Microwave-assisted synthesis of tin sulfide nanoflakes and their electrochemical performance as Li-inserting materials
Microwave-assisted synthesis of tin sulfide nanoflakes and their electrochemical performance as Li-inserting materials
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DOI：
10.1007/s10008-005-0086-7
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发表时间：
2006-05
影响因子：
2.5
通讯作者：
C. Patra;Ayelet Odani;V. Pol;D. Aurbach;A. Gedanken
中科院分区：
文献类型：
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作者：
C. Patra;Ayelet Odani;V. Pol;D. Aurbach;A. Gedanken
采用微波辐射技术，在10-40 min内快速制备了SnS和SnS 2纳米片，产率可达93%。以四氯化锡和四氯化亚锡为锡的前驱体，硫脲为硫的前驱体，乙二醇为溶剂，氩气保护下，在简易微波炉中合成了硫化物。还尝试了元素硫和硫代硫酸钠作为硫的前体。采用X射线粉末衍射（XRD）、差示扫描量热法、能量色散X射线分析、透射电子显微镜、选区电子衍射、拉曼光谱和标准电化学技术对产物的结构、形貌、组成和物理性能进行了表征。XRD图谱表明，微波辐照后得到的合成产物在SnS相的情况下为结晶正交晶，在SnS 2的情况下为非晶。这种SnS 2的热处理产生的结晶六方相。本文提出了形成硫化锡纳米片的可能机制。这些材料作为锂插入材料的电化学性能进行了研究，在一些电解质溶液中，并被发现是高度敏感的解决方案的组成。SnS电极的可逆容量大于600 mAh/g。
A novel and quick method has been developed for the preparation of tin sulfide (SnS and SnS2) nanoflakes in high yield (≈93%) by a microwave irradiation technique for 10–40 min. The sulfides were synthesized in a simple domestic microwave oven (DMO) using stannic chloride and stanous chloride as the precursors of tin and thiourea as the precursor of sulfur in ethylene glycol under argon atmosphere. Elemental sulfur and sodium thiosulfate were also tried as precursors of sulfur. The structures, morphologies, compositions, and physical properties of the products were characterized by powder X-ray diffraction (XRD), differential scanning calorimetry, energy dispersive X-ray analysis, transmission electron microscopy, selected area electron diffraction, Raman spectroscopy, and standard electrochemical techniques. The XRD patterns indicate that the as-synthesized product, obtained after microwave irradiation, is crystalline orthorhombic in the case of the SnS phase and amorphous in the case of SnS2. Heat treatment of this SnS2produced a crystalline hexagonal phase. A possible mechanism for the formation of the tin sulfide nanoflakes is proposed herein. The electrochemical performance of these materials as Li-insertion materials was investigated in a number of electrolyte solutions and was found to be highly sensitive to the solution composition. A stable reversible capacity higher than 600 mAh/g could be obtained with SnS electrodes.