졸겔법으로 제조된 MO- SiO 2   (M=Zn,Sn,In,Ag,Ni)의 구조특성

신용욱; 김상우; Yong-Wook Shin; Sang Woo Kim

Korean Journal of Materials Research, Vol.11, No.7, 603-608, July, 2001

Export Citation

졸겔법으로 제조된 MO- SiO 2 (M=Zn,Sn,In,Ag,Ni)의 구조특성

Structural Properties of MO-SiO 2 (M=Zn, Sn, In, Ag, Ni) by Sol-Gel Method

신용욱, 김상우

한국과학기술연구원 세라믹공정연구센터

Yong-Wook Shin, and Sang Woo Kim

Ceramic Processing Research Center, KIST, Seoul, 136-791, Korea

초록

졸겔법에 의해 제조된 MO?SiO 2 (M=Zn, Sn, In, Ag, Ni)이성분계 실리카 겔에서 금속이온의 종류에 따른 실리카 구조의 변화를 XRD, FT-lR, 29 Si-NMR로 분석하였다. XRD peak을 관찰한 결과 Ag?SiO 2 겔에서 AgNO 3 의 부분적인 재결정화가 나타났지만, 첨가된 금속이온과 실리카 매트릭스의 결합에 의한 결정상은 관찰되지 않았다. FT-IR 분석결과 첨가되는 금속이온 중 Zn, Sn, In은 부분적으로 Si-O-M의 결합형태를 이루어 Si-O-Si 대칭 진동에 의한 흡수 peak의 위치를 변화시켰다. 29 Si-NMR 관찰에 의해 Zn, Sn, In등의 금속이온은 실리카의 저온 졸겔 반응에 영향을 미치지 않고 불완전한 네트워크를 갖는 선형적 실리카 구조 내에서 비가교 산소와 결합하며 존재하였다. Ag, Ni는 실리카 네트워크가 형성되는 과정에서 실리카 형성을 위한 졸겔반응의 촉매로서 작용하여, 이러한 금속이온이 첨가된 실리카 네트워크는 보다 치밀한 구조적 특성을 나타내었다.

MO?SiO 2 (M = Zn, Sn, In, Ag, Ni) binary silica gels were synthesized by sol-gel method and their structural change with the kind of metal ions was characterized by XRD, FT- IR and 29 Si-NMR. Although X-ray analysis showed partial recrystallization of AgNO 3 in Ag?SiO 2 gel, crystalline phase formed by the bonding between metal ion and the silica matrix didn't appear in all MO?SiO 2 gels. The FT-IR analysis showed that Zn, Sn and in partially formed Si-O-M bonding in silica matrix and made an shift of absorption peak to by Si-O-Si symmetrical vibration. In addition, 29 Si?NMR studies showed that Zn, Sn and In didn't affect sol-gel process of silica and were linked with non-bridging oxygen of the linear silica structure, which formed imperfect network because of low temperature sol-gel process. Ag and Ni make a role of catalysis on sol-gel process, resulting in densifying the silica network structure.

Keywords:MO-SiO 2;Zn;Sn;In;Ag;Ni;XRD;FT-IR;NMR;sol-gel

[References]

Boonstra AH, Meeuwsen TPM, Baken JME, Aben GVA, J. Non-Cryst. Solids, 109, 153 (1989)
Brinker CJ, Scherer GW, Sol-Gel Science: The Physics and Chemistry of Sol-Gel Processing, Academic press. San Diego, 1990 (1990)
Her RK, The Chemistry of silica, A WileyInterscience Publication. 1979 (1979)
Flego C, Carluccio L, Rizzo C, Perego C, Catal. Commun., 2, 43 (2001)
Lakshmi JL, Ihasz NJ, Miller JM, J. Mol. Catal. A-Chem., 165(1-2), 199 (2001)
Satyanarayana N, Xie X, Rarnbabu B, Mat. Sci. Eng., 872, 7 (2000)
Ennas G, Mei A, Musinu A, Piccaluga G, Pinna G, Solinas S, J. Non-Cryst. Solids, 232, 587 (1998)
Bruni S, et, ac., Nanosiruc-tured Material, 11(5), 573 (1999)
Lin C, Ritter JA, Amiridis MD, J. Non-Cryst. Solids, 215, 146 (1997)
Ishikawa H, Honjo Y, Watanabe K, Thin Solid Films, 351(1-2), 212 (1999)
Hanaoka H, Ito O, Kaneko K, Kondo H, SID98 DIGEST, 258 (1998)
Yoshino H, Kamiya K, Nasu H, J. Non-Cryst. Solids, 126, 68 (1990)
Almeida RM, J. Non-Cryst. Solids, 106, 347 (1990)
Almeida RM, Guiton TA, Pantano CG, J. Non-cryst, Solids., 121, 193 (1990)
Lippmaa E, Magi M, Samoson A, Engelhardt G, Grimmer AR, J. Am. Chem. Soc, 102, 4889 (1980)
Cannas C, Casu M, Lai A, Musinu A, Piccaluga G, J. Mater. Chem, 9, 1765 (1999)
Casu M, Marincola FC, Lai A, Musinu A, Piccaluga G, v, Noti-cryst, Solids, 32-234. 329 (1998) (1998)

[1] Boonstra AH, Meeuwsen TPM, Baken JME, Aben GVA, J. Non-Cryst. Solids, 109, 153 (1989)

[2] Brinker CJ, Scherer GW, Sol-Gel Science: The Physics and Chemistry of Sol-Gel Processing, Academic press. San Diego, 1990 (1990)

[3] Her RK, The Chemistry of silica, A WileyInterscience Publication. 1979 (1979)

[4] Flego C, Carluccio L, Rizzo C, Perego C, Catal. Commun., 2, 43 (2001)

[5] Lakshmi JL, Ihasz NJ, Miller JM, J. Mol. Catal. A-Chem., 165(1-2), 199 (2001)

[6] Satyanarayana N, Xie X, Rarnbabu B, Mat. Sci. Eng., 872, 7 (2000)

[7] Ennas G, Mei A, Musinu A, Piccaluga G, Pinna G, Solinas S, J. Non-Cryst. Solids, 232, 587 (1998)

[8] Bruni S, et, ac., Nanosiruc-tured Material, 11(5), 573 (1999)

[9] Lin C, Ritter JA, Amiridis MD, J. Non-Cryst. Solids, 215, 146 (1997)

[10] Ishikawa H, Honjo Y, Watanabe K, Thin Solid Films, 351(1-2), 212 (1999)

[11] Hanaoka H, Ito O, Kaneko K, Kondo H, SID98 DIGEST, 258 (1998)

[12] Yoshino H, Kamiya K, Nasu H, J. Non-Cryst. Solids, 126, 68 (1990)

[13] Almeida RM, J. Non-Cryst. Solids, 106, 347 (1990)

[14] Almeida RM, Guiton TA, Pantano CG, J. Non-cryst, Solids., 121, 193 (1990)

[15] Lippmaa E, Magi M, Samoson A, Engelhardt G, Grimmer AR, J. Am. Chem. Soc, 102, 4889 (1980)

[16] Cannas C, Casu M, Lai A, Musinu A, Piccaluga G, J. Mater. Chem, 9, 1765 (1999)

[17] Casu M, Marincola FC, Lai A, Musinu A, Piccaluga G, v, Noti-cryst, Solids, 32-234. 329 (1998) (1998)