Light Metals 2006 Edited by Travis J.
Galloway TMS (The Minerals, Metals & Materials Society), 2006
Crystal Growth Modifying Reagents; Nucleation Control Additives or Agglomeration Aids?
James A Counter1
1
Nalco Australia, 2 Anderson St., Botany, NSW, 2019, Australia
Keywords: precipitation, crystallisation, nucleation, agglomeration, precipitation additive
Abstract
Crystal growth modifiers (CGM) are commonly used in the Bayer
process to increase the average gibbsite particle size and improve
the particle size distribution during crystallisation from
supersaturated sodium aluminate solutions. With respect to the
mechanism of action there has been much debate as to whether
this result could be due to the additives aiding agglomeration or
reducing the number of secondary nuclei.
Presented here is work completed on both synthetic and real
Bayer plant liquors, over various experimental conditions in order
to study the mechanism of action of CGM additives.
Crystallisation kinetics, secondary electron microscopy (SEM)
and atomic force microscopy (AFM) data are collated to examine
the impact that these surface active additives have on the
precipitation process.
Introduction
Crystal growth modifiers were introduced to the Bayer industry
over 20 years ago [1] and have gained general acceptance as
additional control tools within the crystallisation section of the
Bayer process. These products have exhibited widespread utility
under high-agglomeration and all-growth precipitation strategies.
The effect of addition of CGM has lead many plants to a reduction
in ultra fines, tougher particles, liquor productivity increases via
either reduced fill temperatures or increased seed charges and
alumina trihydrate coarsening along with many other benefits
using doses ranging from 5-50 ppm.
Three major crystallisation mechanisms, nucleation, growth and
agglomeration of crystals are in action for producing gibbsite as
the preferred phase. The yield of gibbsite is largely determined by
nucleation and growth of particles, while agglomeration is
responsible for producing a coarse crystal of commercial interest.
The effect of optimising the Bayer plant precipitation parameters
in each of these crystallisation scenarios is the most important part
of the entire industrial process. The relationship between the
operating parameters and gibbsite yield has been detailed in a
number of publications over many years [2-6]. Optimum
conditions for maximum yields do not always coincide with
optimum product size specifications, demanded by the smelters.
CGM additives have allowed Bayer plants around the world to
operate under optimum conditions without product size
compromise.
Although there have been a number of recent publications
postulating the CGM mechanism of action, [7-9] there still exists
a degree of uncertainty as to the impact of these programs and
their influence under various agglomeration and secondary
131
nucleation strategies practiced within the industry. The main
thrust of the present studies is to examine the influence of a CGM
on each of the precipitation scenarios in order to better understand
the mechanism of action, leading to further development of new
and improved products.
This paper presents combined work of the impact of CGM on
both synthetic and real Bayer plant liquors under specific
crystallisation scenarios over a temperature range experienced in
industry. Results from a number of experimental techniques are
collated to answer the questions posed by industry and propose a
general mechanism of action for these additives.
Experimental
Synthetic Bayer Liquor Preparation
Pure synthetic, supersaturated sodium aluminate solutions were
used in this investigation. They were prepared from analytical
grade and high purity grade reagents: aluminium trihydroxide,
Al(OH)3, (C31 grade, 0.01% SiO2, 0.004% Fe2O3, 0.15% Ba2O;
ALCOA, Arkansas USA); sodium hydroxide, (99.0% pure, 0.01%
Si, Merck, Australia); Milli-Q water (surface tension 72.8 μNm-1
at 20ºC, specific conductivity < 0.5 μscm-1 and pH = 5.6).
The synthetic liquors used in the crystallisation measurements
were prepared in a 2.5 dm3 well sealed stainless steel digester
immersed in an oil bath at 150ºC. A known mass of NaOH was
dissolved in 1.3 dm3 of Milli-Q water in the digester with an
agitation rate of 250 rpm. This was followed by slow addition of
a known mass of the aluminium trihydroxide. After complete
dissolution of 3 – 4 hours, the solution was transferred to a 2.0
dm3 volumetric flask and made up to the mark with Milli-Q water.
Bayer Plant Liquor Preparation
The Bayer plant liquor experiments were conducted using
reconstituted plant spent liquor. Spent liquor is the term used in
the Bayer process to describe the liquor after the final
classification stage which returns back to digestion. A desired
weight of spent liquor was measured into a stainless steel beaker
and the volume was reduced by evaporation to approximately
30%. To this a set weight of Al(OH)3 solid was added and the
mixture stirred until it was dissolved. This solution was removed
from the hot-plate and placed on a weighing balance and de-
ionised water added until a desired weight was attained. The
pregnant liquor was filtered to remove any insoluble material.
Final liquor composition was such that A/C = 0.66 ± 0.05 where:
A (aluminium hydroxide) = 150 ± 10 g/L of Al2O3
C (total caustic) = 230 ± 10 g/L of Na2CO3
S (soda, total alkali) = 260 ± 10 g/L of Na2CO3

