导电聚合物复合材料的制备与表征
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摘要
导电聚合物又称为导电高分子,是一类既具有高分子材料的性质又具有导电体性质的聚合物材料。导电聚合物具有质量轻、易成型、电导率范围宽且可调、成本低、结构多变、可分子设计等优点,其独特的电学、光学及磁学性质使得导电聚合物在电极材料、电磁屏蔽材料、隐身材料、防腐材料、传感器材料、电致变色材料等领域具有广泛的应用。在导电聚合物家族中,聚苯胺(PANI)、聚吡咯(PPy)因为具有环境稳定性好、掺杂电导率高、制备简单、原料易得等优点在科研与应用上都引起了人们的广泛关注,成为近年来材料领域的研发热点。然而两者因为具有π共轭刚性结构,其溶熔性及加工性均很差,这严重制约了PANI与PPy的实际应用。通过将导电聚合物与其它材料复合不仅可以显著改善导电聚合物的分散性与加工性,还可以赋予导电聚合物特殊的功能性,如光催化性质、吸波性质、气敏性质等。本论文以制备导电聚合物复合材料为目标,对导电聚合物复合材料的制备配方及实验工艺进行了优化选择,分别制备了SnO2/PANI复合材料、聚苯乙烯-聚(苯乙烯-苯乙烯磺酸钠)(PS-PSS)/PANI核壳复合材料、PPy/聚甲基丙烯酸甲酉(?)(PMMA)核壳复合材料、SnO2/PPy复合材料,分析了各影响因素对导电聚合物复合材料的形貌、尺寸、分散性与导电性等性质的影响。全文的主要内容如下：
(1)第三章首先通过溶胶-凝胶法以SnCl4和乙二醇为原料制备出了纳米SnO2,在此基础上采用微乳液法在SnO2表面包覆PANI制备SnO2/PANI纳米复合材料。反应过程中,SnCl4和乙二醇首先发生络合反应,并脱去HCl和H2O,使得各Sn原子通过-OCH2CH2O-连接,然后经煅烧得到SnO2。在微乳液体系中,苯胺盐增溶在十二烷基磺酸钠(SDS)胶束表面,SnO2被包覆在胶束内部,在氧化剂过硫酸铵(APS)的作用下苯胺被氧化得到SnO2/PANI纳米复合材料。对比实验发现,在SnO2的制备过程中,煅烧温度过高晶粒尺寸容易变大,煅烧温度过低,则SnO2结晶性差。煅烧时间对SnO2粒径和形貌的影响也类似。研究表明,500℃煅烧6h所制备的纳米SnO2呈球形,粒径大约为15nm,分散性和结晶性相对优异。复合材料中,SnO2很好的嵌插在疏松的PANI基体中。Sn02与PANI不是简单的物理共混,两者之间存在着一定的化学作用。PANI并没有影响Sn02的晶体结构,而Sn02在一定程度上阻碍了PANI分子链的规整性生长。Sn02/PANI纳米复合材料的电导率随Sn02用量的增大而减小。当Sn02与PANI的摩尔比控制在0.5：5时,复合材料的电导率可以达到1.75×10-1S/cm,与盐酸掺杂PANI的电导率已经非常接近。
(2)第四章首先采用分散聚合法制备了粒径均匀、分散性优异的PS微球并通过苯乙烯与苯乙烯磺酸钠(SSS)的共聚在PS微球表面引入磺酸基进行磺化形成磺化层(PSS)。再通过化学氧化聚合法在PS-PSS表面聚合得到粒径约为0.9μm的PS-PSS/PANI核壳结构复合材料。对比实验发现,当SSS用量为0.5g,即苯乙烯用量的5%时,所得PS-PSS微球的分散性优异。制备过程中,苯胺单体因为静电吸引作用富集到PS-PSS表面氧化成PANI壳层。PANI在PS-PSS表面的包覆随苯胺用量的提高经历了粒状突起、不完整包覆和完整包覆三个过程。当苯胺单体与PS-PSS的质量比为0.5：0.6时,PANI壳层包覆完整,其电导率达到2.11S/cm,基本接近于纯PANI的电导率。通过溶剂刻蚀法可以除去复合材料中的塑性内核得到PANI空心球。PANI空心球随着复合材料制备过程中苯胺用量的提高逐渐趋于完整。当苯胺单体与PS-PSS的质量比为0.5：0.6时,所得PANI空心球呈很好的球形,粒径为0.91μm,厚度大约为50nm,其电导率达到2.17S/cm。
(3)第五章采用微乳液法以十六烷基三甲基溴化铵(CTAB)为乳化剂、正戊醇为助乳化剂首先合成了单分散性优异的PPy纳米粒子。在此基础上,在含有PPy的胶束中进一步增溶甲基丙烯酸甲酯(MMA)单体,经聚合得到PMMA壳层。所制备复合材料呈明显的核壳结构,单分散性优异。通过对比发现,乳化剂浓度、氧化剂滴加速度、反应温度等条件均影响所制备材料的粒径和分散性。研究发现当CTAB用量为1.7g、正戊醇用量为1.0g,并采用缓慢滴加氧化剂低温聚合时所制备的PPy纳米粒子分散性好,粒径大约为50nm。通过调节MMA用量可以调节复合材料中PMMA壳层的厚度,但随着PMMA壳层厚度的增加复合材料的电导率减小。碘掺杂可以显著提高PPy的电导率,碘掺杂PPy纳米粒子的电导率达到10.425S/cm,碘掺杂PPv/PMMA的电导率为7.856×10-1S/cm。
(4)第六章结合水热法和反相微乳液法以SnCl4和尿素为原料在CTAB、正戊醇、正己烷组成的反相微乳液体系中成功制备了纳米SnO2,并在此基础上进一步合成了SnO2/PPy纳米复合材料。复合材料中纳米SnO2被包覆在疏松多孔的PPy基体中。XRD分析表明,复合材料中PPy的存在并没有改变SnO2的结晶,而SnO2阻碍了PPy分子链的规整排列。根据Debye-Scherrer公式计算SnO2和SnO2/PPy复合材料的粒径分别为3.9nm和3.6nm。FT-IR光谱和Uv-Vis光谱证明SnO2和PPy成功地复合在一起且两者之间存在着一定的相互作用。
Conductive polymers, also called as conductive macromolecules, are a type of materials possessing the properties both of macromolecules and conductors. Conductive polymers are lightweight, easy shaping, low cost, structure flexible, macromolecule designing and possess a wide range of controllable conductivities. Its special electrical, optical and magnetic properties give conductive polymers the wide applications in electrode materials, electromagnetic shielding materials, stealth materials, anti-corrosion materials, sensor materials, electrochromic materials and so on. In the family of conductive polymers, polyaniline(PANI) and polypyrrole(PPy) have attracted increasing attentions both in scientific researches and practical applications due to their good environmental