静电纺丝热塑性聚氨酯纳米纤维的制备

将N,N-二甲基甲酰胺（DMF）和四氢呋喃（THF）按体积比0：4、1：3、2：2、3：1、4：0混合作为溶剂,确定配比后,在不同浓度、电压下对热塑性聚氨酯（TPU）溶液进行静电纺丝。结果表明,DMF与THF的体积比对聚氨酯静电纺丝纤维的形貌、直径及其均匀性有明显影响,当混合溶液体积比为2：2,浓度为0．18g／mL,电压为26kV时,TPU纺丝液纺丝效果最佳,得到最理想的纤维;纤维直径随DMF含量的增多而减小,但当DMF含量过多时,纤维上容易出现液滴,纤维形貌变差;TPU纺丝液浓度增大,纤维直径增大;电压增大,纤维直径减小。     

不同溶剂对静电纺聚乳酸纳米纤维形态结构的影响

以聚乳酸（PLA）为原料,分别用三种不同的溶剂制得三种纺丝液并采用静电纺丝法,制备了聚乳酸纳米纤维。探讨了溶剂、电压、溶液质量分数对纤维形貌和直径的影响。结果表明,溶剂是决定PLA超细纤维形成的关键因素,三氯甲烷（CHC l3）与二甲基甲酰胺（DMF）混合溶剂（体积比为9∶1）是PLA静电纺丝较为理想的溶剂。在PLA质量分数为6%、极距15 cm、电压25 kV,流量2.5 mL/h的工艺条件下,可制备直径为1 200 nm左右的PLA纤维。     

基于静电纺丝技术的PLGA载药纳米纤维膜的制备工艺

同轴静电纺丝法制备的聚乳酸-乙醇酸(PLGA)纳米纤维具有良好的生物相容性和生物可降解性, 加之其高孔隙率和高透氧率, 使其能成为优良的药物载体。本文初步摸索了PLGA的同轴静电纺丝的工艺条件, 并通过同轴静电纺丝法制备了PLGA载氟比洛芬酯(FA)的纳米纤维膜, 应用扫描电子显微镜、红外光谱分析观察纤维的表观形貌并确定其微观结构。重点探究了不同溶剂配比的混合溶剂对载药纤维膜药物释放性能影响。研究结果表明在U⁺为+15.00kV, U^-为-2.50kV, 接受距离为15cm, 壳层推进速度为0.4mm/min, 芯层推进速度为0.1mm/min进行静电纺丝时, 所制备的PLGA(壳)/PVP+FA(核)复合载药纤维膜壳核结构良好, 且成功载了约0.5%的FA。当改变壳层混合溶剂(DCM和DMF)和芯层混合溶剂(无水乙醇和DMF)体积比时, 纤维直径会随着DMF的减少而增大。     

聚醚砜的静电纺丝研究

采用聚醚砜(PES)的良溶剂二甲基甲酰胺(DMF)和非良溶剂丙酮(AC)为共溶剂体系,研究了溶剂组成、纺丝成形条件对静电纺丝PES纤维的形貌及纤维直径的影响。结果表明:DMF/AC的配比对于静电纺丝PES纤维形貌具有直接的调控作用,随着DMF/AC混合溶剂中AC用量的增加,纤维平均直径变大,纤维毡中串珠数目明显减少,纤维均一性变好;随着纺丝液浓度的升高,纺丝电压的增大,纤维的平均直径变大;接收距离的变化对纤维平均直径影响不大;PES最佳纺丝工艺条件为纺丝溶液质量分数13%,纺丝电压15 kV,接收距离10 cm,mDMF/mAC为8.5/1.5,在此条件下,可以获得纤维平均直径为96 nm的PES纤维毡。     

