新型光激放电测量装置研制及典型聚合物PSD谱
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摘要
空间电荷行为在工程电介质电老化击穿过程中起着极其重要的作用,绝缘介质中的空间电荷问题已经成为工程电介质向高压电力设备发展的一个重要的制约因素。同时,随着机电传感应用的迅速发展,机电传感器中由于聚合物驻极体中空间电荷稳定存储的重要性,迫切需要研究清楚空间电荷的长期保持机理。近些年来,聚合物中的空间电荷在上述两方面的作用都一直是相关研究人员关注的焦点问题。而空间电荷往往是各类陷阱俘获造成的,陷阱的性质决定着电荷的存储和输运。因此,准确表征聚合物电介质材料中的电荷陷阱能谱分布对于改进与提高聚合物电介质材料的性质和应用水平具有重要的科学意义和实用价值。
本论文研究了利用光激放电(Photo-stimulated discharge-PSD)原理测量聚合物材料中的陷阱能谱分布,并完成如下工作:
设计制作了国内外第一台基于激光泵浦光参量振动器(Optical Parametric Oscillator-OPO)作为激发光源的PSD测量谱仪。其工作波长范围从长波到短波为2300-210nm,陷阱能量测量范围约为0.50-5.90eV,精度为±0.01eV。同时在全波段范围内输出光子通量密度可达3.0×10 24 cm ?2 s?1以上。该谱仪能很好地满足对聚合物电介质材料陷阱的测试要求。
在新型PSD谱仪中所采用的光源是激光光源,激光辐照在聚合物材料上可能会对材料结构产生破坏作用,针对这一问题,借助傅里叶红外光谱以及拉曼光谱证证实了新型PSD谱仪与被测样品作用后,并没有破坏被测材料的化学结构,从而不会因激光辐照而带来附加的新的电荷陷阱、产生光侵蚀或光降解作用。
利用新型PSD谱仪对光激放电方法进行了较为细致的研究。这里包括对于同一被测样品,在不同的实验条件下(例如没有电荷注入、不同电荷注入方式、不同注入剂量以及不同扫描次数等)的陷阱分布进行较深入的研究。
提出了PSD谱能量校正方法。通过对原始PSD谱影响因素的分析,明确了原始PSD谱中不但包含了陷阱电荷的释放因素,还有激发光源能量变化的影响。为了消除这种影响,提出了能量归一化的PSD谱。经过能量校正后的PSD电流谱能够更真实地反映出电介质中电荷陷阱的分布状态,并给出了在不发生电荷再入陷情况下的陷阱态密度的获取方法。开发了基于Labview的测控软件,可以与硬件系统相配合,实现能量归一化PSD谱的测量。
利用新型的PSD谱仪测试了聚酯、聚酰亚胺、聚丙烯以及聚乙烯等几种典型聚合物材料的PSD谱。发现聚酯中电荷陷阱主要分布在4.10-5.20eV的范围内,聚酰亚胺的陷阱分布在3.10-4.10eV之间,这两种材料的陷阱都与羰基有关,其数值差异也许与羰基所处的微观环境有关;聚丙烯的陷阱在4.80-5.90eV范围内,而聚乙烯的陷阱为4.80eV以上。这两种材料陷阱的最有可能的来源是聚合过程中引发剂的残留。
利用所研制的新型光激放电谱仪结合TSC技术与电声脉冲法PEA详细研究了聚乙烯材料中的载流子陷阱的分布。一般认为,TSC方法由于材料本身耐热温度的限制,只能测量浅陷阱,而PSD方法适合测量较深陷阱。但经过研究发现,由于热运动对陷阱的侵蚀作用,在TSC方法中所测得的结果仅仅是陷阱深度的视在表观值,实际上陷阱电荷的热激发与光激发是来源于同一个陷阱。热激发不但使受陷电荷受到激发,同时也使陷阱深度本身因受到热侵蚀而变浅了。所以,光激发方法更真实地反映了聚合物材料陷阱的本征特性。
Space charge plays an important role in electrical aging and breakdown of engineering dielectrics, and it has becoming an important factor for restricting the development of high electric field of power cable. Meanwhile, with the rapid development of electromechanical sensing applications, the long-term charge-storage mechanisms urgently need to be researched clearly because of the importance of space charge storage stability in polymer electret of electromechanical sensors. In recent years, space charge effects mentioned above in polymer are always the focus problems that are concerned by relevant researchers. Space charge is often captured by the trap, and the trap characteristics decide charge storage and transport. Therefore it has important scientific meaning and practical value to accurately characterize energy distribution of charge trap in polymer dielectric materials in order to improve their properties and application.
