碳纳米管抗氧机理研究及其在聚乙烯树脂改性中的应用
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摘要
碳纳米管(CNT)超强的力学性能、极大的长径比、优异的化学和热稳定性、良好的导电性能以及独特的一维纳米结构,使其在聚烯烃/CNT复合材料中发挥了重要作用。聚烯烃/CNT复合材料潜在的巨大优势,使其成为近年来研究的热点。对聚烯烃/CNT复合材料的研究主要分为“认识研究”和“改造研究”。前者主要研究CNT对聚烯烃的增强效应及机理,以帮助更好地认识、优化材料性能；后者主要是指对CNT进行化学修饰改性以提高其在聚合物基体中分散性及相容性,达到增强或赋予材料新的性能的目的。
本文从这两方面出发,针对聚乙烯的热氧老化行为,考察了CNT对聚乙烯热氧降解行为的影响,探讨了其对聚乙烯热氧稳定化作用机理；为了提高CNT的抗氧能力以及其在聚乙烯基体中的分散性,设计合成了三大类受阻酚接枝的CNT,并研究了其对应的聚乙烯复合材料的性能。主要工作和研究结果如下：
(1)在100℃下对高密度聚乙烯材料进行热烘箱加速老化实验,采用固体核磁共振技术表征聚乙烯老化过程中三相结构及分子链段运动性的变化。研究表明,在氧化诱导期聚乙烯的聚集态结构变化不大,而在自动氧化期,聚乙烯结晶相含量明显增加,无定形相及界面相含量则相应减少。同时,聚乙烯结晶相及界面相中分子链段运动性随着老化程度的加深越来越弱,而无定形相分子链段运动性则得到加强。聚乙烯老化过程中聚集态结构的改变与分子量分布、羰基指数及材料拉伸性能的变化相一致。无定形相中断链反应使得分子量及链缠结密度降低、链段运动性增强,最终导致材料力学性能下降。
(2)选用不同维度的碳纳米填料制备了聚乙烯/碳纳米复合材料,采用差示扫描量热仪研究聚乙烯复合材料的等温及非等温结晶行为。等温结晶数据表明,结晶受成核控制,聚乙烯中纳米材料维度越低,结晶诱导期越长,结晶速率越慢。采用Avrami及Tobin模型对等温结晶行为进行分析,模型指数表明在一维及二维纳米材料存在下,聚乙烯晶体呈二维片晶生长；在零维纳米材料存在下,聚乙烯晶体呈三维球晶生长。与等温结晶相反,聚乙烯非等温结晶受扩散控制,低维度纳米碳材料促进聚乙烯结晶。分别采用Ozawa及Mo模型分析聚乙烯非等温结晶过程,结果表明Mo方程更适用于对聚乙烯非等温结晶行为的描述。
(3)通过氧化诱导实验对比研究了单壁碳纳米管(SWCNT)、多壁碳纳米管(MWCNT)以及羟基化多壁碳纳米管(MWCNT-OH)对聚乙烯热氧稳定性的影响。研究发现,CNT在聚乙烯热氧老化过程中表现出抗氧性能,能显著延长聚乙烯的氧化诱导期。根据聚乙烯氧化诱导期的长短,可得出三种CNT的抗氧能力顺序为：MWCNT-OH> MWCNT> SWCNT。进一步,通过电子自旋共振实验发现,CNT具有显著的自由基清除能力,且三种CNT自由基清除能力顺序与抗氧能力一致,表明CNT在聚乙烯中的抗氧行为遵循自由基清除机理。拉曼光谱分析侧面说明了CNT的自由基清除能力与其结构缺陷引入的酚基、醌基等反应性功能团有关。
(4)采用一种氨基硅烷偶联剂,通过两种合成途径(两步法和一步法),将小分子受阻酚(AO)接枝到MWCNT表面,得到两种功能化的CNT-AO-MWCNT-A和AO-MWCNT-B,并通过熔融共混法制备得到相应的聚乙烯/CNT复合材料。采用红外光谱、拉曼光谱、能谱分析等方法证实了受阻酚抗氧剂成功接枝到CNT表面。CNT的热重分析结果表明,相比于两步法获得的AO-MWCNT-A,一步法合成的AO-MWCNT-B表面受阻酚的接枝量更大,自由基清除能力也更强。对聚乙烯/CNT复合材料的研究表明,功能化后的CNT在聚乙烯中的分散性得到提高。与原始CNT相比,AO-MWCNT-A及AO-MWCNT-B分别使聚乙烯材料的氧化诱导温度进一步提高了11℃和28℃,氧化诱导时间(200℃下)延长了16.6mmin和71.1mmin,且对材料的力学增强效果更显著。抽提实验结果表明,受阻酚接枝到CNT表面后其耐溶剂抽提性比小分子受阻酚明显提高。无论是与原始MWCNT还是与受阻酚抗氧剂相比,受阻酚接枝的CNT在聚乙烯中均表现出更强的力学增强效应、更优异的抗氧性以及稳定性。
