Cellulose nanofibers from curaua fibers

Curaua nanofibers extracted under different conditions were investigated. The raw fibers were mercerized with NaOH solutions; they were then submitted to acid hydrolysis using three different types of acids (H₂SO₄, a mixture of H₂SO₄/HCl and HCl). The fibers were analyzed by cellulose, lignin and hemicellulose contents; viscometry, X-ray diffraction (XRD) and thermal stability by thermogravimetric analysis (TG). The nanofibers were morphologically characterized by transmission electron microscopy (TEM) and their surface charges in suspensions were estimated by Zeta-potential. Their degree of polymerization (DP) was characterized by viscometry, crystallinity by XRD and thermal stability by TG. Increasing the NaOH solution concentration in the mercerization, there was a decrease of hemicellulose and lignin contents and consequently an increase of cellulose content. XRD patterns presented changes in the crystal structure from cellulose I to cellulose II when the fibers were mercerized with 17.5% NaOH solution. All curaua nanofibers presented a rod-like shape, an average diameter (D) of 6–10 nm and length (L) of 80–170 nm, with an aspect ratio (L/D) of around 13–17. The mercerization of fibers with NaOH solutions influenced the crystallinity index and thermal stability of the resulting nanofibers. The fibers mercerized with NaOH solution 17.5% resulted in more crystalline nanofibers, but thermally less stable and inferior DP. The aggregation state increases with the amount of HCl introduced into the extraction, due to the decrease of surface charges (as verified by Zeta Potential analysis). However, this release presented nanofibers with better thermal stability than those whose acid hydrolysis was carried out using only H₂SO₄.     

Stabilization of electrospun poly(vinyl alcohol) nanofibrous mats in aqueous solutions

<正>The stability ofpoly(vinyl alcohol)(PVA) nanofibrous mats in water media was improved by post-electrospinning treatments.Bifunctional glutaraldehyde(GA) in methanol was used as a crosslinking agent to stabilize PVA nanofiber,but fiber twinning was observed frequently,and the highly porous structure of PVA nanofibrous mats was destroyed when the crosslinked fiber was soaked in water.To overcome this shortcoming,chitosan(CS) was introduced into the PVA spinning solution to prepare PVA/CS composite nanofibers.Their treatment in GA/methanol solution could retain the fiber morphology of PVA/CS nanofibers and porous structure of PVA/CS nanofibrous mats even if they were soaked in aqueous solutions for 1 month.Scanning electron microscopy(SEM),X-ray diffraction(XRD),thermal gravimetric analysis(TGA) and differential scanning calorimetry(DSC) were applied to characterize the physicochemical structure and thermal properties of PVA nanofibers.It was found that the water resistance of PVA nanofibrous mats was enhanced because of the improvement of the degree of crosslinking and crystallinity in the electrospun PVA fibers after soaking in GA/methanol solution.     

Mechanical properties of titania nanofiber mats fabricated by electrospinning of sol–gel precursor

Flexible mats of titania fibers are prepared by calcination of electrospun polyvinylpyrrolidone fibers containing titanium isopropoxide precursor. Structural investigation of the calcinated nanofibers by X-ray diffraction (XRD) and electron diffraction (ED) combined with the morphologies by scanning electron microscopy (SEM) and transmission electron microscopy (TEM) show the titania fibers, with an average diameter of 180 nm, were comprised of anatase and rutile crystals. The mechanical, chemical and thermal properties of the titania fiber mats are further investigated by the techniques of Instron mechanical tester, thermogravimetric analyzer (TGA), and Fourier transform infrared spectroscopy (FT-IR). The titania fiber mat prepared in this method exhibited a significant flexibility with 461 MPa Young’s modulus.     

Effect of pyrolysis conditions on the properties of carbonaceous nanofibers obtained from freeze-dried cellulose nanofibers

Carbonaceous nanofibers (CsNFs) were produced by pyrolysis of cellulose nanofibers synthesised from wood pulp using a top-down approach. The effects of heat treatment conditions on the thermal, morphological, crystal and chemical properties of the CsNFs were investigated using TGA, SEM, XRD and FT-IR, respectively. The results showed that heat treatment conditions around the thermal decomposition temperature of cellulose greatly influence the morphology of resulting materials. Slow heating rates (1 °C/min) between 240 and 400 °C as well as prolonged isothermal heat treatment (17 h) at 240 °C were necessary to avoid destruction of the original fibrous morphology in carbonized nanofibers. On the other hand, such heat treatment had little effect on micron sized fibers. The optimized heat treatment conditions led to the release of oxygen and hydrogen from cellulose before thermal breakdown of glycosidic rings, which in turn prevented depolymerization and tar formation, resulting in the preservation of the fibrous morphology.     

