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Construction and Building Materials, Vol. 10, No. 8, pp.

583-588, 1996
1997 Elsevier Science Ltd
Printed in Great Britain. All rights reserved
0950-0618/96 $15.00+0.00
ELSEVIER

PIh S0950-0618(96)00022-0

An investigation into the properties of


micro-sphere insulating concrete
M i r o s l a w a L o s i e w i c z , t D a v i d P. Halsey,** S. J o h n D e w s , * Paul O l o m a i y e * a n d
F r a n k C. Harris*

t Department of Civil Engineering and Architecture, Technical University of Szczecin,


Szczecin, Poland
*School of Construction Engineering and Technology, University of Wolverhampton,
Wulfruna Street, Wolverhampton WVl lSB, UK
Received 27 November 1995; revised 30 June 1996; accepted 31 July 1996
The aim of the investigation was to determine how the density of micro-sphere concrete

influences other selected properties. A total of 672 specimens of different sizes were made from
seven different concrete mixes. The ratio of cement to water mixes ranged 0.18-0.54. The mixes
differed in cement content only, contents of micro-sphere and water being held constant. Due to
the different cement contents, the specimens differed in porosity. The specimens were tested for
compressive strength, thermal conductivity, vapour permeability, water capillary rise, water
absorption and shrinkage, in accordance with the Polish standards. The total porosity of the
concrete varied in the range 72.5%-78.5%, the micro-sphere structural porosity accounting for
about 42% of the porosity. The density at 28 days ranged 760-870 kg m 3 and 480-615 kg m 3 for
wet and oven dried concretes, respectively. When the cement content was varied in the range
15%-45%, the 28-day compressive strength ranged 0.5-3.0 MPa and the thermal conductivity of
the oven-dried concrete varied in the range 0.10-0.16 W m 1K 1. Based on the analysis of all test
data, it is concluded that the micro-sphere concrete may be a suitable substitute for cement
based concretes, such as those made from expanded perlite and exfoliated vermiculite. 1997
Elsevier Science Ltd. All rights reserved.

Keywords: micro-sphere; pulverised fuel ash; concrete

and melt at 1400C 4. The chemical composition of the


Polish micro-spheres is similar to that of the British
cenospheresl~ and 19. In this research, micro-spheres from
the surface of drained lagoons at one of the biggest regional
power stations, Dolna Odra, situated near Szczecin, in
northwest Poland, have been used. The chemical composition is given in Table 1.
The thin walls of the micro-spheres are highly microporous (Figure 1) and their surfaces are generally smooth;
however, on some surfaces, smaller aluminosilicate bobbles
exist as excrescences (Figure 2).
Particle size analysis shows that particles of the
size 0.10-0.32 mm are most frequent (Table 2). Microscopic observations suggest that among the micro-spheres
of the size 0.063-0.40 mm (91.8%), only a very small
number are shapeless (Figure 3), whereas, among particles
of size equal to or greater than 0.63 mm (1.1%), no
spherical particles are found. In this instance, spongystructured sinters, oval in shape with melted surfaces,
predominate. The smaller micro-spheres, i.e., those less
than 0.056 mm (1.6%), contain mostly irregularly shaped
particles and pieces of crushed micro-spheres. The
physical properties of the micro-spheres are provided in
Table 3. Due to the structure of the particle, there is little
water absorption, but much water is needed to wet their
surfaces.

Introduction
For many years, micro-spheres (cenospheres, floaters)
from pulverised fuel ash (PFA, called pulverised fly ash
in some countries) have been substituting for manufactured
glass micro-spheres 1-7. Low-density mineral aggregates,
such as expanded perlite and exfoliated vermiculite are
used for insulating concrete, fills and plasters 8-16. However,
in suitable situations, PFA micro-spheres may act as a
substitute 17. This paper examines the suitability of the
use of the micro-spheres as an aggregate in insulating
concrete.
Fly ash from Polish pulverised coal power stations
contains 3%-52% spherical particles. The content of
thin-walled hollow spheres (micro-spheres) has been
estimated at 0.4%-8.6% by weight 3-5. PFA particles
from Britain, which are predominantly spherical, also
contain a similar extent (about 5% by weight) of hollow
spheres 1,2-20.
According to data from the Power Station By-products
Utilisation Enterprise, Katowice, Poland, the wall-thickness
of tile micro-spheres accounts for 3%-7% of the total
diameter 4. These micro-spheres decrepitate (crackle until
they burst) on heating until 260C is reached; their shells
start to sinter at about 1100C, collapse at about 1300C,
*Correspondence to D. E Halsey

583

584

Properties of micro-sphere insulating concrete: M. Losiewicz et al.

