织物表面金属/导电高分子复合层的构建和性能研究
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摘要
聚苯胺(PANI)因其单体价格便宜、制备条件简单以及较高的电导率和良好的环境稳定性,而成为倍受青睐的导电高分子材料。然而聚苯胺虽然具有较大的电损耗性能,但其电导率与金属相比还具有一定的差距,为了提高材料的导电性能以及拓宽其他附加功能,以满足人们对抗静电和防电磁辐射等特殊要求的日益提高,常将聚苯胺导电材料与金属相结合以制备出具有更高导电性能的新型复合材料。本论文采用化学与电化学两种方式在预制聚苯胺膜的织物表面沉积金属粒子构建由导电高分子与金属组成的导电网络。
首先,着重对聚苯胺复合织物化学镀前处理条件包括聚苯胺膜制备条件、敏化剂浓度、敏化温度、活化剂浓度和活化温度等,对铜/聚苯胺复合织物导电性能的影响进行了系统研究,并得出最佳的前处理条件：SnCl2浓度为15g/L,温度为35℃；AgNO3浓度为2.0g/L,温度为35℃。同时,通过原子力显微镜(AFM)、电感耦合等离子体原子发射光谱仪(ICP)和X射线电子能谱分析(XPS)对活化后聚苯胺纤维进行了结构分析和形貌观察。
其次,利用超声波辅助化学镀工艺,在聚苯胺表面进行金属沉积,将化学镀反应控制在：基质吸附单体浓度1.0mol/L,氧化剂浓度为0.5mol/L, CuSO4浓度为0.5g/L,酒石酸钾钠浓度为30g/L, NaOH浓度为6g/L,还原剂浓度为24ml/L,化学镀时间为15min,温度为45℃,可制备具有良好导电、耐腐蚀性能的聚苯胺-金属复合织物。XRD分析表明所得金属层为面心立方结构,粒径为16.05nnm左右。
最后,采用循环伏安法与线性扫描伏安法,研究了聚苯胺复合织物作为电极进行电沉积的过程,对比不同电流下电沉积金属铜后织物的增重率及导电性能,并采用X射线衍射光谱(XRD)、扫描电镜(SEM)及能谱仪(EDS)等方法对织物进行了表征。结果发现,CuSO4浓度为0.8mol/L, Na2SO4浓度为0.4mol/L,柠檬酸钠浓度为0.06mol/L,电流密度为0.08A/cm2。经过SEM、EDS及XRD分析,织物表面生长了大量金属颗粒,且金属具有良好的晶形,粒径大约为38nm左右。
Polyaniline (PANI) is one of the most investigated conducting polymers (CP). It has been frequently studied due to its low cost, ease in preparation, good environmental stabilities, and high conductivity. Though, PANI has fine electrical dissipation, its conductivity is relative lower than metals. In order to enhance materials'conductivity and expand other functions, the polyaniline is usually combined with metal nanoparticles to prepare novel composite materials which have higher conductivity. So these new composite materials can satisfy people's higher electromagnetic interference shielding and antistatic requirements. In this paper, the metal particles were deposited on the surface of pre-PANI fabric by two methods of chemical and electrochemical, in order to form conductive network with the conductive polymer and metal.
Firstly, the basic properties of PANI films on PET fabric surface in pre-plating conditions were investigated. On base of the experimental data, the reaction parameters including concentration of SnCl2 and AgNO3, sensitization temperature, activation temperature which influence the effect of electroless were studied in detail. The optimum conditions for preparing composite PET fabrics were as follows:the concentration of SnCl2 and AgNO3 were 15g/L and 2.0g/L, temperature of sensitization and activation were 35℃and 35℃. Otherwise, the effects of pre-plating conditions on conductivity and structure of polyaniline deposited on fabric surface were also investigated in detail by AFM, XPS and ICP.
Secondly, to improve the performance of composite conducting fabric, electroless plating was used during depositing copper uniformly with ultrasonic. The effects of concentration of major salt, reducing agent, complexing agent, sodium hydroxide and substrate, time, temperature on the square resistance, the rate of metal deposition and fastness were discussed. The appropriate conditions of electroless plating were obtained, which were CuSO4 5g/L, potassium sodium tartrate 30g/L, sodium hydroxide 6g/L, reducing agent 24ml/L, reaction time within 15min, temperature keeping 45℃. It can be prepared with good electrical conductivity, corrosion resistance of the Metal/Polyaniline Composite Fabrics. XRD result indicated metal layer from face-centered cubic structure, particle size of about 16.05nm.
