Mineralogically Formulated Advanced Shielding Ceramics

Utilizing Red mud and Fly ash

Jeeshan Khan1, S.S. Amritphale 1, Navin Chandra1, Anil K. Gupta1,
Arvind Shrivastava2 and U.S.P. Verma2
1
Environment, Industrial Waste Utilization and Nano materials Division, Advanced Materials &
Processes Research Institute, (C.S.I.R.), Hoshangabad Road, Bhopal 462064, M.P., India
2
Nuclear Power Corporation of India Limited, Mumbai-400094, India

Abstract
Red mud (bauxite waste) emerge as by-product from the caustic leaching of bauxites to
produce alumina and it causes serious problems such as storing and environmental pollution.
In this study, red mud, which is the industrial waste of HINDALCO Aluminium Plant
(INDIA), was investigated for a novel energy efficient process by developing
mineralogically formulated compositions using varying percentage of red mud and fly ash.
The sintering characteristics of red mud- fly ash compositions having 0100% fly ash (w/w)
in the pre fixed presence of 10% (w/w) sodium hexa meta phosphate (SHMP) have been
studied. The sintering of red mud alone with SHMP at 950C produces tiles with low impact
strength; however, the incremental addition of fly ash improves impact strength. The impact
strength of composites with 10-30% (w/w) fly ash in the red mud- fly ash composition
enables achieving the acceptable limit (19.6 J/m) set by the Indian Standards Institute for
wall tiles. Increasing the fly ash content up to 20% (w/w), results in an increase in apparent
density and shrinkage of tiles while water absorption decrease up to 20%. However the
further increase in the fly ash content increase the water absorption. The various mineral
phases formed in the sintered compositions have been identified using X-ray powder
diffraction technique is among the various metal silicates, phosphates and silico phosphates.
The strength observed in the optimized composition is attributed to the formation of these
minerals phases and to the rod shaped morphology of aluminium phosphate as revealed by
the scanning electron micrographs. The shielding, i.e. half value thickness (HVT) for X-ray
photons of the optimum composition has been evaluated and compared with conventionally
used shielding materials namely concrete. The results of this study are presented in this
paper.
Keywords : Red mud; Fly ash; Energy efficient process; Ceramic tile

1. Introduction
The general trend of today for the industrial wastes or by-products, which are produced in
industrial countries, is to examine alternative ways for their exploitation in order to eliminate
cost of disposal and avoid soil and water contamination. Many of these undesirable industrial
materials contain significant amounts of inorganic ingredients, such as oxides of silicon,
aluminum, calcium and iron, which, at suitable combinations, can be used in the production
of building materials such as ceramic tiles, bricks, portland cement clinker.
The Red Mud (RM) residues formed during the extraction of alumina from bauxite by the
Bayer process contain titanium, iron and aluminium compounds that could provide an
interesting source of raw materials for relevant processing industries [1]. It generally exits
276 TRAVAUX Vol. 36 (2011) No. 40

