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Powder Technology 173 (2007) 203 210

www.elsevier.com/locate/powtec

Effect of energy density, pH and temperature on de-aggregation


in nano-particles/water suspensions in high shear mixer
A.W. Pacek , P. Ding, A.T. Utomo
School of Chemical Engineering, University of Birmingham, Edgbaston, Birmingham, B15 2TT, United Kingdom
Received 22 May 2006; received in revised form 16 November 2006; accepted 3 January 2007
Available online 16 January 2007

Abstract
The effect of energy input, pH and temperature on de-aggregation of hydrophilic silicon dioxide powder (particle size 12 nm) in a high
shear mixer was investigated. It has been found that de-aggregation is a two step process. Initially, at low energy input very large aggregates
(31000 m) are gradually broken into smaller secondary aggregates (2100 m) of a single modal size distributions. As the energy input
increases primary aggregates (0.031 m) are eroded from the secondary aggregates leading to bimodal size distributions with the first mode
between 0.03 m and 1 m corresponding to the primary aggregates and the second mode between 2 m and 100 m corresponding to the
secondary aggregates. At a sufficiently high energy density all secondary aggregates are broken into primary aggregates however, even at the
highest energy density employed the primary aggregates could not be broken into single nano-particles. The temperature and the pH affect deaggregation kinetics but do not alter de-aggregation pattern. Increasing pH at low temperature speeds up de-aggregation, whilst increasing pH
at high temperature slows down de-aggregation process.
2007 Elsevier B.V. All rights reserved.
Keywords: Silica nano-particles; Suspensions; De-aggregation; Primary aggregates; Secondary aggregates; Energy density

1. Introduction
Nano-particles such as titanium, aluminium or silicon oxides
have wide industrial applications in manufacturing of pigments,
fillers, ceramics, catalysts as well as electromagnetic and optical
devices. In the majority of those applications nano-particles are
processed as suspensions in different aqueous solutions and
frequently the quality of final products depends on the
properties of these suspensions characterized by the particle
size, size distribution, shape and morphology [1]. Therefore,
nano-particles which are often supplied in the form of dry
powders have to be re-dispersed in aqueous solutions to give
homogenous, stable dispersions and it is essential that the
aggregates inherently present in dry nano-powders are broken
into primary nano-particles during dispersion process.
Large aggregates suspended in a fluid are broken when the
hydrodynamic forces (determined by the flow field) exceed the
cohesive bonds between particles or smaller aggregates. The
strength of individual bonds depends on the type of nano Corresponding author.
E-mail address: A.W.Pacek@bham.ac.uk (A.W. Pacek).
0032-5910/$ - see front matter 2007 Elsevier B.V. All rights reserved.
doi:10.1016/j.powtec.2007.01.006

particles (van der Waals interactions), surface properties


(wettability, electrostatic interactions) and the nature of liquid
bridges within an aggregate [2].
Aggregates can be broken by normal or shear stress by
erosion, e.g., a gradual removal of small fragments from the
aggregates periphery or by bulk rupture, e.g., an abrupt
breakage of the aggregates into a number of relatively large
fragments [3]. The mechanism of breakage depends on the size
of the aggregates and the energy intensity [4]. It has been
postulated that as erosion occurs at low energy intensity and as
the energy intensity increases particles are broken by fragmentation [5]. As the aggregates become smaller during deaggregation, surface forces become more important than mass
forces and for aggregates smaller than 1 m, surface forces are
more than one million times larger than mass force [6].
Therefore, breakage of large aggregates is relatively simple,
whereas breakage of aggregates smaller than 1 m might be
very difficult and it has been suggested that the particles smaller
than 10 to 100 nm cannot be broken by mechanical action [7].
Dispersion and de-aggregation of nano-powders in liquids
can be carried out in ball mills, ultrasonic processors and rotor
stator high shear mixers. The kinetic of de-aggregation in a high

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A.W. Pacek et al. / Powder Technology 173 (2007) 203210

shear mixer is relatively easy to control and such devices are


frequently used in industry to produce different types of
suspensions. Therefore, in this work the effect of energy input,
pH and temperature on de-aggregation of silica nano-particles
in a Silverson high shear mixer has been investigated and the
results are discussed below.
2. Experimental
2.1. Materials
A hydrophilic fumed silicon dioxide (Aerosil 200 V from
Degussa) was supplied as a dry powder. The primary particles
have density of 2200 kg/m3, SiO2 content higher than 99.8%,
specific surface area of 200 m2/g and the average size of 12 nm
(manufacturer's data). The powder was dispersed in de-ionized,
double distilled water and when necessary pH was adjusted with
H2SO4 or NaOH.