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 and characterization of zinc titanate fibers by sol-electrospinning method

A facile and economic electrospinning approach has been developed for the synthesis of zinc titanate-rutile composite fibers as a nanofibrous mat at the first time. The composite fibers with different morphologies were obtained by calcination of the PVP/Ti(OC₄H₉)₄–Zn(CH₃COO)₂ fibers. The reaction mechanism was characterized by thermogravimetry-differential thermal analysis (TG-DTA), X-ray diffractometer (XRD), field emission scanning electron microscopy (FE-SEM) and Fourier transform infraction spectroscopy (FT-IR) spectra techniques. According to the thermal analysis, the phase of ZnTiO₃ occurred at 450 °C and it decomposed at 885 °C. FE-SEM micrographs indicated that the as-spun fibers were round and had a rather uniform and smooth surface with the diameters in the range of 300–800 nm over its length. Its morphology is greatly affected by the calcination temperatures.     

Synthesis of electrospun BaSrTiO<Subscript>3</Subscript>/PVP nanofibers

Ba_1−x Sr _x TiO₃(x = 0–0.5, BST) nanofibers with diameters of 150–210 nm were prepared by using electrospun BST/polyvinylpyrrolidone (PVP) composite fibers by calcination for 2 h at temperatures in the range of 650–800 °C in air. The morphology and crystal structure of calcined BST/PVP nanofibers were characterized as functions of calcination temperature and Sr content with an aid of XRD, FT-IR, and TEM. Although several unknown XRD peaks were detected when the fibers were calcined at temperatures less than 750 °C, they disappeared with increasing the temperature (above 750 °C) due to its thermal decomposition and complete reaction in the formation of BST. In addition, the FT-IR studies of BST/PVP fibers revealed that the intensities of the O–H stretching vibration bands (at 3430 and 1425 cm⁻¹) became weaker with increasing the calcination temperature and a broad band at 540 cm⁻¹, Ti–O vibration, appeared sharper and narrower after calcination above 750 °C due to the formation of metal oxide bonds. However, no effect of Sr content on the crystal structure of the composites was detected.     

Facile fabrication of cerium niobate nano-crystalline fibers by electrospinning technology

In this study, one-dimensional (1D) cerium niobate nano-crystalline fibers were first prepared by a facile sol–gel and electrospinning process, followed by heat treatment. X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), thermogravimetric analysis (TG), scanning electron microscopy (SEM), and high-resolution transmission electron microscopy (HR-TEM) were used to characterize the samples. It can be seen from SEM images that the as-prepared xerogel samples and those annealed at 900 °C presented uniform fibrous morphology, with the diameter of 100–300 nm and length of several centimeters. The XRD and FT-IR results showed that cerium niobate samples had well-crystallized phase of CeNbO_4.25 with the crystallite size of about 28.6 nm at a heat treatment temperature of 900 °C, which can also be validated with the TEM image. The AC impedance of annealed disks made from the CeNbO_4.25 nano-crystalline fibers has been probed.     

Isolation and characterization of cellulose nanofibers from four plant cellulose fibers using a chemical-ultrasonic process

Cellulose nanofibers (CNFs) were isolated from four kinds of plant cellulose fibers by a chemical-ultrasonic treatment. The chemical composition, morphology, crystalline behavior, and thermal properties of the nanofibers and their intermediate products were characterized and compared. The CNFs extracted from wood, bamboo, and wheat straw fibers had uniform diameters of 10–40 nm, whereas the flax fibers were not uniformly nanofibrillated because of their initially high cellulose content. The chemical composition of each kind of nanofibers was mainly cellulose because hemicelluloses and lignin were significantly removed during chemical process. The crystallinity of the nanofibers increased as the chemical treatments were applied. The degradation temperature of each kind of nanofiber reached beyond 330 °C. Based on the properties of the CNFs, we expect that they will be suitable for use in green nanocomposites, filtration media and optically transparent films.     