In this dissertation, we measure the energy distribution of trap in polymer materials by photo-stimulated discharge (PSD), and finish the work as follows: Design and set up the first PSD measuring spectrum analyzer based on optical parametric oscillator (OPO) as exciting light source at home and abroad. The range of output wavelength is 2300-210nm. The range of trap energy measurement is about 0.50-5.90eV and an accuracy is of±0.01eV. At the same time the output photon flux density is up to 3.0×10 24 cm ? 2 s?1 or more in the whole band. The PSD spectrum is better able to meet the measurement requirements from respect of exciting light intensity, output wavelength range, output wavelength tunable properties and the measurement accuracy.
Because the light source of new PSD spectrum analyzer is laser, the output light may damage the chemical structures of polymer materials. In view of such a problem, we prove the new PSD spectrum analyzer dose not has any the destructive action on chemical structures of tested materials by using Fourier infrared and Raman spectroscopy. The molecular chain structures of samples are not broken and they do not generate new free radicals. Therefore the laser irradiation does not generate additional charge trap and not cause either light erosion or photodegradation.
Using the new PSD spectrum analyzer, PSD method is studied in detail. This includes the study of trap distribution in different experimental conditions for the same tested sample, such as no charge injection, different charge injection methods, different charge injection doses, different number of scans and so on. Put forward energy calibration method of PSD spectra. Through the analysis of the original PSD spectra, we identify the original PSD spectra contain the information of not only trap charge release but also exciting light energy change. In order to eliminate the influence of exciting light energy change, we propose energy normalized PSD spectra, which can really give the informations of the distribution of charge trap in dielectric. Based on the Labview, we develop control software, which can combine with the hardware system and achieve energy normalization of the PSD spectra.
PSD spectra of typical polymer materials of polyester, polyimide, polypropylene, and cross-linked polyethylene were tested by the new PSD spectrometer. It was found that the charge traps in polyester is mainly in the range of 4.10-5.20eV, meanwhile 3.10-4.10 eV traps distribution in polyimide. The traps of these two materials are related with the carbonyl. There is a trap distribution of 4.80-5.90eV in polypropylene and trap more than 4.80eV in crosslinked polyethylene, which most likely come from residual catalyst during the polymerization process.
Combine new PSD spectrum analyzer with TSC and PEA to study the distribution of charge trap in PE in detail. Generally speaking, TSC can only measure shallow trap because of the limit to heat-resistance temperature of material itself, while PSD is fit for measuring deep trap. Through our research we find the measurement result of TSC is only the apparent trap depth. In fact, the trap charges by the thermal and the optical excitation are from the same trap. Thermal stimulated method not only stimulates trap charges, but also makes trap depth become shallow due to thermal erosion. Therefore PSD really reflects the intrinsic properties of trap in polymer materials.
本论文研究了利用光激放电(Photo-stimulated discharge-PSD)原理测量聚合物材料中的陷阱能谱分布,并完成如下工作:
设计制作了国内外第一台基于激光泵浦光参量振动器(Optical Parametric Oscillator-OPO)作为激发光源的PSD测量谱仪。其工作波长范围从长波到短波为2300-210nm,陷阱能量测量范围约为0.50-5.90eV,精度为±0.01eV。同时在全波段范围内输出光子通量密度可达3.0×10 24 cm ?2 s?1以上。该谱仪能很好地满足对聚合物电介质材料陷阱的测试要求。
在新型PSD谱仪中所采用的光源是激光光源,激光辐照在聚合物材料上可能会对材料结构产生破坏作用,针对这一问题,借助傅里叶红外光谱以及拉曼光谱证证实了新型PSD谱仪与被测样品作用后,并没有破坏被测材料的化学结构,从而不会因激光辐照而带来附加的新的电荷陷阱、产生光侵蚀或光降解作用。
利用新型PSD谱仪对光激放电方法进行了较为细致的研究。这里包括对于同一被测样品,在不同的实验条件下(例如没有电荷注入、不同电荷注入方式、不同注入剂量以及不同扫描次数等)的陷阱分布进行较深入的研究。
提出了PSD谱能量校正方法。通过对原始PSD谱影响因素的分析,明确了原始PSD谱中不但包含了陷阱电荷的释放因素,还有激发光源能量变化的影响。为了消除这种影响,提出了能量归一化的PSD谱。经过能量校正后的PSD电流谱能够更真实地反映出电介质中电荷陷阱的分布状态,并给出了在不发生电荷再入陷情况下的陷阱态密度的获取方法。开发了基于Labview的测控软件,可以与硬件系统相配合,实现能量归一化PSD谱的测量。
利用新型的PSD谱仪测试了聚酯、聚酰亚胺、聚丙烯以及聚乙烯等几种典型聚合物材料的PSD谱。发现聚酯中电荷陷阱主要分布在4.10-5.20eV的范围内,聚酰亚胺的陷阱分布在3.10-4.10eV之间,这两种材料的陷阱都与羰基有关,其数值差异也许与羰基所处的微观环境有关;聚丙烯的陷阱在4.80-5.90eV范围内,而聚乙烯的陷阱为4.80eV以上。这两种材料陷阱的最有可能的来源是聚合过程中引发剂的残留。
利用所研制的新型光激放电谱仪结合TSC技术与电声脉冲法PEA详细研究了聚乙烯材料中的载流子陷阱的分布。一般认为,TSC方法由于材料本身耐热温度的限制,只能测量浅陷阱,而PSD方法适合测量较深陷阱。但经过研究发现,由于热运动对陷阱的侵蚀作用,在TSC方法中所测得的结果仅仅是陷阱深度的视在表观值,实际上陷阱电荷的热激发与光激发是来源于同一个陷阱。热激发不但使受陷电荷受到激发,同时也使陷阱深度本身因受到热侵蚀而变浅了。所以,光激发方法更真实地反映了聚合物材料陷阱的本征特性。
