Ceramics International 46 (2020) 20129–20137

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Ceramics International
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Microstructure and reactivity evolution of colloidal silica binder in different T

systems at elevated temperatures
Jiancheng Ana,b,1, Yuping Wanga,1, Quanli Jiaa, Fei Zhaoa,∗, Xinhong Liua,∗∗
a
Henan Key Laboratory of High Temperature Functional Ceramics, Zhengzhou University, 75Daxue Road, Zhengzhou, Henan, 450052, China
b
Tongda Refractory Technologies, Co. LTD, 1Anningzhuang East Road, Haidian District, Beijing, 100085, China

ARTICLE INFO ABSTRACT

Keywords: Colloidal silica as nanostructured binder for refractory castables has attracted many attentions in recent years. In
Colloidal silica the present study, phase composition, microstructure and reactivity evolution of silica gel at different heating
Phase composition conditions were investigated to find suitable system for colloidal silica application. The results showed that
Microstructure atmosphere and carbon slightly affected phase composition of the silica gel at elevated temperatures, and the
Reactivity
crystalline phases were composed of major α-cristobalite and minor α-tridymite. The morphology and particle
Particle size
size of the silica gel were greatly affected by atmosphere and carbon during heating. The spherical nano-silica
particles with sizes of 40–50 nm rapidly grew into macroscale rod-like particles with temperature increasing
from 800-1000 °C to above 1200 °C in air, and sintering of silica particles was observed. However, the size and
morphology of the spherical nano-silica particles retained at high temperature in a reducing atmosphere, and
many well developed columnar mullite crystals and some SiC whiskers formed on heating silica gel, alumina
fines and carbon at 1500 °C, which was due to carbon inclusions retarding the growth of nano-silica particles and
the nano silica remained high reactivity at high temperature. Thus, colloidal silica was suitable for application in
carbon-containing refractory castables.

1. Introduction castables in high temperature critical areas. In recent years, hydratable

Refractory castables are universally used in high-temperature in-
dustries because of their unique advantages, such as energy saving,
environment-friendly, high performance, easy installation, and cost
effectiveness [1,2]. Binding systems are closely related to the perfor-
mance and service life of refractory castables, and cement is a con-
ventional binder and has been used in refractory castables for a long
time, as it provides good installation property and cold strength for
castables. However, the low melting point phases (e.g., anorthite and
gehlenite) can form because of CaO in cement reacting with other
components (e.g., microsilica) in castables at high temperature, which
would degrade high temperature performance of the castables. CaO in
cement also easily reacts with Al2O3 in castables to form calcium dia-
luminate (CA2) and calcium hexaluminate (CA6) that cause volumetric
expansion and generate many cracks at high temperatures [3–7].
Therefore, cement as a binder usually generates detrimental compo-
nents in refractory castables at high temperature leading to the service
life decreasing, which limit the application of cement containing
alumina, colloidal silica, and colloidal alumina as new type binders
have been adopted and used in refractory castables [8–13]. Among
these binders, colloidal silica has attracted considerable attentions from
researchers, manufacturers, and consumers. Because colloidal silica has
a high solid content (~50 wt%), and the nano-sized SiO2 particles can
fill pores and gaps, increasing the densification of castables [14,15].
Moreover, incorporating colloidal silica leads to mullite phase forma-
tion at low temperature in alumina-rich castables [16].
However, the current researches about colloidal silica are focused
on its effects on the mixing behavior [17], rheological behavior [18],
setting mechanism [19], green mechanical properties [20,21], and
high-temperature properties of castables [9,22–24]. Less research has
been focused on phase composition, microstructure and reactivity
evolution of silica gel coming from colloidal silica in different systems
at elevated temperatures. Different phases of silica may confer different
properties to refractory castables, and the particle size of silica greatly
affects its reactivity and properties of the castables. Previous researches
have showed that nano oxide particles easily undergo abnormal growth

∗
Corresponding author.
∗∗
Corresponding author.
E-mail addresses: zhaofeiln@zzu.edu.cn (F. Zhao), liuxinhong@zzu.edu.cn (X. Liu).
1
The authors contributed equally to this work.

