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研究生: 江泓晏
Jiang, Hung-Yan
論文名稱: 具超音速粒子衝擊機構之乾式奈米研粉系統研究
Performance of Nano Powder Production System with Supersonic Impingement Mechanism
指導教授: 王覺寬
Wang, Muh-Rong
學位類別: 碩士
Master
系所名稱: 工學院 - 航空太空工程學系
Department of Aeronautics & Astronautics
論文出版年: 2012
畢業學年度: 100
語文別: 中文
論文頁數: 84
中文關鍵詞: 超音速噴嘴對衝粉碎法乾式奈米研粉粒徑分布
外文關鍵詞: Supersonic nozzle, Opposed jet milling, Dry milling, Particle distribution
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  • 本計畫探討超音速粒子對衝型乾式奈米研粉技術,以因應高純度粉體材料,超硬材料粉體之奈米化需求。本技術以超音速粒子對衝式噴嘴,將製程材料以高速氣流加速至超音速,利用超音速粒子對衝機制,提高其粉碎能量,一舉突破傳統機械式粉碎法能量上的限制,以產生超微粒的奈米粉末。此技術由於利用超音速粒子對衝機制,故製程中沒有機械轉動件,而且粉體粒子由高速氣流所推動,沒有機會接觸傳統奈米研磨機的刀片,可以避免奈米粉體在製程中的污染。本研究先以數值方法進行噴嘴及對衝流場模擬,然後進行超音速噴嘴流場測試,再以碳酸鈣粉末進行系統可行性測試。接著以甲殼素粉末進行參數測試,尋找系統最佳化的參數設定。最後根據參數實驗的結果進行碳化矽粉末之研粉實驗。實驗結果顯示,粉末經過一次對衝即可產生5%以上體積比率之細粉含量,具有顯著之粉末微小化效果,可以運用於特殊材料之微小化應用。當氣體操作壓力愈大,以甲殼素粉末為例,所產生的微粉末中,10μm以下的小粒徑比例逐漸遞增。當氣體壓力為2.0 kg/cm2時,小於10μm的粉末所占體積從原粉末的8.46%增加至12.9%,體積增加率為52.5%;而當氣體壓力進一步增加到4.0 kg/cm2時,小於10μm的粉末所占體積增加至18.0%,體積增加率為113%。以碳化矽粉末為例,原粉末中粒徑皆大於4μm,當對衝氣體壓力為2.0 kg/cm2時,微粉末中開始出現小於4μm的粉末,其所占體積百分比為2.34%;而當氣體壓力增加到4.0 kg/cm2時,小於4μm的粉末所占體積百分比提高至5.04%。顯示經過超音速粒子對衝型乾式奈米研粉系統操作之後,粉末粒子互相碰撞會造成粒子的顯著破裂。將來若設計成連續式操作之量產型系統,使粒子能夠在腔體內連續重複對衝,可以產生更微小化的奈米粉末。

    This research develops a supersonic nozzle for the pulverization on the powders with high purity and high hardness. Opposed jet mills offer various advantages such as the ability to produce particles with narrow size distribution, and less contaminations because of autogenous grinding. Numerical simulation of the opposed jet was performed in order to characterize the supersonic nozzle and system. The performance of the supersonic nozzle was then analyzed with compressed gas flow without particle loading. Feasibility analysis of the jet mill system was performed by using calcium carbonate (CaCO3) powder. Finally, optimization on system performance was performed on chitosan and silicon carbide (SiC) particles. Results shows that the differential volume percentage of the fine powder is significantly increased over five percent in one impinging process without particle reflow. It indicates this system can be employed to produce ultra-fine powder with high purity. The differential volume of smaller chitosan particles(<10μm) is enhanced as the operating gas pressure increased. The differential volume of the chitosan particles less than 10μm is increased from 8.46% to 12.9%(about 52.5% enhancement in differential volume percentage)with operating gas pressure 2.0 kg/cm2. As operating gas pressure being increased to 4.0 kg/cm2, the differential volume of the chitosan particles less than 10μm is increased to 18.0%(about 113% enhancement in differential volume percentage).Furthermore, we performed experiment on silicon carbide powders, which have no particles smaller than 4μm before milling. Results show that the differential volume of silicon carbide powders less than 4μm increased from 0% to 2.34% and 0% to 5.04% with operating gas pressure 2.0 kg/cm2 and 4.0 kg/cm2, respectively. The production rate of the fine particles can be further increased as the system is designed for the continuous operation with reflow of the particles.