Studies on the electrospun submicron fibers of SIS and its mechanical properties

The submicron fibers were prepared via electrospinning the styrene–isoprene–styrene (SIS) triblock copolymer from a pure solvent of tetrahydrofuran (THF) and a mixed solvent of THF and N, N‐dimethylformamide (DMF). The addition of DMF to THF resulted in a beneficial effect on the fiber formation and the electrospinnability. The obtained results revealed that the fibers were only formed in a narrow solution concentration range of 8–15 wt %; the morphology, diameter, structure, and mechanical performance of as‐spun fibers from PS and SIS solutions were affected by the composition weight ratio and the solution properties; and those from the solution at the intermediate concentration of 10 wt % exhibited a maximum tensile strength and strain at break. © 2009 Wiley Periodicals, Inc. J Appl Polym Sci, 2009     

高压静电场纺丝法制备羟丙基甲基纤维素邻苯二甲酸酯超细纤维

通过高压静电场纺丝法制备了羟丙基甲基纤维素邻苯二甲酸酯(HPMCP)的超细纤维,并详细研究了溶液浓度、纺丝电压及混合溶剂的配比对纤维形态和直径的影响。当混合溶剂中的无水乙醇与二氯甲烷为1∶1(V/V)时,在纺丝电压为30kV的条件下,HPMCP可纺丝的浓度范围为7%～16%(wt)。溶液浓度为7%时,电纺得到珠状纤维;浓度大于8%时,得到表面光滑的圆柱状纤维。随着纺丝溶液浓度的增大,所得纤维的平均直径逐渐增大。在HPMCP溶液浓度(8%)和溶剂组成(无水乙醇/二氯甲烷=1∶1)保持一定时,随着纺丝电压的增大,所得纤维的平均直径呈下降的趋势。而在纺丝浓度和电压一定的情况下,随着混合溶剂中二氯甲烷体积分数的增大,所得纤维的平均直径先增大后减小,无水乙醇与二氯甲烷体积比为1∶1和1∶2时,所得纤维的直径分布相对集中。     

The morphology,mechanical properties,and flammability of aligned electrospun polycarbonate (PC) nanofibers

The electrospinning of the polycarbonate (PC) solutions was performed for the variable electrospinning parameters such as polymer concentration, solvent composition, applied voltage, flow rate, and take‐up velocity in order to evaluate changes of morphology, mechanical properties, and flammability of the aligned PC nanofibers as a function of the electrospinning parameters. It was found that the ratio of THF/DMF solvent in the electrospinning parameters had a major effect on the spinnability and fiber morphology. Furthermore, it was confirmed that the mechanical properties were dependent upon the fiber morphology. The spinnability of the PC solutions with a lower THF ratio in THF/DMF solvent was poor. The aligned electrospun PC fiber with the best morphology was made in the range of polymer concentration of 22%, solvent ratio of 50:50 THF : DMF, applied voltage of 14 kV, flow rate of 0.050 ml/m, and a take‐up velocity of 7.3 m/s. The ultimate strength and initial modulus of the 80% drawn 22% PC fiber were 64 ± 2 MPa (commercial 55–75 MPa) and 1.9 ± 0.1 GPa. The heat release capacity (HRC) of the 22 and 25% PC fiber were 275 ± 27 J/g K and 198 ± 1 J/g K. It was found that the flame resistance of the electrospun PC nanofiber was superior to that of the PC raw material (HRC ～360 J/g K). POLYM. ENG. SCI., 2008. © 2008 Society of Plastics Engineers     

气流-静电纺丝法制备苯乙烯—丁二烯—苯乙烯嵌段共聚超细纤维

采用75%四氢呋喃(THF)和25%N,N-二甲基甲酰胺(DMF)的混合溶液作溶剂,通过气流-静电纺丝法制备了苯乙烯-丁二烯-苯乙烯嵌段共聚物(SBS)超细纤维。利用扫描电镜(SEM),研究了溶液浓度、电压、接收距离(喷丝孔到接收板的距离)、喷丝孔内径对静电纺纤维的直径和形貌的影响。研究发现:溶液浓度对电纺纤维的直径和形貌有非常重要的影响,当溶液浓度由10%增加到18%时,电纺纤维平均直径随之成线性增加;当电压由23.8kV增加到33.8kV时,纤维平均直径先减小后增加。最佳工艺条件为:溶液质量分数为14%,电压为28.8kV,接收距离为20cm,喷丝孔内径为0.27mm,所得SBS电纺超细纤维平均直径为429nm。     

