Materials Chemistry and Physics 255 (2020) 123611

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Materials Chemistry and Physics

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

Preparation, properties characterization and structure formation

mechanism of silica sand tailings-based ceramic materials
Jiashuo Zhang a, 1, Taoyong Liu a, 1, Qianxing Huang a, Zhiwei Luo a, Anxian Lu a, *, Ligang Zhu b, **
a
School of Materials Science and Engineering, Central South University, Changsha, 410083, PR China
b
Guangxi Key Laboratory of Agricultural Resources Chemistry and Biotechnology, College of Chemistry and Food Science, Yulin Normal University, Yulin, Guangxi,
537000, PR China

H I G H L I G H T S

• Waste-based ceramic tile and ceramic foam were prepared without using agent.
• The composition of glass phase formed in ceramic material was discussed.
• The internal structure formed in prepared ceramic materials was analyzed.
• The property of material can be adjusted based on the chemical composition of waste.

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

Keywords: The preparation of high-performance ceramics using industrial waste as raw materials is an important direction
Full waste-based ceramic in the comprehensive utilization of waste residue. In this paper, we used silica sand tailings and other industrial
Microstructure waste as raw materials to prepare two types of full waste-based ceramic materials without additional agent. The
Pore morphology
results showed that different waste ratios caused the variation in content and composition of glassy phase formed
Glass phase composition
in the full waste-based material, leading to the formation of internal structure in different ceramic materials.
Sintering mechanism
Especially, the composition of glassy phase formed in ceramic foams was transferred from Ca–Al–Si–O to Al–Si–O
glass system, resulting in the difference in pore structure and performance. This work provides a way to design
the composition and control the properties of materials by using coupling reactions between chemical compo­
nents during the material preparation, achieving high value, high efficiency and safe use of waste resources.

1. Introduction
In recent years, considerable efforts have been devoted to developing
waste-to-energy (WTE) technologies that can reduce the volume of
waste and mitigate its negative effects on the environment [1]. The main
treatment methods for industrial solid waste are as follows: metal
extraction, filling mining area, production of building materials and
improved soil [2]. Mass use of waste in preparation of ceramic materials
may be an effective method to solve the problems above. So far, a variety
of solid waste (like red mud, fly ash, coal gangue, slag, tailings and other
waste) has been used as raw materials for the preparation of ceramic
materials. For instance: 1) Red mud: Xu et al. [3] prepared ceramic tile
with excellent performance at low firing temperatures, using four red
muds and 40 wt% addition as raw materials. 2) Fly ash: Luo et al. [4,5]
found that the pre-activation of fly ash can improve the performance of
fly ash-based ceramic materials significantly. 3) Coal gangue: Li et al. [6,
7] found that a glass ceramic foam material prepared by using coal
gangue and quartz sand has controlled pore structure and properties
through adjusting the composition ratio and sintering process. 4) Slag
and tailings: Teo et al. [8] produced ceramic tile at 1180 ◦ C by using
electric arc furnace and ball clay as raw materials and analyzed the
sintering mechanism and leaching assessment; Deng et al. [9] used blast
furnace slag, Bayan Obo tailings, and fly ash as the raw materials to
prepare glass ceramic composites and investigated the crystallization

* Corresponding author.
** Corresponding author.
E-mail addresses: 1334001588@qq.com (J. Zhang), 57139446@qq.com (T. Liu), 31431645@qq.com (Q. Huang), 106351204@qq.com (Z. Luo), axlu@mail.csu.
edu.cn, 1445082896@qq.com (A. Lu), zhuligang1@163.com, 779032911@qq.com (L. Zhu).
1
These authors contributed equally to this work and should be considered co-first authors.

https://doi.org/10.1016/j.matchemphys.2020.123611
Received 15 May 2020; Received in revised form 21 July 2020; Accepted 25 July 2020
Available online 2 August 2020
0254-0584/© 2020 Elsevier B.V. All rights reserved.
J. Zhang et al. Materials Chemistry and Physics 255 (2020) 123611

