离子液体中Ⅰ-ⅡB族纳/微米材料的制备
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摘要
离子液体作为一种新型的绿色环保溶剂,与传统溶剂相比,它具有很多独特的性质,如可忽略的蒸汽压、高热稳定性、很宽的液相温度、高极性、低毒性、宽电势窗等,被广泛的用于各领域。目前,已经利用离子液体合成出了纳米金属粒子、金属氧化物、多孔材料、分子筛等,为纳米材料的制备开辟了一条新的途径。
本文中通过把离子液体和超声波、微波加热相结合,采用一种快速、无毒、环境友好的绿色方法,合成了氧化锌纳米材料。采用离子液体-水为介质的体系下,通过液相法,简单有效的合成了硫化铜纳米材料和银纳米材料。用X-射线粉末衍射仪(XRD)、场发射扫描电镜(FESEM)、高分辨透射电镜(HRTEM)、紫外-可见光分光光度计(UV-Vis)和荧光分光光度计(PL)对样品进行了分析和表征。本硕士论文主要研究以下几个内容：
1.超声的空化作用可以使液体在高强度超声作用下形成气泡,并迅速的生长和爆炸性的溃灭,在气泡溃灭的瞬间能产生高温高压的环境,从而诱发高能化学反应。而离子液体具有低的蒸汽压,非常适合超声作用的环境。因此,在本论文中将超声作用和离子液体相结合,首次在离子液体[BMIM][PF6]超声辅助下制备出了形貌均匀、直径在50 nm左右、长度约为1-2μm的氧化锌纳米棒,并提出了改纳米棒的生长机制。实验发现由于离子液体[BMIM][PF6]的粘度较大,有效的控制了反应溶液中离子的扩散速度,非常有利于该纳米棒的形成。
2.微波加热能显著提高反应速度和反应选择性,且在加热的同时,能够快速的改变电场使离子极化,导致在反应系统中的晶体各项异性生长。同时,离子液体本身具有很高的极化率,是一种良好的微波吸收剂。两者相结合大大的缩短了反应合成时间。本论文中结合离子液体和微波加热的优点,首次在离子液体[BMIM][PF6]微波辅助下成功的制备出大小均匀、长径比较大、结晶性良好的氧化锌纳米棒,该纳米棒的直径在20 nm左右,长度在400～500nm左右。实验表明,该纳米棒具有良好的光学性能,在362nm处有明显的紫外吸收峰,并且在389 nm处有较强的紫外发射峰,而深能级发光较弱。实验中还发现离子液体[BMIM][PF6]对纳米棒的形成起着至关重要的作用,并提出了该纳米棒的生长机制。
3.液相沉淀法是一种合成纳米材料最简单普遍的方法。本论文中以氯化铜和硫代乙酰胺为反应原料,室温下运用液相沉淀法首次在[BMIM][PF6]中成功制备出硫化铜花状球纳／微米材料。该花状球大小均匀、直径在1μm左右。从紫外-可见光光谱图可以看出,CuS花状球最强的紫外吸收峰位于268nm处。从荧光光谱图可以看出,该花状球在可见光区存在两强发射峰,分别在432 nm和570 nm处,表明该样品具有很好的光学性质。实验发现,离子液体[BMIM][PF6]在该花状球的形成过程中起着重要的作用。
4.本论文运用液相还原法以硝酸银和维C为反应原料,柠檬酸为配位剂,室温下在离子液体[BMIM][PF6]的水溶液中合成出了大小均匀的花状银纳米结构。研究发现该花状结构是由很多厚度在30 nm左右的花瓣组成的。实验发现,反应时间和离子液体对产物形貌有重要的影响。
As a new type of green environment friendly solvent, room temperature ionic liquid(RTIL) have great advantage over the traditional solvents, such as negligible vapor pressure, low melting points, wide range of liquid temperatures, high polarity, low toxicity, large electrochemical window, high ionic conductively and thermal stability, etc.. So, RTIL have been widely used in the organic chemical reactions, separation, and electrochemical. Presently, RTIL have been widely used in the synthesis of metal nanoparticles, metal-oxide, nano-porous materials, molecular sieve and so on, and provide a new route for the synthesis of nano-materials.
