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.
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