静电纺制备纳米孔结构聚乳酸(PLLA)超细纤维

采用静电纺丝法制备了孔径为40～150 nm的PLLA纳米孔结构超细纤维,纳米孔不仅分布在纤维表面,而且存在于纤维内部.通过扫面电镜观察了纤维表面形貌.探讨了混合溶剂二氯甲烷/N,N-二甲基甲酰胺的比例、PLLA浓度、电场强度对PLLA纤维纳米孔大小、分布密度、深度的影响.结果表明通过调节PLLA溶液性质和纺丝参数,PLLA纤维的表面形貌可以在3种状态即光滑无孔、疏浅凹坑、密集深孔之间可控.二氯甲烷/N,N-二甲基甲酰胺比例为1∶4,PLLA浓度9%,电场强度1 kV/cm,环境温湿度分别为30℃和52%,静电纺丝所得PLLA超细纤维表面孔洞直径为150 nm,孔洞分布密集.纳米孔PLLA纤维形成的主要机理是由于静电纺丝过程中溶剂的快速挥发引起纤维表面温度急剧降低导致热致相分离而产生多孔结构.PLLA纤维膜的疏水性与纤维表面孔洞结构密切相关,纤维膜接触角最高可达146.6°.由于PLLA纤维的多孔结构,这种高疏水性的PLLA纤维膜能够快速、大量地吸油,90 s内吸收柴油达到90 g/g,25 min内可以达到145 g/g.     

静电纺丝法制备交联多孔纳米碳纤维膜及其电化学电容性能

以聚丙烯腈(PAN)和三聚氰胺为原料,通过静电纺丝法制备了三聚氰胺改性聚丙烯腈纳米纤维前驱体,经预氧化、碳化后得到交联的多孔纳米碳纤维.采用红外光谱(FTIR)仪、热重分析(TGA)仪、扫描电子显微镜(SEM)、X射线衍射(XRD)仪、拉曼光谱仪和比表面积分析仪等对前驱体及纤维进行了表征.结果表明,经过三聚氰胺改性的聚丙烯腈纳米纤维前驱体在碳化后有效地交联,形成含有微孔、介孔和大孔多级的合理孔道结构,氮掺杂量高达14.3%,纤维直径大幅缩减,平均直径仅约89 nm.电化学测试结果表明,交联多孔纳米碳纤维电极在0.05 A·g^-1电流密度下未经活化时的质量比电容值高达194 F·g^-1(0.05 A·g^-1),在2 A·g^-1的电流密度下经过1000次循环充放电后的比电容仍然保持99.2%,表现出优异的电化学特性.     

水和辛胺对ZnO多孔纳米块体孔道结构的影响

以ZnO纳米颗粒为原料, 分别用水和辛胺水溶液作为造孔剂, 利用溶剂热压方法制备了ZnO多孔纳米块体. 实验结果表明, 当以水作造孔剂时, 随着ZnO纳米粉/水(质量比)比值的减小, ZnO多孔纳米块体的孔径分布变宽, 比表面积和孔隙率增加; 加入辛胺后, ZnO多孔纳米块体的孔径分布变窄, 但比表面积和孔隙率略有减少. 随着辛胺用量的增加, 比表面积和孔隙率又同时呈上升趋势. 对ZnO多孔纳米块体进行的红外吸收测试结果表明, 在制备多孔纳米块体过程中, 水及辛胺基本上都从样品中逸出, 孔道中只有微量残留.     

