CLAY-03924; No of Pages 8

Applied Clay Science xxx (2016) xxx–xxx

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Applied Clay Science

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In situ high temperature X-ray diffraction study on high strength

aluminous porcelain insulator with the Al2O3-SiO2-K2O-Na2O system
Yong Meng a,b, Guohong Gong a,⁎, Dongtian Wei a,b, Yumin Xie c
a
State Key Laboratory of Ore Deposit Geochemistry, Institute of Geochemistry, Chinese Academy of Sciences, Guiyang 550002, Guizhou, China
b
University of Chinese Academy of Sciences, Beijing 100049, China
c
Bijie Highland Porcelain Insulator Limited Liability Company, Bijie 551700, Guizhou, China

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

Article history: The high strength aluminous porcelain insulator with a mineral composition of kaolinite, corundum, microcline,
Received 27 February 2016 quartz, small amounts of albite and anatase was investigated by in situ high temperature XRD (HTXRD) from
Received in revised form 16 July 2016 25 °C to 1300 °C. The amount change and reaction of minerals contained in the porcelain insulator were present-
Accepted 16 July 2016
ed vividly. The full process occurred in successive stages: 1) kaolinite decomposed into amorphous metakaolinite
Available online xxxx
in the temperature range of 500–600 °C; 2) metakaolinite kept amorphous form up to about 1000 °C; 3) at about
Keywords:
1000 °C, amorphous metakaolinite generated primary mullite; 4) after bout 1200 °C, microcline began to melt,
In situ high temperature forming an alkaline liquid phase which facilitated the growth of primary mullite into secondary mullite; 5) the
XRD alkaline liquid phase could etch β-quartz, resulting in the reflection intensity of β-quartz decreasing; 6) corun-
Porcelain insulator dum was very stable in the whole heating process.
Mineral © 2016 Published by Elsevier B.V.
Reaction

1. Introduction
Kaolin, composed mainly by aluminosilicate, is an essential raw ma-
terial in the ceramic industry (De Aza et al., 2014; Dondi et al., 2014). It
has diverse applications such as sanitary ware, building ceramics, re-
fractory ceramics and porcelain insulator (Lee et al., 2008; Ngun et al.,
2011; De Aza et al., 2014). Among the applications mentioned, porcelain
insulator possesses the highest mechanical strength, and its manufac-
ture process is complicated (Liebermann, 2003). Porcelain insulators,
before put into application, need to pass about 20 standard property
tests (e.g. electromechanical failure load test, flash test and power fre-
quency sparking test), which are strict to guarantee safety.
Insulators, as indispensible elements, are widely used on power
transmission and distribution network. They have two major functions:
fastening mechanically and insulating electrically the active compo-
nents of electric network (Liebermann and Schulle, 2002). As an eligible
insulator, it is required to possess the properties such as high resistivity,
high dielectric strength, low loss factor, superior mechanical strength,
excellent in radiating heat and insulating components even in humid
and corrosive condition (Liebermann, 2002; Amigó et al., 2005; Piva
et al., 2013). According to the material composition, insulators could
be divided into three main kinds of insulators, namely porcelain insula-
tor, composite insulator and glass insulator.
⁎ Corresponding author.
E-mail address: gongguohong@vip.gyig.ac.cn (G. Gong).
Porcelain insulator, having been put into application more than
160 years since 1850 when insulators were introduced in the construc-
tion of power network by Werner Von Siemens (Liebermann, 2003;
Islam, 2004; Meng et al., 2012; Meng et al., 2014), is most widely used
among the three kinds of insulators. Porcelain insulator possesses sever-
al outstanding properties simultaneously (i.e. high mechanical strength,
high resistance and corrosive resistance), which could not be realized by
other materials (Meng et al., 2012; Meng et al., 2014). Even so, the glass
insulator also occupies a significant market share and is widely accepted
by many countries and areas in recent years.
The properties of insulator are closely related to a few major factors:
the constituent phases resulting from high temperature reaction involv-
ing the raw materials used; the microstructure of the body; the degree
of densification and the sintering process (Liebermann, 2003).
Although the sintering process of porcelain insulator has been stud-
ied for a long time in the porcelain insulator industry, there still remain
some details which are interesting but not well presented or under-
stood for the restriction of experimental equipment and method. It is
still meaningful to investigate the sintering process of porcelain
insulator.
The aim of this work is to present the high temperature behavior of
minerals contained in the porcelain body as well as reactions happened
between different minerals by in situ high temperature x-ray diffraction
(HTXRD) vividly. The in situ HTXRD is a significant technology to inves-
tigate reaction and phase conversion upon high temperature. It makes
that available to monitor the short-lived phase during heating. Particu-
larly, we want to detail the decomposition of kaolinite to metakaolinite,

http://dx.doi.org/10.1016/j.clay.2016.07.014
0169-1317/© 2016 Published by Elsevier B.V.