stability, high doping conductivities, simple preparation and easy obtention of raw materials. The research of PANI and PPy has become as one of the hot spots in the research of materials. However, both of them possess rigid π-conjugated structures and therefore their solubility, fusibility, and processibility are bad. These defects seriously restrict the practical applications of PANI and PPy. To composite conductive polymers with other materials can not only significantly improves the solubility and processibility of conductive polymers, but also can endows conductive polymers with some special functions such as photocatalytic properties, wave absorbing properties and gas sensing properties. In this paper, to aim for the conductive polymer composites, we optimized the structure, recipes and experimental technology of conductive polymer composites and prepared polystyrene-poly(styrene-co-sodium4-styrenesulfonate)(PS-PSS)/PANI core-shell microparticles, SnO2/PANI nanocomposites, PPy/poly(methyl methacrylate)(PMMA) core-shell nanocomposites and SnO2/PPy nanocomposites. We analysed the influencing factors for the morphology, size, dispersity and conductivities of conductive polymer composites. The main contents could be summarized as follows:
In the third chapter, nanostructured SnO2was prepared via a sol-gel process of SnCl4. SnO2/PANI nanocomposites were prepared by microemulsion polymerization in which aniline was polymerized on the surface of SnO2nanoparticles. In the reaction process, complex reaction was occurred between SnCl4and ethylene glycol. Sn atoms were linked with each other through the-OCH2CH2O-group after HCl and H2O was removed. The products were calcined and SnO2nanoparticles were obtained. In the microemulsion system, aniline salt was dissolved in micelles of SDS, and SnO2nanoparticles were enwrapped by SDS micelles. In the presence of oxidant APS, aniline monomer was polymerized on the surface of SnO2nanoparticles and SnO2/PANI nanocomposites were obtained. Comparing with the results prepared with different conditions, we found that the size of SnO2nanoparticles became big at high calcined temperature. However, when the calcined temperature was low, the SnO2nanoparticles showed a bad crystallinity. Similar results were found when we studied the influence of calcined time on the morphology and size of SnO2nanoparticles. Results showed that calcined at500℃for6h was the optimum condition to get the monodisperse nanoscale SnO2particles. The diameter of SnO2nanoparticles prepared on the above condition was around15nm. In the composites the SnO2nanoparticles with a diameter of ca.15nm were embedded well in the porous PANI. The SnO2particles and PANI were successfully composited with each other and there was an interaction between them. The crystal structure of SnO2was not modified by PANI. However, the crystallization of PANI was hampered by the SnO2nanoparticles. Conductivity analysis showed that the conductivity of SnO2/PANI nanocomposites was between the conductivity of PANI and SnO2particles. With the decrease of n (SnO2):n (aniline), the conductivity of the nanocomposites was increased. When the molar ratio of SnO2to aniline was kept at0.5:5, the conductivity of SnO2/PANI nanocomposites was1.75×10-1S/cm, which was very close to the conductivity of PANI.
