Mechanical and thermal properties of waste silk fiber‐reinforced poly(butylene succinate) biocomposites

This article reports the mechanical and thermal properties of poly(butylene succinate) (PBS) biocomposites reinforced with industrially available waste silk fibers, fabricated with varying fiber contents and lengths. The result indicates that use of waste silk fibers may be a potential as reinforcement for effectively improving the static and dynamic mechanical properties of a biodegradable polymer matrix resin, depending on the waste silk fiber content and length in the present biocomposite system. The “as‐separated” waste silk/PBS biocomposites showed the maximum tensile and flexural properties at a fiber loading of 40 wt %, and the “chopped” waste silk/PBS biocomposites showed the optimal strength and modulus with waste silk fibers of 12.7 mm length. The chopped waste silk fibers play a more contributing role in improving the mechanical properties of waste silk/PBS biocomposites than the as‐separated waste silk fibers at a fixed fiber loading. Above the glass transition temperature, the storage modulus of waste silk/PBS biocomposites was significantly greater than that of PBS resin, especially in the higher temperature region. © 2006 Wiley Periodicals, Inc. J Appl Polym Sci 100: 4972–4980, 2006     

Mechanical properties of tussah silk fibers treated with methacrylamide

Tussah silk fibers were treated with methacrylamide (MAA). The polymerization of MAA onto tussah silk fibers and the mechanical properties of the MAA-treated tussah silk fibers were investigated. The tanning agent contained in tussah silk fibers acted as an inhibitor to the radical polymerization of MAA. The alkali treatment enhanced the swelling of noncrystalline regions of the tussah silk fibers and promoted the polymerization of MAA onto the tussah silk fibers. The cross-sectional area of the MAA-treated tussah silk fiber was given by the sum of the cross-sectional area of the original silk fiber and that of the MAA polymer. Breaking load of the fibers was almost unchanged by the MAA treatment, while rigidity was markedly increased. Young's modulus of the MAA-treated tussah silk fibers decreased with decreasing volume fractions of the fiber in the MAA-treated tussah silk fibers. Young's modulus of the MAA polymer in the MAA-treated tussah silk fibers was estimated by extrapolating the relation between Young's moduli and the volume fractions of the fiber to zero volume fraction. Young's modulus of the MAA polymer in the MAA-treated tussah silk fibers was significantly larger than the modulus of a MAA polymer plate. © 1997 John Wiley & Sons, Inc. J Appl Polym Sci 65: 2051–2057, 1997     

Chemical modification of nylon 6 and polyester fabrics by ozone‐gas treatment

In a previous article, we reported on the ozone‐gas treatment of wool and silk fabrics in relation to the gas‐phase processing of textile fabrics. The treatment incorporated an oxygen element into the fiber surface and contributed to an increase in water penetration into the fabric. In this study, nylon 6 and polyester fabrics were treated with ozone gas in the same way as that of the wool and silk fabrics. The treatment incorporated much more oxygen into the fiber surface in the form of ? COH and ? COOH, as shown by electron spectroscopy for chemical analysis. Water penetration increased considerably with treatment, and the apparent dyeing rate and equilibrium dye uptake were also improved, especially for the polyester fabric, despite an increase in the crystallinity. Therefore, it seemed that the treatment brought about a change not only in the fiber surface but also in the internal structure of the fibers (the crystalline and amorphous regions) with regard to the dyeing behavior. Further, the mechanical characteristics of the ozone‐gas‐treated polyester and nylon 6 fabrics were measured with a Kawabata evaluation system apparatus. The shearing modulus and hysteresis widths increased with treatment, especially for the polyester fabric. Therefore, it was clear that the treatment caused a change in the fabric hand to crisp. © 2006 Wiley Periodicals, Inc. J Appl Polym Sci 100: 1344–1348, 2006     

Discrete element method models of elastic and elastoplastic fiber assemblies

Geometry-dependency and plasticity are considered in the contact force models for the discrete element method simulations of elastic and elastoplastic fiber assemblies subject to uniaxial compression. It is observed that the contact force models have a significant impact on compressive loads. A simplified normal contact force model leads to smaller loads at large solid volume fractions compared to the experimental results, while the present geometry-dependent models give better predictions. Simulations with a simple Coulombic tangential contact force model (considering sliding friction only) significantly underestimate the loads, while a Mindlin tangential force model that considers static friction improves the predictions. For the modeling of the fibers that undergo large plastic deformations, plasticity should be considered for both the fiber bending and fiber–fiber normal contact in order to obtain correct simulation results. Elastic models for fiber–fiber contact and fiber bending deformation remarkably overpredict the loads for the plastic fibers.     

