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研究生： 吳信哲
Tanapon - Sukachonmakul
論文名稱： 聚矽氮烷與其聚合物轉變－矽基陶瓷對氮化鋁表面處理於矽橡膠複合材料之應用
Surface Modification of Aluminum Nitride by Polysilazane and Its Polymer-derived Silicon-based Ceramics for Silicone Rubber Composites
指導教授： 邱顯堂
Hsien-Tang Chiu
口試委員: 邱文英
Wen-Yen Chiu
楊銘乾
Ming-Chien Yang
翁祖炘
Teuu-Hsing Ueng
陳志堅
Jyh-Chien Chen
施劭儒
Shao-Ju Shih
學位類別： 博士
Doctor
系所名稱： 工程學院 - 材料科學與工程系
Department of Materials Science and Engineering
論文出版年： 2014
畢業學年度： 102
語文別： 英文
論文頁數： 132
中文關鍵詞： 氮化鋁 、矽基陶瓷 、熱傳導係數 、聚矽氮烷 、矽橡膠
外文關鍵詞： Aluminum nitride, silicon-based ceramics, thermal conductivity, polysilazane, silicone rubber
相關次數： 點閱：430  下載：12 
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  •  上一筆

    • 本研究主要以聚矽氮烷(polysilazane，PSZ) 包覆於氮化鋁(AlN)粉末表面，分別利用空氣(air)、氬氣(Ar)、氮氣(N2)和氨氣(NH3)不同氣體環境在700和1600 oC溫度下進行熱處理，在不同熱處理條件下包覆AlN的PSZ將轉變成矽基陶瓷(Si-based ceramics)結構包覆著AlN，並應用於矽橡膠複合材料的導熱填充材。本研究將分成三個部分進行探討，藉由PSZ和Si-based ceramic結構的表面改質改善矽橡膠複合材料導熱的可行性。

    本研究第一部分聚焦於利用濕氣交聯法，將PSZ和其聚合物轉變陶瓷─矽氧碳陶瓷(polymer-derived amorphous silicon oxycarbide (SiOC) ceramic) 包覆於AlN粉末表面，並在air中700 oC熱處理溫度下促使PSZ轉變陶瓷─SiOC包覆在AlN表面。經由傅氏紅外線轉換光譜儀（FTIR）、化學分析電子能譜儀（XPS）和電子顯微鏡（SEM），結果顯示AlN粉體表面成功的被包覆於PSZ和SiOC薄膜。並發現到PSZ和SiOC薄膜改善界面附著性，由於在填充物的基體界面的熱邊界層阻力降低，導致改質後的AlN粉體(PSZ/AlN 和 SiOC/AlN)和矽橡膠複合材料的導熱性增加。然而，引進的SiOC作為AlN和矽橡膠之間的中間層可以幫助增加熱能輸送在填料與基體的界面而不是使用PSZ。這個結果是由於PSZ在air中經由700oC熱處理後造成表面粗糙度和膜的厚度減少。

    本研究第二部分聚焦於使用陶瓷前驅體-PSZ利用包覆法包覆AlN粉體，用於製備SiOC和矽氧氮碳(SiONC)陶瓷薄膜，並依據熱處理溫度700oC在不同氣體環境(air、Ar、N2和NH3)下，分別使PSZ轉變成SiOCair和SiONC (Ar, N2 and NH3)。經由FTIR, X射線繞射分析儀(XRD) 和XPS測試結果發現有非晶SiOCair和SiONC (Ar, N2 and NH3)薄膜在AlN表面。引進氣體環境後的SiOCair和SiONC (Ar, N2 and NH3)薄膜在AlN表面，矽橡膠和AlN之間界面接著性有顯著底改善。透過AFM可發現PSZ熱處理在不同氣體環境之下影響薄膜在AlN表面型態，即SiOCair和SiONC NH3薄膜比起SiONC (Ar, N2 )薄膜平滑。除此之外，SiOCair和SiONC (Ar, N2 and NH3)包覆AlN薄膜表面粗糙度的下降促使矽橡膠複合材料熱傳導提升。