In the fourth chapter, the monodispersed PS microparticles were prepared by dispersion polymerization. Through the copolymerization of styrene and sodium4-styrenesulfonate (SSS) on the surface of PS, the PS particles was modified with negatively charged sulfonic groups(PSS). Then through the chemical oxidation method, aniline monomer was polymerized on the surface of PS-PSS particles and PS-PSS/PANI core-shell conductive composites with a diameter around0.9μm were obtained. Comparing with the results of composites prepared with different conditions, when SSS was5%of the amount of styrene, the PS-PSS particles were uniform and monodispersed. The growth process of PANI on the surface of PS-PSS particles was changing from protrusions, incomplete coating shell to complete coating shell. The shell of the composite particles was complete and continuous, when the ratio was [m(PS-PSS):m(aniline)=0.6:0.5]. The conductivity of the core-shell (PS-PSS)/PANI particles was2.11S/cm, which was very close to the conductivity value of pure PANI. The hollow PANI microspheres could be prepared by putting the composite particles into chloroform to extract the plastic core. When the ratio was [m(PS-PSS):m(aniline)=0.6:0.5], the hollow PANI microspheres possessed spherical shape with diameter around0.9μm and thickness around50nm. The conductivity of hollow PANI microspheres prepared in this paper was2.17S/cm.
In the fifth chapter, PPy core particles with good dispersity were prepared in a four-component microemulsion system, which was formed with surfactant cetyltrimethyl ammonium bromide (CTAB), cosurfactant n-pentanol, water and pyrrole. On the basis of PPy nanoparticles, methyl methacrylate monomer (MMA) was dissolved in micelles and polymerized on the surface of PPy nanoparticles to form the PMMA shell. The PPy/PMMA nanocomposites showed obvious core-shell structure with good dispersity. Comparing with the results of composites prepared with different conditions, we found that the reaction conditions such as the concentration of surfactant, the droping rate of oxidant, and the reaction temperature can influence the dispersity and size of the composites. It was found that when the using amount of CTAB was1.7g and n-pentanol1.0g with low oxidant dropping rate at low reaction temperature, the size of PPy nanoparticles was around50nm. The thickness of PMMA shell could be controlled by changing the using amount of MMA monomer. As the thickness of the PMMA shell increased, the conductivity of the composite particles decreased. Iodine could greatly improve the conductivity of PPy nanoparticles, when it was used as a dopping agent in the polymerization of PPy. The conductivity of doping PPy nanoparticles could reach to10.425S/cm. The PPy/PMMA nanocomposites, which were composed of a doping PPy core and a thin PMMA shell, could gain a conductivity of7.856×10-1S/cm.
