静电纺丝技术构筑一维功能纳米结构材料
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摘要
磁光双功能纳米材料因其同时具备磁性质和发光性质,在药物靶向、荧光标记、荧光成像等领域有潜在的应用价值。目前,磁光双功能纳米材料的研究主要集中在磁光双功能纳米颗粒的制备方面,而一维磁光纳米材料的制备与性质研究报道很少。因此,制备一维磁光纳米材料并研究其性质是一个迫切而有意义的研究课题。纳米ZnS、NiO具有特殊的光学、电学和光催化特性,可广泛应用于光催化降解废有机污染物。静电纺丝技术作为一种制备一维纳米材料的有效方法,具有成本低廉、设备简单、灵活多样、产物的尺寸和形貌容易调控等优点。本论文中采用静电纺丝技术,制备了发射红光和绿光的磁光双功能复合纳米纤维和磁光双功能两股并行复合纳米纤维束,以及红-黄-绿光色可调的荧光纳米纤维和磁光双功能两股并行复合纳米纤维束,并研究了它们的磁性质、发光性质以及磁、光性质的相互影响。同时采用静电纺丝技术制备了ZnS纳米纤维和NiO空心纳米管并研究了其光催化性质。
1.通过单轴静电纺丝技术,将稀土配合物、Fe3O4纳米粒子和聚乙烯毗咯烷酮复合,构筑了发射红色荧光的Fe3O4/Eu(BA)3phen/PVP和发射绿色荧光的Fe3O4/Tb(BA)3phen/PVP磁光双功能复合纳米纤维,并研究了纤维形貌、最佳配台物掺入浓度以及掺入不同量Fe3O4纳米粒子对荧光性质和磁性质的影响。结果表明,所制备的Fe3O4/Eu(BA)3phen/PVP和Fe3O4/Tb(BA)3phen/PVP磁光双功能复合纳米纤维的直径为200-250nm。Fe3O4/Eu(B A)3phen/P VP复合纳米纤维在274nm紫外光激发下,在592m和616nm处出现Eu离子的橙光和红光发射峰,且Eu(BA)3phen:PVP的最佳比例为15%; Fe3O4/Tb(BA)3phen/PVP复合纳米纤维在276nm紫外光激发下,在490nm和545nm处出现Tb离子的绿色发射峰,且Tb(BA)3phen:PVP的最佳比例为20%。随着Fe3O4纳米粒子掺入量的增加,复合纳米纤维的荧光强度显著降低,饱和磁化强度增大。
2.为了降低黑色的Fe3O4纳米粒子对激发光及发射光的强烈光吸收而导致磁光纳米纤维荧光强度的大幅下降,本文自行设计并制作了具有并列双喷丝头的并轴静电纺丝装置,首次构筑了Fe3O4/PVP//Eu(BA)3phen/PVP和Fe3O4/PVP//Tb(BA)3phen/PVP磁光双功能两股并行复合纳米纤维束。在两股并行复合纳米纤维束中,Fe3O4纳米粒子只分散在两股并行复合纳米纤维束的一股纤维中,而稀土配合物分散在另一股纤维中,从而使稀土配合物与Fe3O4纳米粒子有效地分离,减少了Fe3O4对稀土配合物荧光的吸收。结果表明,与单轴静电纺丝技术制备的磁光复合纳米纤维相比,当饱和磁化强度相同时,两股并行复合纳米纤维束具有更高的荧光强度,且增大Fe3O4纳米粒子的含量对荧光强度的影响较小。这种磁光双功能两股并行复合纳米纤维束兼具优异的磁性和较强的荧光强度。
3.首次将发射红光的Eu(BA)3phen配合物、发射绿光的Tb(BA)3phen配合物和聚乙烯吡咯烷酮复合,利用单轴静电纺丝技术制备了一系列红-黄-绿荧光颜色可调的PVP/[Tb(BA)3phen+Eu(BA)3phen]复合纳米纤维。样品的发射光谱分析表明,同时掺入Eu(BA)3phen和Tb(BA)3phen的复合纤维既有Eu3+的橙光和红光发射,又有Tb3+的绿光发射,且复合纤维可通过掺入不同比例的Eu(BA)3phen和Tb(BA)3phen,实现在276nm单一激发波长下红-黄-绿的荧光可调控性。
4.首次将Eu(BA)3phen配合物、Tb (BA)3phen配合物和Fe3O4纳米粒子,通过并轴静电纺丝技术构筑了一种既具有较高的荧光强度和磁性可调性,又具有发光颜色可调控特性的Fe3O4/PVP//[Tb(BA)3phen+Eu(BA)3phen]/PVP磁光双功能两股并行复合纳米纤维束。其中,Fe3O4纳米粒子均匀分散在两股并行复合纳米纤维束的一股纤维中,而Eu(BA)3phen配合物和Tb(BA)3phen配合物分散在另一股纤维中。与Fe3O4/[Tb(BA)3phen+Eu(BA)3phen]/PVP复合纳米纤维相比,在相同饱和磁化强度时,Fe3O4/PVP//[Tb(BA)3phen+Eu(BA)3phen]/PVP两股并行复合纳米纤维具有更高的荧光强度。Fe3O4/PVP//[Tb(BA)3phen+Eu(BA)3phen]/PVP两股并行复合纳米纤维束的磁性可通过Fe3O4纳米粒子掺入量来调节,同时荧光颜色可通过Tb (BA)3phen配合物和Eu(BA)3phen配合物的掺入比例在红-黄-绿范围内调节,从而实现了磁-光色可调性。
