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研究生： 葉惠祿
Yasaputera, Robert
論文名稱： 使用球形鋁粉燃燒合成及量產氮化鋁製程開發
Process Development for Combustion Synthesis and Scale-up Production of Aluminum Nitride Using Spherical Aluminum Powder
指導教授： 鍾賢龍
Chung, Shyan-Lung
學位類別： 碩士
Master
系所名稱： 工學院 - 化學工程學系
Department of Chemical Engineering
論文出版年： 2019
畢業學年度： 107
語文別： 英文
論文頁數： 94
外文關鍵詞： Combustion synthesis, Aluminum Nitride, Urea additive, Al(OH)3 additive, NH4Cl Additive, Aluminum Nitride diluent.
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    • The technique for the synthesis of aluminum nitride powder by self-propagating high-temperature synthesis (SHS) has been well developed in our laboratory. The mostly used aluminum powder for the synthesis has been flake in shape with dimensions of 1 mm x 1 mm x 25 μm, and a purity of 99.9 %. This aluminum powder has a high purity and a good reactivity but is relatively costly. In order to reduce the production cost and avoid the monopolization of the source of aluminum powder, we searched for other sources for aluminum powder. In this research, we focused on the synthesis of aluminum nitride powder by using the new, spherical aluminum powder with 21 μm in size combinations (d50). Different nitrogen gas pressure and several additives, including aluminum nitride, urea, Al(OH)3, and NH4Cl, with different amounts and sizes, and there were tested in order to improve the aluminum nitride conversion. The combustion phenomena were also found to be affected by the types, amounts and the size of the additives. An increased of aluminum nitride conversion was synthesized using urea additive with certain amounts and smaller additive size. Using other additive, such as Al(OH)3, results in a poor reactivity to nitridation due to the fine Al2O3 formed after the thermal decomposition of the additive, while using NH4Cl as additive results in an incomplete combustion reaction, and it is speculated because of the ammonium azide formed as a candidate material to hindered further nitridation. Several parameters that were tested in this study, such as different nitrogen pressure, additives amount, and additives size indicating the poor reactivity of the new spherical aluminum powder. It is speculated that the phenomenon also caused by the high reactant packing density of the powder.
    For a small scale production (146.6g AlN per batch), highest conversion achieved was around 99.35% by using AlN (with AlN:Al ratio of 10:90), urea (1wt%) as additives, and under 10 atm of nitrogen pressure. For a large scale production (4.7 kg AlN per batch), due to the poor reactivity and high packing density of the aluminum powder, incomplete combustion with low conversion of aluminum nitride was observed.

    Abstract I Acknowledgement III Table of Contents IV List of Tables VI List of Figures VII Chapter I - Introduction 1 1-1 Introduction to Ceramic Materials 1 1-2 AlN Properties and Applications 2 1-3 AlN Synthesis Method 5 Chapter II – Principles and Literature Reviews 9 2-1 Combustion Synthesis SHS Method 9 2-2 Combustion Synthesis Thermodynamic Analysis 11 2-3 Combustion Synthesis Kinetics Analysis 14 2-4 Effect of reactant porosity and pressure on combustion synthesis reaction 15 2-5 Relationship between temperature profile of combustion synthesis and additives added 17 2-6 Research Motivation 21 Chapter III – Experimental 23 3.1 Raw materials 23 3.2 Equipment for combustion of aluminum nitride (AlN) 24 3.2.1 Small Reactor 24 3.2.2 Mass Production Reactor 25 3.2.3 Grinding and ball milling equipment 26 3.2.3.1 Small grinding 26 3.2.3.2 Ball Mill 27 3.2.4 Other equipment 28 3.3 Analytical Instrument 29 3.3.1 Oxygen and Nitrogen Analyzer 29 3.3.2 Particle Size Analyzer 29 3.3.3 X-Ray Diffractometer (XRD) 30 3.3.4 Field Emission Scanning Electron Microscope (FE-SEM) 31 3.4 Experimental step for aluminum nitride combustion. 31 3.4.1 Reactant preparation. 31 3.4.2 Combustion synthesis reaction 33 3.5 Product analysis 35 3.5.1 Product classification 35 3.5.2 Product conversion analysis 36 Chapter IV – Result and Discussion 39 4.1 Aluminum powder source and its properties 39 4.2 Small scale of Al2 reactant 42 4.2.1 The effect of nitrogen pressure 42 4.2.2 The effect of aluminum nitride diluent addition 44 4.2.2.1 The effect of aluminum nitride diluent ratio 45 4.2.2.2 The effect of aluminum nitride diluent size 47 4.2.3 The effect of urea additive addition 50 4.2.3.1 The effect of urea additive amount 50 4.2.3.1 The effect of urea additive size 53 4.2.4 The effect of Al(OH)3 additive addition 57 4.2.4.1 The effect of Al(OH)3 additive amount 57 4.2.4.2 The effect of Al(OH)3 additive size 68 4.2.5 The effect of NH4Cl additive addition 71 4.2.5.1 The effect of NH4Cl additive amount 71 4.3 Scale-up study of Al2 reactant 79 Chapter V – Conclusion 84 Chapter VI – References 87

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