臺灣博碩士論文加值系統

本研究係利用濕式陶瓷技術、真空脫脂、無壓燒結系統與直流濺鍍系統，製備碳化鉭石墨坩堝保護層。本研究為石墨坩堝碳化鉭保護層製程技術之開發，旨在增加物理氣相傳輸生長單晶碳化矽晶圓之石墨坩堝壽命，將分為漿料條配、塗佈方式與保護層燒結，探討不同燒結溫度與具備鍵結層對於保護層之影響。
漿料調配階段，探討定重量百分比時，不同自製溶劑型高分子黏劑，對於漿料黏度之影響；塗佈階段，探討不同塗佈方式對於保護層緻密度與機械性質之影響；保護層燒結階段，探討於1800oC、2000oC與2100oC對於保護層C/Ta之影響、微觀結構與機械性質之差異；薄膜製程階段，探討具備鍵結層對於保護層接合性之影響。
研究結果顯示，鉭粉於1800°C、2000oC與2100°C皆充分碳化為TaC相，其中2100°C提供更為足夠能量使保護層緻密化，其強度達到548.5Hv0.05。開發之塗佈方式，可製備超過100μm且與石墨坩堝無分離之保護層，且平均收縮率為2.08%。

In this study, Tantalum carbide graphite crucible protective layer was prepared by wet ceramic technology, vacuum debinding, pressureless sintering system and DC sputtering system. This study is the development of tantalum carbide protective layer for graphite crucible process integration technology. It is designed to reduce graphite crucible consumption. Which is divided into slurry blending, coating method and sintering to explore the physical properties of protective layer at all stages.
In this paper, the effect of different polymer binders adhesives on the viscosity of slurry is discussed. The coating method, the effects of different coating methods on density and mechanical properties for protective layer were discussed. For the protective layer sintering at 1800oC, 2000oC, 2100oC, For the phase, micro-morphology and mechanical properties analysis.
The results show that the tantalum powder is fully carbonized into TaC phase at 1800 °C, 2000oC and 2100 °C, furthermore 2100 °C provided more sintering energy to densify the protective layer, and its strength reaches 548.5Hv0.05. The coating method was developed to prepare a tantalum carbide protective layer thickness more than 100 μm and no separated with graphite crucible, and average shrinkage ratio was 2.08%.

摘要 i
ABSTRACT ii
誌謝 iv
目錄 v
表目錄 viii
圖目錄 ix
第一章 緒論 1
1.1前言 1
1.2研究動機與目的 2
第二章 文獻回顧 3
2.1碳化矽塊材製備方式 3
2.1.1化學氣相沉積法(Chemcial vapor depositon, CVD) 3
2.1.2物理氣相傳輸法(Physical vapour transport, PVT) 3
2.1.3物理氣相傳輸法生長碳化矽晶圓之缺陷 5
2.1.4傳統石墨坩堝之應用 7
2.2碳化鉭(Tantalum Carbide)性質 8
2.3碳化鉭應用於石墨坩堝保護層 10
2.4使用鉭粉末固體滲碳機制 13
2.5漿料調配 15
2.5.1粉體形狀與潤濕性對於漿料之影響 15
2.5.2黏結劑對於塗層之影響 16
2.6脫脂 17
2.7燒結理論 18
2.7.1原子移動 19
2.7.2燒結驅動力 22
2.7.3燒結機制 23
2.7.4固相燒結(Solid Phase Sintering) 25
2.8小結 26
第三章 實驗步驟與方法 27
3.1實驗流程 27
3.2石墨坩堝製備 28
3.3製程之漿料調配 28
3.3.1碳化鉭粉末 28
3.3.2自製溶劑型高分子黏結劑 29
3.3.3漿料調配之實驗流程 30
3.3.4碳化鉭漿料之流動性 31
3.4鍵結層製備 31
3.5保護層製備 33
3.6脫脂製程 35
3.7燒結製程 36
3.8實驗儀器及原理 38
3.8.1 X-Ray繞射儀(XRD) 38
3.8.2 場發射掃描式電子顯微鏡(FESEM) 38
3.8.3熱重分析 39
3.8.4聚焦離子束顯微系統(FIB) 39
3.8.5穿透式電子顯微鏡(TEM) 39
3.8.6維克氏硬度量測( Vicker Hardness ) 40
3.8.7孔隙率-影像分析法 40
第四章 結果與討論 41
4.1製程漿料分析 41
4.1.1粉末特性 41
4.1.2黏結劑之流變性 42
4.2熱脫脂與燒結 45
4.2.1熱脫脂分析 45
4.2.2真空熱脫脂 46
4.2.3燒結巨觀分析 47
4.3碳化鉭保護層性質分析 53
4.3.1碳化鉭保護層晶相分析 53
4.3.2碳化鉭保護層微觀結構分析 56
4.3.2.1製程對於保護層微觀結構之影響分析 56
4.3.2.2鍵結層對於保護層微觀結構之影響分析 58
4.3.2.3溫度對於保護層微觀結構之影響 60
4.3.2.4鍵結層相態變化分析 62
4.3.3維克氏硬度分析 66
4.3.4收縮率量測 67
4.3.5緻密度量測 68
第五章結論 70
參考文獻 71

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