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Ceramics International 35 (2009) 471–478

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Lightweight bricks made of diatomaceous earth, lime and gypsum

K. Pimraksa a,*, P. Chindaprasirt b
a
Department of Industrial Chemistry, Faculty of Science, Chiang Mai University, 239 Huey-Kaew Road, Amphor Muang, Chiang Mai 50200, Thailand
b
Department of Civil Engineering, Faculty of Engineering, Khon Kaen University, Khon Kaen 40002, Thailand
Received 4 January 2007; received in revised form 26 October 2007; accepted 2 January 2008
Available online 11 April 2008

Abstract
Diatomaceous earth from Lampang Province in the north of Thailand composes of diatom, kaolinite, montmorillonite and illite, and has porous
cellular structure. In this work, the diatomite, hydrated lime and gypsum are the main ingredients in making autoclaved lightweight bricks. Water
content, pre-curing period, lime content, gypsum content and calcined temperature are the factors investigated. Mechanical and thermal properties
are used to indicate their quality. The nature of hydration products and morphological characteristics of the lightweight bricks are also investigated.
The results show that the diatomaceous earth possesses pozzolanic property and can be used for making lightweight bricks. The bricks made
with untreated diatomite with 15% lime and 5% gypsum shows reasonably high strength of 14.5 MPa and low density of 0.88 g/cm3. Higher
strength (17.5 MPa) and lower density (0.73 g/cm3) are obtained with the use of diatomite calcined at 500 8C. The incorporation of lime and
gypsum with a Ca/Si ratio of 0.55, 50% water content and 6 days pre-curing results in formations of calcium silicate hydrate and gismondine which
enhance strength development. Calcination of diatomaceous earth results in dehydroxylation of the clay minerals and contributes to additional
pozzolanic reaction and better mechanical and thermal properties of the lightweight brick.
# 2008 Elsevier Ltd and Techna Group S.r.l. All rights reserved.

Keywords: Diatomaceous earth; Lightweight brick; Calcium silicate hydrates; Pozzolanic reaction; Alumino-calcium-silicate-hydrate

1. Introduction synthesized using amorphous silica is calcium silicate hydrate

(CSH) gel while the product of crystalline silica is
The deposit of diatomaceous earth clay or diatomite in tobermorite. The hydration products are thus dependent on
Lampang province in the north of Thailand is quite large with reactivity of starting material. By using amorphous silica,
estimation at more than 100 million tons. Its beneficial silicon ion can be readily leached out leading to a decrease in
characteristics are light in weight due to high porosity, the ratio of Ca/Si of hydration products. The type of CSH
relatively attractive in dark-yellow shade due to high content phases plays a crucial role in strength development of the final
of ferrous compound and semi-crystalline siliceous phase product owing to their different van der Waals forces in
similar to opal (SiO2
nH2O) [1]. The pore system is very fine colloidal domains [6]. The variation of Ca/Si ratio directly
and its thermal conductivity is low. Diatomaceous earth affects the type of CSH [7]. The formation of CSH phases
possesses pozzolanic properties similar to other pozzolanic takes place in aqueous solution and therefore the solubility of
materials such as fly ash and metakaolin [2]. Significant uses of individual components heavily influences the formation of
diatomite are, therefore, in construction and insulation new phases. At the surface of silica particles, a small amount
materials such as partial replacement of Portland cement and of SiO2 dissolves and reacts with calcium ions to generate
in calcium silicate brick production [3,4]. CSH phases [8]. The strength of calcium silicate bricks
Calcium silicate brick is produced from the mixture of developed at low temperature is still low due to formation of
Ca(OH)2 and amorphous silica, or alternatively natural quartz CSH-I and CSH-II semi-crystalline structures. Therefore,
under hydrothermal conditions [5]. The nature of products hydrothermal process is necessary for the synthesis to
transform amorphous phases into tobermorite [9]. Not only
CSH is formed, but various types of alkaline alumino-
* Corresponding author. Tel.: +66 5394 3401; fax: +66 5389 2262. calcium-silicate-hydrate compounds are also developed
E-mail address: [email protected] (K. Pimraksa). depending on the ratio of Ca, Al, and Si ions [10].
0272-8842/$34.00 # 2008 Elsevier Ltd and Techna Group S.r.l. All rights reserved.
doi:10.1016/j.ceramint.2008.01.013
472 K. Pimraksa, P. Chindaprasirt / Ceramics International 35 (2009) 471–478