EVOH纳米纤维及其功能膜的制备与性能研究北大核心CSCD

利用熔融纺丝相分离行为制备乙烯-乙烯醇共聚树脂(EVOH)纳米纤维,并利用湿法成网的方法制备EVOH纳米纤维膜,分析表征了EVOH纳米纤维的形态、结构、结晶性能及纤维膜的形态、孔隙率、孔径大小和分布、比表面积等。结果表明:乙烯-乙烯醇共聚树脂/乙酸丁酸纤维素酯(EVOH/CAB)经双螺杆熔融挤出去除CAB后所制备的EVOH纳米纤维平均直径为162～260nm,加工条件和方法对EVOH的结构和结晶性能没有明显影响。随着纤维膜厚度增加,EVOH纳米纤维膜的孔径减小、孔径分布变窄;随着纳米纤维制备过程中EVOH/CAB体系中EVOH含量增大,EVOH纳米纤维直径增大,其功能膜的孔隙率增大、比表面积减小。     

静电纺丝制备空气过滤用抗分层聚酰胺66/聚丙烯腈/聚醚砜(PA-66/PAN/PES)三明治结构膜（英文）

通过在经处理的不锈钢网(SSM)上逐层电纺制备了简易有效的聚酰胺66/聚丙烯腈/聚醚砜(PA-66/PAN/PES)复合纤维过滤材料.材料中间层采用以N,N-二甲基甲酰胺(DMF)为溶剂的PAN/PES共混聚合物电纺而成.扫描电子显微镜表征和比表面积测试结果表明,在相同纺丝条件下PES量的增加有利于减小纤维直径,增大膜的孔隙率.同时,通过拉伸实验测量了未带有SSM的膜的机械性能(5.857 MPa).利用PES的良好疏水性,过滤膜表面具有相对良好的疏水效果,接触角约为130.58°.在样品厚度尽可能相等的情况下,通过对实际空气环境中0.3~5μm的颗粒进行截流测试发现,PAN/PES-3的过滤效率达到且大于99%.通过机械振动和空气反吹考察了过滤膜的再生性能.此外,还通过使用喷雾喷涂SSM研究了防分层过滤介质的基质.     

β-环糊精功能化聚丙烯腈纳米纤维的制备及对亚甲基蓝的吸附性能

以N,N-二甲基甲酰胺(DMF)为溶剂,利用静电纺丝法制备了聚丙烯腈(PAN)/β-环糊精(β-CD)纳米纤维.通过场发射扫描电镜、红外光谱和粉末XRD对纳米纤维进行了表征,并检测了纺丝溶液的电导率和黏度.结果表明,β-CD的添加量可以改善纳米纤维的形貌,固定在纤维上的β-CD保留了空腔结构,为其在纳米纤维中发挥超分子...     

静电纺丝法制备相变调温纤维及其性能

以丙酮和N,N-二甲基甲酰胺（DMF）为混合溶剂,实验室自制固-固相变材料为相变工作物质,醋酸纤维素（CDA）为高分子载体,利用静电纺丝技术制备了相变调温纤维,研究了溶剂配比、纺丝液浓度、纺丝电压等对纤维形貌的影响。结果表明：以N,N-二甲基甲酰胺（DMF）和丙酮为溶剂（体积比为1/4）,在纺丝液质量分数为22%、纺丝...     

静电纺丝制备多孔碳纳米纤维及其电化学电容行为

采用静电纺丝技术,以聚丙烯腈(PAN)/醋酸锌为前驱体制备复合纳米纤维,随后经碳化、酸化获得多孔碳纳米纤维.扫描电子显微镜(SEM)观察发现,碳纳米纤维表面分布大量孔洞.N2吸脱附等温曲线(BET)测试材料比表面积达413m2·g-1.循环伏安法(CV)和恒流充放电(CP)性能测试表明:多孔碳纳米纤维具有较好的电化学性能,在1A·g-1的电流密度下比电容达275F·g-1.相比碳纳米纤维比容量提高了162%.     

