Journal of Critical Reviews

ISSN-2394-5125 Vol 7, Issue 7, 2020

SINTERING BEHAVIOUR OF FINE REACTIVE MGAl2O4 SPINEL POWDER FORMED BY

THE CALCINATION OF MAGNESIUM ALUMINATE HYDRATE POWDER
T. Viswanathan1
1Assistant Professor, Dept. of Chemical Engineering, Karpagam Academy of Higher Education, India.
viswanathan.t@kahedu.edu.in

Received: 17.02.2020 Revised: 03.03.2020 Accepted: 15.04.2020

Abstract
Magnesium aluminate hydrate precursor was made by co-precipitation and the dried powder was calcined in alumina crucibles at
1000°C for 2 hrs. With this calcined powder, different size fractions such as +90 µm, -90 µm and +63 µm, -63 µm and +45 µm, and -45 µm
were separated for body making and green compact pellets were prepared in hydraulic press. The green pellets were sintered in the
range 1500-1650ºC with 2 hrs soaking. Densification studies indicate all the fired pellets have reasonable amount of closed pores due to
abnormal grain growth which halts further densification to a great extent. Closed pores decrease as size of agglomerates decrease at all
firing temperatures and densification gradually improves with reduction of closed pores. Results also reveal the reduction of closed
pores as thickness of pellets decreases from ~0.6cm to ~0.4cm. Fired density of 96.84% theoretical (ƍth) has been achieved with 1.55%
closed porosity in thin pellets made of -45 µm agglomerated spinel powders.
Keywords: Magnesium Aluminate Hydrate, Agglomeration, Spinel Crystallites, Sintered Density, Closed Pores, %Theoretical Density.

© 2020 by Advance Scientific Research. This is an open-access article under the CC BY license (http://creativecommons.org/licenses/by/4.0/)
DOI: http://dx.doi.org/10.31838/jcr.07.07.147

INTRODUCTION
Enormous interest has been created by the interesting ceramic
material MgAl2O4 among scientists for quite some time, and still
it continues to gather attention due to its diverse application
potentials. Among the many important properties of this
advanced ceramic material, some are good mechanical strength
at higher temperatures, unresponsive to chemical attack,
resistant to thermal shock, luminescence property, surface
adsorption, catalytic property, etc. We have done a brief
literature survey of MgAl2O4 compounds [1-24] and presented in
Table 1.

Table 1: Brief literature survey of MgAl2O4 compounds

Sl.
Compound system Properties Applications
No.
Enhanced catalytic stability during steam reforming of
MgAl2O4-SiC Catalytic activity 1
propane [1]
High temperature treat of nano particle
MgAl2O4 Thermal shock resistance[3] 2
compounds
High temperature hot press technique of
Co:MgAl2O4 Saturable absorber for solid state pulse laser operation[4] 3
fabrication
With polymer PVA system exhibit the spray
MgAl2O4 with Si base For spray drying of the ultrasonic-treated suspension [5] 4
drying of the suspension
MgAl2O4 Nano particle solution blending Transparent ceramics with optimized opacity [6] 5
MgAl2O4 with ZnO, TiO2, Best color pigments as function of inorganic precursor
SiO2, ZrO2, SrO, Al2O3, Colour and pigment property composition film-forming polymeric binders, fillers and 6
Y2O3, solvents [7]
MgAl2O4Nanoparticles Surface adsorption Low temperature CO oxidation activity application[10] 7
MgAl2O4 spinel Spinel stabilization Miller indices plan (111) Surface enrichment [11] 8
MgAl2O4:Sm3+ Luminescence property Optical devices –base precursor [12] 9
MgAl2O4 Densification and hydration resistance MgO-CaO refractories [14] 10
MgAl2O4-diethylene
Thermal conductivity Nanofluids [16] 11
glycol
Ni substitution in
Catalytic Property Biogas Reforming for Hydrogen Production [18] 12
MgAl2O4
MgAl2O4 Spinel CO2 Laser Co-Vaporization gives narrow size
Photoluminescence [22] 13
Nanophosphor distribution and well dispersion
Adsorptive material, catalyst support or in Efficient separator for Congo red removal from
MgAl2O4 foam 14
humidity sensors contaminated water [26]
MgAl2O4 Ionic conductivity AC conduction [28] 15
Low crystallite sizes and high specific surface
MgAl2O4-Ca doped Ultrasonic spray pyrolysis [29] 16
area
Olyacrylonitrile nanofibres for 2-chloroethyl ethyl sulfide
MgAl2O4 with MgTiO3 Protective property 17
degradation [35]
Ferromagnetic behaviour, as evidenced by
MgAl2O4 nanoparticles using vibrating sample magnetometer at room Photocatalyst application [36] 18
temperature
MgAl2O4 – Mn doped DC resistivity of material Semiconducting nature of materials [37] 19
Preparation by microwave-resistive hybrid
MgAl2O4 nanoparticles heating showed better transmittance in the IR transparent windows and domes [40] 20
UV-Visible region and in the mid IR region

