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Defective structure of doped carbons obtained from preceramic polymers through Cl2- and NH3-assisted thermolysis
International Journal of Applied Ceramic Technology ( IF 1.8 ) Pub Date : 2022-09-27 , DOI: 10.1111/ijac.14220
Berta Pérez 1 , Fausto Rubio 1 , Juan Rubio 1 , Aitana Tamayo 1
Affiliation  

The processing parameters such as the heat treatment temperature, type of preceramic precursor, and post-synthesis treatments are key factors for the development the different microstructures in polymer-derived ceramics. Moreover, doping with different heteroatoms has increased the ability of the polymer-derived ceramics to produce tunable nanostructures with a controlled pore size and distributions. A preceramic precursor containing P has been prepared from a commercial polysiloxane polymer and a phosphate alkoxide. It has been subjected to thermal treatments in N2, NH3, and Cl2 atmospheres in different order sequences to create differentiated microstructures either in the ceramic matrix and the carbon phase. The structural, textural, and spectroscopic characterization revealed that the P atoms play a key role in the evolution of the microstructure during the thermal treatments. If the chlorination is carried out before the treatment in NH3, a silicophosphate matrix is formed and prevents from nitrogen incorporation into the free carbon phase. On contrary, if the NH3 treatment is carried out before the chlorination, the carbon phase is predominantly modified by the incorporation of P atoms within the free carbon network.

中文翻译:

通过 Cl2 和 NH3 辅助热解从预陶瓷聚合物中获得的掺杂碳的缺陷结构

热处理温度、陶瓷前体类型和合成后处理等工艺参数是聚合物衍生陶瓷形成不同微观结构的关键因素。此外,掺杂不同的杂原子提高了聚合物衍生陶瓷生产具有可控孔径和分布的可调纳米结构的能力。由商业聚硅氧烷聚合物和磷酸醇盐制备了含 P 的预制陶瓷前体。已在 N 2、NH 3和 Cl 2中进行热处理不同顺序的气氛在陶瓷基体和碳相中产生不同的微观结构。结构、织构和光谱表征表明,P 原子在热处理过程中的微观结构演变中起着关键作用。如果在NH 3中处理之前进行氯化,则形成硅磷酸盐基质并防止氮结合到游离碳相中。相反,如果在氯化之前进行NH 3处理,则碳相主要通过在游离碳网络中并入P原子而被改性。
更新日期:2022-09-27
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