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用碘输运法,采用三温区工艺合成和生长 TiS_2单晶。作为高温反应区的中区保持1000℃,两端交替地作为硫冷凝区和供硫区。合成阶段,两端区的温度按一定程序升温,最后直至分别为800℃和900℃。晶体生长阶段,生长区的温度在800℃作±10℃的摆动,用这种温度摆动工艺得到金黄色的片状单晶,最大晶片的面积达10×5毫米~2。晶体经 X 射线衍射分析、扫描电镜观察,看出 TiS_2的特征谱线和六角形层状图象。经化学分析和电子探针微区分析表明符合化学计量比。测得 a 轴和 c 轴的电阻率分别为10~(-3)—10~(-4)和10~(-1)—10~(-2)欧姆·厘米。会聚束电子显微镜作精细结构衍射分析拍得非常清晰的六重对称图案,表明结构完整性很好。制成 Li 电池,能量密度达296瓦·时/公斤,可逆性较好。
Iodine transport method, the use of three temperature zone synthesis and growth of TiS 2 single crystal. The middle zone, which is the high temperature reaction zone, is kept at 1000 ° C, and both ends alternately serve as the sulfur condensation zone and the sulfur supply zone. In the synthesis stage, the temperature of the two end regions is increased by a certain program until the temperature reaches 800 ° C and 900 ° C respectively. In the crystal growth phase, the temperature in the growth zone is oscillated at ± 10 ° C at 800 ° C. The golden yellow sheet single crystal is obtained by this temperature swinging process. The maximum wafer area is 10 × 5 mm -2. X-ray diffraction analysis of the crystal, scanning electron microscopy, see the characteristic lines of TiS_2 and hexagonal layered image. Chemical analysis and electron probe microanalysis showed stoichiometry. The measured resistivities of a-axis and c-axis were 10 -3 -10 -4 and 10 -1 -10 -2 Ω · cm, respectively. Convergence beam electron microscopy for fine structure diffraction analysis takes a very clear six-fold symmetry pattern, indicating good structural integrity. Made of Li batteries, energy density of 296 W · h / kg, reversible better.