再生丝素蛋白水溶液静电纺丝性能的研究

运用静电纺丝方法,从再生蚕丝素蛋白水溶液中制得了念珠状的、圆形的或扁平状的超细再生丝,纤维的直径在100～900nm之间,平均为700nm.溶液浓度和电压强度对静电纺丝性能的影响很大,当纺丝液浓度为28%（质量分数）,电压为20kV,喷射距离为 11cm时,可制得具有光滑表面的圆形再生丝.大角X衍射（WAXD）测试结果认为,静电纺再生丝中含有α螺旋和β-折叠结构,但其结构既不同于无定型丝素膜,也不同于天然蚕丝纤维,介于二者之间.     

二醋酸(SCA)纳米纤维的制备与性能表征

为了研究二醋酸纳米纤维的制备方法和性能,采用静电纺丝技术,选择丙酮和二甲基乙酰胺为溶剂,制备出直径分布均匀的SCA纳米纤维膜.利用原子力显微镜(AFM)和扫描电镜(SEM)及相关软件,分析纳米纤维直径分布及形态;在静电纺电压为16kV、纺丝液质量分数为11%、接收距离(C-SD)为12cm的条件下,纺出连续均匀的纳米纤维,其直径分布在200～300nm之间;对二醋酸纳米纤维膜进行透气性测试发现,纳米纤维膜的透气性与中性定性滤纸的透气性相当.     

MWNTs/丝素/聚酰胺共混静电纺纳米纤维毡的结构和性能

静电纺再生丝素纤雏具有在水中易溶胀、结构稳定性和力学性能差等缺陷.在前期研究聚酰胺6/66对静电纺丝素纤维的结构和性能改进效果的基础上,以多壁碳纳米管(MWNTs)增强静电纺丝素/聚酰胺6/66复合纳米纤维.研究发现,随着MWNTs含量的增加复合纤维毡的颜色由白色变成黑色,纤维直径逐渐减小,并且都在90nm以下.MWNTs的加入,还有效地提高了纤维的结晶度、热稳定性以及纤维毡的拉伸力学性能.     

动态线性电极静电纺PVA纳米纤维的可纺性

为了解决传统针式静电纺针头易堵塞不易产业化的问题,采用铜丝动态线性电极静电纺丝技术对PVA纳米纤维的可纺性进行研究。利用扫描电子显微镜研究了PVA溶液浓度、电压和纺丝距离对PVA纤维形貌及直径分布的影响。结果表明:随PVA溶液浓度降低,溶液粘度和电导率减小,纤维直径及其分布变小。且随纺丝距离增大,纤维直径变细,纤维形貌变好。当PVA浓度为10%(质量分数),电压80 kV,距离30 cm时,可制备出形貌良好的纳米纤维,其直径为433 nm,产量高达 6.8 g/h ;当PVA浓度为5%(质量分数),电压80 kV,距离30 cm, 可纺最细纤维直径为96 nm。本研究可为未来PVA静电纺纳米纤维膜的规模化制备提供参考。     

尼龙66电纺纳米纤维膜的纤维分散形态和结晶性能

采用高压静电纺丝方法,制备了尼龙66电纺纤维膜,纤维的直径为纳米级。运用场发射扫描电镜(EFSEM)观察了纺丝液的浓度、电压、固化距离等参数对尼龙66电纺纤维膜的纤维分散形态和直径大小的影响,运用XRD分析了纺丝液浓度和电压对电纺纤维结晶度的影响。结果表明,纺丝液浓度对纤维分散形态有决定性作用,尼龙66电纺纤维膜结晶度比未纺丝的尼龙66的结晶度要低得多,并且电压对结晶度影响很大,电压增加使结晶度降低,电纺纤维膜的晶体结构趋于无定型。     

仿生制备的再生丝素蛋白水溶液的静电纺丝(Ⅰ)——工艺参数及结构特性

制备出了与蚕腺体内纺丝液浓度和后部丝腺pH值相近的再生丝素蛋白水溶液,利用静电纺丝技术模仿蚕在空气中吐丝的过程得到了再生丝素蛋白纤维.所得纤维的直径在350～4200nm之间,平均直径1700nm.通过正交实验方法考察了各种因素对纤维形态、直径及直径分布的影响,结果表明:所施电压对纤维的形态影响最大;溶液浓度对纤维的直径影响最大;喷头与接受板间距离对纤维直径的分布影响最大.实验得出了一个较好的静电纺丝条件为浓度30%,电压40kV,喷头与接受板间距离20cm.采用拉曼光谱、X衍射、DSC对再生丝素蛋白纤维进行了表征,发现再生丝素蛋白纤维中含有少量的Silk I结晶结构,主要以无定形结构为主,这与天然蚕丝的半结晶结构相比尚有差异.     

