贵金属纳米粒子负载的电纺纤维制备及其性能研究
发布时间：2019-03-09 18:17
【摘要】：静电纺丝技术是一种制备纳米纤维的有效手段,其制备方法简单,原材料广泛,纤维形貌可控并且可以连续制备。为了拓展静电纺丝纤维的应用范围,电纺纤维常与其他功能材料复合。贵金属纳米粒子是一种具有诸多独特理化特性的功能材料,以贵金属纳米粒子复合的电纺纤维在SERS、催化、传感等领域具有广泛的应用。如何通过简单有效的方法制备贵金属纳米粒子负载的电纺复合纤维是目前存在的主要挑战。基于该问题,我们以电纺聚丙烯酸(PAA)/聚乙烯醇(PVA)为基体材料,利用贵金属纳米粒子与纤维之间的相互作用,通过简单的浸泡和混纺等方法将不同形貌的贵金属纳米粒子与电纺纤维复合。主要研究内容及结果如下:(1)以表面带正电的金纳米粒子为表面增强拉曼光谱(Surface-enhanced Raman spectroscopy,SERS)基底构筑单元,利用金纳米粒子与交联处理后的聚丙烯酸(PAA)/聚乙烯醇(PVA)电纺纤维之间的静电作用,通过浸泡的方法将金纳米粒子组装在电纺纤维的表面。所得的复合纤维具有优异的SERS增强效果和SERS信号均匀性。通过基底上不同深度点的SERS性能检测,证明了该复合纤维膜在深度方向上也表现出优异的增强效果,说明金纳米粒子负载的电纺纤维膜为优异的3D SERS基底材料。(2)通过类似的简单浸泡方法将各项异性的金纳米棒负载在电纺PAA/PVA纤维的表面并探索了纺丝时间、浸泡时间以及金纳米棒溶胶的浓度对复合纤维SERS性能的影响。结果表明,随着纺丝时间和金纳米棒溶胶浓度的增加,复合纤维的SERS增强效果逐渐增加;随着浸泡时间的增加,复合纤维的SERS性能先增加后在12 h达到平衡。最终所得的复合纤维具有良好的SERS增强效果和优异的均匀性,并且在放置45天之后仍具有优异的增强效果。(3)另一种各项异性纳米粒子——钯纳米立方体通过类似的方法被负载在电纺PAA/PVA纤维的表面并以4-硝基苯酚催化还原的反应检测了所得复合纤维的催化性能。最终结果表明,钯纳米立方体负载的PAA/PVA电纺复合纤维具有优异的催化活性和重复性,能够快速地催化4-硝基苯酚的还原,并且在6次的重复催化中4-硝基苯酚的转化率均能达到97%以上。(4)通过先混纺后浸泡的方法制备了纤维内部和表面都负载纳米粒子的电纺PAA/PVA复合纤维。金纳米粒子通过混纺的方法分散在电纺纤维PAA/PVA的内部,随后通过浸泡在不同的贵金属纳米粒子溶胶中,在静电作用的驱动下将不同形貌的贵金属纳米粒子负载在纤维的表面,最终得到了纤维内部和表面都负载贵金属纳米粒子的高纳米粒子负载量的复合纤维。此外,对复合纤维的SERS和催化性能进行了检测。结果表明,高负载量纳米粒子复合纤维的SERS性能和催化性能比低负载量纳米粒子的复合纤维更加优异。
[Abstract]:Electrospinning is an effective method for the preparation of nanofibers. The preparation method is simple, the raw materials are wide, the morphology of the fibers is controllable and can be prepared continuously. In order to expand the application range of electrospun fibers, electrospun fibers are often combined with other functional materials. Precious metal nanoparticles are a kind of functional material with many unique physical and chemical properties. Electrospun fibers composed of precious metal nanoparticles have a wide range of applications in SERS, catalysis, sensing and other fields. How to prepare precious metal nanoparticles loaded electrospun composite fibers by a simple and effective method is the main challenge at present. Based on this problem, we used electrospun polyacrylic acid (PAA) / polyvinyl alcohol (PVA) as matrix material, and made use of the interaction between precious metal nanoparticles and fiber. The precious metal nanoparticles with different morphologies were mixed with electrospun fibers by simple immersion and blending. The main contents and results are as follows: (1) the surface positively charged gold nanoparticles were used as the substrate building unit of surface-enhanced Raman spectroscopy (Surface-enhanced Raman spectroscopy,SERS). Using the electrostatic interaction between gold nanoparticles and polyacrylic acid (PAA) / polyvinyl alcohol (PVA) electrospun fibers, gold nanoparticles were assembled on the surface of electrospun fibers by immersion. The obtained composite fibers have excellent SERS enhancement effect and SERS signal uniformity. By testing the SERS performance of different depth points on the substrate, it is proved that the composite fiber membrane also shows excellent enhancement effect in the depth direction. The results show that the gold nanoparticles loaded electrospun fiber films are excellent 3D SERS substrate materials. (2) the anisotropic gold nanorods were loaded on the surface of electrospun PAA/PVA fibers by a similar simple immersion method and the spinning time was explored. The effect of immersion time and the concentration of gold nanorods sol on the properties of composite fiber SERS. The results showed that with the increase of spinning time and sol concentration of gold nanorods, the SERS strengthening effect of the composite fibers increased gradually, and the SERS properties of the composite fibers increased first and then reached equilibrium at 12 h with the increase of immersion time. The resulting composite fiber has good SERS strengthening effect and excellent uniformity. And it still has excellent strengthening effect after 45 days. (3) another anisotropic nano-particle, palladium nano-cube, is loaded on the surface of electrospun PAA/PVA fiber by a similar method and treated with 4-nitrobenzene. The catalytic properties of the composite fibers were determined by phenol reduction reaction. The results show that the PAA/PVA electrospun composite fibers loaded with palladium nano-cubes have excellent catalytic activity and repeatability, and can catalyze the reduction of 4-nitrophenol rapidly. The conversion of 4-nitrophenol was over 97% in 6 times of repeated catalysis. (4) Electrospun PAA/PVA composite fibers loaded with nano-particles were prepared by blending and soaking. Gold nanoparticles are dispersed inside the electrospun fiber PAA/PVA by blending and then immersed in different sols of precious metal nanoparticles. The noble metal nanoparticles with different morphologies were loaded on the surface of the fibers under the action of static electricity. Finally, the composite fibers with high nano-particles loading on the inner and surface of the fibers were obtained. In addition, the SERS and catalytic properties of the composite fibers were tested. The results show that the SERS and catalytic properties of the composite fiber with high loading amount of nano-particles are better than those of the composite fiber with low loading amount of nano-particles.