behaviors and physicochemical properties of the composites. 5) Other Table 1

waste: Peng et al. [10] has reported the preparation of ceramic tiles by Chemical compositions of the used raw materials (wt.%).
using a fine SiO2 waste crucible powder and quartz sand. Jiang et al. Chemical composition Silica sand Shale Red mud Fly ash
[11] combined granite scraps (main composition) with minor clay tail­
Na2O 0.430 0.271 12.86 0.514
ings to synthesize a ceramic foam material. The above results illustrate MgO 0.485 2.521 1.04 0.784
that the waste-based ceramic materials were prepared based on the Al2O3 9.407 15.805 21.76 30.559
characteristics (difference in composition and content) and commonal­ SiO2 86.735 51.099 20.53 57.114
ity (mainly composed of Si and Al compounds) of various tailings. The P2O5 0.066 0.224 – 0.179
K2O 1.185 3.039 1.76 1.069
successful preparation of these materials could provide an experimental CaO 0.247 12.557 17.23 2.771
basis for new and similar material preparation and relative studies in TiO2 0.196 2.359 4.09 1.593
structural-performance. MnO 0.022 0.185 – 0.036
Silica sand is the main raw material for glass, ceramics, refractory Fe2O3 1.125 11.401 10.47 4.161
SrO 0.007 0.007 0.11 0.038
materials, etc. However, due to the strict requirements of glass raw
ZrO2 0.010 0.030 0.14 0.032
materials for ultrafine powders, most of the silica sand fine powders less SO3 0.036 – – 0.626
than 0.125 mm are not recycled, which leads about 10 million tons of F – – – 0.169
silica sand tailings discharge in China each year [12] Such a large Cl 0.027 – – –
amount of silica sand tailings discharge directly causes serious envi­ Cd2O3 0.001 – 0.02 –
ZnO 0.020 0.04 0.018
ronmental pollution, arable land occupation, and siltation of river
–
Rb2O – 0.016 – 0.006
channel reservoirs [2]. In order to protect the environment and make Ga2O3 0.003 – – 0.006
full use of mineral resources, the comprehensive utilization of silica sand PbO – 0.011 0.01 0.012
tailings or other waste is imminent. In general, the chemical composi­ CuO 0.004 – 0.02 0.018
Cr2O3 0.009 0.020 0.03 0.014
tion of silica sand tailings is relatively stable (more than 80 wt% is SiO2),
Bi2O3 0.005 – – –
and it can be used as raw material for inorganic building materials such LOI – – 8.46 –
as cement, glass, wall materials, glass-ceramics, enamel materials et al.
Therefore, the ceramic material can be prepared by adding an appro­
priate kind and content of other raw materials to the silica sand tailings. tailings, fly ash and red mud), the mineralogical phases have been
From the current reports, it was found that a large amount of admixture examined by X-ray diffraction in our previous work [13,14].
was added in the raw materials, which reduced the utilization rate of
solid waste and increased the production cost of the material. 2.2. Samples preparation
Generally, the chemical composition of waste is very complex and it
contains a variety of chemical compositions, such as Si, Al, O, Na, K, Ca, For the ceramic tile, silica sand tailings and shale were selected as the
Mg, Fe, Mn, Ti. During the preparation of materials, there are coupling raw materials and the ratio is 6/4, while for the ceramic foam, silica
reactions between various chemical compositions. For instance, SiO2 sand tailings, fly ash and red mud were used to prepare with different
and Al2O3 can constitute the skeleton of the ceramic during the sinter­ mass ratios, labeled SFR1, SFR2, SFR3, SFR4, SFR5, respectively, and the
ing, giving the ceramic material high strength and high chemical sta­ chemical composition of prepared samples are showed in Table 2.
bility. Alkali metal oxides, alkaline earth metal oxides and Fe2O3 can be After mixing (raw materials), ball-milling (300 rpm for 2 h), drying
used as flux agent to reduce the sintering temperature of the ceramic (120 ◦ C for 6 h) and sieving (300 mesh), the prepared mixture powders
material and reduce the content of additional additives. In particular, with 5 g was pressed into disk shape (diameter = 25 mm, height = 6
Na2O, K2O, CaO, MgO, SrO and other components can react with SiO2 mm) after the uniaxial pressing conducted at 30 MPa. Lastly, the green
and Al2O3 to form a silicate, aluminate, aluminosilicate melt which cools bodies were heated at designated temperatures in an electrical furnace
to form glass phase. Thus, it is expected that ceramic product such as with heating rate of 5 ◦ C/min in air (the sintering temperature of
ceramic tile and ceramic foam can be obtained by using 100 wt% con­ ceramic tile and ceramic foam is 915–1035 ◦ C for 0–2 h and 1160 ◦ C for
tent waste through combining with different kinds of waste. In this 0.5 h, respectively). The preparation procedure of waste-based ceramic
paper, silica sand tailings were selected as the main raw material (the materials is presented in Fig. 2 and the equipment used in the prepa­
relative content ≥ 60 wt%), fly ash, shale and red mud were auxiliary ration process is shown in Table 3.
raw materials. The effects of different sintering temperatures, holding
time and different fly ash/red mud ratios on the phase evolution, 2.3. Characterization
structure and properties of ceramic tile and ceramic foam were inves­
tigated. Additionally, the glass phase, structure formation mechanism X-ray fluorescence spectroscopy (XRF) and X-ray diffractometer
and environmental impact of the prepared samples was discussed. (XRD, Cu Kα, scanning rate at 8◦ /min, scanning range from 10 to 80◦ )
were used to analyze the chemical composition and the crystalline
2. Experimental procedures phases in the raw materials and the ceramic samples, respectively. Laser
particle size analyzer was adopted to determine the particle size distri­
2.1. Raw materials bution of raw materials. The characterization of pore morphology
mainly focused on the pores including shape and size which was
Silica sand tailings (the residue after flotation), fly ash (collected observed by digital camera. The microstructure and the element analysis
from the flue gas after coal combustion) and shale (from mining) were were tested by the scanning electron microscope (SEM) and energy-
derived from Fengyang county in Anhui, China. Red mud which pro­ dispersive X-ray spectroscopy (EDS), respectively, Au as electrode and
duced in Bayer process was from Zhengzhou of China. In this experi­ the tested sample need to pretreatment before measurement (samples
ment, the Japan ZSX Primus II X-ray fluorescence (XRF) spectrometer were etched in 4 vol% HF solution for 60 s, and then washed and dried
was used for quantitative analysis of the chemical composition. The for 12 h). The distribution of pore size which selected at least 150 pores
chemical compositions of the raw materials can be found in Table 1. The from each digital photo was analyzed using an image analyzer. The
particle size distribution and phase compositions of raw materials is experimental facilities for structural test mentioned above are shown in
shown in Fig. 1. For shale, it mainly contains muscovite (KAl(Si3Al) Table 3.
O10(OH,F)2, PDF#06–0263), quartz (SiO2, PDF#46–1045) and calcite In addition, the physical properties of ceramic materials like density
(CaCO3, PDF#47–1743). For the other raw materials (silica sand (ceramic tile), bulk density (ceramic foam), linear shrinkage (ceramic

