TiO  2   /Mg 반응에 의한 흑색산화티타늄 제조시 반응 변수 연구

정중채; 조정웅; 이혁희; 이종현; 원창환; Jung-Chae Jeong; Jeong-Woong Cho; Heuk-Hye Lee; Jong-Hyun Lee; Chang-Whan Won

Korean Journal of Materials Research, Vol.11, No.10, 851-858, October, 2001

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TiO 2 /Mg 반응에 의한 흑색산화티타늄 제조시 반응 변수 연구

Study on the Reaction Parameters in the Preparation of Black Titanium Oxide by the Reaction of TiO 2 /Mg System

정중채^†, 조정웅¹, 이혁희², 이종현, 원창환²

충남대학교 급속응고신소재연구소
¹조선이공대학 금속.귀금속세공과
²한국화학시험연구원 분석그룹

Jung-Chae Jeong^†, Jeong-Woong Cho¹, Heuk-Hye Lee², Jong-Hyun Lee, and Chang-Whan Won²

Rapidly Solidified Materials Research Center, Chungnam National University, Daejoen 305-764, Korea
¹Chemical Analysis Research Division, Korea Research Institute of Chemical Technology, Daejeon, Korea
²Dept. of Metallurgy Precious Metal Craft, Chosun College of Science & Technology, Kwangju, Korea

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One of the important phase of black titanium oxide is Ti 4 O 7 which has the excellent properties such as the greatest electrical conductivity among the titanium oxides, chemical resistance against acidic and alkalic conditions and electro-wave absorption etc., so it has been considered as a promising material to be used widely all over the parts of industries. In this study, Ti 4 O 7 phase was successfully synthesized by the reaction of TiO 2 / Mg system. With the change of the mole of TiO 2 to Mg, the most excellent blackness was appeared in the 3.5 mole which was the smaller amount than the stoichiometric 4.0 mole. In addition, we found that the blackness decreased as the mole ratio of reactent increased. With decreasing particle size of magnesium, blackness of titanium oxide increased. The reaction property was changed with the compaction pressure, and optimum pressure was found to be 10 MPa. At 55 0 ? C of reduction temperature, the blackness increased as the reaction time increased. The blackness of synthesized black titanium oxide was 14 to 18, and the average particle size was 0.2 μm .

Keywords:Black titanium Oxide;Blackness;reduction reaction

[References]

Shibuta et al., 'Process for preparing a titanium oxide powder', U.S. Patent No. 4,668,501 (1987) (1987)
Griffen DT 'Siliacte crystal chemistry' Oxford Uni. Press, (1992) (1992)
Kim JH, et al., Korean J. Mater. Res., A study on the preparation of alumina & titania sols for coating, 4(3) (1994)
Kim DH, et al., Korean J. Mater. Res., The photo catalytic activity of TiO 2 powder prepared by sol-gel method, 6(3) (1996)
Magrini KA, Webb JD, 'Photo catalytic decomposition of aqueous organic compounds as a function of solar irradiation intensity', 1990 ASEM International Solar Energy Conference (1990) (1990)
Bahnemann D, Bockelmann D, Goslich, Solar R, Energy Mat., 24 (1992)
Park SY, Mho SI, Chi EO, Kwon YU, Park HL, Thin Solid Films, Characteristics of Pt thin films on the conducting ceramics TiO and Ebonex (Ti 4 O 7 ) as electrode materials, 258 (1995)
Abbata M, et al., Solid State Commun., The electronic structure of Ti 4 O 7 studied by resonant photo emission, 94(6) (1995)
Boffa AB, et al., Surf. Sci., The growth and structure of titanium oxide films on Pt(lll) investigated by LEED, XPS, ISS, and STM, 326 (1995)
Norenberg H, Briggs GAD, Surf. Sci., Surface structure of the most oxygen deficient Magneli phase an STM syudy of Ti 4 O 7, 402 (1998)
He L, Franzen HF, Johnson DC, J. Appl. Electrochem., Synthesis and characterization of Pt?Ti 4 O 7 microelectrode arrays, 26 (1996)
Chen G, Betterton EA, Arnold RG, J. Appl. Electrochem., Electrolytic oxidation of trichloroethylene using a ceramic anode, 29 (1999)
Smith JR, Walsh FC, J. Appl. Electrochem., Electrodes based on Magneli phase oxides: the properties and applications of Ebonex materials, 28 (1998)
'Reduction of titanium dioxide using metallic titanium powder', Japanese Patent No. 52-12733
Ehrlich P, Z. Elektrochem, 45, 362 (1939)
'Reduction of titanium dioxide using N 2 H 4 ' Japanese Patent No. 64-72923
Ehrlich P, Anorg Z, Allg. Chem., 247, 53 (1941)
'Preparation process of black titanium oxide powder', Japanese Patent No. 1993-193942
Andersson S, Acta Chem Scand., 11 (1957)
Clarke RL, HarnsBurger SK, Am. Lab., 20(6) (1988)
Yang JI, Shin HY, Ann JH, Kim YS, 'A study on manufacturing technology of materials for fine chemical industry use', KIGAM Research Report, (1998) (1998)

