Sol-gel based synthesis of complex oxide nanofibers

Electrospinning is a versatile and straight forward process for synthesizing one-dimensional (1D) nanostructures of diverse materials. Recently, a large variety of oxide ceramics have been synthesized in combination with conventional sol-gel processing. Here, the synthesis of BaTiO₃ nanofibers via electrospinning is reported. The structural evolution from amorphous to crystalline is presented under various heat treatment conditions. Nanofibers with well-defined perovskite tetragonal phase were achieved with an average crystallite size of about 20 nm. Furthermore, single crystalline BaTiO₃ nanofibers with 50 nm in diameter and lengths up to 1 μm were found, which is a novelty in electrospinning of ferroelectrics. XRD peak splitting confirmed the tetragonal perovskite structure, and this was fully supported by further evidence from selected area electron diffraction and Raman spectroscopy.     

Nonenzymatic hydrogen peroxide sensor based on a glassy carbon electrode modified with electrospun PdO-NiO composite nanofibers

A glassy carbon electrode was modified with PdO-NiO composite nanofibers (PdO-NiO-NFs) and applied to the electrocatalytic reduction of hydrogen peroxide (H₂O₂). The PdO-NiO-NFs were synthesized by electrospinning and subsequent thermal treatment, and then characterized by scanning electron microscopy, energy dispersive X-ray spectroscopy, X-ray diffraction, and X-ray photoelectron spectroscopy. Factors such as the composition and fraction of nanofibers, and of the applied potential were also studied. The sensor exhibits high sensitivity for H₂O₂ (583.43 μA?·?mM^?1?·?cm^?2), a wide linear range (from 5.0 μM to 19 mM), a low detection limit (2.94 μM at an SNR of 3), good long term stability, and is resistant to fouling.

聚甲基丙烯酸甲酯包覆(CH3NH3)PbBr3纳米晶静电纺丝膜的制备及对氨气的荧光传感

采用原位合成法制备了聚甲基丙烯酸甲酯包覆MAPbBr₃纳米晶(MAPbBr₃@PMMA,MA=甲铵离子)静电纺丝膜。当氨气(NH₃)通入MAPbBr₃@PMMA纤维膜时与MAPbBr₃中的MA发生取代,能显著降低MAPbBr₃@PMMA纤维的荧光强度,以此构建了基于MAPbBr₃@PMMA纤维荧光猝灭的NH₃传感器。通过扫描电镜、透射电镜、粉末X射线衍射和红外对静电纺丝膜的形貌和结构进行表征,通过紫外可见光谱、荧光光谱对其光学特性进行表征。结果表明,传感器的荧光强度与NH₃浓度在8~90 mg·L^-1之间呈现出良好的线性关系(r=0.995 9),NH₃的检出限低(3 mg·L^-1),且具有良好的重现性和选择性。在实际样品气体的测定中,加标回收率为92.2%~102.1%,相对标准偏差(RSD)为1.8%~3.2%。     

Facile Electrospinning of CeO2/Bi2WO6 Heterostructured Nanofibers with Excellent Visible‐light‐driven Photocatalytic Performance

One‐dimensional (1D) CeO₂/Bi₂WO₆ heterostructured nanofibers with a diameter of about 300 nm were successfully synthesized by using a straightforward strategy combining an electrospinning technique with a sintering process. The acquired products were characterized by thermogravimetric and differential scanning calorimetric (TG‐DSC), Fourier transform infrared (FT‐IR) spectroscopy, scanning electron microscopy (SEM), transmission electron microscopy (TEM), X‐ray diffraction (XRD), X‐ray photoelectron spectroscopy (XPS), Brunauer–Emmett–Teller (BET) surface area measurements, and UV/Vis spectroscopy. The obtained CeO₂/Bi₂WO₆ heterostructured nanofibers exhibited an excellent photocatalytic property for the degradation of Rhodamine B (RhB) dye driven by visible light due to the promoted separation of photoelectrons and holes and the large contact area between the photocatalyst and organic pollutant.     