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J. Zhang et al. Materials Chemistry and Physics 255 (2020) 123611

Fig. 1. The particle size distribution and crystalline phase of raw materials: (a) silica sand tailings; shale; red mud; fly ash; (b) the crystalline phase. (For inter­
pretation of the references to colour in this figure legend, the reader is referred to the Web version of this article.)

Table 2
The ratio of raw materials and the main chemical composition for the prepared ceramic foams.
Samples Silica sand (wt.%) Fly ash (wt.%) Red mud (wt.%) Main chemical composition (wt.%)

SiO2 Al2O3 CaO Fe2O3 (Na, K)2O MOa

SFR1 65 5 30 65.40 14.17 5.47 4.08 5.52 2.16

SFR2 65 10 25 67.22 14.61 4.75 3.77 4.87 2.01
SFR3 65 15 20 69.05 15.05 4.03 3.45 4.21 1.87
SFR4 65 20 15 70.88 15.49 3.30 3.14 3.56 1.73
SFR5 65 25 10 72.71 15.93 2.58 2.82 2.91 1.59
a
MO: MnO, SrO, TiO2.

Table 3
The experimental facilities and test equipment used in experiment.
Name Type Company Country

Ball mill KQM-X 4 Y/ Xianyang Jin Hong General China

BC Machinery Co., Ltd,
Xianyang
Electrical furnace SGM.M 9/17 E Luoyang Sigma Furnace China
Co., Ltd, Luoyang City
X-ray fluorescence ZSX Primus II Rigaku, Tokyo Japan
spectroscopy
X-ray techniques D/max-2550 Rigaku, Tokyo Japan
PC
Differential scanning STA-449-F 3- NETZSCH Group, Selb Germany
calorimetry Jupiter
Digital camera D 7200 Nikon, Tokyo Japan
Scanning electron FEI Quanta- Thermo Fisher Scientific, USA
microscope 200 Waltham, MA
Fatigue testing CSS 44100 Jiʼnan Rui Rui Machinery China
machine Equipment Co., Ltd, Jinan
City
Laser particle size BT-9300 H Baxter Instrument Co., Ltd. China
meter
Inductively coupled ICAP 6300 R Thermo Fisher Company USA
plasma
spectrometer
Image analyzer Nano Department of Chemistry, China
Measurer Fudan University
Fig. 2. The preparation procedure of full waste-based ceramic materials. software

tile), porosity (ceramic foam), water absorption (ceramic tile) and me­ for every performance was taken averagely from at least six measure­
chanical strength (ceramic tile and ceramic foam) were tested according ments to reduce the experimental error. For ceramic tile, the linear
to the reference and formula, as shown in Table 4. The measured value

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J. Zhang et al. Materials Chemistry and Physics 255 (2020) 123611

