An Improved Chemical Reduction Route for Fine Nickel Powders

Chan-Ok Bae; Youn-Hyun Kim; Jung Ho Son; Seong-Ju Hwang; Young-Uk Kwon; Byung-Yoon Lee; Young-Sic Kim

Journal of Industrial and Engineering Chemistry, Vol.11, No.6, 902-910, November, 2005

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An Improved Chemical Reduction Route for Fine Nickel Powders

Chan-Ok Bae, Youn-Hyun Kim¹, Jung Ho Son, Seong-Ju Hwang², Young-Uk Kwon^†, Byung-Yoon Lee¹, and Young-Sic Kim¹

Department of chemistry and BK-21 School of Molecular Science, Sungkyunkwan University, Suwon 440-746, Korea
¹ChangSung Corporation, 11-9, Namdong Industrial Area, Incheon 405-846, Korea
²Division of Nano Sciences and Department of Chemistry, Ewha Womans University, Seoul 120-750, Korea

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We report an improved chemical reduction route toward fine nickel powders by using nickel hydrazine complexes [Ni(N2H4)3SO4 and Ni(N2H4)nCl2 (n = 2 and 3)] as the starting materials, rather than Ni(OH)2, which is used in the conventional procedure. The reductions of the hydrazine complexes had reaction rates that were three to ten-fold higher than those of the conventional method. As a result, the products consist of homogeneous, phase-pure, spherical, fine nickel particles that have smooth surfaces; they were formed without the need for additives or extreme reaction conditions. The reaction rates could be related to the solubilities of the precursors, which increase in the order Ni(N2H4)2Cl2 > Ni(N2H4)3Cl2 > Ni(N2H4)3SO4; we propose a reaction mechanism based on this observation.

Keywords:chemical synthesis;nickel ultrafine powder;hydrazine complex

[References]

Tseng WJ, Lin SY, Mater. Sci. Eng., 362, 160 (2003)
Park SH, Kim CH, Kang YC, Kim YH, J. Mater. Sci. Lett., 22(21), 1537 (2003)
Jeon JK, Koh ST, Park YK, Suh DJ, Ihm SK, J. Ind. Eng. Chem., 11(1), 83 (2005)
Park SJ, Jin SY, J. Ind. Eng. Chem., 11(3), 395 (2005)
Ueyama R, Ueyama T, Koumoto K, J. Ceram. Soc. Jpn., 108, 769 (2000)
Lee JY, Lee JH, Hong SH, Lee YK, Choi JY, Adv. Mater., 15, 1665 (2003)
Hedge MS, Larcher D, Dupont L, Beaudoin B, Elhsissen KT, Tarascon JM, Solid State Ion., 93, 33 (1997)
Zheng HG, Liang JH, Zeng JH, Qian YT, Mater. Res. Bull., 36(5-6), 947 (2001)
Zhang J, Yang S, Xue Q, J. Mater. Res., 15, 541 (2000)
Kim KH, Lee YB, Choi EY, Park HC, Park SS, Mater. Chem. Phys., 86, 420 (2004)
Nicholls D, Rowley M, Swindells R, J. Chem. Soc. A, 950 (1966)
Linke KH, Durholtz F, Handicke D, Anorg Z, Allg. Chem., 365, 113 (1968)
Choy JH, Hwang SJ, Park NG, J. Am. Chem. Soc., 119(7), 1624 (1997)
Konin GA, Bol'shakov AM, Khmelevskaya LV, Russ. J. Coord. Chem., 22, 870 (1996)
Araki T, Toshima Y, Yamaguchi Y, Hayashi T, JP 99-122550 (2000)
Funatsu E, JP 93-151300 (1994)
Li YD, Li LQ, Liao HW, Wang HR, J. Mater. Chem., 9, 2675 (1999)
Chen. DH, Hsieh CH, J. Mater. Chem., 12, 2412 (2002)
Huheey JE, Keiter EA, Keiter RL, Inorganic Chemistry: Principles of Structure and Reactivity, 4th ed., pp. 99-112, Harper Collins, New York (1993)
Schwarzenbach G, Zobrist A, Helv. Chim. Acta, 35, 1291 (1952)
Tsuchiya R, Yonemura M, Uehara A, Kyuno E, Bull. Chem. Soc. Jpn., 47, 660 (1974)
Elemental analysis data of the precipitates: Ni(N2H4)2Cl2 by adding a N2H4ㆍH2O solution at a rate of 0.6 mL/min; found (%): Ni, 30.6; N, 26.63; H, 4.26; calc. (%): Ni, 30.41, N, 28.87, H, 4.12. Ni(N2H4)3Cl2 by pouring a N2H4ㆍH2O solution; found (%): Ni, 25.60; N, 32.17; H, 4.96; calc. (%): Ni, 26.11, N, 37.17, H, 5.31. The elemental analysis data show some discrepancy from the theoretical values because the precipitates are mixtures of the n = 2 and 3 compounds, among others.
Fivet F, in Fine Particles: Synthesis, Characterization, and Mechanisms of Growth, Surf. Sci. Ser., 92, T. Sugimoto Ed., pp. 460-496, Marcel Dekker, New York (2000)

