028 2016

R. Sarkar*, A.D. Samant*

Study on the Effect of Deflocculant Variation in High-Alumina

Low-Cement Castable
R. Sarkar*, A.D. Samant* components of the system that are exposed to the
KEYWORDS: deflocculants, type and amount; castable; properties
environment of above 10,000 a [2]; but in actual application,
Study on the Effect of Deflocculant refractories are used at much higher temperatures. Again as
» Refractories Manual (2016)
Variation in High-Alumina Low- per physical form refractories are of two types, namely,
shaped and unshaped refractories. Unshaped or monolithic
Cement Castable AUTHOR ABSTRACT
refractories are easier and cheaper to install, can take any
shape or size, have lesser number of joints (thus reducing
The corresponding author, Dr. Ritwik Sarkar, Associate The effect of three different types of deflocculants and their amounts on
corrosion), better volume stability and good spalling
Professor, NIT, Rourkela, India, has more than 15 years of high-alumina low-cement castables is studied. Castable formulations
resistance.
experience in ceramics and refractories in different or- were done as per continuous particle size distribution of a Dinger-Funk
In practice, the maximum use of unshaped refractories is in
ganizations, like IFGL Refractories Ltd., IFGL Bioceramics model using a distribution coefficient of q = 0.21. Castable compositions
the form of castables (where a simple casting technique is
Ltd., CG & CRI, R&D of ACC Ltd., and H&R Johnson Ltd., were processed as per conventional processing techniques and varia-
used for shaping a slurry mix) and in most cases the bond
all in India, and at the IKKM, RWTH Aachen, Germany tion in properties were evaluated regarding flowability of the mix and
material is calcium aluminate cement. The presence of lime
The corresponding(DAAD Fellowship).
author, He has
Dr. Ritwik received
Sarkar, various awards
Associate in densification and strength development after drying and firing at 900
in cement is detrimental to high-temperature properties and
his career for academic excellence and his contributions to Ceramics
Professor, NIT, Rourkela, India, has more than 15 years of
and and 1500 °C. Phase analysis of the matrix phase was also done for the
Materials Science, including the Young Scientist Award. A life minimum
member of use1500of°C compositions
cement without much the
to evaluate affect
phaseonformations
other at high tempera-
experience in ceramics and refractories in different properties was achieved by the introduction of ultrafine (<1dispersant was found
the Indian Ceramic Society and Indian Institute of Ceramics,
organizations, like IFGL Refractories Ltd., IFGL Bioceramics
Dr. Sarkar has ture in the presence of cement. The alumina-based
more than 130 research publications and 9 patents to his credit. μm) particles
Ltd., CG & CRI, R&D of ACC Ltd., and H&R Johnson Ltd.,
suchresulted
to have as fumein silica
betterand reactivein alumina
properties [3–
the castable.
E-Mail: ritwiksarkar@rediffmail.com 4]. These ultrafine particles enhanced the packing and help
all in India, and at the IKKM, RWTH Aachen, Germany to formulate low cement and ultralow cement castables
(DAAD Fellowship). He has received various awards in his (depending on cement content) with improved properties
career for academic excellence and his contributions to than that of the traditional cement-containing castables [3–
Ceramics and Materials Science, including the Young 7]. Reduction in cement and increase in fine particle content
1. Introduction
Scientist Award. A life member of the Indian Ceramic
Society and Indian Institute of Ceramics, Dr. Sarkar has
important
reduced the [9–12]. of
water demand Forthe
a properly dispersed
castables, whichsystem,
affects high flowability even
Ceramics is a modern, dynamic and diversified field having its the rootsflow
in andat dispersion
low water content
properties is achievable with other
of the castables. Hencesuperior
a properties before
more than 130 research publications and 9 patents to his
ancient technology that is more than 24,000 years old [1]. Amongst dif- and after firing.
new class of additive, termed as ‘rheology modifiers’ came
credit.
ferent classes of ceramics, refractories are materials whose chemical into and To make
use, which is the refractory
essential for castable slurry dispersed
the development and flowable at reduced
of the
E-Mail:
physicalritwiksarkar@rediffmail.com
properties make them applicable for structures or as components water content,
above castables. They the additives
control the used
flow are called deflocculants
behaviour of a or dispersants.
_____________________________________________
of the system that are exposed to the environment of above 10,000 a [2]; and
castable The better
make the thedispersion,
installation theprocess
higher the slurryand
easier flowability at lower wa-
* Department
but in actual ofapplication,
Ceramic Engineering,
refractories areNational
used at Institute
much higher of tempera- ter content,
faster, resulting hence
in better the better
physical, the packing
mechanical and and the better the properties.
thermo-
Technology, Rourkela (India)
tures. Again as per physical form refractories are of two types, mechanical namely, But a very high
properties [8].flowable
Several mass studiesmayhave
indicate
shown higher
thatsphericity of particles
