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Construction and Building Materials, Vol. 10, No. 8, pp. 583-588, 1996

PIh S0950-0618(96)00022-0

Elsevier Science Ltd

Printed in Great Britain. All rights reserved 0950-0618/96 $15.00+0.00

©

1997

An investigation into the properties of micro-sphere insulating concrete

Miroslawa Losiewicz, t David P. Halsey,** S. John Dews,* Paul Olomaiye* and Frank C. Harris*

tDepartment 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 3for 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

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-spheres1-7. Low-density mineral aggregates, such as expanded perlite and exfoliated vermiculite are used for insulating concrete, fills and plasters8-16. However, in suitable situations, PFA micro-spheres may act as a substitute17. 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 weight3-5. PFA particles from Britain, which are predominantly spherical, also contain a similar extent (about 5% by weight) of hollow

spheres1,2-20.

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 diameter4. These micro-spheres decrepitate (crackle until they burst) on heating until 260°C is reached; their shells start to sinter at about 1100°C, collapse at about 1300°C,

*Correspondence to D. E Halsey

583

and melt at 1400°C4. 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 composi- tion is given in Table 1. The thin walls of the micro-spheres are highly micro- porous (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). Micro- scopic 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, spongy- structured 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.

584

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

Table 1

Chemicalanalysisof micro-spheresfrom PFA (suppliedby the

Table 2

Sieveanalysisof micro-spheresless than 1 mm diameter

Power StationsBy-productsUtilisationEnterprise)

Sieve size

Sieve residue,range

Sieve residue, mean

Oxides

Concentration(% by weight)

(mm)

(% by weight)

(% by weight)

Silicon(SiO2)

53.22-54.82

0.000

0.6-2.7

1.6

Aluminium(A1203)

28.98-31.83

0.056

0.3-1.3

0.9

Iron (Fe203total)

3.22-7.09

0.063

0.4-1.3

0.9

Calcium(CaO)

0.70-2.06

0.071

2.8-8.8

6.3

Magnessium(MgO)

0.90-2.02

0.100

24.6-30.9

28.1

Sodium(Na203)

0.66-0.98

0.160

21.3-30.6

24.1

Potassium(K20)

3.09-4.31

0.200

22.9-27.9

24.7

Water (H20)

0.164).39

0.320

6.3-7.9

7.7

Loss on ignition

0.22-1.35

0.400

3.2-6.6

4.7

 

0.630

0.4-1.0

0.8

0.800

0.2-0.5

0.3

  0.630 0.4-1.0 0.8 0.800 0.2-0.5 0.3 Figure 1 Micro-sphere wall thickness and porosity at 310

Figure

1

Micro-sphere wall thickness and porosity at 310 times

magnification

porosity at 310 times m a g n i f i c a t i o

Figure 2

Excrescenceof the micro-sphereabout0.12mm 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 m3 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

remained equal. A number of cylinders, prisms and plates Figure 3 Micro-sphere0.10 to 0.16 mm in

Figure 3

Micro-sphere0.10 to 0.16 mm in size at 95 times magnifica-

tion.

Table 3

Physicalpropertiesof micro-spheres

Property

Mean value

Range

Dry bulk density(in bulk)

412

kg m -3

395-425kg m -3

Dry bulkdensity(compacted)

453

kg m

3

431--472kg m 3

Particle apparentdensity

674

kg m

3

Shell specificweight

2 240 kg m-3

 

Porosity

70%

 

Thermal conductivity(over-dried)

0.092Wm 1K i

cast to enable the properties determined.

were

of the

concrete to be

Concrete mixes

Technological parameters for the manufacture of the micro- sphere concrete were selected to get the least density and maximum 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 mm mesh, were used as an

aggregate.

lean, the

In general, all concrete mixes

were

cement content ranged from 60-180 kg m -3 (approx.). The lowest cement content was 15% by weight of the micro- spheres. 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.