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 SINTERING BEHAVIOUR OF FINE REACTIVE MGAL 2O4 SPINEL POWDER FORMED BY THE CALCINATION OF
MAGNESIUM ALUMINATE HYDRATE POWDER

Optical ceramic with high homogeneity and high optical

MgAl2O4 Optical property 21
transmission [52]
Cubic structure with high crystallite
MgAl2O4 - Yb3+-doped Spectroscopic applications [56] 22
dispersion
MgAl2O4 with Ni Pigment property To colour product for use in different applications [58] 23
MgAl2O4 - Calcium Oxide Absorbent property CO2 capture from coal power plants [97] 24

Precursor material of spinel has been prepared by numerous
ways viz. spray pyrolysis [25], sol-gel [26],[27], spray drying
[28], and combustion of citrate-nitrate [29], bicarbonate
precursor [30], microwave combustion [31] and co-precipitation
[32-40]. In this work we have prepared magnesium aluminate
hydrate (MAH) precursor powder by co-precipitation technique.
Pellets of the pre-calcined (1000ºC, 2hours) precursor have been
sintered in the range 1500 to 1650ºC and investigated.
EXPERIMENTAL
Preparation of spinel powder by calcination of dried MAH
powder
To get adequate amount of calcined spinel powder for sintering
studies, a bulk co-precipitation was carried out at pH 9.2 and
temperature 30°C. For this purpose, 5000 ml mixed salt solution
of concentration 0.3(M) w.r.t. Al(NO3)3 and 0.15(M) w.r.t.
Mg(NO3)2 was prepared in 10 litre glass beaker. From previous
knowledge, measured amount of 1: 1 ammonia solution was
added with constant stirring to attain pH around 9.0 and later
slowly to achieve pH 9.2. Special care was taken during addition
of ammonia solution so that rate of co-precipitation was
controlled to reduce the size of agglomerated MAH. Even
addition of costly organic additive may have impact on size of
agglomerates, however, that has hardly any effect during
calcination of dried MAH powder to make spinel powders.
After ammonia addition, the co-precipitate gel was stirred for 10
min. The precipitate thus obtained was filtered through What
man No – 41 filter paper kept in perforated plastic basket of
diameter approximately 45cm, and the precipitate was kept for
air drying at room temperature for 72 hrs. The precipitate was
dried at 110°C in glass petri-dishes until weight of the dried mass
was constant. The dried mass was kept in dessicator and agated
into powder. The dried powder was calcined in alumina crucibles
at 1000°C for 2 hrs. This calcined powder was lightly agated to
reduce larger agglomerates and screened through different
sieves viz. 90, 63 and 45 µm. Different size fractions such as +90
µm, -90 µm and +63 µm, -63 µm and +45 µm, and -45 µm were
separated for body making.
Body Making
About 25 gms of each size fraction of agglomerated spinel
powder obtained by calcination was thoroughly mixed with 2
wt% CMC (carboxy methyl cellulose) solution as organic
binder. High carbon steel cylindrical mould of inner diameter
about 2.52 cm was used for green body making by dry pressing
in a hydraulic press (15 Ton Capacity, VB Ceramic Consultants)
at forming pressure 1550 Kgs/cm2. In case of -45µm size fraction,
batch size was 60 gms instead of 25 gms. Four pellets of
thickness ~6 mm were pressed for each size fraction; however,
for -45µm powder another 8 pellets of thickness ~4mm were
made for sintering studies. Green B. D. of each pellet was
measured after drying at 110°C for 24 hours and was calculated
based on loss free basis.
Firing
Four temperatures viz. 1500, 1550, 1600 and 1650°C were
selected for firing the pellets. At each temperature, one thick
(~6mm thickness) pellet for all size fractions and two thin pellets
(~4mm thickness) were fired for 2 hours soaking in a high
temperature muffle furnace with MoSi2 as heating elements.
Heating rate of 5°C/min was maintained up to the firing
temperature. After firing, the pellets were kept for normal
furnace cooling.
Sintered properties of fired pellets
B.D. and %A.P. of each pellet at all firing temperatures i.e. 1500,
1550. 1600 and 1650°C were measured by boiling method. True
specific gravity of stoichiometric spinel powder was determined
by pycnometric method.
Microstructure studies
Scanning Electron Microscope (CARL ZEISS EVO 18 RESERCH)
was used for microstructural studies of calcined spinel powder
and also sintered pellets at all 4 temperatures of firing. EDS
elemental (Mg, Al, O) analysis of sintered pellets at different
temperatures was also done for a few selected samples.
RESULTS & DISCUSSION
Sintered properties of pellets
Sieving by different sieves (Table 2) of 1000ºC 2hrs calcined
powders reveals that size of agglomerates even exceeds 90 µm.
Table 2: Sieve analysis of 1000C/ 2 hours calcined MAH
spine powders formed at pH 9.2 and 30°C
Sieve size (µm) Amount (gms) Weight %
> 90 36.2 19.42
< 90 and > 63 39.4 21.14
< 63 and > 45 42.7 22.91
< 45 68.1 36.53