Fabrication and characterization of NiTiO3 nanofibers by sol–gel assisted electrospinning

Continuous NiTiO₃ nanofibers have been successfully synthesized by a sol–gel assisted electrospinning method followed by calcination at 600 °C in air. These nanofibers were characterized for the morphological, structural and optical properties by scanning electron microscopy (SEM), energy-dispersive X-ray spectrum (EDS), transmission electron microscopy (TEM), X-ray diffraction (XRD), X-ray photoelectron spectra (XPS) and UV–visible (UV–vis) diffuse reflectance spectroscopy (DRS). SEM results reveal that the obtained NiTiO₃ nanofibers are 175 nm in diameter and several micrometers in length after annealing at 600 °C. The XRD analysis shows that the nanofibers possess highly crystalline structure with no impurity phase. In contrast, the NiTiO₃ nanoparticles synthesized at the identical conditions by a sol–gel route have impurities including TiO₂ and NiO. Moreover, the electrospun NiTiO₃ nanofibers are endowed with an obvious optical absorbance in the visible range, demonstrating they have visible light photoresponse.     

聚甲基丙烯酸甲酯包覆(CH3NH3) PbBr3纳米晶静电纺丝膜的制备及对氨气的荧光传感

采用原位合成法制备了聚甲基丙烯酸甲酯包覆MAPbBr₃纳米晶（MAPbBr₃@PMMA,MA=甲铵离子）静电纺丝膜。当氨气（NH₃）通入MAPbBr₃@PMMA纤维膜时与MAPbBr₃中的MA发生取代,能显著降低MAPbBr₃@PMMA纤维的荧光强度,以此构建了基于MAPbBr₃@PMMA纤维荧光猝灭的NH₃传感器。通过扫描电镜、透射电镜、粉末X射线衍射和红外对静电纺丝膜的形貌和结构进行表征,通过紫外可见光谱、荧光光谱对其光学特性进行表征。结果表明,传感器的荧光强度与NH₃浓度在8~90 mg·L^-1之间呈现出良好的线性关系（r=0.995 9）,NH₃的检出限低（3 mg·L^-1）,且具有良好的重现性和选择性。在实际样品气体的测定中,加标回收率为92.2%~102.1%,相对标准偏差（RSD）为1.8%~3.2%。     

CeO2 nanofibers-CdS nanostructures n–n junction with enhanced visible-light photocatalytic activity

In the present work, the n-cerium (IV) oxide (CeO₂)/n-cadmium sulfide (CdS) composite nanofibers were successfully synthesized via a facile electrospinning and hydrothermal synthesis strategy. The physicochemical properties of the synthesized composite nanofibers were investigated by using X-ray diffraction (XRD), field emission scanning electron microscope (FESEM), energy Dispersive X-Ray Spectroscopy (EDS), diffuse Reflectance Spectroscopy (DRS), Fourier-transform infrared (FTIR), photoluminescence (PL), Brunauer–Emmett–Teller (BET) and Raman spectroscopy analysis. The activities of the CeO₂/CdS were evaluated through the photocatalytic degradation of Rose Bengal (RB) in an aqueous solution under blue LED light radiation. CeO₂/CdS composites exhibit higher photocurrent density in photocurrent response experiment and smaller charge-transfer resistance in electrochemical impedance spectroscopy (EIS). Overall, the results confirmed higher charge separation efficiency in CeO₂/CdS composites compared to pristine CeO₂ nanofibers, and CdS, which is related to intimately contact among the CeO₂, and CdS. The present work provides a new approach to construct n-n heterojunction photocatalysts based on electrospinning and a deeper insight for the photocatalytic degradation activity. In addition, possible degradation mechanism and pathways were proposed according to the identified intermediates.     

A novel approach to prepare silver chloride nanoparticles grown on the surface of PAN nanofibre via electrospinning combined with gas–solid reaction

Well-defined silver chloride nanoparticles grown on the surface of PAN nanofibre were synthesized by electrospinning technology combined with gas–solid reaction. This method can avoid the possibility of the waste of raw material as well as enhance the usage rate of AgNO₃. The PAN nanofibre can be recycled easily. X-ray powder diffraction (XRD) shows the presence of crystal AgCl, X-ray photoelectron spectroscopy (XPS) confirm that there are chemical bonds and interaction between the surface modified PAN nanofibre and Ag ions. This will be propitious to prevent nanoparticles from aggregation. Field-emission scanning electron microscopy (FESEM) and transmission electron microscopy (TEM) gave the direct evidence that AgCl nanoparticles have been dispersed on the surface of PAN nanofibre homogeneously.     