Effects of processing parameters on morphology of electrospun polystyrene nanofibers

This study focused on the preparation of electrospun polystyrene (PS) nanofibers. PS solutions were prepared in single (dimethylformamide; DMF, dimethylacetamide; DMAc or tetrahydrofuran; THF) and mixed solvent (DMF/THF and DMAc/THF) systems with and without tetrabutylammonium bromide (TBAB) salt. The effects of PS concentration, solvent system, the addition of salt, appearance and diameter of PS fibers were examined. The average diameter of the as-spun fibers increased upon increasing PS concentration. The morphology of the fibers significantly depended on the properties of the solvents. The obtained fibers were smooth without any beads and their diameters were affected by the amount of THF in the solvent and PS concentration. The beads in the fibers disappeared and the fiber diameter significantly decreased after the addition of TBAB. The smallest diameter and the narrowest diameter distribution of PS nanofibers (376±36 nm) were obtained from 15% PS solution in DMAc with 0.025% w/v TBAB.     

静电纺丝工艺参数对PMMA／富勒烯纤维形貌的影响

采用甲苯与二甲基甲酰胺（DMF）混合溶液做溶剂,以静电纺丝法制备了含有富勒烯（C60）的聚甲基丙烯酸甲酯（PMMA）纤维,利用扫描电镜观察了纤维的形貌,分析了PMMA的质量分数、溶剂比、纺丝电压、收集距离等对纤维形貌及平均直径的影响。结果表明：PMMA溶液的浓度以及溶剂比对纤维的形貌起着主导作用,当二者变化时,纤维结构变化较大。纤维的平均直径随着PMMA浓废、纺丝电压的增大而增大;当甲苯/DMF体积比增大时,纤维平均直径先增大后减小;纤维形貌受收集距离的影响较小。     

静电纺工艺参数对SEBS纤维形貌和直径的影响

通过静电纺丝,将苯乙烯-乙烯-丁烯-苯乙烯嵌段共聚物(SEBS)溶解于四氢呋喃(THF)中的纺丝液制备成SEBS纤维,探索了纺丝液质量分数、纺丝电压和接收距离对纤维形貌及直径的影响。通过扫描电镜观察SEBS纤维的形貌以及Photoshop软件测量了SEBS纤维的直径。结果表明,纺丝液质量分数为25%、纺丝电压为10 kV、接收距离为15 cm时,纤维成型性良好,平均直径为9.7727μm;纤维直径随着电压的增大而减少,随着接收距离的增大而先减小后增大。     

The change of bead morphology formed on electrospun polystyrene fibers

Polystyrene (PS) dissolved in the mixture of tetrahydrofuran (THF) and N,N-dimethyl formamide (DMF) was electrospun to prepare fibers of sub-micron in diameters. Electropinning parameters such as polymer concentration, applied voltage and tip-to-collector distance were controlled. From these parameters it was determined that while the surface tension of polymer solution had linear correlation with the critical voltage, throughput was dependent on electric conductivity. The electrospun PS fibers produced contained irregular beads and electrospinning certainly was enhanced with increasing DMF content. The bead concentration was also controlled by DMF content. The aspect ratio of the formed beads and the diameter of fibers were increased with increasing solution concentration. When PS was dissolved in only THF, an unexpected half hollow spheres (HHS) structure appeared. Also, different shape forms of PS non-woven mats have been prepared by controlling electrospinning parameters.     

The morphology of electrospun polystyrene fibers

Electrospinning is a process of electrostatic fiber formation which uses electrical forces to produce polymer nanofibers from polymer solution. The electrospinning system consists of a syringe feeder system, a collector system, and a high power supplier. The important parameters in the morphology of electrospun polystyrene fibers are concentration, applied voltage, and solvent properties. Higher concentrations of the polymer solution form thicker fibers and fewer beads. When the concentration is 7 wt%, electrospun fibers have an average diameter of 340 nm, but as the concentration of PS increases to 17 wt%, the fiber diameter gradually thickens to 3,610 nm. The fiber morphology under different solvent mixture ratios and solvent mixtures has also been studied.     

