超高分子量聚乙烯基导电复合材料的电/热性能研究
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摘要
聚合物基PTC(Positive temperature coefficient)材料是一类具有重要理论和应用价值的新型功能材料,由于其独特的热电开关特性,及导电性能可调、质量轻、耐腐蚀、成本低、易成型加工等优点,可广泛应用于自控温电热器件、过流保护器和传感器等领域。但是目前聚合物基PTC材料在理论和实际应用方面还有待进一步研究和完善,如PTC效应机理、PTC强度的提高、NTC (Negative temperature coefficient)现象的消除以及高温稳定性和重现性的改进,PTC材料的自发热效率低等。
本文首先利用凝胶结晶溶液方法制备了碳纤维(CF)和镀镍碳纤维(NiCF)填充的超高分子量聚乙烯(UHMWPE)导电聚合物复合材料,利用DSC, SEM, WAXS, DMA和凝胶含量测试等测试手段,研究了导电填料,伽马射线辐射交联,化学交联对材料导电及机械性能的影响。结果表明,NiCF比CF导电性更高,制备的材料的逾渗阈值低。伽马射线辐射交联能够提高材料的PTC效应,而化学交联能提高复合材料的导电性能和导电稳定性,并提高材料的机械性能。
采用UHMWPE和乙烯基甲基丙烯酸甲酯共聚物(EMMA)为聚合物基体,CF为导电填料,利用凝胶结晶溶液方法制备了UHMWPE-EMMA-CF三元导电聚合物复合材料。利用DSC, SEM, WAXS, TGA, DMA,凝胶含量等表征测试手段,系统讨论了EMMA含量,CF含量和伽马射线辐射交联等因素对其导电性,热学性能,形貌特征,机械性能等的影响,并探讨了伽马射线辐射交联机理。结果表明伽马射线辐射处理在聚合物中形成了交联结构。辐射后材料的PTC强度显著提高,基体比例UHMWPE/EMMA为1/1的样品经500kGy辐射后PTC强度达到1010。NTC效应消失,PTC效应重复性提高。
对UHMWPE-EMMA-CF导电聚合物复合材料的自发热性能进行了研究。结果表明,在相同的CF浓度和外加电压时,基体比例为1/6的样品的表面温度大于基体比例为1/1的。伽马射线辐射处理能显著提高材料的自发热性能。在外加电压为20V,基体比例为1/1的样品经500kGy辐射后其表面温度比未辐射样品提高约30℃。基体比例为1/1,1/3和1/6的样品对应的最佳伽马射线辐射剂量分别为1000kGy,500kGy和200kGy。
通过聚合物体积热膨胀实验对聚合物导电复合材料的PTC效应的机理进行了探讨。结果表明体积膨胀是PTC效应的重要影响因素。材料的介电性能分析表明,材料电阻率和介电常数对温度、频率具有强烈依赖性。介电测试结果与复合材料直流PTC性能的实验结论一致,并从微观角度反映了结构的变化及伽马射线对复合材料导电性等性能的影响。
Polymeric PTC composite is a novel functional material with importance both in research and application fields. This kind of composites can be widely applied in many fields such as self-regulating heaters, over-current protectors and sensors due to their advantages as thermoelectrical-switching characteristic, adjustable conductivity, light weight, corrosion resistance, low cost and simple processing technique. However, further research and improvement are necessary for the PTC materials in both theory and practical application respects, which focus on the conductive mechanism, enhance of PTC intensity, elimination of NTC phenomenon and improvement of stability and reproducibility at high temperature, low heat efficiency and so forth.
Firstly, carbon fiber (CF) or nickel-coated carbon fiber (Ni-CF) filled ultra-high-molecular weight polyethylene (UHMWPE) composites were prepared by gelation/crystallization method. DSC, SEM, WAXS, DMA and gel fraction measurements were employed to investigate the electrical and mechanical properties of composites with respect to the effect of content of fillers, gamma ray irradiation and chemical crosslink. Results demonstrated that lower percolation threshold value of composites was obtained by NiCF than CF due to its higher conductivity. PTC effect of composites was improved by gamma ray irradiation, while high and stable conductivity and mechanical properties were realized by means of chemical crosslink method.
Secondly, CF filled UHMWPE and ethylene-methyl methacrylate (EMMA) blend composites were prepared by gelation/crystallization method in solutions with xylene and decalin as solvents, respectively. Then DSC, SEM, WAXS, TGA and DMA were carried out to investigate systematically the effect of factors such as content of EMMA, CF and gamma irradiation on the properties of electrical, thermal, mechanical properties and morphology as well, and the mechanism of gamma ray irradiation was discussed in detail. Results demonstrated that crosslinking structure was formed in the composites after irradiation. PTC intensity of irradiated composites increased, which of composites with matrix ratio of UHMWPE to EMMA reached the maximum of 1010 at 500kGy. NTC effect was removed, and reproducibility was improved by irradiation.
Thirdly, self-heating property of UHMWPE-EMMA-CF composites was discussed in detail. It revealed that surface temperature of composites with matrix ratio of UHMWPE to EMMA of 1/6 was higher than that of composites with matrix ratio of 1/1 at the same concentration of CF and the set applied voltage. The self-heating property of composites was enhanced significantly by gamma ray irradiation. Surface temperature of irradiated composites with 500kGy and matrix ratio of 1/1 was 30℃higher than that of original composites at applied voltage of 20V. The optimal irradiation dose for composites with matrix ratio of 1/1,1/3 and 1/6 was 1000kGy,500kGy and 200kGy, respectively.
