Mrówka Jan, Partyka Janusz, Hasik Magdalena
Department of Silicate Chemistry and Macromolecular Compounds, Faculty of Materials Science and Ceramics, AGH University of Science and Technology, al. Mickiewicza 30, 30-059 Kraków, Poland.
Department of Ceramics and Refractory Materials, Faculty of Materials Science and Ceramics, AGH University of Science and Technology, al. Mickiewicza 30, 30-059 Kraków, Poland.
Materials (Basel). 2021 Sep 29;14(19):5661. doi: 10.3390/ma14195661.
Polysiloxane networks were prepared by hydrosilylation of poly(methylvinylsiloxane) (V polymer) with 1,3,5,7-tetramethylcyclotetrasiloxane (D) at various Si-Vinyl: Si-H groups molar ratios in water-in-oil high internal phase emulsion (HIPE). Curing the emulsions followed by removal of water led to foamed cross-linked polysiloxane systems differing in the cross-linking degrees, as well as residual Si-H and Si-Vinyl group concentrations. Treatment of thus obtained materials in Pd(OAc) solution in tetrahydrofuran resulted in the formation of porous palladium/polymer nanocomposites with different Pd contents (1.09-1.70 wt %). Conducted investigations showed that pyrolysis of the studied materials at 1000 °C in argon atmosphere leads to porous Si-C-O and Si-C-O/Pd ceramics containing amorphous carbon and graphitic phases. Thermogravimetric (TG) analysis of the starting cross-linked polymer materials and those containing Pd nanoparticles revealed that the presence of palladium deteriorates thermal stability and decreases ceramic yields of preceramic networks. The extent of this effect depends on polymer cross-linking density in the system.
通过在油包水型高内相乳液(HIPE)中,使聚(甲基乙烯基硅氧烷)(V聚合物)与1,3,5,7-四甲基环四硅氧烷(D)在不同的硅乙烯基:硅氢基团摩尔比下进行硅氢加成反应,制备了聚硅氧烷网络。将乳液固化,随后除去水,得到了交联度不同、残余硅氢和硅乙烯基浓度也不同的泡沫交联聚硅氧烷体系。将由此得到的材料在四氢呋喃中的醋酸钯溶液中进行处理,形成了具有不同钯含量(1.09 - 1.70 wt%)的多孔钯/聚合物纳米复合材料。进行的研究表明,在氩气气氛中于1000℃对所研究的材料进行热解,会得到含有无定形碳和石墨相的多孔Si-C-O和Si-C-O/Pd陶瓷。对起始交联聚合物材料以及含有钯纳米颗粒的材料进行热重(TG)分析表明,钯的存在会降低热稳定性,并降低陶瓷前驱体网络的陶瓷产率。这种影响的程度取决于体系中聚合物的交联密度。