再生丝素/丝胶蛋白水溶液的同轴干法纺丝

模仿蚕丝的成分、结构和成丝方法,通过同轴干法纺丝初步制备了以添加有金属钙离子（Ca2＋）并调节了pH值的再生丝素蛋白（RSF）为芯层、丝胶蛋白（SS）为皮层的RSF/SS纤维。采用荧光显微镜、扫描电镜、拉曼光谱和材料试验机研究了所得纤维的微观形貌、二级结构和力学性能,并与纯RSF纤维和蚕丝进行了对比。研究结果表明同轴干法纺RSF/SS纤维具有清晰的皮-芯层结构,直径较粗且表面略有皱痕;与纯RSF纤维相比,该初生纤维具有更多的β-折叠构象,力学性能也相对较好,但与天然蚕丝相比尚有较大差距。     

复合同轴生物碳纳米管纤维制备方法

利用同轴静电纺丝方法制备碳纳米管/生物聚合物的"壳-芯"结构纤维,实验发现碳纳米管加入(质量分数)0.01%能很好与聚合物融为一体,纺出内外层均可以复合碳纳米管的复合纤维,外层直径最大4000 nm、内层为2000 nm,而最小外直径165 nm,外层壁厚为127 nm,控制方法比单轴静电纺丝复杂,电压提高有利于纤维直径减小,可达到几微米,但纺丝速率达到最大值有一个最佳电压范围,碳纳米管加入提高了纤维的热稳定性,拉伸提高纤维的结晶度。     

同轴静电纺丝制备PCL-PLA芯-壳结构复合纤维及其形态分析

本文采用同轴静电纺丝技术制备聚己内酯(PCL)-聚乳酸(PLA)芯-壳结构复合纤维。通过扫描电子显微镜(SEM)观察芯层-壳层溶液推进速度、纺丝电压和收集距离对PCL-PLA复合纤维形貌的影响;通过透射电子显微镜(TEM)分析芯层-壳层溶液推进速度比对PCL-PLA芯-壳结构形成的影响。结果表明:当壳层溶液推进速度大于芯层时,形成了完整的芯-壳结构;另外,随着壳层溶液推进速度的增加,PCL-PLA复合纤维芯层含量降低;随着纺丝电压和收集距离的增加,PCL-PLA复合纤维平均直径减小。     

同轴共纺技术制备聚苯乙烯中空亚微米纤维

利用同轴静电纺丝技术制备出壳层为聚苯乙烯(PS),芯层为聚乙烯吡咯烷酮(PVP)的壳-芯结构复合纤维,通过除去芯层PVP,成功地制备出了PS中空亚微米纤维。并对其进行了TEM、SEM测试。结果表明,纺丝过程中内、外液流速比值K直接影响着复合泰勒锥的形成及复合纤维的微观形态,且复合纤维平均直径随K值的增大而减小。     

聚砜的静电纺丝工艺及其产品的热处理

采用N,N’-二甲基甲酰胺（DMF）溶剂制备了聚砜（PSF）静电纺丝溶液,并通过SEM研究了静电纺丝工艺对纤维形态和直径的影响。结果表明,由质量分数为20%的PSF/DMF溶液可以获得连续均匀的纤维。通过SEM、XRD、TG和力学性能测试,研究了热处理温度和时间对静电纺PSF纤维毡的形态结构、聚集态结构和拉伸力学性能的...     