potential powder was dispersed in liquid and suspension was


sheared in a high shear mixer at 8000 rpm for 1 h.
Particles/aggregates size distributions were measured by
particle size analyzer Mastersizer 2000 (Malvern Instruments)
designed for particles in the size range between 20 nm and 2 mm
which gives particles size as a diameter of the spheres with the
volume equal to the volume of measured particles. In this
instrument Mie theory was employed to calculate particle size
distributions from the scattered laser light using the refractive
index of silica particles of 1.46. The accuracy of the
measurements was estimated by measuring average size and
size distributions of calibrated standard particles (supplied by
Duke Scientific) of 10.3 0.05 m and 97 3 nm and for both
sizes experimental error was well bellow 5%. The size and shape
of aggregates/particles were also analyzed with an Environmental Scanning Electron Microscope (ESEM, Philips XL30).
Conductivity of suspension was measured using InLab 730
conductivity probe from Metler Toledo and pH was measured
using Jenway 3020 pH meter.

2.2. Nano-particles/aggregates/suspension characterization


2.3. Experimental rig
Zeta potential of particles/primary aggregates was measured
by Zetamaster (Malvern Instruments) designed for the particles in
size range 20 nm to 3 m. To ensure that the particles/aggregates
were in the required size range, prior to the measurements of zeta

Experiments were carried out in a high shear, rotorstator


mixer (L4R from Silverson) with rotor diameter of 0.028 m,
rotor height of 0.015 m and a gap between the rotor and the

Fig. 1. Transient volume distribution functions at different energy dissipation rates: (a) fragmentation of large secondary aggregates at 4.8 W kg 1; (b) fragmentation of
secondary aggregates at 21.7 W kg 1; (c) fragmentation of secondary aggregates at 89.9 W kg 1 during first 20 min of processing; (d) erosion of primary aggregates
from the surface of secondary aggregates at 89.9 W kg 1 after longer processing time. 5% Aerosil in water, pH 4, t = 20 C.

A.W. Pacek et al. / Powder Technology 173 (2007) 203210

205

stator of 0.5 mm. To improve macro-mixing in the vessel the


rotorstator was mounted off centre in a sealed, stainless steel
jacketed vessel (diameter 0.1 m, height 0.15 m) fitted with
sampling port. The measured power number of this mixer is
equal to 1.7 and it is in a good agreement with the literature data
[8]. The temperature was controlled by the water bath and was
measured by the platinum thermocouple.
2.4. Procedure
In all experiments the same procedure was followed. Silica
powder was pre-dispersed in water in a glass stirred vessel fitted
with Rushton turbine, pH was adjusted to required value (4, 7 or
9) and suspension was stirred for 30 min. After that time the
aggregate size distribution was measured in situ using video
computermicroscope system [9] and in a diluted sample using
Mastersizer 2000. Next the dispersion was transferred to the
high shear mixer from which the air was completely excluded
and the temperature of the water bath was set either to 20 C,
50 C or 70 C. The rotor speed was set to the required value
(3000, 5000 or 8000 rpm) and at each speed the dispersion was
sheared for 3 or 4 h. Small samples of suspension were taken
every 10 min and particles/aggregates size distributions were
measured.
3. Results and discussion
3.1. The effect of energy input on kinetics of de-aggregation
Transient volume distributions functions measured at three
different speeds (different energy dissipation rates) over the
period of 3 h are summarised in Fig. 1. Fig. 1a and b illustrates the
evolution of aggregate size at energy dissipation rate of 4.8 W
kg 1 (3000 rpm) and 21.7 W kg 1 (5000 rpm) respectively and
Fig. 1c and d illustrates the evolution of aggregate size
distributions at energy density of 89.9 W kg 1 (8000 rpm).
From Fig. 1 it appears that de-aggregation of silica powder
can be seen as a two step process. In the first step, at a relatively
low energy input (short processing time at 8000 rpm or low
energy dissipation rates at 3000 and 5000 rpm) large aggregates
(between 5 and 500 m) of initially dry powder shown in Fig. 2a
are broken into a smaller, secondary aggregates with the size
between 3 and 80 m. The transient, single modal volume
distribution functions shown in Fig 1a, b and c are approximately
self preserving and as the time progresses they are gradually
shifting towards the smaller size aggregates. The shape of
volume distribution functions indicates that in this step
fragmentation of secondary aggregates is the main mechanism
of de-aggregation [5]. It is worth to stress that the smallest
aggregates obtained in this step are of the order of 2 m which is
in a good agreement with literature information that the
aggregates/particles larger than 1 m are relatively easy to break.
In the second step, at sufficiently high energy input
(processing at 8000 rpm for approximately 30 min or more)
large secondary aggregates start breaking into a small primary
aggregates clearly seen in Fig. 2b. The transient volume
distributions functions (Fig. 1d) become bimodal, with the first