    目錄 中文摘要 Abstract 致謝 目錄 I 表目錄 IV 圖目錄 V 符號說明 VIII 第一章 緒論 1 1-1簡介 1 1-2文獻回顧 2 1-2-1奈米材料的特殊性質 2 1-2-2奈米粉末的製程技術簡介 5 1-2-3對衝式氣流粉碎法 11 1-3研究動機與目的 14 第二章 實驗設備及儀器 16 2-1實驗設備 16 2-2量測儀器 23 第三章 實驗步驟與方法 29 3-1數值模擬 29 3-1-1基本假設 29 3-1-2統御方程式 30 3-1-3數值方法 31 3-1-4網格系統與邊界條件 31 3-1-5收斂標準 33 3-2超音速粒子對衝型乾式奈米研粉系統性能量測 33 3-2-1氣體流率測試 33 3-2-2負壓測試 35 3-3超音速粒子對衝型乾式奈米研粉系統製程操作 36 3-3-1超音速粒子對衝型乾式奈米研粉系統製程可行性測試 37 3-3-2超音速粒子對衝型乾式奈米研粉系統甲殼素奈米化製程 37 3-3-3超音速粒子對衝型乾式奈米研粉系統碳化矽奈米化製程 38 3-3-4微粉末之防護 38 3-4粒末量測 39 3-4-1粉末粒徑分佈量測 39 3-4-2粉末外觀及成分分析 39 3-5實驗誤差 40 3-5-1超音速粒子對衝型乾式奈米研粉系統製程誤差 40 3-5-2粒徑分析儀之儀器誤差 40 3-5-3掃描式電子顯微鏡之儀器誤差 40 第四章 結果與討論 41 4-1噴嘴流場之數值模擬 41 4-2超音速粒子對衝型乾式奈米研粉系統性能量測 44 4-2-1氣體操作壓力對系統氣體流率影響 44 4-2-2抽氣機頻率對系統氣體流率影響 46 4-2-3抽氣機頻率對負壓之影響 48 4-3超音速粒子對衝型乾式奈米研粉系統製程可行性測試 50 4-4超音速粒子對衝型乾式奈米研粉系統甲殼素奈米化製程 53 4-4-1氣體操作壓力對甲殼素奈米化製程之影響 53 4-4-2抽氣機頻率對甲殼素奈米化製程之影響 62 4-5超音速粒子對衝型乾式奈米研粉系統碳化矽奈米化製程 68 第五章 結論 78 第六章 未來工作 80 參考文獻 81 表目錄 表1-1國內主要供應奈米粉體製造機台之廠商 14 表3-1氣體流率測試實驗操作條件 34 表3-2負壓測試實驗操作條件 35 表3- 3碳酸鈣與碳化矽粉末原料性質表 36 表3- 4甲殼素粉末原料性質表 36 表3-5材料與分散劑一覽 39 表4-1氣體流率隨操作壓力之變化 45 表4-2氣體流率隨抽氣機頻率變化 47 表4-3負壓隨抽氣機頻率變化 49 表4-4碳酸鈣粉末研磨前後粒徑對照表 51 表4- 5甲殼素粉末粒徑隨氣體壓力之變化 56 表4-6甲殼素粉末V10-隨氣體壓力變化增加之百分比 59 表4-7甲殼素粉末V20-隨氣體壓力變化增加之百分比 59 表4- 8甲殼素粉末V30-隨氣體壓力變化增加之百分比 60 表4- 9甲殼素粉末粒徑隨抽氣機頻率之變化 64 表4-10甲殼素粉末V10-隨抽氣機頻率變化增加之百分比 67 表4-11甲殼素粉末V20-隨抽氣機頻率變化增加之百分比 67 表4-12甲殼素粉末V30-隨抽氣機頻率變化增加之百分比 68 表4-13碳化矽粉末粒徑隨氣體壓力之變化 71 表4-14碳化矽粉末V4-隨氣體壓力之變化 73 