静电纺纤维素纳米晶体/壳聚糖-聚乙烯醇复合纳米纤维的制备与表征

通过探索纤维素纳米晶体（CNC）添加量对壳聚糖-聚乙烯醇（CS-PVA）基体性能的影响,为静电纺CNC/CS-PVA复合纳米纤维的制备提供理论支撑。以CNC、CS和PVA为原料,采用静电纺丝法成功制备不同CNC含量（质量分数）的静电纺CNC/CS-PVA复合纳米纤维,并通过SEM、TGA和FTIR等分析手段对CNC/CS-PVA复合纳米纤维的微观结构和性能进行了表征。结果表明：添加CNC后静电纺CNC/CS-PVA复合纳米纤维直径变大,表面变粗糙,力学性能和热学性能提高;随着CNC含量的增加,静电纺CNC/CS-PVA纤维的杨氏模量（E）和抗拉强度（σ）先增强后减弱,而外延起始温度继续上升。当CNC含量为3wt%时,静电纺CNC/CS-PVA复合纳米纤维力学性能最好,相比于CS-PVA复合纳米纤维,E和σ分别提高了43.9%和24.8%;当CNC含量为20wt%时,静电纺CNC/CS-PVA复合纳米纤维直径分布不均匀,可以观察到单根纤维表面存在少量的球状结构物质,同时外延起始温度达到328.83℃;FTIR分析得出,CNC与CS和PVA之间只存在分子间的相互作用而没有发生化学反应;随着溶液的酸性减弱,碱性增强,不同CNC含量的静电纺CNC/CS-PVA复合纳米纤维稳定性逐渐提高,而CNC含量对其稳定性影响不大。     

木薯淀粉接枝苯乙烯/丙烯酸丁酯-聚己内酯壳核纤维的制备及表征EI北大核心CSCD

利用自由基聚合反应制备了木薯淀粉(CS)接枝苯乙烯(St)/丙烯酸丁酯(Ba)共聚物(CS-g-St/Ba),并且通过同轴静电纺丝法制备了以聚己内酯(PCL)为核层,CS-g-St/Ba为壳层的核壳结构纤维膜。分析了核层PCL浓度和流速对纤维形貌的影响,随着核层PCL浓度的增加,珠状纤维逐渐减少,最后形成无珠粒纤维,且纤维的平均直径逐渐增大,随着核层PCL流速的增加,纤维的平均直径先减小后增大;通过对核壳纤维的透射电镜和纤维断面扫描电镜观察可以清晰地看到壳层CS-g-St/Ba和核层PCL;红外光谱分析表明,St和Ba能同时接枝在CS骨架上,核壳纤维膜中同时含有CSg-St/Ba和PCL;核壳结构纤维膜的拉伸强度为1.58MPa,弹性模量为12.63MPa。相对于单轴静电纺CS-g-St/Ba和PCL纤维膜,核壳结构纤维膜的力学性能明显提高。     

超声波振动在静电纺丝技术中的应用

使用自行设计的振动静电纺丝设备分别对聚丙烯腈（PAN）和聚氧乙烯（PEO）进行了振动纺丝实验，实验结果表明，使用具有振动力场作用的静电纺丝设备，对于普通静电纺丝可以纺的溶液，纺出的纤维直径明显降低；对于粘度过高普通静电纺不能纺丝的聚合物溶液，可以进行纺丝。     

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.     

PBS-SF核-壳结构复合超细纤维膜的制备及性能

利用同轴静电纺丝方法, 制备聚丁二酸丁二酯(PBS)-丝素蛋白(SF)核-壳结构复合超细纤维膜, 并对复合超细纤维膜进行FE-SEM、 TEM形态表征, 分析了内层纺丝流率对纤维形貌的影响; 通过FTIR和XRD测试, 比较了甲醇处理前后复合超细纤维膜分子结构和结晶性能的变化, 并进行力学性能测试。结果表明: 通过对纤维核层PBS、 壳层SF和横截面的观察, 复合超细纤维有明显的核-壳结构, 可以清晰看出纤维的核层PBS和壳层SF; 随着核层纺丝流率的增大, 超细纤维的平均直径增大; 甲醇处理后, 复合超细纤维膜中壳层SF分子结构由无规构象转变为β-折叠构象, 复合超细纤维膜核层衍射吸收强度减小, 但整个核-壳结构复合超细纤维膜结晶性能无明显变化; 甲醇处理后拉伸破坏应力从14.9 MPa增大到17.2 MPa, 但拉伸破坏应变从96.8%减小到81.8%。      

丝胶组分和高湿后处理对静电纺丝素纤维结构与性能的影响

利用静电纺丝法制备了再生丝素和再生丝素/丝胶蛋白纤维,并对所得纤维进行了高湿后处理。采用扫描电镜分析了丝胶蛋白和高湿后处理对静电纺再生丝素蛋白纤维形貌的影响,采用拉曼光谱、X射线衍射和热失重分析研究了所得纤维微细结构及热性能。研究结果表明,添加丝胶蛋白有利于降低静电纺再生丝素蛋白纤维的直径及其分布,而高湿后处理对纤维的形貌没有明显影响;添加丝胶蛋白和/或高湿后处理有利于促进丝素发生向β-折叠构象的转变,并使纤维的结晶结构得到改善,从而进一步提高纤维的热稳定性。     