Fig. 2. Images of silica aggregates: (a) secondary aggregates in dispersion


charged into high shear mixer after premixing with Rushton turbine (time 0 in
high shear mixer), width of the image is equal to 1.1 mm; (b) primary aggregates
in the same dispersion after 4 h of shearing at 8000 rpm.

mode ranging from approximately 50 nm to 0.9 m (primary


aggregates) and the second mode ranging from 3 m to 80 m
(secondary aggregates). Increase of energy input leads to a
gradual reduction of volume fractions of the aggregates in the
second mode and an increase of the volume fractions of
aggregates in the first mode. The widths of both modes
practically do not change and the median diameters are
practically constant. It has to be stressed here that even at the
highest investigated energy density (1500 kJ kg 1) reported
here and at even higher energy density during ultrasonication
(of the order of 4300 kJ kg 1), the aggregates in the first mode
(primary aggregates) could not be broken into a single nanoparticles. The qualitative results obtained with Mastersizer
2000 were confirmed by ESEM analysis and the ESEM image
in Fig. 2b clearly shows many primary aggregates in the range
50 nm to 100 nm and practically no single nano-particle (of the
order of 12 nm).
Similar behaviour of polymer latex nano-particles suspended
in surfactant solutions was recently reported by the authors [10]
who postulated that the single nano-particles in the closepacked primary aggregates are close enough to enter into the
primary energy well leading to irreversible aggregation. The
same explanation can be offered here.
The median diameters of the secondary aggregates as a
function of the processing time and as a function of the energy
density are shown in Fig. 3. The median diameters at the two

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A.W. Pacek et al. / Powder Technology 173 (2007) 203210

Fig. 3. Median diameters (d50) of the secondary aggregates at pH 4 and T = 20 C as function of: (a) processing time and (b) energy density at different energy
dissipation rates: = 4.8 W kg 1 ( ), = 21.7 W kg 1 (), = 89.9 W kg 1 (). Solid lines linear regression.

lowest energy dissipation rates were calculated from the size


distributions of all aggregates having single modal size
distributions. At the highest energy dissipation rate where size
distributions become bimodal (see Fig. 1d) median diameter
was calculated from the second mode only e.g., median
diameter in the latter case corresponds to the population of
the secondary aggregates only.
The reduction of the median diameter (or any other mean
diameter) during de-aggregation process can be described in
terms of a processing time and the energy dissipation rate or in
terms of the energy density (sizeenergy model). For high shear
mixer the energy dissipation rate was calculated from:
e Pod N 3 d D5 d q

and the energy density from:


E ed t

Experimental median diameters plotted as a function of time


(Fig. 3a) in the loglog coordinates fall at three distinctive,
nearly parallel straight lines with the slope ranging from 0.23 to
0.20 with coefficient of determination (r2) larger than 0.98.
The reduction of the aggregates mean diameters with time
during grinding/de-aggregation is frequently described by the
so called sizeenergy model [5,7]:
dav Cd E a

