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CERAMICS
INTERNATIONAL
Ceramics International 39 (2013) 1923–1929
www.elsevier.com/locate/ceramint

Preparation and characterization of foam ceramics from red mud

and fly ash using sodium silicate as foaming agent
Xingjun Chen, Anxian Lun, Gao Qu
School of Materials Science and Engineering, Central South University, Changsha 410083, PR China

Received 25 June 2012; received in revised form 24 July 2012; accepted 14 August 2012
Available online 21 August 2012

Abstract

Fly ash from the thermal power plant and red mud from aluminium industry were regarded as hazardous industry waste all over the
world. In order to effectively utilize these industrial wastes, a new foam ceramics was synthesized successfully by conventional ceramic
sintering process using fly ash and red mud as the main raw material, with a small amount of sodium borate as fluxing agent and sodium
silicate as foaming agent. An objective of this research was to investigate the influences of the amounts of red mud/fly ash and sodium
borate as well as of the sintering temperature on the porosity, mechanical strength, bulk density, water absorption, microstructure and
crystalline phase. The results showed that homogeneous microstructures of large pores could be obtained by adding about 40–50 wt%
red mud, 26.25–40 wt% fly ash, 15–20 wt% sodium borate, 5 wt% sodium silicate, and using low sintering temperature (900 1C, 2 h),
leading to foams presenting porosity, compressive strength, flexural strength, bulk density, and water absorption values of about 64.14–
74.15%, 4.04–10.63 MPa, 2.31–8.52 MPa, 0.51–0.64 g/cm3, and 2.31–6.02%, respectively. Good correlations among mechanical
strength, water absorption and microstructure (pore size and distribution) were observed.
& 2012 Elsevier Ltd and Techna Group S.r.l. All rights reserved.

Keywords: Red mud; Fly ash; Foam ceramics; Sodium silicate

1. Introduction their long-term maintenance. Therefore, utilization of red

mud will produce significant benefits in terms of environment
The huge volumes of industrial waste produced today and economics by reducing landfill volume, contamination of
represent one of the world’s greatest environmental pro- soil and ground water, and release of land for alternative
blems and recycling has emerged as a very important uses.
environmental issue nowadays due to the diminishing nature Fly ash is another waste residue produced as a by-product
resources and the increasing amount of solid wastes. Red of coal combustion in power stations [5]. This industrial
mud, as one of the major solid wastes, is produced in the waste is regarded as hazardous material all over the world,
process of alumina extraction from bauxite [1]. Due to its which presents serious problems related to land disposal and
caustic nature, it poses a major environmental problem [2]. environmental pollution [6]. However, in China, there are
For every ton of alumina produced, approximately 1–1.5 more and more thermal power plants being built today to
tons of red mud is generated in the process [3]. In China satisfy the increasing demand for energy resources. And
currently only a small percentage of this waste is utilized, millions of tons of coal fly ash are produced each year.
primarily in the cementitious products (concrete and cement) Therefore, the development of new applications for fly ash is
[4], the remainder being directly discharged into ponds or necessary in order to reduce reliance on landfill and could be
landfills, which is regarded as unsightly, environmentally helpful not only in decreasing environmental pollution, but
undesirable and a non-productive use of land resources, also in producing high value added products. And on the
as well as posing an on-going financial burden through other hand, fly ash containing a large amount of CaO, SiO2,
and Al2O3, which are main glass network formers, can be a
n
Corresponding author. Tel.: þ86 731 88830351; fax: þ 86 731 88877057. good raw material for the CaO–Al2O3–SiO2 system of
E-mail address: axlu@csu.edu.cn (A. Lu). ceramic and glass-ceramic production [7].

