Abstract:Polyhedral oligomeric silsesquioxanes (POSS) including octaphenylsilsesquioxane (OPS), octa(aminophenyl)silsesquioxane (OAPS) and octa(propargylaminophenyl)silsesquioxane (OPAPS) were used to prepare composite resins with pre-polyarylacetylene (PAA). The compatibility and thermal properties of the PAA/POSS composites were studied through SEM, XRD, FT-IR, DSC and TGA. The morphologies of PAA/POSS composites and XRD results proved that there was good compatibility between PAA and OPAPS because the terminal alkynyl groups in OPAPS could react with PAA, while the compatibility between PAA and OPS was the worst due to the OPS could deposit in the bottom of the composites. The FT-IR analysis indicates the formation of a conjugated diene and aromatic ring groups in the thermal curing processes of the resins. DSC analysis implies that the addition of inorganic silica-like core to prePAA decreases the exothermic heat. And incorporation of OPAPS could enhance the curing temperature a little. TGA analysis indicates that addition of OAPS or OPAPS would not reduce the excellent thermal stability so much and somewhat enhance the thermal-oxidative stability.
范海波, 刘艳林, 杨荣杰, 李向梅. 芳炔树脂/POSS固化相容性及热稳定性研究[J]. 材料工程, 2014, 0(3): 1-6.
FAN Hai-bo, LIU Yan-lin, YANG Rong-jie, LI Xiang-mei. Compatibility and Thermostability Between Polyarylacetylene Composites and Polyhedral Oligomeric Silsesquioxanes. Journal of Materials Engineering, 2014, 0(3): 1-6.
[1] LICKISS P D, RATABOUL F. Fully condensed polyhedral oligosilsesquioxanes (POSS): from synthesis to application[J]. Adv Organomet Chem, 2008, 57: 1-116.
[2] CORDES D B, LICKISS P D, RATABOUL F. Recent developments in the chemistry of cubic polyhedral oligosilsesquioxanes[J]. Chem Rev, 2010, 110: 2081-2173.
[3] 杜建科, 杨荣杰. 笼形八苯基硅倍半氧烷的合成及表征[J]. 精细化工, 2005, 22(6): 409-411.DU J K, YANG R J. Synthesis and characterization of polyhedral octaphenylsilsesquioxane[J]. Fine Chemicals, 2005, 22(6): 409-411.
[4] KATZMAN H A, MALLON J J, BARRY W T. Polyarylacetylene-matrix composites for solid rocket motor components[J]. J Adv Mater, 1995, 26(3): 21-27.
[5] ZHANG X Z, HUANG Y D, WANG T Y, et al. Influence of fibre surface oxidation-reduction followed by silsesquioxane coating treatment on interfacial mechanical properties of carbon fibre/polyarylacetylene composites[J]. Compos Part A, 2007, 38(3): 936-944.
[6] 王明存, 魏柳荷, 赵彤, 等. 一种加成固化型热固性树脂PN-PAA固化过程和热稳定性研究[J]. 高分子学报, 2006, (2): 241-246.WANG M C, WEI L H, ZHAO T, et al. Cure and thermal stability of an addition cure type thermoset PN-PAA[J]. Acta Polymerica Sinica, 2006, (2): 241-246.
[7] ZALDIVAR R J, KOBAYASHI R W, RELLICK G S. Carborane-catalyzed graphitization in polyarylacetylene-derived carbon-carbon composites[J]. Carbon, 1991, 29(8): 1145-1153.
[8] ZHANG X Z, HUANG Y D, WANG T Y, et al. Effects of polyhedral oligomeric silsesquioxane coatings on the interface and impact properties of carbon-fiber/polyarylacetylene composites[J]. J App Polym Sci, 2006, 102(6): 5202-5211.
[9] 姚冬梅, 程文, 邹武, 等. 新型含硅芳基乙炔的固化及成炭机理研究[J]. 固体火箭技术, 2009, 32(5): 578-582. YAO D M, CHENG W, ZOU W, et al. Study on curing and pyrolytic mechanism of new PSAA resin[J]. Journal of Solid Rocket Technology, 2009, 32(5): 578-582.
[10] WANG M C, ZHAO T. Polyarylacetylene blends with improved processability and high thermal stability[J]. J App Polym Sci, 2007, 105(5): 2939-2946.
[11] WANG S K, LI M, GU Y Z, et al. Experimental study on crack defects formation in polyarylacetylene composites and modification improvement of resin[J]. Compos Mater, 2010, 44(25): 3017-3032.
[12] 范海波, 杨荣杰, 李定华. 多面体低聚八氨基苯基硅倍半氧烷合成方法改进及其表征[J]. 化学学报, 2012, 70(4): 429-435. FAN H B, YANG R J, LI D H. Synthesis improvement and characterization of polyhedral oligomeric octa(aminophenyl)silsesquioxane[J]. Acta Chimica Sinica, 2012, 70(4): 429-435.
[13] 范海波, 杨荣杰, 李向梅. 多面体低聚八硝基苯基硅倍半氧烷纯度分析[J]. 化学学报, 2012, 70(16): 1737-1742. FAN H B, YANG R J, LI X M. Purity analysis of polyhedral oligomeric octa(nitrophenyl)silsesquioxane[J]. Acta Chimica Sinica, 2012, 70(16): 1737-1742.
[14] FAN H B, YANG R J. Synthesis and characterization of polyhedral oligomeric azido-cctaphenylsilsesquioxane[J]. J App Polym Sci, 2012, 124(5): 4389-4397.
[15] FAN H B, HE J Y, YANG R J. Synthesis, characterization, and thermal curing of a novel polyhedral oligomeric ccta(propargylaminophenyl)silsesquioxane[J]. J App Polym Sci, 2012, 127(1): 463-470
[16] LI Q, ZHOU Y, HUANG X D, et al. Synthesis and characterization of a novel arylacetylene oligomer containing POSS units in main chains[J]. Eur Polym J, 2008, 44(8): 2538-2544.
[17] ZHANG Z P, LIANG G Z, REN P G, et al. Curing behavior of epoxy/POSS/DDS hybrid systems[J]. Polym Compos, 2008, 29(1): 77-83.
[18] 闫联生. 酚醛改性聚芳基乙炔基复合材料探索[J]. 玻璃钢/复合材料, 2001, (2): 22-24. YAN L S. Property improvement of polyarylacetylene matrix composites by phenolic resins[J]. FRP/CM, 2001, (2): 22-24.