(5)设计合成了以丁二胺为核、丙烯酸为重复单元的一代(G1)和二代(G2)树枝状多醇,以G1和G2作为“桥梁分子”共价连接MWCNT与受阻酚抗氧剂,得到两种受阻酚接枝的CNT——MWCNT-G1-AO和MWCNT-G2-AO,通过熔融共混法制得相应的聚乙烯/CNT复合材料。对CNT的分析结果表明,G2比G1活性更高,更容易实现受阻酚的接枝,最终每克MWCNT-G1-AO及MWCNT-G2-AO上受阻酚的接枝量分别为0.159mmol和0.367mmol。由于MWCNT-G2-AO上受阻酚的接枝量更高,因此其对聚乙烯的热氧稳定效应更显著,相比于原始CNT, MWCNT-G2-AO可使聚乙烯复合材料的氧化诱导时间进一步延长93.6min。此外,抗氧剂的复配研究表明,MWCNT-G2-AO与工业亚磷酸酯抗氧剂(Irgafos168)有显著的协同抗氧效果,为受阻酚接枝的CNT的工业应用提供了思路。
(6)以提高CNT上受阻酚的接枝量为目的,选用合成工艺简单、活性较高的聚缩水甘油作为“桥梁分子”,通过在MWCNT表面引发缩水甘油单体开环聚合,得到超支化聚缩水甘油包覆的核壳型CNT,再通过酯化反应合成得到受阻酚接枝的CNT——MWCNT-HPG-AO。对MWCNT-HPG-AO的分析表明,其表面包覆了一层厚度约4nm的有机组分,含量高达85wt%,其中受阻酚接枝量为2.23mmol/g MWCNT.相比于硅烷偶联剂及树枝状多醇,超支化聚缩水甘油使得单位质量的MWCNT表面受阻酚接枝量提高了一个数量级。将本文所合成的所有受阻酚接枝的CNT分别与聚乙烯熔融共混,制备得到MWCNT质量分数相同的聚乙烯复合材料。聚乙烯复合材料的结构及热氧稳定性结果表明,MWCNT-HPG-AO在聚乙烯基体中具有优异的分散性,可实现单根分散,且聚乙烯/MWCNT-HPG-AO复合材料的氧化诱导时间最长,即MWCNT-HPG-AO的抗氧能力最强。对聚乙烯复合材料的氧化动力学的研究表明,MWCNT-HPG-AO可以显著提高复合材料的氧化活化能。
Nowadays, polyolefin/carbon nanotube (CNT) nanocomposites has aroused wide attention of researchers due to their prominently improved mechanical, thermal, optical and physic-chemical properties comparing with the pure or conventional filler-reinforced polyolefin. Generally, the researches are focused on two aspects:(a) the reinforced effect and mechanism of CNTs in polyolefin, which help us to understand and optimize the performance of the composites;(b) the chemical modification of the CNTs, which means to improve their dispersion state in the polymer matrix and thus achieve better physical properties of the composites.
Based on the two aspects, the thermal oxidative stability of polyethylene/CNT nanocomposites and the antioxidant mechanism of CNTs are first studied in this thesis. After that, three kinds of hindered phenol grafted CNTs are synthesized to achieve enhanced antioxidant ability and better dispersion state in the polymer matrix. The main work and results are as follows.