Synthesis of nano-LiFePO4 particles with excellent electrochemical performance by electrospinning-assisted method

Nanoscale LiFePO₄/C particles are synthesized using a combination of electrospinning and annealing. The important advantages of electrospinning technique are the production of separated nanofiber precursor, enabling the precursor particles arrangement to be changed, impeding the growth and agglomeration of the LiFePO₄ particles during the heat treatment, and contributing to the formation of nanosized LiFePO₄ particles. In this study, polyvinylpyrrolidone (PVP) is used as the fiber-forming agent in the electrospinning method, and also provides a reducing agent and carbon source. In situ carbon-coated LiFePO₄ particles are obtained by the pyrolysis of PVP during the thermal treatment. The LiFePO₄ particles are coated with and connected by interlaced carbons, and are uniformly distributed in the size range 50–80?nm. It is found that the as-prepared nanoscale LiFePO₄/C composite has a desirable electrochemical performance. It has discharge capacities of 163.5?mA?h g^?1 and 110.7?mA?h g^?1 at rates of 0.1?C and 10?C, respectively. In addition, this cathode has excellent cyclability with a capacity loss of less than 3?% at 0.1?C and 5?% at 5?C after 500 cycles. An effective synthesis and processing method is presented for obtaining nanosized LiFePO₄ with high electrochemical performance.     

On heat transfer and flow characteristics of jets impinging onto a concave surface with varying jet arrangements

A new electrospinning process was developed for preparing TiO₂ nanofibers using a water-soluble Ti-precursor, [bis(kappa1O-hydroxo)(bis(kappa2O,O′-lactato)titanium(IV)] commonly known as titanium(IV) bis (ammonium lactato) dihydroxide (TiBALDH). The importance of the study is justified by the fact that Ti-precursors used for electrospinning, sol–gel, hydrothermal and other fiber synthesis processes are mostly non-water soluble. Accordingly, anatase TiO₂ nanofibers of diameter between 20 and 140 nm were synthesized by electrospinning and annealing. Polyvinylpyrrolidone (PVP) and different concentrations of TiBALDH were dissolved in a mixture of water, ethyl alcohol and acetic acid to optimize the electrospinning conditions. The thermal decomposition and fragmentation of PVP, TiBALDH and the fibers with 50% mass fraction of TiBALDH were studied by TGA-MS measurements. The fibers were then annealed at 1 °C min^?1 until 600 °C. The TiO₂ fibers were characterized using SEM–EDX, FTIR and XRD

     

Electrospun Polyaniline/Poly(ethylene oxide) Composite Nanofibers Based Gas Sensor

Camphor‐10‐sulfonic acid (HCSA) doped polyaniline (PANI)/poly(ethylene oxide) (PEO) composite nanofibers with different compositions (12 to 52 wt.% of PANI) were synthesized by an electrospinning method and their properties including optical, electrical and sensing were systematically investigated. FT‐IR shows that an increase of IR absorbance ratios of aromatic C? C stretching vibration of benzenoid rings of PANI to C? O? C symmetric vibrational modes of PEO confirmed that the PANI content in nanofiber mats increased proportionally with increase in PANI content in electrospinning solution. The band gap of PANI was determined to be 2.5 eV using UV‐Vis spectroscopy. The electrical conductivities of the nanofibers increased with an increase in the PANI content in the nanofibers. Additionally, the sensitivity toward NH₃ increased as the PANI content increased, but branched nanofibers reduced sensing response. The humidity sensitivity changed from positive to negative as the PANI content increased. The electron transport mechanism was studied by measuring the temperature dependence electrical resistivity. The negative temperature coefficient of resistance revealed a semiconducting behavior for the PANI/PEO nanofibers. The activation energy, calculated by Arrhenius plot, increased as the PANI content decreased. The power law indicated that electrons were being transported in a three dimensional matrix, and the longer hopping distance required more hopping energy for electron transport.     

Synthesis of CaSnO<Subscript>3</Subscript> nanofibers by electrospinning combined with sol–gel

Calcium stannate (CaSnO₃) nanofibers were synthesized by electrospinning technique combined with a sol–gel process. The structure and morphology of the as-prepared CaSnO₃ nanofibers were characterized by X-ray diffraction and scanning electron microscopy, respectively. The samples had a band gap of about 3.87 eV, which was estimated by UV–Vis diffuse reflectance spectroscopy. On the basis of the experiment results, the composite fibers containing polymer and inorganic salt can be changed to pure CaSnO₃ nanofibers only when they were sintered at an appropriate temperature. At the same time, a possible mechanism of the nanofibers forming process was also proposed.     