Seed Preparation and Characterization for Agglomeration
Seed used for the agglomeration experiments was the well
characterized Alcoa C31, having BET surface area of 0.381 m2/g
and d(0,1) = 6.3 μm, d(0,5) = 37.1 μm and d(0,9) = 92.3 μm,
determined by a Malvern Mastersizer.
Seed Preparation and Characterization for 2º Nucleation
Broken seed fragments, formed via secondary nucleation, provide
the main source of new crystals in the Bayer process [10,11]. In
this type of secondary nucleation process, fluid shearing action,
crystal-crystal and crystal-vessel wall/impeller blade collisions are
dominantly responsible for removing nuclei from the growing
seed crystal surfaces into solution. It has been stated that particles
> 20 μm in diameter are less likely to agglomerate as they do not
have sufficient surface energy to do so [2]. Therefore in order to
focus on the effect of the CGM additive on secondary nucleation
alone, especially in the early stages of crystallisation it was
necessary to use a large screened seed, high supersaturation, low
seed charge and enough agitation to allow the seed to remain in
the bulk solution, without settling.
Uniform coarse, gibbsite seed crystals were prepared from high
purity Al(OH)3, (C31) by wet screening using both 55 and 90 μm
sieves to give crystals in the size range 30 – 105 μm. These
crystals were then treated with ultra-sonication, followed by
decantation to remove the fine particles (<10 μm). The resulting
product (washed and dried at room temperature in a desiccator)
consisted of agglomerated, pseudo hexagonal-shaped crystals, in
the size range 30 - 100 μm with reasonably smooth surfaces
(Figure 1) and a corresponding BET surface area of 0.1445 m2g-1.
Figure 1. SEM photomicrograph of gibbsite seed crystals for 2º
nucleation experiments.
Batch Crystalliser
A baffled, well sealed, 2.5 dm3, 316 stainless steel vessel was
used for the crystallisation experiments. A central, 4 blade, 45° –
pitch turbine impeller driven by a 70W, multi-speed motor
provided a constant agitation speed at 400 rpm as well as fully
developed axial flow, moderate shear and a high degree of
132
suspension uniformity within the crystallizer. A thermocouple
sensor and a conductivity probe were fitted through the lid of the
crystallizer. The entire vessel was submerged in a 15 dm3,
thermostatically-controlled oil bath, maintaining a constant
temperature to within ± 0.05°C.
The crystal growth modifier used in this study was the
commercially available Nalco product, 7837, unless otherwise
stated.
Models for the Kinetic Study
Quantification of the crystallisation kinetics data produced from
the crystallisation experiments was performed using the semi-
empirical power law model for secondary nucleation and growth
of gibbsite as shown below:
1 dσ
− = k (σ )n (1)
S dt
where σ is the Al(III) relative supersaturation which is defined as
(C – Ce)/Ce, where C and Ce are the instantaneous Al(III)
concentration and Al(III) equilibrium solubility, respectively; S is
the total particle surface area; k is the nucleation rate constant and
n is the reaction order. To quantify the influence of temperature
and estimate the activation energy from the rate constant k, the
Arrhenius expression was used.
⎛ E ⎞ (2)
k = k o exp⎜ − a ⎟
⎝ RT ⎠
where ko is the pre-exponential factor, Ea is the activation energy,
R is the gas constant and T is the absolute temperature.
Atomic Force Microscope (AFM) Measurements
Interaction force measurements between two gibbsite particles
(sphere and prism) were measured using a Nanoscope III Atomic
Force Microscope (Veeco). A gibbsite spherical particle
(hydrated alumina sphere [12]) was glued onto a triangular silicon
nitride cantilever and an aluminium disk with Epikote heat
sensitive resin. Particle interaction forces were measured using a
fluid cell filled with sodium aluminate liquor at 25oC. The
cantilever spring constant, 0.1 Nm-1 was determined using the
Cleveland method [13].
Results and Discussion
Agglomeration Experiments
The majority of plant test work over the last decade has been
completed by simulating agglomeration conditions of the
particular Bayer site. Fine seed charge into pregnant liquor at
high temperature is the standard method for CGM evaluation.
From the work completed here over a temperature range (58-
78ºC) typical to Bayer plants, coarsening of the fine C31 seed was
evident after 18 hours. The results given in Figure 2 below and
taken from the 68ºC test, indicate the increase in the d(0,1) values
with respect to the CGM dose. It is evident that the increase in
particle size and the subsequent decrease in available seed surface
area results in an overall decrease in yield in the isothermal batch
experiment. Therefore in continuous Bayer plant conditions,
process changes are made to increase yield up to a higher level
without size compromise. Table I. Kinetic parameters for seeded gibbsite agglomeration
experiments at 58, 68 and 78oC.
Terms T(°C) Control 7831 7837
52 61 Treated Treated
51 d(0,1)
ko
50 Yield 60.5 58,68,78 1.10 ×105 32.6 ×105 7.78 × 105
(m-2h-1)

