【作者】 胡坤宏；

【导师】 韩效钊；

【作者基本信息】 合肥工业大学 ， 化学工艺， 2004， 硕士

【摘要】 首先通过酸化M₂S与M₂MoO₄（M为Na⁺或NH₄⁺）混合溶液制备出纳米三硫化钼，然后将制备的三硫化钼在氢气氛下加热脱硫得到纳米二硫化钼。 在制备纳米三硫化钼的反应中，利用单因素条件实验与正交实验研究了各种因素条件对三硫化钼收率的影响，得出了优化工艺条件，利用X射线衍射仪（XRD）和透射电子显微镜（TEM）对优化工艺条件制备的三硫化钼进行了表征，发现无论是用硫化钠与钼酸钠反应体系还是用硫化铵与钼酸铵反应体系，制备的三硫化钼均是典型的非晶态物质，粒子平均粒径约为100nm左右。 在三硫化钼脱硫制备二硫化钼反应中，利用热力学数据分析了反应的可行性，并初步探讨了副反应的发生条件。结合热力学分析及动力学分析讨论了二硫化钼制备的适宜温度范围。研究了反应速率与温度、时间及氢气流量的关系，得出了制备的三硫化钼在氢气氛下脱硫制备二硫化钼反应的动力学方程。借助XRD与TEM表征手段研究了制备工艺条件对二硫化钼的粒径与结晶状态的影响，发现温度是影响粒子尺寸与结晶状态的主要因素。另外不同的反应体系对二硫化钼粒径也存在明显的影响，利用硫化钠与钼酸钠制备的二硫化钼粒径可达30nm左右，而利用硫化铵与钼酸铵制备的二硫化钼的粒径约为80nm。 最后，在MQ-800四球摩擦磨损试验机上对制备的纳米二硫化钼的摩擦学特性进行了初步研究，发现在凡士林体系中，添加了纳米二硫化钼的润滑性能优于添加了工业普通尺寸的二硫化钼（粒径为1.5μm）。另外还研究了纳米二硫化钼与工业普通尺寸的二硫化钼复配时的摩擦学特性，发现在液体石蜡体系中，添加两者复配物的润滑性能比添加单一形式的二硫化钼要优，且纳米二硫化钼在复配物中的含量为15％左右时润滑性能最优。更多还原

【Abstract】 Molybdenum trisulfide (MOS3) nano-particles were firstly obtained by acidifying the mixed solution of M2S and M2MoO4 (M: Na+ or NH/). Then nano-sized molybdenum disulfide (M0S2) particles were produced by the desulphurization of the prepaed M0S3 under H2 atmosphere.In the first-step reaction, an optimized preparation process was investigated after single-factor and orthogonal experiments. Results of characterization by X-ray diffraction (XRD) and transmission electron microscope (TEM) showed that the average size of amorphous M0S3 particles is about 100 nm prepared under the optimized process conditions.Thermodynamic analyses demonstrated the feasibility of the second-step reaction, and studied the possibility of two subsidiary reactions as well. A proper temperature range for the preparation of M0S2 was work out by thermodynamic and kinetic analyses. A kinetic equation was work out to represent the relation of the reaction time and the yield of M0S2. The crystallization and the average sizes of M0S2 particles prepared under different conditions were also investigated by XRD and TEM. The results showed that the reaction temperature is the primary factor affecting the crystallization and size of particles. Moreover, different reaction systems also play an important role in the size-controlling of M0S2 particles. The average size of M0S2 obtained by Na2S and Na2MoO4 is about 30 nm, however, that by (NH4)2S and (NH4)2MoO4 is about 80 nm.Compared with commercial common M0S2 particles (1.5 \xm in diameter), the tribological properties of the prepared M0S2 nanoparticles were carry out with MQ-800 four-ball tribometer. The results showed that samples containing M0S2 nanoparticles are of better lubricating properties than others containing common M0S2. Moreover, the tribological performances of the mixture of M0S2 nanoparticles and commercial M0S2 particles were also studied, and the results showed the complex in liquid paraffin represents a better lubrication than others samples, especially, a highest extreme pressure can be obtained as the ratio of nano-MoS2 and common M0S2 is about 15 : 85 (wt.%).更多还原