the process stream as a highly alkaline slurry (pH 1012.5) with 1530% solids [2-5], and it
is pumped away for appropriate disposal. It is a complex material whose chemical and
mineralogical composition varies widely, depending upon the source of bauxite and the
technological process parameters. Every red mud is composed of as many as 1421 mineral
phases [6].
At all the worlds 85 alumina plants, 1.01.6 tonnes of red mud is generated per tonne of
alumina and it is estimated that over 66 million tonnes of this waste is impounded annually
in the world. The disposal of such a large quantity of this alkaline waste sludge is expensive
(up to 12% of the alumina price), as it requires a lot of land (approximately 1 km2 per 5
years for a 1 Mtpy alumina plant) and causes a number of environmental problems [2]. The
neutralization of red mud and its adequate treatment to allow its reuse seem to be the
realistically convenient steps for the disposal of this industrial residue. There are several
works on red mud utilization, for example, as acidic amender or bottom sealant in disposal
sites construction [7], as catalyst in hydrodechlorination of tetrachloroethylene [8],
sequestration of carbon dioxide (CO2) [9] radiopaque shielding materials[10,11], Nano-
crystal glass-ceramics[12], building materials namely iron rich cement[13,14], red mud
polymer composites panels as wood substitute[15], glazes[16], bricks[17], ceramics,
tiles[18], for iron ore tailing [19.], etc.
Fly ash is also generated from thermal power industries in enormous quantity. The large
quantity of coal burned in these plants generates huge quantity of fly ash. On a per unit of
energy production basis, Indian thermal power plants generate more fly ash as the Indian
coals contain more silica than the coals found in other countries[20]. It is estimated that
currently about 90 million tons of fly ash is generated every year in India alone. Large
quantity of fly ash finds its way into fly ash ponds, which not only occupy valuable land
resources but also pose a threat to ground water, there is a need to find applications where fly
ash may find bulk utilization [21]. Only a small quantity of the total fly ash generated is
utilized in making bricks, concrete blocks or blending with cement [17, 22, 23]. The
extensive research carried out in recent years for finding further applications of fly ash have
led to the development of processes for making, hollow/masonry/concrete blocks[24-26],
glass ceramics[27-29], ceramic wares[30], radiopaque material [31].
In spite of considerable application of red mud and fly ash utilization for making variety of
value added materials, till date the problem of utilization of red mud and other industrial
waste has not been addressed because the sintering temperature of making ceramic materials
using red mud and fly ash is quite high [32-34].
The application of radiation technology in medicine, agriculture, nuclear reactor and other
industries is increasing day by day all over the world. However, the use of radiation is
invariably associated with very well established harmful effects of X-ray radiation, such as
destroying the tissue of animals bodies and white blood cells, i.e. W.B.C. Conventionally,
the shielding materials based on lead and lead containing compositions are well known and
widely used but such shields are characterized by high toxicity in production and recycling
and therefore poses environmental pollution problem [35, 36]. Lead is conventionally used
but ranked number one on the U.S. EPAs Top 20 Hazardous Substance Priority list [37].
The increased awareness has recently led to extend the application of titanium for use as
Jeeshan Khan et al. : Mineralogically Formulated Advanced Shielding Ceramics 277

future non-toxic shielding material, instead of lead because titanium is not a hazardous
material [38]. The use of ceramic, glassceramics and synroc based radiation shielding
materialsis gaining increased research interest for shielding and encapsulationof surplus
radioactive waste from nuclear power plant and defense sources. These materials are based
on one or more of the compositions based on barium aluminosilicate, phosphatesof iron,
titanium, calcium, magnesium, etc [39, 40].
Further, the red mud generated in million tonnes, also contains a fairly high quantity of
titanium oxide (525%), in addition to very high percentage of iron oxide (2065%) and
aluminum oxide (1027%) and therefore it can be used as useful resource material for
making X-ray shielding materials, it was therefore thought worthwhile to explore the
possibility of developing red mud based shielding materials. In this paper the intention of
developing a process for the utilization of red mud and fly ash based ceramic wall tiles for
radiation application.

2. Experimental
2.1 Raw materials and chemicals
A.R. grade sodium hexa meta phosphate (SHMP) (Rankem, India) was used as a binder
without further purification. The red mud procured from Hindustan Aluminium Company
(HINDALCO), Renukoot, India was in the form of clay-type waste residue composed of fine
fraction (mud) and a relatively coarse fraction (sand) with small granules and fly ash
collected was from the electrostatic precipitators of the Sarni Thermal Power Plant in M.P.
(India), and a representative red mud and fly ash sample was prepared by coning and
quartering, used in the present study.
Representative samples of red mud and fly ash were characterized using X-ray diffraction,
and scanning electron microscope. The chemical analysis was carried out using wet chemical
method.
2.2 Preparation of green tile samples and their sintering
The green tiles samples were prepared, red mud (RM), (090% w/w) fly ash (FA) + (10%
w/w) sodium hexa meta phosphate (SHMP) were mixed in selected weight ratios and
thoroughly homogenized and was then compressed in a steel mold of 10.2 x 10.2 cm2 bed
size to a thickness of 0.5-0.7 cm at a pressure of 50 kg/cm2 for 2 min based on our earlier
research [11, 41]. The tile samples were named firstly red mud initial then fly ash initial
(RMFA) and the percentage of fly ash used in red mud. The green samples were dried in an
air oven at 110C for 6 h and then sintered in an electrical muffle furnace. The firing cycle
was programmed as follows: heating from ambient temperature to 400C at a heating rate of
10C per minute, holding for 30 min at 400C, heating to 950C final temperature, soaking
for 1 h at the rate 10C and finally cooling of samples in the furnace itself down to ambient
temperature based on our earlier research [41, 42].
2.3 Testing of sintered tiles
The apparent density determination has been performed as per the standard procedure
prescribed for ceramics [43]. The sintered tiles samples were evaluated for their impact
278 TRAVAUX Vol. 36 (2011) No. 40