https://doi.org/10.1016/j.ceramint.2020.05.088
Received 21 March 2020; Received in revised form 26 April 2020; Accepted 7 May 2020
Available online 11 May 2020
0272-8842/ © 2020 Elsevier Ltd and Techna Group S.r.l. All rights reserved.
J. An, et al.
and partial sintering at high temperature in oxidizing atmosphere, and
that the particle size remains in the nanoscale at high temperatures in
the presence of carbon in a reducing atmosphere [25–27]. However,
some nanoparticles are not stable and easily decompose into other
phases in a reducing atmosphere. For example, nano ZnAl2O4 particles
decompose into α-Al2O3 and ZnO above 1000 °C in reducing atmo-
sphere, and ZnO further reacts with carbon to form Zn (g) discharging
from the samples [27]. If nano-silica particles grow into micro- or
macroscale particles at high temperature, their high reactivity and
filling effect would decrease, the promotion of sintering and mullite
formation at lower temperature may be impossible, and the cost-ef-
fectiveness of silica nanoparticles will be disappeared. If nano silica
particles transform into other substances, the properties of the castables
may also be greatly affected. However, there are no research reports on
changes in silica gel in different systems at elevated temperatures.
In addition, there are diversified research results on mullite for-
mation temperature in materials in presence of colloidal silica. Chen
et al. [28] prepared mullite precursor by mixing alumina powder and
silica sol, and the initial mullite formation temperature was 1250 °C.
J.Q. Xiong et al. [29] addressed that the introduced silica sol could
react with alumina to form mullite at about 1100 °C, leading to the
densification of materials. And mullite has high melting point, high
refractoriness, low expansion coefficient, which is beneficial phase in
refractory castables, mullite formation at lower temperature con-
tributes to improvement in high temperature properties of castables.
However, some studies showed that heating silica sol and alumina
could not produce mullite at low temperature. The research result of
Zhigang Li et al. [30] showed that mullite formed at 1547 °C by heating
mixture of silica gel and Al2O3 micropowders in air, i.e. mullite could
not form at low temperature. Therefore, in order to verify the tem-
perature of mullite formation, and tailor the microstructure and prop-
erties of castables using silica sol binder, the reactivity of silica gel with
alumina at high temperature should be studied.
Nowadays, carbon-free and carbon-containing castables are widely
used in practice. Therefore, in this study, the existing commercial col-
loidal silica was adopted, and the phase composition and micro-
structure evolution as well as the reactivity of silica gel with Al2O3 fines
in systems with and without carbon during heating were investigated.
The possibility of mullite formation at low temperature by heating a
mixture of silica gel and Al2O3 fines and the stability of the silica gel in
a reducing atmosphere were discussed. The suitable system for colloidal
silica application in refractory castables was also proposed.
2. Experimental procedure
Commercial colloidal silica (Shuanglian Chemical Co. Ltd, China;
solid content: 30 wt%) usually used in castables in China, carbon black
(N220, Tianjin Ebory Chemical Co. Ltd, China, C > 99 wt%,
20–30 nm) and tabular alumina fines (Almatis Co. Ltd, Al2O3 > 99 wt
%, 40 μm) were used as starting materials. Silica gel was prepared by
drying the colloidal silica at 110 °C for 24 h. XRD and morphology of
the dried silica gel were shown in Fig. 1(a) and (b), there was only one
broad peak around 22°, indicating that the silica gel was amorphous,
and the diameter of gel particles was in the range of 35–40 nm.
There were three groups of samples: (1) Dried silica gel powder was
fired at 800-1500 °C for 3 h in oxidizing atmosphere, this group was
designated as S0; (2) Dried gel and carbon black powders were fired at
800-1500 °C for 3 h in reducing atmosphere, this group was designated
as S1, and carbon was excess in the sagger and thus created a reducing
atmosphere (including CO and N2); (3) Silica gel powder was mixed
with tabular alumina fines (m(Al2O3): m(SiO2) = 3:2) and fired at
1400-1500 °C both in air and reducing atmosphere, this group was
designated as AS.
Differential thermal analysis and thermogravimetry (DTA-TG) of
silica gel were tested using a thermal analysis apparatus (Netzsch STA-
449C). Crystalline phases of the samples were determined by X-ray
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diffraction (XRD; Philips X′ Pert Pro). Microstructure of the samples was
characterized by scanning electron microscopy (SEM, JEOL JSM-
6500F) equipped with energy-dispersive spectroscopy (EDS).
3. Results and discussion
3.1. TG-DTA of silica gel powder
The TG-DTA curves of silica gel powder are shown in Fig. 2. The
endothermic peak at 55 °C with weight loss of 5.8% is due to free water
discharging. The exothermic peak at 980 °C with no obvious weight loss
is due to the crystallization of silica [31], which may suggest that silica
remains amorphous below 980 °C. Chen et al. [32] address that the
amorphous SiO2 is transformed into the crystalline phase from 800 °C.
Therefore, the heating temperature is selected as 800 °C to 1500 °C for
the following experiments to investigate the silica gel changes in dif-
ferent system at elevated temperature.
3.2. Phase evolution of silica gel powder in different atmosphere
XRD patterns of the samples after fired at 800-1500 °C in air are
shown in Fig. 3a, and the relative content of different phase in samples
is calculated by Rietveld refinement method and shown in Fig. 3b.
