摘要
由NH_4Cl与BCl_3反应合成TCB,然后与(Me_3Si)_2NH和BCl_3在低温下反应获得具有硼氨六元环结构的BN陶瓷先驱体聚硼氮烷,并用IR、MS、UTA、TG等对聚硼氨烷的结构及热稳定性进行了分析表征。结果表明,降低反应温度可提高聚硼氮烷的合成产率,决定产物溶解性能的主要因素是反应物料的配料比,反应所用溶剂对聚硼氮烷的陶瓷产率影响最大。在100℃下陶瓷产率可达35~45%。
The need-like 1,3,5-trichloroborazine(TCB)has been-prepared through the reaction of ammonia chloride with boron trichloride.Then,BN preceramic polymer-polyborazine has been synthesized from reactions of TCB,hexamethyldisilazane and boron trichloride.This study shows that the lower reaction temperature,the higher synthesis yield was obtained.The polyborazine's solubility mainly depend on the ratio of TCB,(Me3Si)2NH and BCl3.The solvent used in reaction has a great effect to the ceramic yield of polyborazine,A soluble polyborazine with good synthesis and ceramic yield can be obtained when reaction temperature is:-15℃,using cyclohexane as solvent and the ratio of TCB:(Me3Si)2NH:BCl3 is 1:6:1.By means of IR and Ms,the structure of the polyborazine was identified and showed as follow:The thermal decomposition of the polyborazine precusor th h-BN has also been examined.The majority of the gas evolution is found to occur below 350℃.However crystalline h-BN is not produced until 1000℃,and the ceramic yield is 35%~45%.
出处
《高分子材料科学与工程》
EI
CAS
CSCD
北大核心
1994年第5期18-23,共6页
Polymer Materials Science & Engineering
关键词
聚硼氮烷
合成
热解
氮化硼陶瓷
s:boron nitride,precursor,polyborazine,synthesis.