Please cite this article as: Meng, Y., et al., In situ high temperature X-ray diffraction study on high strength aluminous porcelain insulator with the
Al2O3-SiO2-K2O-Na2O syste..., Appl. Clay Sci. (2016), http://dx.doi.org/10.1016/j.clay.2016.07.014
2 Y. Meng et al. / Applied Clay Science xxx (2016) xxx–xxx
the crystallization of mullite from amorphous metakaolinite and the
growth of secondary mullite from kaolinite relics with the isolines 3D
view function of XRD analytical software HighScore. It is really an inter-
esting method that can give readers a visualized sight about both phase
composition at each temperature and the variation tendency of reflec-
tion intensity with temperature smoothly (i.e. each phase's amount var-
iation trend). As for the HTXRD isolines 3D view, it is a three
dimensional surface image. Three axes of the image correspond to in-
tensity, 2theta and temperature or time, respectively.
2. Experiment and methodology
2.1. Specimens
Industrial raw materials taken from Bijie Highland Porcelain Insula-
tor Company (Guizhou province, China) were used. Specimens with dif-
ferent mineral composition were prepared. Specimen 1 is the green
body of 420 kN-level high strength porcelain insulator taken from
Bijie Highland Porcelain Insulator Company. This formula has been put
into industrial application successfully and is of high mechanical prop-
erty. The mineral composition of specimen 1 determined by XRD analy-
sis is: kaolinite, corundum, microcline, quartz and small amounts of
albite and anatase. The chemical composition of specimen 1 is shown
in Table 1. Specimen 2 is natural kaolin exploited from Mijiaping (Gui-
zhou province, China) by Bijie Highland Porcelain Insulator Company.
It is mainly composed of kaolinite and small amounts of quartz and an-
atase. Specimen 2 was used as one of the raw materials of specimen 1.
The chemical composition of specimen 2 is shown in Table 1.
2.2. HTXRD experiment
The HTXRD data was collected on a Panalytical multifunction X-ray
diffractometer (model: Empyrean), equipped with an Anton Paar high
temperature accessory (APHTK-16N) and a 3D PIXcel detector. The
heating process was divided into many continuous parts from ambient
temperature to 1300 °C. The heating speed was 20 °C per minute. The
diffraction patterns were recorded every 50 °C or 100 °C and at temper-
ature points interested. About 26 XRD patterns were recorded for each
sample. The total firing time in the Anton Paar chamber was about
300 min.
The measurement was done according to the following steps. Firstly,
specimens were crushed and finely ground with a pestle in an agate
mortar. Secondly, the ground powder was blended with some water
and stirred so that it could form an suspension. Thirdly, the suspension
of specimen was spread on a rectangle platinum film to form a uniform
layer with a size of 2 cm (length) × 1 cm (width) × 0.01 cm (thickness).
Fourthly, the platinum holder was put in the Anton Paar high tempera-
ture accessory. Finally, one could start the measure process.
The HTXRD measurements were performed at diverse temperature
points (ambient pressure), in the 2θ range of 5–65°, in the mode of con-
tinuous scanning with 0.013°in step size and a counting time of 25 s per
step. Working voltage and current were 40 kV and 40 mA, respectively.
Before collecting diffraction pattern at each given temperature point,
the temperature was kept for a few minutes to ensure temperature
uniformity.
Table 1
Chemical compositions (mass%) of specimens.
Al2O3 SiO2 K2O TiO2
Specimen 1 45.30 45.10 2.85 1.75
Specimen 2 38.22 45.92 0.21 1.55
Please cite this article as: Meng, Y., et al., In situ high temperature X-ray diffraction study on high strength aluminous porcelain insulator with the
Al2O3-SiO2-K2O-Na2O syste..., Appl. Clay Sci. (2016), http://dx.doi.org/10.1016/j.clay.2016.07.014
2.3. Scanning electron microscopy observation (SEM)
The specimens undergoing HTXRD analysis were scraped from plat-
inum film. Then the specimens were etched with a 10% (volume) HF so-
lution for 60 s and dried later. Finally the specimens were coated with a
carbon layer for crystal phase observation. The experiments were done
on a scanning electron microscope (model: JSM-6490LV, Japan).
2.4. DSC-TG experiment
The DSC-TG experiment was done on a TG-DTA analyzer (model:
NETZSCH STA 449F3) in the temperature range of 40–1200 °C with a
heating rate of 20 °C per minute (air atmosphere).
2.5. Transmission electron microscope (TEM) observation
The specimens undergoing HTXRD analysis were scraped from plat-
inum film for TEM observation. The experiment was done on a trans-
mission electron microscope (model: TecnaiG2F20S-TWIN TMP).
3. Results and discussion
3.1. Decomposition of kaolinite
The HTXRD isolines 3D view of specimen 1 and specimen 2 are pre-
sented in Fig. 1. It shows that all minerals remained stable when heating
from ambient temperature to 500 °C. The water absorbed was vented
out which was shown on the HDXRD patterns by the decreasing of
background intensity.
The reflection intensity of kaolinite remained the same almost be-
fore 500 °C, which means that kaolinite did not decompose in this tem-
perature range. The 001 and 002 reflections are strong reflections of
kaolinite. In the temperature range of 500–600 °C, the intensity of 001
and 002 reflections sharply decreased as a result of kaolinite
decomposing into metakaolinite with the reaction (Brindley and
Nakahira, 1958; Chakraborty and Ghosh, 1978; Chakraborty, 2003;
Chen et al., 2000; Ptáček et al., 2012; Teklay et al., 2015):
Al2O3·2SiO2·2H2O (kaolinite) → Al2O3·2SiO2 (metakaolinite) + 2H2O
(gas), which was testified by an endothermal peak on the DSC curve
and a mass reducing slope on the TG curve (Fig. 2). The gaseous water
molecular (H2O) could easily leave the reaction interface, i.e., the inter-
val between the silica tetrahedron sheet and the alumina octahedron
sheet in the crystal of kaolinite, which could facilitated the equilibrium
of the reaction moving to the right. After 600 °C, the intensity of back-
ground increased which was shown by the changing of background
color (Fig. 1). The cause may be metakaolinite is an amorphous phase
but it retained some of structure characteristics of kaolinite. So it is
short-range ordered to some extent. The results were also correspond-
ing with the study of De Aza et al. on kaolinite by time-resolved powder
neutron diffraction (De Aza et al., 2014), in which, activation energies of
kaolinite decomposition, mullite nucleation and growth were
calculated.
Kulbicki and Grim (Kulbicki and Grim, 1959; Grim and Kulbicki,
1961; Wahl and Grim, 2012) first studied the phase transformation of
clay minerals such as kaolinite and montmorillonite with the in situ
high temperature XRD method. The decomposition temperature inter-
val of kaolinite observed by them was corresponding with our result,
Fe2O3 Na2O CaO MgO Ablation ratio
0.81 0.74 0.43 0.35 3.5
0.53 0.75 0.21 0.25 12.38
 Y. Meng et al. / Applied Clay Science xxx (2016) xxx–xxx 3

