以過氧化氫(H2O2)為氧化劑將Co(OH)2氧化，得到主體為含結晶水三價氧化鈷Co2O3．H2O的前驅樣品，並利用熱重分析儀(TG)與程溫還原裝置(TPR)加以分析。由TPR的研究分析，此前驅樣品含有4 % CoO2，且發現以四個步驟進行還原：CoO2 → Co2O3 → Co3O4 → CoO → Co，其還原溫度分別為410 K、480 K、520 K和590 K。經由程溫還原和脫附的方法可製得各階段的氧化鈷，並以X光繞射儀(XRD)、紅外光譜儀(IR)、光電子能譜儀(XPS)和X光吸收能譜儀(XANES)進行鑑定分析。其中程溫還原裝置和X光吸收能譜儀證明了不同階段氧化鈷的價數變化。此研究中發現，將初期樣品於420 K的TPR還原可得到純的含結晶水三價氧化鈷Co2O3．H2O，此氧化物在高於670 K的空氣中會分解，而變成Co3O4。

Crude sample of hydrated cobalt (III) oxide, Co2O3． H2O, has been prepared by oxidation of Co(OH)2 precipitates in aqueous solution with hydrogen peroxide. The oxidation state of prepared oxide has been characterized by the thermo-gravimetry (TG) and the temperature programmed reduction (TPR). TPR studies further indicated that the crude sample was contaminated with 4% CoO2 and that the reduction in TPR was proceeded in four distinguishable steps, i.e., CoO2 ® Co2O3 ® Co3O4 ® CoO ® Co, at reduction temperatures of Tr = 410, 480, 520 and 590 K, respectively. The meta-stable intermediates in this reduction sequence have been isolated and physically characterized by combined techniques of the X-ray diffraction (XRD), the infrared spectroscopy (IR), the X-ray photoelectron spectroscopy (XPS) and the X-ray absorption near edge spectroscopy (XANES). Among these techniques, TPR and XANES can provide the average oxidation state for cobalt in solid samples. In this study, a refined sample of cobalt (III) oxide, Co2O3．H2O, has been successfully prepared from a TPR reduction of the crude sample to 420 K. This oxide is thermally unstable at high temperature and tends to decompose into Co3O4 on calcinations at T > 670 K in air.

1. R. Bruce King, “Encyclopedia of Inorganic Chemistry”, Vol. 2 (1994), John Wiley & Sons.
2. H. Hamada, Y. Kintaichi, M. Inaba, M. Tabata, T. Yoshinari, and H. Tsuchida, Catalysis Today, 29 (1996) 53.
3. J. Jansson, J. Catal., 194 (2000) 55.
4. K.W. Kirby and H. Kimura, Sensors and Actuators B, 32 (1996) 49.
5. A. Torncrona, M. Skoglundh, P. Thormahlen, E. Fridell and E. Jobson, Appl. Catal. B, 14 (1997) 131.
6. K. Omata, T. Takada, S. Kasahara and M. Yamada, Appl. Catal. A: General, 146 (1996) 255.
7. St.G. Christoskova, M. Stoyanova, M. Georgieva, and D. Mehandjiev, Mater. Chem. and Phys., 60 (1999) 39.
8. J.-P. Jacobs, A. Maltha, J.G.H. Reintjes, J. Drimal, V. Ponec, and H.H. Brongersma, J. Catal., 147 (1994) 294.
9. 吳岱恩，國立清華大學化學系碩士論文，(2000)
10. S.H. Oh and R.M. Sinkevitch, J. Catal., 142 (1993) 254.
11. I.G. Casella and M.R. Guascito, J. Electroanal. Chem., 476 (1999) 54.
12. St.G. Christoskova, M. Stoyanova, M. Georgieva and D. Mehandjiev, Thermochim. Acta., 292 (1997) 77.
13. M. Elemongy, M. Gouda, Y. Elewady, J. Electroanal. Chem,, 76 (1977) 367.
14. V. Pralong, A. Delahaye-Vidal, B. Beaudoin, B. Gerand and J.-M. Tarascon, J. Mater. Chem., 9 (1999) 955.
15. Kondrashev, Fedorova, Dokl, Akad, Nauk SSSR, 94 (1954) 229.
16. D. Grier and G. McCarthy, North Dakota State University, ICDD Grant-in-Aid, (1991).
17. Douglas A. Skoog and James J. Leary, “Principles of Instrumental Analysis”, 4th ed., Saunders College Publishing.
18. K. Nakamoto, “Infrared Spectra of Inorganic and Coordination Compounds”, 2nd ed., Zhuang-yuan Publisher.
19. B. Raquet, R. Mamy, J.C. Ousset, N. Negre, M. Goiran and C. Guerret-Piecourt, J. Magn. Magn. Mater., 184 (1998) 41.
20. D. Pietrogiacomi, S. Tuti, M.C. Campa and V. Indovina, Appl. Catal. B: Environmental, 28 (2000) 43.
21. J-C. Dupin, D. Gonbeau, P. Vinatier and A. Levasseur, Phys. Chem. Chem. Phys., 1319 (2000) 2.
22. V.M. Jimenez, A. Fernandez, J.P. Espinos and A.R. Gonzalez-Elipe, J. Electron Spectrosco. and Relat. Phonom., 71 (1995) 61.
23. J. Ikonomov, D. Stoychev and T. Marinova, Appl. Surf. Sci., 161 (2000) 94.