5.将单轴静电纺丝技术与硫化工艺相结合,制备了直径为200±79nm的ZnS纳米纤维。在紫外光照射60min后,ZnS纳米纤维对罗丹明B的光催化降解率达到了98.8%,ZnS纳米纤维具有优于ZnO纳米纤维的光催化性能。
6.利用同轴静电纺丝技术制备了Ni(NO3)2/PVP空心纳米纤维,再经焙烧制备了外径为185nm,内径为40nm的NiO纳米管,NiO纳米管的光催化性能优于NiO纳米纤维。
Magnetic-photoluminescent nanomaterials have potential applications in drug targeting, fluorescence labeling and fluorescence imaging, etc due to their unique magnetic and photoluminescent bifunctional properties. At present, some investigations on magnetic-photoluminescent bifunctional nanoparticles have been reported, however, the fabrication and the properties research of one-dimensional magnetic-photoluminescent bifunctional nanomaterials are rarely reported in the literature, and has become an imperative and meaningful subject of study. Nano-ZnS and nano-NiO have special optical, electrical and catalytic properties, which have broad application prospects in photocatalytic degradation of organic pollutants. Electrospinning is an efficient way of fabricating one-dimensional nanomaterials. Compared with other techniques, electrospinning possesses a lot of priorities, such as more cost-effective, simpler, more flexible, and the size and morphology of the product are easy to control, etc. In this thesis, the red and green fluorescence magnetic-photoluminescent bifunctional composite nanofibers, bistrand aligned composite nanofibers bundles, and the luminescent nanofibers and magnetic-photoluminescent bifunctional bistrand aligned composite nanofibers bundle with tunable emitting colour of red-yellow-green were fabricated by electrospinning. The magnetic and luminescent properties and their interactions between them were also investigated. Besides, Zn.S nanofibers and NiO nanotubes were prepared via electrospinning, respectively, and their photocatalytic properties were investigated.
