Nanostructured Aniline Formaldehyde Resin/Polysilazane Hybrid Materials by Twin Polymerization

Nanostructured Aniline Formaldehyde Resin/Polysilazane Hybrid Materials by Twin Polymerization
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DOI:
10.1002/macp.201600152
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发表时间:
2016-11-01
影响因子:
2.5
通讯作者:
Spange, Stefan
Spange, Stefan
中科院分区:
化学4区
文献类型:
--
作者:
Kassner, Lysann;Knoblauch, Anja;Spange, Stefan

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通过2,2 '-螺[3,4-二氢-1H-1,3,2-苯并二氮杂环己基](1)的双聚合制备纳米结构的苯胺甲醛树脂/聚硅氮烷杂化材料。类似杂化材料的另一种合成概念,表观孪晶聚合,通过使用缺陷孪晶单体四(苯基氨基)硅烷(2)与六亚甲基四胺(HMTA)的组合来使用。用于合成聚硅氮烷杂化材料的两种方法都在副产物如氨或芳族氮化合物的挥发下发生。采用差示扫描量热法和热重分析法分别研究了孪晶单体1和2/HMTA组合物的热性能。用固体核磁共振(NMR)和透射电子显微镜(TEM)对苯胺甲醛树脂/聚硅氮烷杂化材料进行了表征。无机网络保持可水解性,并且由于残留的反应性Si-N键,在聚合后在低于500 ° C的温度下可以官能化。在1100摄氏度下的热处理导致非晶Si/C/N杂化材料的形成。
Nanostructured aniline formaldehyde resin/polysilazane hybrid materials are produced by twin polymerization of 2,2'-spirobi[3,4-dihydro-1H-1,3,2-benzodiazasiline] (1). An alternative synthetic concept for similar hybrid materials, the apparent twin polymerization, is employed by using the combination of the deficient twin monomer tetrakis(phenylamino) silane (2) with hexamethylenetetramine (HMTA). Both processes for the synthesis of polysilazane hybrid materials occur under volatilization of byproducts such as ammonia or aromatic nitrogen compounds. The thermal properties of the twin monomer 1 and the combination of 2/HMTA, respectively, are investigated by differential scanning calorimetry and thermogravimetric analysis. Aniline-formaldehyde resin/polysilazane hybrid materials are characterized by solid state C-13- and Si-29-NMR spectroscopy and transmission electron microscopy. The inorganic network remains hydrolyzable and can be functionalized after polymerization at temperatures below 500 degrees C due to residuary reactive Si-N bonds. Thermal treatment at 1100 degrees C leads to the formation of amorphous Si/C/N hybrid materials.