聚合物—十二烷基硫酸钠水溶液中纳米金的可控合成
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摘要
金纳米粒子是目前研究最为热点的一种金属纳米粒子,它的高催化活性,良好的生物相容性和能通过自组装形成特定纳米结构的特点,使其在高级材料的制造上具有很大的应用前景。纳米材料不同于常规物质的独特性质很大程度上取决于它们的形状和尺寸。因此,在纳米技术中,纳米材料的可控合成是最活跃的研究领域。与单一表面活性剂或聚合物模板相比,聚合物-表面活性剂聚集体具有更高级的自组装结构,其聚集状态具有更大的可调控性,并且能够发挥协同模板作用,在特殊形貌无机纳米粒子的制备方面具有更大的应用前景。本论文结合材料化学绿色化的发展趋势,利用聚乙烯吡咯烷酮(PVP),聚乙烯醇(PVA)和羟乙基纤维素(HEC)与阴离子表面活性剂十二烷基硫酸钠(SDS)形成的聚集体为模板,在水溶液中直接利用聚合物还原金盐前体,在低温,无需外加还原剂的条件下,通过一锅法制备出了不同形貌的金纳米粒子,考察了反应时间,SDS浓度,初始HAuCl4浓度等对产物形貌的影响,揭示了聚合物-SDS聚集体在金纳米粒子生长过程中的“两级软模板”作用机制,并初步考察了产物金纳米粒子的应用性能。
PVP-SDS聚集体是目前研究较为全面的一种聚合物-表面活性剂聚集体结构。人们已经明确建立了PVP-SDS聚集体的微观作用模型,这为揭示PVP-SDS聚集体在纳米粒子形成过程中的模板作用机理奠定了良好的基础。在PVP-SDS聚集体水溶液中,以PVP为还原剂制备出了蛇状金纳米粒子。采用紫外-可见-近红外吸收光谱(UV-vis-NIR),透射电子显微镜(TEM),X-射线衍射(XRD),选区电子衍射(SAED)和高分辨透射电子显微(HRTEM)技术等对产物粒子的光谱吸收性质,形貌和晶体结构进行了表征和分析,推测出了金纳米蛇的生长机制。实验发现在相同浓度的单纯PVP溶液中产物为弯弯曲曲的金纳米带。PVP-SDS聚集体溶液中,SDS束缚胶束的存在使得沿着PVP链金盐反应前体出现浓度分布差异,有利于不对称金纳米结构的生长。调节SDS浓度可以改变PVP-SDS聚集体的聚集状态,从而对产物粒子的形貌进行调控。当体系中SDS浓度由3 mmol·L~(-1)增大到10 mmol·L~(-1)时,产物粒子发生了由蛇状→风筝状→片状的形貌转变。实验发现,金纳米蛇对于KOH介质中CH3OH氧化反应具有优异的电催化效果,这一性质使其在直接甲醇燃料电池(DMFC)制备方面具有广阔的应用前景。
PVP的还原作用相对较弱,因此在现有的采用PVP直接作为还原剂和选择性吸附剂制备贵金属纳米粒子的报道中,产物多为2D片状纳米结构物。实验发现,在较高PVP浓度下,向PVP-SDS聚集体水溶液中添加NaOH将AuCl_4~ˉ转变成还原活性较低的AuCl_(4-x)(OH)_x~ˉ,使得体系中初级纳米晶的生长被抑制而相互聚集形成较大聚集体,最终可以长成形貌完整,结构密实的三维(3D)金纳米花。以UV-vis-NIR吸收光谱和TEM跟踪了金纳米花的生长过程,推测出了该体系中金纳米花的生长机制。在相同浓度的单纯PVP溶液中只得到了粒径较小的多脚状金纳米粒子这是因为与PVP-SDS聚集体相比,PVP对于金初级纳米晶的保护能力过强限制了它们的相互聚集和后续的各向异性的生长所致。通过改变SDS浓度可以对产物金纳米花的粒径进行调控。初始HAuCl4浓度对产物形貌影响显著,当体系中初始HAuCl_4浓度由0.1 mmol·L~(-1)增大到0.7 mmol·L~(-1)时,产物由多脚状粒子→3D纳米花→2D纳米花→中心带孔洞的纳米片→完整纳米片转变。实验发现,3D金纳米花具有非常优异的SERS性能。
聚乙烯醇(PVA)可以与SDS发生疏水相互作用形成PVA-SDS有序聚集体,并且PVA分子结构中具有很多羟基基团,在金纳米粒子制备过程中同样可以发挥还原作用。因此将金纳米粒子的制备体系扩展到PVA-SDS聚集体水溶液。首先,采用表面张力法和电导法研究了PVA与SDS的相互作用,确定了形成PVA-SDS聚集体的SDS浓度范围。采用动态激光光散射(DLS)法测定了PVA-SDS聚集体的流体力学半径(R_h)。在PVA-SDS聚集体水溶液中,室温下以PVA直接还原HAuCl_4制备出了风筝状金纳米粒子,而在相同浓度单纯PVA溶液中产物为2D超枝化纳米粒子,说明SDS对于金纳米风筝的形成至关重要。PVA-SDS聚集体溶液中,SDS束缚胶束的存在使得沿着PVA链AuCl_4~ˉ出现浓度分布差异,有利于不对称金纳米结构的生长。初始HAuCl_4浓度对产物粒子的形貌影响显著,当体系中初始HAuCl_4浓度由0.5 mmol·L~(-1)增大到2.2 mmol·L~(-1)时,产物由枝化金纳米粒子逐渐向完整微米片转变。
