聚酰胺610分子链段运动、局域态分布与聚集态结构的关系
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摘要
聚酰胺610是重要的热塑性工程塑料,通过介电和热刺激电流方法精确深入研究不同聚集态结构的聚酰胺610的分子链段运动和局域态分布。因此对聚酰胺610的电荷载流子存储输运特性与聚集态结构关系的研究具有重要的理论和实际意义。总结如下；
1.通过介电松弛研究发现淬火聚酰胺610与退火聚酰胺610一样,在室温以上存在3个松弛行为,随着温度增大顺次为：α松弛、MWS极化、电极极化。对于玻璃化转变的α松弛,退火聚酰胺610偶极松弛时间较大,退火聚酰胺610偶极取向运动的活化能较大。MWS极化对应于聚集在中间相的载流子的松弛行为,退火聚酰胺610的MWS极化过程松弛强度较大,中间相区域增多也导致退火聚酰胺610的MWS极化过程松弛时间较大。在介电测试温度下随着测试温度增大淬火聚酰胺610结晶度增大,中间相逐渐增多,使得淬火聚酰胺610的MWS极化过程松弛强度随介电测试温度增大而增大。发现在110℃-120℃左右存在转折温度,当温度在这个转折温度以下,非晶区的分子链段运动主导中间相的空间电荷输运和存储引起的极化,而当温度在这个转折温度以上,非晶区和中间相的分子链段运动共同主导中间相的空间电荷输运和存储引起的极化。电极极化则对应于聚集在试样表面与电极界面的载流子的松弛行为,空间电荷增多导致退火聚酰胺610电极极化松弛强度较大,并且退火聚酰胺610电极极化过程松弛时间较短。
2.在不同极化温度下对淬火聚酰胺610极化相当于在不同温度下对淬火聚酰胺610进行退火,可知淬火聚酰胺610具有3个局域能级,表现在热刺激电流谱上3个电流峰,分别对应于偶极松弛、非晶区及中间相和晶区陷阱俘获的空间电荷松弛。极化温度为80℃时淬火聚酰胺610的晶区陷阱俘获的空间电荷松弛非常小,通过研究峰电流与极化场强的关系发现,50℃左右的α峰为偶极松弛峰,110℃左右的p1峰为非晶区及中间相空间电荷峰。随着极化温度增大,晶区陷阱俘获的空间电荷松弛pz峰逐渐增大。分子链段运动受抑制导致偶极松弛强度减弱,活化能增大。极化温度增大产生更多的结构缺陷导致非晶区及中间区和晶区陷阱俘获空间电荷能力增加。极化温度增大使得非晶区及中间区被俘获空间电荷的稳定性下降和晶区被俘获空间电荷的稳定性提高。
3.退火聚酰胺610具有3个局域能级,表现在热刺激电流谱上3个电流峰,分别对应于偶极松弛、非晶区及中间相和晶区陷阱俘获的空间电荷松弛。随着退火温度增大,晶区陷阱俘获的空间电荷松弛p2峰逐渐增大。分子链段运动受抑制导致偶极松弛强度减弱,活化能增大。退火温度增大产生更多的结构缺陷导致非晶区及中间区和晶区陷阱俘获空间电荷能力增加。退火温度增大使得非晶区及中间区被俘获空间电荷的稳定性下降和晶区被俘获空间电荷的稳定性提高。
4.溶液成膜的未辐照和辐照聚酰胺610具有4个局域能级,表现在热刺激电流谱上4个电流峰,分别对应于偶极松弛、非晶区、非晶区与晶区之间的中间相和晶区陷阱俘获的空间电荷松弛。非晶区交联使得偶极松弛峰电流强度减弱,活化能增大。随着辐照剂量增大,非晶区交联程度比中间相交联程度增多,导致两相的陷阱能级趋于接近,非晶区和中间相陷阱俘获的空间电荷峰逐渐合并成一个峰。辐照使得晶区结晶破坏和晶相内交联对分子链段运动的作用相互抵消。γ-辐照后,随着更多的结构缺陷产生,非晶区、中间相和晶区陷阱俘获空间电荷能力增加,同时晶区被俘获空间电荷的稳定性基本不变而非晶区、中间相被俘获空间电荷的稳定性提高。
Polyamide 610, which has a molecular structure analogous to polyamide 66, is one of the most important polyamide engineering plastics. Polyamide 610 is a typical semicrystalline polymer with different microstructures under various thermal histories. The investigation of the aggregative state structure effect on chain segment motion and localized state sistributions in polyamide 610 is interesting both from the fundamental and technological point of view. Polymers acquire persistent polarization due to the alignment of dipoles and migration of space charges over macroscopic distance. Information on charge storage and transport phenomena in polymer electrets is of great interest for several industrial applications. The corresponding work is an important topic in the field of polymer electronic properties. It helps leading charge storage and transportation properties further in polymer and then has a great meaning on polymer's application in electrics, optics, acoustics, etc.
