本論文探討以燃燒合成法製備六方晶氮化硼，主要研究重點為氮化硼製程技術開發與純化技術之建立。製程開發分為保溫製程及無保溫製程，兩製程之主要反應物皆為氧化硼、鎂粉、氯化銨及不同壓力之氮氣氣氛;皆以自製鋁箔容器盛裝反應物，反應體為疏鬆且具高孔隙度，隨起始氮壓提高能使氮氣有效滲入反應體內部，增進內部反應物氮化反應進行。反應物氧化硼及鎂粉於引燃後進行氧化還原反應，鎂粉將氧化硼還原成硼，硼再進一步與氮氣反應成氮化硼。添加氯化銨於反應物與無添加氯化銨相比轉化率明顯提高，推測可能原因為其受熱分解產生氯化氫，而氯化氫和硼反應生成氯化硼氣體，並與氮氣反應生成氮化硼，此路徑與硼直接與氮氣反應相比，為較低活化能的反應路徑，添加氯化銨因而具有催化劑的功能。在無保溫製程中，起始氮壓1.0MPa下反應體燃燒溫度超過硼的熔點，造成硼的融聚而使轉化率下降。在添加氮化硼於反應體中心方面，雖嘗試各種不同添加量，但對轉化率而言無明顯提升。無保溫製程於起始氮氣壓力0.8MPa下，得到最高轉化率87%。在保溫製程中，將反應物放置於氧化鋁隔熱材中，所得之產物轉化率有所提升且產物外觀灰黑色產物明顯減少，由溫度測量亦發現反應體燃燒溫度維持在高溫較長時間，推測氧化鋁隔熱材能降低反應體熱量損失，並減少氯化銨裂解出的氯化氫氣體逸散至腔體，有助於氮化反應進行。保溫製程於起始氮氣壓力1.0MPa下，得到最高轉化率90%。本製程產物除氮化硼外亦含有副產物及未反應物(氧化鎂、氧化硼鎂、硼等)，這些副產物及未反應物可藉由酸洗去除，本研究亦探討不同酸洗時間、混和酸使用量及球磨後酸洗等條件對產物純化之影響與效果。

Hexagonal boron nitride powder was synthesized by the combustion synthesis (SHS) method. The SHS processes reported in the present study were divided into two types. In the first type, the reactant powders were placed in the perforated aluminum containers but without placing the aluminum oxide insulation materials around the containers (no heat preservation process). In the second type, the reactant powders were placed in the perforated aluminum containers and also placed the aluminum oxide insulation materials around the containers (heat preservation process). In these two process, the synthesis of h-BN powders used Mg, B2O3, NH4Cl, and nitrogen gas as reactant. The reactant powders were mixed and placed in the perforated aluminum container. Owing to a loose and highly porous structure of the powder stack, the surrounding N2 can penetrate into the inside parts of it easily, and make the nitridation reaction better. B2O3 was reduced to boron by Mg, and then boron reacted with nitrogen gas and formed BN. Addition of NH4Cl was found that can enhance the conversion of BN, and we considered that it created an easier route for the nitridation of boron by first converting boron to BClx, which then reacted with N2 under the reduction of H2. In the no heat preservation process, the coalescence of molten boron appeared because the temperature was higher than the melting point of boron under N2 pressure of 1.0 MPa. Addition of BN as inert particles, though I tried to add different amounts of BN, there were no apparent enhancement of conversion. In the no heat preservation process, a maximum conversion of 87% was achieved under N2 pressure of 0.8 MPa. In the heat preservation process, placing Al2O3 insulation materials around the reactant was found that can enhance the conversion of BN, and the black color product became less in the exterior parts. I considered that it can reduce the amounts of HCl escaping from the reactant, and reduced the heat loss of reactant. This process made the temperature maintain at higher temperature longer time, and improved the nitridation reaction. In the heat preservation process, a maximum conversion of 90% was achieved under N2 pressure of 1.0 MPa. Combustion synthesis of h-BN not only had the product of h-BN but also had other by-products (e.g., MgO, Mg3B2O6 and B). By-products can be removed by acid treatment.

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