| 费志方,李昆锋,杨自春,高文杰,陈国兵.APTES交联型聚酰亚胺气凝胶的制备与表征[J].材料导报,2018,32(20):3623-3627 |
| APTES交联型聚酰亚胺气凝胶的制备与表征 |
| Synthesis and Characterization of the APTES Cross-linked Polyimide Aerogels |
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| DOI：10.11896/j.issn.1005-023X.2018.20.023 |
| 中文关键词: 聚酰亚胺气凝胶 硅烷偶联剂 交联 力学性能 热稳定性 |
| 英文关键词: polyimide aerogel, silane coupling agent, cross-linked, mechanical properties, thermal stability |
| 基金项目:国家自然科学基金(51702364);国家部委基金项目(417212409) |
| 作者 | 单位 | E-mail | | 费志方 | 海军工程大学舰船高温结构复合材料研究室,武汉 430033
海军工程大学动力工程学院,武汉 430033 | fzf_js@126.com,yangzichun11@sina.com | | 李昆锋 | 海军工程大学舰船高温结构复合材料研究室,武汉 430033
海军工程大学动力工程学院,武汉 430033 | | | 杨自春 | 海军工程大学舰船高温结构复合材料研究室,武汉 430033
海军工程大学动力工程学院,武汉 430033 | fzf_js@126.com,yangzichun11@sina.com | | 高文杰 | 海军工程大学舰船高温结构复合材料研究室,武汉 430033
海军工程大学动力工程学院,武汉 430033 | | | 陈国兵 | 海军工程大学舰船高温结构复合材料研究室,武汉 430033
海军工程大学动力工程学院,武汉 430033 | |
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| 中文摘要: |
| 以低成本的3-氨丙基三己氧基硅烷(APTES)为交联剂,4,4′-二氨基二苯醚(ODA)为二胺单体,3,3′,4,4′-联苯四甲酸二酐(BPDA)或均苯四甲酸二酐(PMDA)为二酐单体,采用溶胶-凝胶和化学亚胺化方法,结合CO2超临界干燥技术,制备出两种不同二酐单体的交联型聚酰亚胺气凝胶。采用FTIR、SEM、N2吸脱附、万能材料试验机、热重分析等手段来表征样品的化学组成、微观形貌、孔结构、压缩性能及热稳定性,研究了二酐单体种类对聚酰亚胺气凝胶的压缩性能及热稳定性的影响。结果表明:采用BPDA和PMDA制备的交联型聚酰亚胺气凝胶都具有纳米尺度的纤维状网络结构,具有密度低(0.102 g/cm3和0.121 g/cm3)和比表面积大(295 m2/g和311 m2/g)的特性。以PMDA为单体的交联型聚酰亚胺气凝胶10%应变对应的压缩强度和压缩模量分别为0.37 MPa和5.3 MPa,高于以BPDA为单体的交联型聚酰亚胺气凝胶(0.17 MPa和3.0 MPa)。此外,前者制得的聚酰亚胺的初始热分解温度为543 ℃,高于后者制得的聚酰亚胺的初始热分解温度(502 ℃)。 |
| 英文摘要: |
| Taking the low-cost 3-aminopropyltriethoxysilane (APTES) as crosslinking agent,4,4′-oxydianiline (ODA) as diamine monomer,3,3′,4,4′-biphenyltetracarboxylic dianhydride (BPDA) or pyromellitic dianhydride (PMDA) as dianhydride monomer, cross-linked polyimide aerogels with different dianhydride monomers were successfully synthesized by sol-gel and chemical imidization methods combined with CO2 supercritical drying technique. Then, the chemical composition, micro topography, pore structure, compressibility and thermal stability of the samples were characterized by FTIR, SEM, N2 adsorption and desorption, universal material testing machine and thermogravimetric analysis. Furthermore, the effects of dianhydride monomers on the compressibility and thermal stability of polyimide aerogels were investigated. The results showed that the polyimide aerogels with two kinds of mo-nomers both presented nanoscale fibrous network structure with low density (0.102 g/cm3 and 0.121 g/cm3) and large specific surface area (295 m2/g and 311 m2/g). The cross-linked polyimide aerogels with PMDA as monomer possessed the compressive strength and compressive modulus of 0.37 MPa and 5.3 MPa, which were higher than that of the cross-linked polyimide aerogels with BPDA as monomer (0.17 MPa and 3.0 MPa). Besides, the initial thermal decomposition temperature of the former polyimide was 543 ℃, which was higher than the initial thermal decomposition temperature of the latter polyimide (502 ℃). |
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