Fig. 1. HTXRD isolines 3D view of specimens, a: specimen 1; b: specimen 2; c: top view of b; K: kaolinite; Q: quartz; C: corundum; M: microcline; Pt: platinum.

but the results presented by them were not visualized and vivid as that
in this paper.
3.2. Quartz decrease
Quartz is one of the essential materials of porcelain glaze, but it has
negative effects on the porcelain body (Liebermann, 2001; Chmelík
et al., 2011). It is usually contained in raw material kaolin. The 011 re-
flection is the strongest reflection of quartz. Its intensity, had a jump be-
tween 600 °C and 700 °C, and then remained the same until 1200 °C.
After about 1200 °C, it began to decrease (Fig. 3). This indicated that
the amount of quartz decreased to some extent. The decrease was not
caused by the melting of quartz for the melting temperature of quartz
is 1750 °C which is far higher than the sintering temperature of porce-
lain insulator. At the same time, the 002 reflection of microcline,
which is the strongest among all reflections of microcline, d0ecreased
in intensity after about 1200 °C. The two minerals showed the same de-
creasing tendency. This was caused by the melting of microcline be-
cause its melting temperature is about 1150 °C. Then a melt was
formed after 1200 °C. Quartz has a structure of silica tetrahedrons
connecting each other with four oxygen ions in three dimensions. Silica
tetrahedron is network former. K2O, contained in microcline melt, is

