Fuel 85 (2006) 2250–2259

www.fuelfirst.com

Characteristics of the ultrafine component of fly ash

a,*
M.R. Jones , A. McCarthy a, A.P.P.G. Booth b

a
Concrete Technology Unit, Division of Civil Engineering, University of Dundee, Dundee DD1 4HN, Scotland, UK
b
Hilti Aktiengesellschaft, Liechtenstein

Received 5 May 2005; received in revised form 27 January 2006; accepted 27 January 2006
Available online 9 June 2006

Abstract

Post-production processing of fly ash (FA) is an important issue for its use in concrete. Given (i) the need for environmental protec-
tion, (ii) the measures being applied on coal-fired power stations to reduce acidic gas emissions and (iii) the effect these have had on fly
ash quality, there is a need to consider efficient post-production processing to enhance fly ash characteristics. This is particularly impor-
tant for fly ash used as a cement in concrete production, since the additional residual carbon content and decreased fineness significantly
affect its quality. This paper details the material characteristics of an ultrafine, low-lime fly ash (UF-FA), produced, in this case, by pro-
cessing a coarse FA (referred to as parent FA) from a bituminous coal-fired power station via air-cyclonic separation. The UF-FA is
shown to have much improved material characteristics compared to the parent FA in terms of morphology, mineralogy and chemical
composition. Further results are presented on the effect of UF-FA on the properties of cementitious systems. Improved consistence
and compressive strengths of combined Portland cement (PC) and UF-FA mortars were observed, whilst enhanced PC hydration
and a high degree of FA reactivity were concluded from heat of hydration measurements and calcium hydroxide contents of pastes.
 2006 Elsevier Ltd. All rights reserved.

Keywords: Air-cyclonic processing; Ultrafine fly ash; Material characteristics

1. Introduction which have negatively impacted on its performance in con-

Fly ash (FA) is used worldwide and its premium appli-
cation is as a cement in concrete. It provides significant
technical benefits to concrete, including improved consis-
tence, lower heat of hydration, strength and durability per-
formance [1–3]. In addition, as a low-cost by-product, fly
ash can reduce the overall unit cost of concrete production.
It has been well established [4] the finer the fly ash, the
more effective it becomes in terms of these benefits. How-
ever, modern power stations use low-emission production
methods, resulting in FA with generally coarser physical
characteristics and often high residual carbon contents,
* fine fly ash (UF-FA) obtained by air-cycloning was exam-
Corresponding author. Tel.: +44 1382 384343; fax: +44 1382 384816.
E-mail addresses: m.r.jones@dundee.ac.uk (M.R. Jones), a.z.mccarthy
@dundee.ac.uk (A. McCarthy).
crete [5]. As a result, many ash producers are utilising post-
production processing of FA to remove the carbonaceous
and clay residue materials and/or refine the particle size.
One processing method, which has the potential to achieve
this is cyclonic separation. The advantages of this tech-
nique are that it has low energy consumption and has no
moving parts, but more significantly, the method can be
used to obtain the ultrafine component, i.e., <10 lm, in
ash. This component has the potential to provide greatly
enhanced performance to concrete mixes and, used as an
outlet strategy for holistic FA use, would be attractive to
both producers and users alike.
The laboratory research reported in this paper addresses
the potential of air-cyclonic separation to produce high
quality FA for use in concrete. The finest fraction of ultra-
ined in this study, to determine the maximum potential of
this processing method.