Table 1 Chemical analysisof micro-spheres from PFA (suppliedby the


Power Stations By-products UtilisationEnterprise)
Oxides
Silicon (SiO2)
Aluminium(A1203)
Iron (Fe203 total)
Calcium (CaO)
Magnessium (MgO)
Sodium (Na203)
Potassium (K20)
Water (H20)
Loss on ignition

Concentration(% by weight)
53.22-54.82
28.98-31.83
3.22-7.09
0.70-2.06
0.90-2.02
0.66-0.98
3.09-4.31
0.164).39
0.22-1.35

Figure 1 Micro-sphere wall thickness and porosity at 310 times


magnification

Table 2 Sieveanalysisof micro-spheres less than 1 mm diameter


Sieve size
(mm)
0.000
0.056
0.063
0.071
0.100
0.160
0.200
0.320
0.400
0.630
0.800

Sieve residue, range


(% by weight)

Sieve residue, mean


(% by weight)

0.6-2.7
0.3-1.3
0.4-1.3
2.8-8.8
24.6-30.9
21.3-30.6
22.9-27.9
6.3-7.9
3.2-6.6
0.4-1.0
0.2-0.5

1.6
0.9
0.9
6.3
28.1
24.1
24.7
7.7
4.7
0.8
0.3

Figure 3 Micro-sphere0.10 to 0.16 mm in size at 95 times magnification.

Table 3 Physicalproperties of micro-spheres


Property
Dry bulk density (in bulk)
Dry bulk density (compacted)
Particle apparent density
Shell specific weight
Porosity
Thermal conductivity(over-dried)

Mean value

Range

412 kg m - 3
395-425kg m - 3
453 kg m 3 431--472kg m 3
674 kg m 3
2 240 kg m-3
70%
0.092Wm 1K i

were cast to enable the properties of the concrete to be


determined.

Concrete mixes
Figure 2 Excrescenceof the micro-sphereabout 0.12 mm in size at 310
times magnification

Methodology
The main aim of the investigation was to determine the
influence of the density of micro-sphere concrete upon the
properties of the concrete. For this purpose, a total of seven
0.03 m 3 concrete mixes were made. The mixes differed in
cement content only, with micro-spheres and water contents
held constant. Due to differing cement contents, the mixes
differed in porosity and the ratio of cement to water ranged
from 0.18-0.54; however, the consistency of all mixes
remained equal. A number of cylinders, prisms and plates

Technological parameters for the manufacture of the microsphere concrete were selected to get the least density and
m a x i m u m air entrapment, at a given cement content,
without using air-entraining agents. Ordinary Portland
Cement "35" (ASTM type 1), was used; its physical
properties are shown in Table 4. Oven-dried micro-spheres,
obtained by sieving using a 1 m m mesh, were used as an
aggregate. In general, all concrete mixes were lean, the
cement content ranged from 60-180 kg m -3 (approx.). The
lowest cement content was 15% by weight of the microspheres. The cement contents increased by 5% increments
to 45% (Table 5). The micro-sphere to water ratio was held
constant at 1.2, thus the cement to water ratio ranged from
0.18-0.54.

Properties of micro-sphere insulating concrete: M. Losiewicz et al.


Table 4 Physical properties of Ordinary Portland Cement "35", ASTM
Type 1 (manufacturer's data)
Specific surface area, Blaine

250 m2 kg -1

Compressive strength of prisms made of


standard mortar 1 : 3 : 0.5 at: 3 days
7 days
28 days
Setting time: initial set
final sel

18.5 MPa
31.3 MPa
41.1 MPa
110 min
215 min

Table 5 Mix proportions of micro-sphere concrete (micro-sphere to


water ratio was held constant at 1.2)
Mix number

1
2
3
4
5
6
7

Mix proportions
Cement
(kg m 3)

Cementto water ratio


(by w e i g h t )

60
80
100
120
140
160
180

0.18
0.24
0.30
0.36
0.42
0.48
0.54

% of cement in
micro-sphere
(by weight)
15
20
25
30
35
40
45

The components were mixed in a paddle mixer of


15 dm 3 capacity in three stages: dry components were
mixed, then two-thirds of the total water was added,
followed by the remaining water. Total mixing time for
each mix was 3-5 min. As a result of this procedure, it was
possihle to obtain homogeneous concrete mixes with a stiff
consistency, and a regular coating of cement grout on the
aggre gate.