Fig. 3a indicates that the major α-cristobalite phase and minor α-
tridymite phase co-exist in S0 series samples after fired in air. The peaks
of α-tridymite are very weak after fired at 800 °C; the intensity of peaks
of α-tridymite slightly increases from 800 °C to 1000 °C, and notably
increases on increasing temperature from 1000 °C to 1200 °C. The in-
tensity of peaks of α-tridymite at 1200 °C is almost the same as that at
1500 °C. Fig. 3b demonstrates that the relative content of α-cristobalite
and α-tridymite is 85% and 15% at 800 °C, and the relative content of
α-tridymite increases up to 31% at 1200 °C, α-tridymite slightly in-
creases (33%) with further increasing temperature from 1200 °C to
1500 °C.
The XRD patterns and relative content of the samples after fired at
800-1500 °C in reducing atmosphere are shown in Fig. 4.
Fig. 4 shows that the major α-cristobalite phase and the minor α-
tridymite phase also co-exist in S1 series samples after fired in a re-
ducing atmosphere. On increasing temperature from 800 °C to 1000 °C,
the relative content of the α-tridymite notably increases (from 18% to
26%), and then slightly decreases (from 23% to 20%) with further in-
creasing temperature from 1200 °C to 1500 °C.
Figs. 3 and 4 indicate that the atmosphere and carbon inclusion
have a little effect on phase evolution of silica gel at elevated tem-
perature. The relative content of α-tridymite increases with tempera-
ture rise in air, but the relative content of α-tridymite increases firstly
and then decreases with temperature rise, and the relative content of α-
tridymite fired in air at 1200-1500 °C is more than that fired in reducing
atmosphere.
According to XRD results, the crystal size of silica is determined
using Scherrer formula (Eq. (1)).
D = 0.89λ/(B·cosθ) (1)
Where D is the average crystal size, λ is the wavelength
(λ = 0.15406 nm), θ is the Bragg angle, B is the full-width at half-
maximum of the peaks, and B is the corrected result using experimental
broadening by silicon peaks as reference. The calculated crystal size of
silica is shown in Table 1.
Table 1 indicates that the crystal size of silica is 35–40 nm after fired
at 800-1000 °C in air, and the crystal size significantly increases with
temperature up to 1200 °C (> 100 nm). However, the crystal size of
silica is almost no change in reducing atmosphere with carbon inclu-
sions when the firing temperature increases from 800 °C to 1500 °C, and
the crystal size of silica is in nanoscale (40-47 nm), demonstrating that
carbon can hinder the crystal growth of silica in reducing atmosphere.
J. An, et al.
Fig. 1. (a) XRD pattern; (b) morphology of silica gel.
Fig. 2. TG-DTA curves of silica gel powder.
3.3. Microstructure evolution of silica gel in different atmosphere
Fig. 5 shows the microstructure of the samples fired at 800-1500 °C
in air, indicating that the size of the spherical nano-silica particles is
less than 60 nm after fired at 800-1000 °C. With temperature increasing
up to 1200 °C, the silica particle size significantly increases, growing
into micro-sized particles, and sintering of the particles is observed
(Fig. 5c). With the temperature further increasing up to 1500 °C, the
silica particles grow into macroscale, and particles have sintered and
closely bound to each other (as shown in Fig. 5d). This suggests that the
growth of the nanoscale silica particles has closely related to the fired
temperature in oxidizing atmosphere. The high reactivity and excellent
Fig. 3. XRD patterns (a) and relative content (b) of sample S0 fired at elevated temperature in air.
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properties of the nanoscale silica particles are lost when they abnor-
mally grow into micro- or macroscale at high temperature.
SEM images of the S1 series samples after fired at 800-1500 °C are
shown in Fig. 6. The size of the nano-silica particles is 40–50 nm and
remains almost unchanged with the temperature increasing up to
1500 °C. Further, the spherical morphology of the nano-silica particles
has no change with temperature rise from 800 °C to 1500 °C, indicating
that the carbon can inhibit the nano-silica particles growing, thus re-
taining their fine size and spherical shape at high temperatures. The
spherical shape of the nanoscale silica particles will lead to good filling
effect and high reactivity, which contribute to increase in density and
the formation of mullite at low temperature [33] and improvement in
high temperature properties of refractory castables.
The above results illustrate that carbon black has a crucial effect on
retarding the growth of nanoscale silica particles at high temperature.
In order to illustrate the role and distribution of carbon black in the
samples, EDS analysis is selectively checked on sample S1 after fired at
1000 °C (Fig. 7). The EDS maps reveal that the sample contains Si, O
and C. Carbon is well distributed along the particle boundaries of the
nano-silica particles, which restricts the growth and sintering of these
nanoparticles.
In air, silica particles directly contact with each other, resulting in
agglomeration at low temperature, and on increasing the temperature,
the particles tend to grow and sinter. In a reducing atmosphere, carbon
black is around the boundaries of nanoscale silica particles, creating a
steric hindrance effect, leading to separating each other of different
particles, and a schematic of the effect of carbon is shown in Fig. 8.
3.4. Reactivity of silica gel powder with alumina fines
There are diverse opinions about mullite formation in the presence
of colloidal silica at low temperature in alumina rich castables.
J. An, et al. Ceramics International 46 (2020) 20129–20137