Please cite this article as: Meng, Y., et al., In situ high temperature X-ray diffraction study on high strength aluminous porcelain insulator with the
Al2O3-SiO2-K2O-Na2O syste..., Appl. Clay Sci. (2016), http://dx.doi.org/10.1016/j.clay.2016.07.014
4 Y. Meng et al. / Applied Clay Science xxx (2016) xxx–xxx

Fig. 2. DSC and TG curve of specimen 2.

network changer. The K\\O bond is weaker than Si\\O bond, so the Si4+
ion in silica tetrahedrons could attract the free O2– around. Besides, the
K+ could also weaken the Si\\O bond by attracting the O2– connecting
two adjacent silica tetrahedrons. As a result, Si-O-Si bonds of silica tetra-
hedrons are weakened, and then quartz is decomposed into small
groups of silica tetrahedron. This may be the reason of that the 011 re-
flection of quartz began to decrease after about 1200 °C.
3.3. Microcline melting
Microcline is one of the feldspars used in the ceramic industry. In
specimen 1, microcline was added as an essential mineral. In the
temperature interval of 25 °C ~ 1200 °C, the intensity of 002 reflection
of microcline remained the same. After bout 1200 °C, the 002 reflection
began to decrease in intensity. This indicated that microcline started to
melt. An alkaline liquid phase was formed. The K+ and Na+ ions in the
liquid phase could lower the viscosity of liquid phase and the sintering
temperature of porcelain body. The alkaline liquid phase facilitated pri-
mary mullite growing into secondary mullite and promoted the densifi-
cation of porcelain body. The alkaline liquid phase could etch β-quartz,
which caused the reflection intensity β-quartz decreasing. However, al-
kaline liquid phase cannot etch corundum proved by the reflection in-
tensity of corundum remaining the same during the whole heating
process.

Fig. 3. Isolines 3D view of specimen 1 in the angle range from 24° to 29°; Q: quartz; M: microcline.

Please cite this article as: Meng, Y., et al., In situ high temperature X-ray diffraction study on high strength aluminous porcelain insulator with the
Al2O3-SiO2-K2O-Na2O syste..., Appl. Clay Sci. (2016), http://dx.doi.org/10.1016/j.clay.2016.07.014
 Y. Meng et al. / Applied Clay Science xxx (2016) xxx–xxx 5

Fig. 4. a: Isolines 3D view of specimen 1 in the angle range from 33° to 45°; b: top view of a; C: corundum.

3.4. Stability of corundum
Corundum, added into the formula of porcelain insulator to improve
its mechanical property, served as strengthening phase in the porcelain
body. The 104 and 113 reflections are strong reflections of corundum.
Their intensities almost remained the same during the whole heating
process, which means that the amount of corundum did not change
(Fig. 4). All reflections of corundum shifted to low angle lineally when
temperature rising from 25 °C to 1300 °C. This indicated that the unit
cell volume of corundum was expanding according to the Bragg formu-
la: 2dsinθ = nλ. No phase change on corundum was observed in the
whole temperature range. This demonstrated that corundum was very
stable during the sintering process of porcelain insulator.
3.5. Mullite formation
Kaolinite, after 600 °C, almost decomposed into metakaolinite
completely. Although metakaolinite still kept some structure character-
istics of kaolinite, the structural hydroxyl has been removed.
Metakaolinite is an amorphous phase which has no reflection in XRD
pattern (Fig. 1). In the temperature range of 600–1000 °C, there was
no new phase occurring. At bout 1004 °C, an exothermic peak appeared
on the DSC curve (Fig. 2). According to the study of peers
(Martín-Márquez et al., 2010; Ptáček et al., 2011), this peak
corresponded to the nucleation of primary mullite with the reaction:
3(Al2O3·2SiO2) (metakaolinite) → 3Al2O3·2SiO2 (primary
mullite) + 4SiO2 (amorphous). After about 1100 °C, a series of reflec-
tions appeared in the HTXRD patterns of specimens 1 and 2 at about
16.5°, 33.3°and 40.6°, which corresponded to the 110, 220 and 121 re-
flections of mullite (Fig. 5). The intensities of the reflections mentioned
above increased with temperature (Fig. 5). All the reflections of mullite
were very small. The cause may be the new formed mullite crystallite
did not crystallize well and usually contained some defects such as lat-
tice hole and dislocation. Other cause may be the amount of mullite
formed was small.
Mullite could be divided into two main types: primary mullite and
secondary mullite (Lee and Iqbal, 2001; Martín-Márquez et al., 2010;
Montoya et al., 2010; Marinoni et al., 2011). Primary mullite is cubic-
like, while secondary mullite is needle-like and interlocking. Primary
mullite could grow into secondary mullite if there exists a liquid
phase. Both mullites favor the mechanical property promotion of porce-
lain especially secondary mullite because they could serve as strength-
ening phase of porcelain body.
In specimens 1, in which feldspar was added, mullite was observed
by XRD and SEM (Fig. 6). The secondary mullite formed in specimen 1

