无机化学学报
無機化學學報
무궤화학학보
JOURNAL OF INORGANIC CHEMISTRY
2008年
3期
439-445
,共7页
超临界二氧化碳%正八面体氧化钴
超臨界二氧化碳%正八麵體氧化鈷
초림계이양화탄%정팔면체양화고
supercritieal carbon dioxide%octahedral cobalt oxide
研究了正八面体氧化钴颗粒在超临界二氧化碳体系中的合成过程.在密闭的不锈钢高压反应釜中,1.0 g乙酸钴和12.0 g干冰在450℃下,反应12 h后合成粒径大约10 μm的正八面体氧化钴颗粒.通过XRD、XPS、TEM、SEM以及拉曼光谱的分析,氧化钴颗粒是由八个{111}面包裹着的正八面体单晶组成.条件实验显示,超临界二氧化碳体系是正八面体氧化钴颗粒合成的充分条件.其生长机理可能是:乙酸钴在超临界二氧化碳体系中的热分解;氧化钴的结晶和定向缓慢生长.在性能方面,初步研究了正八面体氧化钴颗粒在作为锂离子电池电极材料的应用.
研究瞭正八麵體氧化鈷顆粒在超臨界二氧化碳體繫中的閤成過程.在密閉的不鏽鋼高壓反應釜中,1.0 g乙痠鈷和12.0 g榦冰在450℃下,反應12 h後閤成粒徑大約10 μm的正八麵體氧化鈷顆粒.通過XRD、XPS、TEM、SEM以及拉曼光譜的分析,氧化鈷顆粒是由八箇{111}麵包裹著的正八麵體單晶組成.條件實驗顯示,超臨界二氧化碳體繫是正八麵體氧化鈷顆粒閤成的充分條件.其生長機理可能是:乙痠鈷在超臨界二氧化碳體繫中的熱分解;氧化鈷的結晶和定嚮緩慢生長.在性能方麵,初步研究瞭正八麵體氧化鈷顆粒在作為鋰離子電池電極材料的應用.
연구료정팔면체양화고과립재초림계이양화탄체계중적합성과정.재밀폐적불수강고압반응부중,1.0 g을산고화12.0 g간빙재450℃하,반응12 h후합성립경대약10 μm적정팔면체양화고과립.통과XRD、XPS、TEM、SEM이급랍만광보적분석,양화고과립시유팔개{111}면포과착적정팔면체단정조성.조건실험현시,초림계이양화탄체계시정팔면체양화고과립합성적충분조건.기생장궤리가능시:을산고재초림계이양화탄체계중적열분해;양화고적결정화정향완만생장.재성능방면,초보연구료정팔면체양화고과립재작위리리자전지전겁재료적응용.
The synthesis of regular octahedron cobalt oxide microcrystals for the application of battery material in supercritical carbon dioxide system was studied. Regular octahedron microcrystals of cobalt oxide with a size about10 μm were prepared at 450℃ in a closed vessel consisting of 1.0 g of cobalt acetate powder and 12.0 g of dry ice. The as-obtained particles were charterized by XRD, XPS, SEM, TEM and Raman spectroscopy techniques. The XRD and Raman spectroscopy results indicate that the crystal structures of the particles (the cobalt oxide microcrystals) are inerratic. SEM and TEM results reveal that the morphology of cobalt oxide microerystals appear to be the regular octahedron enclosed by eight {111} facets. It is found that the supercritical carbon dioxide system is a full condition to the synthesis of regular octahedron cobalt oxide. The size of cobalt oxide microcrystals increases with reaction time and the morphology is temperature dependent. The possible growth mechanism of regular octahedron cobalt oxide microcrystals was discussed based on the pyrolysis of cobalt (111) acetate, crystallization of cobalt oxide and Slowly Orientational Growth (SOG) due to anisotropy in supercritical carbon dioxide environment at reaction temperatures. The charge/discharge properties of regular octahedron microcrystals of cobalt oxide used as battery material wereal so characterized and discussed.