J. Am. Ceram. Soc.
, 85 [9] 2171–76 (2002)
journal
Department of Chemistry, Gorakhpur University, Gorakhpur 273009, India
Calcium silicate hydrate was prepared by hydrothermal reac-
tion between calcium oxide and silica (C/S ⴝ 2.0) at a
temperature of 205°–215°C and a pressure of 17–19 bar. This
reaction with decomposition at 900°C produced highly reactive
␤-dicalcium silicate (specific surface area 4.55 m2/g) contam-
inated with small amounts of wollastonite as an impurity.
Infrared spectral studies have shown that ␤-dicalcium silicate
prepared at 900°C is less symmetric compared with the control
prepared at 1450°C using boron trioxide as a stabilizer. The
specific surface area of ␤-dicalcium silicate decreased with
temperature. The hydration studies were done by determining
the nonevaporable water, calcium hydroxide (CH) contents,
and specific surface area of the hydrated samples. X-ray
diffraction studies were also done. The results showed that
prepared ␤-dicalcium silicate is highly reactive. Calcium chlo-
ride (1.0 wt%) and gypsum retard the hydration. Possible
causes of high reactivity have been discussed.
I. Introduction
P ORTLAND cement clinker is prepared at a very high temperature,
and the average theoretical energy needed is 1750 kJ/kg
clinker. The major portion of this energy is expended in the
dissociation of calcium carbonate of the raw mix. This energy can
be reduced considerably if the calcium carbonate of the raw mix
and, consequently, the tricalcium silicate content of the clinker is
reduced and the dicalcium silicate content is increased.1 However,
dicalcium silicate-rich cements generally harden so slowly that
their usefulness as binding agents is limited or indeed inadequate.
Murdock and Blackadge2 claimed that the cements in which a high
proportion of dicalcium silicate is formed have high resistance to
chemical attack and relatively low drying shrinkage and, therefore,
are the most durable of the Portland cements.
To enhance the hydraulic hardening capacity of belite cements,
numerous methods have been used to produce highly reactive
␤-dicalcium silicate at low temperatures. Any approach to synthe-
size ␤-dicalcium silicate at low temperatures depends on the
ability to combine reagents of high reactivity so that the kinetics of
formation are reasonably fast. When calcium oxide or other oxides
are formed by decomposition reactions, they are initially in a
highly reactive form because of high surface area and poor
crystallinity.3
Karlj et al.4 synthesized ␤-dicalcium silicate by firing a stoi-
chiometric mixture of calcium oxlate and amorphous silica at
950°C. Roy and Oyefesobi5 prepared highly reactive ␤-dicalcium
silicate by gel and spray drying techniques. The spray drying
technique involved spraying droplets of solution into a vertical
tube furnace preheated to temperatures generally between 750°
and 940°C. The 2:1 composition of calcium oxide and silica
reacted most favorably at 940°C. Nanru et al.6,7 prepared a type of
P. W. Brown—contributing editor
Manuscript No. 188155. Received March 15, 2001; approved September 24, 2001.
Financial assistance for this work provided by UGC, New-Delhi.
2171
Highly Reactive ␤-Dicalcium Silicate
Nakshatra B. Singh, Sarita Rai, and Neelam Singh
active ␤-dicalcium silicate by hydrothermal treatment of a stoichi-
ometric mixture of calcium oxide and silica at 100°C and then
igniting at 850°–950°C. Synthesis of dicalcium silicate at 750°C
from calcium nitrate, silica, and gypsum has also been reported.8
Because the calcium nitrate melts and then decomposes, the
reaction starts in the presence of a liquid phase, and sulfate ions
from the gypsum are incorporated into dicalcium silicate forming
solid solution. The use of calcium nitrate produces corrosive fumes
of NOx. Salts of K⫹, Na⫹, Sr2⫹, and Ba2⫹ have also been used as
an activator to ␤-dicalcium silicate.9 Ludwig and Wolter10 found
that an addition of ground clinker of normal composition substan-
tially accelerates the hardening of belite cements. Odler and
Schuppstuhl11 reported that pure tricalcium silicate acts as an
activator and accelerates the hardening of ␤-dicalcium silicate.
Various other investigators12,13 found that rapid cooling of the
clinker enhances the hydraulic hardening capacity of belite.
Ishida and co-workers14 –17 and Komljenovic et al.18 studied in
detail the preparation and hydration of highly reactive ␤-dicalcium
silicate obtained from the thermal decomposition of calcium silicate
hydrates prepared hydrothermally. There are three forms of calcium
silicate hydrates having C/S ⫽ 2.0: hillebrandite (Ca2(SiO3)(OH)2),
␣-dicalcium silicate hydrate (Ca2(SiO4H)(OH)), and dellaite
(Ca6(Si2O7)(SiO4)(OH)2). They decompose to ␤-dicalcium silicate at
temperatures of 520°–540°, 400°– 450°, and 640°–700°C, respec-
tively. The specific surface area of ␤-dicalcium silicate obtained from
the decomposition of hillebrandite at 600°C was found to be 7 m2/g,
stable at room temperature without any stabilizer, and highly reactive.
According to Ishida et al.,17 the hydration reactions completed within
28 d and 1 d at 25° and 80°C, respectively, when w/s ⫽ 0.5 was used.
Chatterjee19,20 reviewed and discussed nontraditional methods for the
preparation of belite cements.
From a survey of the literature, it appears that continuous efforts
are being made to prepare highly reactive ␤-dicalcium silicate at
low temperatures so that a better quality cement can be obtained at
a low cost. In this study, attempts have been made to prepare
highly reactive ␤-dicalcium silicate from the thermal decomposi-
tion of hydrated products obtained by hydrothermal reaction
between calcium oxide and aerosil (C/S ⫽ 2.0). The effect of 1.0
wt% calcium chloride and gypsum on the hydration has also been
investigated. Boron trioxide stabilized ␤-dicalcium silicate has
been used as a control sample.
II. Experimental Procedure
Calcium carbonate (Merck, Darmstadt, FRG) and Aerosil 200
(Merck)(containing 2.25% water) were used as the starting mate-
rials. Calcium chloride and gypsum (Merck) were used as an
admixture during hydration.
III. Methods
(1) Preparation of Highly Reactive ␤-Dicalcium Silicate
Calcium oxide was freshly prepared by heating calcium carbon-
ate at 1050°C for 1 h. Calcium oxide and Aerosil 200 were mixed
in a stoichiometric ratio (C/S ⫽ 2.0). The dry mix was thoroughly
mixed in a plastic bottle by shaking on a roller for 24 h. Water was
then added to produce w/s ⫽ 10. This was again shaken well on the
roller for 4 h. The entire mass was placed in a porcelain dish and
2172 Journal of the American Ceramic Society—Singh et al. Vol. 85, No. 9