静电纺丝制备空气过滤用抗分层聚酰胺66/聚丙烯腈/聚醚砜(PA-66/PAN/PES)三明治结构膜

通过在经处理的不锈钢网(SSM)上逐层电纺制备了简易有效的聚酰胺66/聚丙烯腈/聚醚砜(PA-66/PAN/PES)复合纤维过滤材料.材料中间层采用以N,N-二甲基甲酰胺(DMF)为溶剂的PAN/PES共混聚合物电纺而成.扫描电子显微镜表征和比表面积测试结果表明, 在相同纺丝条件下PES量的增加有利于减小纤维直径, 增大膜的孔隙率.同时, 通过拉伸实验测量了未带有SSM的膜的机械性能(5.857 MPa).利用PES的良好疏水性, 过滤膜表面具有相对良好的疏水效果, 接触角约为130.58°.在样品厚度尽可能相等的情况下, 通过对实际空气环境中0.3~5 μm的颗粒进行截流测试发现, PAN/PES-3的过滤效率达到且大于99%.通过机械振动和空气反吹考察了过滤膜的再生性能.此外, 还通过使用喷雾喷涂SSM研究了防分层过滤介质的基质.     

对叔丁基酰胺化杯[8]芳烃/聚丙烯腈纳米纤维对Cu~(2+)的吸附性能

以N,N-二甲基甲酰胺为溶剂,采用静电纺丝技术制备了对叔丁基酰胺化杯[8]芳烃/聚丙烯腈纳米纤维。当含Cu~(2+)溶液的酸度为pH 4.7,温度为35℃时,该纳米纤维对Cu~(2+)的吸附性能最好。该纳米纤维对Cu~(2+)的吸附既符合Langmuir吸附等温模型,也遵循Freundlich吸附等温模型。     

Process optimization and empirical modeling for electrospun polyacrylonitrile (PAN) nanofiber precursor of carbon nanofibers

Ultrafine fibers were spun from polyacrylonitrile (PAN)/N,N-dimethyl formamide (DMF) solution as a precursor of carbon nanofibers using a homemade electrospinning set-up. Fibers with diameter ranging from 200 nm to 1200 nm were obtained. Morphology of fibers and distribution of fiber diameter were investigated varying concentration and applied voltage by scanning electric microscopy (SEM). Average fiber diameter and distribution were determined from 100 measurements of the random fibers with an image analyzer (SemAfore 5.0, JEOL). A more systematic understanding of process parameters was obtained and a quantitative relationship between electrospinning parameters and average fiber diameter was established by response surface methodology (RSM). It was concluded that concentration of solution played an important role to the diameter of fibers and standard deviation of fiber diameter. Applied voltage had no significant impact on fiber diameter and standard deviation of fiber diameter.     

Electrospun EGNPs reinforced precursor carbon nanofibril composites by using RSM

Response surface methodology (RSM),based on five‐level, four variable Box‐Benkhen technique was investigated for modeling the average fiber diameter of electrospun polyacrylonitrile (PAN) nanofibers. The four important electrospinning parameters were studied including applied voltage (kV), Berry's number, deposition distance from nozzle to collector (cm), and spinning angle (? in degree). The measured fiber diameters were in a good agreement with the predicted results by using RSM technique. High‐regression coefficient between the variables and the response (R² = 87.74%) indicates excellent evaluation of experimental data by second‐order polynomial regression model. The optimum PAN average fiber diameters of 208 and 37‐nm standard deviation were collected at 19 kV, Berry's number = 10, 25^° spinning angle, and 16‐cm deposition distance. The PAN/N,N‐dimethylformamide (DMF) polymer solution with the optimum weight concentration (10 wt.%) was selected to study the effect of dispersing exfoliated graphite nanoplatelets (EGNPs) in PAN/DMF solution on the electrospun EGNP/PAN fibril composite diameter. Five different EGNPs weight concentrations (2, 4, 6, 8, and 10 wt.%) were dispersed in the optimized PAN/DMF polymer solution. Morphology of EGNPs/PAN fibril composites and its distribution were investigated by scanning electron microscopy (SEM) to show the minimum fiber diameter for the above‐mentioned 5 wt. % of EGNPs. A minimum fibril composite diameter of 182 nm was obtained at 10 wt.% of EGNPs. Morphological characteristics of electrospun fibers and their distribution were tested by Raman spectroscopy, SEM, differential light scattering, and high‐resolution transmission electron microscopy.     