    本研究第三部分聚焦於使用陶瓷前驅體-PSZ利用包覆法包覆AlN粉體，接著熱處理溫度1600oC在不同氣體環境(air、Ar、N2和NH3)下製備Si-based ceramics/AlN (Si/AlN)複合粉末。根據XRD、XPS 和SEM/EDS之分析，顯示確實存在著Si-based ceramics在AlN粒子上，其中包括了在air熱處理之下Si/AlNair表面的二氧化矽（SiO2）、Ar中Si/AlNAr表面的碳化矽晶鬚（SiC whisker）、N2 中Si/AlNN2表面的SiC whisker/氮化矽(Si3N4)晶粒以及NH3中Si/AlNNH3表面的Si3N4。此外，使用Ar和NH3熱處理後的Si/AlN複合粉末添加於矽橡膠可提升此複合材料的熱傳導性能，這可能是因為添加了高導熱奈米級SiC whiskers和Si3N4陶瓷膜在於Si/AlNAr與Si/AlNNH3的表面。

    由上述實驗結果得知，使用SiOCair and SiONC(Ar, N2 and NH3)結構並參與導熱粉末的表面改質，可以經由其形成的陶瓷膜層附著於AlN表層，將其導入矽像膠達到提升更高的熱傳導效果。此外，Si/AlN經由在Ar與NH3下1600 oC裂解，可以應用為導熱粉末。

    In this work, we aimed to use polysilazane (PSZ) to coat on aluminum nitride (AlN) by using a dip coating method, followed by pyrolysis at 700 and 1600 oC under air, Ar, N2 and NH3 atmospheres. The pyrolysis under different conditions allowed PSZ coated AlN to convert into different components of Si-based ceramics coated AlN, and then were used as thermally conductive fillers in silicone rubber composites. This work addressed three parts respectively to discuss the feasibility of an alternative surface modification by using PSZ and Si-based ceramics to improve the thermal conductivity of silicone rubber composites.

    Part (i) PSZ and its polymer-derived amorphous silicon oxycarbide (SiOC) ceramic were coated on AlN by using a dip-coating method to allow moisture-crosslinking of PSZ on AlN, followed by heat treatment at 700oC in air to convert PSZ into SiOC on AlN. The results from FTIR, XPS and SEM indicated that the surface of AlN was successfully coated by PSZ and SiOC film. It was found that the introduction of PSZ and SiOC film help improve in the interfacial adhesion between the modified AlN (PSZ/AlN and SiOC/AlN) and silicone rubber lead to the increase in the thermal conductivity of the composites since the thermal boundary resistance at the filler-matrix interface was decreased. However, the introduction of SiOC as an intermediate layer between AlN and silicone rubber could help increase the thermal energy transport at the filler-matrix interface rather than using PSZ. This result was due to the decrease in the surface roughness and thickness of SiOC film after heat treatment at 700 oC in air.

    Part (ii) SiOC and silicon oxynitrocarbide (SiONC) ceramic films coated ALN were prepared by using preceramic-PSZ with dip-coating method, followed by pyrolysis at 700 oC in different (air, Ar, N2 and NH3) atmospheres to convert PSZ into SiOCair and SiONC(Ar, N2 and NH3) ceramics. The existence of amorphous SiOCair and SiONC(Ar, N2 and NH3) ceramic films on AlN surface was characterized by FTIR, XRD and XPS. The interfacial adhesion between silicone rubber and AlN was significantly improved after the introduction of amorphous SiOCair and SiONC(Ar, N2 and NH3) ceramic films on AlN surface. It can be observed from AFM that the pyrolysis of PSZ at different atmosphere strongly affected to films morphology on AlN surface as SiOCair and SiONCNH3 ceramic films were more flat and smooth than SiONCN2 and SiONCAr ceramic films. Besides, the enhancement of the thermal conductivity of silicone rubber composites was found to be related to the decrease in the surface roughness of SiOCair and SiONC(Ar, N2 and NH3) ceramic films on AlN surface.

    Part (iii) Silicon-based ceramics and aluminum nitride (Si/AlN) were fabricated by pyrolysis of preceramic-PSZ coated AlN at 1600 oC in air, Ar, N2 and NH3 atmospheres. The results from XRD, XPS and SEM/EDS revealed the existence of crystalline phase of Si-based ceramics on AlN particles including SiO2 in Si/AlNair, SiC whisker in Si/AlNAr, SiC whisker/Si3N4 grain in Si/AlNN2, and Si3N4 ceramics in Si/AlNNH3. It was found that the thermal conductivity of silicone rubber filled with Si/AlN hybrid fillers which were fabricated in Ar and NH3, was improved. This might be due to the existence of nanoscale SiC whiskers and a thermal conductive layer of Si3N4 on Si/AlNAr and Si/AlNNH3 surface, respectively.