Fabrication and UV-blocking property of nano-ZnO assembled cotton fibers via a two-step hydrothermal method

A novel ZnO/cotton composite, in which ZnO nanoparticles were synthesized directly inside of the lumen and the mesopores of cotton fibers, was fabricated via a simply two-step hydrothermal method in situ using zinc nitrate hexahydrate and hexamethylenetetramine as raw materials. The as-obtained cotton sample was characterized by powder X-ray diffractometer, field emission scanning electron microscopy, and energy-dispersive spectroscopy, respectively. The UV-blocking property of the as-obtained sample was investigated by UV–vis spectrophotometry. The results showed that hexagonal wurtzite nano-ZnO with a diameter of about 30–40 nm was successfully assembled into the lumen as well as the mesoporous structure of the cotton fibers. The UV-blocking property of the modified cotton fibers can be greatly improved by assembling nano-ZnO into the inner of cotton fibers. Comparing with the neat cotton fibers, the UV-blocking ratio of the ZnO assembled cotton fibers inside of KBr disk could reach 80% at 300 nm and 95% at 225 nm, respectively. Therefore, it demonstrated a significant advance in protective functional treatment and provided a potential commercialization.     

Thermal study on electrospun polyvinylpyrrolidone/ammonium metatungstate nanofibers: optimising the annealing conditions for obtaining WO<Subscript>3</Subscript> nanofibers

This article demonstrates how important it is to find the optimal heating conditions when electrospun organic/inorganic composite fibers are annealed to get ceramic nanofibers in appropriate quality (crystal structure, composition, and morphology) and to avoid their disintegration. Polyvinylpyrrolidone [PVP, (C₆H₉NO) _n ] and ammonium metatungstate [AMT, (NH₄)₆[H₂W₁₂O₄₀]·nH₂O] nanofibers were prepared by electrospinning aqueous solutions of PVP and AMT. The as-spun fibers and their annealing were characterized by TG/DTA-MS, XRD, SEM, Raman, and FTIR measurements. The 400–600 nm thick and tens of micrometer long PVP/AMT fibers decomposed thermally in air in four steps, and pure monoclinic WO₃ nanofibers formed between 500 and 600 °C. When a too high heating rate and heating temperature (10 °C min⁻¹, 600 °C) were used, the WO₃ nanofibers completely disintegrated. At lower heating rate but too high temperature (1 °C min⁻¹, 600 °C), the fibers broke into rods. If the heating rate was adequate, but the annealing temperature was too low (1 °C min⁻¹, 500 °C), the nanofiber morphology was excellent, but the sample was less crystalline. When the optimal heating rate and temperature (1 °C min⁻¹, 550 °C) were applied, WO₃ nanofibers with excellent morphology (250 nm thick and tens of micrometer long nanofibers, which consisted of 20–80 nm particles) and crystallinity (monoclinic WO₃) were obtained. The FTIR and Raman measurements confirmed that with these heating parameters the organic matter was effectively removed from the nanofibers and monoclinic WO₃ was present in a highly crystalline and ordered form.     

Effects of hydrolysis conditions on the morphology,crystallinity, and thermal stability of cellulose nanocrystals extracted from kenaf bast fibers

Cellulose nanocrystals (CNC) were first isolated from kenaf bast fibers and then characterized. The raw fibers were subjected to alkali treatment and bleaching treatment and subsequent hydrolysis with sulfuric acid. The influence of the reaction time on the morphology, crystallinity, and thermal stability of CNC was investigated. Fourier transform infrared spectroscopy showed that lignin and hemicellulose were almost entirely removed during the alkali and bleaching treatments. The morphology and dimensions of the fibers and acid-released CNC were characterized by field emission scanning electron microscopy and transmission electron microscopy. X-Ray diffraction analysis revealed that the crystallinity first increases upon hydrolysis and then decreases after long durations of hydrolysis. The optimal extraction time was found to be around 40 min during hydrolysis at 45 °C with 65% sulfuric acid. The thermal stability was found to decrease as the hydrolysis time increased. The electrophoretic mobility of the CNC suspensions was measured using the zeta potential, and it ranged from −8.7 to −95.3 mV.     