1. The experimental dielectric data were analyzed within the formalisms of complex permittivity and electric modulus. The results were discussed in terms of ac conductivity, MWS polarization, electrode polarization, and dc conductivity. Maxwell-Wagner-Sillars (MWS) polarization in polyamide 610 arising from charge carriers accumulated at the interphase between amorphous and crystalline regions and electrode polarization arising from charge carriers accumulating at the interface between an electrode and polyamide 610 have been investigated by means of dielectric relaxation spectra. In the frequency spectra of polyamide 610, the dielectric permittivity showed high values at low frequencies originating from charge carrier movement. The maximum ofε″MWS andε″eiec of quenched polyamide 610 is smaller than that for annealed polyamide 610 because crystallinity of quenched polyamide 610 increases with increase of the temperature and crystallinity of 180℃annealed polyamide 610 doesn't change. The temperature dependence of relaxation time follows the Vogel-Tammann-Fulcher (VTF) type. The results revealed that there is a transition temperature for the MWS polarization and dc conductivity, located between 110 and 120℃, resulting in the separation of two different charge carrier movement mechanisms. Below and above this transition temperature, the charge carrier transport is governed by the motion of the polymer chains. The change of charge carrier movement mechanisms is due to the onset of polymer chain motion in the interphase. For electrode polarization the motion of the polymeric chains was one of the factors leading to charge-carrier transport at temperatures higher than the glass-transition temperature
2. Quenched polyamide 610 polarizing at different temperatures corresponds to annealed polyamide 610 at different temperatures. There are three current peaks (namedα,ρ1 andρ2peak respectively) in TSDC spectra of quenched polyamide 610.αpeak is corresponding to the glass transition,ρ1 peak is attributed to space charge trapped in the bulk of amorphous region and inter-phase between crystalline and amorphous regions, and p2 peak is originated from space charge trapped in crystalline region. By analyzing the characteristic parameters of these peaks, it is found that the increase of polarization temperature induces the decrease of the chain segment mobility and promotes the creation of structural traps in polyamide 610. The decrease of the chain segment mobility in amorphous phase makes intensity of a peak weak and activation energy increscent. The higher of polarization temperature, the higher of degree of crystallinity, the more of charge carriers trapped in crystalline region. So the increase of polarization temperature makes intensity of the p2 peak strong and increases the stability of trapped charge in the crystalline regions, and the increase of polarization temperature makes intensity of the pi peak strong and decreases the stability of trapped charge in the amorphous region and inter-phase.
3. There are three current peaks (namedα,ρ1 andρ2 peak respectively) in the TSDC spectra of annealed polyamide 610. The a peak is attributed to a background dipole relaxation by the motion of chain segments over space charge contribution, theρ1 peak is originated from space charge trapped in amorphous phase and the interphase between crystalline and amorphous phases, and the p2 peak is originated from space charge trapped in crystalline phase. By analyzing the characteristic parameters of these peaks, it was found that annealing induced a decrease of the chain segment mobility and promoted the creation of structural traps in polyamide 610. The decrease of the chain segment mobility in amorphous phase made the intensity of the a peak weak and activation energy increased. The higher the annealing temperature, the higher the degree of crystallinity and the more charge carriers trapped in crystalline phase. So the increase of annealing temperature made the intensity of the p2 peak strong and increased the stability of trapped charge in the crystalline phases. The increase of annealing temperature made the intensity of the pi peak strong and decreased the stability of trapped charge in the amorphous phase and interphase,
4. There are four current peaks (namedα,ρ1,ρ2 andρ3 peak respectively) in TSDC spectra of solution-cast polyamide 610.αpeak corresponds to the glass transition,ρ1 peak is attributed to space charge trapped in the amorphous phase,ρ2 peak is originated from space charge trapped in the interphase between crystalline and amorphous regions andρ3 peak is originated from space charge trapped in crystalline phase. With the increase of irradiation dose from 1.5MGy to 2MGy,ρ1 peak andρ2 peak gradually merge into a peak. So the superiority of the crosslinking in amorphous phase over the crosslinking in interphase makes trap level of the amorphous phase and that of interphase gradually close. By analyzing the characteristic parameters of these peaks, it is found that gamma irradiation induces the decrease of chain segment mobility and increases structural defects in polyamide 610. Irradiation increases the stability of trapped charge in amorphous phase and interphase, but basically makes the stability of trapped charge in crystalline phase unchanged.
