Two polyborosiloxanes （PBSis） with char yield up to 74.13% at 800 ℃ were synthesized by the direct polycondensation of boric acid with phenyltrimethoxysilane in diglyme. The PBSis were characterized by gel permeati...Two polyborosiloxanes （PBSis） with char yield up to 74.13% at 800 ℃ were synthesized by the direct polycondensation of boric acid with phenyltrimethoxysilane in diglyme. The PBSis were characterized by gel permeation chromatography, IR spectroscopy as well as ^1H-, ^29Si- and ^11B-NMR. PBSi modified phenol-formaldehyde resins （PBSi/PFs） were prepared at different PBSi/PF mass ratios and were cured at 150 ℃. The PBSi/PFs were characterized by IR spectroscopy, scanning electron microscopy, thermogravimetric analysis and tensile test. The results revealed that the cured PBSi/PFs had sea-island morphology and higher char yield than the common PF. PBSi/PF blend with PBSi/PF mass ratio of 0.4：1 had char yield up to 70.83% at 800 ℃. The PBSi/PFs had tensile strength similar to PF. The ceramization of PBSi/PFs was also studied. The silicon boron oxycarbide （SiBOC） ceramics formed were characterized by IR spectroscopy and elemental analysis. This method provided a valuable way to prepare easily shapeable polymer blends as ceramic precursors.展开更多
A hydrophobic coating of the silica fiber reinforced silica composites(SiO2f/SiO2) was synthesized by sol-gel method using methyltriethoxy-silane(MTES) and boric acid(B(OH)3) as raw materials. The relationship among b...A hydrophobic coating of the silica fiber reinforced silica composites(SiO2f/SiO2) was synthesized by sol-gel method using methyltriethoxy-silane(MTES) and boric acid(B(OH)3) as raw materials. The relationship among boron doping, chemical structure of precursors and durability of hydrophobic coatings was discussed. The Si-O-B and methyl groups were successfully introduced in the gel precursors according to the FT-IR and XPS results. The resins were filled in the internal and surface holes of the SiO2f/SiO2 composites partially or completely, which is beneficial to reduce the physical adsorption of the moisture. In addition, hydroxyl groups of the SiO2f/SiO2 composites reacted with the resins and hydrophobic methyl groups were introduced, leading to the reduction of the chemical adsorption of water. Also, the boron doping was beneficial to enhancing the physical cross-linking between the coating and the SiO2f/SiO2 composites, and improved the adhesion of the coating to the substrate. The results show that the optimal hydrophobic coating with contact angle 130.33°, moisture absorption 0.33% and adhesion level 1 is obtained when the molar ratio of MTES to B(OH)3 is 10:4. The real permittivity of M10B4 is constant in the range of 2.32–2.51 and the dielectric tangent loss is constant in the range of 5.5 × 10-4–8.7 × 10-3. The hydrophobic coating has excellent dielectric properties.展开更多
文摘Two polyborosiloxanes （PBSis） with char yield up to 74.13% at 800 ℃ were synthesized by the direct polycondensation of boric acid with phenyltrimethoxysilane in diglyme. The PBSis were characterized by gel permeation chromatography, IR spectroscopy as well as ^1H-, ^29Si- and ^11B-NMR. PBSi modified phenol-formaldehyde resins （PBSi/PFs） were prepared at different PBSi/PF mass ratios and were cured at 150 ℃. The PBSi/PFs were characterized by IR spectroscopy, scanning electron microscopy, thermogravimetric analysis and tensile test. The results revealed that the cured PBSi/PFs had sea-island morphology and higher char yield than the common PF. PBSi/PF blend with PBSi/PF mass ratio of 0.4：1 had char yield up to 70.83% at 800 ℃. The PBSi/PFs had tensile strength similar to PF. The ceramization of PBSi/PFs was also studied. The silicon boron oxycarbide （SiBOC） ceramics formed were characterized by IR spectroscopy and elemental analysis. This method provided a valuable way to prepare easily shapeable polymer blends as ceramic precursors.
基金supported by the Taishan Scholar Project(No.ts201511080)the National Natural Science Foundation of China(Nos.51672059,51172050,51102060 and 51302050)the Natural Scientific Research Innovation Foundation in Harbin Institute of Technology(No.HIT.NSRIF.2014129)
文摘A hydrophobic coating of the silica fiber reinforced silica composites(SiO2f/SiO2) was synthesized by sol-gel method using methyltriethoxy-silane(MTES) and boric acid(B(OH)3) as raw materials. The relationship among boron doping, chemical structure of precursors and durability of hydrophobic coatings was discussed. The Si-O-B and methyl groups were successfully introduced in the gel precursors according to the FT-IR and XPS results. The resins were filled in the internal and surface holes of the SiO2f/SiO2 composites partially or completely, which is beneficial to reduce the physical adsorption of the moisture. In addition, hydroxyl groups of the SiO2f/SiO2 composites reacted with the resins and hydrophobic methyl groups were introduced, leading to the reduction of the chemical adsorption of water. Also, the boron doping was beneficial to enhancing the physical cross-linking between the coating and the SiO2f/SiO2 composites, and improved the adhesion of the coating to the substrate. The results show that the optimal hydrophobic coating with contact angle 130.33°, moisture absorption 0.33% and adhesion level 1 is obtained when the molar ratio of MTES to B(OH)3 is 10:4. The real permittivity of M10B4 is constant in the range of 2.32–2.51 and the dielectric tangent loss is constant in the range of 5.5 × 10-4–8.7 × 10-3. The hydrophobic coating has excellent dielectric properties.