Characteristics of cellulose nanofibers isolated from rubberwood and empty fruit bunches of oil palm using chemo-mechanical process

In the present study, chemical-physical properties of nanofibers isolated from rubberwood (Hevea brasiliensis) and empty fruit bunches (EFB) of oil palm (Elaeis guineensis) were analyzed by microscopic, spectroscopic, thermal and X-ray diffraction methods. The isolation was achieved using chemo-mechanical processes. Microscopy study showed that the diameters of the nanofibers isolated from the EFB ranged from 5 to 40 nm while those of the nanofibers isolated from rubberwood had a wider range (10–90 nm). Fourier transform infrared spectroscopy study demonstrated that almost all the lignin and most of the hemicellulose were removed during the chemical treatments. X-ray diffraction analysis revealed that the crystallinity of the studied nanofibers increased after the chemo-mechanical isolation process. The results of thermogravimetric analysis showed that the nanofibers isolated from both sources had higher thermal stability than those of the bleached pulp and untreated fibers.     

Cotton fabrics treated with acylhydrazone-based polyviologen to create innovative multi-stimulus responsive textiles

Novel multi-stimuli responsive cotton fibers were developed via spray-coating with an acylhydrazone-based polyviologen (AHPV). Polyviologen was prepared by supramolecular condensation polymerization of bipyridinium dialdehyde with a hydroxyl-substituted aryldihydrazide in an acidified aqueous medium. Transparent AHPV/resin nanocomposite film was deposited onto the surface of cotton fabric by well-dispersion of AHPV as a chromogenic substance in a resin binding agent. Increasing the temperature of the AHPV-coated cotton fabric from room temperature to 85 °C reversibly triggered a change in color from pale yellow (437 nm) to green (607 nm), respectively. The transparent layer immobilized onto the white cotton surface transformed into green under ultraviolet source as demonstrated by CIE Lab parameters. The photochromic impacts were explored at various AHPV. In addition, the AHPV-coated cotton immediately displayed a vapochromic activity upon exposure to NH_3(g), and then recovered to pale yellow after removing the ammonia source away. The current AHPV-coated cotton fabric displayed a limit of detection (LOD) to NH_3(aq) in the range of 50–150 ppm. The spray-coated cotton fabrics demonstrated a reversible photochromism, thermochromism and vapochromism with high stability. The produced AHPV nanoparticles were also studied by transmission electron microscopy (TEM), demonstrating particle diameter of 74–92 nm. The mechanical and morphological properties of the spray-coated cotton fabrics were also explored. The surface morphology of AHPV-finished samples was examined by Fourier-transform infrared (FTIR) and scanning electron microscopy (SEM). No considerable defects were observed in permeability to air and bending length of AHPV-finished samples. Additionally, high colorfastness was monitored for the AHPV-finished cotton substrates. The cytotoxic activity of the AHPV-finished cotton was also examined. Mechanistic study accounting for the multichromic activity of acylhydrazone-based polyviologen is explored.     

Preparation and characterization of cellulose nanofibers from partly mercerized cotton by mixed acid hydrolysis

Cellulose nanofibers with a diameter of 70 nm and lengths of approximately 400 nm were fabricated from partly mercerized cotton fibers by acid hydrolysis. Morphological evolution of the hydrolyzed cotton fibers was investigated by powder X-ray diffraction, Fourier transform infrared analysis and field emission scanning electron microscopy. The XRD results show that the cellulose I was partially transformed into cellulose II by treatment with 15 % NaOH at 150° for 3 h. The crystallinity of this partially mercerized sample was lower than the samples that were converted completely to cellulose II by higher concentrations of NaOH. The intensities of all of the diffraction peaks were noticeably increased with increased hydrolysis time. Fourier transform infrared results revealed that the chemical composition of the remaining nanofibers of cellulose I and II had no observable change after acidic hydrolysis, and there was no difference between the hydrolysis rates for cellulose I or II. The formation of cellulose nanofibers involves three stages: net-like microfibril formation, then short microfibrils and finally nanofibers.     

