Effects of Mechanically Activated Milling and Calcination Process on the Phase Stability and Particle Morphology of Monoclinic Zirconia Synthesized by Hydrolysis of ZrOCl2 Solution

Young-Geun Lee; Soon-Chul Ur; Iqbal Mahmud; Man-Soon Yoon

Korean Journal of Materials Research, Vol.23, No.10, 543-549, October, 2013

DOI10.3740/MRSK.2013.23.10.543 Export Citation

Effects of Mechanically Activated Milling and Calcination Process on the Phase Stability and Particle Morphology of Monoclinic Zirconia Synthesized by Hydrolysis of ZrOCl2 Solution

Young-Geun Lee, Soon-Chul Ur , Iqbal Mahmud, and Man-Soon Yoon^†

Department of Materials Science and Engineering / RIC-ReSEM, Korea National University of Transportation, Daehakno, Chungju, Chungbuk 380-702, Korea

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The purpose of this paper was to investigate the effect of a high-energy milling (HEM) process on the particle morphology and the correlation between a thermal treatment and tetragonal/monoclinic nanostructured zirconia powders obtained by a precipitation process. To eliminate chloride residue ions from hydrous zirconia, a modified washing method was used. It was found that the used washing method was effective in removing the chloride from the precipitated gel. In order to investigate the effect of a pre-milling process on the particle morphology of the precipitate, dried Zr(OH)4 was milled using a HEM machine with distilled water. The particle size of the Zr(OH)4 powder exposed to HEM reduced to 100~150 nm, whereas that of fresh Zr(OH)4 powder without a pre-milling process had a large and irregular size of 100 nm~1.5 μm. Additionally, modified heat treatment process was proposed to achieve nano-sized zirconia having a pure monoclinic phase. It was evident that two-step calcining process was effective in perfectly eliminating the tetragonal phase, having a small average particle of ~100 nm with good uniformity compared to the sample calcined by a single-step process, showing a large average particle size of ~300 nm with an irregular particle shape and a broad particle size distribution. The modified method is considered to be a promising process for nano-sized zirconia having a fully monoclinic phase.

Keywords:high energy milling;SEM;XRD;calcination

[References]

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Zhou SX, Garnweitner G, Niederberger M, Antonietti M, Langmuir, 23(18), 9178 (2007)
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Coughlin JP, King EG, J. Am. Chem. Soc., 72(5), 2262 (1950)
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Pitcher MW, Ushakov SV, Navrotsky A, Woodfield BF, Li GS, Boerio-Goates J, Tissue BM, J. Am. Ceram. Soc., 88(1), 160 (2005)
Holmes HF, Fuller Jr EL, Gammage RB, J. Phys. Chem., 76(10), 1497 (1972)
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Dechamps M, Djuricic B, Pickering S, J. Am. Ceram. Soc., 78(11), 2873 (1995)
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Pyda W, Haberko K, Bucko MM, J. Am. Ceram. Soc., 74(10), 2622 (1991)
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Vivekanandan R, Kutty TRN, Powder Technology, 57, 181 (1989)
Srinivasan R, Hubbard CR, Cavin OB, Davis BH, Chem. Mater., 5, 27 (1993)

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[2] Metcalfe IS, Catal. Today, 9(1-2), 236 (1991)

[3] Song XM, Sayari A, Catal. Rev.-Sci. Eng., 38(3), 329 (1996)

[4] Tanabe K, Yamaguchi T, Catal. Today, 20(2), 185 (1994)

[5] Zhou SX, Garnweitner G, Niederberger M, Antonietti M, Langmuir, 23(18), 9178 (2007)

[6] Ackermann RJ, Garg SP, Rauh EG, High Temp. Sci., 11(3), 199 (1979)

[7] Coughlin JP, King EG, J. Am. Chem. Soc., 72(5), 2262 (1950)

[8] Garvie RC, J. Phys. Chem., 69(4), 1238 (1965)

[9] Pitcher MW, Ushakov SV, Navrotsky A, Woodfield BF, Li GS, Boerio-Goates J, Tissue BM, J. Am. Ceram. Soc., 88(1), 160 (2005)

[10] Holmes HF, Fuller Jr EL, Gammage RB, J. Phys. Chem., 76(10), 1497 (1972)

[11] Kasatkin I, Girgsdies F, Ressler T, Caruso RA, Schattka JH, Urban J, Weiss K, J. Mater. Sci., 39(6), 2151 (2004)

[12] Dechamps M, Djuricic B, Pickering S, J. Am. Ceram. Soc., 78(11), 2873 (1995)

[13] Matusui K, Suzuki H, Ohagi M, Arashi H, J. Am. Ceram. Soc., 78(1), 146 (1995)

[14] Pyda W, Haberko K, Bucko MM, J. Am. Ceram. Soc., 74(10), 2622 (1991)

[15] Nishizawa H, Yamasaki N, Matsuoka K, Mitsushio H, J. Am. Ceram. Soc., 65(7), 343 (1982)

[16] Dell'Agli G, Mascolo G, J. Eur. Ceram. Soc., 20(2), 139 (2000)

[17] Tani E, Yoshimura M, Somiya S, J. Am. Ceram. Soc., 64(12), C181 (1981)

[18] Tani E, Yoshimura M, Somiya S, J. Am. Ceram. Soc., 66(1), 11 (1983)

[19] Kumazawa H, Inoue T, Sada E, Chem. Eng. J., 55, 93 (1994)

[20] Scott CE, Reed JS, Am. Ceram. Soc. Bull., 58, 587 (1979)

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[22] A. Guinier, Theorie et Technique de la Radiocristallographie, 3rd ed., p.482, Dunod Paris, France. (1964)

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[24] Srinivasan R, Hubbard CR, Cavin OB, Davis BH, Chem. Mater., 5, 27 (1993)