Table 3: Green B.D. (dried 110°C, 24 hrs) of pellets of MAH based processed (1000°C, 2 hrs)
spinel powder (TSG of spinel powder = 3.578)
Avg. Green
Avg. Green B.D.
Green B.D. Green B.D. (gm/cm3) B.D.
Nature of Powders Wt in gms Thickness in cm Loss Free Basis
(gm/cm3) loss free basis Loss free
(% Theor)
basis
100 wt% (+90 µm 5.852 0.659 1.78 1.77
agglomerated) 5.884 0.67 1.76 1.75 1.76 49.19
4 pellets 5.89 0.663 1.78 1.77
5.891 0.667 1.77 1.76
100 wt% (-90 µm + 5.846 0.647 1.81 1.8
63 µm agglomerated) 5.888 0.656 1.8 1.79 1.81 50.59
4 pellets 5.896 0.649 1.82 1.81
5.864 0.642 1.83 1.82
100 wt% (-63 µm + 5.843 0.63 1.86 1.85

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 SINTERING BEHAVIOUR OF FINE REACTIVE MGAL 2O4 SPINEL POWDER FORMED BY THE CALCINATION OF
MAGNESIUM ALUMINATE HYDRATE POWDER

45 µm agglomerated) 5.859 0.635 1.85 1.84 1.84 51.43

4 pellets 5.832 0.632 1.85 1.84
5.841 0.636 1.84 1.83
100 wt% (-45 µm 5.866 0.612 1.92 1.91
agglomerated) 5.859 0.608 1.93 1.91 1.91 53.38
4 pellets 5.667 0.592 1.92 1.91
5.488 0.567 1.94 1.92
100 wt% (-45 µm 3.882 0.397 1.96 1.94
agglomerated) 3.869 0.4 1.94 1.92
(thin pellets) 3.872 0.396 1.96 1.94
8 pellets 3.848 0.395 1.95 1.93 1.93 53.94
3.876 0.4 1.94 1.92
3.855 0.396 1.95 1.92
3.869 0.396 1.96 1.94
3.878 0.401 1.94 1.92

Effect of agglomeration causes some changes in green
compaction and it has been reflected in green density (Table
3). Which increases with reduction of the size of agglomerates.
Larger agglomerates have inter-granular voids which do not
disintegrate during green forming. -45 µm powders have wider
range of agglomerated grain size distribution which helps
better compaction with increase of % ƍth above 4% as
compared to +90 µm agglomerated grains. The effect of
agglomeration causes remarkable change in densification
(Table 4).