0016-2361/$ - see front matter  2006 Elsevier Ltd. All rights reserved.
doi:10.1016/j.fuel.2006.01.028
 M.R. Jones et al. / Fuel 85 (2006) 2250–2259
2. As-produced (parent) fly ash
The parent FA used in this study, typical of UK produc-
tion from a low-lime bituminous coal, conformed to BS
EN 450 (maximum fineness of 40% retained on a 45 lm
sieve [6]) with a fineness of 24% by mass retained on a
45 lm sieve and its LOI of 7.6% exceeded the BS EN
197-1 criteria for cement composition (i.e., upper limit of
7.0% permitted on a national basis [7]).
3. Particle cyclonic separation
A tangential inlet high efficiency cyclone, based on the
Stairmand type cyclone [8], was used to separate the parent
FA. It was decided to obtain the ultrafine fraction of FA,
which, in this case, was arbitrarily selected as being
<10 lm. This provided what may be considered to be the
most active fraction in sufficient quantities.
The geometry of the cyclone used is given in Fig. 1. The
parent FA was fed into the cyclone cone through the inlet
orifice fluidised within a compressed (1.1 bar) air stream
with an inlet manifold velocity of 5 m/s. The ash is initially
spun inside the cyclone cone, the FA accelerated as it
neared the base of the cone, due to the cone’s decreasing
diameter. This creates a central vortex, which travels
upwards and exits the cyclone through the top outlet ori-
fice. As a result, centrifugal and aerodynamic drag forces
are used to separate the FA particles within the cone, based
on their size, shape and density characteristics. The UF-FA
exited the cyclone cone through the top outlet orifice and
was collected by filtering the exhaust air stream, whilst
the oversized, non-spherical and heavier particles were col-
lected below the cyclone cone and, in this case, were
discarded.
4. Material analysis test procedures
4.1. Assessment of particle size distribution
A low angle laser light scattering (Malvern Mastersizer
X) was used to analyse the particle size distribution of
the FA. The test samples were dispersed in de-ionised water
using sodium hexametaphosphate and ultrasonic disag-
glomeration [9]. Three samples were analysed for each test
material.
4.2. Particle morphology
Scanning electron microscopy (SEM) secondary elec-
tron images (Jeol 35 SEM connected to a links system
Si(Li) X-ray detector for EDAX analysis running at
15 kV and 25 kV for visual and chemical analysis, respec-
tively) were taken to investigate particle morphology.
Energy dispersive X-ray analysis (EDXA) was also used
in conjunction with the SEM for individual particle com-
positions. Samples were affixed to a conductive carbon
pad to avoid problems encountered with glue or cement
2251
fixture [10]. A Au–Pd sputter coating was applied to the
surface of the specimens to provide greater depth of
image.
4.3. Particle bulk mineralogy and oxide composition
Particle mineralogy was examined by X-ray diffraction
(XRD), using a Philips PW 1050 Diffractometer. The test
samples were micronised in acetone for 10 min prior to
preparation of sample slides.
Bulk oxide composition was determined by X-ray fluo-
rescence spectrometry (XRFS) using a Philips PW 1410
X-ray spectrometer and calibration curves were used for
quantification. Two representative samples of 4 g were
tested for each material.
5. Mortar and paste test procedures
5.1. Mortar specimen preparation
In total, five mixes were considered in this study with the
following cement combinations:
• Portland cement (CEM I, denoted hereafter as PC) con-
forming to BS EN 197-1 [7].
• C with 15% and 30% by mass parent FA.
• PC with 15% and 30% by mass UF-FA.
Natural sand (GF85) to BS EN 12620 (aggregate stan-
dard for use in concrete [11]), sieved at 2 mm, was used
as fine aggregate at a cement/fine aggregate ratio of 1:3
by mass. A water/cement ratio of 0.50 was adopted
throughout and mixing was carried out in accordance with
BS EN 196-1 (standard describing test methods for cement
[12]). All specimens were cured in water at 20 ± 2 C until
testing.
5.2. Flow behaviour
A standard flow table [13] was used to measure the
degree of spread of the PC and PC/FA mortars.
5.3. Compressive strength
Standard mortar prisms, 40 · 40 · 160 mm, were cast
and covered by a plastic film, demoulded at 24 h and
water-cured until testing. After 28, 90 and 180 days, two
prisms per mix were split into two and tested for equivalent
cube strength to BS EN 196-1 [12].
5.4. Heat of hydration and bulk calcium hydroxide
content
The rate of heat gain and total heat evolution up to 72 h
after mixing were tested on PC and PC/30% FA paste
mixes with a 0.50 w/c ratio. The measurements were carried
out using conduction calorimetry. The bulk calcium
2252 M.R. Jones et al. / Fuel 85 (2006) 2250–2259

