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Materials Letters 62 (2008) 2096 2098

www.elsevier.com/locate/matlet

Preparation of nano-CaO using thermal-decomposition method

Zhen-Xing Tang , David Claveau, Ronan Corcuff, Khaled Belkacemi , Joseph Arul
Department of Food Science and Nutrition, Laval University, Quebec, Canada, G1K 7P4
Received 18 July 2007; accepted 12 November 2007
Available online 28 November 2007

Abstract
CaO is an important inorganic material, which can be used as catalyst, toxic-waste remediation agent, adsorbent etc. In order to make use of
CaO, nano-CaO was prepared by thermal-decomposition method using Ca(NO3)2.4H2O as precursor, NaOH aqueous solution as precipitant, and
ethylene glycol as medium in this paper. Characteristics of samples were measured by TGA, XRD, TEM et al techniques. The results showed that
the size of nano-CaO about 14 nm could be obtained under the conditions (calcinations temperature 500 C, calcinations time 1.5 h, heating rate of
calcinations 5 C/min). It is a very simple and effective method to prepare nano-CaO.
2007 Elsevier B.V. All rights reserved.
Keywords: CaO; Nano-particle; Preparation; Nanomaterials; Minerals

1. Introduction
Calcium oxide (CaO) is an exceptionally important material,
which is used as catalyst, toxic-waste remediation agent, or as
an additive in refractory, paint as well as for fundamental and
application studies [1]. Ultra-fine metal oxide particles can be
used as bactericide, adsorbent, and catalyst. CaO in particular
has shown great promise as a destructive adsorbent for toxic
chemical agent [2].
Few literatures have been mentioned on the preparation of
nano-CaO. There are mainly two methods on the preparation
of nano-CaO according to the literatures. One is thermal
decomposition [3,4]. The other is solgel [1]. Though CaO
nano-particles can be obtained about 4 nm through solgel
method, the cost is very high. What's more, the process is very
complicated and time-consuming. So it is very difficult to
apply solgel method into industry. Thermal decomposition
method has some advantages such as simple process, low cost,
easiness to obtain high purity product etc. So it is quite
promising and facile to be applied into industry. But for
thermal decomposition method, CaO is often obtained directly

Corresponding authors.
0167-577X/$ - see front matter 2007 Elsevier B.V. All rights reserved.
doi:10.1016/j.matlet.2007.11.053

through calcining CaCO3. High calcinations temperature is

needed. It is very difficult to get nano-scale CaO, but
Micrometer CaO (above 100 nm), directly through calcining
CaCO3 [5].
In this paper, CaO nano-particles were prepared by thermaldecomposition method, Ca (NO3)2.4H2O as precursor, NaOH
aqueous solution as precipitant, and ethylene glycol as medium.
It is the first time to prepare nano-CaO using Ca(OH)2 as
precursor. And calcinations temperature is very low. It is a good
method to prepare nano-CaO.
2. Experimental
2.1. Materials
Ca(NO3)2. 4H2O (Mallinkrodt baker inc, ACS); Sodium
hydroxide (BMD chemicals inc, ACS); Ethylene glycol (99%)
was all purchased from BDH inc; Other reagent were gotten
from local supplies.
2.2. Preparation of CaO nano-particles
11.81 g Ca(NO3)2. 4H2O was dissolved in ethylene glycol
solution (25 ml). 12.5 ml NaOH (2.10 g) was added into above
mixture under vigorous stirring. In order to get uniform size

Z.-X. Tang et al. / Materials Letters 62 (2008) 20962098

2097

Fig. 1. TGA of Ca(OH)2. Conditions: hold for 1 min at 50 C; heat from 50 C to 1000 C at the rate 10 C/min; hold for 1 h at 1000 C.

nanoparticles, after it being stirred 10 min, the gel solution was

kept about 5 h at static state. Then it was washed using water.
After that, it was dried under vacuum drying. Finally, different
sizes of CaO nano-particles could be obtained through
calcining.

2.3. Analysis methods

TGA measurements were carried out using Netzsch STA 409
Apparatus; The size and Particle size distribution in ethanol was
recorded on Submicron Particle Sizer (NICOMP 370, USA);

Fig. 2. XRD of nano-CaO. Nano-particles were obtained at calcinations temperature 500 C, calcinations time 1.5 h, heating rate 5 C/min.

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Z.-X. Tang et al. / Materials Letters 62 (2008) 20962098

Fig. 3. The sizes distribution of CaO nano-particles. Nano-particles were

obtained at calcinations temperature 500 C, calcinations time 1.5 h, heating rate
5 C/min.

TEM photomicrographs were obtained using Philips 201

Transmission Electron Microscope. The pictures were taken at
80 kV. The deposit was scraped away from the support and then
transferred to the Fromvar 1595 E (Merck) membrane coated
Cu grid (mesh 400); Rigaku Geiferflex X-ray diffractometer
with Ni-filtered Cu Ka radiation (40 kV, 30 mA) was used to
determine the crystallinity and phase of the samples.
3. Results and discussion
Different intermediates have different decomposition temperatures
[6,7]. According to TGA of Ca(OH)2 (Fig. 1), There were two major
weight losses: from 350 to 500 C and from 500 to 700 C. The
exothermic peak at 400 C was due to the removed chemisorbed water.
This result was the same as reported by Olga [2]. The peak at 400 C
was assigned to the decomposition of Ca(OH)2 to CaO+ H2O. This
20% weight loss was well corresponded with the calculated weight loss
from the reaction. CaO nano-particles could be obtained at 500 C
through calcining the intermediate Ca(OH)2 in this paper. The
calcinations temperature was much lower than that reported by
Bellobono [4]. He prepared CaO through heating CaCO3 directly.

Fig. 4. TEM of nano-CaO. Nano-particles were obtained at calcinations

temperature 500 C, calcinations time 1.5 h, heating rate 5 C/min.

Calcinations temperature was more than 750 C. It was also lower than
that reported by Olga [2]. He prepared CaO nano-particles through sol
gel method. Calcinations temperature was about 600 C. For
intermediates Ca(OH)2 and CaCO3, CaCO3 decomposition temperature is higher than Ca(OH)2 at the same conditions. So, nano-CaO can
be obtained under low calcining temperature.
The structure of nano-CaO was first characterized by XRD (Fig. 2).
All peaks were consistent with the peaks of standard CaO. XRD
patterns of Fig. 2 showed broadening of the peaks indicative of the ultra
fine nature of the crystallite. The crystallite size calculated using
Scherrer's formula was about 14 nm. No peaks from any other phases
of CaO were observed. XRD pattern was same as reported by Olga [2].
The sizes distribution was presented in Fig. 3. From Fig. 3, the sizes
distribution was narrow. Nano-CaO size was between 12 nm and
18 nm. The distribution was consistent with XRD result.
TEM of CaO nano-particles was illustrated in Fig. 4. From Fig. 4,
CaO nano-particles could be dispersed very well in ethanol. Few
aggregate could be found. CaO powder appeared with an average
particle size about 14 nm. The result matched with the particle size,
calculated using XRD. The particles were regular and spherical in
shape.

4. Conclusions
CaO nano-particles were prepared by thermal-decomposition method using Ca(NO3)2.2H2O as precursor, NaOH
aqueous solution as precipitant, and ethylene glycol as medium.
And the smallest size was 14 nm. It was simple and effective
method to prepare CaO nano-particles.
Acknowledgement
This work was supported by a grant from Conseil des
Recherches en Pche et en Agroalimentaire du Qubec
(CORPAQ).
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