malaysia

A R T I C L E I N F O A B S T R A C T

Keywords: The aim of this research is to investigate the combined effects of CeO2 additions and hot-isostatic pressing
Hip sintering (HIPping) technique on the hardness and toughness of ZTA ceramics. Addition of CeO2 to ZTA ceramics
CeO2 added ZTA leads to formation of a secondary phase (CeAl11O18) which played a vital role in affecting the Vickers hardness
Bulk density and toughness. Microstructure investigations showed that HIPping had a significant role in the removal of pores,
Vickers hardness
and consequently affected both hardness and toughness of the samples. The highest Vickers hardness
Fracture toughness
(1838.3 HV) and toughness (8.92 MPa·√m) were obtained with the 5 wt.% CeO2 additions that also had the
highest bulk density (4.48 g/cm3) and the lowest percentage of porosity (0.37%).

1. Introduction
Zirconia toughened alumina (ZTA) as one of the most widely used
ceramics in technological applications has been subjected to extensive
research that focused on their hardness and toughness improvement. As
an example, ZTA ceramic cutting inserts facing its premature tool
failure by chipping or catastrophic failure during services [1,2]. This
failure corresponded to its relatively low hardness, poor room tem-
perature ductility and toughness which limits ZTA as cutting tools ap-
plication. Thus, several solutions have been proposed for hardening and
toughening improvement through the effects of secondary phase dis-
persion [3–12]. The effects that originated from the contribution of
larger and elongated grains have been shown to significantly relate to
the crack mechanisms modes. However, these crack mechanisms
(transgranular or intergranular modes) are only useful for the toughness
improvement. The toughness will be improved by the intergranular
cracks that propagate around the grains which indirectly lengthened
the crack paths [8,13,14]. Therefore, the ZTA ceramics toughness can
be improved by this approach while on the other hand, this occurs at
the expense of microstructural porosity. Rejab et al. [8] improved the
ZTA toughness through the addition of two different oxides i.e. 1 wt.%
of CeO2 and 0.7 wt.% of MgO using pressureless sintering technique at
1600 °C for 4 h. The highest toughness recorded was 6.59 MPa·√m,
however, the hardness value was less than that of pure ZTA. The
hardness reduction is due to the change in Al2O3 grain size, non-uni-
form grain shapes and porosity which was originated from the excessive
grain growth [15–17]. Rejab et al. [18] also introduced CeO2 additive
which acts as a secondary phase dispersion into ZTA matrix. The frac-
ture toughness showed an increase of 30% compared to pure ZTA. The
highest fracture toughness (8.38 MPa·√m) and Vickers hardness
(1688 HV) were obtained from 5 wt.% of CeO2 addition. They in-
vestigated the CeAl11O18 phase formation which was due to exceeding
limit of CeO2 solid solution, and hence contribute to abnormal growth
(platelet grains) among ZrO2 grains.
Consequently, this affects the mechanical properties of ZTA. Study
by Sktani et al. [6] reported the impact of in-situ formation of
CaAl12O19 (hibonite) on the microstructure and mechanical properties
of ZTA. Addition of 0–13 wt.% CaCO3 produced the highest toughness
of 6.3 MPa·√m, however, Vickers hardness decreased from 1603.4 HV
to 654 HV. Furthermore, the porosity of the sample increased from
0.77% to 14.91%. They also found that, the higher the amount of
CaCO3 added, the higher the amounts of CaAl12O19 and porosity. These
contribute to the excessive grain growth which deteriorates the ZTA
properties [18,19]. Therefore, it is obvious that the secondary phase
dispersion approach is only effective to toughness improvement of ZTA
but not to its hardness [20]. This problem needs to be solved to ensure
ZTA-based materials have high toughness without sacrificing their
hardness for higher quality applications.
Basically, both hardness and toughness of ZTA-based materials
could be improved through their microstructure modification [19–21].
Therefore, the best approach to solve the problem is through the im-
provement of their microstructure [22,23]. One of the approaches for
the development and improvement of microstructure is through sin-
tering method. For example, the densification of ZTA has been achieved

⁎
Corresponding author.
E-mail address: srzainal@usm.my (Z.A. Ahmad).