Table 4 the highest density and the lowest water absorption. Therefore, the
The test content and reference in this experiment. sample (silica sand tailings/shale ratio = 6/4) is selected as the object to
Test content Formula Reference investigate the effects of different sintering temperatures and holding
times on the structure and properties of the waste-based ceramic tiles.
Bulk density ρ = M/V [29]
Powder ρ0 = M0/V0 Archimedes drainage The crystalline phase of the ceramic tile sintered at different sintering
density method temperatures and different holding times is shown in Fig. 3. As shown in
Total P (%) = (1-ρ/ρ0) [30] the figure, there is no significant change of the phase composition in all
Porosity samples, the main phase is quartz (SiO2, PDF#46–1045) and a low
Water W (%) = (M2-M1)/M1 [7]
absorption
content of kyanite (Al2SiO5, PDF#11–0046) phase is also found. With
Linear S (%) = (L0-L)/L0 [31] the increase of sintering temperature and the extension of the heat
shrinkage ingress, it can be obvious that the diffraction peak strength of the quartz
Weight loss R (%) = (Ma-M0)/M0 GB/T 1970–1996 phase shows a certain degree of decline. This may be part of the quartz at
Degradation C(mg/h) = Weight loss/Degradation [4]
high temperatures involved in the formation of the glass phase, thereby
rate time
Compressive σ = 2P/πad GB/T 1970–1996 increasing the density of ceramic plates.
strength The SEM images of polished surface of ceramic tile sintered at
Flexural σ = 3PL/2bh2 GB/T 1970–1996 different sintering temperatures (915–1035 ◦ C for 1h) are shown in
strength Fig. 4 (a)-(e). As can be seen, the increase of the sintering temperature
Leaching USEPA, 1992
causes a variation in the microstructure of the samples, which is shown
–
toxicity
the sequence of densification behavior of samples with an increased
sintering temperature. As shown in Fig. 4 (a), a loose structure and a
shrinkage was calculated by measuring the length of the samples before bumpy surface are observed in the sample sintered at 915 ◦ C. Upon
(L0) and after (L) sintering. The water absorption was determined by the sintering at the temperature of 975 ◦ C (Fig. 4 (c)), an uncompleted
boiling water method, i.e., the sample was immersed after 2 h boiling in densification and rough surface is still observed. Increasing the sintering
distillate water and cooled to room temperature. The flexural strength temperature to 1035 ◦ C causes a relative dense surface, the formed
(the tested samples were machined into 45 × 5 × 5 mm) was determined liquid phase has surrounded the particle and filled the particle bound­
by using a fatigue testing machine at a loading rate of 1 mm/min. For ary, leading the microstructure tends to dense, as shown in Fig. 4 (e).
ceramic foam, the bulk density can be calculated at the rate of mass and The same tendency to densification also occurs in the microstructure of
volume. And the total porosity (P) was obtained from the bulk density samples at different holding times, as shown in Fig. 4 (f)–(i). The results
(ρ) and powder density (ρ0). The flexure strength and compressive of SEM illustrate that the increase of sintering temperature and the
strength were tested at the cross-head speed of 0.5 mm/min and the prolongation of holding time are beneficial to the formation of liquid
prepared samples were cut with the dimensions of 40 × 3 × 3 mm and phase which cause “liquid phase sintering”, and the samples can obtain a
15 × 15 × 4 mm, respectively. About the test of chemical stability relatively dense microstructure at a lower sintering temperature.
(degradation resistance), the prepared ceramic samples (ceramic tile In addition, the sample sintered at high temperature leaves some
and ceramic foam) were immersed in sulfuric acid solution with a pH pores (labeled in red line), as shown in Fig. 4 (e) and (i), which is related
value of 2 for different time (24 h, 48 h, 72 h, 96 h and 120 h). The to the interaction of the internal components of the sample. Fig. 4 (j)
leaching toxicity of prepared samples was carried out by using the display the SEM image of the selected ceramic tile sample sintered at
United States Environmental Protection Agency toxicity characteristic 1035 ◦ C for 1h. It can be clear seen that a large number of spherical
leaching procedure method 1311 (USEPA, 1992). The equipment used grains are embedded in the glass phase, and a part of the crystal grains
for performance characterization is also shown in Table 3. are surrounded by the glass phase. Region A and region B were selected
on the crystal phase and the glass phase, respectively, and the element
3. Results and discussion distribution is displayed. The main elements detected in the region A are
Si and O elements, which is consistent with the results of XRD. While in
3.1. Microstructure and properties of the full waste-based ceramic tiles region B, elements such as Ca, Al, K, Mg, and Fe are also be found in
addition to Si and O elements. The results of EDS spectra combining with
In our previous work, the density and water absorption of the sin­ the XRF results of the raw materials can be inferred that the composition
tered ceramic tile with different silica sand/shale ratios were compared. of the liquid phase formed in prepared ceramic tile at high temperature
It is found that when the ratio of silica sand/shale is 6/4, the sample has mainly is the Ca–Al–Si–Fe–O glass system. As a composition of the glass

Fig. 3. The XRD spectra of ceramics prepared at different sintering temperatures and time: (a) sintering at 975 ◦ C for 0–2 h; (b) sintering at 915–1035 ◦ C for 1 h.