Lampang diatomaceous earth (LDE) contains not only silica (c) Lime content. To study the influences of lime content, the
(SiO2) but also some clay minerals [11]. These clay minerals amount of lime were varied between 10 and 50% by weight
possess low degree of reactivity. To transform them into to obtain Ca/Si ratios of 0.14, 0.23, 0.32, 0.55, 0.86 and
pozzolans and to speed up its chemical reaction, it is necessary 1.30. Water content of 50% and pre-curing of 6 days were
to remove hydroxyl groups from clay structures and other used.
organic substances from clay particles by calcining. (d) Gypsum content. The influence of gypsum addition on
Several other factors also influence the properties and microstructures of pozzolanic reaction products was also
performance of LDE. The study on lightweight bricks made of studied. Gypsum was added to the mixtures at LDE:lime:-
LDE should reveal its potential uses as source material for gypsum ratios of 80:20:0 (Ca/Si = 0.32), 80:15:5 (Ca/
making lightweight bricks. The main aim of this study is to Si = 0.32), 75:15:10 (Ca/Si = 0.42) and 70:15:15 (Ca/
obtain low density and strong brick as required by any standard Si = 0.55). Water content of 50% and pre-curing of 6 days
of lightweight constructional material. The obtained knowledge were used.
should also be useful for other research and application work in (e) Calcinations. In addition, calcined LDE (CLDE) using a
related fields. batch furnace at temperatures between 200 and 700 8C
for 4 h were used to investigate the effect of calcination
2. Materials and methods on pozzolanic reaction. In this test, CLDE:lime:gypsum
ratio of 80:15:5 (Ca/Si = 0.32) was used as its bulk
2.1. Materials density is low. Water content of 50% and pre-curing of 6
days were used.
Diatomaceous earth was obtained from Lampang province
in the north of Thailand. The chemical compositions are shown 2.3. Testing methods
in Table 1. Commercially available hydrated lime (Ca(OH)2)
and gypsum (CaSO4
2H2O) were used for this experiment. (a) The plastic limit (PL), liquid limit (LL), and plasticity index
Specific gravities (S.G.) of diatomite, hydrated lime and (PI) were obtained using Atterberg limit test as described by
gypsum are 0.7, 2.27 and 2.33, respectively. ASTM D 4318 [12]. Plastic limit is the boundary between
plastic and semi-solid states. Dry clay powder was mixed
2.2. Brick sample preparation with water to produce a coherent 3 mm diameter plastic
clay thread. The PL is the water content of the plastic clay
The ingredients were mixed to form uniform mixtures and when water is not sufficient to form this thread. The liquid
then pressed at 3.5 MPa to form 3.5 cm  7.5 cm  15.0 cm limit is the boundary between the liquid and plastic states
bricks. Pre-curing at room temperature (27–28 8C) in moist obtained using a Casagrande device. The plasticity index is
cabinet at over 90% RH was carried out to allow green bricks to calculated as PI = LL PL.
gain some strength before subjecting to high pressure under (b) Electrical conductivity (EC) and pH level of LDE were
steam to avoid cracking. The pre-cured bricks were then determined. The conductivity is a fundamental property of a
autoclaved at 0.14 MPa and 130 8C in a saturated steam material and is defined as the conductance in Siemens per
environment for 4 h. Several factors viz., water content, pre- length of sample. The sample was prepared using the ratio
curing period, lime content, gypsum content, and calcinations of solid to water as 1:10 by weight. The suspension was
temperature were studied: stirred vigorously by magnetic stirrer for 10 min and then
measured the EC and pH using the conductivity tester and
(a) Water content. LDE and lime at the ratio of 85:15 (Ca/ pH tester, respectively.
Si = 0.23, molar ratio) with 45, 50, 55 and 60% water (c) Specific gravities, specific surface area, chemical composi-
content and pre-curing for 6 days were used. tion and mineralogical composition of as-received LDE
(b) Pre-curing period. LDE and lime at the ratio of 85:15 (Ca/ were determined using pycnometer, Brunauer–Emmett–
Si = 0.23) were used with 50% water content. Pre-curing in Teller (BET) method, X-ray fluorescence (XRF) and X-ray
moist cabinet for 1, 2, 3, 5, 6, 7 and 11 days were carried out. diffraction (XRD), respectively.
(d) Differential thermal analysis (DTA) and thermal gravitation
Table 1 analysis (TGA) were performed on LDE to investigate its
Oxide compositions of LDE physical and chemical changes during heating.
SiO2 77.5 (e) Mechanical properties such as compressive strength, water
Al2O3 14.16 absorption and bulk density of the autoclaved bricks were
Fe2O3 5.24
measured in accordance with ASTM C 170 [13] and C 373
K2 O 2.08
Na2O 0.20 [14], respectively. After the strength test, the tested samples
CaO 0.00 were used for the studies of mineralogical and morpho-
MgO 0.46 logical compositions using XRD and scanning electron
TiO2 0.53 microscope (SEM).
P2O5 0.25
(f) Shrinkage was determined by direct measurement of a
SO3 0.01
sample length before and after autoclaving.
 K. Pimraksa, P. Chindaprasirt / Ceramics International 35 (2009) 471–478 473