近年来,天然多糖类大分子及其简单改性物的研究和应用受到了越来越多的关注。水溶性的羟乙基纤维素(HEC)分子结构中存在大量羟基基团,可以用作金纳米粒子制备过程中的还原剂。采用表面张力法和电导法研究了HEC与SDS的相互作用。确定了形成HEC-SDS聚集体的SDS浓度范围。以稳态荧光猝灭法测定了HEC-SDS有序聚集体的束缚胶束聚集数Nb。采用DLS法测定了HEC-SDS聚集体的流体力学半径(Rh)。在HEC-SDS聚集体水溶液中,以HEC为还原剂制备出了枝化金纳米粒子和形貌规整的金纳米片。并采用两步种子法制备出了正二十面体金纳米粒子。
Gold nanostructures have attracted great attention for their peculiar properties, such as high catalytic activity, excellent biocompatibility and potentials in constructing advanced materials. Great progress has been achieved in the researches and applications of gold nanostructures in sensor, electronic devices, biochemical engineering (e.g. gene sequencing) and chemical catalysts. The special properties of nanomaterials are dependent on their sizes and shapes. Therefore, controlled synthesis of nanomaterials with certain morphologies is significant and it is the basis of their applications and the precondition of the fabrication of nano-devices. Compared with single surfactant or polymer, the structure of polymer-surfactant aggregations is more advanced and possess greater regulate. Furthermore, polymer-surfactant aggregations can exert synergistic template effect and possess greater prospect in the synthesis of inorganic nanomaterials. In this thesis, the polymer-surfactant aggregations formed by poly(vinyl pyrrolidone) (PVP), polyvinyl alcohol (PVA) and hydroxyethyl cellulose (HEC) with anionic surfactant, sodium dodecyl sulfate (SDS), were used as soft templates to synthesize gold nanostructures by directly reducing gold salt precursor with the polymers. Gold nanostructures with different morphologies were synthesized through a one-pot route, at low temperature and without any additional reducing agent. The influences of reaction time, SDS concentration and initial HAuCl4 concentration were studied in detail. The“secondary template effect”of polymer-SDS aggregations was proposed based on the experiment results. Moreover, the application properties of the synthesized gold nanoparticles were carefully detected.