Space charge plays an important role in electrical aging and breakdown of engineering dielectrics, and it has becoming an important factor for restricting the development of high electric field of power cable. Meanwhile, with the rapid development of electromechanical sensing applications, the long-term charge-storage mechanisms urgently need to be researched clearly because of the importance of space charge storage stability in polymer electret of electromechanical sensors. In recent years, space charge effects mentioned above in polymer are always the focus problems that are concerned by relevant researchers. Space charge is often captured by the trap, and the trap characteristics decide charge storage and transport. Therefore it has important scientific meaning and practical value to accurately characterize energy distribution of charge trap in polymer dielectric materials in order to improve their properties and application.
In this dissertation, we measure the energy distribution of trap in polymer materials by photo-stimulated discharge (PSD), and finish the work as follows: Design and set up the first PSD measuring spectrum analyzer based on optical parametric oscillator (OPO) as exciting light source at home and abroad. The range of output wavelength is 2300-210nm. The range of trap energy measurement is about 0.50-5.90eV and an accuracy is of±0.01eV. At the same time the output photon flux density is up to 3.0×10 24 cm ? 2 s?1 or more in the whole band. The PSD spectrum is better able to meet the measurement requirements from respect of exciting light intensity, output wavelength range, output wavelength tunable properties and the measurement accuracy.
Because the light source of new PSD spectrum analyzer is laser, the output light may damage the chemical structures of polymer materials. In view of such a problem, we prove the new PSD spectrum analyzer dose not has any the destructive action on chemical structures of tested materials by using Fourier infrared and Raman spectroscopy. The molecular chain structures of samples are not broken and they do not generate new free radicals. Therefore the laser irradiation does not generate additional charge trap and not cause either light erosion or photodegradation.
Using the new PSD spectrum analyzer, PSD method is studied in detail. This includes the study of trap distribution in different experimental conditions for the same tested sample, such as no charge injection, different charge injection methods, different charge injection doses, different number of scans and so on. Put forward energy calibration method of PSD spectra. Through the analysis of the original PSD spectra, we identify the original PSD spectra contain the information of not only trap charge release but also exciting light energy change. In order to eliminate the influence of exciting light energy change, we propose energy normalized PSD spectra, which can really give the informations of the distribution of charge trap in dielectric. Based on the Labview, we develop control software, which can combine with the hardware system and achieve energy normalization of the PSD spectra.
PSD spectra of typical polymer materials of polyester, polyimide, polypropylene, and cross-linked polyethylene were tested by the new PSD spectrometer. It was found that the charge traps in polyester is mainly in the range of 4.10-5.20eV, meanwhile 3.10-4.10 eV traps distribution in polyimide. The traps of these two materials are related with the carbonyl. There is a trap distribution of 4.80-5.90eV in polypropylene and trap more than 4.80eV in crosslinked polyethylene, which most likely come from residual catalyst during the polymerization process.
Combine new PSD spectrum analyzer with TSC and PEA to study the distribution of charge trap in PE in detail. Generally speaking, TSC can only measure shallow trap because of the limit to heat-resistance temperature of material itself, while PSD is fit for measuring deep trap. Through our research we find the measurement result of TSC is only the apparent trap depth. In fact, the trap charges by the thermal and the optical excitation are from the same trap. Thermal stimulated method not only stimulates trap charges, but also makes trap depth become shallow due to thermal erosion. Therefore PSD really reflects the intrinsic properties of trap in polymer materials.
引文
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