Fig. 4. XRD patterns (a) and relative content (b) of sample S1 fired at elevated temperatures in reducing atmosphere.

Table 1 The relative content of different phase in samples fired at 1500 °C

Crystal size (nm) of silica. (Fig. 9c) indicating that more silica particles have reacted with alumina
Samples 800 °C 1000 °C 1200 °C 1500 °C
to form more mullite (30%) in reducing atmosphere than that in air
(22%).
S0 35 40 > 100 - Fig. 5 indicated that nanoscale silica particles grew into micro- or
S1 40 45 47 45 macroscale particles after heating above 1200 °C and their reactivity
degraded; however, size of silica particles is in nanoscale at 800-
1500 °C (Fig. 6), therefore, more mullite can form at 1500 °C due to the
Therefore, to investigate the possibility of mullite phase forms at rela-
high reactivity of nanoscale silica particles. Though nano silica particles
tively low temperatures in the presence of silica sol, a mixture of the
are in nanoscale at 1400 °C in reducing atmosphere, and mullite dif-
dried silica gel powder and tabular alumina fines (m (Al2O3): m
fraction peaks are not observed after fired at 1400 °C (Fig. 9a), in-
(SiO2) = 3:2) has been fired at 1400-1500 °C for 3 h both in air and in
dicating that mullite can not form in presence of colloidal silica at low
reducing atmosphere.
temperature (≤1400 °C) in high purity system.
Fig. 9a shows the XRD results of samples after fired at 1400 °C, and
Fig. 10 indicates that the SEM image and EDS results of sample AS
the crystalline phases include corundum and cristobalite, no mullite
after fired at 1400 °C in air. Fig. 10 illustrates that silica and alumina
crystal phase is observed in samples fired both in air and in reducing
particles are present in the AS sample, further confirming the absence of
atmosphere. Fig. 9b shows that mullite phase generates in samples fired
mullite at 1400 °C, and the result is in accordance with XRD result in
in both atmospheres at 1500 °C, the intensity of mullite peaks in sample
Fig. 9a.
fired in reducing atmosphere is a little stronger than those fired in air.
The SEM image and EDS result of AS sample fired at 1500 °C in air

Fig. 5. Microstructure of S0 sample after fired in air: (a) 800 °C, (b) 1000 °C, (c) 1200 °C, and (d) 1500 °C.