In the sixth chapter, we combined the merits of reverse microemulsion and hydrothermal method and successfully synthesized SnO2nanoparticles. The typical quaternary microemulsion was formed with surfactant CTAB, cosurfactant n-pentanol, n-hexane, and water. SnCl4and urea was used as the starting material to synthesize SnO2nanoparticles. Then pyrrole monomer was polymerized in the microemulsion system to form SnO2/PPy nanocomposites. In the nanocomposites, SnO2nanoparticles were embedded well in the porous PPy. Results showed that the crystal structure of SnO2is not modified by PPy. However, the crystallization of PPy was hampered by the SnO2nanoparticles. The particle size of SnO2and SnO2/PPy was calculated by XRD as3.9and3.6nm, respectively. FT-IR and UV-vis spectra proved that SnO2was successfully enwrapped by PPy with an interaction between them.
(1)第三章首先通过溶胶-凝胶法以SnCl4和乙二醇为原料制备出了纳米SnO2,在此基础上采用微乳液法在SnO2表面包覆PANI制备SnO2/PANI纳米复合材料。反应过程中,SnCl4和乙二醇首先发生络合反应,并脱去HCl和H2O,使得各Sn原子通过-OCH2CH2O-连接,然后经煅烧得到SnO2。在微乳液体系中,苯胺盐增溶在十二烷基磺酸钠(SDS)胶束表面,SnO2被包覆在胶束内部,在氧化剂过硫酸铵(APS)的作用下苯胺被氧化得到SnO2/PANI纳米复合材料。对比实验发现,在SnO2的制备过程中,煅烧温度过高晶粒尺寸容易变大,煅烧温度过低,则SnO2结晶性差。煅烧时间对SnO2粒径和形貌的影响也类似。研究表明,500℃煅烧6h所制备的纳米SnO2呈球形,粒径大约为15nm,分散性和结晶性相对优异。复合材料中,SnO2很好的嵌插在疏松的PANI基体中。Sn02与PANI不是简单的物理共混,两者之间存在着一定的化学作用。PANI并没有影响Sn02的晶体结构,而Sn02在一定程度上阻碍了PANI分子链的规整性生长。Sn02/PANI纳米复合材料的电导率随Sn02用量的增大而减小。当Sn02与PANI的摩尔比控制在0.5：5时,复合材料的电导率可以达到1.75×10-1S/cm,与盐酸掺杂PANI的电导率已经非常接近。
(2)第四章首先采用分散聚合法制备了粒径均匀、分散性优异的PS微球并通过苯乙烯与苯乙烯磺酸钠(SSS)的共聚在PS微球表面引入磺酸基进行磺化形成磺化层(PSS)。再通过化学氧化聚合法在PS-PSS表面聚合得到粒径约为0.9μm的PS-PSS/PANI核壳结构复合材料。对比实验发现,当SSS用量为0.5g,即苯乙烯用量的5%时,所得PS-PSS微球的分散性优异。制备过程中,苯胺单体因为静电吸引作用富集到PS-PSS表面氧化成PANI壳层。PANI在PS-PSS表面的包覆随苯胺用量的提高经历了粒状突起、不完整包覆和完整包覆三个过程。当苯胺单体与PS-PSS的质量比为0.5：0.6时,PANI壳层包覆完整,其电导率达到2.11S/cm,基本接近于纯PANI的电导率。通过溶剂刻蚀法可以除去复合材料中的塑性内核得到PANI空心球。PANI空心球随着复合材料制备过程中苯胺用量的提高逐渐趋于完整。当苯胺单体与PS-PSS的质量比为0.5：0.6时,所得PANI空心球呈很好的球形,粒径为0.91μm,厚度大约为50nm,其电导率达到2.17S/cm。
(3)第五章采用微乳液法以十六烷基三甲基溴化铵(CTAB)为乳化剂、正戊醇为助乳化剂首先合成了单分散性优异的PPy纳米粒子。在此基础上,在含有PPy的胶束中进一步增溶甲基丙烯酸甲酯(MMA)单体,经聚合得到PMMA壳层。所制备复合材料呈明显的核壳结构,单分散性优异。通过对比发现,乳化剂浓度、氧化剂滴加速度、反应温度等条件均影响所制备材料的粒径和分散性。研究发现当CTAB用量为1.7g、正戊醇用量为1.0g,并采用缓慢滴加氧化剂低温聚合时所制备的PPy纳米粒子分散性好,粒径大约为50nm。通过调节MMA用量可以调节复合材料中PMMA壳层的厚度,但随着PMMA壳层厚度的增加复合材料的电导率减小。碘掺杂可以显著提高PPy的电导率,碘掺杂PPy纳米粒子的电导率达到10.425S/cm,碘掺杂PPv/PMMA的电导率为7.856×10-1S/cm。
(4)第六章结合水热法和反相微乳液法以SnCl4和尿素为原料在CTAB、正戊醇、正己烷组成的反相微乳液体系中成功制备了纳米SnO2,并在此基础上进一步合成了SnO2/PPy纳米复合材料。复合材料中纳米SnO2被包覆在疏松多孔的PPy基体中。XRD分析表明,复合材料中PPy的存在并没有改变SnO2的结晶,而SnO2阻碍了PPy分子链的规整排列。根据Debye-Scherrer公式计算SnO2和SnO2/PPy复合材料的粒径分别为3.9nm和3.6nm。FT-IR光谱和Uv-Vis光谱证明SnO2和PPy成功地复合在一起且两者之间存在着一定的相互作用。
Conductive polymers, also called as conductive macromolecules, are a type of materials possessing the properties both of macromolecules and conductors. Conductive polymers are lightweight, easy shaping, low cost, structure flexible, macromolecule designing and possess a wide range of controllable conductivities. Its special electrical, optical and magnetic properties give conductive polymers the wide applications in electrode materials, electromagnetic shielding materials, stealth materials, anti-corrosion materials, sensor materials, electrochromic materials and so on. In the family of conductive polymers, polyaniline(PANI) and polypyrrole(PPy) have attracted increasing attentions both in scientific researches and practical applications due to their good environmental