PVP-SDS aggregation was one of the most widely studied polymer-surfactant assemblies. The interaction model of PVP and SDS has been builted up which is the basis for their further application in the synthesis of inorganic nanomaterials. In PVP-SDS aggregations solution, gold nanosnakes were synthesized by directly using PVP as reducing agent. The optical properties, morphologies and crystal structures were characterized by UV-vis-NIR spectra, transmission electron microscope (TEM), X-ray diffraction (XRD), selected area electron diffraction (SAED) and high-resolution transmission electron microscopy (HRTEM). A tentative growth mechanism of gold nanosnakes was given out based on the time-course measurements of TEM at the initial growth stages of gold nanosnakes. In pure PVP solution, only tortuous gold nanobelts were synthesized. In PVP-SDS necklace-like aggregations solution, the concentration of gold salt precursor at the vicinity of SDS bound micelles and PVP blank chains will be different because of the electrostatic repulsion between SDS bound micelles and gold salt precursor which facilitate the formation of asymmetrical nanostructures. The structures of PVP-SDS aggregations can be adjusted by changing SDS concentration which will induce the morphologies variation of the products. When SDS concentration was increased from 3 mmol·L~(-1) to 10 mmol·L~(-1), the morphologies of the products changed from snake-like to kite-like and finally to plate. Gold nanosnakes exhibited excellent electrocatalytic property toward the oxidation of methanol indicating their potential applications in direct methanol fuel cells (DMFC).
2-dimentional (2D) planar precious metal nanoparticles were the most common synthesized products by using PVP directly as reducing agent due to its weak reducing power. In PVP-SDS aggregations aqueous solution, a certain amount of added NaOH induced the transformation of gold salt precursor from AuCl_4~ˉto AuCl_(4-x)(OH)_x~ˉwith lower reducing activity. The growing rate of the incipient small nanocrystals was slowed down which made them tend to aggregate to form larger aggregations and finally evolved to complete and compact 3D nanoflowers. The growth process of gold nanoflowers was monitored by UV-vis-NIR spectra and TEM based on which a tentative growth mechanism of gold nanoflowers was proposed. The diameters of the synthesized gold nanoflowers can be adjusted by changing SDS concentration. The initial HAuCl4 concentration was found to be of paramount importance to the final shape of the products. When HAuCl4 concentration was increased from 0.1 mmol·L~(-1) to 0.7 mmol·L~(-1), the synthesized products changed from multipod to 3D nanoflowers, 2D nanoflowers, nanoplates with a hole in the center and complete nanoplates. In pure PVP solution, the products were multipod nanoparticles of 43 nm in diameter and only possessed 4 to 8 branches which indicated that the protection effect of PVP was stronger than PVP-SDS aggregations and the exorbitant sufficient protecting effect might impede small nanocrystals agglomerating to form larger loose agglomerations and obstruct the subsequent anisotropic growing of the loose agglomerations. Moreover, the synthesized gold nanoflowers exhibited excellent SERS property.
In aqueous solution, PVA can interact with SDS to form PVA-SDS aggregations through hydrophobic interaction and the hydroxyl groups in PVA molecular structure make it an available reducing agent in the synthesis of gold nanoparticles. Interaction of PVA and SDS was investigated by surface tension and specific conductance methods and determined the SDS concentration range for the formation of PVA-SDS aggregations. The hydrodynamic radius (Rh) of PVP-SDS aggregations was detected by dynamic light scattering (DLS) method. Gold nanokites were synthesized in PVA-SDS aggregations solution at room temperature by directly reducing HAuCl4 with PVA. However, in pure PVA solution, the products were 2D superbranched gold nanostructures which indicated that SDS was indispensable for the synthesis of the unique gold nanokites. In PVA-SDS aggregations solution, the concentration of AuCl_4~ˉat the vicinity of SDS bound micelles and PVA blank chains will be different because of the electrostatic repulsion between SDS bound micelles and AuCl_4~ˉwhich facilitate the formation of asymmetrical nanostructures. The initial HAuCl4 concentration was found to be of paramount importance to the final shape of the products. When HAuCl4 concentration was increased from 0.5 mmol·L~(-1) to 2.2 mmol·L~(-1), the synthesized products changed from branched nanostructures to complete microplates.
