서냉 소성법에 의한 육티탄산칼륨 Whisker의 합성에 관한 연구

이철태; 최웅수; 김영명

Journal of the Korean Industrial and Engineering Chemistry, Vol.5, No.1, 160-175, February, 1994

Export Citation

서냉 소성법에 의한 육티탄산칼륨 Whisker의 합성에 관한 연구

A Study on the Synthesis of Potassium Hexatitanate Whisker by the Slow Cooling Calcination Process

이철태, 최웅수, 김영명

초록

육티탄산칼륨을 860∼1100℃의 온도범위에서 서냉소성법에 의해 효과적으로 합성하였다 섬유상의 K₂Ti₆O₁₃의 결정을 얻기 위해서는 소성온도 1100℃, K₂O₃에 대한 TiO₂의 mole ratio는 4.5가 가장 적절하였다. 소성 후 서냉조작은 결정상의 티탄산칼륨과 K₂O와 TiO₂의 혼합물 액상과의 화합으로 티탄산칼륨의 섬유상 결정화에 효과적이며, 적절한 서냉속도는 860℃까지 0.5℃/min이었다. 서냉 소성 후 물에 의한 알칼리 침출 조작에 의해 단상의 K₂Ti₆O₁₃의 섬유상이 얻어지며 이때의 침출조건은 끓는물에서 10시간이 적절하였다. 또한 소성시료인 K₂CO₃와 TiO₂ 혼합물에 대한 가압은 티탄산칼륨의 섬유화에 매우 효과적이었다. 최종적으로 얻어진 육티탄산칼륨은 직경 0.5∼l㎛, 길이는 100∼1000㎛로 aspect ratio 100∼1000의 섬유상 결정이었다.

Fibrous potassium hexatitanate whisker with the size of ID=0.5∼1㎛ and length=100∼1000㎛ (aspect ratio=100∼1000) was produced through the reaction between titanium dioxide and potassium carbonate using the slow-cooling calcination followed by water leaching treatment. The optimum condition for the production of fibrous potassium titanate was calcination temperature of 1100℃ for 5hrs, TiO₂ mole ratlo to K₂CO₃ of 4.5 and slow-cooling rate of 0.5℃/min to 860℃. Fibrous crystal are grown by the association between the solid potassium titanate and liquid phase during the slow-cooling process. The Proper water leaching condition for removing of K component was leaching time of 10hrs in boiling water. Pressurizing of the mixture of K₂CO₃ and TiO₂ to be calcinated became effective on the growth of fibrous crystal.

[References]

Berry KL, U.S. Patent, 2,841,470
Salzberg PL, U.S. Patent, 2,833,620
Shimizu T, Yogyo-Kyokai-Shi, 85(4), 189 (1977)
Schmitzu O, Monatsh. Chem., 90, 134 (1959)
Mitsuhashi T, Yogyo-Kyokai-Shi, 90(11), 676 (1982)
Hasegawa Y, Yogyo-Kyokai-Shi, 91(12), 565 (1983)
Automotive Friction Materials Evolution During the Past Decade, Wear 100, 503 (1984)
Buchner W, Schliebs R, Winter G, Buchel KH, "Industrial Inorganic Chemistry," VCH Pub. N.Y. (1989)
U.S. Patent, 427858410
Emslie RS, Gullege HC, U.S. Patent, 3,328,117
Ohta N, Fujiki Y, Yogyo-Kyokai-Shi, 89(3), 134 (1981)
Shimizu T, Yogyo-Kyokai-Shi, 85(12), 567 (1977)
Fujiki Y, Yogyo-Kyokai-Shi, 91(4), 189 (1983)
Shimizu T, Yogyo-Kyokai-Shi, 83(6), 305 (1975)
Fujiki Y, Izumi F, Yogyo-Kyokai-Shi, 85(4), 155 (1977)
Fujiki Y, Ohta N, Yogyo-Kyokai-Shi, 88(3), 112 (1980)
Shimizu T, Yogyo-Kyokai-Shi, 86(8), 339 (1978)
Shimizu T, Yogyo-Kyokai-Shi, 87(11), 565 (1979)
Fujiki Y, セラミツクス, 19, 3 (1984)
Fujiki Y, Yogyo-Kyokai-Shi, 91(4), 189 (1983)
Berry KL, Aftandilian VD, Gilbert WW, Meibohm EPH, J. Inorg. Nucl. Chem., 14, 231 (1960)

[Referenced By]

[1] Berry KL, U.S. Patent, 2,841,470

[2] Salzberg PL, U.S. Patent, 2,833,620

[3] Shimizu T, Yogyo-Kyokai-Shi, 85(4), 189 (1977)

[4] Schmitzu O, Monatsh. Chem., 90, 134 (1959)

[5] Mitsuhashi T, Yogyo-Kyokai-Shi, 90(11), 676 (1982)

[6] Hasegawa Y, Yogyo-Kyokai-Shi, 91(12), 565 (1983)

[7] Automotive Friction Materials Evolution During the Past Decade, Wear 100, 503 (1984)

[8] Buchner W, Schliebs R, Winter G, Buchel KH, "Industrial Inorganic Chemistry," VCH Pub. N.Y. (1989)

[9] U.S. Patent, 427858410

[10] Emslie RS, Gullege HC, U.S. Patent, 3,328,117

[11] Ohta N, Fujiki Y, Yogyo-Kyokai-Shi, 89(3), 134 (1981)

[12] Shimizu T, Yogyo-Kyokai-Shi, 85(12), 567 (1977)

[13] Fujiki Y, Yogyo-Kyokai-Shi, 91(4), 189 (1983)

[14] Shimizu T, Yogyo-Kyokai-Shi, 83(6), 305 (1975)

[15] Fujiki Y, Izumi F, Yogyo-Kyokai-Shi, 85(4), 155 (1977)

[16] Fujiki Y, Ohta N, Yogyo-Kyokai-Shi, 88(3), 112 (1980)

[17] Shimizu T, Yogyo-Kyokai-Shi, 86(8), 339 (1978)

[18] Shimizu T, Yogyo-Kyokai-Shi, 87(11), 565 (1979)

[19] Fujiki Y, セラミツクス, 19, 3 (1984)

[20] Fujiki Y, Yogyo-Kyokai-Shi, 91(4), 189 (1983)

[21] Berry KL, Aftandilian VD, Gilbert WW, Meibohm EPH, J. Inorg. Nucl. Chem., 14, 231 (1960)