[1] Shibuta et al., 'Process for preparing a titanium oxide powder', U.S. Patent No. 4,668,501 (1987) (1987)

[2] Griffen DT 'Siliacte crystal chemistry' Oxford Uni. Press, (1992) (1992)

[3] Kim JH, et al., Korean J. Mater. Res., A study on the preparation of alumina & titania sols for coating, 4(3) (1994)

[4] Kim DH, et al., Korean J. Mater. Res., The photo catalytic activity of TiO 2 powder prepared by sol-gel method, 6(3) (1996)

[5] Magrini KA, Webb JD, 'Photo catalytic decomposition of aqueous organic compounds as a function of solar irradiation intensity', 1990 ASEM International Solar Energy Conference (1990) (1990)

[6] Bahnemann D, Bockelmann D, Goslich, Solar R, Energy Mat., 24 (1992)

[7] Park SY, Mho SI, Chi EO, Kwon YU, Park HL, Thin Solid Films, Characteristics of Pt thin films on the conducting ceramics TiO and Ebonex (Ti 4 O 7 ) as electrode materials, 258 (1995)

[8] Abbata M, et al., Solid State Commun., The electronic structure of Ti 4 O 7 studied by resonant photo emission, 94(6) (1995)

[9] Boffa AB, et al., Surf. Sci., The growth and structure of titanium oxide films on Pt(lll) investigated by LEED, XPS, ISS, and STM, 326 (1995)

[10] Norenberg H, Briggs GAD, Surf. Sci., Surface structure of the most oxygen deficient Magneli phase an STM syudy of Ti 4 O 7, 402 (1998)

[11] He L, Franzen HF, Johnson DC, J. Appl. Electrochem., Synthesis and characterization of Pt?Ti 4 O 7 microelectrode arrays, 26 (1996)

[12] Chen G, Betterton EA, Arnold RG, J. Appl. Electrochem., Electrolytic oxidation of trichloroethylene using a ceramic anode, 29 (1999)

[13] Smith JR, Walsh FC, J. Appl. Electrochem., Electrodes based on Magneli phase oxides: the properties and applications of Ebonex materials, 28 (1998)

[14] 'Reduction of titanium dioxide using metallic titanium powder', Japanese Patent No. 52-12733

[15] Ehrlich P, Z. Elektrochem, 45, 362 (1939)

[16] 'Reduction of titanium dioxide using N 2 H 4 ' Japanese Patent No. 64-72923

[17] Ehrlich P, Anorg Z, Allg. Chem., 247, 53 (1941)

[18] 'Preparation process of black titanium oxide powder', Japanese Patent No. 1993-193942

[19] Andersson S, Acta Chem Scand., 11 (1957)

[20] Clarke RL, HarnsBurger SK, Am. Lab., 20(6) (1988)

[21] Yang JI, Shin HY, Ann JH, Kim YS, 'A study on manufacturing technology of materials for fine chemical industry use', KIGAM Research Report, (1998) (1998)