kept in an autoclave at 205°–215°C for 24 h at a pressure of 17–19
bar. The autoclave took nearly 24 h to achieve this temperature and
pressure. The hydrated mass was then heated at 105°C for 3 h to
remove excess water. This was further heated at varying temper-
atures (700°–1200°C) for 1 h each to produce ␤-dicalcium silicate.
The ␤-dicalcium silicate obtained at 900°C was used for detailed
investigations. The product of hydrothermal reaction was analyzed
by X-ray diffraction (XRD) and thermogravimetry and differential
thermal analyzer (TG–DTG–DTA) techniques. ␤-Dicalcium sili-
cate obtained at 900°C was characterized by XRD.
Surface areas of ␤-dicalcium silicate obtained at different
temperatures (700°–1200°C) were determined by BET (Brunauer–
Emmet–Teller) apparatus. Free lime values were determined by
modified Franke method.21
(2) Preparation of ␤-Dicalcium Silicate Using Boron
Trioxide as Stabilizer
Calcium carbonate and areosil were mixed in 2:1M ratio; 0.5
wt% boron trioxide was added into the same mix. The mixture was
thoroughly mixed and pelletized (1.12 cm ⫻ 1.0 cm) by applying
a pressure of 1.4 kN. The pellets were fired at 1450°C for 3 h to
produce ␤-dicalcium silicate. The specific surface area was 0.5
m2/g.
(3) FTIR Spectral Studies
Fourier transform infrared (FTIR) spectra of ␤-dicalcium sili-
cate prepared at 900°C (highly reactive) and that prepared in a
conventional manner at 1450°C using boron trioxide as stabilizer
(control) were recorded with an FTIR spectrometer (Model 5300,
Jasco, Tokyo, Japan) in KBr phase.
III. Results and Discussion
The XRD pattern of C2SHx (Fig. 1) shows peaks caused by the
presence of hillebrandite and xonotlite, indicating that C2SHx is a
mixture of the two minerals. (A list of the nomenclature used in
this paper is given in the Appendix.) TG–DTG–DTA studies
support these results. DTA gives two endothermic peaks at 550°
and 735°C caused by decomposition of hillebrandite and xonotlite
phases, respectively. Mitsuda et al.22 also reported that hillebran-
dite is always associated with the impurity of xonotlite. From our
results and the literature data, it can be inferred that the type of
product from hydrothermal reaction between lime and silica
depends on C/S ratio, type of silica used, temperature and pressure,
and the time of heating and stirring during the reaction.
C2SHx when heated at 700°C for 1 h gave ␤-dicalcium silicate
associated with small amounts of wollastanite as an impurity.
Because in the TG experiment weight losses in C2SHx continued
up to 850°C, ␤-dicalcium silicate was prepared by heating C2SHx
at 900°C. The ␤-dicalcium silicate thus obtained was also contam-
inated with small amounts of wollastanite as indicated by the XRD
pattern. Wollastanite may be formed by the decomposition of
xonotlite present in C2SHx.
SEM studies (Fig. 2(a)) revealed that the morphology of C2SHx
is needle shaped and when it is heated at 900°C to give
␤-dicalcium silicate, the morphology remained unchanged (Fig.
2(b)). This showed that highly reactive ␤-dicalcium silicate is
formed from C2SHx topotactically.