Fixed vertical rotation point Horizontal angle of inclination

against air stream

Inlet air Moveable vane

stream attachment
Raw Feed
Container
Alteration of air
and particle flows

Top outlet orifice

Feed Control
Valve
Applied
vibration Filter

Compressed
Fine material
Air Supply
Cyclone Collection
Cone

Coarse material
Collection
Vessel

125

44

Top FA outlet
orifice

108

22

h1
103

Inlet orifice
variable from
318
wi
23 55 to 215mm

All measurements Ø 11.3o

in mm

Oversize PFA
outlet orifice
39

Fig. 1. Schematic layout of the laboratory cyclone system.

hydroxide content of the paste cubes (prepared as for the
strength prisms) was measured after 3, 7, 28, 56 and 90
days using thermogravimetry, at a temperature rise of
10 C per minute from 0 to 1000 C. One specimen was
tested for each mix. This was freeze-dried prior to testing,
to stop any further hydration.
6. Fly ash properties
6.1. Particle size distribution
The particle size distribution of the parent and ultrafine
FAs is given in Fig. 2. As expected, the UF-FA demon-
 M.R. Jones et al. / Fuel 85 (2006) 2250–2259 2253

Fig. 2. Particle size distribution curves.

strated a very even mono-model particle size distribution. Table 1

This is in contrast to the parent FA, which had a bi-model Summary of effects of air-cyclonic processing
(and arguably tri-model) particle size distribution but had Properties Parent Cycloned Improvement
an extremely predominant coarse peak. The reason for FA FA in comparison
to parent
this change in frequency distribution behaviour is probably material (%)
associated with inhomogeneity in the particle chara-
(a) Ultrafine fly ash (UF-FA)
cteristics, which is greatly reduced by the cyclonic pro-
cessing. Fineness, lm d(v, 0.1) 1.9 0.9 53
d(v, 0.5) 19.2 2.0 90
Some statistical information of the key particle FA size
d(v, 0.9) 76.8 4.5 94
characteristics is summarised in Table 1. The UF-FA mean Volume above, % 10 lm 64.7 0.2 100
particle size was 2 lm, compared to 19.2 lm for the parent 20 lm 49.0 0.0 100
ash. Furthermore, the d(v, 0.9) and d(v, 0.1) reduced by 94% 45 lm 24.2 0.0 100
and 55%, respectively, with air-cycloning, corresponding to Composition Al2O3 19.0 23.0 21
SiO2 42.6 44.0 3
virtually an elimination of particles >10 lm. The potential
LOI 7.6 5.0 34
yield of UF-FA from the parent FA was shown to be
around 35%, based on the percentage of particles (b) PC/UF-FA mortars and pastes
<10 lm. However, the d(v, 0.1) value for the parent was Flow table spread PC/15% FAa N/Ab N/Ab 101
1.9 lm and is, thus, close to the mean of the UF-FA. This PC/30% FAa N/Ab N/Ab 226
suggests that the yield, using the present cyclone at its cur- 28-day strength, PC/15% FAa 35.5 45.0 27
N/mm2 PC/30% FAa 25.5 41.0 61
rent efficiency, could reach a maximum of around 20% of 90-day strength, PC/15% FAa 43.0 58.5 36
the parent FA volume. This yield figure also corresponds N/mm2 PC/30% FAa 35.5 51.5 45
to the relationship between the d(v, 0.9) value of the UF- 180-day strength, PC/15% FAa 46.0 64.0 39
FA (4.5 lm) and the percentage of particles below 4.5 lm N/mm2 PC/30% FAa 37.0 60.5 64
for the parent FA (20.4%). Increasing the efficiency of the Total heat of PC/15% FAa 870 959 10
hydration (72 h), PC/30% FAa 967 1066 10
cyclone, so as to obtain a higher quantity of UF-FA, would J/100 g PC
alter the nature of the UF-FA by increasing its mean par- Ca(OH)2 consumption N/Ab N/Ab 112
ticle size. after 90 days
a
% By mass.
6.2. Particle morphology b
N/A: data not available.

