Preparation of Zirconium Sol by Precipitation Method

Abstract:

Zirconium sol was prepared using precipitation method. In the process, ZrO(OH)₂ precipitate was firstly obtained through the addition of strong base into the zirconium ions, and then was washed to remove the chloride ion. Lastly, the obtained ZrO(OH)₂ precipitate was dissolved in nitric acid solution to obtain the white mixed solution. The clear and transparent zirconium sol can be obtained after heated the white mixed solution in a water bath. In this study, the effects of three precipitating agents on the properties of zirconium sol were studied. Zirconium sol prepared by using ammonia as precipitating agent is easy to peptize, while its viscosity is very high. On the other hand, zirconium sol prepared by using urea as precipitating agent exhibits low solid content. Notably, the performance of zirconium sol prepared using ammonia and NH₄Cl solution as precipitating agent is best due to its low viscosity and high solid content. In addition, zirconium sol, xerogel and zirconium dioxide powder prepared using ammonia and NH₄Cl solution as precipitating agent were systematically characterized by SEM, viscometer, XRD, FTIR. The optimal zirconium sol was synthesized using a peptizing time of 8 h under a peptizing temperature was 80 °C, and the dried amorphous xerogel was converted to tetragonal ZrO₂ after calcined at 600 °C, while monoclinic at 1000 °C.

• Periodical: Solid State Phenomena (Volume 281)
• Pages: 52-57
• DOI: https://doi.org/10.4028/www.scientific.net/SSP.281.52
• Online since: August 2018
• Authors: Lan Li, Yuan Yuan Song, Guang Ren Geng, Fu Tian Liu*
• Keywords: Precipitating Agent, Solid Content, Stable, Viscosity, Zirconium Sol

References

[1] Y. Gao, Y. Masuda, H. Ohtaetal. Room-temperautre preparation of ZrO2 precursor thin filminan aqueous peroxo zirconium-complex solution. Chem. Mater, 16 (2004) 2615-2622.

DOI: 10.1021/cm049771i

[2] P. F. Becher. Advances in the Design of Toughened Ceramics. J. Ceram Soc Jpn, 99 (1992) 962-967.

[3] Y. Y. Cui, Z. K. Chen, X. X. Liu. Preparation of UV-curing polymer-ZrO2 hybrid nano composites via auto-hydrolysis sol-gel process using zirconium oxychloride octahydrate coordinated with organic amine. Prog. Org. Coat, 100 (2016) 178-187.

DOI: 10.1016/j.porgcoat.2016.03.028

[4] C. Xia, H. Cao, H.Wang, et al. Sol–gel synthesis of yttria stabilized zirconia membranes through controlled hydrolysis of zirconium alkoxide. J Membr Sci, 162 (1999) 181–188.

DOI: 10.1016/s0376-7388(99)00137-4

[5] X. Bokhimi, A Morales, O. Novaro, et al. The effect of hydrolysis initiator on the phase formation in sulfated sol–gel zirconia. Polyhedron, 19 (2000) 2283–2287.

DOI: 10.1016/s0277-5387(00)00490-3

[6] H. Uchiyama, K.Takagi, H. Kozuka. Solvothermal synthesis of size-controlled ZrO2 microspheres via hydrolysis of alkoxides modified with acetylacetone. Colloids Surf A, 403 (2012) 121–128.

DOI: 10.1016/j.colsurfa.2012.03.065

[7] F. Davar, A. Hassankhani, MR. Loghman-Estarki. Controllable synthesis of metastable tetragonal zirconia nanocrystals using citric acid assisted sol–gel method. Ceram Int, 39 (2013) 2933–2941.

DOI: 10.1016/j.ceramint.2012.09.067

[8] G. Yu , L. Zhu, X. Wang, et al. Fabrication of silica supported ZrO2 mesoporous fibers with high thermal stability by sol–gel method through a controlled hydrolysis–condensation process. Microporous Mesoporous Mater, 130 (2010) 189–196.

DOI: 10.1016/j.micromeso.2009.11.004

[9] V. Chernov, A. Belykh, R. Meléndrez, M. Barboza-Flores. Beta radiation induced thermoluminescence in pure ZrO2 prepared by sol-gel. J. Non-Cryst Solids, 352 (2006) 2543–2547.

DOI: 10.1016/j.jnoncrysol.2006.03.048

[10] A. Mondal, S. Ram. Controlled phase transformations in Al3+ stabilized ZrO2 nanoparticles via forced hydrolysis of metal cations in water. Mater. Lett, 57 (2003) 1696–1706.

DOI: 10.1016/s0167-577x(02)01054-6

[11] K. Kim, K. Adachu, Y. Chujo. Polymer hybrids of functionalized silsesquioxanes and organic polymers utilizing the sol-gel reaction tetramethoxysilane. Polymer, 43 (2002) 1171–1175.

DOI: 10.1016/s0032-3861(01)00732-7

[12] Y. Wang, Q. Chang , J Zhou, et al. Preparation of nanosized ZrO2 by controllable sol–gel method. Synth. Cryst, 38 (2004) 1012–1017.

[13] H. Xie, W.F. Shi. Polymer/SiO2 hybrid nano composites prepared through the photo initiator-free UV curing and sol-gel processes, Compos. Sci. Technol, 93(2014) 90–96.

DOI: 10.1016/j.compscitech.2014.01.004