Finally, polyaniline conducting fabrics is used as electrodes to electrodeposite metal with cyclic voltammetry and Linear Scan Voltammetry. Composite fabrics, electrodeposited metal in different currents, were compared in the weight gain rate and surface resistance. The properties of the samples were characterized by X-ray powder diffraction (XRD), SEM, EDS. The results show that the optimum conditions for preparing composite fabric by electrodepositing copper as follows:CUSO4 concentration of 0.8mol/L, Na2SO4 concentration of 0.4mol/L, sodium citrate concentration of 0.06mol/L, current density 0.08A/cm2. On the surface of fabric, the growth of a large metal particles, and the metal has a good shape, the size is about 38nm.
首先,着重对聚苯胺复合织物化学镀前处理条件包括聚苯胺膜制备条件、敏化剂浓度、敏化温度、活化剂浓度和活化温度等,对铜/聚苯胺复合织物导电性能的影响进行了系统研究,并得出最佳的前处理条件：SnCl2浓度为15g/L,温度为35℃；AgNO3浓度为2.0g/L,温度为35℃。同时,通过原子力显微镜(AFM)、电感耦合等离子体原子发射光谱仪(ICP)和X射线电子能谱分析(XPS)对活化后聚苯胺纤维进行了结构分析和形貌观察。
其次,利用超声波辅助化学镀工艺,在聚苯胺表面进行金属沉积,将化学镀反应控制在：基质吸附单体浓度1.0mol/L,氧化剂浓度为0.5mol/L, CuSO4浓度为0.5g/L,酒石酸钾钠浓度为30g/L, NaOH浓度为6g/L,还原剂浓度为24ml/L,化学镀时间为15min,温度为45℃,可制备具有良好导电、耐腐蚀性能的聚苯胺-金属复合织物。XRD分析表明所得金属层为面心立方结构,粒径为16.05nnm左右。
最后,采用循环伏安法与线性扫描伏安法,研究了聚苯胺复合织物作为电极进行电沉积的过程,对比不同电流下电沉积金属铜后织物的增重率及导电性能,并采用X射线衍射光谱(XRD)、扫描电镜(SEM)及能谱仪(EDS)等方法对织物进行了表征。结果发现,CuSO4浓度为0.8mol/L, Na2SO4浓度为0.4mol/L,柠檬酸钠浓度为0.06mol/L,电流密度为0.08A/cm2。经过SEM、EDS及XRD分析,织物表面生长了大量金属颗粒,且金属具有良好的晶形,粒径大约为38nm左右。
Polyaniline (PANI) is one of the most investigated conducting polymers (CP). It has been frequently studied due to its low cost, ease in preparation, good environmental stabilities, and high conductivity. Though, PANI has fine electrical dissipation, its conductivity is relative lower than metals. In order to enhance materials'conductivity and expand other functions, the polyaniline is usually combined with metal nanoparticles to prepare novel composite materials which have higher conductivity. So these new composite materials can satisfy people's higher electromagnetic interference shielding and antistatic requirements. In this paper, the metal particles were deposited on the surface of pre-PANI fabric by two methods of chemical and electrochemical, in order to form conductive network with the conductive polymer and metal.
Firstly, the basic properties of PANI films on PET fabric surface in pre-plating conditions were investigated. On base of the experimental data, the reaction parameters including concentration of SnCl2 and AgNO3, sensitization temperature, activation temperature which influence the effect of electroless were studied in detail. The optimum conditions for preparing composite PET fabrics were as follows:the concentration of SnCl2 and AgNO3 were 15g/L and 2.0g/L, temperature of sensitization and activation were 35℃and 35℃. Otherwise, the effects of pre-plating conditions on conductivity and structure of polyaniline deposited on fabric surface were also investigated in detail by AFM, XPS and ICP.
Secondly, to improve the performance of composite conducting fabric, electroless plating was used during depositing copper uniformly with ultrasonic. The effects of concentration of major salt, reducing agent, complexing agent, sodium hydroxide and substrate, time, temperature on the square resistance, the rate of metal deposition and fastness were discussed. The appropriate conditions of electroless plating were obtained, which were CuSO4 5g/L, potassium sodium tartrate 30g/L, sodium hydroxide 6g/L, reducing agent 24ml/L, reaction time within 15min, temperature keeping 45℃. It can be prepared with good electrical conductivity, corrosion resistance of the Metal/Polyaniline Composite Fabrics. XRD result indicated metal layer from face-centered cubic structure, particle size of about 16.05nm.
Finally, polyaniline conducting fabrics is used as electrodes to electrodeposite metal with cyclic voltammetry and Linear Scan Voltammetry. Composite fabrics, electrodeposited metal in different currents, were compared in the weight gain rate and surface resistance. The properties of the samples were characterized by X-ray powder diffraction (XRD), SEM, EDS. The results show that the optimum conditions for preparing composite fabric by electrodepositing copper as follows:CUSO4 concentration of 0.8mol/L, Na2SO4 concentration of 0.4mol/L, sodium citrate concentration of 0.06mol/L, current density 0.08A/cm2. On the surface of fabric, the growth of a large metal particles, and the metal has a good shape, the size is about 38nm.
引文
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