In this paper, ZnO nano-materials have been synthesized the ultrasonic or microwave irradiation method in the RTIL [BMIM][PF6]. This method is a rapid, nontoxic and environment friendly synthesis route. CuS and Ag nano-materials have been synthesized via liquid phase method in the ionic liquid ([BMIM][PF6]) aqueous solution. The products were characterized by XRD, EDX, FESEM, TEM, HRTEM, UV-Vis and PL techniques. The main points can be summarized as followed:
1. Sonochemistry is a result of acoustic cavitations:the formation, growth, and implosive collapse of bubbles in a liquid. The chemical effects of cavitations are highly dependent on the contents of the collapsing bubble and hence on the choice of solvent. However, the solvent with lower vapor pressure would favor the sonochemical reaction. In this meaning, RTILs are suitable candidates to play such role. So, Rod-like ZnO nanocrystals have been synthesized via an ultrasound-assisted way in the ionic liquid aqueous solution. The as-prepared ZnO nanorods have a diameter of about 50 nm and a length of 1-2μm. A plausible four-step mechanism was proposed to explain the formation of ZnO nanorods. It was found that the lowered ion diffusion velocity in the water-ionic liquid medium could largely contribute to the formation of the ZnO nanorods.
2. The microwave-assisted RTILs method is a facile and environment friendly route to the preparation nanostructured materials. Heating by microwave can accelerate the reaction evidently, and the polarization of ions under the rapidly changing electric field of the microwave results in anisotropic growth of crystals. While, the RTILs with the high ionic conductivity and polarizability of cations is an excellent microwave absorbing agent, leading to a high heating rate and a shorten reaction time. By combing the advantages of both RTILs and microwave heating, ZnO nanorods have been successfully synthesized. The results showed that the as-prepared ZnO nanorods have a diameter of about 20 nm and a length of 400～500 nm, and the ionic liquid [BMIM][PF6] played a key role. A plausible three-step mechanism was proposed to explain the formation of ZnO nanorods. This facile and environment friendly synthetic strategy many open new route to the preparation of other ID functional nanomatericals.
3. Liquid precipitation method is one of the most popular methods of synthesis nanometer powders. CuS flower-like sphere micro/nanostructure have successfully synthesized via liquid precipitation method by the reaction between CuCl2·2H2O and TAA in the ionic liquid [BMIM][PF6] aqueous solution. The results showed that the as-prepared CuS flower-like sphere have a diameter of about lμm and the ionic liquid [BMIM][PF6] played a key role. UV-Vis curves indicate a single peak centered at 268 nm. PL curves indicated the two peaks centered at 432 nm and 570 nm. The results showed the CuS flower-like sphere micro/nanostructure have a good optical properties.
4. The flower-like Ag nanostructure was synthesized via liquid phase reduction method in the presence of silver nitrate, ascorbic acid and citric acid in the ionic liquid [BMIM][PF6] aqueous solution at room temperature. The flower-like Ag nanostructure is composed of nano-petals of the diameter of about 30 nm. The results showed reaction time and IL play important roles in the formation of Ag nanostructure.
本文中通过把离子液体和超声波、微波加热相结合,采用一种快速、无毒、环境友好的绿色方法,合成了氧化锌纳米材料。采用离子液体-水为介质的体系下,通过液相法,简单有效的合成了硫化铜纳米材料和银纳米材料。用X-射线粉末衍射仪(XRD)、场发射扫描电镜(FESEM)、高分辨透射电镜(HRTEM)、紫外-可见光分光光度计(UV-Vis)和荧光分光光度计(PL)对样品进行了分析和表征。本硕士论文主要研究以下几个内容：
1.超声的空化作用可以使液体在高强度超声作用下形成气泡,并迅速的生长和爆炸性的溃灭,在气泡溃灭的瞬间能产生高温高压的环境,从而诱发高能化学反应。而离子液体具有低的蒸汽压,非常适合超声作用的环境。因此,在本论文中将超声作用和离子液体相结合,首次在离子液体[BMIM][PF6]超声辅助下制备出了形貌均匀、直径在50 nm左右、长度约为1-2μm的氧化锌纳米棒,并提出了改纳米棒的生长机制。实验发现由于离子液体[BMIM][PF6]的粘度较大,有效的控制了反应溶液中离子的扩散速度,非常有利于该纳米棒的形成。
2.微波加热能显著提高反应速度和反应选择性,且在加热的同时,能够快速的改变电场使离子极化,导致在反应系统中的晶体各项异性生长。同时,离子液体本身具有很高的极化率,是一种良好的微波吸收剂。两者相结合大大的缩短了反应合成时间。本论文中结合离子液体和微波加热的优点,首次在离子液体[BMIM][PF6]微波辅助下成功的制备出大小均匀、长径比较大、结晶性良好的氧化锌纳米棒,该纳米棒的直径在20 nm左右,长度在400～500nm左右。实验表明,该纳米棒具有良好的光学性能,在362nm处有明显的紫外吸收峰,并且在389 nm处有较强的紫外发射峰,而深能级发光较弱。实验中还发现离子液体[BMIM][PF6]对纳米棒的形成起着至关重要的作用,并提出了该纳米棒的生长机制。
3.液相沉淀法是一种合成纳米材料最简单普遍的方法。本论文中以氯化铜和硫代乙酰胺为反应原料,室温下运用液相沉淀法首次在[BMIM][PF6]中成功制备出硫化铜花状球纳／微米材料。该花状球大小均匀、直径在1μm左右。从紫外-可见光光谱图可以看出,CuS花状球最强的紫外吸收峰位于268nm处。从荧光光谱图可以看出,该花状球在可见光区存在两强发射峰,分别在432 nm和570 nm处,表明该样品具有很好的光学性质。实验发现,离子液体[BMIM][PF6]在该花状球的形成过程中起着重要的作用。