strength following the procedure laid down in the specifications drawn for ceramic tiles [44].
The bulk density, percent linear shrinkage and percent water absorption following the
procedures described earlier [21, 45].
The procedure for measuring impact strength involved use of failing weight type instrument.
The impact strength was carried out by placing the bottom surface of the tile on a 60mm
equilateral triangular support. A steel ball of 30 g weight was allowed to drop on the top
surface of the tile sample from an initial height of 25 cm. The height of the free fall of the
steel ball was increased in small increments till failure. Impact strength was calculated as per
the formula [46].
Wh
Impact strength =
t
where W is the weight of the steel ball in (kg), h the height of free fall of steel ball in (m) and
t is the thickness of the tile in (cm).
2.4 Determination of X-ray attenuation characteristics
The determination of X-ray attenuation characteristics of optimized tile was carried out in
the Standard Safety System Division of Bhabha Atomic Research Center (BARC), Mumbai,
India, under following measurement conditions:
(i) Measurements were done with (I) and without filters (I0) to determine the tenth value
thickness (TVT) of the beams.
(ii) Measurements were done at a distance of 60 cm from the surface of the cone to the
center of the chamber (i.e. at a distance of 100 cm from the X-ray focal spot).
(iii) Dose rate meter UNFORS Instrument (Sweden) type 9001, sr. no. 12394.
2.5 Characterization
Different instrumental techniques such as X-ray powder diffraction and SEM were used for
characterization of the raw materials as well as of all the sintered tile samples. The
identification of the various mineral phases of the finely ground sample of raw materials and
ceramic tiles was carried out with the help of a Philips X-ray diffractometer (Model
PW1710) using Cu-K radiation and operated at 40 kV and 20 mA. The XRD patterns were
recorded from 10 to 70 2 with a scanning speed of 0.02 2 per second. In order to
examine the morphology of the various mineral phases in the samples a scanning electron
microscope (JEOL, Model JSM 5600) was used.

3. Results and discussion

3.1 Characterization of raw materials
The chemical composition of red mud (RM) and fly ash (FA) were determined by standard
wet chemical analysis method of chemical analysis [47]. The chemical analysis confirmed
the presence of various metal oxides of RM and FA are shown in (Table 1 and Fig.1. A & B)
the presence of various prospective mineral phases. The results of chemical analysis of red
mud and fly ash samples appear very similar to the chemical analysis of red mud and fly ash
as described elsewhere [41, 48,].
Jeeshan Khan et al. : Mineralogically Formulated Advanced Shielding Ceramics 279

Table 1. The Typical chemical analysis of red mud (RM) and fly ash (FA) samples.

Fe2O3 TiO2 Al2O3 SiO2 CaO Na2O MgO K2 O LOI*

Red mud (%) 31.21 21.20 20.10 8.50 2.99 6.00 - - 10
Fly ash (%) 5.55 1.38 21.30 62.12 0.53 0.32 1.58 4.24 3.30
*LOI- Loss of Ignition

Fig 1. Chemical analysis of (A) RM and (B) FA and major prospective mineral phases.

3.2 Phase identification in red mud and RMFA system (containing 050% fly ash +
10% SHMP) based tiles
The X-ray diffractograms of red mud, fly ash and optimized RMFA 20 tile (containing 20%
fly ash in red mud + 10% SHMP) based tiles at 950 C are shown in (Fig.2). The RM sample
is found to contain anatase (d values: 1.692,2.420,1.830), rutile (d values: 1.692, 2.206,
2.115, 1.482), quartz (d values: 3.355, 4.18), hematite (d values: 2.70, 2.514, 1.692),
boehmite (d values: 2.206, 1.482), gibbsite (d values: 4.843, 2.206 ), bayerite (d values:
1.692, 1.452, 2.206,), Na5Al3CSi3O15 (d values: 3.67, 2.115, 6.36), cancrinite (d values:
1.452, 3.67, 2.115, 1.482), chantalite (d values: 3.355, 1.452, 4.18, 1.482,) and calcite (d
values: 3.036). For the sake of comparison, the X-ray diffractogram of the fly ash (FA) also
shown. The X-ray diffraction results of fly ash show the presence of major phases of quartz
(d values: 3.348, 4.264, 1.820, 2.291, 2.457), mullite (d values: 3.393, 5.385, 2.207,
2.885, 2.124), and minor phases of hematite (d values: 2.543, 2.694), are identified in XRD
[31].
From the x-ray diffraction pattern of RMFA 20 system based tiles, it is observed that the
intensity of the peaks corresponding to gibbsite vanishes completely, and NA5Al3CSi3O15,
chantalite are observed to decrease significantly, leading to the formation of an array of new
additional phases namely iron silicate (d values: 2.510, 1.688, 1.481), potasium titanium
oxide (d values: 2.690, 2.505, 3.343), sodium calcium silicate (d values: 2.690, 3.343,
1.835, 2.199), sodium iron titanium silicate (d values: 2.690, 2.510), sodium calcium iron
silicate (d values: 2.690, 3.343, 2.199), aluminium iron oxide (d values: 2.690, 1.481,
1.448), calcium aluminium silicate (d values: 2.690, 1.835, 2.199), iron aluminium
phosphate (d values: 3.343, 3.838, 2.994), silcon phosphate (d values: 2.671, 3.343,
280 TRAVAUX Vol. 36 (2011) No. 40

