形貌可控的纳米Ag和Ag/ZnO复合材料的制备与表征
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摘要
由于Ag纳米材料本身具有极大优越性,即具有独特的光学性、高导电性、高催化性和高抗菌性,使其在光电材料、电极材料、催化材料及抗菌材料等领域中占有重要地位,而纳米Ag这些优异特性主要取决于其形貌和尺寸,因此,对纳米Ag形貌可控制备研究成为纳米材料研究热点。本文采用微波辅助多元醇法,系统的研究了可控制备不同形貌纳米Ag及形成机理,并以所得Ag纳米线为原料,采用微波法和水热法,研究了蠕虫状结构Ag/ZnO和鞭炮状结构Ag/ZnO制备及其生长机理。主要研究结果如下：
1、以乙二醇(EG)为还原剂和溶剂,在表面活性剂聚乙烯吡咯烷酮(PVP)存在下,微波加热快速制备了Ag纳米颗粒。分别研究了反应时间、微波功率、AgNO3浓度、PVP浓度对Ag纳米颗粒的影响。结果表明：Ag纳米颗粒分散性较好,且PVP能够吸附于Ag晶体表面,防止Ag纳米颗粒的团聚。随着反应时间增加,PVP对Ag晶核的吸附作用大于晶核生长速度,有利于形成小尺寸Ag纳米颗粒；而随着微波功率和AgNO3浓度的增加,其形核速度大于生长速度,从而有利于形成小尺寸Ag纳米颗粒。
2、以Na2S为控制剂,制备了Ag纳米线和纳米立方体。添加低浓度Na2S时可制备尺寸可控的Ag纳米立方体。由于Ag2S胶体为n型半导体,低浓度下催化还原Ag+,加大Ag+还原速度,促使溶液中Ag原子过饱和状态,从而形成更多单晶晶种,在PVP吸附下而快速形成Ag纳米立方体。而添加高浓度Na2S时,可制备尺寸可控的Ag纳米线。高浓度Ag2S胶体的形成减少了溶液中自由Ag+浓度,导致Ag+还原速度减小,从而利于十面体孪晶晶种形成。由于PVP对晶种{100}晶面族的选择吸附作用,使得十面体孪晶晶种各向异性生长而形成Ag纳米线。随着Na2S浓度的变大,可获得尺寸较大的Ag纳米线。
3、以CuCl2为控制剂,可制备出尺寸可控Ag纳米线。研究了CuCl2浓度、Cu2+存在等对Ag纳米线的影响。结果表明：C1-与Ag+形成AgCl胶体,减少溶液中Ag+的浓度,使得Ag原子还原速度减低,从而促进十面体孪晶晶种形成。随着反应进行,AgCl不断将Ag+释放到溶液中。Cu2+被EG还原成Cu+,而Cu+被O2氧化成Cu2+以此不断消耗02,从而抑制十面体孪晶晶种被C1-/O2蚀刻。这些晶种在PVP选择吸附下快速长成Ag纳米线。
4、以前期所得Ag纳米线、醋酸锌、三乙醇胺(TEA)为原料,微波法合成蠕虫状Ag/ZnO核壳结构。该结构是由ZnO(为壳)包覆Ag纳米线(为核)生长而成。以前期所得Ag纳米线、硝酸锌、六次甲基四胺(HMT)为原料,水热法制备了鞭炮状Ag/ZnO异质结。该结构由约100nm ZnO纳米棒垂直于Ag纳米线长度方向生长而形成。
Silver nanostructures have great advantages, such as unique optical properties, high electrical conductivity, high catalytic ability, high antibacterial activity. These advantages determine that Silver nanostructures play an important role in photoelectric materials, electrode materials, catalytic materials, and antibacterial materials. However, the excellent properties of silver nanostructures are mainly dependent on their shapes and sizes. Thus, the shape-controllable synthesis of silver nanostructures has garnered a significant attention. In this paper, the synthesis and growth mechanism of shape-controlled silver nanostructures were investigated systematically by microwave assisted polyols method. The wormlike Ag/ZnO and firecracker-like Ag/ZnO were synthesized with prepared silver nanowires by microwave method and hydrothermal method. And their formation mechanisms were also clarified. These main results are listed as below:
1. Uniform silver nanoparticles were prepared with ethylene glycol (EG) as reducing agent and solvent and with poly (vintlpyrrolidone)(PVP) as surfactant. The effects of reaction time, microwave power, PVP concentration, and AgNO3 concentration on the morphology and size of silver nanostructures were studied. The results show that the dispersivity of Ag nanoparticles was good, and the surfaces of silver nanoparticles were easily absorbed and covered by PVP, which prevented the agglomeration of silver nanoparticles. As the reaction time increased, the adsorption effect of PVP was greater than that of growth rate, promoting the formation of small size Ag nanoparticles. As the microwave power and the AgNO3concentration increased, the nucleation rate became higher than growth rate, promoting the formation of small size Ag nanoparticles.