不同分子量聚丙烯腈的制备及其高压静电纺丝研究

采用DMSO/H2O混合溶剂法制备了5种不同分子量的PAN,并以PAN为原料,DMF为溶剂,配成纺丝溶液,通过高压静电纺丝技术制备超细纤维毡(UFFM)。研究表明,相同单体组成和浓度、相同反应条件情况下,通过聚合制备PAN,随着混合溶剂中水含量的增加,生成的PAN粘均分子量相应增加,其转化率也增加。聚合所得的不同分子量PAN的热重分析显示,随着PAN分子量的增加,热重曲线的剧烈失重区会越来越明显,剧烈失重区的失重率也呈增加的趋势;高压静电纺丝研究发现,PAN-4和PAN-5纺丝溶液由于分子量过高而不可纺;另外,研究还发现,较高的纺丝电压有利于纤维直径的减小,但相应的纺丝稳定性减小,导致纤维直径分布的离散度增加。     

Design,Preparation and Properties of Bio-inspired Hierarchical Structure Yarns with Enhanced Thermal Insulation and Water Transfer Ability

Encouraged by the porous and stable structure of cold-resist animals' hair or feather, bio-inspired hierarchical structure yarns combining polyacrylonitrile(PAN) nanofibers and polypropylene(PP) hollow microfibers have been developed by a modified conjugate electrospinning technology. Physical cross-linking has been built to increase fibers adhesion and construct interlayer support for nanofibrous assembly. The nanofibers and hollow microfibers construct a stable porous structure with porosity of 62%, providing excellent thermal insulating ability[temperature diffe-rence(|ΔT|) between skin and yarn surface is 4.9℃] as well as good mechanical property. More interestingly, the water transfer ability (infiltrate the yarn in 10 s) of synthetic fibers has been improved greatly by the combination of thin diameter nanofibers to the yarn. It is believed that the research lays the foundation for bio-inspired engineering technology in the manufacture of thermal comfort.     

The morphology and crystalline region distribution of polyacrylonitrile nanofibers prepared by electrospinning

The effects of electrospinning parameters in a wider range on the morphology and diameters of polyacrylonitrile (PAN) fibers are studied in detail. The fibers’ diameter increases from 288 to 3469 nm swiftly with the increasing PAN concentration. With the increasing voltage or prolonging gap distance, the diameter increases primarily and decreases later. The combined effects of surface tension, splitting and stretching, electric force, viscosity, and solvent volatilization are the main reasons. Ultrasonic etching method, Atomic force microscope (AFM), Scanning electron microscope (SEM) and X-ray diffraction (XRD) technology have been utilized to verify the nature structure of electrospun PAN fibers. Combining all the results, it is deduced that there are many grooves arranging nearly perpendicular to the fiber axis on the surface of electrospun PAN fibers. The thickness of relative ordered region is 40 to 190 nm and the thickness of amorphous region is 20 to 35 nm.     

Controlling electrospun nanofiber morphology and mechanical properties using humidity

Electrospinning is a fiber spinning technique used to produce nanoscale polymeric fibers with superior interconnectivity and specific surface area. The fiber diameter, surface morphology, and mechanical strength are important properties of electrospun fibers that can be tuned for diverse applications. In this study, the authors investigate how the humidity during electrospinning influences these specific properties of the fiber mat. Using two previously uninvestigated polymers, poly(acrylonitrile) (PAN) and polysulfone (PSU) dissolved in N,N‐Dimethylformamide (DMF), experimental results show that increasing humidity during spinning causes an increase in fiber diameter and a decrease in mechanical strength. Moreover, surface features such as roughness or pores become evident when electrospinning in an atmosphere with high relative humidity (RH). However, PAN and PSU fibers are affected differently. PAN has a narrower distribution of fiber diameter regardless of the RH, whereas PSU has a wider and more bimodal distribution under high RH. In addition, PSU fibers spun at high humidity exhibit surface pores and higher specific surface area whereas PAN fibers exhibit an increased surface roughness but no visible pores. These fiber morphologies are caused by a complex interaction between the nonsolvent (water), the hygroscopic solvent (DMF), and the polymer. © 2011 Wiley Periodicals, Inc. J Polym Sci Part B: Polym Phys, 2011     

