Nanostructured Aniline Formaldehyde Resin/Polysilazane Hybrid Materials by Twin Polymerization

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 combinatio...

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Published in:Macromolecular chemistry and physics 2016-11, Vol.217 (22), p.2462-2472
Main Authors: Kaßner, Lysann, Knoblauch, Anja, Seifert, Andreas, Grützner, Rolf-Egbert, Cox, Gerhard, Lange, Arno, Csihony, Szilard, Simon, Frank, Anders, Susann, Kroll, Lothar, Rahaman, Mahfujur, Zahn, Dietrich, Mertens, Lutz, Weber, Marcus, Mehring, Michael, Spange, Stefan
Format: Article
Language:English
Subjects:
Aniline
Formaldehyde resins
Hexamethylenetetramine
Monomers
nanocomposites
Nanostructure
organic/inorganic hybrid materials
Polymerization
Polysilazane
silicon nitride
Solid state
twin polymerization
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Summary: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 13C‐ and 29Si‐NMR spectroscopy and transmission electron microscopy. The inorganic network remains hydrolyzable and can be functionalized after polymerization at temperatures below 500 °C due to residuary reactive Si−N bonds. Thermal treatment at 1100 °C leads to the formation of amorphous Si/C/N hybrid materials. The concept of twin polymerization is customized to oxygen free systems such as 2,2′‐spirobi[3,4‐dihydro‐1H‐1,3,2‐benzodiazasiline] and the combination tetrakis(phenylamino)silane/hexamethylenetetramine to produce silicon‐nitride related hybrid materials. Nanostructured aniline formaldehyde resin/polysilazane hybrid materials are produced within one procedure. After pyrolysis Si/C/N materials are received. For characterization of the products electron microscopy, DSC‐, TGA‐, XPS‐, and solid state NMR experiments are employed.
ISSN:1022-1352
1521-3935
DOI:10.1002/macp.201600152