0272-8842/$ - see front matter & 2012 Elsevier Ltd and Techna Group S.r.l. All rights reserved.
http://dx.doi.org/10.1016/j.ceramint.2012.08.042
1924 X. Chen et al. / Ceramics International 39 (2013) 1923–1929

There are several researches on red mud and fly ash 2. Experimental

reuse; for example, Li et al. [8] evaluated the use of red
mud and fly ash to remove toxic materials from waste 2.1. Raw materials
water; Karasu et al. [9] investigated the effects of red mud
based pigments on wall and floor tile glazes; Amritphale Red mud and fly ash used in the present experiment were
et al. [10] proposed a novel method for making radiation supplied by Henan Aluminum Co. Ltd. and Changsha
shielding materials utilizing red mud and other additives. Power Plant, respectively. The chemical compositions of
Unfortunately, red mud reuse techniques consume rela- red mud and fly ash were determined by X-ray fluorescence
tively small amounts of waste, compared to a huge analysis and the results are shown in Table 1. XRD
quantity of red mud discharged from the alumina produc- analysis was used to investigate the crystalline phase of
tion every year. Thus, in order to realize bulk use in red the raw materials, and the XRD patterns are shown in
mud and fly ash, recently, the exploration has been focused Figs. 1 and 2. As shown in Fig. 1, the major crystalline
on the construction and building industry [11,12], especial phases in fly ash are Quartz SiO2 (PDF no. 8590798) and
in light weight construction products. For example, Yang Mullite Al6Si2O13 (PDF no. 15-0776). As shown in Fig. 2,
et al. [13] found that the addition of up to 40 wt% of red the major mineral phases in red mud are identified as
mud waste was possible in the production of the ceramics Katoite Ca3Al2(SiO4)(OH)8 (PDF no 38-0368), Kaolinite
tiles; Sglavo et al. [14] has added 50 wt% red mud in clay- 1 A Al2Si2O5(OH)4, Calcite Ca(CO3) (PDF no. 64-9630)
based ceramics; Yang et al. [15] successful synthesized and Cancrinite Na7.6(Al6Si6O24)(HCO3)1.2(CO3)0.2(H2O)2.28
glass-ceramics with the total addition of up to 85 wt% of (PDF no. 70-5030). And iron oxide present as Hematite
red mud and fly ash. There are obvious environmental Fe2O3 (PDF no. 87-1164) was also detected in red mud.
benefits to be gained from the recycling of wastes in The amount of red mud and fly ash in the foam ceramics
producing ceramic tiles, ceramics and glass-ceramics. samples was designed to be as high as possible because the
Unfortunately, some aspects limit their applications as experimental purpose was the comprehensive utilization of
well as their commercial success, such as impurities (Fe2O3, red mud and fly ash. The sample with the amount of red
MnO) in the wastes which often color the final products mud in the range of 40–60 wt% and fly ash in the range of
[16], and the complex densification mechanism which limits 20–40 wt% has been prepared and the properties have been
the amount of waste that can be used when preparing studied in detail.
dense products. Development of foam ceramics from red Sodium silicate, as an additive, which was introduced
mud and fly ash might solve the problem. The porosity of into a ceramic foam batch in small quantities is called a
foam ceramics makes it possess the properties of sound
and thermal insulation [17] and it could be used as light
weight construction materials. But little research has been
conducted to focus on preparing the foam ceramics.
In our previous work, the waste-based foam glasses
containing fly ash of 70 wt% have been successfully
prepared by another group of ours [18,19]. In this study,
authors firstly prepared foam ceramics using red mud and
fly ash as raw materials simultaneously, and with sodium
borate and sodium silicate as additives. The effects of
different ratio of red mud and fly ash on sample properties
were studied in detail, mainly including phase composi-
tions, microstructure, porosity and mechanical properties.
And also, the effects of fluxing agent sodium borate as well
as different sintering temperatures on the main properties
of foam ceramics were studied. Foam ceramics may have a
good application in the market of light weight construction
materials because of its lower energy consumption and
costs in the current process, and may play an important
role to eliminate the storage of red mud in China. Fig. 1. XRD pattern of the fly ash.

Table 1
Chemical composition (wt%) of fly ash and red mud.

