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研究生： 鍾志育
Chung, Chih-Yu
論文名稱： 鈦添加量及燒結時間對無壓液相燒結鑽石銅基複合材料之界面微結構及熱性質的影響
Effect of Titanium Addition and Varying Sintering Time on the Interface Structure and Thermal Properties of Diamond/Cu Composites Fabricated by Pressureless Liquid Phase Sintering
指導教授： 林樹均
Lin, Su-Jien
口試委員: 李勝隆
洪健龍
曹春暉
朝春光
學位類別： 博士
Doctor
系所名稱： 工學院 - 材料科學工程學系
Materials Science and Engineering
論文出版年： 2014
畢業學年度： 102
語文別： 中文
論文頁數： 143
中文關鍵詞： 複合材料 、熱傳導係數 、熱膨脹係數 、液相燒結法
外文關鍵詞： Composite, Thermal conductivity, Coefficient of thermal expansion, Liquid phase sintering
相關次數： 點閱：3  下載：0 
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    • 本實驗使用無壓液相燒結法製備鑽石銅基複合材料。由於金屬銅在鑽石表面上的潤濕性不佳，因此選擇添加活性元素至基材中，希望藉此改善界面間的潤濕性，進而得到具有良好的熱傳導性質的複合材料。而經由實驗結果得知，以鈦元素的添加具有最好的提升界面潤濕的效果。更進一步研究鑽石體積分率變化、鈦添加量多寡，以及燒結時間對於整體複合材料熱性質的影響，並且在改變燒結時間的實驗中，利用 SEM 以及 TEM 的觀測，分析鑽石與基材間的界面成長方式，以建立界面成長的機制。由界面微結構分析指出，界面層主要是由碳化鈦所組成，且界面的厚度會隨燒結時間及鈦含量的增加而變厚，對於複材的熱傳導性質有著決定性的影響。所製備出的複合材料，在鑽石體積分率 50%、鈦添加量 0.6 at% 的條件下，其熱傳導係數可高達 620 W/mK，熱膨脹係數為 6.9 ppm/K；而在鑽石顆粒雙粒徑的添加系統中，鑽石總體積分率 60% 的複材，其熱傳導值更可高達 683 W/mK。經由理論計算，本實驗製備的複合材料熱傳導值可高達理論值的 77 ~ 86%，熱膨脹係數則介於 Kerner upper line 與 Kener lower line 之間，代表此製成製備的複合材料性質良好，幾乎可與理論值吻合。另外，由於此製程為一無壓燒結製程，無須加壓設備，將可大幅降低設備成本，並且製程簡便，可用於大量生產，使此鑽石/銅基複合材料在電子構裝散熱材的應用上更具潛力。

    In this study, minor-addition elements such as Si, Co, Cr, W, Mo and Ti were added into matrix to improve the wettability between the diamonds and Cu matrix. The pressureless liquid phase sintering technique adopted in this study provides a low-cost method for producing diamond/Cu composites with high potential for industrial mass-production. Thermal properties of the diamond/Cu-Ti composites fabricated by pressureless liquid phase sintering at 1373 K with variations in Ti contents and in sintering times were thoroughly investigated. SEM and TEM analyses were
    utilized to study the growth mechanism of the TiC at the interface between diamonds and Cu matrix. A probable mechanism of the interface structure formation was proposed. The composites exhibited thermal conductivity as high as 620 W/m•K for 50 vol% diamond/Cu-0.6 at% Ti composite with diamond particle size of 300 µm. This value comes up to 85% of the thermal conductivity calculated by Hasselman and Johnson (H-J) theoretical analysis. Under these conditions a suitable coefficient of thermal expansion of 6.9 ppm/K was obtained.