585

Table 4 Physical properties of Ordinary Portland Cement "35", ASTM Type 1 (manufacturer'sdata)

Specific surface area, Blaine 250 m2kg-1

Compressive strength

of prisms made of

18.5 MPa

standard mortar 1 : 3 : 0.5 at: 3 days

 

7

days

31.3 MPa

28

days

41.1 MPa

Setting time: initial set

 

110 min

final

sel

215 min

Table 5

water ratio was held constant at 1.2)

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

Mix

number

Mix proportions

Cement (kg m 3)

Cementto water ratio (by weight)

% of cement in micro-sphere (by weight)

1

60

0.18

15

2

80

0.24

20

3

100

0.30

25

4

120

0.36

30

5

140

0.42

35

6

160

0.48

40

7

180

0.54

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.

Preparation, casting and testing of specimens

All mixes were compacted on a vibrating table, at a

frequency of 8000rpm, within 15 s. After

moulded specimens were kept at an air temperature of about 20°C 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/B- 06263, PN-80/B-06258, PN-80/B-04300). Forty-eight

80 mm by 80 mm cylinders from each mix, were tested

for density, porosity, compressive strength and water

casting, all

absorption at 28 days. All specimens were oven-dried at 105°C, until a constant weight was obtained, before testing. Six 50 mm by 50 mm by 250 mm prisms, from each mix, were tested for capillary absorption. The macro- porosity of the hardened concrete, defined as the ratio of volume of pores of 1-3 mm 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 mm by 50 mm by 250 mm prisms, from each mix, were tested for shrinkage in a climatic chamber,

at a relative humidity of 65% and an air temperature of

20°C. 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 mm by 55 mm cylinders, from each mix, were used to test the coefficient of thermal expansion using a Direct Dilatometer DO-105 (Poland). Six 250mm by 250 mm by 50 mm 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 mm by 20 mm cylinders, from each mix, were used for testing concrete vapour permeability at a stationary vapour flow, using the wet method.

Results

and discussion

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 mm

Table 6

Summaryof micro-sphere concrete properties at 28 days

Mix namber

Total porosity

Apparent density,

Apparent density,

Compressive

aThennal

 

aVapour

(%)

wet

oven-dried

strength

conductivity

~aerrneability

1

 

(kgm 3)

(kgm -3)

(MPa)

(Wm

1K 1)

(10

gm-lh-lpa

)

1 78.37

760

481

0.55

0.111

116.5

2 77.20

779

507

0.84

0.118

105.6

3 76.16

788

530

1.03

0.124

89.1

4 75.30

815

550

1.46

0.132

75.0

5 74.47

817

568

1.68

0.142

67.7

6 73.07

851

599

2.29

0.149

64.2

7 72.44

867

613

2.88

0.153

52.8

aForthese tests, the temperaturewas 20°C, 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

586

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

7001

600

500 ,.~/

400

3.0

2.5

2.0

1.5

i.O

T

~

2O

20

f

.~

i

30

t

i

40

40

r

c,%

c, %

W/InK

0.16

O.V.

0.10

 

t

21o

'

3~

I

t.;

re,/°

120

I00

80

60

a;O

.

 

i

t

I

i

i

~

r

 

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

(a) (b)
(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,

standard deviation

respectively. The

MPa and about 2.9 MPa, standard deviation respectively. The Figure 6 Polished section of concrete with

Figure 6 Polished section of concrete with a cement content of 15% at 62 times magnification

W/inK

MPa

 

4

0,16

2.5

." "2~""

0.1 t

20

.

"

": :'"

.'

".

o.12

1.s

~

'.".

". '".

0.10

,.0

.

.; ~.':"

 

i

i

p

0.5

b

 

kg/mr"

I

r

T

I

1()6g/mhPa

500

550

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

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

capillarity2].

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

0.7-1.3 mm m -t (approx.) (Table 8). The

shrinkage stabilizes within 100-130 days in the case of the

and amounts to

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

587

Table 7

Rate of moisture transfer by capillary absorption during first 3 h

Mix number

Capillary rise of mositure (cm) after:

1

2

3

4

5

6

7

10 min

20 min

40 min

60

min

120 min

180 min

10.0

14.0

void

void

void

void

7.3

10.2

13.4

15.3

18.3

20.0

6.0

8.3

11.3

13.3

16.5

18.4

4.5

6.3

9.0

10.9

14.0

16.4

3.3

4.6

6.5

8.1

11.0

12.5

2.7

3.7

5.3

6.35

8.7

10.5

2.0

3.0

4.3

6.5

7.8

9.5

Table 8

Shrinkage of micro-sphere concrete (specimens were 4 cm by 4 cm by 16 cm, temperature was 20°C and relative humidity was 65%)

