本論文研究主題為石英長晶坩堝耐高溫防沾黏抗侵蝕矽酸鋇及氮化硼塗層製程開發。氮化硼具有耐高溫、防沾黏、抗侵蝕、潤滑等特性，故氮化硼為優先考量之保護層材料；另一方面，有專利提及矽酸鋇塗層對於石英轉換成方石英具有抑制之效果，並提及可應用於矽長晶坩堝塗層，故矽酸鋇塗層也為一值得考慮的材料。因兩種材料之探討，本研究共分為兩部分:第一部分即利用熱擴散製程生長氮化硼塗層於石英基材上，反應物採用尿素、硼酸當作原料，其最佳操作條件為尿素比硼酸為3比1，於氮氣氣氛下操作溫度900°C持溫16小時並升溫至1250°C持溫1小時，生成之鍍層氧含量約9%，推測氧存在原因為硼酸與尿素反應形成BN後所帶有的OH基，或者仍有微量氧化硼生成，但塗層仍非連續貌，且附著度僅為ASTM D3359附著度測試中之2B等級。另外將此組配方升溫至1400°C持溫1小時於氮氣氣氛下進行測試，其表面形貌則出現許多裂縫及高低差情形，即方石英所產生之巨大體積效應，故可確認氮化硼塗層並無法抑制方石英產生巨大體積效應；因在氮化硼塗層方面，已確認氮化硼不具有抑制方石英產生巨大體積效應之效果，故塗層設計改變為先生成矽酸鋇再生成氮化硼之構想，此即為本研究之第二部分，即利用浸塗製程生長矽酸鋇塗層於石英基材上做為第一層塗層，使其能抑制方石英產生巨大體積效應，而第二層塗層即為氮化硼塗層，使氮化硼生長於矽酸鋇塗層上，其矽酸鋇塗層採用氫氧化鋇、去離子水配置溶液並利用浸塗製程生長矽酸鋇塗層於石英基材上。吾人先進行空白實驗，即將未有塗層之石英基材升溫至1400°C持溫1小時，由GIR檢驗確認有方石英生成，使用SEM/TOPO檢驗則發現具有裂縫及高低差之形貌，可斷定為石英轉變方石英所造成之巨大體積效應所導致，且附著度僅為ASTM D3359附著度測試中之1B等級。而將浸塗5次所生長之矽酸鋇塗層升溫至1400°C且持溫1小時熱處理後，經由GIR檢驗確認仍有方石英生成，但SEM/TOPO檢驗可發現僅形成裂縫，並無高低差之形貌，可確認矽酸鋇塗層能抑制方石英生成時所產生之巨大體積效應，且附著度達ASTM D3359附著度測試中之5B等級，故能防止方石英結晶層剝落之情況，因此經由浸塗5次所生長之矽酸鋇即可列為後續進行生長第二層塗層之配方。

The research topic of thesis is Process Development for High Temperature Non-wetting Anticorrosion Barium Silicate and Boron Nitride Coating on Quartz Crucibles for Silicon Crystal Growth. The boron nitride coating is a top priority material for protection layer because boron nitride has a great properties of high temperature resistance, anti-corrosion, non-wetting, lubrication and so on. On the other hand, it was found that barium silicate coating can inhibit the situation which is formation of cristobalite and be applied for coating on quartz crucibles of silicon crystal growth in the patents. So the barium silicate coating can be considered. The research is divided into two part because the research investigates for two types of materials. The first part is that grows h-BN layer on the quartz via thermal diffusion method and urea, boric acid are used as the reactant. The optimum operating condition is that the ratio of urea and boric oxide is three to one and the operating temperature is heated up to 900°C for 16 hours and than heated up to 1250°C for 1 hour by nitrogen gas flow. The oxygen of coating amount decreased to 9%. It’s speculated that the existence of oxygen is the OH group by the reaction of boric acid with urea to boron nitride , or boron oxide is a little formed in the process. However, the coating isn’t uniform and the adhesion test of ASTM D3359 is only 2B. In addition, the sample of optimum operating condition was heated up to 1400°C for 1 hour by nitrogen gas flow to test. There were many cracks and high and low level morphology of the surface that is the phenomenon which is huge volume effect of cristobalite formation. Therefore, it can be determined that the boron nitride can’t inhibit the phenomenon which cristobalite generated huge volume effect; It’s confirmed that boron nitride can’t inhibit the huge volume effect so the coating design must be modified. So the second part is that grows barium silicate layer on the quartz via dip coating method as the first layer and then boron nitride coating is as the second layer. The meaning is that boron nitride coating grows on the barium silicate layer. The reaction solution is prepared by using barium hydroxide and DI water and then grows barium silicate coating on the quartz via dip coating method with reaction solution. First up, the quartz without any coating which is blank experiment was heated up to 1400°C for 1 hour, and it’s confirmed that the cristobalite formed via GIR analysis. Not only that there were many cracks and high and low level morphology of the surface via SEM/TOPO analysis that is the phenomenon which quartz transformed into cristobalite and the adhesion test of ASTM D3359 is only 1B. On the other hand, barium silicate were heated up to 1400°C for 1 hour by 5 circles, and it’s confirmed that the cristobalite formed via GIR analysis. The most different is that there still had cracks but hadn’t high and low level morphology via SEM/TOPO analysis. It’s confirmed that the barium silicate coating can inhibit the phenomenon which cristobalite generated huge volume effect and adhesion test of ASTM D3359 is 5B. So barium silicate coating can prevent the circumstances which the coating is peeling off. Therefore, the barium silicate coating by dipping 5 circles can be used for growing the second layer.

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