Preparation of poly(ether sulfone) nanofibers by gas‐jet/electrospinning

Poly(ether sulfone) (PES) nanofibers were prepared by the gas‐jet/electrospinning of its solutions in N,N‐dimethylformamide (DMF). The gas used in this gas‐jet/electrospinning process was nitrogen. The morphology of the PES nanofibers was investigated with scanning electron microscopy. The process parameters studied in this work included the concentration of the polymer solution, the applied voltage, the tip–collector distance (TCD), the inner diameter of the needle, and the gas flow rate. It was found from experimental results that the average diameter of the electrospun PES fibers depended strongly on these process parameters. A decrease in the polymer concentration in the spinning solutions resulted in the formation of nanofibers with a smaller diameter. The use of an 18 wt % polymer solution yielded PES nanofibers with an average diameter of about 80 nm. However, a morphology of mixed bead fibers was formed when the concentration of PES in DMF was below 20 wt % during gas‐jet/electrospinning. Uniform PES nanofibers with an average diameter of about 200 nm were prepared by this electrospinning with the following optimal process parameters: the concentration of PES in DMF was 25 wt %, the applied voltage was 28.8 kV, the gas flow was 10.0 L/min, the inner diameter of the needle was 0.24 mm, the TCD was 20 cm, and the flow rate was 6.0 mL/h. © 2007 Wiley Periodicals, Inc. J Appl Polym Sci 2008     

PSU/PPSU复合纤维制备

对双酚A型聚砜(PSU)/聚亚苯基砜(PPSU)的混纺性以及纺丝工艺进行研究。采用扫描电镜(SEM)对不同条件下制备的PPSU/PSU复合纤维的形态进行表征。实验结果表明当溶液浓度为18.3%～21.2%,纺丝电压为10～25kV,溶剂配比二甲基乙酰胺(DMAC)∶丙酮为7∶3的时候可以得到均一的纤维。     

Processing and characterization of electrospun poly(3-hydroxybutyrate-co-3-hydroxyhexanoate) nanofibrous membranes

Poly(3-hydroxybutyrate-co-3-hydroxyhexanoate) (PHBHHx) nanofibrous membranes were first fabricated via electrospinning from chloroform (CHCl₃) or CHCl₃/dimethylformamide (DMF) polymer solutions. The electrospinning conditions such as the polymer concentration, the solvent composition, and the applied voltage were optimized in order to get smooth and nano-sized fibers. The crystalline structure, the melting behaviors and the mechanical properties of the obtained nanofibrous membranes were characterized. With pure CHCl₃ as the solvent in the electrospinning process, the finest smooth PHBHHx fibers were about 1 μm in diameter. When DMF is added to CHCl₃ as a co-solvent, the conductivity and volatility of the solution increased and reduced, respectively, and the electrospinnability of the polymer solution increased as a result. The averaged diameters of PHBHHx fibers could be reduced down to 300-500 nm when the polymer concentration was kept at 3 wt%, the ratio of DMF/CHCl₃ was maintained at 20/80 (wt%), and the applied voltage was fixed at 15 kV during electrospinning. WAXD and DSC results indicated that the crystallization of the PHBHHx nanofibers was restricted to specific crystalline planes due to the molecular orientation along the axial direction of the fibers. The crystallization behaviors of the electrospun nanofibers were significantly different from that of the cast membranes because of the rapid solidification and the one-dimensional fiber size effect in the electrospinning process. Mechanically, the electrospun PHBHHx nanofibrous membranes were soft but tough, and their elongation at break averaged 240-300% and could be up to 450% in some cases. This study demonstrated how the size of electrospun PHBHHx fibers could be reduced by adding DMF in the solvent and gave a clue of the presence of oriented molecular chain packing in the crystalline phase of the electrospun PHBHHx fibers.     