    This present work provided an alternative surface modification of thermally conductive fillers by coating with amorphous SiOCair and SiONC(Ar, N2 and NH3) ceramic films to improve the interfacial adhesion between filler-matrix interface, then enhanced the thermal conductivity of silicon rubber composites. Moreover, Si/AlN hybrid fillers pyrolyzed at 1600 oC in Ar and NH3 could be applicable to use as thermally conductive fillers.

    中文摘要 I ABSTRACT III 誌謝 V LIST OF FIGURES IX LIST OF TABLES XII CHAPTER 1 INTRODUCTION 1 1.1 Motivation 2 1.2 Research Objectives 4 1.3 References 4 CHAPTER 2 RESEARCH BACKGROUND 6 2.1 Heat Transfer 7 2.1.1 Definition 7 2.1.2 Mechanism 7 2.1.3 Thermal conductivity measurement 11 2.1.3.1 Steady-state methods 11 2.1.3.2 Transient methods 12 2.2 Thermally Conductive Polymer Materials 18 2.2.1 Fillers for thermally conductive composites 20 2.2.1.1 Ceramic fillers 22 2.2.1.2 Metallic fillers 25 2.2.1.3 Carbon-based fillers 26 2.2.2 Application of thermally conductive polymer composites. 26 2.2.3 Improvement of the thermal conductivity in thermally conductive polymer composites. 31 2.3 Preceramic Polymer 35 2.3.1 The classification of preceramic polymer 36 2.3.2 Advantages of preceramic polymer 39 2.4 Polysilazane 41 2.4.1 Synthesis and structure of polysilazane 41 2.4.2 Crosslinking of Polysilazane 44 2.4.3 Properties and application 46 2.4.4 Processing from PSZ to ceramic materials 47 2.5 References 50 CHAPTER 3 SURFACE MODIFICATION OF ALUMINUM NITRIDE BY POLYSILAZANE AND ITS POLYMER-DERIVED AMORPHOUS SILICON OXYCARBIDE CERAMIC FOR THE ENHANCEMENT OF THERMAL CONDUCTIVITY IN SILICONE RUBBER COMPOSITE 60 Abstract 61 3.1 Introduction 62 3.2 Experimental Methods and Materials 64 3.2.1 Materials 64 3.2.2 Surface modification of AlN 64 3.2.3 Preparation of silicone rubber filled PSZ/AlN and SiOC/AlN 64 3.2.4 Characterization 66 3.3 Results and Discussion 67 3.3.1 Surface Characterization of Polysilazane and Its Polymer-derived Amorphous Silicon Oxycarbide Ceramic Coated Aluminum Nitride 67 3.3.2 Effect of polysilazane and its polymer-derived amorphous silicon oxycarbide ceramic film coated aluminum nitride on thermal conductivity of silicone rubber composites 76 3.3.3 Characterization of thermal stability and mechanical properties of silicone rubber filled with PSZ/AlN and SiOC/AlN 80 3.4 Conclusions 82 3.5 References 83 CHAPTER 4 EFFECT OF PYROLYSIS ATMOSPHERES ON THE MORPHOLOGY OF POLYMER-DERIVED SILICON OXYNITROCARBIDE CERAMIC FILMS COATED ALUMINUM NITRIDE SURFACE AND THE THERMAL CONDUCTIVITY OF SILICONE RUBER COMPOSITES 88 Abstract 89 4.1 Introduction 90 4.2 Experimental Methods and Materials 92 4.2.1 Materials 92 4.2.2 Surface modification of AlN 92 4.2.3 Preparation of silicone rubber filled PSZ/AlN and SiOC/AlN 92 4.2.4 Characterization 93 4.3 Results and Discussion 95 4.3.1 Characterization of SiOC/AlNair and SiONC/AlN(Ar, N2 and NH3) 95 4.3.2 Thermal conductivity of silicone rubber filled with SiOC/AlNair and SiONC/AlN(Ar, N2 and NH3). 101 4.4 Conclusions 108 4.5 References 109 CHAPTER 5 FABRICATION AND CHARACTERIZATION OF SILICON-BASED CERAMIC/ALUMINUM NITRIDE AS THERMALLY CONDUCTIVE HYBRID FILLER IN SILICONE RUBBER COMPOSITE 113 Abstract 114 5.1 Introduction 115 5.2 Experimental Methods and Materials 117 5.3 Results and Discussion 118 5.3.1 Characterization of Si/AlN hybrid fillers 118 5.3.2 Thermal conductivity of silicone rubber filled with Si/AlN hybrid fillers 124 5.4 Conclusions 126 5.5 References 127 CHAPTER 6 CONCLUSIONS 130 CONCLUSIONS 131

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