Recently, the studies and applications of natural or modified polysaccharides have attracted great attention. Water-soluble HEC possesses many hydroxyl groups in their molecular structures and can be used as reducing agent in the synthesis of gold nanoparticles. Interaction of HEC and SDS was investigated by surface tension and specific conductance methods and determined the SDS concentration range for the formation of HEC-SDS aggregations. The bound micelles aggregation number (N_b) of SDS in HEC-SDS aggregations have been investigated by steady state fluorescence quenching. The hydrodynamic radius (R_h) of PVP-SDS aggregations was detected by DLS method. In HEC-SDS aggregations solution, branched gold nanostructures and gold nanoplates were synthesized. Moreover, well defined gold icosahedrons were synthesized through a two-step seed mediated method in HEC-SDS growth solution.
PVP-SDS聚集体是目前研究较为全面的一种聚合物-表面活性剂聚集体结构。人们已经明确建立了PVP-SDS聚集体的微观作用模型,这为揭示PVP-SDS聚集体在纳米粒子形成过程中的模板作用机理奠定了良好的基础。在PVP-SDS聚集体水溶液中,以PVP为还原剂制备出了蛇状金纳米粒子。采用紫外-可见-近红外吸收光谱(UV-vis-NIR),透射电子显微镜(TEM),X-射线衍射(XRD),选区电子衍射(SAED)和高分辨透射电子显微(HRTEM)技术等对产物粒子的光谱吸收性质,形貌和晶体结构进行了表征和分析,推测出了金纳米蛇的生长机制。实验发现在相同浓度的单纯PVP溶液中产物为弯弯曲曲的金纳米带。PVP-SDS聚集体溶液中,SDS束缚胶束的存在使得沿着PVP链金盐反应前体出现浓度分布差异,有利于不对称金纳米结构的生长。调节SDS浓度可以改变PVP-SDS聚集体的聚集状态,从而对产物粒子的形貌进行调控。当体系中SDS浓度由3 mmol·L~(-1)增大到10 mmol·L~(-1)时,产物粒子发生了由蛇状→风筝状→片状的形貌转变。实验发现,金纳米蛇对于KOH介质中CH3OH氧化反应具有优异的电催化效果,这一性质使其在直接甲醇燃料电池(DMFC)制备方面具有广阔的应用前景。
PVP的还原作用相对较弱,因此在现有的采用PVP直接作为还原剂和选择性吸附剂制备贵金属纳米粒子的报道中,产物多为2D片状纳米结构物。实验发现,在较高PVP浓度下,向PVP-SDS聚集体水溶液中添加NaOH将AuCl_4~ˉ转变成还原活性较低的AuCl_(4-x)(OH)_x~ˉ,使得体系中初级纳米晶的生长被抑制而相互聚集形成较大聚集体,最终可以长成形貌完整,结构密实的三维(3D)金纳米花。以UV-vis-NIR吸收光谱和TEM跟踪了金纳米花的生长过程,推测出了该体系中金纳米花的生长机制。在相同浓度的单纯PVP溶液中只得到了粒径较小的多脚状金纳米粒子这是因为与PVP-SDS聚集体相比,PVP对于金初级纳米晶的保护能力过强限制了它们的相互聚集和后续的各向异性的生长所致。通过改变SDS浓度可以对产物金纳米花的粒径进行调控。初始HAuCl4浓度对产物形貌影响显著,当体系中初始HAuCl_4浓度由0.1 mmol·L~(-1)增大到0.7 mmol·L~(-1)时,产物由多脚状粒子→3D纳米花→2D纳米花→中心带孔洞的纳米片→完整纳米片转变。实验发现,3D金纳米花具有非常优异的SERS性能。
聚乙烯醇(PVA)可以与SDS发生疏水相互作用形成PVA-SDS有序聚集体,并且PVA分子结构中具有很多羟基基团,在金纳米粒子制备过程中同样可以发挥还原作用。因此将金纳米粒子的制备体系扩展到PVA-SDS聚集体水溶液。首先,采用表面张力法和电导法研究了PVA与SDS的相互作用,确定了形成PVA-SDS聚集体的SDS浓度范围。采用动态激光光散射(DLS)法测定了PVA-SDS聚集体的流体力学半径(R_h)。在PVA-SDS聚集体水溶液中,室温下以PVA直接还原HAuCl_4制备出了风筝状金纳米粒子,而在相同浓度单纯PVA溶液中产物为2D超枝化纳米粒子,说明SDS对于金纳米风筝的形成至关重要。PVA-SDS聚集体溶液中,SDS束缚胶束的存在使得沿着PVA链AuCl_4~ˉ出现浓度分布差异,有利于不对称金纳米结构的生长。初始HAuCl_4浓度对产物粒子的形貌影响显著,当体系中初始HAuCl_4浓度由0.5 mmol·L~(-1)增大到2.2 mmol·L~(-1)时,产物由枝化金纳米粒子逐渐向完整微米片转变。
近年来,天然多糖类大分子及其简单改性物的研究和应用受到了越来越多的关注。水溶性的羟乙基纤维素(HEC)分子结构中存在大量羟基基团,可以用作金纳米粒子制备过程中的还原剂。采用表面张力法和电导法研究了HEC与SDS的相互作用。确定了形成HEC-SDS聚集体的SDS浓度范围。以稳态荧光猝灭法测定了HEC-SDS有序聚集体的束缚胶束聚集数Nb。采用DLS法测定了HEC-SDS聚集体的流体力学半径(Rh)。在HEC-SDS聚集体水溶液中,以HEC为还原剂制备出了枝化金纳米粒子和形貌规整的金纳米片。并采用两步种子法制备出了正二十面体金纳米粒子。