表4-15研磨後碳化矽粉末成份分析 76 圖目錄 圖1-1奈米粉體製備方法[2] 5 圖1-2球磨法製粉示意圖[4] 6 圖1-3行星式球磨機示意圖[5] 7 圖1-4螺旋式氣流粉碎示意圖[8] 8 圖1-5靶式氣流粉碎法示意圖[12] 9 圖1-6對衝式氣體粉碎法示意圖[8] 10 圖2- 1超音速粒子對衝型乾式奈米研粉系統示意圖 16 圖2-2實驗系統照相圖 17 圖2-3振動篩分機示意圖 18 圖2-4螺旋饋料機照相圖 19 圖2-5對衝式衝擊腔體照相圖 20 圖2-6超音速粒子對衝型乾式奈米研粉系統作用及機制示意圖 21 圖2-7粉末收集器照相圖 22 圖2- 8浮子式流量計[33] 25 圖2- 9浮子式流量計尺寸示意圖[33] 25 圖2-10 BECKMAN COULTER Ls230 雷射繞射粒徑分析儀 26 圖2-11 Hitachi SU8000 掃描式電子顯微鏡 28 圖3- 1三維流場網格(一) 32 圖3- 2三維流場網格(二) 32 圖4- 1對衝流場之速度分佈圖 42 圖4- 2對衝流場之馬赫數分佈圖 42 圖4- 3衝擊腔體碰撞區 43 圖4- 4對衝流場之溫度分佈圖 43 圖4- 5氣體流率隨操作壓力之變化 45 圖4- 6氣體流率隨抽氣機頻率變化 47 圖4- 7負壓隨抽氣機頻率變化 48 圖4- 8研磨前後碳酸鈣粉末粒徑累積體積分布 51 圖4-9碳酸鈣粉末經研磨後之SEM照相圖 52 圖4- 10研磨前後甲殼素粉末粒徑累積體積分布 54 圖4- 11甲殼素粉末Dv50隨氣體壓力之變化 55 圖4- 12研磨前後甲殼素粉末粒徑累積體積分布 55 圖4- 13甲殼素粉末V10-隨氣體壓力之變化 57 圖4- 14甲殼素粉末V20-隨氣體壓力之變化 57 圖4- 15甲殼素粉末V30-隨氣體壓力之變化 58 圖4- 16甲殼素粉末之 ΔV10- 、ΔV20- 及ΔV30-隨氣體壓力之變化 58 圖4-17甲殼素粉末原料SEM照相圖 61 圖4-18甲殼素粉末經過超音速氣流衝擊一次SEM照相圖(一) 61 圖4-19甲殼素粉末經過超音速氣流衝擊一次SEM照相圖(二) 62 圖4- 20甲殼素粉末Dv50隨抽氣機頻率之變化 64 圖4- 21甲殼素粉末V10-隨抽氣機頻率之變化 65 圖4- 22甲殼素粉末V20-隨抽氣機頻率之變化 65 圖4- 23甲殼素粉末V30-隨抽氣機頻率之變化 66 圖4- 24甲殼素粉末 ΔV10- 、ΔV20- 及ΔV30-隨抽氣機頻率之變化 66 圖4- 25碳化矽原料粉末粒徑分布圖 70 圖4- 26碳化矽粉末Dv50隨氣體壓力之變化 70 圖4- 27研磨前後碳化矽粉末粒徑累積體積分布 71 圖4- 28研磨前後碳化矽粉末粒徑累積體積分布 72 圖4- 29碳化矽粉末V4-隨氣體壓力之變化 72 圖4-30碳化矽粉末原料SEM照相圖 74 圖4-31碳化矽粉末經過超音速氣流衝擊一次SEM照相圖 74 圖4-32碳化矽粉末經過超音速氣流衝擊一次SEM照相圖 75 圖4-33碳化矽粉末經過超音速氣流衝擊一次SEM照相圖 75 圖4-34研磨後碳化矽粉末成份分析 77

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