A comparison of the particle morphologies of the parent

and air-cycloned FAs is given in Fig. 3. The parent FA
consisted of large illite clay residue vesicular particles, con-
taining trapped small spherical grains (see Fig. 3a). In addi-
tion, carbon, large rounded and widely dispersed small
particles and clay and crystalline fragments (probably
quartz) were abundant.
Figs. 3b–d are typical of UF-FA particles. The domi-
nant morphology of UF-FA comprised small spherical
grains (Fig. 3b), minor fragments of clay/shale residue
(Fig. 3c) and loose particle agglomerations (Fig. 3d).
The residue fragments shown in Fig. 3c were identified
by EDXA as illite. A typical FA particle agglomeration
is shown in more detail in Fig. 3d. Overall, these ranged
from a few microns up to 100 lm in size and their shapes
varied widely; from elongated to curved or circular. A
clearly evident vesicular fragment skeleton was present
within some agglomerations. It is thought that the
2254 M.R. Jones et al. / Fuel 85 (2006) 2250–2259

Fig. 3. Differences in particle morphology of parent and ultrafine fly ashes.

agglomerations of fine spherical particles could be pres-
ent in the parent ash [14], but are likely to be limited.
Given that the agglomerations were easily dispersed in
water by light stirring, it would appear that bonding of
the particles occurred due solely to electrostatic surface
charges.
Small crystalline particles of quartz were also found. No
carbon particles were noted in the UF-FA, suggesting that
cyclonic processing removed them completely. Some larger
rounded particles, around 10 lm, were coated in magnetite
but were infrequent.
Based on these observations, it is suggested that cyclonic
processing of FA is particularly selective of non-spherical
morphologies, such that even very small such particles
are removed preferentially. This would appear to support
boundary layer theory as the main processing action, as
spherical particle shapes present far less aero-dynamic drag
than those with irregular morphologies. This also helps to
explain the almost exclusive cenospheric nature of the UF-
FA.
6.3. Particle bulk mineralogy
Qualitative XRD traces of the parent and ultrafine FAs
are given in Fig. 4. It was evident from these that the phase
composition of the UF-FA was less crystalline than that of
the parent FA. This observation has also been made on lig-
nitic FA [15]. From the traces, quartz appeared to reduce
the most with cycloning. This is perhaps, initially, surpris-
ing, as the detrital quartz normally consists of very fine
particle grains and thus should have been carried through
to the UF-FA, thereby resulting in a higher concentration.
 M.R. Jones et al. / Fuel 85 (2006) 2250–2259 2255

Fig. 4. XRD mineralogical analysis of parent and ultrafine fly ashes.

However, given the irregular shape of detrital quartz [16],
its removal is likely to be due to cyclonic boundary layer
effects. The graphite peak appeared in the same range as
the major quartz peak, suggesting that a reduction of
graphite within the UF-FA was taking place and contribut-
ing to the much reduced quartz peak. The quartz that
remained is likely to be a cryptocrystalline phase within
the glass of the UF-FA spherical particles and thus, non-
removable.
Hematite and magnetite were also reduced with air-cycl-
oning, probably as a result of density separation. Mullite
content changed the least, suggesting (i) an equal distribu-
tion of it throughout the particle size range of the parent
FA and (ii) it being a constituent of the rounded particles.
The remaining magnetite will have been a neocrystallisa-
tion adhered to the surface of FA spherical grains, partic-
ularly the larger ones [16].
Given this reduction in crystalline phases, the pozzolani-
cally active amorphous phase of the UF-FA is likely to be
increased. This is, indeed, evident from the increased amor-
phous hump present below the crystalline peaks.
6.4. Particle bulk oxide composition
The differences in bulk oxide composition and LOI of
the parent and ultrafine FAs can be seen in Fig. 5. Air-cycl-
oning led to a significant increase in the Al2O3 content, due
to the almost exclusive cenospheric nature of UF-FA,
which are rich in Al2O3 [16–18]. The increase in SiO2 con-
tent was less noted, although, like the Al2O3, is probably a
reactive, rather than crystalline component, since very little
quartz was noted in the UF-FA.
The reduction in CaO and Fe2O3 contents was probably
due to the removal of the clay residue and iron-coated
spherical particles during processing.
Surprisingly, the SO3 content of the UF-FA was sig-
nificantly higher than that in the parent FA. This sug-
gests that SO3 occurs as a gaseous condensate during
FA formation and is largely concentrated on the finer
particles due to their higher surface area [18]. The great-
est change noted in bulk chemistry (34% difference) was
the reduction in LOI with cycloning. In this case, the
reduction was enough to bring the LOI value of the