同轴静电纺再生丝素/丝胶蛋白纤维的制备及其形态结构表征

模仿蚕丝的组成和结构,利用同轴静电纺丝法制备了以再生丝素蛋白（RSF）为＂芯＂、丝胶蛋白（SS）为＂皮＂的双组分静电纺纤维。通过扫描电镜和透射电镜研究了内层纺丝液流速（Qc）、电压（U）、接收距离（D）以及场强（E）等参数对同轴静电纺RSF/SS纤维形态结构的影响。研究结果表明纤维的平均直径在1400～2100nm左右,皮-芯层结构清晰;Qc对纤维皮-芯层结构的影响较大,过大的内层纺丝液流速会因外层丝胶对内层丝素的包裹不均匀而导致偏芯现象;随E的增加（U增加或D减小）,纤维的直径及其分布显著减小,皮-芯层结构清晰;相同E下,高电压、长距离利于纤维的细化,使直径变细且分布均匀,皮-芯层结构明显。     

静电纺工艺参数对含银PA6纳米纤维直径的影响

为了研究静电纺工艺参数对含银PA6纳米纤维直径分布的影响,采用静电纺丝技术,在不同含银量、纺丝液质量分数、纺丝电压、接收距离(C-SD)、喷嘴直径条件下制备出含银PA6纳米纤维膜.利用扫描电镜(SEM)及相关软件分析纳米纤维直径分布及形态,在银溶胶质量分数0.2%～0.4%、纺丝液质量分数10%～16%、纺丝电压12～21kV、接收距离9～18cm、喷嘴直径0.5～1.2mm的实验范围内,纳米纤维的平均直径为70～90nm;纳米纤维直径随银溶胶质量分数的增加而减小,随纺丝液质量分数的增加而增大,随喷嘴直径的增大而增大;电压和接收距离对纳米纤维直径的影响较小.     

静电纺丝制备聚乙烯醇/再生柞蚕丝素蛋白复合纳米纤维

将聚乙烯醇(PVA)与再生柞蚕丝素蛋白(RWSF)共混,通过静电纺丝技术制备了PVA/RWSF复合纳米纤维,在保持材料降解性能和力学强度不变的前提下,获得了具有生物活性的表面。应用正交法优选出PVA/RWSF复合纳米纤维的最佳制备工艺参数。扫描电镜观察到,各组电纺膜中纤维的形貌较好,不同参数条件下纤维的直径和均匀程度有较大差别;方差分析表明,静电纺丝过程中纺丝液浓度、PVA/RWSF质量比和纺丝电压对纤维均匀性的影响显著;结合后期验证性实验确定PVA/RWSF复合纳米纤维最佳电纺参数为电纺液浓度0.09 g/mL、PVA/RWSF质量比90/10、纺丝电压18kV、推进速度1.5mL/h、接收距离14cm,此时制备的纤维均一、纤细,重复性好。     

动态线纺聚乙烯醇/海藻酸钠纳米纤维膜的制备

为了实现静电纺纳米纤维产量化的制备,使用自主设计的无针式动态线性电极静电纺丝机制备聚乙烯醇(PVA)/海藻酸钠(SA)(AP)纳米纤维膜。采用扫描电子显微镜(SEM)研究PVA/SA配比、收集距离和纺丝电压对纤维形貌及直径分布的影响。结果表明,PVA/SA配比对纤维形貌影响最大,随着SA含量降低,溶液牵伸顺利;在此基础上随着距离增加,纤维形貌逐渐改善但不匀率有所增加。当7.5%PVA与2%SA按体积比9∶1共混时,所得纤维形貌及直径分布最佳,最佳纺丝电压和距离分别为75 kV和25 cm,纤维平均直径为(187±44) nm,产量可达2.5 g/h。为AP纳米纤维膜的规模化制备提供了参考。     