(g) Thermal conductivity of lightweight brick was measured

using heat conduction unit (WL 370, GUNT, Hamburg,
Germany). The brick samples were cut into the disc shape
with diameter of 2.4 cm and 0.4 cm thick. The applied
power was 4 W for the measurement.

3. Results and discussions

3.1. Properties of as-received and calcined LDE

The LDE contains cylindrical-shaped particles with square

cellular structure and its fragments with d50 of 32 mm as shown
in Fig. 1. Major mineral phases are alpha quartz, kaolinite,
montmorillonite and illite. EC and pH of the diatomite are
5170 mS/cm and 7.8, respectively. This EC value is similar to
that of a pozzolan such as a fly ash reported by Mccarter and Fig. 2. DTA and TG curves of LDE.
Tran [15] and much higher than the EC of locally available
clays deposited in Lampang basin [16]. It represents that LDE
contains water-soluble compounds incorporating with some
soluble salts commonly located in clay minerals. The major
oxides, as shown in Table 1, are silica, alumina and ferric oxide.
The silica and alumina contents are 77.5 and 14.6%,
respectively and are in accordance with the requirement of
natural pozzolan type N per ASTM C518.
PL and LL of LDE are 50 and 56, respectively. For mixes
with 85% LDE and 15% hydrated lime (Ca/Si = 0.23), PL
and LL are 55 and 67, respectively. The PI of as-received
LDE is 6 while that of 85% LDE and 15% hydrated lime is
12. An increase of lime content produces an increase in PI
for quartzite system. This is due to the silica–water
interaction that acquires the negative charged surfaces
[17]. The diatomite, by virtue of its very high surface area
(BET: 17,000 m2/kg) comparable to microsilica [15]
therefore can strongly fix the Ca2+ contributing electrical Fig. 3. XRD patterns of LDE with different calcined temperatures. H = hea-
matite; I = illite; K = kaolinite; M = muscovite; MT = montmorillonite;
double layers. As Ca ion can generate the narrow double
Q = quartz.
layer thickness, the strong interaction of diatomite particles
takes place and thus plasticity index enhance. The increase of
PI helps in resisting crack forming after pressing due to a containing in LDE, respectively. Phase transformations on
decrease in residual stress. calcinations monitored by XRD of cooled products are shown
Fig. 2 shows the results of DTA and TGA of LDE on heating. in Fig. 3. At 700 8C, dehydroxylation of kaolinite and
Endothermic peaks are observed at 92 8C and 490 8C with montmorillonite results in the collapses of clay mineral
corresponding mass losses of 10 and 3.5%, respectively. The structures and left with illite and muscovite as confirmed by
peaks are ascribed to losses of adsorbed water on particle the disappearances of montmorillonite and kaolinite main
surfaces of LDE and dehydroxylation of clay minerals peaks at 6.58 and 12.58 (2u), respectively. Calcined clay

Fig. 1. SEM photomicrographs of as-received LDE particles.

