本研究利用初濕含浸法、離子交換法與沉澱吸附法來製備高價氧化態的支撐性氧化鈷。接著以程溫還原(TPR)觀察製作樣品的還原現象，並以X光吸收近邊緣光譜術(XANES)進行樣品上氧化鈷的價數和結構的分析。
從樣品的TPR圖譜發現，被擔載的氧化鈷主要有二種型態，分別是小顆粒的沉積態(D態)及與擔體接觸的作用態(I態)。而不同的製備方法及擔體的種類會影響氧化鈷在這二態間的分佈﹔初濕含浸法及氧化矽偏好D態的分佈，沉澱吸附法及氧化鋁則以I態分佈為主。不同型態的氧化鈷在TPR中會有不同的還原現象，D態的氧化鈷呈現階段式的還原行為(Co2O3→ Co3O4→ CoO→ Co)，I態的氧化鈷則傾向一步式的還原(Co3+→ Co，Co2+→ Co)。

從XANES圖譜可得知樣品中鈷的價數變化。初濕含浸法則以四氧化三鈷為主要的氧化鈷型態，三價的氧化鈷主要由沉澱吸附法獲得。

Samples of Co/SiO2 and Co/Al2O3 were prepared by means of incipient wetness impregnation (IW) and precipitation-adsorption (PA). The prepared samples were further oxidized by calcined in air and treatment of H2O2. The extent of oxidation in oxidized samples was characterized with temperature-programmed reduction (TPR). Co2O3 was dominated in PA samples, while Co3O4 was favored in IW samples.
TPR results also indicated that dispersed cobalt oxides might be distinguished in two types, i.e., deposit particles (D type) negligibly perturbed by support and a species interacted with support surface (I type). Distribution of dispersed cobalt oxides between these two types depended on the method of preparation and the property of support. The IW method and silica support favored a formation of D type. However, I type was generally formed by the PA method and on alumina support. The type of Co2O3 has a significant effect on its reductive phenomena in TPR. The D type was reduced in sequential steps (Co2O3→Co3O4→CoO→Co), and Co2O3 of I type was reduced in a single step to metallic Co (Co3+→Co).

1. John Wiley and Sons, Inc., “ Inorganic Structural Chemistry ” 2nd Ed., 1993
2. Yamaura, H., Moriya, K., Miura, N., Yamazoe, N., Sensors and Actuators B, 2000, 65, 39
3. Lichtenberg, F., Kleinsorgen, K., J. Power Sources, 1996, 62, 207
4. 吳岱恩，國立清華大學化學系碩士論文，2000
5. P. Arnoldy, J. A. Moulijn, J. Catal., 1985, 93, 38
6. A. Lapidus, A. Krylova, V. Kazanskii, V. Borovkov, A. Zaitsev, J. Rathousky, A.Zukal, M. Jancalkova, Appl. Catal., 1991, 73, 65
7. Hui Ming, Bruce G. Baker, Appl. Catal. A, 1995, 123, 23
8. D. Schanke, S. Vada, E. A. Blekkan, A. M. Hilmen, A. Hoff, A. Holmen, J. Catal., 1995, 156, 85
9. Eric van Steen, Gary S. Swewll, Rafene A. Makhothe, Craig Micklethwaite, Heiko Manstein, Martijn de Lange, Cyril T. O’Connor, J. Catal., 1996, 162, 220
10. H. C. Tung, C. T. Yeh, C. T. Hong, J. Catal., 1990, 122, 211
11. Bunjcrd Jongsomjit, Joongjai, Panpranot, James G. Goodwin, Jr., J. Catal., 2001, 204, 98
12. J. F. Huang, A. Hung, C. B. Wang, C. T. Yeh, J. Chin. Chem. Soc., 2002, 49, 819
13. 黃進發，國立清華大學化學系碩士論文，2001
14. J. F. Lee, “ Chemistry ”, Vol. 53, 1995
15. Shanmugam Yuvaraj, F. Y. Lin, T. H. Chang, C. T. Yeh, J. Phys. Chem. B, 2003, 107, 1044