stability, high doping conductivities, simple preparation and easy obtention of raw materials. The research of PANI and PPy has become as one of the hot spots in the research of materials. However, both of them possess rigid π-conjugated structures and therefore their solubility, fusibility, and processibility are bad. These defects seriously restrict the practical applications of PANI and PPy. To composite conductive polymers with other materials can not only significantly improves the solubility and processibility of conductive polymers, but also can endows conductive polymers with some special functions such as photocatalytic properties, wave absorbing properties and gas sensing properties. In this paper, to aim for the conductive polymer composites, we optimized the structure, recipes and experimental technology of conductive polymer composites and prepared polystyrene-poly(styrene-co-sodium4-styrenesulfonate)(PS-PSS)/PANI core-shell microparticles, SnO2/PANI nanocomposites, PPy/poly(methyl methacrylate)(PMMA) core-shell nanocomposites and SnO2/PPy nanocomposites. We analysed the influencing factors for the morphology, size, dispersity and conductivities of conductive polymer composites. The main contents could be summarized as follows:
In the third chapter, nanostructured SnO2was prepared via a sol-gel process of SnCl4. SnO2/PANI nanocomposites were prepared by microemulsion polymerization in which aniline was polymerized on the surface of SnO2nanoparticles. In the reaction process, complex reaction was occurred between SnCl4and ethylene glycol. Sn atoms were linked with each other through the-OCH2CH2O-group after HCl and H2O was removed. The products were calcined and SnO2nanoparticles were obtained. In the microemulsion system, aniline salt was dissolved in micelles of SDS, and SnO2nanoparticles were enwrapped by SDS micelles. In the presence of oxidant APS, aniline monomer was polymerized on the surface of SnO2nanoparticles and SnO2/PANI nanocomposites were obtained. Comparing with the results prepared with different conditions, we found that the size of SnO2nanoparticles became big at high calcined temperature. However, when the calcined temperature was low, the SnO2nanoparticles showed a bad crystallinity. Similar results were found when we studied the influence of calcined time on the morphology and size of SnO2nanoparticles. Results showed that calcined at500℃for6h was the optimum condition to get the monodisperse nanoscale SnO2particles. The diameter of SnO2nanoparticles prepared on the above condition was around15nm. In the composites the SnO2nanoparticles with a diameter of ca.15nm were embedded well in the porous PANI. The SnO2particles and PANI were successfully composited with each other and there was an interaction between them. The crystal structure of SnO2was not modified by PANI. However, the crystallization of PANI was hampered by the SnO2nanoparticles. Conductivity analysis showed that the conductivity of SnO2/PANI nanocomposites was between the conductivity of PANI and SnO2particles. With the decrease of n (SnO2):n (aniline), the conductivity of the nanocomposites was increased. When the molar ratio of SnO2to aniline was kept at0.5:5, the conductivity of SnO2/PANI nanocomposites was1.75×10-1S/cm, which was very close to the conductivity of PANI.