芳纶的压缩弯曲性能对比分析

对5种芳纶试样进行单纤维压缩弯曲性能测试,得到了芳纶的压缩弯曲性能表征参数,包括最大力、抗弯刚度、等效弯曲模量等,并根据这些参数绘制出曲线图进行对比分析。结果表明:间位芳纶压缩弯曲曲线较对位芳纶平缓,而对位芳纶所受的载荷在达到最大力值后,随位移的增加逐渐降低。     

Uniaxial tensile properties of TiO2 coated single wool fibers by sol‐gel method: The effect of heat treatment

Single wool fibers were coated with TiO₂ by using the sol‐gel method. The uniaxial tensile properties of TiO₂ coated single wool fibers heated at different temperatures from 25 to 200°C were investigated and compared with those of uncoated single wool fibers. It was observed that the shape of the stress–strain curve of TiO₂ coated wool fibers became the same as uncoated wool fibers and showed a similar tendency of change to uncoated wool fibers with increasing temperature. But, the TiO₂ coated wool fibers obtained higher rigidity than uncoated wool fibers and up to their rupture points; they obtained higher stress levels in three deformation regions in the stress–strain curves, which indicates stronger wool fibers. Although the breaking extension of TiO₂ coated wool fibers decreased little by about 8%, the Young's modulus of TiO₂ coated wool fibers increased significantly by 19%, which was caused mostly by an increment in the stiffness of the cuticle layer of the wool fiber, and remained relatively higher than that of uncoated wool fibers after heat treatments. Structural changes in both uncoated and TiO₂ coated single wool fibers due to thermal effect, which caused the changes in the uniaxial tensile properties and the thermal behaviors of these fibers were discussed by using spectroscopic and thermal analysis methods in detail. © 2013 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 130: 898‐907, 2013     

Preparation of metal‐containing protein fibers and their antimicrobial properties

Bombyx mori silk, Antheraea pernyi silk, and wool fibers were chemically modified by treatment with tannic acid (TA) or by acylation with ethylenediaminetetraacetic (EDTA) dianhydride. Kinetics of TA loading or acylation with EDTA‐dianhydride varied from fiber to fiber. B. mori silk and wool displayed the highest weight gains with TA and EDTA‐dianhydride, respectively. The uptake of different metal ions (Ag⁺, Cu²⁺, Co²⁺) by protein fibers, either untreated or chemically modified, was studied as a function of weight gain and pH of the aqueous metal solution. Below pH 7, absorption of metal ions by untreated and TA‐treated fibers was negligible. Acylation with EDTA‐dianhydride enabled protein fibers to absorb and bind significant amounts of metal ions in the acidic and neutral pH range. The levels of metal desorption at acidic pH depended on the fiber‐metal combination. Untreated protein fibers usually displayed the lowest stability of the metal complex. Metal complexes with protein fibers exhibited prominent antimicrobial activity against the plant pathogen Cornebacterium. © 2003 Wiley Periodicals, Inc. J Appl Polym Sci 89: 638–644, 2003     

Structure of silk fibroin fibers made by an electrospinning process from a silk fibroin aqueous solution

In this article, the electrospun silk fibroin (SF) fibers with an average diameter of 700 nm were prepared from a concentrated aqueous solution with an electrospinning technique. The morphology, conformation, and crystalline structure of the SF fibers were characterized by scanning electron microscopy, Raman spectroscopy, and wide‐angle X‐ray diffraction, respectively. The structure and morphology of the fibers were strongly influenced by the solution concentration and the processing voltage. In addition, the fiber formation parameters, including spinning velocity, elongation rate, and draw ratio, were also calculated. A kind of SF fiber with a structure between an amorphous film and a natural silk was found. We suggest that the high draw ratio was not the only factor in the transformation of SF from random‐coil and α‐helix conformations to a β‐sheet conformation. © 2006 Wiley Periodicals, Inc. J Appl Polym Sci 101: 961–968, 2006     