585

absorption at 28 days. All specimens were oven-dried at


105C, until a constant weight was obtained, before testing.
Six 50 m m by 50 m m by 250 m m prisms, from each
mix, were tested for capillary absorption. The macroporosity of the hardened concrete, defined as the ratio of
volume of pores of 1-3 m m diameter to the total volume of
concrete was estimated from polished microscopic sections,
using a microscope equipped with an Eltinor 4 Integrating
Unit (Germany).
Twenty-four 50 m m by 50 m m by 250 m m prisms, from
each mix, were tested for shrinkage in a climatic chamber,
at a relative humidity of 65% and an air temperature of
20C. Half of the specimens were put into the climatic
chamber for a 3-day moist curing, and the other half for a
28-day moist curing. The length of all specimens was
measured using a dial indicator having an accuracy of
__.0.005 mm.
Six 4 m m by 55 m m cylinders, from each mix, were
used to test the coefficient of thermal expansion using a
Direct Dilatometer DO-105 (Poland). Six 2 5 0 m m by
250 m m by 50 m m oven-dried plates, from each mix, were
tested for thermal conductivity at a stationary heat flow
using the Bock apparatus (Germany). The Bock apparatus
involves the sample being placed between a heated and
cooled plate. The power of the heater (in W) and the
temperature difference between the hot and cold sides of
the sample were used to calculate the thermal conductivity.
Six 100 m m by 20 m m cylinders, from each mix, were used
for testing concrete vapour permeability at a stationary
vapour flow, using the wet method.

Preparation, casting and testing of specimens

Results and discussion

All mixes were compacted on a vibrating table, at a


frequency of 8 0 0 0 r p m , within 15 s. After casting, all
moulded specimens were kept at an air temperature of
about 20C in moist-curing boxes. These boxes were water
tight with water in the base, and the concrete samples
placed on a grate above the water level. After 2 or 3 days,
the specimens were de-moulded and replaced in the boxes,
until required for testing.
Testing of the concrete was conducted in compliance
with ':he Polish standards, relevant to lightweight aggregate
and cellular concrete, as well as fine mortars (PN-75/B06263, PN-80/B-06258, PN-80/B-04300). F o r t y - e i g h t
80 m m by 80 m m cylinders from each mix, were tested
for density, porosity, compressive strength and water

A total of 420 cylinders, 210 prisms and 42 plates were


tested. A summary of the porosity, density, compressive
strength, thermal conductivity and vapour permeability of
the specimens is shown in Table 6. The total porosity of
micro-sphere concrete with 15% to 45% cement content
varies between 78.4% and 72.4%, respectively. The
apparent density of the wet concrete at 28 days ranges
from 760-867 kg m -3, when it is oven-dried (Table 6). The
relationship between the cement content and dry density of
the concrete is linear (Figure 4(a)).
The total porosity, determined from the density and
specific gravity of the specimens, is composed of the
structural porosity of the micro-spheres and cement paste,
air:voids, and incidental air bubbles. Air bubbles, 1-3 m m

Table 6 Summaryof micro-sphere concrete properties at 28 days


Mix namber

1
2
3
4
5
6
7

Total porosity
(%)
78.37
77.20
76.16
75.30
74.47
73.07
72.44

Apparent density,
wet
(kgm 3)
760
779
788
815
817
851
867

Apparent density,
oven-dried
(kgm -3)

Compressive
strength
(MPa)

aThennal
conductivity
(Wm 1K 1)

aVapour
~aerrneability 1
(10 gm-lh-lpa )

481
507
530
550
568
599
613

0.55
0.84
1.03
1.46
1.68
2.29
2.88

0.111
0.118
0.124
0.132
0.142
0.149
0.153

116.5
105.6
89.1
75.0
67.7
64.2
52.8

aFor these tests, the temperaturewas 20C, and the samples were over-dried; the relative humidity during vapour permeability testing was 100% on one
side of the sample and 45% on the other side

Properties of micro-sphere insulating concrete: M. Losiewicz et al.

