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Chinese Journal of Materials Research  2015, Vol. 29 Issue (7): 542-548    DOI: 10.11901/1005.3093.2014.532
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Diethanolamine Controlled Hydrothermal Synthesis of Submicron Spherical CoAl2O4 Pigments
Xingfuzi ZHONG1,Xilong LU1,Chun'e CAO1,**(),Yunxia CHEN1,2,Huarong SHEN1
1. School of Material Science and Engineering, Jingdezhen Ceramic Institute, Jingdezhen 333403, China
2. Jiangxi Key Laboratory of Advanced Ceramic Materials, Jingdezhen 333000, China
Cite this article: 

Xingfuzi ZHONG,Xilong LU,Chun'e CAO,Yunxia CHEN,Huarong SHEN. Diethanolamine Controlled Hydrothermal Synthesis of Submicron Spherical CoAl2O4 Pigments. Chinese Journal of Materials Research, 2015, 29(7): 542-548.

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Abstract  

Submicron spherical CoAl2O4 pigments were hydrothermal synthesized using CoCl2·6H2O and AlCl3 as raw materials, NaOH as the precipitant and diethanolamine (DEA) as capping agent, respectively. The effect of the concentration of raw materials, the ratio of nCo/nAl and the amount of DEA on the phase composition, particle size and morphology as well as the chroma of the as-prepared pigments was investigated by means of XRD, TEM and calorimetric analysis. The results show that submicron spherical CoAl2O4 pigments with size in a range of 100-230 nm could be synthesized under the conditions of nCo/nAl=1: 2, Co2+ concentration 0.05 mol/L and DEA 12%(V/V). The formation of spherical particles was analyzed from the point of view of kinetically controlled crystal growth in the presence of DEA. It follows that during the nucleation and growth process of the crystalline particles, DEA molecules can be adsorbed onto the edges and vertices of the particles in a highly oriented manner thus causing steric hindrance, which enable the spherical growth of the crystalline particles to be possible.

Key words:  inorganic non-metallic materials      spherical CoAl2O4      hydrothermal method      diethanolamine      capping agent     
Received:  26 September 2014     
Fund: *Supported by National Natural Science Foundation of China No.51162016, and Graduate Innovation Foundation of Jingdezhen Ceramic Institute No.JYC1105.

URL: 

https://www.cjmr.org/EN/10.11901/1005.3093.2014.532     OR     https://www.cjmr.org/EN/Y2015/V29/I7/542

c(Co2+) (molL-1) nCo/nAl DEA proportion (%)
0.3、0.15、 0.1、0.05 1:2 12
0.05 1:1.5、1:1.75、 1:2、1:2.25、1:2.5 12
0.05 1:2 3、6、9、12、15
Table 1  Experimental arrangements
Fig.1  XRD patterns of samples with different Co2+ ion concentrations
Fig.2  TEM photos of samples with different Co2+ ion concentrations (a) 0.3 mol/L, (b) 0.15 mol/L, (c) 0.1 mol/L, (d) 0.05 mol/L
c(Co2+) (molL-1) L* a* b*
0.05 40.52 -9.25 -18.76
0.1 41.79 -8.79 -13.12
0.15 42.23 -8.93 -11.99
0.3 47.17 -8.17 -23.28
Table 2  Colorimetric test results of samples prepared at different Co2+ ion concentrations
Fig.3  XRD patterns of samples with various nCo/nAl
nCo/nAl L* a* b*
1:1.5 62.1 -1.81 -11.76
1:1.75 49.5 -6.29 -18.89
1:2 42.01 -8.98 -19.96
1:2.25 44.23 -8.75 -19.04
1:2.5 45.71 -8.92 -18.87
Table 3  Colourimetric test results of samples with various nCo/nAl
Fig.4  XRD patterns of samples with different DEA proportions
Fig.5  TEM images of samples prepared with different DEA proportions (a) 3%, (b) 6%, (c) 9%, (d) 12%, (e) 15%
DEA proportion/% L* a* b*
3 42.22 -9.23 -15.4
6 42.02 -9.46 -16.98
9 41.33 -9.53 -17.31
12 40.31 -9.15 -19.55
15 39.43 -9.89 -17.02
Table 4  Colourimetric test results of samples with different DEA proportions
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