Gold nanostructures have attracted great attention for their peculiar properties, such as high catalytic activity, excellent biocompatibility and potentials in constructing advanced materials. Great progress has been achieved in the researches and applications of gold nanostructures in sensor, electronic devices, biochemical engineering (e.g. gene sequencing) and chemical catalysts. The special properties of nanomaterials are dependent on their sizes and shapes. Therefore, controlled synthesis of nanomaterials with certain morphologies is significant and it is the basis of their applications and the precondition of the fabrication of nano-devices. Compared with single surfactant or polymer, the structure of polymer-surfactant aggregations is more advanced and possess greater regulate. Furthermore, polymer-surfactant aggregations can exert synergistic template effect and possess greater prospect in the synthesis of inorganic nanomaterials. In this thesis, the polymer-surfactant aggregations formed by poly(vinyl pyrrolidone) (PVP), polyvinyl alcohol (PVA) and hydroxyethyl cellulose (HEC) with anionic surfactant, sodium dodecyl sulfate (SDS), were used as soft templates to synthesize gold nanostructures by directly reducing gold salt precursor with the polymers. Gold nanostructures with different morphologies were synthesized through a one-pot route, at low temperature and without any additional reducing agent. The influences of reaction time, SDS concentration and initial HAuCl4 concentration were studied in detail. The“secondary template effect”of polymer-SDS aggregations was proposed based on the experiment results. Moreover, the application properties of the synthesized gold nanoparticles were carefully detected.
PVP-SDS aggregation was one of the most widely studied polymer-surfactant assemblies. The interaction model of PVP and SDS has been builted up which is the basis for their further application in the synthesis of inorganic nanomaterials. In PVP-SDS aggregations solution, gold nanosnakes were synthesized by directly using PVP as reducing agent. The optical properties, morphologies and crystal structures were characterized by UV-vis-NIR spectra, transmission electron microscope (TEM), X-ray diffraction (XRD), selected area electron diffraction (SAED) and high-resolution transmission electron microscopy (HRTEM). A tentative growth mechanism of gold nanosnakes was given out based on the time-course measurements of TEM at the initial growth stages of gold nanosnakes. In pure PVP solution, only tortuous gold nanobelts were synthesized. In PVP-SDS necklace-like aggregations solution, the concentration of gold salt precursor at the vicinity of SDS bound micelles and PVP blank chains will be different because of the electrostatic repulsion between SDS bound micelles and gold salt precursor which facilitate the formation of asymmetrical nanostructures. The structures of PVP-SDS aggregations can be adjusted by changing SDS concentration which will induce the morphologies variation of the products. When SDS concentration was increased from 3 mmol·L~(-1) to 10 mmol·L~(-1), the morphologies of the products changed from snake-like to kite-like and finally to plate. Gold nanosnakes exhibited excellent electrocatalytic property toward the oxidation of methanol indicating their potential applications in direct methanol fuel cells (DMFC).