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J. Zhang et al. Materials Chemistry and Physics 255 (2020) 123611

Fig. 4. The SEM images of polished surface of ceramic tile sintered at different sintering temperatures and time: (a) 915 ◦ C/1h; (b) 945 ◦ C/1h; (c) 975 ◦ C/1h; (d)
1005 ◦ C/1h; (e)1035 ◦ C/1h; (f) 975 ◦ C/0 h; (g) 975 ◦ C/1 h; (h) 975 ◦ C/1.5 h; (i) 975 ◦ C/2 h; (j) the EDS test results.

phase, Fe element mainly come from the reaction of Fe2O3 at high
temperature [15] When liquid phase was formed, a little Fe2O3 could
melt into the liquid phase and the following reaction was occurred:
4Fe3+ + 2O2− → 4Fe2+ + O2. On the one hand, Fe2+ would destroy the
[Si–O] net structure and decrease the viscosity of glass, resulting in a
dense microstructure [16]. On the other hand, the released O2 would be
dissolved in the liquid phase and continuously fused into large bubbles
under the action of plastic flow. After sample cooling, the liquid phase
viscosity increases and some isolated big pores were formed in the
sample, as shown in Fig. 4 (e) and (i).
The physical properties of ceramic tile, including density, water
absorption, liner shrinkage and mechanical strength, as a function of
sintering temperature and holding time, are shown in Fig. 5. As the
sintering temperature increases, the density of samples gradually in­
creases (as shown in Fig. 5 (a)), especially the density of the sample after
sintering at 1005 ◦ C for 1 h exceeds 2.0 g/cm3, mainly because the
microstructure tends to dense constantly with the increase of sintering
temperature. The increased density also leads to an increase in the
flexural strength and the linear shrinkage, while the water absorption
shows an opposite trend, as shown in Fig. 5 (b) Fig. 5 (c) and (d) show
the flexural strength, density, water absorption, and linear shrinkage of
the sintered samples as a function of holding time. It is found that these
performance curves display the similar trends with the temperature
profile, which corresponds to the variation of microstructure in sample.

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J. Zhang et al. Materials Chemistry and Physics 255 (2020) 123611

Fig. 5. The physical properties of ceramic tile at different sintering temperatures and different holding time: (a), (b)sintering at 915–1035 ◦ C for 1h; (c), (d) sintering
at 975 ◦ C for 0–2 h.

By comparing the effect of sintering temperature and holding time on

performance, increasing the temperature has a greater influence on
improving the performance than extending the holding time.

3.2. Structure and properties of the full waste-based ceramic foams

The above chapter mainly studied the preparation of ceramic tiles

using silica sand and shale as raw materials, the added silica sand con­
tent up to 60 wt%. In order to further improve the utilization of silica
sand, we will prepare ceramics foams using silica sand as the main
component and combine fly ash and red mud. The effect of composi­
tional changes on the structure and properties of the prepared ceramic
foam was studied by adjusting the ratio of fly ash and red mud. Fig. 6 is
the XRD result of the sintered ceramic foam with different proportions of
waste. As the proportion of fly ash/red mud increases, the crystalline
phase of the sample gradually changes from a single quartz (SiO2,
PDF#46–1045) phase to a quartz phase and a kyanite (Al2SiO5,
PDF#11–0046) phase. This is mainly due to a solid phase reaction of
Al2O3 introduced by fly ash with SiO2 in the raw material to form
kyanite phase. As the fly ash content further increases, cristobalite (SiO2, Fig. 6. XRD patterns of the sintered ceramic foam with different proportions
PDF#27–0605) phase appears and kyanite phase disappears. Moreover, of waste.
it is also apparent that the formed glass phase has a tendency to
decrease, that is, the broad background at 20–30◦ is continuously
sample. Fig. 7 (h) present the EDS test results and microtopography of
declining. The continuously increasing Al2O3 enhances the softening
the SFR1, SFR2, SFR3, SFR4 and SFR5, respectively, and the selected red
temperature of the samples, resulting in a gradual decrease in the liquid
squares represent the glass phase. It is obvious found that the decrease of
phase content formed in the sample.
red mud content results in the variation of glass phase composition, i.e.
Fig. 7 (a)-(g) shows the pore structure and pore size distribution of
from Ca–Al–Si–O glass system to Al–Si–O glass system, which leads to
samples with different fly ash content. As shown in the figure, the in­
the series of changes in the pore structure. In addition, a physical image
crease of fly ash content not only lead to the formation of closed-pores
of the SFR2 sample at different temperatures is also displayed in Fig. 7
with different size inside the sample, but also leads to the narrowing
(i). As can be seen, the sample reached a relative maximum shrinkage at
of the pore size distribution. It also can be found that the formed pores
1100 ◦ C and then expanded significantly, indicating that a large amount
are uneven and the resulting pore walls show a noticeable gloss, which
of liquid phase was formed inside the sample above 1100 ◦ C. The gases
indicates that a large number of glass phases have formed inside the

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J. Zhang et al. Materials Chemistry and Physics 255 (2020) 123611

Fig. 7. The pore structure and pore size distribution of samples with different fly ash content: (a) 5%; (b) 10%; (c) 15%; (d) 20%; (e) 25%; (f) pore size distribution;
(g) microstructure; (h) the EDS test results; (i) the physical image of the SFR2 sample at different temperatures.