Electrospinning of Hyaluronic Acid (HA) and HA/Gelatin Blends

Summary: In the present study, electrospinning of hyaluronic acid (HA) and hyaluronic acid/gelatin (HA‐GE) blends in N,N‐dimethylformamide (DMF)/water‐mixed solvents have been investigated. When the volume ratio of DMF to water was in the range of 1.5–0.5, HA solutions could be electrospun into fibrous membranes successfully. The average diameter of HA fibers was about 200 nm. The HA‐GE composite nanofibrous membranes with varied HA/GE weight ratio in the range of 100/20–100/100 have also been successfully fabricated. The average diameter of HA‐GE fibers was in the range of 190–500 nm. The decrease in surface tension could promote fiber formation. Thus, an introduction of DMF that could decrease the surface tension distinctively, without significant change or increase in viscosity of the solution, could bypass the use of blowing‐assisted electrospinning. Our postulated picture is that the lower surface tension could help the ejection of stream with relatively high viscosity and reduce or prevent the droplet formation during the spinning process.

HA/GE (100/80) nanofibrous membrane produced by electrospinning.     

Morphology control of polyacrylonitrile (PAN) fibers by phase separation technique

Based on the constructed theoretical ternary phase diagrams of water/dimethyl sulfoxide (DMSO)/polyacrylonitrile (PAN) terpolymer system, the phase separation behavior for PAN fibers preparation was investigated. Theoretical ternary phase diagrams were determined by the extended Flory‐Huggins theory. To investigate the temperature dependence of theoretical ternary phase diagrams, all binary interaction parameters at different temperatures were determined accurately and thoroughly revisited. From numerical calculations, it was found that a small quantity of water was needed to induce phase demixing. Meanwhile, the cloud point data of the system for more dilute PAN terpolymer solutions were determined by cloud point titration, and the cloud point data for more concentrated PAN terpolymer solutions were calculated by Boom's linearized cloud point (LCP) curve correlation. Furthermore, the morphology of PAN fibers was investigated by using scanning electron microscopy (SEM). With increasing the concentration of PAN terpolymer solutions as well as the quenching depth, the morphology of PAN fibers turns from large open channels to small bead‐like structures, accompanying with a reduction of the porosity of PAN fibers. Judging from our investigation, it was clear that the final morphology of PAN fibers was mainly determined by phase separation in fiber‐forming process. © 2008 Wiley Periodicals, Inc. J Polym Sci Part B: Polym Phys 47: 261–275, 2009     

Preparation of electrospun shape memory polyurethane fibers in optimized electrospinning conditions via response surface methodology

Herein, the electrospinning method, as an effective approach, was utilized to fabricate poly (ε‐caprolactone)‐based polyurethane (PCL‐based PU) fibers. PCL was synthesized by ring‐opening polymerization, and characterized by proton nuclear magnetic resonance (¹H NMR) and Fourier‐transform infrared (FTIR) spectroscopies. Afterward, PU was prepared by step‐growth polymerization. The effects of solution concentration and solvent type on fibers' diameter were investigated. Scanning electron microscopy (SEM) images revealed that the optimum solution was N, N‐dimethylformamide(DMF): chloroform with a ratio of 60:40. In addition, results showed that bead‐less nanofibers could be achieved by a concentration of 5 w/v% (polymer to solvent). Various optimum practical parameters, such as applied voltage, feeding rate, and needle‐to‐collector distance, were obtained and compared with the results of response surface methodology (RSM). On the other hand, the mechanical evaluations indicated that the porous structure of scaffolds caused them to possess lower mechanical properties, as well as shape fixity ratios than those of bulk samples.