http://dx.doi.org/10.1016/j.ijrmhm.2017.08.002
Received 21 June 2017; Received in revised form 25 July 2017; Accepted 1 August 2017
Available online 04 August 2017
0263-4368/ © 2017 Published by Elsevier Ltd.
N.A. Rejab et al.
mostly by hot isostatic pressing (HIPping) from 1400 °C to 1650 °C
[24–26]. This process has been recognised to be an effective sintering
technique to achieve full densification [27]. Dong et al. [26] found that
the best mechanical properties were obtained from HIPped ZTA at
100 MPa and 1600 °C for 1 h. They found that the density obtained was
almost the maximum theoretical density. These specimens have a four-
point bend strength of 940 ± 15 MPa at room temperature and
540 ± 15 MPa at 1000 °C and an indentation fracture toughness at
room temperature of 9.4 ± 0.2 MPa·√m. This property are attributed
to the “healing” of flaws at the higher HIPping temperature, which
results in a reduction in critical flaw size. Although, the effectiveness of
using HIPping towards the density, strength and toughness of ZTA
ceramics have been reported, specifically there is no report about the
influence of secondary phase dispersion on the combination properties
of toughness and hardness improvement via direct HIPping method.
Therefore, this paper reports the effect of direct HIPping on the
hardness and toughness properties of ZTA ceramics by using CeO2 ad-
dition in ZTA. The results were compared to our previous work [18]
where pressureless sintering was used in order to show the influence of
HIPping condition on microstructure.
2. Materials and methods
The composition of CeO2 was varied from 0 wt.% to 7.0 wt.%. The
starting materials was mixed continuously for 8 h and dried in oven at
90 °C for 24 h [5]. The mixture is then subsequently hydraulically
pressed into cylinder mould (Ø 13 mm) at 10 MPa to form pellets. The
pressed samples were sintered in the hot-isostatic pressing (American
Isostatic Presses, INC HP630) at 1600 °C for 1 h soaking time under
150 MPa using Ar gas. The pressureless sintering was carried out to
perform a comparison between the two techniques of the same mate-
rials. The analysis of structure was carried out by X-ray diffraction
(XRD) using the Bruker D8 Advance with CuKa radiation (40 kV,
30 mA) diffracted beam monochromator, using a step scan mode with a
step size of 0.1° in the range of 20°–80° of 2ϴ°. Field emission scanning
electron microscopy (Carl Zeiss, Germany) was employed to study the
microstructure of the grinded and polished samples. Sample grinding
process was executed using Metkon 120, 240, 500, 800 and 1200 grit
61
International Journal of Refractory Metals & Hard Materials 69 (2017) 60–65
Fig. 1. Schematic diagram of typical radial crack
propagation for Vickers indentation fracture tough-
ness measurement: top view of Vickers indents with
corresponding crack and diagonal lengths; cross sec-
tion view of (a) the Palmqvist crack and (b) the
median crack.
alumina abrasive grade papers. The samples were polished by using
Imptech grinder polisher with 1 μm and 0.05 μm Al2O3 particle as
polishing medium. The density and porosity values were obtained ac-
cording to the ASTM C 830-00 test procedure. The Vickers hardness test
(Shimadzu HSV-20) was carried out to obtain both Vickers hardness
and fracture toughness values. Fracture toughness (KIc) was calculated
using Niihara's equation [28]. This equation is fundamentally derived
with a general and common assumption that normally governs the
crack formation in brittle materials with relatively low toughness
(considered to follow median mode), and for cracks with relatively high
toughness, it corresponded to Palmqvist mode. These crack modes can
be determined from the l/a ratio, which presumed to be indicative of
the type of crack system. Niihara [28] derived the proportionality for
Palmqvist crack length to be 0.25 ≤ l/a ≤ 2.5 and median crack
lengths to be 2.5 ≤ c/a ≤ 3.5, where a, l and c are shown in Fig. 1.
Both hardness and KIc can be determined by Vickers indentations. In
present work, 10 indentations per sample were performed under 30 kgf
for 10 s. Optical investigation using a built-in microscope of the hard-
ness machine was carried out to measure the crack length. The cracks
were measured based on the straight line method and have been
identified as Palmqvist cracks. Therefore, the KIc of the ZTA-CeO2
samples was calculated using Niihara's equation, which is valid for
Palmqvist cracks with an average of l/a ≤ 2.5. This equation is ac-
ceptable since the current study is only focused on the behavioural
trend of the fracture toughness when ZTA is added with various
amounts of CeO2. Therefore, the fracture toughness (KIc) was calculated
using dimensional analysis [28] as follows:
3KIc = 0.035(Ha1 2)(3E H)0.4 (l a)−0.5 (1)
where KIc is the fracture toughness, ‘H’ is Vickers hardness, ‘a’ is the half
length of Vickers diagonal (μm), ‘E’ is equal to the Young modulus of
the samples, and ‘l’ is the length of the radial crack size (μm).
3. Results and discussion
Fig. 2 shows the effects of various amount of CeO2 added to ZTA on
bulk density and porosity when fabricated by pressureless and HIP
routes, respectively. Fig. 2a shows the bulk density of hipped ZTA-CeO2
N.A. Rejab et al.
Fig. 2. Results of (a) bulk density and (b) percentage of porosity for ZTA as a function of CeO2.
ceramic sample, it increases from 4.24 g/cm3 (pure ZTA) to 4.28 g/cm3
(1.0 wt.% CeO2) while pressureless samples always recorded a lower
value. The bulk density is gradually increased until reaching the op-
timum value at 5 wt.% for both fabrication methods. However, the
porosity for all samples (Fig. 2b) shows an opposite trend of their bulk
density. Therefore, both bulk density and porosity of the samples are
greatly affected by the amount of CeO2 added and also the fabrication
method.
These observations can be confirmed from their microstructure
development when examined by FESEM as shown in Fig. 3. The