Please cite this article as: Meng, Y., et al., In situ high temperature X-ray diffraction study on high strength aluminous porcelain insulator with the
Al2O3-SiO2-K2O-Na2O syste..., Appl. Clay Sci. (2016), http://dx.doi.org/10.1016/j.clay.2016.07.014
6 Y. Meng et al. / Applied Clay Science xxx (2016) xxx–xxx

Fig. 5. Reflections of mullite formed in specimens 1 and 2; a, b and c are the 220, 110 and 121 reflections of mullite in specimen 1, respectively; e, f and g are the 220, 110 and 121 reflections
of mullite in specimen 2, respectively; Mu: mullite.

is needle-like with a few μm in length. Its length is shorter than the
value expected according to our experience. The cause may be the
time keeping in high temperature was not enough.
In specimen 2, which only contained kaolinite and small amounts of
quartz and anatase without feldspar, mullite was hardly observed by
SEM (Fig. 6), although there were reflections of mullite in its HTXRD
patterns after about 1100 °C. In order to observe the form of mullite in
specimen 2, TEM experiment was done on specimen 2 after the in site
HTXRD measurement. It was definite that the mullite formed in speci-
men 2 was primary mullite, which sporadically distributed in the matrix
of metakaolinite (Fig. 7). The primary mullite was cubic-like with about
20 nm in length. This was the cause why it could not be observed by
SEM. The area around the primary mullite was disordered, which was
the so-called metakaolinite.
From the result and discussion above we could reach the conclusion
that a feldspar melt is of great importance on the growth of primary
mullite into secondary mullite. Besides, the result also proves the
viewpoint of Lee et al. (Lee and Iqbal, 2001) that in a kaolinite-based
system, the mullite formed without an alkaline liquid phase should be
primary mullite, while the mullite formed with an alkaline liquid
phase should be secondary mullite.
4. Conclusion
The HTXRD is a useful method which allowed the visualization of
changes in lattice spacing and amount of crystalline constitutive phases.
The 420 kN-level high strength aluminous porcelain insulator with the
Al2O3-SiO2-K2O-Na2O system was investigated by in situ HTXRD from
25 °C to 1300 °C. The behaviors of minerals contained in the specimens
such as kaolinite, quartz, corundum and mullite during the sintering
process were detailed. A few results were achieved as follows:
a) Kaolinite sharply decomposed into metakaolinite during the tem-
perature range of 500–600 °C. Metakaolinite is an amorphous

Please cite this article as: Meng, Y., et al., In situ high temperature X-ray diffraction study on high strength aluminous porcelain insulator with the
Al2O3-SiO2-K2O-Na2O syste..., Appl. Clay Sci. (2016), http://dx.doi.org/10.1016/j.clay.2016.07.014
 Y. Meng et al. / Applied Clay Science xxx (2016) xxx–xxx
phase which had no reflection in HTXRD patterns in the temperature
range of 600–1000 °C.
b) At about 1000 °C, Metakaolinite grew into primary mullite which
was cubic-like with a length of about 20 nm.
c) Microcline melted after bout 1200 °C, and formed a alkaline liquid
phase which facilitated the primary mullite growing into secondary
mullite. The alkaline liquid phase could etch β-quartz resulting in
the reflection intensity decrease of β-quartz.
d) Corundum was very stable during the whole heating process.
Fig. 6. SEM micrograph of specimens 1 and 2; a&b: mullite in specimen 1; c: specimen 2; P:
primary mullite; S: secondary mullite.
Please cite this article as: Meng, Y., et al., In situ high temperature X-ray diffraction study on high strength aluminous porcelain insulator with the
Al2O3-SiO2-K2O-Na2O syste..., Appl. Clay Sci. (2016), http://dx.doi.org/10.1016/j.clay.2016.07.014
7
Fig. 7. TEM micrograph of specimens 2, P:primary mullite; M: metakaolinite.
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Please cite this article as: Meng, Y., et al., In situ high temperature X-ray diffraction study on high strength aluminous porcelain insulator with the
Al2O3-SiO2-K2O-Na2O syste..., Appl. Clay Sci. (2016), http://dx.doi.org/10.1016/j.clay.2016.07.014