导电PAN及PAN/PI复合薄膜的制备与环境稳定性研究
摘要
聚苯胺由于具有结构多样化的特点,而呈现广泛的应用前景。目前,聚苯胺在应用上的热点和难点主要集中在导电聚苯胺的可加工性、稳定性。
本文利用乳液法,以十二烷基苯磺酸(DBSA)为乳化剂,同时也为掺杂剂,以过硫酸铵(APS)为氧化剂合成了导电聚苯胺(PAN);利用溶液法,以N-甲基-2-吡咯烷酮(NMP)为溶剂,在室温下,4,4'-二胺基二苯醚(ODA)与均苯四甲酸二酐(PMDA)合成出聚亚胺酸(PAA)。通过热亚胺化法制备了聚酰亚胺(PI),在此基础上,制备了PAN/PI复合材料。
在臭氧腐蚀和紫外辐照100 h后,掺杂聚苯胺的导电性能下降,但随时间的延长,电导率的下降速率减缓,仍在半导体范围内。PI在紫外辐照100 h前后的电导率始终在0.5~0.6×10~(-4) S/cm范围内波动;在紫外辐照50 h后,在50 kHz以前,PI介电损耗值由0.33下降到0.05,而在50 kHz以后,介电损耗值保持在0.05。聚苯胺改性聚酰亚胺后,使聚酰亚胺的电导率由0.6×10~(-4) S/cm提高到1.4·10~(-4)×S/cm;而介电损耗由0.05逐渐上升到0.10。PAN/PI在紫外辐照100 h前后的电导率由1.4×10~(-4) S/cm下降到1.1×10~(-4) S/cm。热分析结果表明聚苯胺在400℃才完全分解,PAN/PI复合材料的分解温度范围为540℃~670℃,在臭氧、紫外环境下具有良好的稳定性。
Polyaniline have potential applications as their variable strueture, The Problems of Polyaniline are mainly focused on the Processibiling and stability of polyaniline.
The conductive polyaniline was prepared with emulsion polymerization method in this article, dodecyl benzene sulfonic acid (DBSA) as the emulsifier and doping agent; and ammonium sulfate (APS) as oxidant. The polyimine acid (PAA) was prepared via solution polymerization with N-methyl-2- pyrrolidone as solvent, pyromellinc dianhydnde (PMDA) and 4, 4'-amino ether (ODA) as monomers at room temperature. Technics was fixed, Then polyimide was prepared. On this basis of, PAN/PI composites was prepared.
After corrosion of ozone and ultraviolet irradiation for 100h, the conductivity of polyaniline is decreased, but as the irradiation time increases, electrical conductivity tends to level off, and still in the rang of semiconductor. The conductivity of PI is changed in the range of 0.5~0.6×10~(-4) S/cm before sand after 100 h irradiation. After UV irradiation for 50 h, the dielectric loss of PI is decreased from 0.33 to 0.05 before 50 kHz, whereas after 50 kHz, it remains at 0.05; The conductivity of PAN/PI composites decreased from the 1.4×10~(-4) S/cm to 1.1×10~(-4) S/cm after 100 h UV irradiation. After modified with polyaniline, the conductivity of polyimide is increased from 0.6×10~(-4) S/cm to 1.4×10~(-4) S/cm while the dielectric loss of the PAN/PI composites is increased gradually from 0.05 to 0.10. It is proved that polyaniline is decomposed completely at 400℃via thermal analysis, decocmposition temperature of PAN/PI composites was from 540℃to 670℃, and its stability is good enough in the ozone and UV environment.
本文利用乳液法,以十二烷基苯磺酸(DBSA)为乳化剂,同时也为掺杂剂,以过硫酸铵(APS)为氧化剂合成了导电聚苯胺(PAN);利用溶液法,以N-甲基-2-吡咯烷酮(NMP)为溶剂,在室温下,4,4'-二胺基二苯醚(ODA)与均苯四甲酸二酐(PMDA)合成出聚亚胺酸(PAA)。通过热亚胺化法制备了聚酰亚胺(PI),在此基础上,制备了PAN/PI复合材料。
在臭氧腐蚀和紫外辐照100 h后,掺杂聚苯胺的导电性能下降,但随时间的延长,电导率的下降速率减缓,仍在半导体范围内。PI在紫外辐照100 h前后的电导率始终在0.5~0.6×10~(-4) S/cm范围内波动;在紫外辐照50 h后,在50 kHz以前,PI介电损耗值由0.33下降到0.05,而在50 kHz以后,介电损耗值保持在0.05。聚苯胺改性聚酰亚胺后,使聚酰亚胺的电导率由0.6×10~(-4) S/cm提高到1.4·10~(-4)×S/cm;而介电损耗由0.05逐渐上升到0.10。PAN/PI在紫外辐照100 h前后的电导率由1.4×10~(-4) S/cm下降到1.1×10~(-4) S/cm。热分析结果表明聚苯胺在400℃才完全分解,PAN/PI复合材料的分解温度范围为540℃~670℃,在臭氧、紫外环境下具有良好的稳定性。
Polyaniline have potential applications as their variable strueture, The Problems of Polyaniline are mainly focused on the Processibiling and stability of polyaniline.
The conductive polyaniline was prepared with emulsion polymerization method in this article, dodecyl benzene sulfonic acid (DBSA) as the emulsifier and doping agent; and ammonium sulfate (APS) as oxidant. The polyimine acid (PAA) was prepared via solution polymerization with N-methyl-2- pyrrolidone as solvent, pyromellinc dianhydnde (PMDA) and 4, 4'-amino ether (ODA) as monomers at room temperature. Technics was fixed, Then polyimide was prepared. On this basis of, PAN/PI composites was prepared.
After corrosion of ozone and ultraviolet irradiation for 100h, the conductivity of polyaniline is decreased, but as the irradiation time increases, electrical conductivity tends to level off, and still in the rang of semiconductor. The conductivity of PI is changed in the range of 0.5~0.6×10~(-4) S/cm before sand after 100 h irradiation. After UV irradiation for 50 h, the dielectric loss of PI is decreased from 0.33 to 0.05 before 50 kHz, whereas after 50 kHz, it remains at 0.05; The conductivity of PAN/PI composites decreased from the 1.4×10~(-4) S/cm to 1.1×10~(-4) S/cm after 100 h UV irradiation. After modified with polyaniline, the conductivity of polyimide is increased from 0.6×10~(-4) S/cm to 1.4×10~(-4) S/cm while the dielectric loss of the PAN/PI composites is increased gradually from 0.05 to 0.10. It is proved that polyaniline is decomposed completely at 400℃via thermal analysis, decocmposition temperature of PAN/PI composites was from 540℃to 670℃, and its stability is good enough in the ozone and UV environment.
引文
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