【学位授予单位】：中北大学
【学位级别】：硕士
【学位授予年份】：2017
【分类号】：TB383.1;TQ340.64
本文编号：2437735
[Abstract]:Electrospinning is an effective method for the preparation of nanofibers. The preparation method is simple, the raw materials are wide, the morphology of the fibers is controllable and can be prepared continuously. In order to expand the application range of electrospun fibers, electrospun fibers are often combined with other functional materials. Precious metal nanoparticles are a kind of functional material with many unique physical and chemical properties. Electrospun fibers composed of precious metal nanoparticles have a wide range of applications in SERS, catalysis, sensing and other fields. How to prepare precious metal nanoparticles loaded electrospun composite fibers by a simple and effective method is the main challenge at present. Based on this problem, we used electrospun polyacrylic acid (PAA) / polyvinyl alcohol (PVA) as matrix material, and made use of the interaction between precious metal nanoparticles and fiber. The precious metal nanoparticles with different morphologies were mixed with electrospun fibers by simple immersion and blending. The main contents and results are as follows: (1) the surface positively charged gold nanoparticles were used as the substrate building unit of surface-enhanced Raman spectroscopy (Surface-enhanced Raman spectroscopy,SERS). Using the electrostatic interaction between gold nanoparticles and polyacrylic acid (PAA) / polyvinyl alcohol (PVA) electrospun fibers, gold nanoparticles were assembled on the surface of electrospun fibers by immersion. The obtained composite fibers have excellent SERS enhancement effect and SERS signal uniformity. By testing the SERS performance of different depth points on the substrate, it is proved that the composite fiber membrane also shows excellent enhancement effect in the depth direction. The results show that the gold nanoparticles loaded electrospun fiber films are excellent 3D SERS substrate materials. (2) the anisotropic gold nanorods were loaded on the surface of electrospun PAA/PVA fibers by a similar simple immersion method and the spinning time was explored. The effect of immersion time and the concentration of gold nanorods sol on the properties of composite fiber SERS. The results showed that with the increase of spinning time and sol concentration of gold nanorods, the SERS strengthening effect of the composite fibers increased gradually, and the SERS properties of the composite fibers increased first and then reached equilibrium at 12 h with the increase of immersion time. The resulting composite fiber has good SERS strengthening effect and excellent uniformity. And it still has excellent strengthening effect after 45 days. (3) another anisotropic nano-particle, palladium nano-cube, is loaded on the surface of electrospun PAA/PVA fiber by a similar method and treated with 4-nitrobenzene. The catalytic properties of the composite fibers were determined by phenol reduction reaction. The results show that the PAA/PVA electrospun composite fibers loaded with palladium nano-cubes have excellent catalytic activity and repeatability, and can catalyze the reduction of 4-nitrophenol rapidly. The conversion of 4-nitrophenol was over 97% in 6 times of repeated catalysis. (4) Electrospun PAA/PVA composite fibers loaded with nano-particles were prepared by blending and soaking. Gold nanoparticles are dispersed inside the electrospun fiber PAA/PVA by blending and then immersed in different sols of precious metal nanoparticles. The noble metal nanoparticles with different morphologies were loaded on the surface of the fibers under the action of static electricity. Finally, the composite fibers with high nano-particles loading on the inner and surface of the fibers were obtained. In addition, the SERS and catalytic properties of the composite fibers were tested. The results show that the SERS and catalytic properties of the composite fiber with high loading amount of nano-particles are better than those of the composite fiber with low loading amount of nano-particles.
【学位授予单位】：中北大学
【学位级别】：硕士
【学位授予年份】：2017
【分类号】：TB383.1;TQ340.64
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