1. Red fluorescence Fe3O4/Eu(BA)3phen/PVP and green fluorescence Fe3O4/Tb(BA)3pben/PVP magnetic-photoluminescent bifunctional composite nanofibers based on ferroferric oxide nanoparticles, europium complex Eu(BA)3phen or terbium complexes Tb(BA)3phen and PVP were fabricated by single axial electrospinning. The morphology of the fibers, optimum adding concentration of the rare earth comlex and the impact of introducing various amounts of Fe3O4nanoparticles(NPs) on the magnetic and luminescent properties were studied. Results show that the diameters of the two kinds of nanofibers are200-250nm. The Fe3O4/Eu(BA)3phen/PVP composite nanofibers exhibited red emissions of predominant peaks at592nm and616nm of Eu3+under the excitation of274nm ultraviolet light, and the optimum concentration of Eu(BA)3phen to PVP as15%; Fe3O4/Tb(BA)3phen/PVP composite nanofibers exhibited green emissions of predominant peaks at490nm and545nm of Tb3+under the excitation of276nm ultraviolet light, and the optimum concentration of Tb(BA)3phen to PVP is20%. With introducing more Fe3O4nanoparticles into the composite nanofibers,the luminescent intensity of the fibers is greatly decreased while the saturation magnetization is enhanced.
2. In order to decrease the absorption of the exciting and emitting light when black-coloured Fe3O4nanoparticles were scattered in the composite nanofibers. Fe3O4/PVP//Eu(BA)3phen/PVP and Fe3O4/PVP//Tb(BA)3phen/PVP magnetic-photoluminescent bifunctional bistrand aligned composite nanofibers bundles were fabricated by employing a homemade parallel axial electrospinning setup with the side by side dual spinnerets for the first time. Fe3O4NPs and rare earth complex were respectively dispersed into the individual strand fiber of the bistrand aligned composite nanofibers bundles, so that the rare earth complex was effectively isolated from Fe3O4NPs, which greatly reduced the effect of Fe3O4NPs on the luminescence of complex. The results indicated that the fluorescence intensity of bistrand aligned composite nanofibers bundles was obviously higher than that of the above composite nanofibers prepared by single axial electrospinning when the two nanostructures have the same saturation magnetization. The luminescent intensity is hardly decreased when more Fe3O4NPs were added. This kind of magnetic-photoluminescent bifunctional bistrand aligned composite nanofibers bundles possesses excellent magnetic properties and higher fluorescence intensity.
3. A new kind of color-tunable PVP/[Tb(BA)3phen+Eu(BA)3phen] luminescent composite nanofibers which consisted of europium complex, terbium complex and PVP were prepared by single axial electrospinning for the first time. The emission spectrum analysis of samples showed that the emitting color of the PVP/[Tb(BA)3phen+Eu(BA)3phen] luminescent composite nanofibers can be tuned under the excitation of276nm single-wavelength ultraviolet light by adjusting the ratio of terbium and europium complexes in a wide color range of red-yellow-green.
4. For the first time, a new kind of Fe3O4/PVP//[Tb(BA)3phen+Eu(BA)3phen]/PVP magnetic-photoluminescent bifunctional bistrand aligned composite nanofibers bundles with high fluorescence intensity, magnetism-tunable and colour-tuned characteristics were successfully prepared by parallel axial electrospinning. Fe3O4NPs and rare earth complex (Tb(BA)3phen and Eu(BA)3phen) were respectively dispersed into the individual strand fiber of the bistrand aligned composite nanofibers bundles. The fluorescence intensity of the Fe3O4/PVP//[Tb(BA)3phen+Eu(BA)3phen]/PVP bistrand aligned composite nanofibers bundles was obviously higher than that of Fe3O4/[Tb(BA)3phen+Eu(BA)3phen]/PVP composite nanofibers when they have the same saturation magnetization. The magnetism of the bistrand aligned composite nanofibers bundles could be tuned by adding different amounts of Fe3O4nanoparticles. The emitting color of the Fe3O4/PVP//[Tb(BA)3phen+Eu(BA)3phen]/PVP bistrand aligned composite nanofibers bundles can be tuned by adjusting the ratio of europium and terbium complexes in a wide color range of red-yellow-green. Thus, a kind of magnetic and color-tunable bifunctional bistrand aligned composite nanofibers bundles were obtained.