produced near or above this temperature (mainly is the reduction re­ and the thinner the pore wall, resulting in an increase of the porosity and
action of Fe2O3 [14,17]) could be encapsulated by the formed liquid a decrease of the mechanical strength, making the deterioration of
phase and cause the sample to expand. Meanwhile, it is also found that overall properties of the prepared material which is difficult to meet
the volume expansion of the sample changes from the horizontal di­ practical application. Thus, the ratio of fly ash/red mud in 10/25–15/
rection to the longitudinal direction with the sintering temperature and 20, the sample’s comprehensive performance prepared in this work is
holding time further increasing. This is mainly because: when the vis­ optimal, i.e. a bulk density of 0.45–0.61 g/cm3, a porosity of
cosity of liquid phase is lowered, the expansion force of the gas phase is 78.3–85.2% and the mechanical strength is higher than 4.0 MPa.
greater than the surface tension of the liquid phase. Under the action of
external air pressure, the gas has a tendency to move upwards, causing
3.3. Chemical stability and leaching toxicity of the full waste-based
the sample to expand in this direction. When the sample is cooled, a
ceramic materials
large number of pits are formed on the surface due to gas shrinkage.
The physical and mechanical properties of the prepared ceramic
Due to solid waste contains some toxic and harmful substances
foam are displayed in Table 5. It can be seen that the trends in the
(mainly heavy metal ions), the environmental impact of waste-based
properties of the prepared samples in line with the performance char­
ceramic materials has become a key concern. China is a large coal
acteristics of porous materials, that is, the higher the porosity, the lower
producing country, and the annual consumption of coal is more than 4
the bulk density and the worse the mechanical strength, which corre­
billion tons. The acid gas released forms an acid rain and falls back to the
sponds to the evolution of pore structure. For ceramic foam materials
ground [18]. Thus, the prepared ceramic materials are usually exposed
prepared at high temperatures, the higher the content of the low-
to a weakly acidic environment and its chemical stability is a key issue to
viscosity glass phase formed in the sample, the larger the pore size
be considered. In order to safely apply waste-derived materials, the
chemical stability of the developed material must be assessed through
Table 5 the acid degradation resistance and leaching toxicity test. The variation
Physical properties including bulk density, porosity, bending and compressive of mass loss of samples after soaking in acid solution is present in Fig. 8
strength of the ceramic foam. (a). It can be seen that the values of weight loss and degradation rate of
Sample Bulk density Porosity Bending Compressive ceramic materials are in the range from 4.14 to 9.20‰ and from 0.002 to
(g/cm3) (%) strength (MPa) strength (MPa) 0.126 mg/h, respectively. With the increase of degradation time, the
SFR1 0.37 ± 0.04 88.5 ± 3.7 1.4 ± 0.3 2.9 ± 0.2 values of weight loss increase and the degradation rate has a tendency to
SFR2 0.45 ± 0.05 85.2 ± 2.8 2.6 ± 0.2 4.5 ± 0.4 decrease, as shown in Fig. 8 (b). From the above analysis results of the
SFR3 0.61 ± 0.05 78.3 ± 2.3 4.3 ± 0.4 8.1 ± 0.3 chemical stability, it can be known that the prepared ceramic materials
SFR4 0.92 ± 0.03 51.1 ± 1.5 8.7 ± 0.3 15.2 ± 0.5 have high acid degradation resistance (greater than 99%) and low
SFR5 1.51 ± 0.02 23.2 ± 0.5 10.5 ± 0.2 40.8 ± 0.6
leaching rate of toxicity ions, which is mainly due to the effective

