이온교환된 X형 및 Y형 제올라이트의 Ols 전자에 대한 X선 광전자분광학적 해석

김명철; 김종택

Journal of the Korean Industrial and Engineering Chemistry, Vol.3, No.2, 240-246, June, 1992

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이온교환된 X형 및 Y형 제올라이트의 Ols 전자에 대한 X선 광전자분광학적 해석

XPS Studies for O_ls Electrons of Ion Exchanged Zeolite X and Y

김명철, 김종택

초록

X선 광전자분광법을 이용하여 교환된 제올라이트내 산소원자의 전자구조를 조사하였다. Na⁺, Fe²⁺ 및 Fe³⁺로 교환된 X형 및 Y형 제올라이트에 대하여 얻어진 O_ls스펙트럼은 골격산소의 결합에너지를 밝히기 위하여 분해하였다. 각 스펙트럼에서는 2-3개의 분해띠들이 있었다. 분해된 각 띠들의 특성은 교환된 양이온에 따라서 O_ls 전자의 결합에너지와 띠면적의 관점에서 고찰되었다. 분해된 띠들을 각각 골격내 가교산소에 의한 것(띠 1), 양이온에 결합된 산소에 의한 것(띠 2), 양이온에 배위된 물분자내 산소에 의한 것(띠 3)으로 해석되었다. O_ls스펙트럼 면적의 대부분을 차지하고 있는 띠 1은 제올라이트내 Al함량의 감소에 따라서 결합에너지상의 증가를 나타내었다.

The electronic structure of oxygen atom of cation-exchanged zeolite was investigated by utilizing X-ray photoelectron spectroscopy(XPS). The obtained O₁₅ spectra of Na⁺-, Fe²⁺- and Fe³⁺- exchanged zeolite X and Y were deconvoluted to demonstrate electronic binding energy of framework oxygens. There were 2-3 bands in each spectrum. The characteristics of separated band have been studied in terms of binding energy and relative area of O₁₅ electron with respect to the exchanged cation. Those bands were assigned to the bridged oxygen in framework (band 1), cation bonded oxygen in cationic site (band 2) and oxygen in water coordinated to the cation (band 3) each other. The band 1 occupying the majority area of O₁₅ spectrum was shifted to higher region on binding energy according to the decrease of Al content in zeolite.

[References]

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[1] Decanio SJ, Sohn JR, Fritz PO, Lunsford JH, J. Catal., 101, 132 (1986)

[2] Rabo JA, "Zeolite Chemistry and Catalysis," ACS Monograph, 171, Washington D.C. (1976)

[3] Aparicio LM, Dumesic JA, Fang SM, Long MA, Ulla MA, Millman WS, Hall WK, J. Catal., 104, 381 (1987)

[4] Kuhl CH, Zeolites, 5, 4 (1985)

[5] Kim JT, Kim MC, Okamoto Y, Imanaka T, J. Catal., 115, 319 (1989)

[6] Okamoto Y, Ogawa M, Maezawa A, Imanaka T, J. Catal., 112, 427 (1988)

[7] Break DW, "Zeolite Molecular Sieves," John-Wiley & Sons, New York (1974)

[8] Ozin GA, Baker MD, Godber J, Shihua W, J. Am. Chem. Soc., 107, 1995 (1985)

[9] Godber J, Ozin GA, J. Phys. Chem., 92, 2841 (1988)

[10] Firor RL, Seff K, J. Phys. Chem., 82, 1950 (1978)

[11] Heo NH, Patalinghug WC, Seff K, J. Phys. Chem. Soc., 90, 3931 (1986)

[12] Melchoir MT, Vaughan DEW, Jacobson AJ, J. Am. Chem. Soc., 104, 4859 (1982)

[13] Sohn JR, Decanio SJ, Lunsford JH, Odonell DJ, Zeolites, 6, 225 (1986)

[14] Szostak R, Thomas T, J. Catal., 101, 549 (1986)

[15] Contarini S, Kevan L, J. Phys. Chem., 90, 1630 (1986)

[16] Contarini S, Michalik J, Narayama M, Kevan L, J. Phys. Chem., 90, 4586 (1986)

[17] Calson TA, "Photoelectron and Auger Spectroscopy," 2nd ed., Plenum Press, New York (1978)

[18] Jones RN, Appl. Opt., 8, 597 (1969)

[19] Pitha J, Jones RN, Can. J. Chem. Soc. Faraday, 68 (1972)

[20] Morgan SL, Deming SN, Anal. Chem., 46, 1170 (1974)

[21] Kim MC, Kim JT, HWAHAK KONGHAK, 28(4), 411 (1990)

[22] Barr TL, Lishka MA, J. Am. Chem. Soc., 108, 3178 (1986)

[23] Huheey JE, "Inorganic Chemistry," 3rd ed., Happer & Row Co., New York (1983)

[24] Roosmalen A, J. Chem. Phys., 83, 2485 (1979)