Yield g/L
49
d(0,1)

58 2.0 ± 0.2 2.0 ± 0.2 2.0 ± 0.2

48 60 Reaction
68 2.0 ± 0.2 2.0 ± 0.2 2.0 ± 0.2
47 Order (n)
46 59.5 78 2.0 ± 0.2 2.0 ± 0.2 2.0 ± 0.2
45 Ea
61.2 70.3 66.6
44 59 (kJmol-1)
Control 1 3 5

CGM Dosage mg/m2

Figure 2. d(0,1) and yield results for 68ºC agglomeration test.
SEM images given below show the difference between the control
and CGM dosed test at 68ºC. The control, given in Figure 3
below exhibits large amounts of fine particles, yet to be fully
incorporated into the crystal structure of the parent seed. It is
clearly evident that over the 18 hour experiment the CGM
additive has reduced the number of fine particles and achieved a
more robust, block-like hexagonal morphology, under these
conditions.
Higher activation energy means greater sensitivity to temperature
in the presence of the additive. The increase in the pre-
exponential factor of ko indicates the additive aids in increasing
the successful collision rate of fine seed particles during the
agglomeration stage. In this case the product 7831 has a higher ko
possibly indicating a greater successful collision rate than 7837.
Consider the information thus far in terms of the mechanism of
agglomeration put forward by Low [15] and given in Figure 5
below. The action of the CGM additive would be aiding the
cementation process during agglomeration and in terms of
attrition the additive appears to successfully reduce the breakdown
of particles, forming a fully cemented agglomerate, which is
evident in the morphology of the SEM images given in Figure 4.

Individual
particles

Agglomerate
(fully cemented)

Breakdown

Floc (no
cementing)

Figure 3. SEM images of control agglomeration test for 68ºC. Aggregate

(cementing by hydrate deposition)

Figure 5. Mechanism of agglomeration, Low [15].