(1) The thermal oxidative degradation of high density polyethylene (HDPE) was investigated during oven aging at100℃.1H low-field solid-state nuclear magnetic resonance (NMR) was used to characterize the behavior of molecular chains and the changes in phase content of HDPE during aging. The prolongation of aging led to a progressive increase in the amount of the crystalline phase at the expense of the other two phases. A slight decrease in chain mobility of the crystalline phase and interphase was observed simultaneously. The results obtained from other traditional technical approaches are also discussed in the context of the molecular dynamics properties revealed by NMR. The reduction in molecular weight, in chain mobility and the increase in crystallinity during thermo-oxidation were the main factors which caused the loss of mechanical performance of HDPE.
(2) The isothermal and non-isothermal crystallization behavior of polyethylene containing various zero, one, and two dimensional (0-D,1-D, and2-D) carbon nanofillers were investigated by means of differential scanning calorimetry. For a given temperature, the isothermal crystallization rate got slower with the addition of lower dimensional carbon nanofillers. The values of Avrami and Tobin exponents indicated that the isothermal crystallization of polyethylene followed two-dimensional crystal growth in the presence of2-D/1-D carbon nanofillers, while exhibited three-dimensional heterogeneous crystal growth in the presence of0-D carbon nanofillers. Contrary to the isothermal study, the non-isothermal crystallization of polyethylene was accelerated in the presence of lower dimensional nanofillers. Ozawa and Mo methods were used to analyze the non-isothermal crystallization data. It was observed that only Mo approach could successfully describe the non-isothermal crystallization process of polyethylene/carbon nanocomposites.
(3) The influence of Single-walled carbon nanotubes (SWCNTs), multiple-walled carbon nanotubes (MWCNTs), and hydroxylated multiple-walled carbon nanotubes (MWCNTs-OH) on the thermal oxidative degradation of polyethylene was studied respectively. The thermal oxidative stability of polyethylene was enhanced with the addition of CNTs. Based on the oxidation induction experiments, it was found that the antioxidant capacity of the CNTs was in the following order:MWCNTs-OH> MWCNTs> SWCNTs. The antioxidant ability and mechanism of CNTs were further examined by electron spin resonance spectra and Raman spectra. It was observed that the antioxidant behavior of CNTs obeys a free radical scavenging mechanism. The difference in their defect concentration was one of the factors which caused different antioxidant capacity between these CNTs.
(4) To improve the antioxidant ability and dispersion state of CNTs in the polymer matrix, a hindered phenolic antioxidant (AO) has been covalently grafted onto the surface of MWCNTs using a silane coupling agent. Two contrasting routes, two-step functionalization and one-step functionalization of MWCNTs, were developed. The corresponding polyethylene/MWCNT composites were prepared by melt blending. Fourier transform infrared spectroscopy, energy dispersive X-ray spectroscopy, thermal gravimetric analysis, transmission electron microscopy, and Raman spectroscopy confirmed the successful functionalization of MWCNTs. Electron spin resonance spectra revealed that the free radical scavenging activity of MWCNTs was greatly increased after functionalization. The resultant MWCNTs exhibited improved dispersion and antioxidant efficiency in the polyethylene matrix. Compared with the two-step functionalized MWCNTs, the one-step functionalized MWCNTs were more efficient in preventing polyethylene from thermal oxidative degradation.
(5) The first and second generation of dendritic polyols (G1and G2) with butanediamine as core and acrylic acid as repeating unit are synthesized and used as linkage to covalently connect MWCNTs and AO. The resultant CNTs (MWCNTs-G1-AO and MWCNTs-G2-AO) and corresponding polyethylene/CNT nanocomposites were prepared. It was found that G2are more efficient in grafting AO than Gl. Due to a higher loading of antioxidant groups, the antioxidant ability of MWCNTs-G2-AO are stronger than MWCNTs-G1-AO. Comparing with the pristine CNTs, MWCNTs-G2-AO can further extent the oxidation induction time (200℃) of the polyethylene by93.6min. Furthermore, it was found that there is a significant antioxidant synergy between MWCNTs-G2-AO and Irgafos168.
(6) To further improve the loading of AO on the surface of the CNTs, a hyperbranched linkage was proposed. Firstly, the hyperbranched polyglycerol was grown from the surface of MWCNTs by ring-opening polymerization. After that, AO was grafted onto the MWCNTs through esterification. It showed that the obtained MWCNTs-HPG-AO were coated with an organic layer of about4nm. The result indicated that the loading of AO was2.23mmol for per gram MWCNTs, which increased about an order of magnitude comparing with CNTs functionalized through other methods. Polyethylene nanocomposites incorporated with different kinds of functionalized CNTs were prepared respectively. The MWCNTs-HPG-AO were separately dispersed in the polyethylene. Among all the nanocomposites, polyethylene/MWCNT-HPG-AO nanocopmosite was the most stable during thermal oxidation. It showed that the oxidation activation energy of polyethylene was improved with the addition of MWCNTs-HPG-AO.