(4) Hydration Studies

Hydrations of highly reactive ␤-dicalcium silicate obtained at
900°C were conducted at a w/s ⫽ 2.5 (because of high surface
area, a larger amount of water was required to make a paste) at
room temperature (20°C). The hydrations were stopped at different
intervals. The effect of 1.0 wt% calcium chloride and gypsum on
the hydration was also studied. Boron trioxide stabilized
␤-dicalcium silicate was hydrated as a control sample at a w/s ⫽
0.5.
CH content in the hydrated samples was determined by modi-
fied Franke method.21 A hydrated sample of ⬃1 g was refluxed
with 40 mL isopropyl alcohol-acetoacetic ester (20:3) mixture for
1 h and the filtrate was titrated against 0.1 N HCl using bromo-
phenol blue as an indicator. The nonevaporable water contents
(Wn) were determined by measuring the weight loss at 1000°C.
Specific surface area of the hydrated samples was determined
by area meter (BET). XRD patterns of the hydrated samples and a
scanning electron microscopic (SEM) picture of ␤-dicalcium
silicate hydrated at 14 d were also recorded.

Fig. 1. XRD pattern of hydrothermally prepared calcium silicate hydrate Fig. 2. SEM micrographs of (a) hydrothermally prepared calcium silicate
(“X” denotes xonotlite, and “H” represents hillebrandite). hydrate and (b) highly reactive ␤-dicalcium silicate obtained at 900°C.
September 2002 Highly Reactive ␤-Dicalcium Silicate 2173

Because of high specific surface area of highly reactive

Fig. 3. Variation of surface area of highly reactive ␤-dicalcium silicate
obtained by thermal decomposition of hydrothermally prepared calcium
silicate hydrate at different temperatures (heating duration at each temper-
ature: 1 h).
␤-Dicalcium silicate obtained by heating dicalcium silicate
hydrate at different temperatures, contain varying amounts of free
lime and possess different specific surface area. Both the surface
area and the free lime decreased with the increase of temperature
(Figs. 3 and 4) as usually expected.
␤-dicalcium silicate (4.5 m2/g), the paste could be prepared at a w/s
ratio of 2.5. The variation of nonevaporable water contents of the
hydrated samples is shown in Fig. 5. There is very little increase in the
Wn values up to 3 d of hydration; however, after that, there is a rapid
increase up to 28 d (the time of investigation). A nucleation and
growth mechanism is suggested in which the dormant period is
characterized by the formation of critical size nuclei of hydration
products. Thereafter, hydration proceeds at a much higher rate. Such
mechanisms have been described for tricalcium silicate hydration by
Ludwig and Singh.23 As the hydration progressed, the amount of
hydration product increased. Probably the hydration products are
colloidal in nature as indicated by increased surface area (Fig. 6). The
surface area of hydrated ␤-dicalcium silicate increased significantly
up to 28 d. Ishida et al.,24 on the other hand, reported that the specific
surface area of hydrated ␤-dicalcium silicate increased with curing
time and reached a maximum value at 7 d of hydration. This
difference may be because of differences in the specific surface area
of the ␤-dicalcium silicate. Further, it appears that the hydration
products are porous in nature and do not greatly hinder the approach
of water molecules to the fresh surface of ␤-dicalcium silicate, and as
a result the reaction continued. If we consider the following stoichi-
ometry25 for the hydration reaction
2C2S ⫹ 5H ⫽ C3S2H4 ⫹ CH

Fig. 4. Variation of free lime in highly reactive ␤-dicalcium silicate obtained by thermal decomposition of hydrothermally prepared calcium silicate hydrate
at different temperatures (heating duration at each temperature: 1 h).