    目錄 摘要…………………………………………………………………………I Abstract…………………………………………………………………III 致謝.............................................................................................................IV 目錄……………………………………………………………………….VI 圖目錄…………………………………………………………………...XI 表目錄.....................................................................................................XVII 壹、前言…………………………………………………………………….1 貳、文獻回顧……………………………………………………………….3 2.1. 散熱的重要性…………………………………………………..3 2.2. 散熱材料的發展………………………………………………..7 2.2.1. 傳統散熱材料………………………………………….7 2.2.2. 先進散熱材料………………………………………...10 2.3. 金屬基複合材料………………………………………………15 2.3.1. 金屬基複合材料常見製程…………………………….15 2.3.1.1. 攪拌鑄造法…………………………………..15 2.3.1.2. 熱壓法………………………………………..16 2.3.1.3. 氣壓浸透法…………………………………..17 2.3.1.4. 擠壓鑄造法…………………………………..17 2.3.1.5. 火花電漿燒結法……………………………..18 2.3.2. 金屬基複合材料之理論性質..........................................23 2.3.2.1. 密度................................................................23 2.3.2.2. 比熱................................................................23 2.3.2.3. 熱膨脹係數....................................................24 2.3.2.4. 熱傳導係數....................................................26 2.4. 影響鑽石複合材料熱傳導性質的因素....................................28 2.4.1. 鑽石與基材間界面接合及潤濕性的問題...................28 2.4.2. 活性元素添加對潤濕性的影響...................................32 2.4.3. 添加活性元素至複合材中改善界面接合的例子.......38 2.4.3.1. 鑽石/鋁基複合材料.......................................38 2.4.3.2. 鑽石/銀基複合材料.......................................43 2.4.3.3. 鑽石/銅基複合材料.......................................46 2.4.4. 界面厚度對熱傳導性質的影響...................................49 2.4.5. 雙粒徑強化材添加的影響...........................................54 參、實驗方法與步驟...................................................................................56 3.1 實驗設計與流程.........................................................................56 3.1.1. 成份來源及性質...........................................................56 3.1.2. 實驗設計原理...............................................................56 3.1.3. 實驗步驟.......................................................................57 3.1.3.1. 乾式混粉與冷壓成形.....................................57 3.1.3.2. 無壓真空液相燒結.........................................57 3.2. 複合材料性質分析....................................................................62 3.2.1. 試片表面結構及微結構觀察.......................................62 3.2.2. 緻密度量測...................................................................62 3.2.3. 熱膨脹係數量測...........................................................63 3.2.4. 熱傳導係數量測...........................................................64 3.2.5. XRD 分析......................................................................67 3.2.6. TEM 分析......................................................................67 肆、結果與討論...........................................................................................68 4.1. 乾式混粉前之組成粉末觀察....................................................68 4.2. 活性元素選擇............................................................................72 4.3. 活性元素鈦添加量的影響........................................................76 4.3.1. 鈦含量對於鑽石體積分率 50% 的複合材料的影響...................................................................................76 4.3.1.1. 試片表面結構及微結構觀察........................76 4.3.1.2. XRD分析結果................................................77 4.3.1.3. TEM 分析結果...............................................78 4.3.1.4. 試片熱性質分析結果....................................81 4.3.1.5. 破斷面微結構的觀察.....................................82 4.3.2. 鈦含量對於鑽石體積分率 60% 的複合材料的影響...................................................................................90 4.3.2.1. 試片中最佳鈦含量添加的理論計算............90 4.3.2.2. 試片表面微結構觀察....................................91 4.3.2.3. XRD 分析結果...............................................91 4.3.2.4. 試片熱性質分析結果....................................92 4.3.3. 鑽石體積分率 50% 及 60% 的試片之性質比較....93 4.4. 鑽石顆粒雙粒徑添加對熱性質的影響....................................98 4.5. 