本文从这两方面出发,针对聚乙烯的热氧老化行为,考察了CNT对聚乙烯热氧降解行为的影响,探讨了其对聚乙烯热氧稳定化作用机理；为了提高CNT的抗氧能力以及其在聚乙烯基体中的分散性,设计合成了三大类受阻酚接枝的CNT,并研究了其对应的聚乙烯复合材料的性能。主要工作和研究结果如下：
(1)在100℃下对高密度聚乙烯材料进行热烘箱加速老化实验,采用固体核磁共振技术表征聚乙烯老化过程中三相结构及分子链段运动性的变化。研究表明,在氧化诱导期聚乙烯的聚集态结构变化不大,而在自动氧化期,聚乙烯结晶相含量明显增加,无定形相及界面相含量则相应减少。同时,聚乙烯结晶相及界面相中分子链段运动性随着老化程度的加深越来越弱,而无定形相分子链段运动性则得到加强。聚乙烯老化过程中聚集态结构的改变与分子量分布、羰基指数及材料拉伸性能的变化相一致。无定形相中断链反应使得分子量及链缠结密度降低、链段运动性增强,最终导致材料力学性能下降。
(2)选用不同维度的碳纳米填料制备了聚乙烯/碳纳米复合材料,采用差示扫描量热仪研究聚乙烯复合材料的等温及非等温结晶行为。等温结晶数据表明,结晶受成核控制,聚乙烯中纳米材料维度越低,结晶诱导期越长,结晶速率越慢。采用Avrami及Tobin模型对等温结晶行为进行分析,模型指数表明在一维及二维纳米材料存在下,聚乙烯晶体呈二维片晶生长；在零维纳米材料存在下,聚乙烯晶体呈三维球晶生长。与等温结晶相反,聚乙烯非等温结晶受扩散控制,低维度纳米碳材料促进聚乙烯结晶。分别采用Ozawa及Mo模型分析聚乙烯非等温结晶过程,结果表明Mo方程更适用于对聚乙烯非等温结晶行为的描述。
(3)通过氧化诱导实验对比研究了单壁碳纳米管(SWCNT)、多壁碳纳米管(MWCNT)以及羟基化多壁碳纳米管(MWCNT-OH)对聚乙烯热氧稳定性的影响。研究发现,CNT在聚乙烯热氧老化过程中表现出抗氧性能,能显著延长聚乙烯的氧化诱导期。根据聚乙烯氧化诱导期的长短,可得出三种CNT的抗氧能力顺序为：MWCNT-OH> MWCNT> SWCNT。进一步,通过电子自旋共振实验发现,CNT具有显著的自由基清除能力,且三种CNT自由基清除能力顺序与抗氧能力一致,表明CNT在聚乙烯中的抗氧行为遵循自由基清除机理。拉曼光谱分析侧面说明了CNT的自由基清除能力与其结构缺陷引入的酚基、醌基等反应性功能团有关。
(4)采用一种氨基硅烷偶联剂,通过两种合成途径(两步法和一步法),将小分子受阻酚(AO)接枝到MWCNT表面,得到两种功能化的CNT-AO-MWCNT-A和AO-MWCNT-B,并通过熔融共混法制备得到相应的聚乙烯/CNT复合材料。采用红外光谱、拉曼光谱、能谱分析等方法证实了受阻酚抗氧剂成功接枝到CNT表面。CNT的热重分析结果表明,相比于两步法获得的AO-MWCNT-A,一步法合成的AO-MWCNT-B表面受阻酚的接枝量更大,自由基清除能力也更强。对聚乙烯/CNT复合材料的研究表明,功能化后的CNT在聚乙烯中的分散性得到提高。与原始CNT相比,AO-MWCNT-A及AO-MWCNT-B分别使聚乙烯材料的氧化诱导温度进一步提高了11℃和28℃,氧化诱导时间(200℃下)延长了16.6mmin和71.1mmin,且对材料的力学增强效果更显著。抽提实验结果表明,受阻酚接枝到CNT表面后其耐溶剂抽提性比小分子受阻酚明显提高。无论是与原始MWCNT还是与受阻酚抗氧剂相比,受阻酚接枝的CNT在聚乙烯中均表现出更强的力学增强效应、更优异的抗氧性以及稳定性。
(5)设计合成了以丁二胺为核、丙烯酸为重复单元的一代(G1)和二代(G2)树枝状多醇,以G1和G2作为“桥梁分子”共价连接MWCNT与受阻酚抗氧剂,得到两种受阻酚接枝的CNT——MWCNT-G1-AO和MWCNT-G2-AO,通过熔融共混法制得相应的聚乙烯/CNT复合材料。对CNT的分析结果表明,G2比G1活性更高,更容易实现受阻酚的接枝,最终每克MWCNT-G1-AO及MWCNT-G2-AO上受阻酚的接枝量分别为0.159mmol和0.367mmol。由于MWCNT-G2-AO上受阻酚的接枝量更高,因此其对聚乙烯的热氧稳定效应更显著,相比于原始CNT, MWCNT-G2-AO可使聚乙烯复合材料的氧化诱导时间进一步延长93.6min。此外,抗氧剂的复配研究表明,MWCNT-G2-AO与工业亚磷酸酯抗氧剂(Irgafos168)有显著的协同抗氧效果,为受阻酚接枝的CNT的工业应用提供了思路。