2. Silver nanowires and nanocubes were obtained by adding different concentrations of Na2S into the solution. Silver nanocubes were synthesized under low concentration of Na2S. The low concentration of Ag2S, which is an n-type semiconductor as catalytic agent, catalyzed Ag+reduction, increased the rate of Ag+reduction, and promoted supersaturation with silver seeds and subsequent formation of single-crystalline seeds. The seeds fast grew into silver nanocubes with the PVP adsorption. Silver nanowires were synthesized of high concentration of Na2S. A high concentration of Ag2S as controlling agents reduced the concentration of free Ag+in the solution, decreased the rate of Ag+reduction, and promoted the formation of the decahedral twinned nanoparticle. In the subsequent reaction, Ag+ions were gradually released from Ag2S colloids into the solution, keeping the equilibrium concentrations of in soluble and soluble salts. The twincrystal nanparticles fast grew into silver nanowires with the adsorption of PVP on the{100} facets. When the concentration of Na2S gradually increased (rang from2.0mM to3.5mM), silver nanowires with large diameters were obtained.
3. Silver nanowires were obtained using CuCl2as controlling agents. The results show that AgCl colloids were formed from Cl-and free Ag+in the solution, reducing the concentration of Ag+ions in solution, decreasing the rate of Ag+reduction, and resulting in formation of multiply twinned seeds of decahedral shape. In the subsequent reaction, Ag+ions were gradually released from AgCl colloids into the solution. Cu2+was reduced Cu+, and then Cu+was oxidized Cu to consume O2and thus to prevent the silver seeds from being etched by Cr/O2.These multiply twinned seeds of decahedral shape can grew into silver nanowires due to selective adsorption of PVP on{100} facets.
4. Wormlike Ag/ZnO core-shell structures were synthesized by microwave method with silver nanowires, zinc acetate, and triethanolamine (TEA) as raw materials. The structures were composed of single crystal Ag nanowires (core) and dense regular ZnO particles (shell) grown on Ag nanowires. Firecracker-like Ag/ZnO heterojunction was synthesized by hydrothermal method using silver nanowires, zinc nitrate, and hexamethylene tetramine (HMT) as raw materials. The structures were formed by the growth of about100nm ZnO nanorods perpendicular to the axis of Ag nanowires.
1、以乙二醇(EG)为还原剂和溶剂,在表面活性剂聚乙烯吡咯烷酮(PVP)存在下,微波加热快速制备了Ag纳米颗粒。分别研究了反应时间、微波功率、AgNO3浓度、PVP浓度对Ag纳米颗粒的影响。结果表明：Ag纳米颗粒分散性较好,且PVP能够吸附于Ag晶体表面,防止Ag纳米颗粒的团聚。随着反应时间增加,PVP对Ag晶核的吸附作用大于晶核生长速度,有利于形成小尺寸Ag纳米颗粒；而随着微波功率和AgNO3浓度的增加,其形核速度大于生长速度,从而有利于形成小尺寸Ag纳米颗粒。
2、以Na2S为控制剂,制备了Ag纳米线和纳米立方体。添加低浓度Na2S时可制备尺寸可控的Ag纳米立方体。由于Ag2S胶体为n型半导体,低浓度下催化还原Ag+,加大Ag+还原速度,促使溶液中Ag原子过饱和状态,从而形成更多单晶晶种,在PVP吸附下而快速形成Ag纳米立方体。而添加高浓度Na2S时,可制备尺寸可控的Ag纳米线。高浓度Ag2S胶体的形成减少了溶液中自由Ag+浓度,导致Ag+还原速度减小,从而利于十面体孪晶晶种形成。由于PVP对晶种{100}晶面族的选择吸附作用,使得十面体孪晶晶种各向异性生长而形成Ag纳米线。随着Na2S浓度的变大,可获得尺寸较大的Ag纳米线。
3、以CuCl2为控制剂,可制备出尺寸可控Ag纳米线。研究了CuCl2浓度、Cu2+存在等对Ag纳米线的影响。结果表明：C1-与Ag+形成AgCl胶体,减少溶液中Ag+的浓度,使得Ag原子还原速度减低,从而促进十面体孪晶晶种形成。随着反应进行,AgCl不断将Ag+释放到溶液中。Cu2+被EG还原成Cu+,而Cu+被O2氧化成Cu2+以此不断消耗02,从而抑制十面体孪晶晶种被C1-/O2蚀刻。这些晶种在PVP选择吸附下快速长成Ag纳米线。
4、以前期所得Ag纳米线、醋酸锌、三乙醇胺(TEA)为原料,微波法合成蠕虫状Ag/ZnO核壳结构。该结构是由ZnO(为壳)包覆Ag纳米线(为核)生长而成。以前期所得Ag纳米线、硝酸锌、六次甲基四胺(HMT)为原料,水热法制备了鞭炮状Ag/ZnO异质结。该结构由约100nm ZnO纳米棒垂直于Ag纳米线长度方向生长而形成。