In the fourth chapter, the monodispersed PS microparticles were prepared by dispersion polymerization. Through the copolymerization of styrene and sodium4-styrenesulfonate (SSS) on the surface of PS, the PS particles was modified with negatively charged sulfonic groups(PSS). Then through the chemical oxidation method, aniline monomer was polymerized on the surface of PS-PSS particles and PS-PSS/PANI core-shell conductive composites with a diameter around0.9μm were obtained. Comparing with the results of composites prepared with different conditions, when SSS was5%of the amount of styrene, the PS-PSS particles were uniform and monodispersed. The growth process of PANI on the surface of PS-PSS particles was changing from protrusions, incomplete coating shell to complete coating shell. The shell of the composite particles was complete and continuous, when the ratio was [m(PS-PSS):m(aniline)=0.6:0.5]. The conductivity of the core-shell (PS-PSS)/PANI particles was2.11S/cm, which was very close to the conductivity value of pure PANI. The hollow PANI microspheres could be prepared by putting the composite particles into chloroform to extract the plastic core. When the ratio was [m(PS-PSS):m(aniline)=0.6:0.5], the hollow PANI microspheres possessed spherical shape with diameter around0.9μm and thickness around50nm. The conductivity of hollow PANI microspheres prepared in this paper was2.17S/cm.
In the fifth chapter, PPy core particles with good dispersity were prepared in a four-component microemulsion system, which was formed with surfactant cetyltrimethyl ammonium bromide (CTAB), cosurfactant n-pentanol, water and pyrrole. On the basis of PPy nanoparticles, methyl methacrylate monomer (MMA) was dissolved in micelles and polymerized on the surface of PPy nanoparticles to form the PMMA shell. The PPy/PMMA nanocomposites showed obvious core-shell structure with good dispersity. Comparing with the results of composites prepared with different conditions, we found that the reaction conditions such as the concentration of surfactant, the droping rate of oxidant, and the reaction temperature can influence the dispersity and size of the composites. It was found that when the using amount of CTAB was1.7g and n-pentanol1.0g with low oxidant dropping rate at low reaction temperature, the size of PPy nanoparticles was around50nm. The thickness of PMMA shell could be controlled by changing the using amount of MMA monomer. As the thickness of the PMMA shell increased, the conductivity of the composite particles decreased. Iodine could greatly improve the conductivity of PPy nanoparticles, when it was used as a dopping agent in the polymerization of PPy. The conductivity of doping PPy nanoparticles could reach to10.425S/cm. The PPy/PMMA nanocomposites, which were composed of a doping PPy core and a thin PMMA shell, could gain a conductivity of7.856×10-1S/cm.
In the sixth chapter, we combined the merits of reverse microemulsion and hydrothermal method and successfully synthesized SnO2nanoparticles. The typical quaternary microemulsion was formed with surfactant CTAB, cosurfactant n-pentanol, n-hexane, and water. SnCl4and urea was used as the starting material to synthesize SnO2nanoparticles. Then pyrrole monomer was polymerized in the microemulsion system to form SnO2/PPy nanocomposites. In the nanocomposites, SnO2nanoparticles were embedded well in the porous PPy. Results showed that the crystal structure of SnO2is not modified by PPy. However, the crystallization of PPy was hampered by the SnO2nanoparticles. The particle size of SnO2and SnO2/PPy was calculated by XRD as3.9and3.6nm, respectively. FT-IR and UV-vis spectra proved that SnO2was successfully enwrapped by PPy with an interaction between them.
引文
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