5. ZnS nanofibers with the diameters of200±79nm were prepared by the combination of single axial electrospinning with vulcanization technology, and their photocatalytic properties were investigated. The results showed that the photocatalytic degradation rate of ZnS nanofibers on rhodamine B was higher than ZnO nanofibers, and reached up to98.8%after UV illumination for60min.Therefore, the prepared ZnS nanofibers had outstanding photocatalytic property.
6. Ni(NO3)2/PVP hollow composite nanofibers were prepared by coaxial electrospinning, and NiO nanotubes with the outside diameters of185nm and inside diameters of40nm were fabricated by calcining the relevant composite nanofibers. The photocatalytic properties were studied. The results showed that the photocatalytic degradation effect of NiO nanotubes on rhodamine B was better than NiO nanofibers.
1.通过单轴静电纺丝技术,将稀土配合物、Fe3O4纳米粒子和聚乙烯毗咯烷酮复合,构筑了发射红色荧光的Fe3O4/Eu(BA)3phen/PVP和发射绿色荧光的Fe3O4/Tb(BA)3phen/PVP磁光双功能复合纳米纤维,并研究了纤维形貌、最佳配台物掺入浓度以及掺入不同量Fe3O4纳米粒子对荧光性质和磁性质的影响。结果表明,所制备的Fe3O4/Eu(BA)3phen/PVP和Fe3O4/Tb(BA)3phen/PVP磁光双功能复合纳米纤维的直径为200-250nm。Fe3O4/Eu(B A)3phen/P VP复合纳米纤维在274nm紫外光激发下,在592m和616nm处出现Eu离子的橙光和红光发射峰,且Eu(BA)3phen:PVP的最佳比例为15%; Fe3O4/Tb(BA)3phen/PVP复合纳米纤维在276nm紫外光激发下,在490nm和545nm处出现Tb离子的绿色发射峰,且Tb(BA)3phen:PVP的最佳比例为20%。随着Fe3O4纳米粒子掺入量的增加,复合纳米纤维的荧光强度显著降低,饱和磁化强度增大。
2.为了降低黑色的Fe3O4纳米粒子对激发光及发射光的强烈光吸收而导致磁光纳米纤维荧光强度的大幅下降,本文自行设计并制作了具有并列双喷丝头的并轴静电纺丝装置,首次构筑了Fe3O4/PVP//Eu(BA)3phen/PVP和Fe3O4/PVP//Tb(BA)3phen/PVP磁光双功能两股并行复合纳米纤维束。在两股并行复合纳米纤维束中,Fe3O4纳米粒子只分散在两股并行复合纳米纤维束的一股纤维中,而稀土配合物分散在另一股纤维中,从而使稀土配合物与Fe3O4纳米粒子有效地分离,减少了Fe3O4对稀土配合物荧光的吸收。结果表明,与单轴静电纺丝技术制备的磁光复合纳米纤维相比,当饱和磁化强度相同时,两股并行复合纳米纤维束具有更高的荧光强度,且增大Fe3O4纳米粒子的含量对荧光强度的影响较小。这种磁光双功能两股并行复合纳米纤维束兼具优异的磁性和较强的荧光强度。
3.首次将发射红光的Eu(BA)3phen配合物、发射绿光的Tb(BA)3phen配合物和聚乙烯吡咯烷酮复合,利用单轴静电纺丝技术制备了一系列红-黄-绿荧光颜色可调的PVP/[Tb(BA)3phen+Eu(BA)3phen]复合纳米纤维。样品的发射光谱分析表明,同时掺入Eu(BA)3phen和Tb(BA)3phen的复合纤维既有Eu3+的橙光和红光发射,又有Tb3+的绿光发射,且复合纤维可通过掺入不同比例的Eu(BA)3phen和Tb(BA)3phen,实现在276nm单一激发波长下红-黄-绿的荧光可调控性。
4.首次将Eu(BA)3phen配合物、Tb (BA)3phen配合物和Fe3O4纳米粒子,通过并轴静电纺丝技术构筑了一种既具有较高的荧光强度和磁性可调性,又具有发光颜色可调控特性的Fe3O4/PVP//[Tb(BA)3phen+Eu(BA)3phen]/PVP磁光双功能两股并行复合纳米纤维束。其中,Fe3O4纳米粒子均匀分散在两股并行复合纳米纤维束的一股纤维中,而Eu(BA)3phen配合物和Tb(BA)3phen配合物分散在另一股纤维中。与Fe3O4/[Tb(BA)3phen+Eu(BA)3phen]/PVP复合纳米纤维相比,在相同饱和磁化强度时,Fe3O4/PVP//[Tb(BA)3phen+Eu(BA)3phen]/PVP两股并行复合纳米纤维具有更高的荧光强度。Fe3O4/PVP//[Tb(BA)3phen+Eu(BA)3phen]/PVP两股并行复合纳米纤维束的磁性可通过Fe3O4纳米粒子掺入量来调节,同时荧光颜色可通过Tb (BA)3phen配合物和Eu(BA)3phen配合物的掺入比例在红-黄-绿范围内调节,从而实现了磁-光色可调性。
5.将单轴静电纺丝技术与硫化工艺相结合,制备了直径为200±79nm的ZnS纳米纤维。在紫外光照射60min后,ZnS纳米纤维对罗丹明B的光催化降解率达到了98.8%,ZnS纳米纤维具有优于ZnO纳米纤维的光催化性能。
6.利用同轴静电纺丝技术制备了Ni(NO3)2/PVP空心纳米纤维,再经焙烧制备了外径为185nm,内径为40nm的NiO纳米管,NiO纳米管的光催化性能优于NiO纳米纤维。
