非晶态Ni-B合金的制备及表征.doc

实验八 非晶态Ni-B合金的制备及表征一、实验背景镍催化剂被广泛应用于化学工业的加氢反应。非晶态镍基合金，例如Ni-B和Ni-P都是很好的加氢材料，因为同其它加氢催化材料相比，它们表现出优秀的催化活性和高的选择性。而且，在制备方法上，可以获得与具有高比表面积的超细非晶态合金，这通过传统的骤冷法是难以得到的。非晶态合金优秀的催化活性主要归功于非晶相的原子排列和类金属原子的电子效应（如B和P）。二、实验目的学习利用化学还原法制备非负载非晶态Ni-B合金，并初步掌握DSC、XRD和TEM等大型仪器的使用及结果分析。三、实验提示1主要参考文献1 闵恩泽, 李成岳等著. 第六章 非晶态合金催化剂及其催化性能. 绿色石化技术的科学与工程基础. 中国石化出版社, 北京, 2002, 250-2712 张荣斌, 石秋杰, 李凤仪, 罗来涛. 非晶态合金催化剂研究进展. 江西科学 1999, 17(3),190-1962查阅文献的关键词非晶态合金，镍硼3实验关键（1）步中NH3H2O 络合Ni2必须15min。（2）步中溶液没有气泡产生就可停止反应。（3）步中产物必须用乙醇洗涤，以避免氧化。（4）步中产物必须放入乙醇中保存，以避免着火。四、实验药品与仪器药品：NiSO46H2O；NH3H2O；KBH4；AgNO3；无水乙醇仪器：小烧杯；水浴锅；磁力搅拌；循环水泵；抽滤装置表征所用仪器：DSC；XRD；TEM五、实验要求1阅读给定的文献，并用关键词在网上或在图书馆查阅相关的参考文献。2制定研究方案（合成和表征），3探索化学法制备非晶态合金的规律。4对研究的结果展开讨论。5提交研究论文。六、思考题1. 影响产率的因素有哪些？2. DSC、XRD和TEM表征的结果能给我们什么信息？Preparation and Characterization of Amorphous Ni-B AlloysBackgroundNickel catalysts are widely used in the chemical industry for hydrogenation reactions. Amorphous nickel alloys, such as nickel boride (Ni-B) and nickel phosphide (Ni-P), are particularly interesting as hydrogenation catalysts, since these materials may exhibit higher activity, greater selectivity, and better stability, than their crystalline counter parts. Moreover, recent advances in sample preparation have produced ultrafine amorphous alloy particles, having significantly higher surface area than amorphous alloy ribbons and films prepared by conventional melt-quench techniques. The attractive catalytic properties of these amorphous alloys have been attributed to a random arrangement of atoms in the amorphous phase and also to an electronic effect contributed by the metalloid elements (e.g., B and P).IntentionStudents prepare amorphous alloys using a chemical route, and learn to make use of DSC, XRD and TEM for analyzing results.Clue1Main Literatures1 Min Enze, Li Chengyue. sixth chapter catalysis and catalytic performance of amorphous alloys. The foundation of science and engineering for green petrifaction technology. Petrifaction publishing company of China, Beiking, 2002, 250-2712 Zhang Rongbin, Shi Qiujie, Li Fengyi, Luo Laitao. Research of amorphous alloys catalyst science jiangxi 1999, 17(3),190-1962Key WordsAmorphous alloys, Ni-B3Key Processing（1）Maintaining 15 min for NH3H2O and Ni2 ions.（2）Ceasing the reaction when the bubbles vanish in the solution.（3）The sample is washed using ethanol to avoid oxidation.（4）The sample is saved in ethanol to avoid take fire.Reagents and InstrumentsReagents：NiSO46H2O；NH3H2O；KBH4；AgNO3；ethanolInstruments： beaker； heater；stirrer； water pump； the instrument for filtrationInstruments for Characterization：DSC；XRD；TEMDemandStudents search the literatures on the internet and read them.1Confirm the experimental scheme and explore the rule for preparing amorphous alloys.2Discuss the experimental results.3Pro