摘要
将V2O5溶解于有机酸溶液中, 通过喷雾干燥制得非晶态含钒的粉末前驱体, 将前驱体粉末还原/碳化后得到V8C7粉末. 采用X射线衍射仪﹑扫描电镜﹑透射电镜﹑碳氧分析仪对工艺过程产品进行分析. 结果表明: 前驱体是粒度为10~20 μm非晶态球形粉末, 当温度升高到400 ℃时, 前驱体粉末开始分解;当温度升高到600 ℃时, 前驱体粉末全部转变为V2O3与游离C原子级别混合均匀的复合粉末;随着温度的升高, 游离C还原碳化V2O3, 当温度升高到800 ℃时, 出现V4C3相;在约1 100 ℃时, 得到相成分均一的V8C7粉末, 其形貌是粒径为30~50 nm的一次颗粒形成的多孔空壳球形, 其总C含量为17.38%, 游离C含量为0.47%. 前驱体粉末在加热过程中相成分转变过程为: V2O3→V4C3→V8C7, 不经历V2O3 转变为VO的过程.
Dissolving V2O5 in organic acid solution, the amorphous powder precursor which contained vanadium was obtained by spray drying, and the nanometer V8C7 powder was prepared through reduction/carbonization of the precursor powder. The technological process was investigated and analyzed using X-ray diffractometer, scanning electron microscope (SEM), transmission electron microscope (TEM) and carbon & oxygen analyzer. The results show that the pre- cursor is amorphous spherical powder of 10 - 20μm. When the temperature rises to 400℃ in vacuum, the precursor begins to decompose; when the temperature rises to 600℃, all the precursor powder is transformed into the composite powder in which V2O3 mixes with free carbon homogeneously atom-level; V2O3 is reduced and carbonized by free carbon with the temperature, and when the temperature goes up to 800℃, the V4C3 phase occurs. At about 1 100 ℃, the VC7 powder is obtained with single phase, and its morphology is of porous hollow sphere formed by many first particles of 30 - 50 nm. The total carbon content is 17.38% and the free carbon content is 0.47%. In the process of reduction/carbonization, the precusor powders undergo the following phase transformation: V2O3→V3C3→V8C7, without undergoing the process of phase transformation from V2O3 into VO phase.
出处
《中南大学学报(自然科学版)》
EI
CAS
CSCD
北大核心
2005年第5期771-775,共5页
Journal of Central South University:Science and Technology
基金
国家高技术研究发展计划资助项目(2002AA331090)
关键词
碳化钒
纳米
喷雾干燥
还原/碳化
晶粒抑制剂
vanadium carbides nanometer
spray dried
reduction/carburization
grain growthinhibitor