燒結時間對複合材料性質的影響..........................................100 4.5.1. 界面微結構觀察.........................................................100 4.5.2. 熱性質的影響.............................................................101 4.5.3. 界面成長機制的探討及建立.....................................101 4.6. 不同形貌鑽石的影響..............................................................106 4.7. 熱傳導係數實驗值及理論值的比較......................................109 4.8. 熱膨脹係數實驗值及理論值的比較......................................114 4.9. 鑽石/銀基複合材料的比較.....................................................118 伍、結論.....................................................................................................123 陸、建議未來研究方向.............................................................................126 柒、參考文獻.............................................................................................127 圖目錄 圖 2-1 晶片熱通量及冷卻技術極限的示意圖..........................................5 圖 2-2 晶片上的溫度分佈及局部熱點示意圖..........................................5 圖 2-3 常用電子構裝材料的熱傳導係數對熱膨脹係數關係圖..............8 圖 2-4 攪拌鑄造法示意圖.....................................................................19 圖 2-5(a) 間接熱壓, (b) 直接熱壓示意圖............................................20 圖 2-6 氣壓浸透法示意圖.....................................................................21 圖 2-7 擠壓鑄造法示意圖.....................................................................21 圖 2-8 脈衝電漿燒結示意圖.................................................................22 圖 2-9 脈衝電漿燒結原理示意圖.........................................................22 圖 2-10 接觸角與表面張力關係圖.......................................................30 圖 2-11 液相金屬與鑽石之間的附著功...............................................31 圖 2-12 純錫與純鉛的表面張力隨溫度的變化...................................35 圖 2-13 在不同溫度下，鉛添加量對錫鉛合金表面張力的影響.........35 圖 2-14 在970 °C、真空度為10-4 Pa下，Ag-Zr合金在AlN基板上接觸角隨時間的變化..................................................................36 圖 2-15 在1000 °C、真空度為10-3 Pa下，銀合金在BN基板上接觸角與活性元素濃度的關係圖：(1) Ti (2) Zr (3) Hf..................36 圖 2-16 在1100 °C、真空度為3×10-4 Pa下，Cu-Ti合金在石墨基板上接觸角隨時間的變化..........................................................37 圖 2-17 在1100 °C、真空度為3×10-4 Pa下，Cu-Cr合金在石墨基板上接觸角隨時間的變化..........................................................37 圖 2-18 使用鍍鈦鑽石燒結之 Diamond /Al composites 表面元素分布： (a) 表面形貌, (b) C, (c) Al, (d) Ti, (e) Si, and (f) O........42 圖2-19 Ag-Si相圖...................................................................................45 圖2-20 Si-C相圖.....................................................................................45 圖 2-21 氣壓滲透法鑽石鋁基複材斷面觀察圖，可發現 Al 附著在鑽石(100) 面上...........................................................................51 圖 2-22 氣壓滲透法鑽石鋁基複材斷面經電化學蝕刻，Al4C3 選擇性附著在 (100) 面上.................................................................51 圖 2-23 鑽石 (100) 面上 Al4C3 板狀物突起......................................52 圖 2-24 二次擠壓鑄造後斷面觀察，Al4C3 無法與鑽石 (100) 面接合..............................................................................................52 圖 2-25 HR-SEM 顯示 Diamond/Cu-Cr 複材中界面反應物 Cr3C2.........................................................................................53 圖 2-26 Diamond/Cu-Cr 複材界面反應物之 TEM 與電子繞射圖...53 圖 2-27 粒徑比與體積分率比對堆積密度之影響...............................55 圖 3-1 C-Ti 相圖....................................................................................59 圖 3-2 NT-100H 粉末成型機.................................................................60 圖 3-3 水平爐管內試片放置示意圖.....................................................60 圖 3-4 Cu-Ti 相圖..................................................................................61 圖 3-5 TMA熱膨脹係數量測-試片放置示意圖...................................63 圖 3-6 LFA 447 熱擴散係數量測與試片放置示意圖..........................65 圖 4-1 實驗所用銅粉外觀........................................................................70 圖 4-2 實驗所用鈦粉外觀........................................................................70 圖 4-3 實驗所用鑽石粉末外觀：(a) 