2.994), iron titanium oxide (d values: 2.690, 1.688, 1.481, 1.448), magnetite (d values:
2.510, 1.481), sillimanite (d values: 2.129,2.454), aluminium phosphate (d values: 2.199,
2.690,1.381) are identified in XRD.
The major phases in the RMFA 20 are calcium aluminum silicate, aluminium phosphate,
Iron aluminium phosphate, iron silicate and potassium titanium oxide. These phases
responsible for observed reinforcement and strength leading to the densification in the matrix
of ceramic tiles for X- radiation shielding. The decomposition of gibbsite, cancrinite and
chantalite leads to the formation of calcium aluminium silicate. The formation of potassium
titanium oxide results from the reaction between potassium of fly ash and titanium oxide
content of red mud [49].

Fig 2. X-ray diffraction patterns of red mud (RM), fly ash (FA) and optimized RMFA
20 system (containing 20 % fly ash + 10% SHMP) at 950C
3.3 Impact strength of RMFA system tiles
The impact strength versus percentage in RMFA system (containing 090% fly ash + 10%
SHMP) is shown in (Fig. 3). The impact strength of sintered tiles made from either alone red
mud or alone fly ash and 10% SHMP is found to be very low. However, as the content of FA
Jeeshan Khan et al. : Mineralogically Formulated Advanced Shielding Ceramics 281

addition, the formation of metal silicate phases namely calcium aluminum silicate, iron
silicate, potassium titanium oxide and magnetite takes place respectively and consequently
leading to a sharp increase in impact strength as these phases provides reinforcement [49].
These crystals phases act like whiskers and therefore enhancing the strength [50].
The tiles in the RMSP10- 20 % SP system meets the impact strength as per the is standard
i.e. 19.6 J/m. However, the RMFA 20 sintered tiles optimized composition exhibited highest
impact strength.
Further the beyond 20% fly ash content, in the RMFA system, as the availability of heavy
metal from red mud to form metal silicate phases becomes a limiting factor, the impact
strength decreases significantly.

24

22

20
Impact strength (J/m)

18

16

14

12

10

8
0 20 40 60 80 100

% fly ash(w/w) in RMFA system

Fig 3. Effect of the addition of fly ash (090%) + 10 % SHMP in RMFA system on the
impact strength of the sintered tiles

3.4 Apparent density and % linear shrinkage of RMFA system based tiles
The effect of, addition of fly ash in the red mud, on the % linear shrinkage and apparent
density of fired tiles has been studied and the results are given in (Fig. 4). Both, the % linear
shrinkage and apparent density are observed to increase with increase up to 20% of fly ash
content in the tile. The increase in % linear shrinkage indicates enhanced densification of
tiles due to increase in fly ash which contains fluxing agent i.e. potassium.
Furthermore above 20% of fly ash addition, the apparent density and % linear shrinkage both
decrease significantly due to increasing fly ash content, which may be attributed to the
increase in quartz content with the further increase of fly ash content and decrease of metals
contribution from red mud as the red mud percentage decreases.
282 TRAVAUX Vol. 36 (2011) No. 40

3.0 10
-3
Apparent density (g/cm )
2.8
% linear shrinkage
8
2.6
Apparent density (g/cm )
-3