These tests have only considered one of the possible

crystallisation mechanisms present under Bayer conditions. It
was necessary to perform experiments under nucleating
conditions in order to establish a more conclusive mechanism of
the action of the additive.

Secondary Nucleation Experiments

To investigate the influence of the additive on secondary

Figure 4. SEM images of CGM treated agglomeration test for
68ºC.
Data from the kinetic analysis of this system is given in Table I.
The reaction order at each temperature was found to be n = 2,
corresponding to values reported extensively in literature for
systems under comparable conditions. Activation energies for the
control and CGM additive tests were estimated from Arrhenius
plots. Values fall comfortably in the 53 -83 range reported in the
literature for pure sodium aluminate solutions [3, 6, 14].
nucleation, isothermal batch crystallisation experiments were
carried out over 24 hours. The tests were conducted in pure
synthetic liquors, under constant conditions of NaOH = 4 M,
initial σAl = 1.5, seed surface area = 7.23 m2dm-3 at temperatures
of 60, 65 and 70oC. Results are discussed in terms of new crystal
formation, kinetics and morphology.
New Crystal Formation
The observation of new fine particles (secondary nuclei) in the
size range of 0.1 – 30 μm during all of the crystallisation tests

133
over the first hour are summarised in Table II. There is a marked
difference between the control and treated samples for the 60 and SEM analysis strongly supported the above observations. The
65°C runs, however no discernable difference could be detected images of the product crystals revealed the existence of significant
over the first hour for the higher 70°C temperature run. differences in the development and growth of the new surface
layer and microstructures at the seed crystal surfaces, between the
Table II. Number of new particles generated for all crystallisation control and CGM treated tests. After 4 hours the SEM images for
experiments under constant conditions over the first hour. the control experiments exhibited expected temperature
New Particles < 30 μm dependences. At 60°C only 2° nucleation was observed, at 65°C
T (°C) (1010h-1 per 25 mL) a mixture of 2° nucleation and separate aggregates and at 70°C the
Control With CGM majority of particles formed were separate aggregates. The
60 3.1 1.1 primary crystals were pseudo-hexagonal plates (Figure 7b) which
65 10.1 3.7 agglomerated and grew to secondary crystals with a size range of
70 17.5 18.4 10 – 30 μm. Very few, if any secondary nuclei were found to
attach and grow on the parent seed surface (Figure 7a). In general
The induction times for the appearance of secondary nuclei were for the control solutions it was found that as the isothermal batch
measured by conductivity. At a constant initial σ = 1.5 and seed temperature was increased the aggregation of the small nuclei,
charge of 7.23 m2dm-3 the induction time was found to decrease broken off the parent seed surface, increased. These aggregates
with increasing temperature for both the control and treated are evident in the Figure 7a, with sizes of up to ~30 μm
experiments. However, the induction time was significantly
shorter in the control experiment than in the treated solutions at 60
and 65oC. At 70oC there was no detectable difference in the
induction time measurement for the two scenarios. This
observation would imply that the CGM additive could be
affecting solution speciation and/or crystal surface processes
during the secondary nucleation. It is plausible that the CGM
additive initially deactivated the seed surface to a high extent
resulting in a lengthened time for generating sufficient active sites
for fast growth. The negative effect of additive on the processes
was negated at the higher temperature.
(a)
The net, total crystal surface area with time, is shown in Figure 6
and appears to contradict the number of new particles generated
given in Table II. The control tests displayed a lower total surface
area than that of CGM treated tests at the same temperature,
which would tend to indicate the possible impact of
agglomeration during the crystallisation. However, it is proposed
that initially a larger number of secondary nuclei formed in the
treated solutions and these nuclei immediately were either
adsorbed back on the seed surface or rapidly agglomerated with
each other to form aggregates with a high porosity. This resulted
in a low number and a high net surface area of the crystals.