A novel electrospun silk fibroin/hydroxyapatite hybrid nanofibers

A novel electrospinning of silk fibroin/hydroxyapatite hybrid nanofibers with different composition ratios was performed with methanoic acid as a spinning solvent. The silk fibroin/hydroxyapatite hybrids containing up to 30% hydroxyapatite nanoparticles could be electrospun into the continuous fibrous structure. The electrospun silk fibroin/hydroxyapatite hybrid nanofibers showed bigger diameter and wider diameter distribution than pure silk fibroin nanofibers, and the average diameter gradually increased from 95 to 582 nm. At the same time, the secondary structure of silk fibroin/hydroxyapatite nanofibers was characterized by X-ray diffraction, Fourier transform infrared analysis, and DSC measurement. Comparing with the pure silk fibroin nanofibers, the crystal structure of silk fibroin was mainly amorphous structure in the hybrid nanofibers. X-ray diffraction results demonstrated the hydroxyapatite crystalline nature remained as evidenced from the diffraction planes (002), (211), (300), and (202) of the hydroxyapatite crystallites, which was also confirmed by Fourier transform infrared analysis. The thermal behavior of hybrid nanofibers exhibited the endothermic peak of moisture evaporation ranging from 86 to 113 °C, and the degradation peak at 286 °C appeared. The SF/HAp nanofibers mats containing 30% HAp nanoparticles showed higher breaking tenacity and extension at break for 1.1688 ± 0.0398 MPa and 6.55 ± 1.95%, respectively. Therefore, the electrospun silk fibroin/hydroxyapatite hybrid nanofibers should be provided potentially useful options for the fabrication of biomaterial scaffolds for bone tissue engineering.     

载药电纺丝素蛋白纤维毡的结晶含量对其药物释放的影响

以水溶液体系的再生丝素蛋白为原料,利用静电纺丝技术制备了载罗丹明B的丝素蛋白纤维毡。利用甲醇水溶液对其进行后处理,考察了不同处理时间下丝素蛋白的结晶含量对药物释放的影响。通过水溶性质量损失率、接触角、扫描电镜、傅里叶红外光谱、X射线衍射光谱及紫外光谱对处理前后的丝素蛋白纤维毡的表面形貌和结构以及药物释放行为进行了表征。结果表明,随着甲醇水溶液处理时间的延长,电纺丝纤维的质量损失率减小,亲水性减弱,丝纤维中的Silk II结晶(由β-折叠结构组成)含量增加,药物释放速率也增加。即通过控制处理时间,可以控制丝纤维中Silk II结晶的含量,从而控制药物的释放速率。     

Bacterial cellulose nanocrystals-embedded silk nanofibers

Nanofibrous Bacterial cellulose nanocrystals (BCNs)-embedded silk fibroin were successfully fabricated using electrospinning. The morphology, structure and mechanical properties of the silk fibroin nanofibers were investigated at various BCNs concentrations from 0 to 7 wt%. SEM, TEM and XRD analyses were conducted to confirm the incorporation of the BCNs in the electrospun silk fibroin nanofibers. The average diameter of the silk fibroin/BCNs nanofibers increased from 230 to 430 nm according to the increasing of the BCNs ratio due to the rising solute content. The FT-IR spectra confirmed the conformational transition of the silk fibroin, from a random coil to a beta-sheet structure, which shows the enhanced mechanical properties of silk fibroin based nanofibers even with small amounts of the BCNs. Moreover, it was observed that the Young's modulus of the silk fibroin/BCNs nanofibers unexpectedly increased with the formation of BCNs with a percolation structure at a concentration between 3 and 5 wt%.     

The influence of electrospinning parameters on the morphology and diameter of poly(vinyledene fluoride) nanofibers- effect of sodium chloride

Electrospinning was used to produce PVDF nonwoven fiber mats under varying parameters of polymer concentration, applied voltage, salt content, and spinning distance. The results indicated that both the polymer and salt concentration had a noteworthy influence on both the morphology and diameter of the nanofibers. Improved fiber morphology and increased PVDF fiber diameter were observed as the PVDF concentration was increased. Adding different concentrations of NaCl to the PVDF polymer solution resulted in improved electrospinnability of PVDF resulting in better morphology and with increasing salt content, smaller fiber diameter. In particular increasing the salt content led to well defined fibers in otherwise nonfiber-producing formulations. The applied voltage and spinning distance were also seen to have an influence on the properties of the PVDF nanofibers. Nanofibers without beads were formed under the improved conditions of the different parameters studied.     