This simple experimental model developed in the mid-1950s


is still used to calculate the mean (usually median) particle size in
a different type of grinding devices. The exponent can be
interpreted as a reduction rate of the median diameter and
constant C as a size of aggregate at unit specific energy input.
This simple two parameter model allows the quick prediction of
the mean size in a given grinding device and it also allows easy
comparison between different types of grinding devices. The
major disadvantage of this model is that it does not allow the
prediction of size distributions and it can be used to model
grinding processes where size distributions are single modal.
Considering that the alternative way of predicting the mean

particle size and size distribution is the solution of the population


balance model (integro-differential equation usually convertible
to a set of differential equations) which is rather complex and
time consuming, it is not surprising that this model has been
successfully used in literature to describe the grinding of solid
particles [5,7] where of the order of 0.680.72 was obtained. It
has also been adopted to correlate average drop size with energy
input during liquid/liquid emulsification in different types of
high shear mixers and in those processes in which of the order
of 0.4 was reported [11].
Fig. 3b shows that by plotting experimental d50 as a function
of energy density in loglog coordinates all data points can be
collapsed (with engineering accuracy) into a straight line with
an average slope = 0.26 and r2 = 0.91 which indicates that that
first step of de-aggregation of silica powder (when size
distributions are single modal) can also be described by this
model.
Whilst the breakage of secondary aggregates having the
single modal size distributions can be analyzed in terms of
rather simple sizeenergy model, the analysis of de-aggregation
when size distributions become bimodal is more complex. In
case of bimodal size distributions the mean sizes cannot be used
to describe the changes of the population of the aggregates and
in principle the evolution of bimodal size distribution with time
should be analyzed within the framework of population balance
model [12]. Whilst such analysis is currently performed and the
results will be reported soon, the whole process of deaggregation can be qualitatively discussed in terms of transient
aggregate size distributions (Fig. 1) or it can be quantified in
terms of breakage of the secondary aggregates (Fig 3) combined
with the analysis of the increase of a cumulative mass fraction of
the primary aggregates (Fig 4).
The volume fraction of the primary aggregates and d90 as a
function of the processing time at 8000 rpm are summarised in
Fig. 4. It is interesting to note that primary aggregates are
generated only after a certain amount of energy has been put
into the dispersion (or after a certain processing time, see Fig. 1c
and d). As the volume fraction of the primary aggregates levels
at an approximately 0.95, d90 falls below 1 m and stays
practically constant indicating that practically all the secondary

A.W. Pacek et al. / Powder Technology 173 (2007) 203210

Fig. 4. Fraction of aggregates smaller than 1 m (primary aggregates) and d90 of


whole population of aggregates as a function of processing time at pH 4,
T = 20 C and = 89.9 W kg 1.

aggregates were broken. Until the secondary aggregates are


present in the suspension the volume fraction of primary
aggregates increases linearly with the processing time at the rate
of the order of 0.01 s 1. After d90 falls below 1 m the rate of
increase of the volume fraction of the primary aggregates
reduces to approximately 0.0005. It is worth to notice that even
after 4 h of processing at 8000 rpm nano-particles were not
observed in the suspension (see Fig. 1d) which indicates that the
primary aggregates were not broken.
Similar pattern of breakage of silica aggregates built from
0.3 m nano-particles was reported by Kusters et al. [4] where,
based on similar evidence as presented above, authors
concluded that silica aggregates are broken by erosion in the
whole range of the energy density. In our case it appears that at
low energy density fragmentation of the large aggregates occurs
and at a high energy density primary aggregates are sheared
from surface of the secondary aggregates.

207

the analysis of aggregate size/size distributions (Figs. 5b and 6)


shows that this is the case only at a low temperature. At 20 C an
increase of pH from 4 to 9 speeds up de-aggregation as can be
seen from an increase of median size reduction rate from 0.23
at pH 4 to 0.29 at pH 9. Also, at pH 9 after 10 min 30% of the
secondary aggregates were broken into the primary aggregates,
whereas at pH 4 after 30 min only 21% of the secondary
aggregates were broken however, in both cases after 4 h of
shearing 95% of the secondary aggregates were broken into the
primary aggregates. Fig. 6a also shows that even when the
breakage rate was highest (at pH 9, t = 20 C) the primary
aggregates (size range 50100 nm) were not broken into a
single nano-particles (average size 12 nm).
As the temperature increased to 50 C, the opposite effect of
pH on breakage kinetics was observed and at pH 4 (small
repulsive forces) de-aggregation was faster than at the higher pH.
Further increase of temperature to 70 C leads to a further, very
strong reduction of the breakage rate at the highest pH (more than
4 h was needed to break 90% of secondary aggregates, = 0.19)
but at pH 4 the breakage rate increased (90% of secondary
aggregates were broken within 55 min, = 0.27).
Whilst, as discussed above and as shown in Fig. 5b, both the
temperature and the pH have a strong effect on the kinetics of deaggregation and breakage rate, the effect of both those parameters
on the final size distribution of the primary aggregates is
negligible. There is a pronounced difference between the transient
volume distributions functions shown in Fig. 6a and b with much
faster shift towards smaller particles in Fig. 6a (pH 9, t = 20 C)