Table 4: Fired properties of sintered pellets of MAH based processed spinel powders (TSG = 3.578)
Fired properties (2
Green B. D. Loss Sintering
Nature of Powders hrs soaking) B.D. % A.P. % T.P. % C.P.
free basis Temp. (°C)
gm/cm3
100 wt% (+90 µm 1.77 1500 2.86 15.16 20.07 4.91
agglomerated) 1.75 1550 2.98 8.08 16.71 8.63
4 pellets 1.77 1600 3.08 4.50 13.92 9.42
1.76 1650 3.12 3.00 12.80 9.8
100 wt% (-90 µm + 63 µm 1.80 1500 2.92 14.08 18.39 4.31
agglomerated) 1.79 1550 3.01 8.05 15.87 7.82
4 pellets 1.81 1600 3.09 5.04 13.64 8.6
1.82 1650 3.14 3.34 12.24 8.9
100 wt% (-63 µm + 45 µm 1.85 1500 2.97 13.79 16.99 3.2
agglomerated) 1.84 1550 3.06 8.08 14.48 6.4
4 pellets 1.84 1600 3.11 5.18 13.08 7.9
1.83 1650 3.16 3.48 11.68 8.2
100 wt% (-45 µm 1.91 1500 3.04 11.44 15.04 3.6
agglomerated) 1.91 1550 3.13 7.12 12.52 5.4
4 pellets 1.91 1600 3.22 4.21 10.01 5.8
1.92 1650 3.32 1.01 7.21 6.2
100 wt% (-45 µm 1.94 1500 3.16 9.70 11.68 1.98
agglomerated) 1.92 1500 3.17 9.66 11.40 1.74
(thin pellets) 1.94 1550 3.27 5.93 8.61 2.68
8 pellets 1.93 1550 3.28 5.47 8.33 2.86
1.92 1600 3.38 3.29 5.53 2.24
1.92 1600 3.4 2.30 4.97 2.67
1.94 1650 3.46 1.65 3.30 1.65
1.92 1650 3.47 1.56 3.02 1.46

during firing at all temperatures in the range 1500 to 1650°C of closed pores due to abnormal grain growth which halts
for 2 hrs soaking. All the fired pellets have reasonable amount further densification to a great extent. Results (Table 5).

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 SINTERING BEHAVIOUR OF FINE REACTIVE MGAL 2O4 SPINEL POWDER FORMED BY THE CALCINATION OF
MAGNESIUM ALUMINATE HYDRATE POWDER

Table 5: Variation of sintered density (% ƍth) and %Closed Pores of agglomerated spinel powders with size of agglomerates
and pellet thickness of sintered pellets at different temperatures with 2 hrs soaking (True Specific Gravity 3.578)
Size of Pellet Sintered density (% ƍth) % Closed Pores
agglomerates Thickness 1500°C 1550°C 1600°C 1650°C 1500°C 1550°C 1600°C 1650°C
in µm in cm
> 90 ~ 0.6 79.93 83.29 86.08 87.2 4.91 8.63 9.42 9.81
< 90 and > 63 ~ 0.6 81.41 84.13 86.36 87.76 4.31 7.82 8.6 8.92
< 63 and > 45 ~ 0.6 83.01 85.52 86.92 88.32 3.2 6.4 7.9 8.23
< 45 ~ 0.6 84.96 87.48 89.99 92.79 3.6 5.4 5.8 6.22
< 45 ~ 0.4 88.46 91.53 94.8 96.84 1.86 2.77 2.45 1.55

Indicate that % C.P. decrease as size of agglomerates decrease at

all firing temperatures and densification gradually improves with
reduction of closed pores.
Results also reveal the reduction of closed pores as thickness of
pellets decreases from ~0.6cm to ~0.4cm. Fired density of
96.84% ƍth has been achieved with 1.55% closed porosity in thin
pellets made of -45 µm agglomerated spinel powders.