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Fig. 6. Microstructure of S1 sample after fired in reducing atmosphere: (a) 800 °C, (b) 1000 °C, (c) 1200 °C, and (d) 1500 °C.

are shown in Fig. 11 (a) and (b). Fig. 11a and b indicate that some
needle-like mullite crystals form in sample after fired at 1500 °C in air,
and the mullite crystals are fine, develop not good enough. The sin-
tering phenomenon of sample is observed from Fig. 11a, and it is dif-
ficult to find nanosilica particles.
Fig. 12 (a)-(b) show the SEM image and EDS result of sample AS
fired at 1500 °C in reducing atmosphere.
Fig. 12 (a) and (b) demonstrate that many well developed columnar
mullite crystals in sample fired in reducing atmosphere at 1500 °C, and
the mullite crystals are easily found by SEM observation. And many
nanoscale silica particles are also observed, and the particle size of nano
silica is about 50 nm, the silica particles have small size and high re-
activity, which are benefit for the further application in refractory ca-
stables.
The above results indicate that the atmosphere has great effect on
the formation mechanism of mullite at high temperature. Because the
system is relatively high purity in this study, the mullite formation is via
solid-state reactions in air, as follows.
3Al2O3(s) +2SiO2(s) = 3Al2O3.2SiO2(s) (2)
The rate of mullite formation is controlled by solid diffusion, and
the solid diffusion rate is relatively low, the mullite formation and
growth rate is low, thus the mullite crystals are not well developed at
1500 °C in air. Therefore, the morphology of mullite is tiny needle-like.
However, in reducing atmosphere, the highly reactive nano silica
will react with carbon to form SiO(g), SiO(g) reacts with Al2O3 to form
mullite nuclei. Because the SiO(g) is continuously provided at high
temperature, leading to mullite nuclei growing into well-developed
columnar-like. Mullite growth is controlled by vapor-solid mechanism,
which is agreement with reference [34].

Fig. 7. EDS maps of Si, O, and C elements of sample S1 after fired at 1000 °C.

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Fig. 8. Schematic of steric hindrance effect of carbon.
Moreover, many whiskers are observed on surface of the sample
S1fired at 1500 °C in the reducing atmosphere. The microstructure, EDS
and XRD of the whiskers are shown in Fig. 13 (a)-(d).
The EDS result in Fig.13(c) and XRD of Fig.13(d) indicate that these
whiskers are SiC, and the SiC whiskers have a chain-bead structure
(Fig. 13(a)-(b)), with O element present in the bead. The obtained SiC
whiskers are several tens of microns in length and several hundreds
nanometer in diameters. In presence of carbon, nanoscale silica parti-
cles react with C to form SiO (g) and CO (g), and SiO (g) further reacts
with C or CO (g) to form SiC whiskers and SiO2 [35]. According to
literature [36], the in-situ formed SiC whiskers exhibited good
Fig. 9. XRD patterns of AS samples after fired at 1400 °C (a) and 1500 °C (b); relative content of samples fired at 1500 °C (c).
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strengthening and toughening effects, thus would improve the me-
chanical properties of refractory materials. Therefore, colloidal silica is
suitable for carbon containing refractory castables.
4. Conclusions
The phase composition, microstructure and reactivity evolution of
silica gel in different systems at elevated temperature were in-
vestigated. The results showed that carbon and atmosphere slightly
affected phase composition of silica gel during heating. The crystalline
phases included the major α-cristobalite phase and minor α-tridymite
phase. Carbon and atmosphere greatly affected the morphology and
particle size of the silica gel during heating. The spherical nano-silica
particles rapidly grew into micro- or macroscale rod-like particles with
temperature increasing from 800-1000 °C to above 1200 °C in air, and
the particles sintered with each other. However, the particle size of
spherical nano-silica with high reactivity was almost unchanged on
heating a mixture of silica gel and carbon in a reducing atmosphere at
high temperature, and many well developed columnar mullite crystals
and SiC whiskers formed on heating the silica gel powder, alumina fines
and carbon black at 1500 °C, which was due to carbon inclusions re-
tarding the growth of nanoscale silica particles and nano silica re-
mained high reactivity, thus making colloidal silica suitable for appli-
cation in carbon-containing refractory castables.
Declaration of competing interest
The authors declare that they have no known competing financial
interests or personal relationships that could have appeared to influ-
ence the work reported in this paper.
J. An, et al. Ceramics International 46 (2020) 20129–20137

Fig. 10. SEM image (a) and EDS results (b, c) of AS sample after fired at 1400 °C.

Fig. 11. Microstructure (a) and EDS result (b) of AS sample fired at 1500 °C in air.

Fig. 12. Microstructure (a) and EDS result (b) of AS sample fired at 1500 °C in reducing atmosphere.

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Fig. 13. Microstructure and EDS result of S1 sample after fired at 1500 °C in reducing atmosphere.
Acknowledgements
The work was financially supported by the National Natural Science
Foundation of China (51672253, 51872266).
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