3.2. The effect of pH and temperature on kinetics of


de-aggregation
The change of pH of the suspension leads to a change of
electrostatic charges on the aggregates surfaces which in turns
affects the repulsive forces between them and might alter the
kinetics of de-aggregation. To assess and to quantify the effect
of pH on de-aggregation kinetics the relation between pH and
the charge of the particles surface, zeta potential at different pH
has been measured and the results are summarised in Fig. 5a.
The combined effect of pH and temperature on the kinetics of
de-aggregation is summarised in Fig. 5b and typical transient
distributions during de-aggregation at pH 4 and pH 9 are
compared in Fig. 6.
The higher the absolute values of zeta potential, the larger the
electrostatic repulsive forces and the separation of the particles
becomes easier. In investigated system zeta potentials at pH 7
and higher are of the order of 40 mV and zeta potential at pH 4
is approximately 15 mV which indicates that the repulsive
forces at pH 9 are larger than at pH 4. This suggest that deaggregation at pH 9 and pH 7 should be faster than at pH 4 but

Fig. 5. (a) Zeta potential of primary aggregates as a function of pH for 1% ( )


and 5% () w/w silica in water; (b) the effect of pH and temperature on time
necessary to break 95% of secondary aggregates into aggregates smaller than
1 m; ( ) pH 4, () pH 7, () pH 9.

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A.W. Pacek et al. / Powder Technology 173 (2007) 203210

which Stern potential can be replaced with the measured zeta


potential [15,17]:
 

 
eWs 2 1
jh
1tanh
6
VE 2Z 2 nkT
2
kT j
Hydration energy (VH) has an effective range of few
nanometers and exponentially decays with distance [18]. It
can be calculated from the experimental correlation [15]:
VH V1 d eh=h1 V2 d eh=h2

where: V1/2R = 0.14 J/m2, h1 = 0.057 nm, V2/2R = 5.4 10 3


J/m2 and h2 = 0.48 nm are experimentally determined parameters [14].
All components of the interaction energy between two silica
particles of the same diameter were calculated from Eqs. (4)(7)
and the results are summarised in Fig. 7a for the particles
separated by more than 1 nm and in Fig. 7b for the particles
separated by less than 1 nm. In both cases it is clear that the
interactions between the silica particles in water are dominated by
the repulsive hydration force. The repulsive electrostatic energies
at different pH (see insert in Fig. 7a) are two orders of magnitude

Fig. 6. Transient volume distribution functions in 5% Aerosil/water suspension


at rotor speed of 8000 rpm at the following processing conditions: (a) pH 9,
T = 20 C after processing times of: 0 min ( ), 10 min (), 20 min (), 240 min
(); (b) pH 4, T = 20 C after processing times of: 0 min ( ), 20 min (),
50 min (), 240 min ().

than in Fig. 6b (pH 4, t = 20 C), but again the final volume


distributions (after 240 min) are practically identical.
In principle the effect of pH and temperature on the
interactions between particles/aggregates can be analyzed
using extended DLVO (DerjaguinLandauVerweyOverbeek) model. In this model the interaction force between two
spheres of the same radii (R) is expressed in terms of the van der
Waals energy (VA), the electrostatic energy (VE) and the
hydration energy (VH) between two flat surfaces [13,14]:
F pRVA VE VH

Attractive van der Waals energy (VA) between two flat


surfaces can be calculated from [13]:
VA

A
12ph2

where values of Hamaker constant for silicasilica in water


reported in literature [1416] are in the range 0.46 10 20 J to
1.02 10 20 J.
The electrostatic repulsive energy (VE) depends on the
charge on particles surface and the properties of the liquid. For
constant surface potential it can be estimated from Eq. (6) in

Fig. 7. Components of interaction energy between particles: VA attractive van


der Waals energy, VE repulsive electrostatic energy, VH repulsive hydration
energy; (a) particles separated by more than 1 nm (aggregates); (b) particles
separated by less than 1 nm (single particles).