474 K. Pimraksa, P. Chindaprasirt / Ceramics International 35 (2009) 471–478

Table 2
Mechanical properties of bricks with different water content
Water content (%) Dry density (g/cm3) Water absorption (%) Shrinkage (%) Compressive strength (MPa)
45 1.10 62 0.48 13.0
50 1.15 63 0.48 14.5
55 0.92 68 0.50 13.5
60 0.94 72 0.56 10.0
Note: Ca/Si = 0.23 and 6 days pre-curing.

Table 3
Mechanical properties of bricks with different periods of pre-curing
Pre-curing (days) Bulk density (g/cm3) Water absorption (%) Shrinkage (%) Compressive strength (MPa)
3 0.96 64 0.48 12.5
5 0.91 65 0.51 13.0
6 1.02 64 0.61 14.5
7 0.94 63 0.55 14.0
11 0.87 67 0.60 9.0
Note: Ca/Si = 0.23 and water content of 50%.

minerals contain highly charged surfaces, thus can be active in treatment. The strength developed by curing at ordinary
fixing Ca ions [18]. temperature results from CSH gel formation. The highest
mechanical strength and bulk density of brick are obtained with
3.2. Effect of water content 6 days pre-curing. Less than 3 days pre-curing promotes the
cracking within bricks during the hydrothermal process due to
The results of mechanical properties of brick with insufficient green strength. For longer pre-curing period, the
different water contents are shown in Table 2. Bricks with reaction is quite advanced with more well-developed products
50% mixing water show the highest strength of 14.5 MPa. In and less water in the pore system. The CSH gel can be
this case, Ca2+ ions are fixed to the faces of clay particles transformed into the new CSH phases with higher degree of
resulting in a reduction of the repulsive forces and clay crystallinity at high temperature and a sufficient amount of the
particles become flocculated. Moreover, more space is pore water is required for the reaction. The length of pre-curing
sufficient for reaction products to grow undisturbed. An periods thus produces brick with lower strength.
increase in the mixing water content beyond optimum value
disperses the solid particles and increases the shrinkage due 3.4. Effect of lime content
to overloading pore water [10] and thus causes the reverse
compaction effect due to the widening of the electrical The results of mechanical properties of brick with various
double layers [19]. Water/solid ratio is an important lime contents and corresponding Ca/Si ratio are shown in
parameter for compaction and for hydration of cementitious Table 4. Strength and bulk density of bricks increase and water
materials. absorption decreases with an increase in Ca/Si ratio as a result

3.3. Effect of pre-curing period

The results of test on mechanical properties of brick with

different pre-curing periods are shown in Table 3. Pre-curing
stage is needed to let green bricks obtain a certain green
strength to avoid cracking when subjected to hydrothermal

Table 4
Properties of bricks with various Ca/Si ratios
Ca/Si Bulk Water Compressive
density (g/cm3) absorption (%) strength (MPa)
0.14 1.05 67 13.0
0.23 1.02 64 14.5
0.32 1.27 47 15.5
0.55 1.29 45 16.5
0.86 1.29 41 17.0
1.30 1.38 43 17.0
Fig. 4. XRD patterns of LDE bricks with various ratios of Ca/Si. C = calcite;
Note: 50% mixing water and 6 days pre-curing. CSH = calcium silicate hydrate; G = gismondine; Q = Quartz.
 K. Pimraksa, P. Chindaprasirt / Ceramics International 35 (2009) 471–478 475

Fig. 5. SEM photomicrographs of LDE bricks with various ratios of Ca/Si: (a) 0.14; (b) 0.23; (c) 0.32; (d) 0.55; (e) 0.86; (f) 1.30.