Fig. 5. Variation of nonevaporable water contents with hydration time: w/s ⫽ 2.5 for highly reactive ␤-dicalcium silicate, and w/s ⫽ 0.5 for control.
2174 Journal of the American Ceramic Society—Singh et al.
Fig. 6. Variation of specific surface area of hydrated ␤-dicalcium silicate with hydration time: w/s ⫽ 2.5 for highly reactive ␤-dicalcium silicate, and w/s ⫽
0.5 for control.
The nonevaporable water content for complete hydration will be
26.12%. In the present case, Wn value is 23.8%. This gives the
degree of hydration of 91% at 28 d of hydration.
In the presence of 1% calcium chloride and gypsum, the
nonevaporable water contents and specific surface area of hydrated
␤-dicalcium silicate are lower compared with that of ␤-dicalcium
silicate hydrated alone. It appears that both calcium chloride and
gypsum are adsorbed at the surface of ␤-dicalcium silicate and
makes the surface less reactive, resulting in the decrease of
hydration. It is already reported26 that gypsum is adsorbed at the
surface of hydrated tricalcium silicate. The Wn and specific surface
area values in the case of control are much lower, indicating a
lesser degree of hydration compared with that of ␤-dicalcium
silicate.
The variation of CH content with hydration time is given in Fig.
7, and the values increase with time and are much higher than the
control and those reported by Nanru et al.6 for highly reactive
␤-dicalcium silicate. Okada et al.,17 however, found that almost no
CH is formed even after complete hydration. In the present system,
because the w/s ratio is very high (w/s ⫽ 2.5), it is possible that
CH crystals are formed easily and the amount increased with time.
The CH contents in the presence of calcium chloride and gypsum
are lower compared with that of highly reactive ␤-dicalcium
silicate, but at 28 d of hydration the values are almost equal.
XRD patterns of ␤-dicalcium silicate hydrated at different
intervals are shown in Fig. 8. At 1 and 2 d of hydration, there is a
very little change in the intensities of the X-ray peaks, indicating
Fig. 7. Variation of CH contents with hydration time: w/s ⫽ 2.5 for highly reactive ␤-dicalcium silicate, and w/s ⫽ 0.5 for control.
Vol. 85, No. 9
that the hydration is very slow; however, at 7 d, the extent of
hydration is increased as indicated by the decrease of the intensi-
ties of the peaks of ␤-dicalcium silicate and an enhanced peak at
2␪ ⫽ 18° (d ⫽ 4.9 Å) because of CH formation. Further, at 14 d
of hydration, the intensities of the peaks caused by ␤-dicalcium
silicate are decreased considerably and the intensity of the peak
caused by CH formation is increased significantly. This indicates
that the extent of hydration is much higher. This has been
supported by SEM micrographs. The results conform with the
results obtained by nonevaporable water contents and CH deter-
minations on the hydrated samples of ␤-dicalcium silicate. At 28 d
of hydration, the intensity of the peaks caused by ␤-dicalcium
silicate are almost negligible but have not vanished completely,
indicating that the hydration is still not complete. However, the
intensities at 2␪ ⫽ 29.16°, 31.82°, 49.895° (d ⫽ 3.06, 2.81, 1.8263
Å, respectively) are appreciable. This may be because of the
formation of C-S-H. The intensity of the CH peak at 2␪ ⫽ 18° is
lower than that of the sample hydrated at 14 d. There may be two
possibilities: (i) a part of CH is amorphous, or (ii) a part of CH has
reacted with C-S-H gel. The possibility of CH being amorphous in
nature is more because the extraction method gives higher values
of free lime at 28 d compared with that at 14 d.
The results have shown that the reactivity of highly reactive
␤-dicalcium silicate is much higher compared with that of
␤-dicalcium silicate prepared in a conventional manner (control).
The factors that may contribute toward high reactivity of
␤-dicalcium silicate may be (i) high surface area, (ii) imperfection,
September 2002 Highly Reactive ␤-Dicalcium Silicate 2175

IV. Conclusions

The hydrothermal reaction between calcium oxide and silica

(C/S ⫽ 2.0) gave a mixture of hillebrandite and xonotlite, which
when heated to ⬎700°C gave ␤-dicalcium silicate of high specific
surface area. The decomposition reaction appeared to be topotactic
in nature. ␤-dicalcium silicate was always associated with small
amounts of wollastanite. Hydration studies revealed that it is
highly reactive. A 1.0 wt% calcium chloride and gypsum retard the
hydration. The main causes of higher reactivity of ␤-dicalcium
silicate may be high specific surface area, grain boundaries, and
distorted [SiO4]4⫺ tetrahedron present in the molecule.

Appendix

Nomenclature Used

The following terms and symbols have been used in this paper:

Table AI. Nomenclature Used

Symbol/term Description

C2SHx Hydrothermally prepared calcium silicate

hydrate
␤-C2S ␤-dicalcium silicate
␤-C2S-CaCl2 ␤-dicalcium silicate hydrated in the presence
of 1.0 wt% calcium chloride
␤-C2S-gypsum ␤-dicalcium silicate hydrated in the presence
of 1.0 wt% gypsum
Control ␤-dicalcium silicate stabilized with boron
trioxide
Wn Nonevaporable water content
CH Lime in the hydrated sample

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