聚苯胺和导电银纳米结构的形貌控制制备
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摘要
随着社会的快速发展,传统的导电材料无法满足在伸缩的情况下保持电性能不变的功能,目前亟需开发柔性导体来满足科技的需求。柔性导体的制备包括导电填料的制备和加工工艺,导电填料是柔性导体的关键材料,低维导电纳米结构因其具有巨大的比表面积、量子效应、比传统材料具有更好的光电、磁学、催化、传感等性能,在纳米光电器件、传感器、纳米生物技术、能量存储及转换等领域具有极其重要的作用。聚苯胺有掺杂/脱掺杂质子可调控性、环境稳定性以及合成简便、原料易得等优点,将纳米技术引入导电聚苯胺的合成工艺中,可以使其集导电性和纳米结构功能于一体,能极大地改善导电聚苯胺的加工性,聚苯胺纳米管具有空心结构,质轻,比表面积大等优点,聚苯胺纳米片具有覆盖面积大,渗滤阀值低的优点,而螺旋型聚苯胺有特殊的形貌,它们作为导电填料将在柔性导体中得到潜在的应用。纳米银具有高的电导率,抗氧化性强,电性能稳定,独特的物理和化学性质,尤其银纳米棒具有两端裸露,侧面包覆PVP的特点,为连接组装提供了条件,在柔性导体中应用提供了理论基础,但特定形貌的银纳米棒大规模可控制备是一个难点,其形成机理和调控仍然存在挑战。本论文制备了聚苯胺纳米结构(管、片、螺旋)和银纳米棒,解决了聚苯胺纳米结构控制和银纳米棒大规模制备的问题,阐明了它们的形成机理。具体内容如下：
(1)本论文围绕聚苯胺纳米结构制备方法中存在的问题展开,研究了简单、有效构建多种形貌聚苯胺纳米结构的方法,提出了其形成机理。首次调控碳酸盐简便地合成出聚苯胺纳米结构,机理为碳酸盐与聚苯胺原位聚合产生的硫酸反应生成气泡,通过控制添加的碳酸盐种类和用量来控制气泡量,在无碳酸盐或用量较少时,能得到表面带有小棒的聚苯胺纳米管,当碳酸盐用量一定时,能得到表面光滑的聚苯胺纳米管,当碳酸盐用量较多时,由于产生气泡的微扰作用破坏了软模板胶束,得到聚苯胺纳米片。进一步添加不放出气泡的弱酸盐或调控体系的pH值,对聚苯胺纳米管影响较小,证明了气泡调控聚苯胺纳米结构的形成机理。
(2)聚苯胺螺旋因其具有导电性和可伸缩性的潜能,在柔性导体中有着潜在的应用。但是先前在手性樟脑磺酸的作用下,制备网状结构螺旋型聚苯胺,非可分散的,在一维单根器件上的应用受到限制。本文采用界面聚合的方法,有效降低聚苯胺的二次生长速度,由于手性聚苯胺低聚物为水溶性的,能溶解在上层水相中,不会沉淀且能有效降低其聚集作用,生成可分散的聚苯胺螺旋结构。形成的机理是：手性樟脑磺酸与苯胺通过N-H氢键作用,同时手性碳的诱导使苯胺能有序地在聚苯胺低聚物同一侧面结合而形成了螺旋结构。邻氨基酚为苯胺的衍生物,带有活泼羟基,可以通过氧化聚合得到电活性高分子,为了能制备可伸缩的螺旋结构,先制备出聚邻氨基酚螺旋,使螺旋结构带有改性的羟基,为进一步改性引入热敏、气敏或光敏高分子材料提供条件,使其成为具有可伸缩性能应用到柔性导体中。在聚乙二醇的作用下,制备螺旋型聚邻氨基酚。其形成机理归结为聚乙二醇长链的柔顺性,邻氨基酚的刚性结构苯环在长链柔性分子上的堆积,形成微米螺旋结构。最后,对聚苯胺螺旋和聚邻氨基酚螺旋的FT-IR、UV-Vis、能谱分析和电性能等进行了表征。
(3)常规使用乙二醇作为溶剂和还原剂,PVP作为盖帽剂,将AgNO3还原制取银纳米捧,AgNO3的浓度不能超过0.10M。本论文发现,在银晶种作用下,控制AgNO3和PVP的滴加速度,AgNO3的浓度可高达0.50M,制备出长度为2～15μm,直径为200～880nm的银纳米棒。研究了高浓度制备银纳米棒的影响因素,得到最佳的合成条件为：银晶种的浓度为6.54～9.81mM,AgNO3和PVP的滴加速度为0.30～0.43mL/min,PVP/AgNO3的摩尔比为1.1～1.4,搅拌速度为350rpm,反应温度为160℃。形成机理是：溶液中存在一定浓度和形貌的银晶种提供更多的表面积,能够增加被还原的银原子在银晶种上的生长速度,使得银结晶生长速度和溶液中高的硝酸银还原速度相匹配,由于PVP选择性覆盖在[100]面,银原子在[111]面沉积生长,能高效生成银纳米棒。对反应进行了放大,通过空间效应和速度匹配效应的原理来优化放大的反应条件,该方法在不引入其它金属或盐的条件下,能提高银纳米棒的产量,同时降低80%乙二醇的用量。
With the rapid development of society, the traditional conductive material cannot maintain both stability of electricity and properties of strength at the same time, so it is urgent to exploit flexible conductor to satisfy the needs of technology and industry. The conductor fillers are the primary and key material for preparing flexible conducto r. Low-dimensional conductive materials are better than traditional materials in the photoelectric, magnetic, catalytic, sensor field for its huge surface area and quantum effects. It plays an extremely important role in the field of nano-optoelectronic devices, sensors, nano-biotechnology, energy storage and conversion. Polyaniline has good characteristics of doping/dedoping protons regulation, environmental stability, convenient synthesis and facile materials. However, it is difficult to dissolve and melt. Difficult processing hinders the practical application of polyaniline. The nanotechnological synthesis of conductive polyaniline, can combine the electrical conductivity and nano-structure, and greatly improve the processing of the conducting polyaniline. Since nano-structural polyaniline has both advantages of low-dimensional materials and organic conductors, now it becomes a hot focus as a new kind of flexiable conductive material. Nano-silver receives increasing interest because of its high conductivity, unique physical