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通过碳热还原法由聚甲基氢硅氧烷衍生的多孔碳化硅和碳化硅/碳陶瓷微球

Porous SiC and SiC/C Ceramic Microspheres Derived from Polyhydromethylsiloxane by Carbothermal Reduction.

作者信息

Mizerska Urszula, Fortuniak Witold, Chojnowski Julian, Rubinsztajn Slawomir, Zakrzewska Joanna, Bak-Sypien Irena, Nyczyk-Malinowska Anna

机构信息

Center of Molecular and Macromolecular Studies, Polish Academy of Sciences, ul. Sienkiewicza 112, 90-363 Lodz, Poland.

Faculty of Materials Science and Ceramics, AGH-University of Science and Technology, Al. Mickiewicza 30, 30-059 Krakow, Poland.

出版信息

Materials (Basel). 2021 Dec 23;15(1):81. doi: 10.3390/ma15010081.

DOI:10.3390/ma15010081
PMID:35009245
原文链接:https://pmc.ncbi.nlm.nih.gov/articles/PMC8745781/
Abstract

A simple and inexpensive method for the preparation of porous SiC microspheres is presented. Polysiloxane microspheres derived from polyhydromethylsiloxane (PHMS) cross-linked with divinylbenzene (DVB) were ceramized under conditions leading to the removal of oxygen from the material. The content of free carbon (C) in highly crystalline silicon carbide (SiC) particles can be controlled by using various proportions of DVB in the synthesis of the pre-ceramic material. The chemical structure of the ceramic microspheres was studied by elemental analysis for carbon and oxygen, Si MAS NMR, C MAS NMR, SEM/EDS, XRD and Raman spectroscopies, and their morphology by SEM, nitrogen adsorption and mercury intrusion porosimetries. The gaseous products of the thermal reduction processes formed during ceramization created a porous structure of the microspheres. In the SiC/C microspheres, meso/micro pores were formed, while in carbon-free SiC, microspheres macroporosity dominated.

摘要

本文提出了一种制备多孔碳化硅微球的简单且低成本的方法。由聚甲基氢硅氧烷（PHMS）与二乙烯基苯（DVB）交联得到的聚硅氧烷微球在能使材料中氧去除的条件下进行陶瓷化。在预陶瓷材料合成过程中，通过使用不同比例的DVB，可以控制高度结晶的碳化硅（SiC）颗粒中游离碳（C）的含量。通过对碳和氧的元素分析、硅的核磁共振（Si MAS NMR）、碳的核磁共振（C MAS NMR）、扫描电子显微镜/能谱分析（SEM/EDS）、X射线衍射（XRD）和拉曼光谱对陶瓷微球的化学结构进行了研究，并通过扫描电子显微镜、氮气吸附和压汞孔隙率测定法对其形态进行了研究。陶瓷化过程中形成的热还原过程的气态产物造就了微球的多孔结构。在SiC/C微球中形成了介孔/微孔，而在无碳SiC微球中，大孔占主导。

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