2.4
6

% linear shrinkage
2.2

2.0 4

1.8
2
1.6

1.4
0

1.2
0 20 40 60 80 100

% fly ash (w/w) in RMFA system

Fig 4. Effect of the addition of fly ash (090%) + 10 % SHMP in RMFA system on the
apparent density and linear percent shrinkage of the sintered tiles
3.5 Percentage water absorption of RMFA system based tiles
The plot of %water absorption versus percentage of fly ash in RMFA system shown in
(Fig. 5). It is observed that initially, the % water absorption values decrease with increase in
fly ash content up to about 20% but found to increase on further increase of fly ash content.
The increase in % water absorption beyond 20% fly ash may be, the formation of
microcracks in the time of cooling of sintered tiles due to the inversion of quartz is
responsible for the creation of voids; hence, the fly ash tiles exhibit greater water absorption.
The lower content of quartz in fly ash and the formation of interlocking structures, which
resist microcracks, are responsible for the lower water absorption observed in red mud rich
tiles [51], while the initial decrease in % water absorption may be attributed to an increased
densification on addition of fly ash, as also indicated by the trends of increase in the fired
density of tiles. Since the percent water absorption is high (>15%), the tiles can be fixed on
the walls by cementing process.
22

20

18
% water absorption

16

14

12

10

0 20 40 60 80 100

% fly ash (w/w) in RMFA system

Fig 5. Effect of the addition of fly ash (090%) + 10 % SHMP in RMFA system on
the percent water absorption of the sintered tiles.
Jeeshan Khan et al. : Mineralogically Formulated Advanced Shielding Ceramics 283

3.4 Determination of the attenuation characteristics of the optimized ceramic tile

composition
The results of narrow beam X-ray attenuation characteristics of ceramic tile at 100 kV
energy of X-ray in terms of the half value thickness (HVT) of X-ray photons are given in
(Fig. 6). On the basis of data the half value thickness (HVT) has been compared with
conventional concrete and lead material [52]. From the HVT value of shielding material at
100 kV of X-ray photon, it is found that shielding material can preferably be used for the
construction of X-ray diagnostic.

Fig 6. Comparison of shielding thickness in terms of half value thickness (HVT)

at 100 kV of X-ray
3.5 Morphological studies on red mud, fly ash and RMFA 20
The scanning electron microphotographs exhibiting microstructure of red mud as such is
given in (Fig. 7. A) shows the red mud scattered morphology texture like aluminium silicates
distributed with heavy constituent phases, such as tetragonal anatase and rutile, spherical
hematite, hexagonal cancrinite and orthorhombic boehmite. The scanning microphotograph
of the fly ash given in (Fig. 7. B) shows predominantly broken spherical particles.
Further, (Fig. 8 C & D) shows the morphology of optimized RMFA 20 revealing the
rhombohedral shaped crystals of calcium aluminum silicate in the matrix. From the above
experimental studies, it is inferred that the rhombohedral crystals of metal silicate namely
calcium aluminum silicate, and the elongated crystal formation of metals silicate and
phosphate in the aggregate. These crystals act like whiskers enhancing the strength, which
acts as reinforcement to the ceramic matrix and is responsible for providing strength in the
sintered tile bodies [50] for X-ray shielding application. The tiles made from above 20 % fly
ash content results in low strength of the ceramic tiles due to presence of highly content of
quartz.
284 TRAVAUX Vol. 36 (2011) No. 40

A B

Fig 7. SEM micrographs of red mud RM (A), fly ash FA (B).

C D

Fig 8. SEM micrographs of optimized RMFA 20 shielding material (C & D).

4. Conclusions
The following points can be summarized from the above studies;
1. The developed process is energy efficient as it is enables the sintering of tiles at
low temperature of 950C using SHMP binder against the high sintering
temperature 1300-1400C required in the conventional system.
2. The addition of FA in the RMFA system as little as 10 % only sufficient to obtain
the ceramic tiles having impact strength as required in the IS No. 7771970.
3. The major phases in the optimized RMFA 20 are among the calcium aluminum
silicate, iron silicate, potassium titanium oxide and magnetite which are
responsible for observed reinforcement and strength leading to the densification
in the matrix of ceramic tiles for X-ray radiation shielding applications.
4. The scanning electron micrographs shows the rhombohedral shaped crystals of
metal silicate namely calcium aluminum silicate, and the elongated crystal
formation of metals silicate and phosphate in the aggregate. These crystals act
like whiskers enhancing the strength, which acts as reinforcement to the ceramic
matrix and also responsible for providing strength in the sintered tile bodies for
shielding application.
Jeeshan Khan et al. : Mineralogically Formulated Advanced Shielding Ceramics 285

5. Acknowledgments
Jeeshan Khan is obliged to CSIR, India for providing SRF to carry out his research work.
We are highly thankful to Dr. M. Singh, A. Khare, Shafiq M. and Prasanth N. for their
cordial help in characterizations.

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