Synthesis and optical property of NaTaO<Subscript>3</Subscript> nanofibers prepared by electrospinning

This paper describes a procedure of preparing sodium tantalite nanofibers for the first time. Sodium tantalite nanofibers were synthesised by electrospinning a sol–gel precursor solution of poly(vinyl pyrrolidone)/sodium tantalite, followed by careful sintering of the as-electrospun composite fibers at 550 °C for 3 h. The morphology, microstructure and crystal phase were investigated by transmission electron microcopy and X-ray diffraction. The optical property was characterized by ultraviolet–visible (UV–vis) spectrometer. Typical nanofibers were with diameter between 70 and 90 nm and length exceeding 0.1 mm. An unusual phenomenon, the red-shift of optical absorption band edge happened, indicated the fabricated NaTaO₃ nanofibers were potential good candidates for photocatalytic application. The experiment photodegradation of methylene blue by NaTaO₃ nanofibers under UV light irradiation was performed.     

One-dimensional GdVO4:Ln (Ln=Eu, Dy, Sm) nanofibers: Electrospinning preparation and luminescence properties

One-dimensional GdVO₄:Ln³⁺ (Ln=Eu, Dy, Sm) nanofibers have been prepared by a combination method of sol-gel process and electrospinning technology. X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), thermogravimetric and differential thermal analysis (TG-DTA), scanning electron microscopy (SEM), transmission electron microscopy (TEM), photoluminescence (PL), quantum efficiency (QE), and cathodoluminescence (CL) spectra as well as kinetic decays were used to characterize the samples. The XRD, FT-IR, and TG-DTA results show that GdVO₄:Ln³⁺ nanofibers samples crystallize at 700 °C. SEM images indicate that the as prepared precursor fibers are smooth. After being calcined at 700 °C for 4 h, the fibers still maintain their fiberlike morphology with rough surface. TEM image further manifests that the GdVO₄:Ln³⁺ nanofibers consist of nanoparticles. Under ultraviolet excitation and low-voltage electron beam excitation, GdVO₄:Ln³⁺ phosphors showed their strong characteristic emission due to an efficient energy transfer from vanadate groups to dopants. The optimum doping concentration of Ln³⁺ in the GdVO₄ nanofibers also has been investigated.     

碳纤维表面原位SiC纳米纤维的合成与生长

基于化学气相反应法,以高纯Si和SiO₂为反应源材料,在碳纤维表面原位生长β-SiC纳米纤维。采用XRD、SEM和TEM 等分析测试手段对SiC纳米纤维进行了表征分析,研究了不同反应温度和时间对生成β-SiC纳米纤维微观形貌和结构的影响,并探讨了β-SiC纳米纤维的生长机制。研究结果表明：采取化学气相反应法能够制备高质量、高纯度的β-SiC纳米纤维,纳米纤维的直径约为100~300 nm。随着反应温度的提高和时间的延长,纳米纤维的产额增加,且微观组织形貌发生了变化。结合制备过程和纳米纤维微观结构的观察分析,表明气-固(VS)机制是SiC纳米纤维生长的主要机理。     

碳纤维表面原位SiC纳米纤维的合成与生长

基于化学气相反应法,以高纯Si和SiO₂为反应源材料,在碳纤维表面原位生长β-SiC纳米纤维。采用XRD、SEM和TEM 等分析测试手段对SiC纳米纤维进行了表征分析,研究了不同反应温度和时间对生成β-SiC纳米纤维微观形貌和结构的影响,并探讨了β-SiC纳米纤维的生长机制。研究结果表明：采取化学气相反应法能够制备高质量、高纯度的β-SiC纳米纤维,纳米纤维的直径约为100~300 nm。随着反应温度的提高和时间的延长,纳米纤维的产额增加,且微观组织形貌发生了变化。结合制备过程和纳米纤维微观结构的观察分析,表明气-固(VS)机制是SiC纳米纤维生长的主要机理。     

静电纺丝法制备Mn2O3纳米纤维及其磁性研究

采用溶胶-凝胶过程和静电纺丝技术相结合方法, 以聚丙烯腈和醋酸锰为前驱物, 制得了PAN/Mn(CH₃COO)₂复合纳米纤维. 将该复合纤维高温煅烧, 获得了Mn₂O₃纳米纤维. 采用扫描电镜(SEM)、红外光谱(FTIR)、差热-热重(TG-DTA)和X射线衍射(XRD)分析等对样品进行了表征. 结果表明, Mn₂O₃纳米纤维为规则的一维结构, 直径分布均匀, 具有铁磁性-反铁磁性-顺磁性相互转化的特性.