Fig. 5. Differences in chemical composition and LOI of parent and ultrafine fly ashes.
2256 M.R. Jones et al. / Fuel 85 (2006) 2250–2259
UF-FA to well within the 7.0% maximum permissible
value in BS 3892-1 (describing the requirements for pul-
verised-fuel ash for use with PC [13]) and BS EN 197-1
[7]. The very pale beige colour of the UF-FA ash, com-
pared to the dark grey of the parent FA, is thought to
indicate that the reduced LOI of 5.0% is not due to
unburned carbon but attributed to the presence of other
components [19].
The MgO content also showed a significant increase
with cyclonic processing, although there is no particular
consequence of this for bituminous ashes [13]. The alkalis
were essentially unchanged, suggesting equal distribution
throughout the parent FA, whilst P2O5 doubled in value
(from 0.2% to 0.4%), suggesting that, like MgO, this was
concentrated in the UF particles. Again, there is no noted
consequence of this to concrete practice.
7. Properties of PC/FA mortars and pastes
7.1. Consistence
The mortar flows obtained, given in Fig. 6, are presented
as a percentage of that of the PC mix. As can be seen, the
coarse parent FA replacement of PC at 15% and 30% levels
by mass had an adverse effect on mortar consistence, as
flow decreased with increasing FA contents. On the other
hand, the addition of UF-FA increased the flow of the
mortar considerably (compared to both PC and PC/parent
FA mortars), particularly at 30% level. The enhanced con-
sistence with the UF-FA was as expected, given the almost
exclusive cenospheric nature of the processed material,
however, the degree of improvement (increase of 220%)
was high.
7.2. Compressive strength
Fig. 7 provides a comparison of compressive strengths
of the PC and PC/FA mortars at 28, 90 and 180 days.
As expected, given the direct (by mass) replacement of
Fig. 6. Flow spread of PC and PC/FA mortars.
PC with FA, the strengths of all the PC/FA mortars were
lower than those of the PC mixes at 28 days. At 90 days,
however, the strength of the 15% UF-FA mix was 12%
higher than that of the PC. By the conclusion of the test
(180 days), both the 15% and 30% UF-FA mixes had
exceeded the strength of the PC and were 20.5% and
12.0% higher, respectively. At all test ages, the mortars
containing the parent FA exhibited lower strengths than
the PC mixes, with the greatest reduction in values at
30% FA addition level. Overall, the improvement in per-
formance of the processed against the parent ash is
manifest.
7.3. Heat of hydration and calcium hydroxide content
The rate of heat evolution and total heat of hydration
are given in Figs. 8 and 9, respectively. As can be seen in
Fig. 8, there was an obvious retardation in rate of heat evo-
lution of 2 h with the parent FA and 5 h with the UF-FA,
compared to PC, which is due to retardation of C3A hydra-
tion [20]. However, it is possible that physical surface
effects also contributed to this behaviour. More specifically,
UF particles surrounding the surface of the PC grains
would reduce the surface area available for initial hydra-
tion. Fig. 9, however, shows that after approximately
20 h, the PC/UF-FA mix had produced more heat than
the parent FA mix, suggesting increased PC hydration,
probably as a result of a greater dispersion of PC grains
and improved mix homogeneity. A further observation,
as shown in Fig. 8, is the reduced rate of descent of the
C3S heat evolution peak for the PC/UF-FA mix. This
may suggest the encouragement of C3A hydration.
The bulk calcium hydroxide (Ca(OH)2) contents for the
PC and PC/FA mixes differed significantly, as can be seen
in Fig. 10. The PC/parent FA mix showed the highest
Ca(OH)2 content at early ages, due to the acceleration of
PC hydration and, thereafter, a gradual reduction with
time through pozzolanic activity. In contrast, the PC/UF-
FA mix contained a much lower Ca(OH)2 content at early
 M.R. Jones et al. / Fuel 85 (2006) 2250–2259 2257