shaped and unshaped refractories. Unshaped or monolithic refractories for better or flowuse properties,
of a higher amount of dispersant
the dispersion of a orcastable
higher water level, resulting
ABSTRACT
are easier and cheaper to install, can take any shape or size, havesystem lesser (especially
in lower strength
the matrix and other
part properties.
containingDeflocculants
the fine work based on the
Thenumber
effect ofof joints
three (thus reducing
different types corrosion), better and
of deflocculants volumetheirstability and iselectrosteric
particles) very important mechanism,
[9–12]. Forwhere charged dispersed
a properly molecules from dispersant get
good spalling
amounts resistance. low-cement castables is studied. system, high
on high-alumina adsorbed on the even
flowability refractoryat particles
low water to form a stericis and electrical double
content
In practice, the maximum
Castable formulations were doneuse ofasunshaped refractories
per continuous is in theachievable
particle form of layer.with Double layers of properties
other superior two differentbeforerefractory
and particles
after create a repulsive
castables
size (where
distribution of aa simple castingmodel
Dinger-Funk technique
usingis aused for shaping firing.
distribution a slurry force that is sufficiently strong to overcome the attractive van der Waals
mix) and inofmost
coefficient q =cases the bond
0.21. material
Castable is calcium aluminate
compositions were cement.
To make forces. Thus the particles
the refractory castableremainslurryin adispersed
repulsive dispersed
and state and retain
The presence
processed as perof lime in cement isprocessing
conventional detrimentaltechniques
to high-temperature
and prop- the flowable character. Again the
flowable at reduced water content, the additives used are
excessive use of these additives may
erties and
variation minimum use
in properties were of cement
evaluated without muchflowability
regarding affect on other prop- cause excessive adhesion of
called deflocculants or dispersants. The better the
charged molecules resulting in a reduced
of erties
the mixwasand achieved by the and
densification introduction of ultrafine (<1
strength development afterμm) particles double layer thickness or excessive
dispersion, the higher the slurry flowability at lower water
increase in a double layer that may
such and
drying as fume
firingsilica andand
at 900 reactive
1500alumina
°C. Phase[3–4]. These of
analysis ultrafine
the particles entrap a considerable amount of
content, hence the better the packing and the better the
water and thus negatively affect the flow
enhanced
matrix phasethe waspacking
also doneand for
helptheto1500
formulate low cementtoand ultralow behaviour [13].
°C compositions properties. But a very high flowable mass may indicate
cement the
evaluate castables
phase(depending
formationsonatcement content) within improved
high temperature the prop- The industrial production of refractory castables started almost 85 years
higher sphericity of particles or use of a higher amount of
erties than
presence of that
cement.of theThetraditional cement-containing
alumina-based dispersant castables
was [3–7]. ago in the United States and later on in Japan [8] and so the develop-
dispersant or higher water level, resulting in lower strength
Reduction
found to haveinresulted
cement inand increase
better in fineinparticle
properties content reduced the mental activity on this material is also quiet strong. The use of defloccu-
the castable. and other properties. Deflocculants work based on the
water demand of the castables, which affects the flow and dispersion lants for the betterment of the properties of the castables has been stud-
properties of the castables. Hence a new class of additive, termedelectrosteric
KEYWORDS as ‘rhe- iedmechanism,
for a long time, where charged molecules from
and many research works are available in that area
dispersant get adsorbed on the refractory particles to form a
ology modifiers’
deflocculants, typecame
and into use, which
amount, is essential
castable, propertiesfor the development of [14–22]. The main deflocculants that are studied for refractory castable
steric and electrical double layer. Double layers of two
the above castables. They control the flow behaviour of a castable and systems are sodium polyphosphates [23–31] and polyacrylates [24, 26,
make the installation process easier and faster, resulting in different
better phys- refractory particles create a repulsive force that is
1. Introduction
ical, mechanical and thermo-mechanical properties [8]. Several studies strong to overcome the attractive van der Waals
Ceramics is a modern, dynamic and diversified field having
sufficiently
have shown that for better flow properties, the dispersion of a castable forces. Thus the particles remain in a repulsive dispersed
its roots in ancient technology that is more than 24,000 * Department of Ceramic Engineering, National Institute of Technology, Rourkela (India)
system (especially the matrix part containing the fine particles)state and retain the flowable character. Again the excessive
is very
years old [1]. Amongst different classes of ceramics, use of these additives may cause excessive adhesion of
refractories are materials whose chemical and physical charged molecules resulting in a reduced double layer
properties make them applicable for structures or as
REVIEW PAPERS 029