minimum porosity is from both sample added with 5 wt.% CeO2. It is
obvious that addition of CeO2 has induced the formation of elongated
grains. The corresponding EDX analysis for these elongated grains is
shown in Fig. 4 which consists of Ce, Al and O. This compound was
determined by XRD analysis as CeAl11O18 phase as shown in Fig. 5. The
higher amount of CeO2 addition resulted in the formation of more
elongated grains.
As the number is increased, the microstructure becomes less uni-
form, creating a greater ratio between the elongated and spherical
grains. Hence, the grains were unable to closely pack together and tend
to interlock each other [6], resulting in high percentage of porosity.
This also affected their density as clearly shown by 7.0 wt.% of CeO2
addition (Fig. 3j). However, the lowest porosity is shown by 5.0 wt.%
CeO2 addition which shows the most compact microstructure (Fig. 3i).
The superior effect of HIPping compared to pressureless sintering is due
to its ability to exert pressure uniformly throughout the sample and
hence, produced less porosity. Hence, the pores in the microstructure
can be reduced effectively leading to enhanced densification.
Fig. 5 shows the stacking of XRD analysis for ZTA samples mixed
with various amount of CeO2 (0 wt.% to 7.0 wt.%) for both HIPping and
pressureless techniques. For pressureless samples (Fig. 3a), only cor-
undum, Al2O3 (designated as “◊”) and zirconium yittria oxide,
Zr0.935Y0.065O1.968, YSZ (designated as “Δ”) were identified. Based on
our previous work, a secondary phase was detected with the addition of
≥ 10 wt.% of CeO2 which proved that the solubility limit was exceeded
compositionally [18]. Thus, maximum addition of 7 wt.% in the current
work is not exceeding solubility limits of ZTA-Ce composition. How-
ever, through HIPping process, the formation of secondary phase
(CeAl11O18) can be detected as early as at 3 wt.% CeO2 addition
(Fig. 4b). The peaks intensity of the CeAl11O18 in the ZTA-CeO2 ceramic
increased in proportion to the increase of CeO2 amount added. Con-
versely, the peaks intensity of the Al2O3 decreased proportionately with
the formation of CeAl11O18, while the peak intensity of YSZ remained
almost constant. CeO2 is very sensitive to the sintering atmosphere and
can form nonstoichiometric oxides such as Ce2O3 [29,30]. As a result,
CeO2 could be reduced to Ce2O3 and combine with Al2O3 during sin-
tering which resulted to the formation of CeAl11O18 phase [31].
Therefore, combination of high sintering temperature and pressure
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International Journal of Refractory Metals & Hard Materials 69 (2017) 60–65
during HIPping process accelerated the formation of CeAl11O18 phase.
Fig. 6 shows the consistent improvement of hardness and toughness
when ZTA was added to CeO2 when fabricated by hip compared to
pressureless sintering technique. Both hardness and toughness trends
show a gradual increase from 0 wt.% to 5 wt.% of CeO2 additions be-
fore decreasing with 7 wt.% addition. The ZTA samples produced
through HIPping shows a gradual increment in hardness from
1625.7 HV (0 wt.% CeO2) to 1838.3 HV (5.0 wt.% CeO2). Meanwhile,
the fracture toughness for those ZTA samples reveals a gradual en-
hancement from 6.66 MPa·√m (0 wt.% CeO2) to 8.92 MPa·√m (5.0 wt.%
CeO2) which was 25% increment compared to the pure ZTA.
The Vickers hardness behaviour basically follows the similar trend
of both bulk density and porosity percentage shown in Fig. 2. The ZTA
added with 5.0 wt.% CeO2 has the highest Vickers hardness among ZTA
ceramics (1838.3 HV) obtained from HIPping technique, while for the
pressureless gave 1688 HV [8]. The major contribution to the hardness
improvement came from the reduction of porosity in the micro-
structure. Porosity affects the hardness of ceramic materials in two
ways; firstly, it reduces the resistance of the microstructure against the
applied loads [32,33]. Second, pores act as the stress concentration
points; once the stress reaches a critical level, a crack is formed and
propagates throughout the structure [34,35]. Since the ceramics does
not show any plasticity, the fracture energy is not absorbed and it is
then transferred to ceramics. Once the crack is initiated, it propagates
until the fracture occurs [18,36,37]. In ceramic materials, a crack will
propagate spontaneously if the stress energy released is equal to or
more than the energy required propagating the crack surfaces [38].
Based on previous finding [18], pores (i.e., their size, shape, and
amount) reduce the strength of ceramics because they reduce the cross-
sectional areas over which a load can be applied and, consequently,
lower the stress that these materials can support. Therefore, the higher
the porosity, the lower the resistance to applied loads and easier for
cracks to propagate and distribute through the ceramics structure.
Nevertheless, further increment of CeO2 addition after 5.0 wt.%
causes the reduction of Vickers hardness. This is due to the presence of
higher amount of secondary phase (CeAl11O18) in the ZTA-CeO2
ceramic composite according to the FESEM micrographs and XRD
analysis (Fig. 3 and Fig. 5). Furthermore, the increase in elongated
grains' number causes the grains to unable to pack densely and thereby
reducing the hardness of the ceramics.
As regards the fracture toughness, HIPping techniques has positive
impact on the improvement of the fracture toughness of ZTA added
with CeO2 ceramics as compared to pressureless samples. The fracture
toughness of hipped ZTA-CeO2 ceramic also shows a gradually increase
(7.37%) at the beginning from 6.66 MPa·√m (0 wt.% CeO2) to
7.19 MPa·√m (1.0 wt.% CeO2) until the formation of elongated grains
(CeAl11O18 phase) due to the reaction between CeO2 and Al2O3.
Ultimately, the fracture toughness of hipped samples is increased to
N.A. Rejab et al. International Journal of Refractory Metals & Hard Materials 69 (2017) 60–65