586

W/InK

700 1
600
500

0.16

O.V.

,.~/

400

0.10
T

~
2O

i
40

c,%

21o '

3~

t.;

re,/

3.0
120

2.5

I00

2.0
1.5

80
60

i.O

a;O
i

20

30

40

c, %

20

30

Z.O

c. %

Figure 4 Relationship between cement and (a) dry density, (b) thermal
conductivity, (c) compressive strength and (d) vapour permeability, of the
concrete

Figure 6 Polished section of concrete with a cement content of 15% at


62 times magnification
W/inK

MPa

0,16

2.5

0.1 t

20

o.12

1.s

0.10

." "2~""
. " ": :'" .' ".

,.0
i

1()6g/mhPa

~..'.". ". '".

. .; ~.':" ..

0.5

kg/mr"

r
500

T
550

b
I
600 kg/m3

120
100
80
6O

,;o ,;o ,'5o ,;o,,~


Figure 7 Influence of the density upon thermal conductivity (a),
compressive strength (b) and vapour permeability (c) of micro-sphere
concrete

(a)

(b)

Figure 5 Polished sections of micro-sphere concrete with a cement


content of (a) 15% and (b) 45%, at 13 times magnification
in diameter are regularly distributed in the concrete and
occupy a mean volume of about 4%. The pore structure of
the hardened concrete is shown from the cut sections in
Figures 5 and 6.
With cement content varying between 15% and 45%, the
mean 28-day compressive strength varies between 0.6 MPa
and about 2.9 MPa, respectively. The standard deviation

varies between 0.1 and 0.4, respectively, indicating reliable


values despite low compressive strengths. The curvilinear
relationship between the compressive strength and cement
content or concrete density is shown in Figures 4(c) and
7(b). At the density 450-550kg m -3, the compressive
strength of micro-sphere concrete is rather lower than that
of the perlite concrete (1.2-2.0 MPa t2) and vermiculite
concrete (1.2-1.3 MPaa2). This may be due to the lower
cement content and the lack of modifying agents.
The results of water absorption show that the concrete
volume absorption amounts to about 42% and the moisture
content at the end of 1 hour of water saturation is 24% by
volume, and only 25% after 24 hours.
From the moisture transfer findings, it appears that the
capillary absorption for the micro-sphere concrete is high.
As shown in Table 7, the rate of the moisture transfer
increases with reduction of concrete density. Capillary
absorption of the micro-sphere concrete, having a cement
content of 35%-45%, is very similar to ceramic brick
capillarity 2].
Shrinkage of the micro-sphere concrete increases as the
cement content increases. At the end of the 3-day moist
curing, the final shrinkage of the concrete amounts to about
0.3-0.7 mm m -1, whereas, at the end of the 28-day moist
curing, the final shrinkage of the concrete is almost double
and amounts to 0.7-1.3 mm m - t (approx.) (Table 8). The
shrinkage stabilizes within 100-130 days in the case of the

Properties of micro-sphere insulating concrete: M. Losiewicz et


Table 7

Capillary rise of mositure (cm) after:

1
2
3
4
5
6
7

10 min

20 min

40 min

60 min

10.0
7.3
6.0
4.5
3.3
2.7
2.0

14.0
10.2
8.3
6.3
4.6
3.7
3.0

void
13.4
11.3
9.0
6.5
5.3
4.3

void
15.3
13.3
10.9
8.1
6.35
6.5

Initial

28
day
moist
curing

120 min

180 min

void
18.3
16.5
14.0
11.0
8.7
7.8

void
20.0
18.4
16.4
12.5
10.5
9.5

Shrinkage of micro-sphere concrete (specimens were 4 cm by 4 cm by 16 cm, temperature was 20C and relative humidity was 65%)
Mix no. Moisture content (% by weight)

3
days
moist
curing;

587

Rate of moisture transfer by capillary absorption during first 3 h

Mix number

Table 8

al.