of reductions in LDE content. Increase in strength is, however, alumina at their lattices. It suggests that the illite and muscovite
from increases in lime content and hence additional hydration. are less involved in the pozzolanic reaction than kaolinite and
At low Ca/Si ratio (<0.7), amorphous Z-phase CSH is obtained montmorillonite because illite and muscovite require a higher
while at high Ca/Si ratio (0.7–1.5), 14 Å tobermorite is lime content to initiate the chemical reaction. This is in a good
obtained [20] and its degree of crystallinity tends to decrease agreement with XRD results since their peaks have collapsed
[21]. Different types of CSH are responsible for different when the Ca/Si ratio reaches 1.3.
strength behaviors due to their different characteristics. By the The morphological characteristics of bricks are shown in
smaller size, the higher aspect ratio and the larger specific Fig. 5. Fig. 5(a)–(c) show the photos of CSHs and Fig. 5(d)
surface area of the particles, the higher attractive forces shows amorphous sieve-liked CSH phase. At high Ca/Si ratio of
between particles can be obtained. 0.86, the CSH is different from that obtained from the lower Ca/
Fig. 4 shows XRD patterns of CSH compounds with Ca/Si Si ratio as shown in Fig. 5(e). At very high Ca/Si ratio of 1.30,
ratio of 0.14 and greater. At Ca/Si ratio of 1.30, CSH phase is tobermorite mostly appears as shown in Fig. 5(f) similar to the
detected as a sharp peak indicating tobermorite mineral. Calcite findings of Zheng and Wang [23]. The Ca/Si ratio and the
(CaCO3) is also obtained at Ca/Si ratio of 1.3 due to a reactivity of primary components are important factors
carbonation of excess Ca(OH)2. The strong bricks with less determining mineral composition of the final products.
than 40% lime (Ca/Si < 1.30) are due to the formation of not
well-developed crystalline CSH confirmed by XRD. Zeolite- 3.5. Effect of gypsum
like mineral named ‘‘gismondine (Ca4Al8Si8O32
16H2O)’’ is
also detected with Ca/Si ratio of 1.3. Normally, its production The results of mechanical properties of brick with various
requires Ca/Si ratio of 0.5 and Al/Si ratio of 1 while it is percentages of gypsum are shown in Table 5. For 80% LDE
produced with Ca/Si ratio of 0.86 in the present work. This brick, the replacement of 5% lime with 5% gypsum results in a
could be due to some inert silica phases such as crystobalite large reduction in bulk density and a large increase in the water
contained in LDE. The dissolutions of primary quartz in LDE absorption. Additional increase in gypsum in place of LDE
and clay minerals result in supersaturation of new phases as the results in an increase in bulk density and strength and a
peaks of clay minerals disappears and the intensity of quartz
reduces providing the larger amount of CSH when Ca/Si ratio Table 5
increases from 0.14 to 1.3. Properties of brick with different gypsum content
When lime is added to clay minerals, the Ca2+ ions are LDE:lime:gypsum Bulk density Water Compressive
adsorbed on clay minerals and are not available for pozzolanic (Ca/Si) (g/cm3) absorption (%) strength (MPa)
reactions until clay charges are balanced with Ca2+ ions [22]. 80:20:0 (0.32) 1.27 47 15.5
Therefore, there exists two chemical reactions viz., lime and 80:15:5 (0.32) 0.88 66 14.5
silica reaction and lime and alumino-silicate reaction. As such, 75:15:10 (0.42) 0.97 57 15.5
there are cation exchanges on montmorillonite and kaolinite 70:15:15 (0.55) 1.02 32 18.0
surfaces as well as pozzolanic reaction between silica and Note: 50% mixing water and 6 days pre-curing.
476 K. Pimraksa, P. Chindaprasirt / Ceramics International 35 (2009) 471–478

