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Zn3N2粉末的高效制备和表征

Efficient preparation and characterization of Zn3N2powder

  • 摘要:以金属锌粉为原料,氨气为氮源,甘油为添加剂,利用高温直接氮化法制备Zn 3N 2粉末。研究了甘油含量、反应温度以及反应时间对产物中Zn 3N 2质量分数的影响。通过X射线衍射仪、扫描电子显微镜、X射线能量色散光谱仪、X射线光电子能谱分析了产物的物相组成、微观形貌、元素分布以及样品表面的化学状态。结果表明:甘油分子内部的键在加热后开始断裂,产生的还原性物质可以还原锌粉表面的ZnO,减少了ZnO的含量,从而有利于后期Zn与NH 3之间的反应,提高产物中Zn 3N 2含量,改善Zn 3N 2粉末分散性。当甘油与锌粉比例(体积/质量,mL/g)为0.20时,经600 ℃加热3 h,可以制备出Zn 3N 2质量分数为95.72%的粉末,获得Zn 3N 2粉末的光学带隙为2.60 eV。

    Abstract:Zn 3N 2powders were prepared by the high-temperature direct nitriding method using metallic zinc powder as the raw material, ammonia gas as the nitrogen source, and glycerol as the additive. The effects of glycerol content, reaction temperature, and reaction time on the mass fraction of Zn 3N 2in the products were studied. The phase composition, microstructure, elemental distribution, and the sample surface chemical state of the products were analyzed by X-ray diffractometer, scanning electron microscope, X-ray energy dispersive spectrometer, and X-ray photoelectron spectroscopy. In the results, the glycerol bonds within the molecule begin to break after heating, which makes the reducing substances reduce ZnO on the surface of zinc powders, lowering the content of ZnO. This is conducive to the reaction between Zn and NH 3in the later stage, increasing the content of Zn 3N 2in the products and improving the dispersibility of Zn 3N 2powders. When the ratio of glycerol to zinc powder (volume/mass, mL/g) is 0.20, after heating at 600 ℃ for 3 h, the Zn 3N 2powders with mass fraction of of 95.72% can be prepared, and the optical band gap of the obtained Zn 3N 2powders is 2.60 eV.

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