2-dimentional (2D) planar precious metal nanoparticles were the most common synthesized products by using PVP directly as reducing agent due to its weak reducing power. In PVP-SDS aggregations aqueous solution, a certain amount of added NaOH induced the transformation of gold salt precursor from AuCl_4~ˉto AuCl_(4-x)(OH)_x~ˉwith lower reducing activity. The growing rate of the incipient small nanocrystals was slowed down which made them tend to aggregate to form larger aggregations and finally evolved to complete and compact 3D nanoflowers. The growth process of gold nanoflowers was monitored by UV-vis-NIR spectra and TEM based on which a tentative growth mechanism of gold nanoflowers was proposed. The diameters of the synthesized gold nanoflowers can be adjusted by changing SDS concentration. The initial HAuCl4 concentration was found to be of paramount importance to the final shape of the products. When HAuCl4 concentration was increased from 0.1 mmol·L~(-1) to 0.7 mmol·L~(-1), the synthesized products changed from multipod to 3D nanoflowers, 2D nanoflowers, nanoplates with a hole in the center and complete nanoplates. In pure PVP solution, the products were multipod nanoparticles of 43 nm in diameter and only possessed 4 to 8 branches which indicated that the protection effect of PVP was stronger than PVP-SDS aggregations and the exorbitant sufficient protecting effect might impede small nanocrystals agglomerating to form larger loose agglomerations and obstruct the subsequent anisotropic growing of the loose agglomerations. Moreover, the synthesized gold nanoflowers exhibited excellent SERS property.
In aqueous solution, PVA can interact with SDS to form PVA-SDS aggregations through hydrophobic interaction and the hydroxyl groups in PVA molecular structure make it an available reducing agent in the synthesis of gold nanoparticles. Interaction of PVA and SDS was investigated by surface tension and specific conductance methods and determined the SDS concentration range for the formation of PVA-SDS aggregations. The hydrodynamic radius (Rh) of PVP-SDS aggregations was detected by dynamic light scattering (DLS) method. Gold nanokites were synthesized in PVA-SDS aggregations solution at room temperature by directly reducing HAuCl4 with PVA. However, in pure PVA solution, the products were 2D superbranched gold nanostructures which indicated that SDS was indispensable for the synthesis of the unique gold nanokites. In PVA-SDS aggregations solution, the concentration of AuCl_4~ˉat the vicinity of SDS bound micelles and PVA blank chains will be different because of the electrostatic repulsion between SDS bound micelles and AuCl_4~ˉwhich facilitate the formation of asymmetrical nanostructures. The initial HAuCl4 concentration was found to be of paramount importance to the final shape of the products. When HAuCl4 concentration was increased from 0.5 mmol·L~(-1) to 2.2 mmol·L~(-1), the synthesized products changed from branched nanostructures to complete microplates.
Recently, the studies and applications of natural or modified polysaccharides have attracted great attention. Water-soluble HEC possesses many hydroxyl groups in their molecular structures and can be used as reducing agent in the synthesis of gold nanoparticles. Interaction of HEC and SDS was investigated by surface tension and specific conductance methods and determined the SDS concentration range for the formation of HEC-SDS aggregations. The bound micelles aggregation number (N_b) of SDS in HEC-SDS aggregations have been investigated by steady state fluorescence quenching. The hydrodynamic radius (R_h) of PVP-SDS aggregations was detected by DLS method. In HEC-SDS aggregations solution, branched gold nanostructures and gold nanoplates were synthesized. Moreover, well defined gold icosahedrons were synthesized through a two-step seed mediated method in HEC-SDS growth solution.
引文
[1]施利毅.纳米材料[M].上海:华东理工大学出版社,2007. 1.
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