Electrospun nanofibers of block copolymer of trimethylene carbonate and ϵ‐caprolactone

The electrospinning behavior of a block copolymer of trimethylene carbonate (TMC) and ε‐caprolactone dissolved in N,N‐dimethylformamide (DMF) and methylene chloride (MC) was studied. The effects of the blended solvent volume ratio, concentration, voltage, and tip–collector distance (TCD) on the morphology of the electrospun fibers were investigated by scanning electron microscopy. The results indicated that the diameter of the electrospun fibers decreased with a decreasing molar ratio of MC to DMF, but beads formed gradually. With a decreasing concentration of the solution, the fiber diameter decreased; at the same time, beads also appeared and changed from spindlelike to spherical. A higher voltage and larger TCD favored the formation of smaller diameter electrospun fibers. The results of differential scanning calorimetry and X‐ray diffraction showed that the crystallinity and melting point of the electrospun fibers decreased when increasing the TMC content in the copolymer. Compared with the corresponding films, the crystallinity and melting point of the electrospun fibers were obviously increased. © 2005 Wiley Periodicals, Inc. J Appl Polym Sci 99: 1462–1470, 2006     

Physical and morphological characterisation of poly(L-lactide) acid-based electrospun fibrous structures: tunning solution properties

ABSTRACT

Poly(l-lactide) nano/micro fibres were produced using the electrospinning technique. The influence of solvent type and solution concentration on the morphology and structure of electrospun fibres were investigated. For this purpose, the electrospinning was performed using 2, 2, 2-trifluoroethanol (TFE) or dichloromethane (DCM) solvents at solution concentrations in a range of 5–9?wt-%. Morphological studies showed that versus DCM-based fibres with beaded structures and porous surface, when using TFE as a solvent, the uniform bead-free fibres with a smooth surface morphology were produced. Compared to DCM, the fibre diameter decreased using TFE as a solvent with lower vapour pressure while the crystallinity of the fibres increased. By increasing the solution concentration up to 9?wt-%, uniform fibres were produced with growing average diameters. Following these results, we conclude that varying the solution concentration and solvent type can modulate the final properties of electrospun fibres.     

Electrospinning of uniform polystyrene fibers: The effect of solvent conductivity

By means of the electrospinning technique, micron- and nanofibers can be obtained from polymer solutions under a very high electrical field. A special challenge is to produce bead-free uniform fibers since any minor changes in the electrospinning parameters such as slight variations in the polymer solutions and/or electrospinning experimental parameters may result in significant variations in the final nanofiber morphology. Furthermore, it is often not trivial at all to obtain reproducible uniform electrospun nanofibers for the optimized electrospinning conditions. Here we report that the conductivity of the solvent is the key factor for the reproducible electrospinning of uniform polystyrene (PS) fibers from dimethylformamide (DMF) solutions. It is shown that even slight changes in the conductivity of the DMF solutions can greatly affect the morphology of the resulting electrospun PS fibers. Here, we have carried out a thorough and systematic study on the effect of solution conductivity on the electrospinning of bead-free polystyrene (PS) fibers when dimethylformamide (DMF) was used as the solvent. Interestingly, we found out that different grades of solvent as-received (DMF) from various suppliers have slightly different solution conductivities. Consequently, the polymer solutions prepared with the same PS concentration have different conductivities, which are shown to have significant changes on the morphology of the PS fibers resulting in beaded or bead-free uniform fibers when electrospun under the identical electrospinning conditions. Such as, bead-free PS fibers were obtained from PS solutions in the range of 20% (w/v) through 30% (w/v) depending on the DMF grade used. In brief, it was observed that solutions with a higher conductivity yielded bead-free fibers from lower polymer concentrations, which confirms that the solution conductivity plays a very significant role in producing bead-free uniform PS fibers.     

电纺法制备聚丙烯腈基纳米碳纤维

用电纺法制备了聚丙烯腈（PAN）纳米纤维，用场发射扫描电镜（FESEM）对其形态进行了研究，讨论了不同工艺参数对纤维直径和分散形态的影响。结果发现，纤维直径随着浓度的增加而增大，随着电压升高而减小，接收距离和溶剂类型对纤维直径的影响不大。将形态最好的纤维在240℃下进行活化处理，然后将活化处理过的纤维在氮气氛中煅烧，用FESEM观察了煅烧的纤维直径及形态的变化，红外（IR）分析了纤维化学结构的变化，证实了经900℃煅烧后的纤维为碳纳米纤维。