A.W. Pacek et al. / Powder Technology 173 (2007) 203210

209

lower than van der Waals and hydration energies and they are
practically negligible both at shorter and at longer separation
distances. It is possible to postulate that as the surface of
aggregates is not very smooth the shortest distance separating
them is probably larger than 1 nm and at such a distance the
repulsive hydration energy does not allow entry into the deep
primary well. This means that the secondary aggregates which
are built from the primary aggregates are relatively weak and can
be broken at low energy input as discussed above. Very strong
repulsive hydration interactions also explain exceptional stability
of the suspensions of primary silica aggregates even at pH
corresponding to the iso-electric point [11,14]. On the other hand,
the distance between smooth, small single particles (of the order
of 12 nm) can be below 0.1 nm which allows them to aggregate
irreversibly by entering the primary well. It is also possible that
the strength of these very small, primary aggregates might
depend on the solubility of silica in water. As the pH and
temperature increase from 20 C to 70 C the solubility of silica
increases drastically [19] which might lead to a faster conversion
of the liquid bridges containing relatively large amounts of
dissolved silica into very strong solid silica bridges.
Theoretically predicted effect of pH on the electrostatic
repulsive forces is very small and it does not allow explanation
of rather strong effect of pH on de-aggregation kinetics at elevated
temperature observed experimentally. This confirms the literature
suggestions that electrostatic interactions within DLVO model
have serious limitations in the case of silica nano-particles.

Nomenclature
A
Hamaker constant
C
Constant defined by Eq. (3)
d32
Sauter mean diameter
d90- 90% (volume) of aggregates below d90%
D
Rotor diameter
e
Electron charge
E
Energy density
h
Distance between particles
kB
Boltzman constant
N
Rotor speed
Po
Power number
V
Interaction energy
R
Particle radius
r2
Coefficient of determination
t
Time
t95% Time necessary to break 95% of secondary
aggregates below 1 m
T
Absolute temperature
z
Valency

Constant defined by Eq. (3)

Electrostatic potential

Average energy dissipation rate

Inverse Debye length

Liquid density

4. Conclusions

This work is a part of the PROFORM (Transforming Nanoparticles into Sustainable Consumer Products Through Advanced Product and Process Formulation EC Reference
NMP4-CT-2004-505645) project which is partially funded by
the 6th Framework Programme of EC. The contents of this
paper reflect only the authors' view. The authors gratefully
acknowledge the useful discussions held with other partners of
the Consortium: Bayer Technology Services GmbH; BHR
Group Limited; Centre for Computational Continuum Mechanics (C3M); Karlsruhe University, Inst. of Food Process Eng;
Loughborough University, Department of Chemical Eng;
Poznan University of Technology, Inst. of Chemical Technology and Eng; Rockfield Software Limited; Unilever UK Port
Sunlight, Warsaw University of Technology, Department of
Chemical and Process Eng.

This study has revealed the two stage mechanism of deaggregation of large (+ 50 m) secondary aggregates made of
silica nano-particles (size 12 nm) and the effect of the
temperature and pH on the kinetics of de-aggregation and size
distributions of the primary aggregates. In the first stage, at low
energy density, the large aggregates of single modal size
distributions are broken by fracture and the transient size
distributions slowly shift towards smaller sizes as energy
density increases. The median size of the aggregates at this stage
is well correlated by the sizeenergy model. At higher energy
density, the mechanism of breakage changes into erosion of
primary aggregates (50 nm to 1 m) from the surface of the
secondary aggregates. This leads to bimodal volume distributions with the first mode between 50 nm and 1 m and the
second mode between 3 and 80 m. At a sufficiently high
energy density, the secondary aggregates disappear leaving only
small primary aggregates in the suspension.
The effect of pH on the kinetics of de-aggregation depends on
the temperature; at low temperatures the increase of pH increases
the de-aggregation rate but as the temperature increases the
increase of pH leads to a significant reduction of de-aggregation
rate. Even at the most favourable conditions (low temperature,
high pH, high energy density), breakage of the primary
aggregates which were smaller than 1 m into single nanoparticles was not observed. This implies that primary aggregation is an irreversible process, e.g., primary aggregates cannot be
broken into single silica oxide nano-particles.

[J]
[m]
[m]
[m]
[C]
[kJ kg 1]
[m]
[J K 1]
[s 1]
[]
[J/m2]
[m]
[]
[min]
[min]
[K]
[]
[]
[V]
[W kg 1]
[m 1]
[kg m 3]

Acknowledgement

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