Raw materials SiO2 Al2O3 Na2O K2O MgO CaO Fe2O3 P2O5 MnO TiO2 LOI

Fly ash 54.37 24.47 1.44 1.71 0.99 4.85 5.50 0.27 0.04 1.45 4.27
Red mud 20.53 21.76 12.06 1.76 1.04 17.23 10.47 0.16 0.01 4.10 10.8
 X. Chen et al. / Ceramics International 39 (2013) 1923–1929 1925

forming agent. Several processes take place under the weight, respectively. The compounds designed in Table 2
thermal treatment of such a mixture, resulting in foam were combined and prepared by uniaxial dry-pressing into
formation. Sodium borate, as an additive which could disk shapes with a diameter of 50 mm, thickness of 10 mm,
reduce the softening temperature, and was introduced into using a pressure of 10 MPa. Then the mixtures would be
mixture is called a fluxing agent. Solid sodium borate melts used in further sintering process. The obtained green
at about 741 1C and reacts with R2O (R ¼ Na þ , K þ ), MO samples are firstly treated at 400 1C for 1 h in order to
(M ¼ Mg2 þ , Ca2 þ ) and partial SiO2 in red mud and fly remove the residue water and protect the samples from
ash, resulting in the formation of multi-component liquid cracking caused by the uneven thermal distribution. Sub-
phase. On one hand, the liquid phase can accelerate the sequently, the samples were heated at 800–1100 1C for 2 h
particle diffusion during sintering process, thereby redu- in an electrical furnace with air atmosphere. The heating
cing the sintering temperature; on the other hand, when rate of 3 1C/min was adopted during total sintering process
the temperature of the mixture exceeds the softening from room temperature to 800–1100 1C.
temperature, particles start sintering and form a contin-
uous sintered body. Particles of the pore-forming agent 2.3. Microstructure characterization
become insulated by softening glass. After a certain
temperature is reached, they start emitting gases or losing The crystalline phases precipitated in the prepared
crystal water, and frothing the glass melt. The various samples are investigated by Rigaku D/max 2550PC
experimental plans are shown in Table 2. X-ray (CuKa, scanning rate: 81/min, scanning range: 10–
801). The surface of the sample was polished by sand paper
2.2. Sample preparation and investigated by scanning electronic microscopy using a
Quanta 200.
Red mud and fly ash were mixed with different amounts
ranging from 20%–40% and 60%–40% of the solid 2.4. Porosity and water absorption

The bulk density was measured with helium psychome-

try. The total porosity was obtained from the bulk density
and the powder density using the following equation:
Porosity ð%Þ ¼ ð1Bulk density=Powder densityÞ
100% ð1Þ
The water absorption was measured by the waterlogged
method using the following equation; we weighed the
samples masses before and after saturation with water:
Water absorption ð%Þ ¼ ðm2 m1 Þ=m1  100% ð2Þ
where m1 and m2 are the weights of the samples before and
after saturation with water.

2.5. Mechanical strength

The specimens used in the flexural strength test are

Fig. 2. XRD pattern of the red mud. machined into 20 mm  6 mm  7 mm test bars. Square foam

Table 2
Amount of raw materials and chemical composition provided by red mud and fly ash in different experimental plans.

Sample Main raw material ratio (wt%) Main chemical composition provided by red mud and fly ash (wt%)

Red mud Fly ash Sodium silicate Sodium borate SiO2 Al2O3 Alkaline oxides Alkaline earth oxides

A1 40 40 5 15 29.96 18.49 6.79 9.64

A2 50 30 5 15 26.58 18.22 7.86 10.89
A3 60 20 5 15 23.19 17.95 8.92 12.13
A4 46.88 28.13 5 20 24.92 17.08 7.36 10.21
A5 43.75 26.25 5 25 23.25 15.94 6.87 9.53
A6 60 20 5 15 23.19 17.95 8.92 12.13
A7 60 20 5 15 23.19 17.95 8.92 12.13
A8 60 20 5 15 23.19 17.95 8.92 12.13
1926 X. Chen et al. / Ceramics International 39 (2013) 1923–1929