1.通过介电松弛研究发现淬火聚酰胺610与退火聚酰胺610一样,在室温以上存在3个松弛行为,随着温度增大顺次为：α松弛、MWS极化、电极极化。对于玻璃化转变的α松弛,退火聚酰胺610偶极松弛时间较大,退火聚酰胺610偶极取向运动的活化能较大。MWS极化对应于聚集在中间相的载流子的松弛行为,退火聚酰胺610的MWS极化过程松弛强度较大,中间相区域增多也导致退火聚酰胺610的MWS极化过程松弛时间较大。在介电测试温度下随着测试温度增大淬火聚酰胺610结晶度增大,中间相逐渐增多,使得淬火聚酰胺610的MWS极化过程松弛强度随介电测试温度增大而增大。发现在110℃-120℃左右存在转折温度,当温度在这个转折温度以下,非晶区的分子链段运动主导中间相的空间电荷输运和存储引起的极化,而当温度在这个转折温度以上,非晶区和中间相的分子链段运动共同主导中间相的空间电荷输运和存储引起的极化。电极极化则对应于聚集在试样表面与电极界面的载流子的松弛行为,空间电荷增多导致退火聚酰胺610电极极化松弛强度较大,并且退火聚酰胺610电极极化过程松弛时间较短。
2.在不同极化温度下对淬火聚酰胺610极化相当于在不同温度下对淬火聚酰胺610进行退火,可知淬火聚酰胺610具有3个局域能级,表现在热刺激电流谱上3个电流峰,分别对应于偶极松弛、非晶区及中间相和晶区陷阱俘获的空间电荷松弛。极化温度为80℃时淬火聚酰胺610的晶区陷阱俘获的空间电荷松弛非常小,通过研究峰电流与极化场强的关系发现,50℃左右的α峰为偶极松弛峰,110℃左右的p1峰为非晶区及中间相空间电荷峰。随着极化温度增大,晶区陷阱俘获的空间电荷松弛pz峰逐渐增大。分子链段运动受抑制导致偶极松弛强度减弱,活化能增大。极化温度增大产生更多的结构缺陷导致非晶区及中间区和晶区陷阱俘获空间电荷能力增加。极化温度增大使得非晶区及中间区被俘获空间电荷的稳定性下降和晶区被俘获空间电荷的稳定性提高。
3.退火聚酰胺610具有3个局域能级,表现在热刺激电流谱上3个电流峰,分别对应于偶极松弛、非晶区及中间相和晶区陷阱俘获的空间电荷松弛。随着退火温度增大,晶区陷阱俘获的空间电荷松弛p2峰逐渐增大。分子链段运动受抑制导致偶极松弛强度减弱,活化能增大。退火温度增大产生更多的结构缺陷导致非晶区及中间区和晶区陷阱俘获空间电荷能力增加。退火温度增大使得非晶区及中间区被俘获空间电荷的稳定性下降和晶区被俘获空间电荷的稳定性提高。
4.溶液成膜的未辐照和辐照聚酰胺610具有4个局域能级,表现在热刺激电流谱上4个电流峰,分别对应于偶极松弛、非晶区、非晶区与晶区之间的中间相和晶区陷阱俘获的空间电荷松弛。非晶区交联使得偶极松弛峰电流强度减弱,活化能增大。随着辐照剂量增大,非晶区交联程度比中间相交联程度增多,导致两相的陷阱能级趋于接近,非晶区和中间相陷阱俘获的空间电荷峰逐渐合并成一个峰。辐照使得晶区结晶破坏和晶相内交联对分子链段运动的作用相互抵消。γ-辐照后,随着更多的结构缺陷产生,非晶区、中间相和晶区陷阱俘获空间电荷能力增加,同时晶区被俘获空间电荷的稳定性基本不变而非晶区、中间相被俘获空间电荷的稳定性提高。
Polyamide 610, which has a molecular structure analogous to polyamide 66, is one of the most important polyamide engineering plastics. Polyamide 610 is a typical semicrystalline polymer with different microstructures under various thermal histories. The investigation of the aggregative state structure effect on chain segment motion and localized state sistributions in polyamide 610 is interesting both from the fundamental and technological point of view. Polymers acquire persistent polarization due to the alignment of dipoles and migration of space charges over macroscopic distance. Information on charge storage and transport phenomena in polymer electrets is of great interest for several industrial applications. The corresponding work is an important topic in the field of polymer electronic properties. It helps leading charge storage and transportation properties further in polymer and then has a great meaning on polymer's application in electrics, optics, acoustics, etc.