Magnetic-photoluminescent nanomaterials have potential applications in drug targeting, fluorescence labeling and fluorescence imaging, etc due to their unique magnetic and photoluminescent bifunctional properties. At present, some investigations on magnetic-photoluminescent bifunctional nanoparticles have been reported, however, the fabrication and the properties research of one-dimensional magnetic-photoluminescent bifunctional nanomaterials are rarely reported in the literature, and has become an imperative and meaningful subject of study. Nano-ZnS and nano-NiO have special optical, electrical and catalytic properties, which have broad application prospects in photocatalytic degradation of organic pollutants. Electrospinning is an efficient way of fabricating one-dimensional nanomaterials. Compared with other techniques, electrospinning possesses a lot of priorities, such as more cost-effective, simpler, more flexible, and the size and morphology of the product are easy to control, etc. In this thesis, the red and green fluorescence magnetic-photoluminescent bifunctional composite nanofibers, bistrand aligned composite nanofibers bundles, and the luminescent nanofibers and magnetic-photoluminescent bifunctional bistrand aligned composite nanofibers bundle with tunable emitting colour of red-yellow-green were fabricated by electrospinning. The magnetic and luminescent properties and their interactions between them were also investigated. Besides, Zn.S nanofibers and NiO nanotubes were prepared via electrospinning, respectively, and their photocatalytic properties were investigated.
1. Red fluorescence Fe3O4/Eu(BA)3phen/PVP and green fluorescence Fe3O4/Tb(BA)3pben/PVP magnetic-photoluminescent bifunctional composite nanofibers based on ferroferric oxide nanoparticles, europium complex Eu(BA)3phen or terbium complexes Tb(BA)3phen and PVP were fabricated by single axial electrospinning. The morphology of the fibers, optimum adding concentration of the rare earth comlex and the impact of introducing various amounts of Fe3O4nanoparticles(NPs) on the magnetic and luminescent properties were studied. Results show that the diameters of the two kinds of nanofibers are200-250nm. The Fe3O4/Eu(BA)3phen/PVP composite nanofibers exhibited red emissions of predominant peaks at592nm and616nm of Eu3+under the excitation of274nm ultraviolet light, and the optimum concentration of Eu(BA)3phen to PVP as15%; Fe3O4/Tb(BA)3phen/PVP composite nanofibers exhibited green emissions of predominant peaks at490nm and545nm of Tb3+under the excitation of276nm ultraviolet light, and the optimum concentration of Tb(BA)3phen to PVP is20%. With introducing more Fe3O4nanoparticles into the composite nanofibers,the luminescent intensity of the fibers is greatly decreased while the saturation magnetization is enhanced.