Analysis of the structural characteristics of nanoscale silk particles

Nanoscale silk particles were prepared from silk fibers by a special pretreatment with the aid of specially designed machinery and techniques. Scanning electron micrographs showed that the particle sizes of the silk powders produced from silk fibers around 9–11 μm in diameter decreased from a microscale to a nanoscale after three stages of pulverization, and this was further confirmed with a laser particle size analyzer. Fourier transmission infrared analysis showed that there were no substantial changes in the chemical structure of the silk after the pulverization processes. The silk powders after the second and third pulverizations slightly differed from that of the silk fiber and the particles after the first pulverization with a greater amount of the primary aliphatic amines. Also, there were secondary amides present in the silk fiber and the powders after the first and second pulverizations but absent in the powders after the third pulverization. Moreover, the silk powders after the third pulverization had a greater number of C(CH₃)₃ groups than the silk fibers and the powders after the first and second pulverizations. X‐ray diffraction analysis showed that the crystallinity of the silk powders decreased when the particle sizes decreased, particularly to nanoscales. © 2006 Wiley Periodicals, Inc. J Appl Polym Sci 100: 268–274, 2006     

Tribological analysis of glass fibers using atomic force microscopy (AFM)/lateral force microscopy (LFM)

By using atomic force microscopy (AFM)/lateral force microscopy (LFM), a comparative study of the topography as well as the tribological properties (at a micrometer scale) of sized E‐glass fibers was done. Normal and lateral deflection signals are recorded when an AFM tip scans a fiber surface. Friction force data were obtained from the forward and backward scans of lateral force images whose contrasts reveal differences in friction coefficient values and, hence, surface chemical heterogeneity of certain‐sized glass fibers. Sizes having an epoxy film former lead to a higher friction coefficient value than those containing a starch film former. Moreover, the epoxy‐containing size is more readily plowed by the AFM tip. Annealing of this size lowers its friction coefficient. © 2000 John Wiley & Sons, Inc. J Appl Polym Sci 75: 1013–1025, 2000     

Tensile stress–strain and recovery behavior of Indian silk fibers and their structural dependence

The tensile stress–strain and recovery behavior of all the four commercial varieties of Indian silk fibers, namely Mulberry, Tasar, Eri, and Muga, have been studied along with their structures. Compared to the non‐Mulberry silk fibers, Mulberry silk fiber is much finer and has crystallites of smaller size, higher molecular orientation, and a more compact overall packing of molecules. These structural differences have been shown to result in (1) the presence of a distinct yield and a yield plateau in non‐Mulberry silk and their absence in Mulberry silk, and (2) relatively higher initial modulus and tenacity along with lower elongation‐to‐break and toughness and superior elstic recovery behavior of mulberry silk compared to non‐Mulberry silk. It is also observed that fine silk fibers have a relatively more ordered and compact structure with higher orientation compared to their coarse counterparts, and this gives rise to higher initial modulus and higher strength in the finer fibers. © 2000 John Wiley & Sons, Inc. J Appl Polym Sci 77: 2418–2429, 2000     

Computational and Experimental Studies of Flexible Fiber Flows in a Normal-Stress-Fixed Shear Cell

Flow properties of flexible fibers are poorly understood compared to those of rigid particles. In this study, a Schulze ring shear tester is used to measure the flow properties of fibers made of cut fishing wire and cut rubber cord, which have different levels of flexibility. For a comprehensive study, the discrete element method is employed to simulate flexible fiber flows. The simulations are validated by comparing with the experimental measurements. Studies show that an increase in fiber bending modulus leads to a reduction in the deformation and solid volume fraction, but it has no effect on the shear stress with the same normal stress. An increase in fiber-fiber friction coefficient, below a critical value of 0.8, can augment the angle of internal friction. The contact stiffness, contact damping coefficient, and bond damping coefficient only have limited impact on the shear flow behavior in the ranges considered. © 2018 American Institute of Chemical Engineers AIChE J, 65: 64–74, 2019     

Effect of silk fiber to the mechanical and thermal properties of its biodegradable composites