再生丝素/丝胶共混蛋白水溶液的静电纺丝

采用静电纺丝方法制备了再生丝素/丝胶共混纤维,分析了共混配比对再生丝素/丝胶水溶液流变性能和静电纺可纺性的影响,通过扫描电镜、拉曼光谱和DSC等手段研究了所得纤维的形态和微细结构及其力学性能。研究结果表明:随着溶液中丝胶含量的增加,体系的表观粘度增大,静电纺纤维的直径减小且直径分布变窄;并且丝胶的存在有利于丝素蛋白从无规卷曲或α-螺旋结构向β-折叠结构转变,由此可提高静电纺纤维的力学性能。     

Fabrication and characterization of fibroin solution and nanoparticle from silk fibers of Bombyx mori

The present investigation aims to study the effect of degumming time on the structural property of silk fiber obtained by silk cocoons of Bombyx mori, followed by preparation of the regenerated silk fibroin (RSF) solution which can be subsequently molded into silk nanoparticles. Silk fibers degummed with different media at different time intervals were investigated for the degumming loss and were characterized using Ffourier transform infrared (FTIR), differential scanning calorimetry (DSC), x-ray diffraction (XRD), and scanning electron microscopy (SEM). Maximum degumming was observed when the fibers were treated with sodium carbonate for 60 min. SEM and atomic force microscopy (AFM) images of RSF solution showed aggregation of silk globules resulting in formation of solvated macrochains and giving it an appearance of island-like morphology. Blank silk nanoparticles prepared from the RSF solution showed a smooth and spherical surface devoid of any adhesion using SEM, AFM, and transmission electron microscopy (TEM). The prepared silk nanoparticles may further be explored for loading drug entities and targeting.     

Release of lysozyme from electrospun PVA/lysozyme-gelatin scaffolds

This article describes an electrospinning process in fabricating ultra fine fibers with core-shell structure. A biodegradable polymer, poly(vinyl alcohol) (PVA), was used as the shell; lysozyme was a kind of antioxidant; and gelatin were used as the core.Morphology and microstructure of the ultra fine fibers were characterized by scanning electron microscope (SEM), transmission electron microscopy (TEM) and X-ray photoelectron spectroscopy (XPS) analysis. As a comparison, composite nanofiber PVA/lysozyme-gelatin blend was prepared by a normal electrospinning process. In vitro drug release behaviors of the nanofibrous membranes were determined in phosphatebuffered saline (PBS) solution. It was found that core-shell nanofibers PVA/lysozyme-gelatin obviously exhibit higher initial release rates compared to that of PVA/lysozymegelatin blend nanofibers. The current method may find wide application in controlled release of bioactive proteins and tissue engineering.     

Release of lysozyme from electrospun PVA/lysozyme-gelatin scaffolds

This article describes an electrospinning process in fabricating ultra fine fibers with core-shell structure. A biodegradable polymer, poly(vinyl alcohol) (PVA), was used as the shell; lysozyme was a kind of antioxidant; and gelatin were used as the core. Morphology and microstructure of the ultra fine fibers were characterized by scanning electron microscope (SEM), transmission electron microscopy (TEM) and X-ray photoelectron spectroscopy (XPS) analysis. As a comparison, composite nanofiber PVA/lysozyme-gelatin blend was prepared by a normal electrospinning process. In vitro drug release behaviors of the nanofibrous membranes were determined in phosphate-buffered saline (PBS) solution. It was found that core-shell nanofibers PVA/lysozyme-gelatin obviously exhibit higher initial release rates compared to that of PVA/lysozyme-gelatin blend nanofibers. The current method may find wide application in controlled release of bioactive proteins and tissue engineering.     

