摘要以乙酸镍为原料，二巯基丁二酸(DMSA)为螯合剂，乙醇为溶剂，采用溶剂热法制备了NiS2纳米粒子。采用XRD、SEM、TEM对所制备的纳米粒子晶体结构和形貌进行了表征。结果表明：通过控制反应物用量、温度、反应时间等条件，发现在200 ℃反应16 h，Ni2+与DMSA的比例是1:2时，所制备的纳米粒子分布最为均一、大小最为均一，且核壳结构明显，开口结构也最多，得到了近单分散的具有核壳结构的NiS2纳米粒子。其平均粒径约为500 nm，其中核的直径约为400 nm，是结晶性良好的立方相的NiS2纳米粒子。同时也研究了DMSA与其它金属离子包括Ag+、Co2+、Cu2+、Fe3+等的反应，研究了产物的形貌和晶体结构。63806

毕业论文关键词  DMSA 溶剂热 NiS2 核壳结构 

毕业设计说明书(论文)外文摘要

Title   DMSA (Meso-2,3-dimercaptosuccinic acid) Controlled Synthesis of Metal Sulfide Nanoparticles                                      

Abstract

In this thesis, NiS2 nanoparticles were successfully prepared by solvothermal method, with Ni(CH3COO)2·4H2O as reactant, meso-2,3-dimercaptosuccinic acid (DMSA) as chelating agent and C2H5OH as solvent. The crystal structure and morphology of as-prepared products were characterized by XRD, SEM and TEM methods. The optimum nanoparticles were synthesized via controlling the amount of reactant, temperature and reaction time. The results show that when the ratio of Ni2+ and DMSA was 1:2 reacting under 200 C for 16 hours, the nearly monodispersed NiS2 nanoparticles with core-shell structure can be obtained. The obtained nanoparticles have the homogeneous distribution, uniform sizes and the distinct core-shell structures, which were well crystalline cubic NiS2 with more opening structures. The average particle size is about 500 nm, and the diameter of the core is around 400 nm. We also studied the reactions of DMSA with other metal ions such as Ag+、Co2+、Cu2+、Fe3+ and the morphology and crystal structure were discussed.

Keywords  DMSA solvothermal NiS2 core-shell structure 

1绪论 1

1.1 金属硫化物概述 1

1.2 金属硫化物纳米材料的制备 2

1.2.1 固相法 2

1.2.1.1 物理粉碎法 2

1.2.1.2 固相反应法 2

1.2.2 液相法 3

1.2.2.1 水热/溶剂热法 3

1.2.2.2 热分解法 3

1.2.2.3 微乳液法 4

1.2.2.4 模板合成法 4

1.2.3 气相法 5

1.2.3.1 化学气相沉积法 5

1.2.3.2 气体蒸发法 5

1.3 具有分级结构的材料 6

1.4 二巯基丁二酸(DMSA)简介及其在纳米材料控制合成中的应用 6

1.5 本课题的主要研究内容及实验方案 7

1.5.1研究内容与目的 7

1.5.2 实验方案 7

2 二硫化镍的制备 7

2.1 实验试剂与仪器分析 8

2.1.1 实验试剂与仪器 8

2.1.2 实验表征方法