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J. Zhang et al.
Fig. 8. The chemical stability of the ceramic samples: (a) mass loss of samples; (b) degradation rate; (c) leaching toxicity.
prevention of the glass phase formed by the synergetic effect between
the components of the waste.
For the results of leaching toxicity (Fig. 8 (c)), it was shown that the
concentration of toxic elements (Pb, Zn, Cr, Cd and Cu) in prepared
ceramic samples is significantly lower than the regulatory standard of
the United States Environmental Protection Agency (USEPA). Due to the
toxic elements being bound physically (trapping) and chemically
(forming the stable chemical bonding) in the glass phase, the reaction
between the acidic solution and the substrate was eliminated [5,19]). In
addition, the crystal also has a non-negligible effect in solidification of
heavy metal ions except the encapsulation for heavy metal ions in glass
phase. In general, the hazardous metals can be consolidated by the
[SiO4] and [AlO4] tetrahedron structure in the silicate mineral based on
the charge balance effect [20]. The XRD analysis shows that the phase of
the SFR sample contains kyanite which belongs to a nesosilicate mineral.
The previous work shows that the structure of kyanite is composed of
[SiO4] tetrahedron and [AlO6] octahedron in crystal structure [21].
During the formation of crystalline phase, the Si–O tetrahedrons can
connect some elements (M) in the process of reorganization. Thus, a part
of the Si4+ in the [SiO4] tetrahedron may be replaced by Mx+ to form
[Mx+O4]4− x (eg. [AlO4]-), resulting in the formation of many negative
charges in the three-dimensional network structures. In order to balance
these negative charges, positively charged heavy metal ions will enter
the network gap of crystal structure to balance charges of the system,
which causes the heavy metal elements can be solidified in crystal lat­
tice. The ability of silicate mineral to capture heavy metal ions (such as
Cd2+, Co2+, Cr3+, etc.) has been reported in previous studies [22–24].
Based on the above analysis, multiple solidification mechanisms may
co-exist and cause heavy metal ions to be cured in the samples, which is
conducive to the safety of the prepared material.
3.4. Discussion of the structure formed in full waste-based ceramic
materials
The above experimental results illustrate that the glass phase formed
inside the sample promotes the densification in ceramic material and the
formation of a high-temperature porous structure. The formation of the
glass phase is a result of the interaction of different chemical composi­
tions inside the sample, we call this interaction between waste chemical
components during sintering as the “synergistic complementary effect”.
It means that in sintering process, the main chemical composition of
waste like SiO2 and Al2O3 would interact with each other to form the
main frame structure of the material, which increases the mechanical
strength of the material (synergistic effect), while other chemical
composition of waste like alkali metal oxides, alkaline earth metal ox­
ides and Fe2O3 etc. would interact with the main chemical composition
to produce glass phase (complementary effect). Based on this concept,
the composition of ceramic materials can be designed by combining a
certain proportion of various waste, which not only improves the utili­
zation rate of waste but also reduces the preparation temperature of the
8
Materials Chemistry and Physics 255 (2020) 123611
material, and it also can adjust the structure and properties of the pre­
pared materials (as shown in our previous work [25]). As can be seen,
the four raw materials used in this experiment mainly contain four el­
ements of Si, Al, Ca and Fe, which were considered for the contribution
of liquid phase formation. Therefore, we can analyze and discuss the
effect of this synergistic complementary effect between the chemical
composition of the waste on the liquid phase formation of ceramic tile
and foaming behavior of ceramic foam by describing the position of the
chemical composition of each sample in the phase diagram. Based on the
previous work, the phase diagram system of CaO–Fe2O3–SiO2,
CaO–Al2O3–SiO2 and “SiO2–Al2O3-fluxing” is introduced to analyze the
bloating behavior of the prepared samples, as shown in Fig. 9 (a), (b) and
(c), respectively [26–28]. The obtained results illustrate the existence of
some fluxes such as alkali metals and alkaline earth metals promoted the
liquid phase formed at relative low temperature. That is to say, the
multi-component interaction (like synergistic complementary effect) in
the raw materials ensures a sufficiently liquid phase, leading to the pores
form.
In order to better describe the formation process of the internal
structure (dense and porous) of the prepared ceramic materials, the
related schematic diagram was drawn, as shown in Fig. 10. On the one
hand, the A-D stage represents the densification process. As the tem­
perature increases, the interstices within the sample become smaller (A-
B); some substances such as SiO2 and Al2O3 will react with the fluxing to
form liquid phase at an appropriate temperature. The formed liquid
phase accelerates the mass transfer process, making the internal struc­
ture of the sample become closer, which provides effective strength
guarantee for the frame structure of the ceramic material (B–C); When
the temperature further increases, a part of Fe2O3 participates in the
formation of the liquid phase and promotes the increase of the relative
content of the liquid phase and the decrease of the relative viscosity of
the liquid phase, while releasing a small amount of gases (C-D). Due to
the limited final sintering temperature, the generated gas expansion
force is less than the surface tension of the liquid phase, so it is difficult
for small pores to converge into large pores. As a result, a small number
of pores were left in the internal structure of the sample, as shown in the
red area in Fig. 4 (e) and (i). On the other hand, C-G represents the
process of the formation of porous structure. When the temperature
increased to 1100 ◦ C, the liquid phase content increases and its relative
viscosity decreases. The reduction reaction of Fe2O3 is occurred, forming
lots of small bubbles (C-E); these bubbles flow in a low viscosity liquid
phase between the particles, and become large bubbles under the
combination of liquid phase surface tension and gas expansion force (E-
F); When the temperature rises to the sintering temperature and is in a
holding state, the expanded bubbles and flowing liquid phase disperse
the particles, forming a “gaseous-liquid-solid phase” structure, which
shows a pore structure from macroscopical view (F-G). It can be seen
that no matter what kind of structure is formed, densification is a stage
that must be experienced, and the main factor leading to the formation
of the two structures is the final sintering temperature. For the ceramic
J. Zhang et al. Materials Chemistry and Physics 255 (2020) 123611

Fig. 9. (a) The ternary plot of CaO–Fe2O3–SiO2; (b) The ternary plot of CaO–Al2O3–SiO2: (c) The ternary plot of Fluxing-Al2O3–SiO2.