and chemical properties. Recently, a facile method capable of massively synthesizing silver nanorods with high aspect ratios is strongly desired to provide support for their application in commercial areas. This paper deals with the problems of the low dimensional nano-structural polyaniline preparation and morphology control, convenient method for the highly efficient preparation of large amount of silver nanorods and their formation mechanism. The specific contents are as follows:
(1)Through chemical oxidation polymerization of aniline using ammonium persulfate as oxidant in the presence of sodium dodecyl sulfonate (SDS) as soft template polyaniline nanotubes with small sticks on the surface was synthesized. However, polyaniline nanotubes with smooth surface was prepared by adding a certain amount of carbonate to the polymerization process. The effects of kind and dosage of carbonates on the nanostructures of the polyaniline product were investigated. The results showed that, with increasing the amount of gas bubbles evolved, nanostructure of polyaniline was transformed from the nanotubes with smaller nano-rods on the surface, to the nanotubes with smooth surface, or to nanoflakes, according to the amount of carbon dioxide gas evolved. However, the morphology of polyaniline nanomaterials was almost not affected by changing the pH value of the system or addition of other salt which cannot produce gas bubble in the polymerization system. Though the carbonates changed the nanostructures of polyaniline, the molecular structure and crystallinity of polyaniline remained unchanged. All these facts demonstrated that gas bubbles formed during the polymerization process have an important influence on the formation of nanostructure of polyaniline. The mechanism was suggested that the CO2bubbles generated by the reaction of the carbonate with the sulfuric acid formed in-situ in the polymerization process can control different nano-structures of polyaniline.
(2)Helical polyaniline nanostructure was synthesized in the presence of dextral camphor sulfonic acid. However, the helical polyaniline is a network structure. According to the application, which is limited in the low dimensional single device. Mono-disperse helical polyaniline nano-fiber was synthesized in a two-phase solution of water-organic solvent by interfacial polymerization method, which can effectively reduce the rate of its secondary growth. Dissolution of polyaniline in the upper aqueous layer can effectively reduce its aggregation or deposition. The formation mechanism is that through interaction of N-H hydrogen bond between camphor sulfonic acid and aniline, aniline can orderly combine and form at the same side of the oligomer, due to the induction of chiral carbon. Furthermore the helical poly(o-aminophenol) a hydroxyl derivative of polyaniline, was synthesized in the presence of polyethylene glycol. The formation mechanism is attributed to the role of long-chain flexible polyethylene glycol, benzene ring accumulation in long-chain flexible molecules and formation of micro-helical structure. The FT-IR, UV-Vis, elemental analysis and electrical properties of the helical polyaniline and helical poly(o-aminophenol) were measured.