Table 1 · Details of the different starting materials

Constituent WTA grain WFA grain Alumina fines Fume silica HAC
SiO2 0.03 0.1 0.03 96.2 0.21
Al2O3 99.34 98.93 99.3 0.4 71.64
Fe2O3 0.035 0.06 0.03 0.1 0.11
TiO2 - Trace Trace - -
CaO - 0.1 0.02 0.2 26.91
MgO - - 0.01 0.1 0.32
Na2O + K 2O 0.15 0.4 0.1 0.4 0.27
Property WTA grain WFA grain Alumina fines Fume silica HAC
Particle size / μm - - D50 = 2.5 >99 % <45 -
Bulk density / g/cm3 3.61 3.77 - - -
Apparent porosity / % 3.93 1.8 - - -
Sp. Surface area - - 3.1 m2/gm 20 m2/gm 4400 cm2/gm
Phase analysis Corundum Corundum Corundum Amorphous CA2, CA

Table 2 · Details of the batches

Batch code Deflocculant’s chemical name Amount used / mass-%
D-C 0.3 0.3
Ammonium Polymethacrylate
D-C 0.5 0.5
Shmp 0.3 0.3
Sodium Hexametaphosphate
Shmp 0.5 0.5
A 0.3 Alumina Dispersant Summer + 0.3 + 0.3
A 0.5 Alumina Dispersed Winter 0.5 + 0.5

32–33], polycarboxylate ethers [17, 27, 34–36], dispersing alumina
[37–40] and their amounts [41–45]. However, most of the studies were
based on the available or industrially practised castable formulations
and did not have much theoretical base on the particle size distribution
(PSD). It has already been established for a long time (since about 1930)
that PSD is also a very influential tool for the flowability of a granular
slurry. Andreasen [46–47] proposed that a continuous PSD allows the
flowability in a granular mix along with its compaction, whereas a com-
monly practised discrete PSD only results in a compact mix with very
poor flowability. The formula as proposed by Andreasen to calculate the
continuous PSD of a granular system was further modified by Dinger and
Funk [48–50] and this modified formula is also practically viable.
In the present work, the effect of three different deflocculants at two
different concentrations was studied on the high-alumina low-cement
castable, formulated as per the Dinger and Funk formula with a distri-
bution co-efficient of 0.21. Castables were processed conventionally
and evaluated for flowability properties during casting, and density and
strength development at different temperatures.
2. Experimental
High-alumina low-cement castables were prepared using white tabular
alumina (WTA) (Almatis /IN), white fused alumina (WFA) (Chinese source)
grains/aggregates, alumina fines (Almatis/IN), high-alumina cement
(HAC) (Almatis /IN) and silica fume (Elkem/IN). Deflocculants used for this
study are polyacrylate-based (Vanderbilt Minerals, Norwalk, US), phos-
phate-based (Loba Chemie, India) and alumina-based (Almatis, India)
ones. Details of the physico-chemical properties of the starting materials
are provided in Table 1. All the raw materials were weighed as per the
weight fractions as calculated from PSD obtained from the Dinger and
Funk formula and as shown in Fig. 1. Six different castable batches were
prepared to contain 4 mass-% HAC and 5 mass-% fume silica for these
three different deflocculants used at two different percentages. Details of
the batch variations are shown in Table 2. Citric acid (0.1 mass-%) and
polypropylene fibers (0.05 mass-%) were also used as a set retarder and
organic fibre in the castable compositions. All the castable batches were
processed under similar conditions.
First, all the raw materials were dry mixed in a planetary mixer (Ho-
bart/UK, model N50), then water was added to the mix to attain proper
consistency. Around 6 vol.- to mass-% (6 cm3 per 100 g batch) of water
was required to attain the proper consistency. Mixed compositions were
then characterized for flowability measurement, using a flow cup, as per
Fang et al. [51]. Mixed castable compositions were placed in the cup,
then the filled cup was placed on a vibrating table (AIMIL, India) with
3200–3600 vibrations per min (vpm) and an amplitude of 0.5mm and
then allowed to vibrate on for 30 s after drawing the only cup upward.
Measurement of flow (dimension of spread material) was done in eight
different directions and the average value was presented. Next, the
 D-C 0.5 0.5
Shmp 0.3 Sodium Hexametaphosphate 0.3
Shmp 0.5 0.5
030 A 0.3 Alumina Dispersant Summer + 20160.3 + 0.3
A 0.5 Alumina Dispersed Winter 0.5 + 0.5