In recent years, natural fiber‐reinforced biodegradable thermoplastics are being recognized as an emerging new environmentally friendly material for industrial, commercial, and biomedical applications. Among different types of natural fibers, silk fiber is a common type of animal‐based fiber, has been used for biomedical engineering and surgical operation applications for many years because of its biocompatible and bioresorbable properties. On the basis of our previous study, a novel biodegradable biocomposite for biomedical applications was developed by mixing chopped silk fiber and polylactic acid (PLA) through the injection molding process. This article is aimed at studying the dynamic mechanical and thermal properties of the composite in relation to its biodegradation effect. At the beginning, it was found that the initial storage modulus of a silk fiber/PLA composite increased while its glass transition temperature decreased as compared with a pristine PLA sample. Besides, the coefficient of linear thermal expansions (CLTE) of the composite was reduced by 28%. This phenomenon was attributed to the fiber–matrix interaction that restricted the mobility of polymer chains adhered to the fiber surface, and consequently reduced the T_g and CLTE. It was found that the degraded composite exhibited lower initial storage modulus, loss modulus and tan delta (tan δ) but the T_g was higher than the silk fiber/PLA composite. This result was mainly due to the increase of crystallinity of the composite during its degradation process. © 2012 Wiley Periodicals, Inc. J. Appl. Polym. Sci., 2013     

The preparation of poly[N(n-butoxymethyl) methacrylamide] grafted silk fibers by polymerization using a low pH system

The graft polymerizations of the N(n-butoxymethyl) methacrylamide (BMA) monomer onto silk fibers were effected after reducing the pH of the grafting system to 2.5 by the addition of a formic acid solution. We compared the grafting efficiencies, surface characteristics, and thermal behaviors, as well as the whiteness levels and the extent of reduction of the rate of yellowing following UV irradiation, with the equivalent features of poly(BMA)-grafted silk fibers, prepared under normal (pH 6) conditions. The grafting efficiency [as poly(BMA) weight gain] onto silk fiber that was attained was almost 100% through optimization of the pH environment in the polymerization system by the addition of formic acid. The stiffness of the silk fabrics observed, following the conventional grafting, was markedly higher than that of equivalent silks after the polymerization at pH 2.5. The rates of yellowness index increase, for these latter silk fabrics following UV irradiation were also reduced, specifically in the initial irradiation period (up to 60 h). The SEM of the grafted silk fabrics reveal the absence of granules on the surface of the grafted silk fiber, when the silk was grafted with poly(BMA), after reducing the pH of the grafting system to 2.5. These findings suggest that the BMA monomer was polymerized specifically within the silk fiber and not on the surface. It is suggested that the increase in the polymer weight gain, and the reduced adverse effect on the fabric handle, arise because of the modified polymer location. © 1993 John Wiley & Sons, Inc.     

Investigation of Synthetic Spider Silk Crystallinity and Alignment via Electrothermal,Pyroelectric, Literature XRD,and Tensile Techniques

The processes used to create synthetic spider silk greatly affect the properties of the produced fibers. This paper investigates the effect of process variations during artificial spinning on the thermal and mechanical properties of the produced silk. Property values are also compared to the ones of the natural dragline silk of the Nephila clavipes spider, and to unprocessed (as‐spun) synthetic silk. Structural characterization by scanning pyroelectric microscopy is employed to provide insight into the axial orientation of the crystalline regions of the fiber and is supported by X‐ray diffraction data. The results show that stretching and passage through liquid baths induce crystal formation and axial alignment in synthetic fibers, but with different structural organization than natural silks. Furthermore, an increase in thermal diffusivity and elastic modulus is observed with decreasing fiber diameter, trending toward properties of natural fiber. This effect seems to be related to silk fibers being subjected to a radial gradient during production.

     

Evaluation of some of the properties of plasma treated wool fabric

Low temperature plasma (LTP) treatment was applied to wool fabric with the use of a nonpolymerizing gas, namely oxygen. Properties of the LTP‐treated samples including low stress mechanical behavior, air permeability, and thermal characteristics were evaluated in this study. Kawabata evaluation system fabric (KES‐F) was employed to determine the tensile, shearing, bending, and compression strength properties and surface roughness of the specimens. The changes in these properties are believed to be closely related to the interfiber and interyarn frictional force induced by the LTP. The decrease in the air permeability of the LTP‐treated wool fabric was found to be probably because of the plasma action effect on increasing the fabric thickness and a change in fabric surface morphology, which was confirmed by scanning electron microscopy micrographs. The change in the thermal properties of the LTP‐treated wool fabric was in good agreement with the earlier findings and can be attributed to the amount of air trapped between the yarns and fibers. This study suggested that the LTP treatment can influence the final properties of the wool fabric, and also provide information for developing LTP‐treated wool fabric for industrial use. © 2006 Wiley Periodicals, Inc. J Appl Polym Sci 102: 5958–5964, 2006     

