Octaphenylsilesquioxane (OPS) with high yield was synthesized via limited-hydrolytic-polycon-densation-rearrangement of phenyltrimethoxysilane (PTMS) using tetramethylammonium as the catalyst in short reaction time. The morphology, structure and thermal properties of the products were characterized by TEM, FT-IR, 29Si NMR, 1H NMR, 13C NMR, elemental analysis and TGA. The results showed that octaphenyl-silesquioxane was regular rectangular nanoparticle with size less than 400 nm and high thermal stability, whose thermal decomposition temperature (weight loss at 5%) was more than 450 ℃ in both N2 and air. The intermediate product was also determined by FT-IR in order to infer the synthesis mechanism.%苯基三甲氧基硅烷在四甲基氢氧化铵催化下经有限水解-缩聚-重排制备笼形八苯基硅倍半氧烷,反应时间短,产率高.采用透射电镜(TEM)、傅立叶红外光谱(FT-IR)、29Si核磁共振光谱(29Si NMR)、1H核磁共振光谱(1H NMR)、13C核磁共振光谱(13C NMR)、元素分析和热分析(TGA)等对笼形八苯基硅倍半氧烷的形貌、结构和热性能进行研究.结果表明：笼形八苯基硅倍半氧烷是不规则长方体纳米颗粒,粒径小于400 nm,热稳定性高,在N2和空气中的初始分解温度(失重5%)均大于450℃.同时,对中间产物进行红外表征以推测反应机理.
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