Ni-S二元化合物的杂化微波合成及性能表征  

Hybrid Microwave Synthesis of Nickel Sulfides and Property Characterization

作　　者：葛林慧[1,2] 董成[2] 何维[1] 贺兵[2] 杨立红[2] 慕利斌[2] 陈晓超[2] 

机构地区：[1]广西大学材料科学与工程学院,南宁530004 [2]中国科学院物理研究所超导国家重点实验室,北京100080

出　　处：《材料导报》2012年第24期41-45,共5页Materials Reports

基　　金：国家自然科学基金面上项目(20871119;50961002);科技部973项目(2011CBA00112;2011CB808202)

摘　　要：采用可控温、通气氛的杂化微波加热技术,成功合成了Ni3S2、ε-NiS、δ-NiS和NiS2四种化合物。采用XRD和SEM对样品的物相和形貌进行了表征,结果表明此方法容易合成单相的Ni3S2,通过改变烧结条件可获得主相分别为ε-NiS和δ-NiS的样品,合成单相NiS2则比较困难。电磁测量和低温XRD衍射的结果表明,随着温度上升,δ-NiS在260K附近发生顺磁-反铁磁(金属-非金属)转变,同时晶体点阵参数a、c分别减小0.38%和1.4%,在相变温区表现负热膨胀性。Ni3S2单相样品显示顺磁金属性质。A novel temperature-controlled hybrid-microwave method for the synthesis of binary nickel sulfides under argon atmosphere was demonstrated. Using this method, four binary compounds Ni3S2,δ-NiS, ε-NiS and NiS2 were successfully synthesized by adjusting the heating-rate, reaction time and temperature. The products were characterized by means of X-ray powder diffraction and scanning electron microscopy. XRD phase analyses indicate that single-phased NiaS2 can be prepared easily, while δ-NiS and ε-NiS can be obtained as the major phase by adjusting the preparing condition. It is difficult to prepare single-phased NiS2 sample by the microwave method due to the vaporization of sulfur. The temperature dependence of the electrical resistivity and lattice parameters of the δ-NiS phase were measured in the temperature range of 5-300K. The δ-NiS sample exhibits a paramagnetie to antiferromagnetic （metal-nonmetal） phase transition near 260K, accompanied by 0. 38% and 1.4% increasing of the lattice parameters a and c, respectively. Nia S2 shows paramagnetic metal behavior.

关 键 词：杂化微波合成 镍的二元硫化物 电阻率磁化率 

分 类 号：O644[理学—物理化学]