[1] Tseng WJ, Lin SY, Mater. Sci. Eng., 362, 160 (2003)

[2] Park SH, Kim CH, Kang YC, Kim YH, J. Mater. Sci. Lett., 22(21), 1537 (2003)

[3] Jeon JK, Koh ST, Park YK, Suh DJ, Ihm SK, J. Ind. Eng. Chem., 11(1), 83 (2005)

[4] Park SJ, Jin SY, J. Ind. Eng. Chem., 11(3), 395 (2005)

[5] Ueyama R, Ueyama T, Koumoto K, J. Ceram. Soc. Jpn., 108, 769 (2000)

[6] Lee JY, Lee JH, Hong SH, Lee YK, Choi JY, Adv. Mater., 15, 1665 (2003)

[7] Hedge MS, Larcher D, Dupont L, Beaudoin B, Elhsissen KT, Tarascon JM, Solid State Ion., 93, 33 (1997)

[8] Zheng HG, Liang JH, Zeng JH, Qian YT, Mater. Res. Bull., 36(5-6), 947 (2001)

[9] Zhang J, Yang S, Xue Q, J. Mater. Res., 15, 541 (2000)

[10] Kim KH, Lee YB, Choi EY, Park HC, Park SS, Mater. Chem. Phys., 86, 420 (2004)

[11] Nicholls D, Rowley M, Swindells R, J. Chem. Soc. A, 950 (1966)

[12] Linke KH, Durholtz F, Handicke D, Anorg Z, Allg. Chem., 365, 113 (1968)

[13] Choy JH, Hwang SJ, Park NG, J. Am. Chem. Soc., 119(7), 1624 (1997)

[14] Konin GA, Bol'shakov AM, Khmelevskaya LV, Russ. J. Coord. Chem., 22, 870 (1996)

[15] Araki T, Toshima Y, Yamaguchi Y, Hayashi T, JP 99-122550 (2000)

[16] Funatsu E, JP 93-151300 (1994)

[17] Li YD, Li LQ, Liao HW, Wang HR, J. Mater. Chem., 9, 2675 (1999)

[18] Chen. DH, Hsieh CH, J. Mater. Chem., 12, 2412 (2002)

[19] Huheey JE, Keiter EA, Keiter RL, Inorganic Chemistry: Principles of Structure and Reactivity, 4th ed., pp. 99-112, Harper Collins, New York (1993)

[20] Schwarzenbach G, Zobrist A, Helv. Chim. Acta, 35, 1291 (1952)

[21] Tsuchiya R, Yonemura M, Uehara A, Kyuno E, Bull. Chem. Soc. Jpn., 47, 660 (1974)

[22] Elemental analysis data of the precipitates: Ni(N2H4)2Cl2 by adding a N2H4ㆍH2O solution at a rate of 0.6 mL/min; found (%): Ni, 30.6; N, 26.63; H, 4.26; calc. (%): Ni, 30.41, N, 28.87, H, 4.12. Ni(N2H4)3Cl2 by pouring a N2H4ㆍH2O solution; found (%): Ni, 25.60; N, 32.17; H, 4.96; calc. (%): Ni, 26.11, N, 37.17, H, 5.31. The elemental analysis data show some discrepancy from the theoretical values because the precipitates are mixtures of the n = 2 and 3 compounds, among others.

[23] Fivet F, in Fine Particles: Synthesis, Characterization, and Mechanisms of Growth, Surf. Sci. Ser., 92, T. Sugimoto Ed., pp. 460-496, Marcel Dekker, New York (2000)