mixed batches were poured into lubricated iron moulds of dimensionFig. 11

50 mm3. The excess mix was scraped off and smoothed by a trowel. The
mixes were kept within the mould for 24 h in humid conditions. Then the
molds were loosened and the cast samples were demolded and allowed
to air dry for 24 h followed by oven drying at 110 °C/24 h. The dried sam-
ples were then fired at 900 and 1500 °C with 2 h soaking time at peak

CPFT / mass-%
temperatures. All the firings were done in electrical resistance furnace
(Bysakh & Co., India, make).
Dried and fired samples were characterized for bulk density (BD) and
cold crushing strength (CCS). The characterizations were done as per
Bureau of Indian Standard (BIS) specifications, IS 10570, reaffirmed in
2002. Each datum represented here is an average of six individual mea-
surements. Phase analysis study of the matrix part of the 1500 °C fired
samples was also done to evaluate the reactions that have occurred
during firing. Only the matrix phase was selected to avoid the interfer-
ence of the main granular corundum phase so that minute phases that
might have formed due to reaction at high temperatures in the matrix Alumina particle size / mm
phase can be traced out. The phase analysis study was carried out in an
X-ray diffractometer (Multipurpose X-Ray Diffraction System, Rigaku Fig.1 • Particle size distribution plot of the castables, with distribution co-
Japan, make, model Ultima-IV), with Cu-Kα1 radiation with a scanning efficient 0.21
rate of 10 ° per min. The whole experimental process used in the study is
shown in Fig. 2, as a flow diagram.
dehydroxylation of the cement hydrate phase (loss of chemically bonded
water), resulting in a loss of mass and lower density values. Again BD
3. Results and discussions values were found to increase at 1500 °C due to sintering at high tem-
Physico-chemical properties of the starting raw materials indicate peratures. A relatively sharp rise in density values was observed for the
(Table 1) that the materials are pure and contain a very minimum amount alumina dispersants at 1500 °C, which may be due to the formation of
of impurities. Figure 1 shows the PSD plot of the castables formulated in nascent or reactive alumina in the castable composition from the defloc-
the form of cumulative percent finer than (CPFT) of a particular size of culant that has further enhanced the densification.
particle against particle size with the value of q = 0.21. The highest par-
ticle size used is 3 mm, which shows 100 % CPFT value and the minimum 3.3 Strength study
particle size is ~1 μm, which shows 0 % CPFT. There is a gradual decrease Strength, in terms of CCS values of different castables, are shown in Fig. 5.
in the slope with reducing particle size range and sudden change in the It is observed that higher deflocculant-containing compositions showed
slope of the plot below 0.3 mm size due high fines content (38.67 mass-%) greater strength, possibly associated with the better flow, compaction
in the formulation. and densification in the compositions. Degradation of strength at 900 °C
was observed for all the compositions, which may be associated with the
3.1 Flowability value dehydroxylation of the cement hydrate phase (loss of chemically bond-
Flow values during casting of all the castables were compared at similar ed water), resulting in a bond rupturing of the cement hydrate bonds.
water content (~6 mass- to vol.-%) and under similar conditions. The The presence of hydraulic bonds at dried condition (110 °C) has shown
flow values, as shown in Fig. 3, indicate that increase in deflocculant con- greater strength compared to the 900 °C fired ones. Again increase in
tent increases the flow value for all the different deflocculants. Improved temperature to 1500 °C results in sintering and formation of ceramic
dispersion with increasing amount of dispersant was observed for all the bonds in the compositions and enhances the strength values. Alumina
deflocculant types in the experimental range. No segregation of grains dispersants showed higher strength values at 1500 °C, possibly due to
and fines and also water was observed. Again the alumina-based disper- better sintering from nascent alumina present in the compositions at
sant was found to result in better flow characteristics. high temperatures.