Fig. 7. Compressive strength of water-cured PC and PC/FA mortars.

Fig. 8. Rate of heat of hydration evolution of PC and PC/FA pastes.

ages, followed by a significant reduction at the conclusion is initiated as early as 3 days, which correlates well with
of the test at 90 days. This suggests the pozzolanic reaction strength gains observed. Consumption of Ca(OH)2 with
2258 M.R. Jones et al. / Fuel 85 (2006) 2250–2259

Fig. 9. Total heat of hydration evolution of PC and PC/FA pastes.

Fig. 10. Calcium hydroxide development with time of PC and PC/FA pastes.

UF-FA continued throughout the test period and, by 90 the parent FA. Again, this relates well to the strength
days, was 70% lower than the PC mix and 67% lower than behaviour.
 M.R. Jones et al. / Fuel 85 (2006) 2250–2259
8. Conclusions
The study has shown that a UF-FA can simply and effi-
ciently be produced from relatively coarse FA with a high
efficiency cyclone, using air as the fluidisation medium. The
yield achieved will depend on the original particle size char-
acteristics of the parent FA, but a potential yield of around
20% was observed for the material used in this study. The
UF-FA particle sizes were <10 lm with a d(v, 0.5) of 2 lm.
Furthermore, the particles size distribution was mono-
model and evenly distributed, providing a well-graded
material. Particle agglomerations occurred frequently in
the UF-FA, probably due to electrostatic attraction, but
these were easily dispersed in water and have no implica-
tions for practice. Minor quantities of vesicular clay residue
were also noted. In terms of composition, crystalline min-
eral components were significantly reduced with air-cyclon-
ing, while the amorphous silica and alumina contents of
UF-FA were increased, compared to the parent FA. Whilst
the alkali content was essentially unchanged, both MgO
and SO3 were increased significantly, although the latter
satisfied the specification requirements.
The UF-FA, used as an addition to PC, also provided
significant improvements in the fresh behaviour and com-
pressive strength of mortar. In addition, PC hydration
was enhanced with the presence of UF-FA and the material
itself had a high degree of pozzolanic reactivity. This was
attributed to physical surface effects between the PC grains
and FA particles and the enhanced distribution of the mix
water. The high pozzolanic reactivity was a direct result of
the high amorphous content of the UF-FA. It is also pos-
sible that the physical effect of the FA in enhancing the
packing density of the cementitious systems was a contrib-
uting factor. Overall, this was reflected in 20.5% and 12.0%
increases in 180-day compressive strength, at 15% and 30%
addition levels, respectively, compared to the PC reference
and the fact that the parent FA only gained 87% and 69%
of the PC strength. A summary of the overall improved
material characteristics achieved via air-cyclonic processing
is given in Table 1.
Thus, air-cyclonic processing of FA represents a feasible
undertaking due to the significant technical benefits that
can be achieved. Moreover, this form of processing
requires no further energy input and would be relatively
simple to retro-fit to existing production facilities. Further
work is needed to realise the potential yields suggested and
to determine the optimum level of processing in terms of
yield/performance values. The coarse residue ash could
possibly be used in concrete as fine aggregate or, as is com-
mon practice at present, as a fill material.
Acknowledgements
The authors wish to acknowledge the Engineering and
Physical Sciences Research Council (EPSRC) who pro-
vided funding for this study.
2259
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