2. In order to decrease the absorption of the exciting and emitting light when black-coloured Fe3O4nanoparticles were scattered in the composite nanofibers. Fe3O4/PVP//Eu(BA)3phen/PVP and Fe3O4/PVP//Tb(BA)3phen/PVP magnetic-photoluminescent bifunctional bistrand aligned composite nanofibers bundles were fabricated by employing a homemade parallel axial electrospinning setup with the side by side dual spinnerets for the first time. Fe3O4NPs and rare earth complex were respectively dispersed into the individual strand fiber of the bistrand aligned composite nanofibers bundles, so that the rare earth complex was effectively isolated from Fe3O4NPs, which greatly reduced the effect of Fe3O4NPs on the luminescence of complex. The results indicated that the fluorescence intensity of bistrand aligned composite nanofibers bundles was obviously higher than that of the above composite nanofibers prepared by single axial electrospinning when the two nanostructures have the same saturation magnetization. The luminescent intensity is hardly decreased when more Fe3O4NPs were added. This kind of magnetic-photoluminescent bifunctional bistrand aligned composite nanofibers bundles possesses excellent magnetic properties and higher fluorescence intensity.
3. A new kind of color-tunable PVP/[Tb(BA)3phen+Eu(BA)3phen] luminescent composite nanofibers which consisted of europium complex, terbium complex and PVP were prepared by single axial electrospinning for the first time. The emission spectrum analysis of samples showed that the emitting color of the PVP/[Tb(BA)3phen+Eu(BA)3phen] luminescent composite nanofibers can be tuned under the excitation of276nm single-wavelength ultraviolet light by adjusting the ratio of terbium and europium complexes in a wide color range of red-yellow-green.
4. For the first time, a new kind of Fe3O4/PVP//[Tb(BA)3phen+Eu(BA)3phen]/PVP magnetic-photoluminescent bifunctional bistrand aligned composite nanofibers bundles with high fluorescence intensity, magnetism-tunable and colour-tuned characteristics were successfully prepared by parallel axial electrospinning. Fe3O4NPs and rare earth complex (Tb(BA)3phen and Eu(BA)3phen) were respectively dispersed into the individual strand fiber of the bistrand aligned composite nanofibers bundles. The fluorescence intensity of the Fe3O4/PVP//[Tb(BA)3phen+Eu(BA)3phen]/PVP bistrand aligned composite nanofibers bundles was obviously higher than that of Fe3O4/[Tb(BA)3phen+Eu(BA)3phen]/PVP composite nanofibers when they have the same saturation magnetization. The magnetism of the bistrand aligned composite nanofibers bundles could be tuned by adding different amounts of Fe3O4nanoparticles. The emitting color of the Fe3O4/PVP//[Tb(BA)3phen+Eu(BA)3phen]/PVP bistrand aligned composite nanofibers bundles can be tuned by adjusting the ratio of europium and terbium complexes in a wide color range of red-yellow-green. Thus, a kind of magnetic and color-tunable bifunctional bistrand aligned composite nanofibers bundles were obtained.
5. ZnS nanofibers with the diameters of200±79nm were prepared by the combination of single axial electrospinning with vulcanization technology, and their photocatalytic properties were investigated. The results showed that the photocatalytic degradation rate of ZnS nanofibers on rhodamine B was higher than ZnO nanofibers, and reached up to98.8%after UV illumination for60min.Therefore, the prepared ZnS nanofibers had outstanding photocatalytic property.
6. Ni(NO3)2/PVP hollow composite nanofibers were prepared by coaxial electrospinning, and NiO nanotubes with the outside diameters of185nm and inside diameters of40nm were fabricated by calcining the relevant composite nanofibers. The photocatalytic properties were studied. The results showed that the photocatalytic degradation effect of NiO nanotubes on rhodamine B was better than NiO nanofibers.
引文
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