(6)以提高CNT上受阻酚的接枝量为目的,选用合成工艺简单、活性较高的聚缩水甘油作为“桥梁分子”,通过在MWCNT表面引发缩水甘油单体开环聚合,得到超支化聚缩水甘油包覆的核壳型CNT,再通过酯化反应合成得到受阻酚接枝的CNT——MWCNT-HPG-AO。对MWCNT-HPG-AO的分析表明,其表面包覆了一层厚度约4nm的有机组分,含量高达85wt%,其中受阻酚接枝量为2.23mmol/g MWCNT.相比于硅烷偶联剂及树枝状多醇,超支化聚缩水甘油使得单位质量的MWCNT表面受阻酚接枝量提高了一个数量级。将本文所合成的所有受阻酚接枝的CNT分别与聚乙烯熔融共混,制备得到MWCNT质量分数相同的聚乙烯复合材料。聚乙烯复合材料的结构及热氧稳定性结果表明,MWCNT-HPG-AO在聚乙烯基体中具有优异的分散性,可实现单根分散,且聚乙烯/MWCNT-HPG-AO复合材料的氧化诱导时间最长,即MWCNT-HPG-AO的抗氧能力最强。对聚乙烯复合材料的氧化动力学的研究表明,MWCNT-HPG-AO可以显著提高复合材料的氧化活化能。
Nowadays, polyolefin/carbon nanotube (CNT) nanocomposites has aroused wide attention of researchers due to their prominently improved mechanical, thermal, optical and physic-chemical properties comparing with the pure or conventional filler-reinforced polyolefin. Generally, the researches are focused on two aspects:(a) the reinforced effect and mechanism of CNTs in polyolefin, which help us to understand and optimize the performance of the composites;(b) the chemical modification of the CNTs, which means to improve their dispersion state in the polymer matrix and thus achieve better physical properties of the composites.
Based on the two aspects, the thermal oxidative stability of polyethylene/CNT nanocomposites and the antioxidant mechanism of CNTs are first studied in this thesis. After that, three kinds of hindered phenol grafted CNTs are synthesized to achieve enhanced antioxidant ability and better dispersion state in the polymer matrix. The main work and results are as follows.
(1) The thermal oxidative degradation of high density polyethylene (HDPE) was investigated during oven aging at100℃.1H low-field solid-state nuclear magnetic resonance (NMR) was used to characterize the behavior of molecular chains and the changes in phase content of HDPE during aging. The prolongation of aging led to a progressive increase in the amount of the crystalline phase at the expense of the other two phases. A slight decrease in chain mobility of the crystalline phase and interphase was observed simultaneously. The results obtained from other traditional technical approaches are also discussed in the context of the molecular dynamics properties revealed by NMR. The reduction in molecular weight, in chain mobility and the increase in crystallinity during thermo-oxidation were the main factors which caused the loss of mechanical performance of HDPE.