50
(b)
45
Figure 7. SEM image for the control test after 4 hours at 65ºC.
40 Low (a) and high (b) magnification.
Surface Area (m^2/L)

35
In contrast, the SEM images for the CGM dosed experiments
30
showed that at 60°C only 2° nucleation on the surface was
25 observed, at 65°C a mixture of 2° nucleation and aggregates, but
20 not separate from the parent seed, they had re-adsorbed and at
15 Control at 70C
70°C the majority of particles were secondary nuclei or
CGM treated at 70C aggregates on the seed surface. The primary crystals
10 Control at 65C
CGM treated at 65C
predominately exhibited pseudo-hexagonal plates with some
5 Control at 60C elongated hexagonal shaped crystals produced. The parent seed
CGM treated at 60C
0 surfaces were partly or fully covered by fine particles (Figure 8b).
0 1 2 3 4 5 These particles exhibited stick or needle-like morphology along
Time (hours) with the pseudo-hexagonal plates growing on the surface of seeds.
The size of these primary crystals were in the range of 0.5 – 10
μm, implying quick attachment as soon as the nuclei formed.
Figure 6. The variation of total available surface area for the
crystallising slurry as a function of temperature for seeded, control In the presence of CGM a majority of the fine particles adhered
and CGM treated tests over time. and grew on the seed surface, the degree to which the nuclei

134
remained on the parent seed surface increased with increasing
isothermal batch temperature. The remaining fraction of fine
particles formed aggregates in the bulk solution, with some re-
attaching to the parent seed surface. This is clear evidence for the
observation of the higher net surface area and correlates well with
the lower number of new crystals in the treated systems compared
with the control.
(a)
(b)
Figure 8. SEM image for the CGM dosed test after 4 hours at
65ºC. Low (a) and high (b) magnification.
The conclusion from this evidence is that the involvement of the
CGM additive in the seeded gibbsite crystallisation for all
temperatures not only enhanced the parent seed growth
mechanism, through accelerated secondary nucleation, with less
attrition and hence particle surface roughening but also enhanced
the secondary nuclei agglomeration behaviour.
Kinetics of Secondary Nucleation
As the growth rate of gibbsite is relatively slow when compared
with other inorganic crystals [3,10,16-18] it is feasible to assume
the initial kinetics to be dominated by secondary nucleation at
high σ (> 1.15). Therefore, the birth rate of 3-dimensional nuclei,
reflected in a dramatic crystal population increase, is considered
to far exceed the rate of growth (2-dimensional nucleation
process) of both parent seed crystals and the nuclei [16,17].
The crystallisation kinetics data produced from the seeded
crystallisation at a high initial σ = 1.5 for which secondary
nucleation occurred were analysed. Plots of ln[(-1/S)(dσ/dt)]
versus lnσ for both the control and CGM treated solutions over 4
hours at each of the specific temperatures yielded linear
relationships. The secondary nucleation dominated-reaction order
(n) was derived from the slopes of these plots and reproducibly
found to be equal to 4. The results are summarised in Table III.
Similar values have been reported for secondary nucleation of
gibbsite from sodium aluminate solutions under comparable
conditions [14,19].
135
Table III. Kinetic parameters for seeded gibbsite secondary
nucleation experiments at 60, 65 and 70oC.
Terms T (°C) Control CGM Treated
ko (m-2h-1) 60, 65, 70 3.81 × 1022 4.50 × 1034
60 4.2 ± 0.2 4.1 ± 0.2
React Order (n) 65 3.9 ± 0.2 4.0 ± 0.2
70 4.0 ± 0.2 4.1 ± 0.2
Ea (kJmol-1) 162 ± 30 239 ± 40
Activation energies for gibbsite secondary nucleation for the
control and CGM additive tests were estimated from Arrhenius
plots. Ea values of 162 ± 30 and 239 ± 40 kJmol-1 for secondary
nucleation were calculated for the control and additive tests,
respectively. These values are higher than the 132 ± 15 kJmol–1
reported for secondary nucleation from synthetic sodium
aluminate solutions under similar conditions to the control [19],
but are much closer to the value of 160 kJmol-1, reported in earlier
work [14]. The increase in Ea in the presence of the additive
suggests that more temperature-induced, chemical perturbations
occur in these treated solutions. It is proposed that the additive is
not only involved in the clustering of aluminate ions in
supersaturated sodium aluminate solution but also the interactions
between the clusters and surfaces of seed crystal, which are
responsible for the development of microscopic growth units. As
was the case for the agglomeration work, the pre-exponential
factor of ko was found to be much higher for the CGM treated
gibbsite secondary nucleation than for the control tests. It is
therefore obvious that the successful collision frequency between
the nuclei forming, Al(III) containing species was enhanced by
the presence of additive.
Interaction Forces
The direct interaction forces between two gibbsite particles under
Bayer conditions were measured in-situ and the effect of a crystal
growth modifier determined, using the atomic force microscope
(AFM). Synthetic liquor was prepared containing 4 M NaOH and
σ = 1.5 at 25ºC. The fluid cell was allowed to equilibrate for 20
minutes prior to collection of data.
Initially the interaction force between the gibbsite particles was
first measured in pure sodium aluminate liquor. As illustrated by
the force curves (repeat approaches) in Figure 9, there is only a
small repulsion on approach between the particles, which would
be expected as the electrostatic repulsive forces are screened as a
result of the high ionic strength of the sodium aluminate liquor.
On separation of the surfaces, a very weak adhesive force is
observed. In addition, there appears to be some hysteresis in the
approach and retract curves. This may be a result of the viscous
nature of the solution introducing some hydrodynamic forces into
the system.
The CGM was mixed with the synthetic liquor for 10 minutes
prior to addition into the fluid cell. It is clearly evident the
difference the CGM additive has on the interaction forces by
examining Figure 10. On approach, as for the case in the control
experiment, there was very little interaction. However, upon
separation of the gibbsite surfaces an adhesion is observed that
varies with position on the surface. This is a common observation
in systems where a chemical additive is used that does not form an
even monolayer of coverage.
 A comparison of the interaction between gibbsite particles in the
0.01 control and CGM dosed experiments is illustrated in Figure 11.
On approach there is little difference between the interaction force
curves. The repulsive force is very small and would allow the
0.006
particles to contact each other under normal processing
conditions. On separation however, there is a significant increase
F/R, mN/m