1. The experimental dielectric data were analyzed within the formalisms of complex permittivity and electric modulus. The results were discussed in terms of ac conductivity, MWS polarization, electrode polarization, and dc conductivity. Maxwell-Wagner-Sillars (MWS) polarization in polyamide 610 arising from charge carriers accumulated at the interphase between amorphous and crystalline regions and electrode polarization arising from charge carriers accumulating at the interface between an electrode and polyamide 610 have been investigated by means of dielectric relaxation spectra. In the frequency spectra of polyamide 610, the dielectric permittivity showed high values at low frequencies originating from charge carrier movement. The maximum ofε″MWS andε″eiec of quenched polyamide 610 is smaller than that for annealed polyamide 610 because crystallinity of quenched polyamide 610 increases with increase of the temperature and crystallinity of 180℃annealed polyamide 610 doesn't change. The temperature dependence of relaxation time follows the Vogel-Tammann-Fulcher (VTF) type. The results revealed that there is a transition temperature for the MWS polarization and dc conductivity, located between 110 and 120℃, resulting in the separation of two different charge carrier movement mechanisms. Below and above this transition temperature, the charge carrier transport is governed by the motion of the polymer chains. The change of charge carrier movement mechanisms is due to the onset of polymer chain motion in the interphase. For electrode polarization the motion of the polymeric chains was one of the factors leading to charge-carrier transport at temperatures higher than the glass-transition temperature
2. Quenched polyamide 610 polarizing at different temperatures corresponds to annealed polyamide 610 at different temperatures. There are three current peaks (namedα,ρ1 andρ2peak respectively) in TSDC spectra of quenched polyamide 610.αpeak is corresponding to the glass transition,ρ1 peak is attributed to space charge trapped in the bulk of amorphous region and inter-phase between crystalline and amorphous regions, and p2 peak is originated from space charge trapped in crystalline region. By analyzing the characteristic parameters of these peaks, it is found that the increase of polarization temperature induces the decrease of the chain segment mobility and promotes the creation of structural traps in polyamide 610. The decrease of the chain segment mobility in amorphous phase makes intensity of a peak weak and activation energy increscent. The higher of polarization temperature, the higher of degree of crystallinity, the more of charge carriers trapped in crystalline region. So the increase of polarization temperature makes intensity of the p2 peak strong and increases the stability of trapped charge in the crystalline regions, and the increase of polarization temperature makes intensity of the pi peak strong and decreases the stability of trapped charge in the amorphous region and inter-phase.
3. There are three current peaks (namedα,ρ1 andρ2 peak respectively) in the TSDC spectra of annealed polyamide 610. The a peak is attributed to a background dipole relaxation by the motion of chain segments over space charge contribution, theρ1 peak is originated from space charge trapped in amorphous phase and the interphase between crystalline and amorphous phases, and the p2 peak is originated from space charge trapped in crystalline phase. By analyzing the characteristic parameters of these peaks, it was found that annealing induced a decrease of the chain segment mobility and promoted the creation of structural traps in polyamide 610. The decrease of the chain segment mobility in amorphous phase made the intensity of the a peak weak and activation energy increased. The higher the annealing temperature, the higher the degree of crystallinity and the more charge carriers trapped in crystalline phase. So the increase of annealing temperature made the intensity of the p2 peak strong and increased the stability of trapped charge in the crystalline phases. The increase of annealing temperature made the intensity of the pi peak strong and decreased the stability of trapped charge in the amorphous phase and interphase,
4. There are four current peaks (namedα,ρ1,ρ2 andρ3 peak respectively) in TSDC spectra of solution-cast polyamide 610.αpeak corresponds to the glass transition,ρ1 peak is attributed to space charge trapped in the amorphous phase,ρ2 peak is originated from space charge trapped in the interphase between crystalline and amorphous regions andρ3 peak is originated from space charge trapped in crystalline phase. With the increase of irradiation dose from 1.5MGy to 2MGy,ρ1 peak andρ2 peak gradually merge into a peak. So the superiority of the crosslinking in amorphous phase over the crosslinking in interphase makes trap level of the amorphous phase and that of interphase gradually close. By analyzing the characteristic parameters of these peaks, it is found that gamma irradiation induces the decrease of chain segment mobility and increases structural defects in polyamide 610. Irradiation increases the stability of trapped charge in amorphous phase and interphase, but basically makes the stability of trapped charge in crystalline phase unchanged.
引文
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