Silver nanostructures have great advantages, such as unique optical properties, high electrical conductivity, high catalytic ability, high antibacterial activity. These advantages determine that Silver nanostructures play an important role in photoelectric materials, electrode materials, catalytic materials, and antibacterial materials. However, the excellent properties of silver nanostructures are mainly dependent on their shapes and sizes. Thus, the shape-controllable synthesis of silver nanostructures has garnered a significant attention. In this paper, the synthesis and growth mechanism of shape-controlled silver nanostructures were investigated systematically by microwave assisted polyols method. The wormlike Ag/ZnO and firecracker-like Ag/ZnO were synthesized with prepared silver nanowires by microwave method and hydrothermal method. And their formation mechanisms were also clarified. These main results are listed as below:
1. Uniform silver nanoparticles were prepared with ethylene glycol (EG) as reducing agent and solvent and with poly (vintlpyrrolidone)(PVP) as surfactant. The effects of reaction time, microwave power, PVP concentration, and AgNO3 concentration on the morphology and size of silver nanostructures were studied. The results show that the dispersivity of Ag nanoparticles was good, and the surfaces of silver nanoparticles were easily absorbed and covered by PVP, which prevented the agglomeration of silver nanoparticles. As the reaction time increased, the adsorption effect of PVP was greater than that of growth rate, promoting the formation of small size Ag nanoparticles. As the microwave power and the AgNO3concentration increased, the nucleation rate became higher than growth rate, promoting the formation of small size Ag nanoparticles.
2. Silver nanowires and nanocubes were obtained by adding different concentrations of Na2S into the solution. Silver nanocubes were synthesized under low concentration of Na2S. The low concentration of Ag2S, which is an n-type semiconductor as catalytic agent, catalyzed Ag+reduction, increased the rate of Ag+reduction, and promoted supersaturation with silver seeds and subsequent formation of single-crystalline seeds. The seeds fast grew into silver nanocubes with the PVP adsorption. Silver nanowires were synthesized of high concentration of Na2S. A high concentration of Ag2S as controlling agents reduced the concentration of free Ag+in the solution, decreased the rate of Ag+reduction, and promoted the formation of the decahedral twinned nanoparticle. In the subsequent reaction, Ag+ions were gradually released from Ag2S colloids into the solution, keeping the equilibrium concentrations of in soluble and soluble salts. The twincrystal nanparticles fast grew into silver nanowires with the adsorption of PVP on the{100} facets. When the concentration of Na2S gradually increased (rang from2.0mM to3.5mM), silver nanowires with large diameters were obtained.
3. Silver nanowires were obtained using CuCl2as controlling agents. The results show that AgCl colloids were formed from Cl-and free Ag+in the solution, reducing the concentration of Ag+ions in solution, decreasing the rate of Ag+reduction, and resulting in formation of multiply twinned seeds of decahedral shape. In the subsequent reaction, Ag+ions were gradually released from AgCl colloids into the solution. Cu2+was reduced Cu+, and then Cu+was oxidized Cu to consume O2and thus to prevent the silver seeds from being etched by Cr/O2.These multiply twinned seeds of decahedral shape can grew into silver nanowires due to selective adsorption of PVP on{100} facets.
4. Wormlike Ag/ZnO core-shell structures were synthesized by microwave method with silver nanowires, zinc acetate, and triethanolamine (TEA) as raw materials. The structures were composed of single crystal Ag nanowires (core) and dense regular ZnO particles (shell) grown on Ag nanowires. Firecracker-like Ag/ZnO heterojunction was synthesized by hydrothermal method using silver nanowires, zinc nitrate, and hexamethylene tetramine (HMT) as raw materials. The structures were formed by the growth of about100nm ZnO nanorods perpendicular to the axis of Ag nanowires.
引文
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