Mix no. Moisture content (% by weight)

Capillary shrinkage (ram m -1) after:

3

days

moist

curing;

28

day

moist

curing

 

Initial

Final

1

57.8

1.1

2

52.8

1.2

3

47.0

1.3

4

46.6

1.4

5

38.9

1.7

6

36.4

1.8

7

35.6

1.9

1

56.5

1.5

2

54.6

1.7

3

43.0

1.8

4

38.4

2.0

5

37.0

2.1

6

38.5

2.3

7

35.0

2.5

7 days

28 days

0.165

0.225

0.215

0.245

0.250

0.345

0.295

0.375

0.445

0.530

0.470

0.565

0.470

0.610

0.385

0.480

0.430

0.575

0.515

0.655

0.575

0.765

0.605

0.905

0.690

0.970

0.690

0.995

3-day moist curing, before the air drying process, and 130- 180 days in the case of the 28-day moist curing. Air- shrinkage 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 -20-100°C, varies in the range 3.1-4.2x10 6°C-1. This is lower than that of perlite and vermiculite concretes, which range from 7.6-

11 x 10-6°C

1 between -22°C and 56°C 14.

Thermal conductivity of the micro-sphere concrete ranges from 0.11-0.15Wm-IK -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 0.097- 0.131 W m-lK ill (approx.) and that of the vermiculite ranges from 0.09-0.16 W m-lK -ur. Vapour permeability of the oven-dried concrete de- creases as the cement content increases, and ranges from 53-117× 10-6g m-th 1pa-1 (approx.) (Table 6). The cur- vilirlear 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,

56 days

100 days

130 days

160 days

190 days

0.255

0.280

0.295

0.295

0.295

0.275

0.290

0.305

0.305

0.305

0.390

0.405

0.405

0.405

0.405

0.415

0.470

0.470

0.470

0.470

0.595

0.655

0.655

0.655

0.655

0.655

0.685

0.685

0.685

0.685

0.675

0.690

0.705

0.705

0.705

0.530

0.545

0.560

0.565

0.570

0.615

0.645

0.650

0.655

0.655

0.710

0.740

0.765

0.770

0.770

0.845

0.890

0.920

0.930

0.965

0.985

1.030

1.050

1.050

1.060

1.045

1.110

1.140

1.140

1.170

1.090

1.180

1.200

1.235

1.250

 

55O

500

450

"~

400

0.16

0.14

0.12

Thermalconductivity

W/mK

~ E

25

Cement% of micro-sphere

15

20

30 35 40

45

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 con- ductivity 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 60-

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

180kgm -3

of

cement

are

sufficiently favourable

588

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

industry.

A

model

(Figure8), 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 Wolverhamp- ton. Two anonymous referees provided many useful

comments upon an earlier draft of this paper.

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12 Cormon, P. Betons Logers d'Anjourd Hui. Eyrolles, Paris, 1973.

13 Anon. Special Concretes and Concrete Products. John Wiely, Chichester, 1975.

14 Neville, A.M. Properties of Concrete (Second Metric Edition). Pitman, London, 1973.

15 Neville, A.M. and Brooks, JJ. Concrete Technology. Longman, London, 1987.

16 Shetty, M.S. Concrete Technology: Theory and Practice. S. Chand, New Delhi, 1992.

17 Losiewicz, M., Matyszewski, T. The Use of Micro-spheres as an Aggragate for Insulating Concretes. In XXV Jubileuszowa Konfer- encja KILiW PAN i KN PZITB, Wroclaw, Krynica, 1979, 115-122.

18 Raask, E., Cenospheres in Pulverised Fuel Ash Journal of the Institute of Fuel, 1969, 41(332), 334-339.

19 Barber, E.G., Jones, G.T., Knight, R.G.K. and Miles, M.H. PFA Utilisation, Central Electricity Generation Board, London, 1972.

20 Anon. The Use of GGBS and PFA in concrete. Concrete Society Technical Report, 1991, 40.

21 Ptonski, W. and Pogorzelski, J.A. Building Physics. Arkady Warszawa, 1979.