glass samples of 12.5 mm length and 5 mm  5 mm section matrix. The size and the number of the pores were
area are subjected to uniaxial compressive loading. The obviously smaller than those in A1 and A2, with values
flexural strength and compressive strength are measured for of bulk density 1.13 g/cm3 and porosity 33.67%. Due to
specimen bars with a span of 10 mm at a cross-head speed of the inertness of red mud, the softening temperature
1 mm/min, using a CSS44100 testing machine. Each result is increased obviously with the addition of red mud, which
the average of five measurements. led to high viscosity unnecessary for foaming and dimin-
ished the pore sizes.
3. Results and discussion Table 3 (A1, A2 and A3) reports sample properties
versus different ratios of red mud to fly ash tested. It can
3.1. The effects of red mud and fly ash on sample properties be observed that sample A1 showed high water absorption
with value 6.02%. Sample A2 had lower water absorption
In the experimental results, labeled A1, A2 and A3, value 3.26%. The lowest value of 1.55% was obtained in
effects of different ratios of red mud to fly ash on sample the sample A3. It was found that water absorption of the
properties were investigated, shown in Table 3. In the samples decreased linearly with the addition of red mud.
sample, the raw material is red mud and fly ash, and Apparently, the water absorption of the porous ceramics
sodium silicate is added as foaming agent and sodium was related to the amount of waste residue that was added.
bauxite as fluxing agent. The red mud contents 40 wt%, Essentially, water absorption was directly related to the
50 wt% and 60 wt% were used in A1, A2 and A3, porosity, and correlated with the number of open pores in
respectively. And also, the fly ash contents 40 wt%, sample appearance. In short, the porosity of the products
30 wt% and 20 wt% were used in A1, A2 and A3, increases, and the water absorption falls.
respectively. The flexural strengths of the sample A1, A2 and A3 were
Fig. 3 illustrates the evolution of microstructure of the 2.31 MPa, 6.25 MPa and 11.25 MPa, respectively. And the
samples A1, A2 and A3 heat treated at 900 1C for 2 h. As corresponding compressive strengths vary from 4.04 MPa,
presented in A1, the matrix is filled with majority of round 9.52 MPa to 17.29 MPa. Both compressive strength and
shaped large pores (diameter of 1.5–2.5 mm) and minority flexural strength increase with the increase of red mud
of small pores (diameter of 0.3–0.5 mm) that can easily be percentage. Moreover, higher porosity led to lower
inferred in accordance with the results of bulk density mechanical strength. As shown, it can be concluded that
0.64 g/cm3 and porosity 69.32%. In sample A2, it presents a negative correlation between mechanical strength and
round shaped small pores (diameter of 1.0–1.5 mm) and water absorption is obtained in this foam ceramics.
denser microstructure, and showed higher values of bulk Fig. 4 illustrates the XRD patterns of the sample with
density (1.13 g/cm3) and slightly low porosity 44.33%. In the various proportions of red mud and fly ash. It can be
sample A3, many unshaped pores were distributed in the seen that no Nepheline KNa3Al4Si4O16 (PDF no. 74-1718)

Table 3
Sample properties of the eight experimental plans.

Sample A1 A2 A3 A4 A5 A6 A7 A8

Bulk density (g/cm3) 0.64 1.13 1.63 0.60 0.51 1.52 1.19 1.67
Powder density (g/cm3) 2.08 2.03 2.47 8.84 14.77 1.96 1.91 2.32
Porosity (%) 69.32 44.33 33.67 74.15 64.14 22.83 37.72 28.10
Water absorption (%) 6.02 3.26 1.55 2.31 4.68 2.69 1.48 1.32
Flexural strength (MPa) 2.31 6.25 11.25 8.52 4.74 6.93 8.21 5.02
Compression strength (MPa) 4.04 9.52 17.29 10.63 6.32 15.78 15.46 13.64