(3)It was reported that using ethylene glycol as solvent and reductant, polyvinyl pyrrolidone(PVP) as capping agent, silver nanorods was prepared by reducing silver nitrate, but the concentration of AgNO3was not exceed0.10M. In this paper, under the action of appropriately preformed silver crystal seeds and controlled addition rates of silver nitrate and PVP solution, silver nanorods with length of2-15μm and diameter of200-880nm can be obtained in high concentration of AgNO3as0.50M. Through study of the effects of various factors on the nanostructure of silver, the favorable conditions are:appropriately preformed seeds concentration at6.54-9.81mM, addition rate of AgNO3solution at0.30-0.43mL/min and molar ratio of PVP/AgNO3at1.1-1.4, the stirring speed was350rpm and the reaction temperature was160℃. The mechanism of preparing silver nanorods in high concentration was suggested as follows:When the AgNO3concentration was high, in the presence of a certain concentration of silver seeds (multiply twinned particles of decahedral shape), which can increase the growth rate of silver atoms on the seeds, due to the existence of more surface area of the silver seeds, thus making the crystal growth rate match the high reduction rate of AgNO3by ethylene glycol. With the help of the capping action of PVP on facets [100] and silver growth on facets [111], silver nanorods were produced. This method without using other metal or salt can not only improve yield of silver nanorods, but can also save80%dosage of glycol.
(1)本论文围绕聚苯胺纳米结构制备方法中存在的问题展开,研究了简单、有效构建多种形貌聚苯胺纳米结构的方法,提出了其形成机理。首次调控碳酸盐简便地合成出聚苯胺纳米结构,机理为碳酸盐与聚苯胺原位聚合产生的硫酸反应生成气泡,通过控制添加的碳酸盐种类和用量来控制气泡量,在无碳酸盐或用量较少时,能得到表面带有小棒的聚苯胺纳米管,当碳酸盐用量一定时,能得到表面光滑的聚苯胺纳米管,当碳酸盐用量较多时,由于产生气泡的微扰作用破坏了软模板胶束,得到聚苯胺纳米片。进一步添加不放出气泡的弱酸盐或调控体系的pH值,对聚苯胺纳米管影响较小,证明了气泡调控聚苯胺纳米结构的形成机理。
(2)聚苯胺螺旋因其具有导电性和可伸缩性的潜能,在柔性导体中有着潜在的应用。但是先前在手性樟脑磺酸的作用下,制备网状结构螺旋型聚苯胺,非可分散的,在一维单根器件上的应用受到限制。本文采用界面聚合的方法,有效降低聚苯胺的二次生长速度,由于手性聚苯胺低聚物为水溶性的,能溶解在上层水相中,不会沉淀且能有效降低其聚集作用,生成可分散的聚苯胺螺旋结构。形成的机理是：手性樟脑磺酸与苯胺通过N-H氢键作用,同时手性碳的诱导使苯胺能有序地在聚苯胺低聚物同一侧面结合而形成了螺旋结构。邻氨基酚为苯胺的衍生物,带有活泼羟基,可以通过氧化聚合得到电活性高分子,为了能制备可伸缩的螺旋结构,先制备出聚邻氨基酚螺旋,使螺旋结构带有改性的羟基,为进一步改性引入热敏、气敏或光敏高分子材料提供条件,使其成为具有可伸缩性能应用到柔性导体中。在聚乙二醇的作用下,制备螺旋型聚邻氨基酚。其形成机理归结为聚乙二醇长链的柔顺性,邻氨基酚的刚性结构苯环在长链柔性分子上的堆积,形成微米螺旋结构。最后,对聚苯胺螺旋和聚邻氨基酚螺旋的FT-IR、UV-Vis、能谱分析和电性能等进行了表征。
(3)常规使用乙二醇作为溶剂和还原剂,PVP作为盖帽剂,将AgNO3还原制取银纳米捧,AgNO3的浓度不能超过0.10M。本论文发现,在银晶种作用下,控制AgNO3和PVP的滴加速度,AgNO3的浓度可高达0.50M,制备出长度为2～15μm,直径为200～880nm的银纳米棒。研究了高浓度制备银纳米棒的影响因素,得到最佳的合成条件为：银晶种的浓度为6.54～9.81mM,AgNO3和PVP的滴加速度为0.30～0.43mL/min,PVP/AgNO3的摩尔比为1.1～1.4,搅拌速度为350rpm,反应温度为160℃。形成机理是：溶液中存在一定浓度和形貌的银晶种提供更多的表面积,能够增加被还原的银原子在银晶种上的生长速度,使得银结晶生长速度和溶液中高的硝酸银还原速度相匹配,由于PVP选择性覆盖在[100]面,银原子在[111]面沉积生长,能高效生成银纳米棒。对反应进行了放大,通过空间效应和速度匹配效应的原理来优化放大的反应条件,该方法在不引入其它金属或盐的条件下,能提高银纳米棒的产量,同时降低80%乙二醇的用量。
With the rapid development of society, the traditional conductive material cannot maintain both stability of electricity and properties of strength at the same time, so it is urgent to exploit flexible conductor to satisfy the needs of technology and industry. The conductor fillers are the primary and key material for preparing flexible conducto r. Low-dimensional conductive materials are better than traditional materials in the photoelectric, magnetic, catalytic, sensor field for its huge surface area and quantum effects. It plays an extremely important role in the field of nano-optoelectronic devices, sensors, nano-biotechnology, energy storage and conversion. Polyaniline has good characteristics of doping/dedoping protons regulation, environmental stability, convenient synthesis and facile materials. However, it is difficult to dissolve and melt. Difficult processing hinders the practical application of polyaniline. The nanotechnological synthesis of conductive polyaniline, can combine the electrical conductivity and nano-structure, and greatly improve the processing of the conducting polyaniline. Since nano-structural polyaniline has both advantages of low-dimensional materials and organic conductors, now it becomes a hot focus as a new kind of flexiable conductive material. Nano-silver receives increasing interest because of its high conductivity, unique physical and chemical properties. Recently, a facile method capable of massively synthesizing silver nanorods with high aspect ratios is strongly desired to provide support for their application in commercial areas. This paper deals with the problems of the low dimensional nano-structural polyaniline preparation and morphology control, convenient method for the highly efficient preparation of large amount of silver nanorods and their formation mechanism. The specific contents are as follows:
(1)Through chemical oxidation polymerization of aniline using ammonium persulfate as oxidant in the presence of sodium dodecyl sulfonate (SDS) as soft template polyaniline nanotubes with small sticks on the surface was synthesized. However, polyaniline nanotubes with smooth surface was prepared by adding a certain amount of carbonate to the polymerization process. The effects of kind and dosage of carbonates on the nanostructures of the polyaniline product were investigated. The results showed that, with increasing the amount of gas bubbles evolved, nanostructure of polyaniline was transformed from the nanotubes with smaller nano-rods on the surface, to the nanotubes with smooth surface, or to nanoflakes, according to the amount of carbon dioxide gas evolved. However, the morphology of polyaniline nanomaterials was almost not affected by changing the pH value of the system or addition of other salt which cannot produce gas bubble in the polymerization system. Though the carbonates changed the nanostructures of polyaniline, the molecular structure and crystallinity of polyaniline remained unchanged. All these facts demonstrated that gas bubbles formed during the polymerization process have an important influence on the formation of nanostructure of polyaniline. The mechanism was suggested that the CO2bubbles generated by the reaction of the carbonate with the sulfuric acid formed in-situ in the polymerization process can control different nano-structures of polyaniline.
(2)Helical polyaniline nanostructure was synthesized in the presence of dextral camphor sulfonic acid. However, the helical polyaniline is a network structure. According to the application, which is limited in the low dimensional single device. Mono-disperse helical polyaniline nano-fiber was synthesized in a two-phase solution of water-organic solvent by interfacial polymerization method, which can effectively reduce the rate of its secondary growth. Dissolution of polyaniline in the upper aqueous layer can effectively reduce its aggregation or deposition. The formation mechanism is that through interaction of N-H hydrogen bond between camphor sulfonic acid and aniline, aniline can orderly combine and form at the same side of the oligomer, due to the induction of chiral carbon. Furthermore the helical poly(o-aminophenol) a hydroxyl derivative of polyaniline, was synthesized in the presence of polyethylene glycol. The formation mechanism is attributed to the role of long-chain flexible polyethylene glycol, benzene ring accumulation in long-chain flexible molecules and formation of micro-helical structure. The FT-IR, UV-Vis, elemental analysis and electrical properties of the helical polyaniline and helical poly(o-aminophenol) were measured.
(3)It was reported that using ethylene glycol as solvent and reductant, polyvinyl pyrrolidone(PVP) as capping agent, silver nanorods was prepared by reducing silver nitrate, but the concentration of AgNO3was not exceed0.10M. In this paper, under the action of appropriately preformed silver crystal seeds and controlled addition rates of silver nitrate and PVP solution, silver nanorods with length of2-15μm and diameter of200-880nm can be obtained in high concentration of AgNO3as0.50M. Through study of the effects of various factors on the nanostructure of silver, the favorable conditions are:appropriately preformed seeds concentration at6.54-9.81mM, addition rate of AgNO3solution at0.30-0.43mL/min and molar ratio of PVP/AgNO3at1.1-1.4, the stirring speed was350rpm and the reaction temperature was160℃. The mechanism of preparing silver nanorods in high concentration was suggested as follows:When the AgNO3concentration was high, in the presence of a certain concentration of silver seeds (multiply twinned particles of decahedral shape), which can increase the growth rate of silver atoms on the seeds, due to the existence of more surface area of the silver seeds, thus making the crystal growth rate match the high reduction rate of AgNO3by ethylene glycol. With the help of the capping action of PVP on facets [100] and silver growth on facets [111], silver nanorods were produced. This method without using other metal or salt can not only improve yield of silver nanorods, but can also save80%dosage of glycol.
引文
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