(2) The isothermal and non-isothermal crystallization behavior of polyethylene containing various zero, one, and two dimensional (0-D,1-D, and2-D) carbon nanofillers were investigated by means of differential scanning calorimetry. For a given temperature, the isothermal crystallization rate got slower with the addition of lower dimensional carbon nanofillers. The values of Avrami and Tobin exponents indicated that the isothermal crystallization of polyethylene followed two-dimensional crystal growth in the presence of2-D/1-D carbon nanofillers, while exhibited three-dimensional heterogeneous crystal growth in the presence of0-D carbon nanofillers. Contrary to the isothermal study, the non-isothermal crystallization of polyethylene was accelerated in the presence of lower dimensional nanofillers. Ozawa and Mo methods were used to analyze the non-isothermal crystallization data. It was observed that only Mo approach could successfully describe the non-isothermal crystallization process of polyethylene/carbon nanocomposites.
(3) The influence of Single-walled carbon nanotubes (SWCNTs), multiple-walled carbon nanotubes (MWCNTs), and hydroxylated multiple-walled carbon nanotubes (MWCNTs-OH) on the thermal oxidative degradation of polyethylene was studied respectively. The thermal oxidative stability of polyethylene was enhanced with the addition of CNTs. Based on the oxidation induction experiments, it was found that the antioxidant capacity of the CNTs was in the following order:MWCNTs-OH> MWCNTs> SWCNTs. The antioxidant ability and mechanism of CNTs were further examined by electron spin resonance spectra and Raman spectra. It was observed that the antioxidant behavior of CNTs obeys a free radical scavenging mechanism. The difference in their defect concentration was one of the factors which caused different antioxidant capacity between these CNTs.
(4) To improve the antioxidant ability and dispersion state of CNTs in the polymer matrix, a hindered phenolic antioxidant (AO) has been covalently grafted onto the surface of MWCNTs using a silane coupling agent. Two contrasting routes, two-step functionalization and one-step functionalization of MWCNTs, were developed. The corresponding polyethylene/MWCNT composites were prepared by melt blending. Fourier transform infrared spectroscopy, energy dispersive X-ray spectroscopy, thermal gravimetric analysis, transmission electron microscopy, and Raman spectroscopy confirmed the successful functionalization of MWCNTs. Electron spin resonance spectra revealed that the free radical scavenging activity of MWCNTs was greatly increased after functionalization. The resultant MWCNTs exhibited improved dispersion and antioxidant efficiency in the polyethylene matrix. Compared with the two-step functionalized MWCNTs, the one-step functionalized MWCNTs were more efficient in preventing polyethylene from thermal oxidative degradation.
(5) The first and second generation of dendritic polyols (G1and G2) with butanediamine as core and acrylic acid as repeating unit are synthesized and used as linkage to covalently connect MWCNTs and AO. The resultant CNTs (MWCNTs-G1-AO and MWCNTs-G2-AO) and corresponding polyethylene/CNT nanocomposites were prepared. It was found that G2are more efficient in grafting AO than Gl. Due to a higher loading of antioxidant groups, the antioxidant ability of MWCNTs-G2-AO are stronger than MWCNTs-G1-AO. Comparing with the pristine CNTs, MWCNTs-G2-AO can further extent the oxidation induction time (200℃) of the polyethylene by93.6min. Furthermore, it was found that there is a significant antioxidant synergy between MWCNTs-G2-AO and Irgafos168.
(6) To further improve the loading of AO on the surface of the CNTs, a hyperbranched linkage was proposed. Firstly, the hyperbranched polyglycerol was grown from the surface of MWCNTs by ring-opening polymerization. After that, AO was grafted onto the MWCNTs through esterification. It showed that the obtained MWCNTs-HPG-AO were coated with an organic layer of about4nm. The result indicated that the loading of AO was2.23mmol for per gram MWCNTs, which increased about an order of magnitude comparing with CNTs functionalized through other methods. Polyethylene nanocomposites incorporated with different kinds of functionalized CNTs were prepared respectively. The MWCNTs-HPG-AO were separately dispersed in the polyethylene. Among all the nanocomposites, polyethylene/MWCNT-HPG-AO nanocopmosite was the most stable during thermal oxidation. It showed that the oxidation activation energy of polyethylene was improved with the addition of MWCNTs-HPG-AO.
引文
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