of 0.42, only bassanite remains. At Ca/Si ratio of 0.55, both

gypsum and bassanite are not detected. With an increase in
gypsum content, sulfate ions can be located in CSH structure as
substitution in silicate tetrahedral site. The products contain
mainly CSH and gismondine resulting in relatively high
strength brick. It has been reported that a low Ca/Si ratio
promotes the formation of poorly crystallized CSH and
prevents tobermorite formation [24]. It should be pointed out
here that the left behind bassanite should not exist in a large
quantity since it can hydrate and form gypsum which causes
large expansion and cracks.
Fig. 6. XRD patterns of LDE bricks with various amount of gypsum. B = bas-
The morphology of bricks with gypsum is shown in Fig. 7.
sanite; CSH = calcium silicate hydrate; C = calcite; G = gismondine; Again CSH phases are detected with gypsum contents of 0, 5,
GP = gypsum; Q = quartz. 10 and 15% corresponding to Ca/Si ratio of 0.32, 0.32, 0.42 and
0.55. At high Ca/Si ratio of 0.55, CSH phases as shown in
reduction in water absorption. This is because sulfate from Fig. 7(d) look similar to gypsum added brick at Ca/Si ratio of
gypsum easily attacks Al ions and produces additional 0.55 which is slightly lower than 0.86 of brick without gypsum.
hydration product that contributing to the strength develop-
ment. 3.6. Effect of calcining temperature
It has been shown that the reactions produce CSH and a
small amount of gismondine at low Ca/Si ratio of 0.32. With an The properties of bricks with different calcination tempera-
increase of Ca/Si ratio, the amounts of gismondine and CSH tures of LDE are shown in Table 6. The use of LDE calcined at
increase as confirmed by the enhancement of the intensities of 500 8C produces bricks with high strength (17.4 MPa) and low
XRD peaks shown in Fig. 6. At Ca/Si ratio of 0.32 with 5% density (0.73 g/cm3). It is apparent that dehydroxylation of clay
gypsum addition, gypsum and bassanite are detected. It is minerals at 500 8C contributes to the strength development.
believed that the hydrothermal temperature can transform the With calcination, clay mineral structures contain highly
added gypsum into bassanite (CaSO4
(1/2)H2O). At Ca/Si ratio negative charged surfaces. At high calcination temperature

Fig. 7. SEM photomicrographs of LDE bricks with various amount of gypsum: (a) no gypsum (Ca/Si = 0.32); (b) 5% gypsum (Ca/Si = 0.32); (c) 10% gypsum (Ca/
Si = 0.42); (d) 15% gypsum (Ca/Si = 0.55).
 K. Pimraksa, P. Chindaprasirt / Ceramics International 35 (2009) 471–478 477

Table 6
Properties of brick with different calcined temperature
Calcined temperature (8C) Bulk density (g/cm3) Water absorption (%) Compressive strength (MPa) Thermal conductivity (W/(m K))
Uncalcined 0.88 66 14.5 0.165
200 0.76 56 15.0 0.144
350 0.79 50 15.5 0.152
500 0.73 46 17.5 0.130
700 0.76 49 12.5 0.150
Note: CLDE:lime:gypsum of 80:15:5 (Ca/Si = 0.32), 50% mixing water and 6 days pre-curing.

of 700 8C, strength reduces due to the formation of bassanite.

The reactive clay minerals can be obtained between 500 and
700 8C. XRD peaks, particularly kaolinite and montmorillonite
peaks, disappear in this temperature range as shown in Fig. 3.
The proper calcination temperature of LDE is slightly higher
than 500 8C because the most reactive phases can be attained
right after the dissociation of hydroxyl ions from clay
structures. The DTA and TGA curves shown in Fig. 2 indicate
the proper calcination condition. With calcination, sulfate ions
can be located in the structure of CSH as a silicate ion
substitution while uncalcined condition has no substitution at
the Ca/Si ratio of 0.32. Therefore, the calcinations is beneficial
to the chemical reaction for low Ca/Si ratio. Illite and
muscovite do not undergo pozzolanic reaction with lime at low
Fig. 8. XRD patterns of bricks with different calcined temperatures (Ca/ Ca/Si ratio as they need high calcine temperature of 700 8C.
Si = 0.32). B = bassanite; C = calcite; CSH = calcium silicate hydrate; G = gis- The reduction of bulk density with an increase in calcination
mondine; Q = quartz; I = illite; M = muscovite. temperatures is due to the increase of negatively charged clay
surfaces. This results in an increase of particle–particle

Fig. 9. SEM photomicrographs of bricks with different calcined temperatures (Ca/Si = 0.32): (a) 200 8C; (b) 350 8C; (c) 500 8C; (d) 700 8C.
478 K. Pimraksa, P. Chindaprasirt / Ceramics International 35 (2009) 471–478

repulsive forces of CLDE and the formations of pozzolanic Kurzweil, Vienna University; and Mrs. Nongkarn Chaiwong,
reaction products and gismondine. An increase of bulk density Chiang Mai University are gratefully acknowledged.
is due to the reduction of the repulsive forces on account of the
disappearance of meta-stable phases. The results of thermal References
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