Fig. 3. SEM images of sample A1 (40 wt% red mud, 40 wt% fly ash), A2 (50 wt% red mud, 30 wt% fly ash), and A3 (60 wt% red mud, 20 wt% fly ash).
 X. Chen et al. / Ceramics International 39 (2013) 1923–1929 1927

phase is observed in A1. With content of red mud Fig. 5 clearly illustrates the evolution of microstructure
increased to 50 wt% or 60 wt%, nepheline phase appears of samples A2, A4 and A5 heat treated at 900 1C for 2 h.
in A2 and A3. The major phases in these three samples are The morphology of A2 has been described above. In
Hauyne K1.4Ca2.4Na4.32(Al6Si6O24)(SO4)1.52 (PDF no. 78– sample A4, the round shape pores (diameter 1–1.5 mm)
2490) and Andradite Ca3Fe2(SiO4)3 (PDF no. 84-2160). By were formed in the matrix, with values of porosity 74.15%,
increasing the amount of red mud, the peak intensity of and bulk density 0.60 g/cm3. Moreover, from Fig. 5 (A4),
nepheline phase and hauyne phase increased, but the peak pores were distributed uniformly in the matrix and formed
intensity of glass phase in these three samples gradually homogeneous structure which contributes more to the
decreased. Mostly, the peak intensity of andradite phase in mechanical strength. In sample A5, the pores present
A2 is stronger than that in A1 and A3. According to these mainly in large scale (diameter 1.5–3 mm), irregular shape
phenomena above, it can be inferred that, phase transfor- and non-uniform distribution in the matrix, with porosity
mation exists here, including glass phase changed into 64.14%, and bulk density 0.51 g/cm3. Pores with uniform
nepheline phase, and andradite phase changed into hauyne distribution result in high porosity obtained by A4 than
phase or nepheline phase. This was seemingly achieved due other samples with non-uniformly distributed pores.
to the change of the content of raw materials (red mud and Table 3 (A2, A4 and A5) reports sample properties
fly ash) and especially the replacement among ions versus different contents of sodium borate tested. It was
occurred in structure vacancy. found that water absorption decreases with sodium borate
percentage at first and increases later. The water absorp-
tions of samples A2, A4 and A5 were 3.26%, 2.31% and
3.2. The effect of sodium borate on sample properties 4.68%, respectively. The evolution of the water absorption
also fits well with the sintering behavior of ceramics
In the experimental results, labeled A2, A4 and A5, the affected by the formation of a ‘‘transitory liquid’’ phase
influences of sodium borate content on sample properties which improves densification of the green body. Proper
were investigated, shown in Table 2. In the sample, sodium percentage of sodium borate is necessary for the densifica-
borate contents of 15 wt%, 20 wt% and 25 wt% were used tion of sample body and foam formation in the matrix (not
in A2, A4 and A5, respectively. on the matrix surface). The effects caused by sodium
borate percentage mainly include: (i) small amount of
fluxing agents, in the matrix at 900 1C, cannot sufficiently
make the matrix softened in the sintering process and
formed densification body adversely. Due to the pressing
caused by physical block, the foam formed by foaming
agents cannot grow in this unsoftened matrix, (ii) excess
amounts of fluxing agent, tend to enhance the softening
ability of the system. And on the surface of sample at 900
1C, high content of sodium borate caused serious collapse
phenomenon. The foam formed by foaming agents can
easily cross the matrix and form large open pores in the
sample surface. Also, the high value of water absorption in
A5 is most probably due to large open pores present in the
sample surface.
The influence of sodium borate content on mechanical
strength was investigated, also presented in Table 3 (A2,
A4 and A5). The relationship between mechanical strength
and water absorption also presents a negative correlation
Fig. 4. XRD patterns of samples A1, A2 and A3. as we described above. As shown, the mechanical strength