SEM analysis a) 1500°C top surface of thick pellet;

Here grain boundaries and smaller grains are not distinct; it
seems the presence of loosely packed smaller agglomerates on
the surface of larger grains. Grain size of 1650°C, 2hrs sintered
pellet (top surface) varies from submicron to a few microns in
size (Figure 2b)

Figure 1: SEM of MAH calcined highly agglomerated spinel

powder at 1000°C, 2hrs formed at pH 9.2 and 30°C – a) large
agglomerate of size +90µm; b) 1650°C SEM micrograph of top surface of thick pellet;

Figure 1a shows large cluster formation (+ 90 µm) having a large and grain boundaries and grain surfaces are distinct. This uneven
number of pores due to agglomeration of nano size spinel grain size distribution causes entrapment of pores (closed pores)
crystallites. In case of ground (agated for 30 minutes) spinel which are evident in the fractured surface of 1650°C sintered
powders (Figure 1b) pellet (Figure 2d).

c) 1650°C top surface of thin pellet

b) Milled agglomerate of smaller size.
Thin pellet (1650°C, 2hrs) shows dense microstructure (Figure
2c)
Size of agglomerates reduces submicron to a few µm in size.
Existence of individual nano spinel crystallites is also viewed in
the microphotographs. Due to agglomeration, some bigger inter-
granular pores are also formed during green forming. These
agglomerates cause abnormal grain growth and many pores are
entrapped creating closed pores during firing. Theses closed
pores hinders densification during sintering. Top surface of
1500°C, 2hrs sintered pellet is viewed in Figure 2a.

d) 1650°C fracture surface of thick pellet

Figure 2: SEM of co-precipitated MAH based sintered spinel
pellets –

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 SINTERING BEHAVIOUR OF FINE REACTIVE MGAL 2O4 SPINEL POWDER FORMED BY THE CALCINATION OF
MAGNESIUM ALUMINATE HYDRATE POWDER

having narrow grain size distribution (1 to 6 µm approximately)

and achieved sintered density 96.84% ƍth having restricted close EDS elemental analysis
pores to 1.55%.

Table 6: EDS elemental (Mg, Al, O) analysis of sintered spinel pellet formed by MAH calcined (1000°C, 2hrs) spinel powders by
SEM
Stooichiometric Calculated
Wt% Al2O3 (chemical estimation by
spinel sintered at
Element Wt% At% Molar ratio MgO: Wt% wet chemical method of MAH at pH
different
Al2O3 Al2O3 9.2 and 30°C
temperatures
OK 47.41 59.34
1500°C MgK 16.19 13.54 1.0: 1.0015 72.13 72.17
AlK 36.49 27.12
OK 49.77 61.74
1600°C MgK 15.82 12.92 1.0: 0.9797 71.42 72.17
AlK 34.41 25.32
OK 57.36 68.69
1650°C MgK 13.22 10.42 1.0: 1.0024 71.88 72.17
AlK 29.42 20.89

(Table 6) of sintered pellets reveals compositional homogeneity
of co-precipitation process having molar ratio of MgO: Al2O3 in
the very close range of 1: 1 when all process parameters viz. pH
and temperature are maintained same in scaled up batches of
5000 ml mixed solution from 100ml batch. This process can also
be scaled up as per the requirement of the industries.
CONCLUSIONS
Agglomeration causes some change in green compaction and the
effect is seen in green density which increases with reduction of
the size of agglomerates. Further, agglomeration causes notable
change in densification during firing in the temperature range
1500 to 1650°C for 2 hours soaking. All the fired pellets have
closed pores due to abnormal grain growth which halts further
densification to a great extent. Closed pores decrease as size of
agglomerates decrease at all firing temperatures and
densification gradually improves with reduction of closed pores.
Results also reveal the reduction of closed pores as thickness of
pellets decreases from ~0.6cm to ~0.4cm. Fired density of
96.84% ƍth has been achieved with 1.55% closed porosity in thin
pellets made of -45 µm agglomerated spinel powders.
ACKNOWLEDGMENTS
The funding provided by DST-SERB (Govt. of India) under project
scheme (SB/FT/CS-076/2013) to carry out the work is highly
appreciated and thanked. Important discussions and advice by
Dr. P.G. Pal (Retd. Professor, Govt. College of Engineering &
Ceramic Technology, Kolkata) is acknowledged highly.
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 SINTERING BEHAVIOUR OF FINE REACTIVE MGAL 2O4 SPINEL POWDER FORMED BY THE CALCINATION OF
MAGNESIUM ALUMINATE HYDRATE POWDER

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