• International Journal of Industrial Entomology and Biomaterials
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• 제21권1호
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• pp.145-150
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• 2010

The regenerated silk fibroin with various molecular weights (MW) was prepared by different dissolution condition and the effect of coagulant on the wet spinnability of the various MW silk fibroin solutions dissolved in formic acid was investigated by the observation of wet spun filament in coagulant and the measurement of maximum draw ratio. The observation on the wet spun filament in coagulation bath revealed that good fibers without bead were formed in a high MW and a very high MW silk fibroin samples. In contrast, beads were observed in the silk fibroin sample with medium MW. The maximum draw ratio of wet spun silk fibroin filament decreased with MW reduction. The decrease of maximum draw ratio in isopropanol, acetone, DMF and THF was remarkably higher than that in methanol and ethanol, indicating that the coagulant type strongly influenced the wet spinnability. The two simple evaluation methods used in this study showed complementary information for wet spinnability: (a) The observation of filament in coagulant was effective to check a continuous fiber formation and a bead formation, and (b) the maximum draw ratio measurement was useful to examine the post drawing ability related to molecular orientation.

• International Journal of Industrial Entomology and Biomaterials
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• 제45권2호
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• pp.70-77
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• 2022

Wet-spun regenerated silk fibroin (RSF) fibers have been extensively studied owing to their 1) useful properties as biomaterials, including good blood compatibility and cyto-compatibility; 2) the various methods available to control the structural characteristics and morphology of the fiber, and 3) the possibility of fabricating blended fibers and new material-embedded fibers. In this study, silk nanofibrils prepared using a new method were embedded in RSF to fabricate wet-spun silk nanofibril/RSF composite fibers. Up to 2% addition of silk nanofibril, the silk nanofibril/RSF dope solution showed slight shear thinning, and the G' and G" of the dope solution were similar. However, above 3% silk nanofibril content, the viscosity of the dope solution significantly increased. In addition, shear thinning was remarkably evident, and the G' of the dope solution was much higher than the G", indicating a very elastic state. As the silk nanofibril content was increased, the wet-spun silk nanofibril/RSF composite fiber became uneven, with a rough surface, and more beaded fibers were produced. Scanning electron microscopy observations revealed that the beaded fibers were attributed to the inhomogeneous dispersion and presence of agglomerates of the silk nanofibrils. As the silk nanofibril content and RSF concentration increased, the maximum draw ratio decreased, indicating the deterioration of the wet spinnability and post-drawing performance of silk nanofibril/RSF.

• International Journal of Industrial Entomology and Biomaterials
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• 제30권2호
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• pp.75-80
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• 2015

The wet spinning of silk solution has attracted researchers' attention because of 1) unique properties of silk as a biomedical material and 2) easy control of the structure and properties of the regenerated silk fiber. Recently, studies have reported that different silkworm varieties produce silk with differences in the molecular weight (MW) and other mechanical properties of the regenerated silk fibroin (SF) film. In this study, we look at the effect of different Bombyx mori varieties on the wet spinning of SF. Although five regenerated SFs from different silkworm varieties have different MWs and solution viscosity, the wet spinnability and post drawing performance of regenerated SFs were not different. This result is due to low variability in the MW of the regenerated SF samples from the different silkworm varieties. In addition, unlike regenerated SF films, the mechanical properties of wet spun regenerated SF filament were not affected by silkworm variety. This result suggests that the mechanical properties of wet spun SF filament are less affected by MW than those of SF film are.

• International Journal of Industrial Entomology and Biomaterials
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• 제19권1호
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• pp.181-185
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• 2009

In this paper, the regenerated silk fibroin (SF)/hydroxypropyl methylcellulose (HPMC) blend filaments were prepared by wet spinning and the effect of HPMC concentration on the post drawing and morphology of blend filaments was elucidated. The result of maximum draw ratio indicated that the wet spinnability of wet spun SF / HPMC was improved with increasing HPMC concentration until 8% and remained constant after that concentration. The SEM observation revealed that the enhanced wet spinnability of blend filaments was strongly related to the morphological change by increasing HPMC concentration. Regardless of HPMC concentration, as SF content was reduced, the wet spinnability of blend film decreased resulting in reduced maximum draw ratio. It was also found by SEM observation that the cross section of blend filament deviated from circularity with an increase of HPMC content.