Fig. 5. SEM images of samples A2, A4 and A5 with 15 wt%, 20 wt% and 25 wt% sodium silicate content, respectively.
1928 X. Chen et al. / Ceramics International 39 (2013) 1923–1929

increases with the increase of sodium borate percentage at Thus, calcium, magnesium, iron and aluminum might occupy
first and decreases later. The flexural strengths of samples structure vacancy and cause this transformation.
A2, A4 and A5 were 6.25 MPa, 8.52 MPa and 4.74 MPa,
respectively. And the corresponding compressive strengths
vary from 9.52 MPa, 10.63 MPa to 6.32 MPa. Sample A4 3.3. The effect of heat-treatment temperature on sample
with high porosity exhibits relatively high mechanical properties
strength value. This phenomenon can be ascribed to
porous structure (including the number, the denser micro- In the experimental results, labeled A3, A6, A7 and A8,
structure, and uniform distribution of the pore) of the effects of sintering temperature on sample properties were
produced materials. While carrying out mechanical test on investigated, shown in Table 2. In the sample, the sintering
the samples with uniformly distributed pores, the area temperatures of 800 1C, 900 1C, 1000 1C and 1100 1C were
which can be effectively contacted with plunger tip on the used in A6, A3, A7 and A8, respectively.
surface gets larger and the force can be well distributed on Fig. 7 schematically illustrates the evolution of micro-
the samples. So under the condition of loading force, high structure for the samples heat treatment at 800–1100 1C.
stress would be used to damage the samples. Round shape pores with diameter of 1 mm were gradually
Fig. 6 (A2, A4 and A5) shows the XRD patterns of the formed at 10001C. The samples sintered at lower tempera-
foam ceramics with sodium borate contents 15 wt%, 20 wt% tures (800 and 900 1C) showed a denser microstructure,
and 25 wt%. The crystalline phase present in the samples and many of the unformed pores (100 mm in diameter) in
corresponds to hauyne, nepheline and andradite. The peak A6 (with porosity 22.83%) and A3 (with porosity 33.67%)
intensity of andradite could be simply compared and described can be clearly seen from the SEM images. With sintering at
by A24A44A5. But peak intensities of hauyne and nephe- higher temperature (1200 1C), the sample exhibits a char-
line, in these three samples, show the same correlation with acteristic of relatively quick densification which is well
A44A24A5. With the amount of sodium borate increasing, verified by the quick increase in bulk density (1.67 g/cm3).
it caused the transformation in crystalline phase and most And the quantity of pores (1.5 mm in diameter) in A8
probably due to the chain silicate structure of the crystalline (with porosity 28.10%), was obviously less than that in A7
phase it enables solubility of various ions in their structure. (with porosity 37.72%). This was seemingly achieved due
to a higher liquid phase viscosity.
As shown in Table 3 (A6, A3, A7 and A8), when the
proportion of the raw materials was fixed as red mud
60 wt%, fly ash 20 wt%, sodium silicate 5 wt% and
sodium borate 15 wt%, their properties were less sensitive
to temperature variations. It was found that as the
sintering temperature increases, the water absorption
decreases. The result was influenced by the densification
sintering degree under different sintering temperatures.
The mechanical strength displayed the nonlinear trend
with the heat treatment temperature increasing. As the
temperature from 800 to 900 1C, the flexural strength
increased from 6.93 MPa to 15.78 MPa and the compres-
sion strength increased from 15.78 MPa to 17.29 MPa. But
when the temperature exceeds 900 1C, the flexural strength
and compression strength decreased from 11.25 MPa to
5.02 MPa and 17.29 MPa to 13.64 MPa, respectively. Also,
the measurement (such as the test method, sample
preparation and calculation) caused relatively small
Fig. 6. XRD patterns of samples A2, A4 and A5. impacts in sample properties. For the foam materials, it

Fig. 7. SEM images of samples A6, A3, A7 and A8 sintered at 800 1C, 900 1C, 1000 1C and 1100 1C, respectively.
 X. Chen et al. / Ceramics International 39 (2013) 1923–1929 1929

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neous Material Mechanics, ICHMM 2008, June 3, 2008–June 8, 2008,
This work has been supported by the Key Project DEStech Publications Inc., Huangshan, China, 2008, pp. 905–908.
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Foundation of Science and Technology Plans of Changsha
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