Fig. 3. Microstructures of ZTA with (a) 0 wt.% CeO2,

(b) 1.0 wt.% CeO2, (c) 3.0 wt.% CeO2, (d) 5.0 wt.%
CeO2, and (e) 7.0 wt.% CeO2.

63
N.A. Rejab et al. International Journal of Refractory Metals & Hard Materials 69 (2017) 60–65

Fig. 4. Microstructure and EDX analysis of

the ZTA added with 7 wt.% CeO2.

about 25%; from 6.66 MPa·√m (1.0 wt.% CeO2) to 8.92 MPa·√m
(5.0 wt.% CeO2). According to Sha et al. [39], elongated grains in the
microstructure force a crack to deflect in more than one plane to get
around the grain. More energy is required to move through the elon-
gated grains compared to the energy needed to move through flat
platelets in the microstructure. Therefore, the fracture toughness are
correlated with the elongated grains.
However, further addition of CeO2 after 5.0 wt.% caused the frac-
ture toughness to decrease due to abundant number of porosity in the
microstructure. Furthermore, the relatively high number of elongated
grains has adverse effect on the fracture toughness [40]. The high
number of elongated grains caused the grains to interlock with each
other and packed randomly. As a result, there are more blunt crack tips
in the microstructure. These make it difficult for the elongated grains to
Fig. 6. Vickers hardness and fracture toughness for pressureless and HIP method on ZTA
force a crack to deflect in more than one plane to get around the grain
as a function of CeO2 wt.%.
[32]. The optimum values for both hardness and toughness were re-
corded for the sample with 5 wt.% addition fabricated by HIP tech-
nique, which produced 1838.3 HV and 8.92 MPa·√m, respectively. reduced the porosity of the samples and effectively increased its hard-
Therefore, application of HIP technique is a better approach to fabricate ness, while the fracture toughness was enhanced due to formation of
superior properties of ZTA-based ceramics. elongated grains of secondary phase (CeAl11O18). The presence of these
elongated grains contributed to higher fracture toughness, which cor-
responded to crack deflection propagation along grain boundaries. The
4. Conclusion
ceramics synthesis produced by HIP technique with 5 wt.% CeO2 ad-
dition produced the products with optimum hardness (1838.3 HV) and
Hot isostatic pressing (HIP) technique has significantly enhanced
toughness (8.92 MPa·√m).
both hardness and toughness of ZTA-CeO2 ceramics. This technique

Fig. 5. Stacking of XRD analysis for ZTA with different CeO2 composition (a) pressureless samples, and (b) hot isostatic pressing samples.

64
N.A. Rejab et al.
Acknowledgments
The authors are grateful to Mr. Zaini Saari (X-ray technician) for
conducting the X-ray diffraction machine and Mr. Khairi (SEM techni-
cian) for conducting the SEM machine testing required for this project.
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