Preparation of regenerated silk sericin/silk fibroin blend microparticles by emulsification–diffusion method for controlled release drug delivery

This study reports drug-loaded silk sericin (SS)/silk fibroin (SF) blend microparticles being fabricated by the water-in-oil emulsion solvent diffusion of a SS/SF aqueous blend solution. Blue dextran was used as the water-soluble drug model. The influence of the SS/SF blend ratio on the characteristics and drug release behavior of the blend microparticles was investigated. The blend microparticles were analyzed by scanning electron microscopy (SEM), Fourier transform infrared (FTIR) spectroscopy, thermogravimetric analysis (TGA) and UV-vis spectroscopy. The blend microparticles were nearly spherical in shape as determined from SEM micrographs. The FTIR and TG results demonstrated that interactions between SS and SF molecules had occurred. The blend microparticles showed very high drug loading efficiency (94–98%) for all blend ratios. The in vitro drug release significantly decreased with decreasing SS blend ratio. The results demonstrated that the SS/SF blend microparticles could be used as biocompatible and biodegradable microparticles for controlled release drug delivery applications.     

A novel route to synthesize CdS quantum dots on the surface of silk fibers via γ-radiation

CdS quantum dots (QDs) were successfully synthesized on the surface of silk fibers via γ-ray irradiation. Scanning electron microscope (SEM) measurement revealed that the particles on the silk fibers were less than 15nm in diameter. The energy dispersion spectrum (EDS), X-ray diffraction (XRD), laser scanning confocal microscope (LSCM) were also used to identify and investigate the properties of products. Moreover, a mechanism for the formation of CdS QDs on silk fibers under γ-radiation was generally discussed. The resulting silk fibers coated with CdS QDs might be useful as smart structural fabrics in a range of applications.     

Preparation and characterization of electrospun nanofibers based on silk sericin powders

The present contribution reports the fabrication and characterization of silk sericin (SS) nanofibers via electrospinning. The function of solution concentration on morphological appearance and average diameter of the electrospun SS membranes was investigated by scanning electron microscopy. The structure and physical properties were observed by Fourier transform infrared spectroscopy (FT-IR), differential scanning calorimetry (DSC), and thermogravimetric analysis (TG). All beads were acquired in lower concentration of SS solution, 1.3–8.5 wt% of SS solutions, and beaded fibers were produced from 9.6, 11.7, 14.2, and 16.5 wt% of SS solution. The perfect nanofibers acquiring average diameters of 145 and 184 nm were fabricated from 20.9 to 22.9 wt% of SS solution, respectively. Results from FT-IR showed that in the as-spun fibers, SS was present in a random coil conformation, while after heat treatment, the molecular structure of SS was transformed into a β-sheet containing structure. DSC and TG analysis illustrated that trifluoroacetic acid can be eliminated by heating. The availability of SS nanofibers introduces a new set of possible uses of these amazing fibers at a scale not explored before. New uses include small diameter fibers for cell proliferation purposes, nanocomposite reinforcing fibers for nanotechnology, wound dressing, scaffolds for tissue engineering, and other biomedical applications.     

Synthesis of oriented hydroxyapatite crystals: Effect of reaction conditions in the presence or absence of silk sericin

The purpose of this study was to investigate the effect of silk sericin (SS) on the morphology and crystallinity of hydroxyapatite (HAp) crystals synthesized at the pH 7.4-12 and 50 °C via a biomimetic method. Using X-ray diffraction (XRD), transmission electron microscope (TEM) and high-resolution transmission electron microscope (HRTEM), it was revealed that a homogeneous assembly could be obtained in the presence of SS, which held a highly ordered microstructure and poor crystallinity. But in the absence of SS, an oriented aggregate could be prepared at 50 °C and pH 10, which held more confused crystal lattice lines. The results proved that the biomimetic structure of HAp could be constructed under the controlled reaction conditions, which may offer a new clue on the understanding of the process of biomineralization.     

以LiBr/C_2H_5OH/H_2O为溶剂的PVA/SF共混体系的相容性

采用LiBr/C2H5OH混合溶剂制备丝素(SF)溶液,与聚乙烯醇(PVA)水溶液进行溶液共混后得到PVA/SF共混膜,采用扫描电镜,差示扫描量热分析,红外光谱,X射线衍射等方法对共混膜进行了形态和结构表征。研究表明,相对于将PVA水溶液与SF水溶液共混得到的共混体系,此方法制备的体系中两组分的相容性得到了一定程度的提高。在SF含量较小的情况下,共混体系中几乎观察不到两相结构的存在。证明在PVA/SF体系中,SF的溶剂选择及SF的含量影响两种组分的相容性。