Acylation of silk and wool with acid anhydrides and preparation of water-repellent fibers

Silk and wool fibers were acylated with two acid anhydrides, dodecenylsuccinic anhydride (DDSA) and octadecenylsuccinic anhydride (ODSA), at 75°C with N,N-dimethylformamide (DMF) or dimethyl sulfoxide (DMSO) as the solvent, the latter of which allowed higher weight gains to be reached. The weight gain and acyl content of wool was always higher than that of silk. Tensile properties of silk remained unchanged regardless of weight gain, whereas wool displayed a noticeably higher extensibility at high weight gain. Fine structural changes of acylated wool were detected by DSC analysis. Moisture regain and water retention of acylated silk and wool decreased significantly, whereas water repellency increased. SEM analysis showed the presence of foreign material firmly adherent to the surface of both silk and wool, whose amount increased with increasing weight gain. These deposits were attributed to the presence of the modifying agents at the fiber surface on the basis of the characteristic IR bands. The possible application of silk and wool fibers acylated with DDSA or ODSA for the preparation of water-repellent textile materials is discussed. © 2001 John Wiley & Sons, Inc. J Appl Polym Sci 82: 2832–2841, 2001     

不同应变率下聚甲醛纤维机场道面混凝土弯曲性能研究

机场道面混凝土结构在不同性质荷载作用下的力学行为受应变率的影响较大。为研究应变率对聚甲醛纤维机场道面混凝土(PFAPC)弯曲性能的影响,通过四点弯曲试验,分析不同应变率(10^-5~10^-1 s^-1)下PFAPC抗弯挠度、弯曲模量、弯曲强度及韧性指数的变化规律,并观察断口纤维的微观形貌,总结不同应变率下的纤维失效模式。结果表明:PFAPC的弯曲峰值强度、极限抗弯挠度及弯曲模量随应变率的增加呈上升趋势;与峰值强度相比,应变率对PFAPC残余强度影响较小,但随应变率增大总体呈上升趋势;与极限抗弯挠度相比,峰值挠度随应变率的增加波动上升;聚甲醛纤维在各应变率作用下主要为拔出破坏模式;PFAPC在车辆及飞机冲击作用下能吸收较大能量,呈现出一定的延性破坏特征,具有良好的弯曲韧性。     

Preparation and characterization of Bombyx mori silk fibroin and wool keratin

Silk and wool are well‐known protein‐based fibers. Their environmental stability, biocompatibility, and unique mechanical properties provide an important basis for using these natural proteins in biomedical applications. To use them as biomaterials in the form of fibers, films, or membranes, it is necessary to characterize these proteins in their solution and solid states because structural characteristics and morphological features have a great influence on the physical and mechanical properties of these new regenerated protein forms. Therefore, in the present study, silk fibroin and wool keratin were dissolved and their solution behaviors and secondary structures are analyzed and compared, using particle size distribution, molecular weight distribution (SDS‐PAGE), Fourier transform infrared, and X‐ray diffraction techniques. It was shown that keratin is more stable in solution and more amorphous in the solid state. © 2006 Wiley Periodicals, Inc. J Appl Polym Sci 100:4260–4264, 2006     

凝固条件对纤维素/丝素蛋白纤维相形态及性能的影响

蛋白质纤维具有光滑柔顺、透气吸湿等优点,然而天然蛋白纤维产量有限。再生蛋白纤维的制备通常采用与其它成纤高分子接枝或共混的方法,有利于提高再生蛋白纤维的断裂强度。选用同为天然高分子的纤维素为基体,以共溶剂溶解纤维素与蛋白质,进而纺丝成形制得力学性能满足要求的纤维素/丝素蛋白共混纤维。为了探究凝固剂组成对纤维素/丝素蛋白共混纤维相形态及性能的影响,选用水、乙醇、乙醇/1-丁基-3-甲基咪唑氯盐([BMIM]Cl)等作为凝固剂。研究发现:乙醇作为凝固剂时,纤维素与丝素蛋白能很好地同时凝固;而当在乙醇凝固浴中加入适量的[BMIM]Cl径向均匀分散。通过对凝固剂组成的调控能有效提升纤维的力学强度。