300 µm (TYPE YK-9E)、(b) 50 µm (TYPE PK-5) 、(c) 300 µm (TYPE YK-5E)...............................71 圖 4-4 未添加活性元素燒結後之鑽石/銅基複合材料...........................74 圖 4-5 添加各種活性元素燒結後的鑽石/銅基複合材料試片外觀：(a) 矽添加、(b) 鈷添加、(c) 鉻添加、(d) 鎢添加、(e) 鉬添加，及 (f) 鈦添加.............................................................................74 圖 4-6 添加不同活性元素之鑽石/銅基複合材料之表面微結構：(a) 鎢添加、(b) 鉬添加，及 (c) 鈦添加..............................................75 圖 4-7 鑽石體積分率 50%、鈦變量之複材試片外觀：(a) 0.2 at% 鈦添加、(b) 0.3 at% 鈦添加，及 (c) 0.6 at% 鈦添加.......................84 圖 4-8 鑽石體積分率 50%、鈦變量之複材表面微結構：(a) 0.3 at% 鈦添加、(b) 0.4 at% 鈦添加、(c) 0.6 at% 鈦添加，及 0.9 at% 鈦添加.............................................................................................84 圖 4-9 鑽石體積分率 50%、鈦變量之複材 X 光結晶繞射分析圖.....85 圖 4-10 鑽石體積分率 50%、鈦添加量 0.6 at% 之複合材料界面 TEM 分析結果.....................................................................................85 圖 4-11 鑽石體積分率 50%、鈦添加量 0.6 at% 之複合材料界面 TEM 分析結果：(a) TEM 影像、(b)(c) 溝槽狀結構與鑽石界面之原子影像圖.....................................................................................86 圖 4-12 鑽石體積分率 50%、鈦添加量 0.6 at%、燒結 30 分鐘的試片，其碳化鈦與銅界面間的原子影像圖.........................................87 圖 4-13 鑽石體積分率 50%、鈦添加量 0.9 at% 之複合材料界面 TEM 分析結果，其中 I 為鑽石區、II 為 銅、碳混合區、III 為碳化鈦區、IV 為銅基地區，及 V 為試片表面氧化鈦區 (其 EDS 成份分析如插入表所示)..................................................88 圖 4-14 鑽石體積分率 50% 的複合材料之熱傳導係數、熱膨脹係數及緻密度對鈦含量的變化趨勢圖.................................................88 圖 4-15 鑽石體積分率 50%、燒結時間 30 分鐘，鈦變量的試片破斷面微結構圖：(a) 0.3 at 鈦添加、(b) 0.4 at% 鈦添加、(c) 0.6 at% 鈦添加，及(d) 0.9 at% 鈦添加...................................89 圖 4-16 鑽石體積分率 60%、燒結時間 30 分鐘，鈦變量的試片，其表面微結構分析：(a) 0.62 at%、(b) 0.72 at%，及 (c) 0.92 at%...............................................................................................95 圖 4-17 鑽石體積分率 60%、燒結 30 分鐘，鈦變量的試片之 XRD 分析.................................................................................................96 圖 4-18 鑽石體積分率 60% 的複合材料之熱傳導係數、熱膨脹係數及緻密度對鈦含量的變化趨勢圖.................................................96 圖 4-19 鑽石/銅-鈦複合材料破斷面微結構：(a) 鑽石體積分率 50%、(b) 鑽石體積分率 60%.............................................................97 圖 4-20圖 4-20 鑽石體積60%、雙粒徑鑽石添加試片之表面微結構.................................................................................................99 圖 4-21 鑽石體積分率 50%、鈦含量 0.6 at% 之複合材料界面微結構對燒結時間的變化圖：(a) 5 分鐘、(b) 15 分鐘、(c) 30分鐘，及 (d) 180 分鐘.......................................................................104 圖 4-22 鑽石體積分率 50%、鈦含量 0.6 at% 之複合材料熱傳導係數及緻密度對燒結時間的變化.....................................................104 圖 4-23 界面碳化鈦隨燒結時間變化之成長機制示意圖：(a) < 5 分鐘、(b) ~ 5 分鐘、(c) ~ 15分鐘，及 (d) ~ 30 分鐘..........................105 圖 4-24 鑽石體積分率 50% 及 60%、燒結 30 分鐘的複合材，其鈦變量對熱性質的變化：(a) 50%、(b) 60%...................................108 圖 4-25 不同鑽石體積分率下、不同鈦添加量的複材熱膨脹係數與理論值的比較...................................................................................117 圖 4-26 不同鈦添加量之鑽石/銀基複合材料表面微結構圖，由左至右分別為鈦添加量 1 at%、3 at%，及 5 at%...............................121 圖 4-27 鑽石體積分率 50%、鈦添加量 3 at%、燒結時間 30 分鐘之複合材料 XRD 分析..............................................................121 圖 4-28 鑽石體積分率 50%、燒結 30 分鐘之鑽石/銀基複合材料，其緻密度及熱傳導係數對鈦含量的變化...................................122 表目錄 表 2-1 相關冷卻技術的比較...................................................................6 表 2-2 傳統上應用於熱管理和電子構裝的材料...................................9 表 2-3 高熱傳導係數、低膨脹係數複合材料之性質...........................13 表 2-4 不同研究單位所開發之高導熱複材.........................................14 表 2-5 常見純金屬對鑽石的接觸角關係.............................................30 表 3-1 鑽石、銅及鈦的基本性質...........................................................59 表 4-1 銅、碳化鈦及鑽石的縱波、橫波聲速及熱傳導係數..................112 表 4-2 不同參數之鑽石/銅-鈦複合材料，利用 DMM model 計算出的界面間熱阻及界面有效熱傳導理論值.....................................113 表 4-3 不同參數之鑽石/銅-鈦複合材料熱傳導性質理論值與實際值之比較.............................................................................................113

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