静电纺丝技术制备二氧化钛纳米材料与表征
摘要
在过去的十年中,静电纺丝技术作为一种简单而又快捷地制备一维纳米-亚微米材料的方法获得了迅速的发展,并逐渐成为纳米材料研究领域的热点。静电纺丝是基于高压静电场下导电流体产生高速喷射的原理发展而来,其基本过程是:聚合物溶液或熔体在几千至几万伏的高压静电场下克服表面张力而产生带电喷射流,溶液或熔体射流在喷射过程中干燥,并保持一定电荷量,最终落在接收板上形成纤维。静电纺丝制成的超细纤维膜具有多孔结构及较高的比表面积,在过滤、纳米复合材料、伤口敷料以及组织上支架等方面具有许多潜在的用途。
本文采用溶胶-凝胶法配制出有一定粘度的前驱溶液,采用静电纺丝技术成功地制备出PVP(K30)/Ti(SO_4)_2、PVP(K90)/Ti(SO_4)_2复合纤维以及PVP(K90)+PMMA/ Ti(OC_4H_9)_4、PMMA/Al((CH_3)_2CHO)_3纳米带,经过高温焙烧成为多孔空心二氧化钛纳米纤维、柔性二氧化钛纳米纤维、二氧化钛纳米带以及氧化铝纳米带。
对工艺条件的影响进行了系统的研究,发现PVP(PMMA)浓度、电压、固化距离和无机盐的含量是影响复合纤维特性的主要因素。
二氧化钛纳米纤维直径在100-200nm,长度为200μm。二氧化钛、氧化铝纳米带宽度在8-15μm,长度为200-300μm。利用XRD、TEM、SEM、TG-DTA、FTIR等手段对样品进行了表征。结果表明不同于以往所报道的单晶纳米纤维、纳米带,本实验中所制备的纳米纤维、纳米带呈现出典型的多晶结构,这种新结构纳米纤维、纳米带的合成为纳米材料的制备提供了一条新途径。
As a simple and quick method for preparation of nano- or submicrometer fibers, great progress has been made in electrospinning technique in the past decade. Therefore, electrospinning technique has become one of the current studied subjects in the nanomaterials research field. Electrospinning origins from that electrically charged fluid is forced jets in the high voltage electrostatic field. Electrospinning occurs when the electrical forces at the surface of a polymer solution or melt overcome the surface tension and cause an electrically charged jet to eject. When the jet is dried or solidified, an electrically charged fiber remains. This charged fiber can be directed or accelerated by electrical forces and then collected in mats or other useful geometrical forms. Nonwoven membranes composed of electrospun fibers have a large specific surface area and small pore size compared with commercial textiles, and have many potential applications in the fields of filters, nanocomposites, wound dressings and engineering scaffolds.
In this dissertation, sol-gel method was applied to prepare the precursor solution with a viscosity, and electrospinning technique was used to fabricate PVP(K30)/Ti(SO_4)_2, PVP(K90)/Ti(SO_4)_2, PVP(K90)+PMMA/Ti(OC_4H_9)_4、PMMA/Al((CH_3)_2CHO)_3 composite nanoribbons. TiO_2 nanofibers with porous surface, TiO_2 nanofibers with flexibility, TiO_2 nanoribbons and Al_2O_3 nanoribbons were obtained by calcinations of the above relevant composite microfibers.
The morphology of fibers were discussed by adjusting all the important parameters such as concentration of PVP(PMMA), voltage, distance between tip and collector, the mass of metal salts added to the sol. It was found that these factors were the main factors affecting the properties of the composites.
The TiO_2 nanofibers with diameters of 100-200nm and a length of 200μm. The TiO_2, Al_2O_3 nanoribbons with a width of 8-15μm and a length of 200-300μm.The samples were characterized with XRD, TEM, SEM, TG-DTA and FTIR in detail. It was indicated that the as-prepared nanofibers and nanoribbons exhibited polycrystalline structure which were different from monocrystalline structures of the TiO_2 nanofibers and TiO_2, Al_2O_3 nanoribbons previously reported. The synthesis of the nanoribbon with this new microstructure might provide a novel route to the nanomaterials.
本文采用溶胶-凝胶法配制出有一定粘度的前驱溶液,采用静电纺丝技术成功地制备出PVP(K30)/Ti(SO_4)_2、PVP(K90)/Ti(SO_4)_2复合纤维以及PVP(K90)+PMMA/ Ti(OC_4H_9)_4、PMMA/Al((CH_3)_2CHO)_3纳米带,经过高温焙烧成为多孔空心二氧化钛纳米纤维、柔性二氧化钛纳米纤维、二氧化钛纳米带以及氧化铝纳米带。
对工艺条件的影响进行了系统的研究,发现PVP(PMMA)浓度、电压、固化距离和无机盐的含量是影响复合纤维特性的主要因素。
二氧化钛纳米纤维直径在100-200nm,长度为200μm。二氧化钛、氧化铝纳米带宽度在8-15μm,长度为200-300μm。利用XRD、TEM、SEM、TG-DTA、FTIR等手段对样品进行了表征。结果表明不同于以往所报道的单晶纳米纤维、纳米带,本实验中所制备的纳米纤维、纳米带呈现出典型的多晶结构,这种新结构纳米纤维、纳米带的合成为纳米材料的制备提供了一条新途径。
As a simple and quick method for preparation of nano- or submicrometer fibers, great progress has been made in electrospinning technique in the past decade. Therefore, electrospinning technique has become one of the current studied subjects in the nanomaterials research field. Electrospinning origins from that electrically charged fluid is forced jets in the high voltage electrostatic field. Electrospinning occurs when the electrical forces at the surface of a polymer solution or melt overcome the surface tension and cause an electrically charged jet to eject. When the jet is dried or solidified, an electrically charged fiber remains. This charged fiber can be directed or accelerated by electrical forces and then collected in mats or other useful geometrical forms. Nonwoven membranes composed of electrospun fibers have a large specific surface area and small pore size compared with commercial textiles, and have many potential applications in the fields of filters, nanocomposites, wound dressings and engineering scaffolds.
In this dissertation, sol-gel method was applied to prepare the precursor solution with a viscosity, and electrospinning technique was used to fabricate PVP(K30)/Ti(SO_4)_2, PVP(K90)/Ti(SO_4)_2, PVP(K90)+PMMA/Ti(OC_4H_9)_4、PMMA/Al((CH_3)_2CHO)_3 composite nanoribbons. TiO_2 nanofibers with porous surface, TiO_2 nanofibers with flexibility, TiO_2 nanoribbons and Al_2O_3 nanoribbons were obtained by calcinations of the above relevant composite microfibers.
The morphology of fibers were discussed by adjusting all the important parameters such as concentration of PVP(PMMA), voltage, distance between tip and collector, the mass of metal salts added to the sol. It was found that these factors were the main factors affecting the properties of the composites.
The TiO_2 nanofibers with diameters of 100-200nm and a length of 200μm. The TiO_2, Al_2O_3 nanoribbons with a width of 8-15μm and a length of 200-300μm.The samples were characterized with XRD, TEM, SEM, TG-DTA and FTIR in detail. It was indicated that the as-prepared nanofibers and nanoribbons exhibited polycrystalline structure which were different from monocrystalline structures of the TiO_2 nanofibers and TiO_2, Al_2O_3 nanoribbons previously reported. The synthesis of the nanoribbon with this new microstructure might provide a novel route to the nanomaterials.
引文
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