聚-DL/L-丙交酯(30DL/70L)纳米纤维的电纺研究

对生物可吸收聚-DL/L-丙交酯(30DL/70L)体系进行了静电纺丝.研究了聚-DL/L-丙交酯(30DL/70L)的浓度,加料速度,电压,喷头与接收体之间的距离等因素对纤维形态的影响,制备出纳米纤维膜,并用扫描电镜(SEM)等对纤维膜进行表征.结果表明,电纺溶液浓度和溶剂对纤维直径影响比较明显,减小电纺溶液浓度和采用复合溶剂CHCl3/DMF可得到更细的纳米纤维;一定范围内适当的增加电压、减小距离和减小加料速度有利于减小纤维直径.在聚-DL/L-丙交酯(30DL/70L)浓度为5g/100mL溶剂、加料速度1mL/h、喷头与接收体之间的距离6cm、电压15kV电纺条件下,可制备直径50nm左右的聚-DL/L-丙交酯(30DL/70L)纳米纤维膜.     

Statistical optimization of the electrospinning process for chitosan/polylactide nanofabrication using response surface methodology

In this study, chitosan/polylactide (CP) blend solutions in trifluoroacetic acid as a co-solvent with different blend ratio were electrospun. Effects of different CP ratio and process parameters on the diameter of electrospun nanofibers were experimentally investigated. The fiber morphology and the distribution of fiber diameter were investigated by scanning electron microscopy. Response surface methodology (RSM) was used to define and evaluate a quantitative relationship between electrospinning parameters, average fiber diameters and its distribution for each chitosan–polylactide ratio. Applied voltage and polymer solution extrusion rate are the process variables which control the fiber diameter at similar spinning distances (15 cm). Fiber diameter was correlated to these variables by using a second-order polynomial function. The fibers were of diameter ranging from 94 to 389 nm. The predicted fiber diameters were in good agreement with the experimental results. Contour plots were obtained to identify the processing variables suitable for producing nanofibers. It was concluded that ratio of polylactide and chitosan in the blend polymer played an important role to the diameter of fibers and standard deviation of fiber diameter. The processing factors were found statistically significant in the production of nanofibers.     

Study on the structure of SF fiber mats electrospun with HFIP and FA and cells behavior

Bombyx mori silk fibroin (SF) fiber mats were prepared by electrospinning with the solvent of hexafluoroisopropanol (HFIP) and formic acid (FA). The average diameters of SF fiber mats observed by SEM were 2.0 and 0.3 μm when different solvent, HFIP and FA, were used. Fourier transform infrared and X-ray diffraction were employed to study the secondary structure of the SF fiber mats; the results showed that the electrospin solvent not only affect the secondary structure of as-spun SF fiber mats, but also indirectly affect the structure transition of SF fiber mats post-treatment with ethanol. And the SF fiber mats electrospun with FA showed more β-sheet structure before and after ethanol treatment. The differential thermal analysis curve indicated that the solvent of HFIP or FA had a weak effect on the thermal properties of SF fiber mats. To assay the cytocompatibility and cell behavior on the SF fiber mats, cell attachment, spreading, and proliferation of normal human epidermal fibroblasts (NHEF) seeded on the scaffolds was studied. The results indicated that the SF fiber mats support NHEF attachment and growth on SF fiber mats in vitro, and no difference between the SF fiber mats electrospun with HFIP and FA was observed. In this article, a desired morphology and secondary structure of SF fiber mats could be prepared by choosing different electrospinning solvent.     

Silver nanoparticles incorporated electrospun silk fibers

We present a simple and mass-producible method of incorporating silver nanoparticles on the surface of electrospun silk non-woven membranes for the fabrication of antimicrobial wound dressings. Nanofibrous silk membranes with fiber diameters of 460 +/- 40 nm were electrospun from an aqueous Bombyx mori fibroin solution. The electrospun membranes incorporating silver nanoparticles were prepared by dipping the membranes in aqueous silver nitrate (AgNO3) solution (0.5 or 1.0 wt%) followed by photoreduction. Field emission scanning and transmission electron microscopy showed that silver nanoparticles were generated on the electrospun silk fibroin nanofibers as well as inside them. The interaction between the silver nanoparticles and amide groups in the silk fibroin molecules was characterized using X-ray photoelectron spectroscopy.