Synthesis,characterization and photocatalytic properties of cesium tungstate (Cs<Subscript>2</Subscript>W<Subscript>3</Subscript>O<Subscript>10</Subscript>) nanofibers

In the paper cesium tungstate nanofibers for the first time have been fabricated successfully by a simple electrospinning technique followed by heat treatment. The cesium tungstate nanofibers have been characterized by XRD, SEM, and FTIR techniques. The results indicated the morphology and quality of the annealed electrospun samples are strongly dependent on the citric acid content within electrospinning solution. It is found with increasing the citric acid content from 7 to 22% the samples morphology changed from a particle structure to a fibrous structure. The average diameter of nanofibers was ~350 nm. XRD analysis reveals that all of the samples have good crystallinity with the same diffraction peaks that can be indexed to the tetragonal phase of Cs₂W₃O₁₀. Furthermore, the photocatalyst properties of cesium tungstate has not been reported to date. In the work the synthesized Cs₂W₃O₁₀ nanofibers were found to exhibit photocatalytic performance in the photodegradation of RhB aqueous solution used as a pollutant model.     

Fabrication and characterization of UV‐crosslinkable thermoresponsive composite fibers with magnetic properties

Crosslinking magnetic thermoresponsive composite (MTC) fiber mats were fabricated by electrospinning process and followed by UV curing. Thermoresponsive poly‐(N‐isopropylacrylamide) (PNIPAAm) and magnetic Fe₃O₄ were firstly synthesized by redox‐initiated polymerization and co‐precipitation, respectively. A crosslinking agent (dipentaerythritol hexylacrylate) and photoinitiator for providing crosslinking ability were then mixed with PNIPAAm and Fe₃O₄ in ethanol as the electrospinning solution. After electrospinning and subsequent UV irradiation, the MTC fiber mats were thus obtained. Thermoresponsivity of the MTC fibers was measured by both DSC and swelling test. MTC fiber mat exhibited better water‐absorption capability and thermoresponsivity than corresponding film. Morphological analysis was observed by SEM and TEM, and the magnetic property was measured by SQUID. The thermoresponsive magnetic behavior of MTC fiber mat in water was observed under various temperatures and magnetic fields. Vitamin B₁₂ used as a model drug was loaded in the MTC fiber mats and the drug‐release behavior was then studied. © 2015 Wiley Periodicals, Inc. J. Polym. Sci., Part A: Polym. Chem. 2015 , 53, 2152–2162     

Enhancement of the photocatalytic activity of modified TiO2 nanoparticles with Zn2+. correlation between structure and properties

Zinc-doped and undoped TiO₂ photocatalysts were synthesized via sol-gel techniques. Doping of TiO₂ with M²⁺ (M-Zn) was intended to create tail states within the band gap of TiO2. These can subsequently be employed as efficient photocatalysts which can effectively decompose organic contaminants only with visible light activation. The structure, physico-chemical and optical properties of the products were characterized by using the X-ray diffraction (XRD), Raman spectra, UV-vis diffuse reflectance spectroscopy (DRS) and electrochemical impedance spectroscopy (EIS) techniques. Doping shifts the optical absorption edge to the visible region and decreases the charge-transfer resistance. Under visible light, the composite nanoparticles very efficiently catalyze the MB dye. Results implied that Zn doping increased photoinduced charge transfer rate, and the use of described methods is a powerful tool toward predicting and understanding the photocatalytic processes and behaviors.     

Preparation of ultrafine fast-dissolving feruloyl-oleyl-glycerol-loaded polyvinylpyrrolidone fiber mats via electrospinning

Fast-dissolving drug delivery membranes for poorly water-soluble drugs were prepared by electrospinning using feruloyl-oleyl-glycerol (FOG) as a model drug and polyvinylpyrrolidone (PVP) K90 as a polymer matrix in a mixed solvent of chloroform/ethanol (4:1, v/v). Results from Fourier-transform infrared spectroscopy (FT-IR) illustrated good compatibility between FOG and PVP as well as a good distribution of FOG within the fibers. The morphology and diameter of the fibers were influenced by the concentration of PVP and the applied voltage. When the PVP concentration was 5% (w/v) and the applied voltage was 14 kV, uniform and smooth fibers were obtained, with diameter 700-800 nm. Wetting time assays confirmed fast-dissolving properties with the average dissolution time for FOG-loaded PVP fiber membranes being 2.0±1.5 s. These results demonstrate the potential of electrospinning solid dispersions to improve the dissolution profile of poorly water-soluble drugs.     