4.本论文运用液相还原法以硝酸银和维C为反应原料,柠檬酸为配位剂,室温下在离子液体[BMIM][PF6]的水溶液中合成出了大小均匀的花状银纳米结构。研究发现该花状结构是由很多厚度在30 nm左右的花瓣组成的。实验发现,反应时间和离子液体对产物形貌有重要的影响。
As a new type of green environment friendly solvent, room temperature ionic liquid(RTIL) have great advantage over the traditional solvents, such as negligible vapor pressure, low melting points, wide range of liquid temperatures, high polarity, low toxicity, large electrochemical window, high ionic conductively and thermal stability, etc.. So, RTIL have been widely used in the organic chemical reactions, separation, and electrochemical. Presently, RTIL have been widely used in the synthesis of metal nanoparticles, metal-oxide, nano-porous materials, molecular sieve and so on, and provide a new route for the synthesis of nano-materials.
In this paper, ZnO nano-materials have been synthesized the ultrasonic or microwave irradiation method in the RTIL [BMIM][PF6]. This method is a rapid, nontoxic and environment friendly synthesis route. CuS and Ag nano-materials have been synthesized via liquid phase method in the ionic liquid ([BMIM][PF6]) aqueous solution. The products were characterized by XRD, EDX, FESEM, TEM, HRTEM, UV-Vis and PL techniques. The main points can be summarized as followed:
1. Sonochemistry is a result of acoustic cavitations:the formation, growth, and implosive collapse of bubbles in a liquid. The chemical effects of cavitations are highly dependent on the contents of the collapsing bubble and hence on the choice of solvent. However, the solvent with lower vapor pressure would favor the sonochemical reaction. In this meaning, RTILs are suitable candidates to play such role. So, Rod-like ZnO nanocrystals have been synthesized via an ultrasound-assisted way in the ionic liquid aqueous solution. The as-prepared ZnO nanorods have a diameter of about 50 nm and a length of 1-2μm. A plausible four-step mechanism was proposed to explain the formation of ZnO nanorods. It was found that the lowered ion diffusion velocity in the water-ionic liquid medium could largely contribute to the formation of the ZnO nanorods.
2. The microwave-assisted RTILs method is a facile and environment friendly route to the preparation nanostructured materials. Heating by microwave can accelerate the reaction evidently, and the polarization of ions under the rapidly changing electric field of the microwave results in anisotropic growth of crystals. While, the RTILs with the high ionic conductivity and polarizability of cations is an excellent microwave absorbing agent, leading to a high heating rate and a shorten reaction time. By combing the advantages of both RTILs and microwave heating, ZnO nanorods have been successfully synthesized. The results showed that the as-prepared ZnO nanorods have a diameter of about 20 nm and a length of 400～500 nm, and the ionic liquid [BMIM][PF6] played a key role. A plausible three-step mechanism was proposed to explain the formation of ZnO nanorods. This facile and environment friendly synthetic strategy many open new route to the preparation of other ID functional nanomatericals.
3. Liquid precipitation method is one of the most popular methods of synthesis nanometer powders. CuS flower-like sphere micro/nanostructure have successfully synthesized via liquid precipitation method by the reaction between CuCl2·2H2O and TAA in the ionic liquid [BMIM][PF6] aqueous solution. The results showed that the as-prepared CuS flower-like sphere have a diameter of about lμm and the ionic liquid [BMIM][PF6] played a key role. UV-Vis curves indicate a single peak centered at 268 nm. PL curves indicated the two peaks centered at 432 nm and 570 nm. The results showed the CuS flower-like sphere micro/nanostructure have a good optical properties.
4. The flower-like Ag nanostructure was synthesized via liquid phase reduction method in the presence of silver nitrate, ascorbic acid and citric acid in the ionic liquid [BMIM][PF6] aqueous solution at room temperature. The flower-like Ag nanostructure is composed of nano-petals of the diameter of about 30 nm. The results showed reaction time and IL play important roles in the formation of Ag nanostructure.
引文
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