Fig. 10. Schematic diagram of internal structure formation of the ceramic tiles and ceramic foams.

material foamed at high temperature, higher temperatures ensure the
formation of sufficient liquid phase content and release a large amount
of gases.
3.5. Advantages and prospects of the prepared full waste-based ceramic
materials
At present, the rural urbanization, urban transformation and
improvement of working and living conditions are closely related to the
construction field. The development of the construction industry pro­
vides a broad space for development of building materials. Therefore,
ceramic materials prepared by using various tailings have broad
application prospects in the construction field. In order to evaluate the
properties of material prepared in this experiment, some ceramic tiles
and ceramics foam prepared from waste in recent years are selected, and
their main properties are compared, including waste content, additive,
physical properties and mechanical strength, as shown in Table 6.
Although some materials have more advantages in performance (such as
higher strength), the materials prepared in this work also have some
obvious characteristics, such as a high utilization of waste and a wide
variation of performance. This is mainly because the raw materials of the
prepared samples are all from different types of waste, and its chemical
compositions are more complex. The content variation of any waste will
cause the change of material properties. With the deepening of our

Table 6
The waste content, additive, physical properties and mechanical strength of various ceramic tiles and ceramic foams.
Ceramic tiles Waste (%) Additive (%) Density (g/cm3) Water absorption (%) Flexural Strength (MPa) Compressive strength (MPa)

[32] 70 30 0.82–2.50 – 11.21–138.52 70.48–1129.36

[33] 0–50 50–100 0.35–1.34 – – 23.9–52.7
[34] 60–80 20–40 2.36 – – 32.3
[35] 65.8–70 30–34.2 1.45–1.71 5.5–5.7 168.3–185.6 –
[36] >5 <95 3.09 6 _ >35
This work 100 0 1.86–2.4 0.3–16.4 8.9–80.8 –

Ceramic foams Waste (%) Additive (%) Bulk density (g/cm3) Porosity (%) Flexural Strength (MPa) Compressive strength (MPa)
[37] 98 2 0.29–0.37 – – 1.32–2.88
[38] <98.75 >1.25 0.32–2.1 <94.20 – >1.8
[39] 70–84 30–16 0.59–0.96 41.8–63.5 2.44–5.82 4.22–8.38
[40] 76.6 23.4 >0.46 <85 – 4.20–10.5
[13] 80 20 0.58–1.15 34.8–78.5 – 4.60–25.3
This work 100 0 0.37–1.51 23.2–85.2 1.4–10.5 0.9–40.7

9
J. Zhang et al.
research works, the role of each component of waste in material prep­
aration, pore structure distribution, performance control and other as­
pects will gradually become clear, providing technical guidance for the
subsequent high-efficiency and high-content utilization of the waste. In
short, the properties of the two ceramic materials prepared in this paper
have unique performance characteristics, which can be used in the field
of architecture as an alternative to existing building materials in the
future.
4. Conclusions
In this work, two types of full waste-based ceramic materials:
ceramic tile and ceramic foam were prepared by using a variety of solid
waste as raw materials, the crystalline phase, structure, physical prop­
erties and relevant formation mechanism of internal structure in pre­
pared samples were analyzed and discussed. The obtained results
illustrated that the liquid phase of Ca–Al–Si–Fe–O glass system was
formed in ceramic tile sample, which promotes the microstructure tends
to dense at relative lower sintering temperature. For ceramic foam
samples, the gases derived from the reduction reaction of ferric iron was
wrapped by the formed Ca–Al–Si–O system glass phase, resulting in the
formation of pore structure. Meanwhile, the properties of the prepared
ceramic foams could be controlled by adjusting the ratio of fly ash/red
mud. Under the synergistic complementary effect of the multi-
component chemical composition, the internal structure of the pre­
pared ceramic material was determined by the formed liquid phase. The
purpose of this work is to obtain a way to utilize industrial waste effi­
ciently such as silica sand tailings, which not only consumes a lot of
tailings (the content of industrial solid waste is 100 wt%), but also ob­
tains some low-cost and high value-added products.
CRediT authorship contribution statement
Jiashuo Zhang: Conceptualization, Methodology, Writing - original
draft. Taoyong Liu: Conceptualization, Methodology, Writing - original
draft. Qianxing Huang: Investigation, Formal analysis, Validation.
Zhiwei Luo: Project administration. Anxian Lu: Writing - review &
editing, Project administration, Supervision. Ligang Zhu: Writing - re­
view & editing, Project administration, Supervision.
Declaration of competing interest
The authors declare that they have no known competing financial
interests or personal relationships that could have appeared to influence
the work reported in this paper.
Acknowledgments
This work has been supported by the major projects of science and
technology in Changsha city (KQ1703014) and the Natural Science
Foundation of China (51862034).
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