0.002 in the adhesion observed between the gibbsite particles in the

presence of the CGM additive. Under process conditions, the
gibbsite particles would therefore be likely to agglomerate in the
-0.002 0 20 40 60 80
presence of a CGM.

-0.006 Conclusion

In a process where the chemical inclusion of the particle onto the

-0.01 surface of the seed is the rate limiting step and where particles are
Apparent separtion, nm colliding and continually breaking off parent seed crystals, the
addition of CGM may just allow the particle sufficient time to
Figure 9. Interaction forces on approach (filled symbols) and chemically bond with the seed surface and be incorporated into
separation (crosses) between gibbsite particles in-situ at 25oC. the structure. Evidence has been presented here which shows the
increase in the successful collision frequency of not only Al(III)
containing species but also small fractured gibbsite particles and
0.01 fine seed crystals in the presence of the additive.

0.005 Two gibbsite particles will agglomerate if they have sufficient

surface energy to do so and also have sufficient time to allow
0
cementation to take place [2]. It is postulated that the CGM
F/R, mN/m

modified seed surfaces possessed a high surface energy

0 20 40 60 80
interacting with the nuclei strongly with little or no repulsive
-0.005
energy barrier. Therefore to conclude, addition of a CGM
additive induces strong adhesive interaction forces between the
-0.01 gibbsite particles and nuclei, and under specific crystallization
process conditions, this would markedly enhance both
-0.015 agglomeration and coarsening of the particles and also allow for
secondary nucleation control.
-0.02
Apparent separtion, nm References

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