Finally, thermal volume expansion experiment of UHMWPE-based composites was conducted to explore the mechanism of PTC effect of composites. Results indicated that volume expansion was one of the important factors but not the only one for PTC effect. On the other hand, results of dielectric property of composites showed that resistivity and dielectric parameters of composites were depend strongly on temperature and frequency. Results of dielectric analysis were in good agreement with that of PTC effect in mechanism of electrical conductivity. Furthermore, it reflected the change of microstructure and the effect of gamma ray irradiation on the electrical properties.
本文首先利用凝胶结晶溶液方法制备了碳纤维(CF)和镀镍碳纤维(NiCF)填充的超高分子量聚乙烯(UHMWPE)导电聚合物复合材料,利用DSC, SEM, WAXS, DMA和凝胶含量测试等测试手段,研究了导电填料,伽马射线辐射交联,化学交联对材料导电及机械性能的影响。结果表明,NiCF比CF导电性更高,制备的材料的逾渗阈值低。伽马射线辐射交联能够提高材料的PTC效应,而化学交联能提高复合材料的导电性能和导电稳定性,并提高材料的机械性能。
采用UHMWPE和乙烯基甲基丙烯酸甲酯共聚物(EMMA)为聚合物基体,CF为导电填料,利用凝胶结晶溶液方法制备了UHMWPE-EMMA-CF三元导电聚合物复合材料。利用DSC, SEM, WAXS, TGA, DMA,凝胶含量等表征测试手段,系统讨论了EMMA含量,CF含量和伽马射线辐射交联等因素对其导电性,热学性能,形貌特征,机械性能等的影响,并探讨了伽马射线辐射交联机理。结果表明伽马射线辐射处理在聚合物中形成了交联结构。辐射后材料的PTC强度显著提高,基体比例UHMWPE/EMMA为1/1的样品经500kGy辐射后PTC强度达到1010。NTC效应消失,PTC效应重复性提高。
对UHMWPE-EMMA-CF导电聚合物复合材料的自发热性能进行了研究。结果表明,在相同的CF浓度和外加电压时,基体比例为1/6的样品的表面温度大于基体比例为1/1的。伽马射线辐射处理能显著提高材料的自发热性能。在外加电压为20V,基体比例为1/1的样品经500kGy辐射后其表面温度比未辐射样品提高约30℃。基体比例为1/1,1/3和1/6的样品对应的最佳伽马射线辐射剂量分别为1000kGy,500kGy和200kGy。
通过聚合物体积热膨胀实验对聚合物导电复合材料的PTC效应的机理进行了探讨。结果表明体积膨胀是PTC效应的重要影响因素。材料的介电性能分析表明,材料电阻率和介电常数对温度、频率具有强烈依赖性。介电测试结果与复合材料直流PTC性能的实验结论一致,并从微观角度反映了结构的变化及伽马射线对复合材料导电性等性能的影响。
Polymeric PTC composite is a novel functional material with importance both in research and application fields. This kind of composites can be widely applied in many fields such as self-regulating heaters, over-current protectors and sensors due to their advantages as thermoelectrical-switching characteristic, adjustable conductivity, light weight, corrosion resistance, low cost and simple processing technique. However, further research and improvement are necessary for the PTC materials in both theory and practical application respects, which focus on the conductive mechanism, enhance of PTC intensity, elimination of NTC phenomenon and improvement of stability and reproducibility at high temperature, low heat efficiency and so forth.
Firstly, carbon fiber (CF) or nickel-coated carbon fiber (Ni-CF) filled ultra-high-molecular weight polyethylene (UHMWPE) composites were prepared by gelation/crystallization method. DSC, SEM, WAXS, DMA and gel fraction measurements were employed to investigate the electrical and mechanical properties of composites with respect to the effect of content of fillers, gamma ray irradiation and chemical crosslink. Results demonstrated that lower percolation threshold value of composites was obtained by NiCF than CF due to its higher conductivity. PTC effect of composites was improved by gamma ray irradiation, while high and stable conductivity and mechanical properties were realized by means of chemical crosslink method.
Secondly, CF filled UHMWPE and ethylene-methyl methacrylate (EMMA) blend composites were prepared by gelation/crystallization method in solutions with xylene and decalin as solvents, respectively. Then DSC, SEM, WAXS, TGA and DMA were carried out to investigate systematically the effect of factors such as content of EMMA, CF and gamma irradiation on the properties of electrical, thermal, mechanical properties and morphology as well, and the mechanism of gamma ray irradiation was discussed in detail. Results demonstrated that crosslinking structure was formed in the composites after irradiation. PTC intensity of irradiated composites increased, which of composites with matrix ratio of UHMWPE to EMMA reached the maximum of 1010 at 500kGy. NTC effect was removed, and reproducibility was improved by irradiation.
Thirdly, self-heating property of UHMWPE-EMMA-CF composites was discussed in detail. It revealed that surface temperature of composites with matrix ratio of UHMWPE to EMMA of 1/6 was higher than that of composites with matrix ratio of 1/1 at the same concentration of CF and the set applied voltage. The self-heating property of composites was enhanced significantly by gamma ray irradiation. Surface temperature of irradiated composites with 500kGy and matrix ratio of 1/1 was 30℃higher than that of original composites at applied voltage of 20V. The optimal irradiation dose for composites with matrix ratio of 1/1,1/3 and 1/6 was 1000kGy,500kGy and 200kGy, respectively.
Finally, thermal volume expansion experiment of UHMWPE-based composites was conducted to explore the mechanism of PTC effect of composites. Results indicated that volume expansion was one of the important factors but not the only one for PTC effect. On the other hand, results of dielectric property of composites showed that resistivity and dielectric parameters of composites were depend strongly on temperature and frequency. Results of dielectric analysis were in good agreement with that of PTC effect in mechanism of electrical conductivity. Furthermore, it reflected the change of microstructure and the effect of gamma ray irradiation on the electrical properties.
引文
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