Nanostructured Aniline Formaldehyde Resin/Polysilazane Hybrid Materials by Twin Polymerization

Abstract

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.

Expanding the portfolio of tribo-positive materials: Aniline formaldehyde condensates for high charge density triboelectric nanogenerators

“…This peak has also been attributed to an overlap of the amine, amide and imide contributions for nitrogen-containing polymers [35,36]. The O 1s spectra show the presence of components at 531.5 eV and 532.9 eV, corresponding to C-O and C=O groups, respectively [35,36]. It should be noted that oxygen is not usually expected in the chemical structure of AFR, but owing to the low-vacuum curing process, surface oxygen is observed which is absent in the bulk of the material (as confirmed from in-situ XPS Ar + sputtering (see Fig.…”

“…All the high-resolution corelevel spectra were fitted using Gaussian components to identify the diverse chemical bonding states present in the AFR samples. The high binding energy asymmetrical C 1s spectrum was deconvoluted into four components centred at 284.8 eV, 285.8 eV, 287.0 eV and 288.7 eV, corresponding to sp 2 bonds, C-N bonds in amino groups and/or amine-sided carbon atoms, C-O groups and C=O groups, respectively apart from the satellite peak at ~291 eV [35]. The N 1s spectra show only a single peak at ~ 399.7 eV, corresponding to the nitrogen bonded to carbon in amino and/or amino and/or amide groups [35,36].…”

“…The high binding energy asymmetrical C 1s spectrum was deconvoluted into four components centred at 284.8 eV, 285.8 eV, 287.0 eV and 288.7 eV, corresponding to sp 2 bonds, C-N bonds in amino groups and/or amine-sided carbon atoms, C-O groups and C=O groups, respectively apart from the satellite peak at ~291 eV [35]. The N 1s spectra show only a single peak at ~ 399.7 eV, corresponding to the nitrogen bonded to carbon in amino and/or amino and/or amide groups [35,36]. This peak has also been attributed to an overlap of the amine, amide and imide contributions for nitrogen-containing polymers [35,36].…”

“…The N 1s spectra show only a single peak at ~ 399.7 eV, corresponding to the nitrogen bonded to carbon in amino and/or amino and/or amide groups [35,36]. This peak has also been attributed to an overlap of the amine, amide and imide contributions for nitrogen-containing polymers [35,36]. The O 1s spectra show the presence of components at 531.5 eV and 532.9 eV, corresponding to C-O and C=O groups, respectively [35,36].…”

Porous carbon–carbon composite electrodes for vanadium redox flow batteries synthesized by twin polymerization

“…Spange et al developed a sophisticated synthesis route called twin polymerization, to produce simultaneously two interpenetrating polymers forming an organic-inorganic hybrid material with only one monomer and one catalyst required. [34][35][36][37][38][39] Moreover, the twin polymerization approach offers several major advantages. As a well-established example the twin monomer 2,2 0 -spirobi[benzo-4H-1,3,2-dioxasiline] forms phenolic resin and silica without producing any side products, which reduces the shrinking commonly experienced during the stabilization step.…”