Removal of Acidic Organic Ionic Dyes from Water by Electrospinning a Polyacrylonitrile Composite MIL101(Fe)-NH2 Nanofiber Membrane

A nanofiber metal–organic framework filter, a polyacrylonitrile (PAN) nanofiber membrane composite with an iron/2-amino-terephthalic acid-based metal–organic framework (MIL101(Fe)-NH₂), was prepared by one-step electrospinning. MIL101(Fe)-NH₂ was combined into the polymer nanofibers in situ. PAN-MIL101(Fe)-NH₂ composite nanofiber membranes (NFMs) were prepared from a homogeneous spinning stock containing MIL101(Fe)-NH₂ prebody fluid and PAN. Crystallization of MIL101(Fe)-NH₂ and solidification of the polymer occurred simultaneously during electrospinning. The PAN-MIL101(Fe)-NH₂ composite NFM showed that MIL101(Fe)-NH₂ was uniformly distributed throughout the nanofiber and was used to adsorb and separate acidic organic ionic dyes from the aqueous solution. The results of Fourier transform infrared spectroscopy, energy-dispersive X-ray spectroscopy, and X-ray diffraction analysis showed that MIL101(Fe)-NH₂ crystals were effectively bonded in the PAN nanofiber matrix, and the crystallinity of MIL101(Fe)-NH₂ crystals remained good, while the distribution was uniform. Owing to the synergistic effect of PAN and the MIL101(Fe)-NH₂ crystal, the PAN-MIL101(Fe)-NH₂ composite NFM showed a fast adsorption rate for acidic ionic dyes. This study provides a reference for the rapid separation and purification of organic ionic dyes from wastewater.     

Evaluating the electrochemical properties of PEO‐based nanofibrous electrolytes incorporated with TiO2 nanofiller applicable in lithium‐ion batteries

In the present work, nanofibrous composite polymer electrolytes consist of polyethylene oxide (PEO), ethylene carbonate (EC), propylene carbonate (PC), lithium perchlorate (LiClO₄), and titanium dioxide (TiO₂) were designed using response surface method (RSM) and synthesized via an electrospinning process. Morphological properties of the as‐prepared electrolytes were studied using SEM. FTIR spectroscopy was conducted to investigate the interaction between the components of the composites. The highest room temperature ionic conductivity of 0.085 mS.cm^?1 was obtained with incorporation of 0.175 wt. % TiO₂ filler into the plasticized nanofibrous electrolyte by EC. Moreover, the optimum structure was compared with a film polymeric electrolyte prepared using a film casting method. Despite more amorphous structure of the film electrolyte, the nanofibrous electrolyte showed superior ion conductivity possibly due to the highly porous structure of the nanofibrous membranes. Furthermore, the mechanical properties illustrated slight deterioration with incorporation of the TiO₂ nanoparticles into the electrospun electrolytes. This investigation indicated the great potential of the electrospun structures as all‐solid‐state polymeric electrolytes applicable in lithium ion batteries.     

静电纺丝制备g-C3N4/C纳米纤维及其可见光降解性能

采用g-C_3N_4纳米片与聚丙烯腈进行静电复合纺丝,再经预氧化和碳化制得g-C_3N_4/C纳米纤维。利用傅立叶变换红外光谱仪(FTIR)、X射线衍射仪(XRD)、拉曼光谱(Raman)和扫描电子显微镜(SEM)对样品结构和形貌进行表征,通过紫外-可见漫反射光谱(UV-Vis DRS)分析可见光响应性。研究表明,复合纳米纤维对罗丹明B表现出较好的可见光降解活性,源于无定形相/石墨相混合结构的碳基体能够降低g-C_3N_4的光生电子-空穴对复合的几率。复合纳米纤维膜在光催化降解搅拌条件下始终能保持完整,经过多次回收和光催化实验,对罗丹明B的光降解率依然较高,表现出较优异的循环利用稳定性。     

静电纺丝制备g-C3N4/C纳米纤维及其可见光降解性能

采用g-C₃N₄纳米片与聚丙烯腈进行静电复合纺丝,再经预氧化和碳化制得g-C₃N₄/C纳米纤维。利用傅立叶变换红外光谱仪（FTIR）、X射线衍射仪（XRD）、拉曼光谱（Raman）和扫描电子显微镜（SEM）对样品结构和形貌进行表征,通过紫外-可见漫反射光谱（UV-Vis DRS）分析可见光响应性。研究表明,复合纳米纤维对罗丹明B表现出较好的可见光降解活性,源于无定形相/石墨相混合结构的碳基体能够降低g-C₃N₄的光生电子-空穴对复合的几率。复合纳米纤维膜在光催化降解搅拌条件下始终能保持完整,经过多次回收和光催化实验,对罗丹明B的光降解率依然较高,表现出较优异的循环利用稳定性。