Capillary shrinkage (ram m -1) after:

Final

7 days

28 days

56 days

100 days

130 days

160 days

190 days

1
2
3
4
5
6
7

57.8
52.8
47.0
46.6
38.9
36.4
35.6

1.1
1.2
1.3
1.4
1.7
1.8
1.9

0.165
0.215
0.250
0.295
0.445
0.470
0.470

0.225
0.245
0.345
0.375
0.530
0.565
0.610

0.255
0.275
0.390
0.415
0.595
0.655
0.675

0.280
0.290
0.405
0.470
0.655
0.685
0.690

0.295
0.305
0.405
0.470
0.655
0.685
0.705

0.295
0.305
0.405
0.470
0.655
0.685
0.705

0.295
0.305
0.405
0.470
0.655
0.685
0.705

1
2
3
4
5
6
7

56.5
54.6
43.0
38.4
37.0
38.5
35.0

1.5
1.7
1.8
2.0
2.1
2.3
2.5

0.385
0.430
0.515
0.575
0.605
0.690
0.690

0.480
0.575
0.655
0.765
0.905
0.970
0.995

0.530
0.615
0.710
0.845
0.985
1.045
1.090

0.545
0.645
0.740
0.890
1.030
1.110
1.180

0.560
0.650
0.765
0.920
1.050
1.140
1.200

0.565
0.655
0.770
0.930
1.050
1.140
1.235

0.570
0.655
0.770
0.965
1.060
1.170
1.250

3-day moist curing, before the air drying process, and 130180 days in the case of the 28-day moist curing. Airshrinkage of the micro-sphere concrete is lower than the
shriiLkage of vermiculite- or perlite- concrete of the same
density. This may be due to a lower cement content, but
drying-shrinkage is also affected by volume fraction,
stiffuess of the aggregates and water content.
The coefficient of thermal expansion of micro-sphere
concrete within the temperature range -20-100C, varies
in the range 3.1-4.2x10 6C-1. This is lower than that of
perlite and vermiculite concretes, which range from 7.611 x 10-6C 1 between -22C and 5 6 C 14.
Thermal conductivity of the micro-sphere concrete
ranges from 0 . 1 1 - 0 . 1 5 W m - I K - t depending on the
cement content (Table 6). Figures 4(b) and 7(a) show the
linear character of the relationship between thermal
conductivity and cement content and thermal conductivity
and dry density. There is a high similarity in the insulating
value of the micro-sphere and perlite/vermiculite concrete.
At the dry density of 400-560kg m -3, the thermal
conductivity of the perlite concrete ranges from 0.0970.131 W m - l K ill (approx.) and that of the vermiculite
ranges from 0.09-0.16 W m - l K - u r .
Vapour permeability of the oven-dried concrete decreases as the cement content increases, and ranges from
53-117 10-6g m - t h 1pa-1 (approx.) (Table 6). The curvilirlear character of the relationship between permeability
and cement content, and concrete density is shown in
Figures 4(d) and 7(c).
Proportions of micro-sphere concrete mixes influence
den~dty, porosity, compressive strength, water absorption,
shrinkage absorption, thermal conductivity and expansion,

55O
500

450
"~ 400

0.16 0.14 0.12


Thermalconductivity
W/mK

E..~
15 20 25 30 35 40 45
Cement% of micro-sphere
Figure 8 General pattern of relationship between thermal conductivity
(A), dry density (() of micro-sphere concrete and proportions of concrete
mixes>

and vapour permeability. A summary of the influence of the


concrete mix properties upon density and thermal conductivity is provided in Figure 8. This may be useful for the
preliminary design of micro-sphere concrete mixes.

Conclusion
The properties of micro-sphere concrete containing 601 8 0 k g m -3 of cement are sufficiently favourable that
micro-sphere concrete may act as a suitable substitute for
cement based concretes, such as those made from expanded
perlite and exfoliated vermiculite, used in the construction

588

Properties of micro-sphere insulating concrete: M. Losiewicz et al.

industry. A model (Figure 8), that may be useful for


preliminary design of micro-sphere concrete mixes, is
provided.
Acknowledgements

We gratefully acknowledge members of staff at the


Technical University of Szczecin for their help in materials
testing. This paper was written while M. Losiewicz was a
Visiting Research Fellow at the University of Wolverhampton. Two anonymous referees provided many useful
comments upon an earlier draft of this paper.
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Warszawa, 1979.

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