3.2 Densification study 3.4 Phase analysis

Density values of different castables are shown in Fig. 4. It is observed
that compositions with 0.5 mass-% of deflocculant showed higher val-
ues compared to that of 0.3 mass%-containing compositions for all the
deflocculants. The higher amount of deflocculant has increased the flow-
ability of the castable slurry, resulting in better compaction of the ma-
terial and producing higher density values. At 900 °C there is a decrease
in the density values for all of the compositions. This may be due to the
There is no variation in the phase content of the different compositions
fired at 1500 °C, as shown in Fig. 6. The deflocculants are mostly organ-
ic-based materials and are used in a very low percentage in the compo-
sition. Hence they do not affect the phase content. All the compositions
showed corundum as the major phase with anorthite and grosite as the
minor ones. Formation of anorthite (CaO•Al2O3•2SiO2) in the composi-
tions may be due to the reaction:
REVIEW PAPERS 031

2
Al2O3 grains and fines +
Cement bonded (CAC) +
Fume Silica

Weighed

Mixing Water addition

By Hobart's Particle
mixer (20 min) Deflocculant added

Viscous mass was casted in a mold

Tapping using Vibrating platform

Demolding (after 1 day)

Air drying (1day)

Drying (110 °C/24 h)

Weight and dimensions observed

Cold crushing Fired at 900 °C Fired at 1500 °C

strength (CCS) (1 h soaking time) (1 h soaking time)
6 samples

Weight and dimensions observed Weight and dimensions observed

CCS CCS
6 samples 6 samples

XRD analysis

Fig.2 • Flow diagram of the process used

Fig. 3
3
Flow value / mm

0.3 mass-% 0.5 mass-% 0.3 mass-% 0.5 mass-% 0.3 mass-% 0.5 mass-%

Fig.3 • Variation of the flow values of different batches

Fig. 4
032 2016

Fig.54
Fig.
4
D-C 0.5 mass-% D-C 0.3 mass-%
Fig.44
Fig. SHMP 0.5 mass-% SHMP 0.3 mass-%
ADS ADW 0.5 mass-% ADS ADW 0.3 mass-%
Bulk density / g/cm3

110 900 1500

Temperature / °
Fig.4 • Variation ofFig.
the bulk
5 density values of different batches heat treated at different temperatures

5 Fig.55
Fig.
D-C 0.5 mass-% D-C 0.3 mass-%
SHMP 0.5 mass-% SHMP 0.3 mass-%
ADS ADW 0.5 mass-% ADS ADW 0.3 mass-%
CCS / MPa

110 900 1500

Temperature / °
Fig.5 • Variation of the CCS values of different batches heat treated at different temperatures

CaO ·Al2O3/CaO·2Al2O3 + SiO2 → CaO·Al2O3 ·2SiO2 (Anorthite) Grossite
(CaO 2Al2O3) may be formed due to the reaction between CA phase pres-
ent in the cement with fine alumina in the matrix phase:
CaO · Al2O3 + Al2O3 → CaO ·2Al2O3
4. Conclusions
 Six different castable compositions were formulated and cast with dis-
tribution co-efficient 0.21 using three different types of deflocculants
at two different percentages.
 An alumina-based dispersant and higher amount of deflocculant
showed better dispersion and higher flow values.
 Densification and strength values were found to be higher for the alu-
mina dispersant, and also for higher dispersant amounts, which is asso-
ciated with the greater flowability and compaction of the composition.
 In phase analysis grossite and anorthite phases were observed other
than the major corundum phase. The minor phases are the reaction
products in the matrix phase of the castables, due to reactions between
cement and fine alumina, and cement and fume silica respectively.
5. Acknowledgments
The authors are thankful to Mr S. Mukherjee and Mr S. Chatterjee of Al-
matis, India for their support regarding the materials used, and staff of
the Department of Ceramic Engineering, NIT Rourkela for their help and
facilities during the work.
REVIEW PAPERS 033

Fig. 6
6

Batch-
Darvan C
0.5 mass-%
Intensity / a.u.

Batch-
SHMP
0.5 mass-%

Batch-
ADS ADW
0.5 mass-%

2θ / °
Fig.6 • Phase analysis of the castable compositions containing 0.5 mass-% deflocculants fired at 1500 °C

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