• 한국염색가공학회지
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• 제33권3호
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• pp.131-140
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• 2021

Collagen and chitosan are used in medical and cosmetic materials as natural polymers. In order to utilize the advantages of the materials, collagen/chitosan conjugated wet-spun fibers were prepared. The analysis of surface, optical, thermal and mechanical properties was carried out on the various composition of collagen and chitosan. As a result of images analysis, it was verified that the collagen/chitosan conjugated fibers were stably spun. In addition, the optical and thermal properties of fibers were observed to be changed by hydrogen bond. As a result, an optimized composition could be found at an appropriate content. Moreover, the optimized fibers have mechanical properties similar to chitosan fibers, while improving the structural and thermal stability by its hydrogen bond. In addition, the wet-spun collagen/chitosan conjugated fibers can be applied to medical and various fields through mechanical properties according to content control.

• Composites Research
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• 제26권2호
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• pp.123-128
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• 2013

PVDF(polyvinylidene fluoride) 섬유는 습식방사방법을 적용하여 제조하였다. PVDF 분자 내 압전 특성과 밀접한 관련을 갖는 ${\beta}$형태의 결정 함량을 높이기 위하여, 본 연구에서는 습식방사 된 섬유에 1단계 연신, 2단계 어닐링 공정으로 구성하여 후 처리를 도입하였다. 후 처리는 PVDF 고분자의 유리전이 온도($T_g$)와 용융온도($T_m$) 사이의 온도범위에서 진행하여, 최대의 ${\beta}$형태 결정을 생성 할 수 있는 열처리 조건을 최적화 하였다. 제조된 PVDF 섬유 내 분자 배향 특성과 결정 구조를 확인하기 위하여 적외선 분광 광도계(FT-IR)와 X선 회절 분석기(XRD)를 이용하여 분석하였으며, 전자현미경(SEM)을 통하여 섬유의 표면을 관찰하여 섬유의 평균직경을 확인하였다. 분석 결과, 후 처리 공정이 PVDF 결정 구조의 영향을 미치며, ${\beta}$형태의 결정 비율을 증가시킨다는 것을 확인하였다. 더불어 ${\beta}$형태 결정 향상으로 인해 기계적 강도가 증가되었으며, 압전 특성 향상까지 기대할 수 있었다.

• International Journal of Industrial Entomology and Biomaterials
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• 제26권2호
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• pp.81-88
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• 2013

Wet-spun silk fibers have attracted the attention of many researchers because of 1) the unique properties of silk as a biomaterial, including good biocompatibility and cyto-compatability and 2) the various methods available to control the structure and properties of the fiber. Cellulose nanofibrils (CNFs) have typically been used as a reinforcing material for natural and synthetic polymers. In this study, CNF-embedded silk fibroin (SF) nanocomposite fibers were prepared for the first time. The effects of CNF content on the rheology of the dope solution and the characteristics of wet-spun CNF/SF composite fibers were also examined. A 5% SF formic acid solution that contained no CNFs showed nearly Newtonian fluid behavior, with slight shear thinning. However, after the addition of 1% CNFs, the viscosity of the dope solution increased significantly, and apparent shear thinning was observed. The maximum draw ratio of the CNF/SF composite fibers decreased as the CNF content increased. Interestingly, the crystallinity index for the silk in the CNF/SF fibers was sequentially reduced as the CNF content was increased. This phenomenon may be due to the fact that the CNFs prevent ${\beta}$-sheet crystallization of the SF by elimination of formic acid from the dope solution during the coagulation process. The CNF/SF composite fibers displayed a relatively smooth surface with stripes, at low magnification (${\times}500$). However, a rugged nanoscale surface was observed at high magnification (${\times}10,000$), and the surface roughness increased with the CNF content.

• Fibers and Polymers
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• 제1권2호
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• pp.92-96
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• 2000

A high molecular weight polyhydroxyamide (PHA) solution in N, N-dimethyl acetamide (DMAc) was prepared from 3, 3'-dihydroxybenzidine and isophthalic chloride (IPC), which was used for spinning PHA fiber. Before spinning, the diffusion property of DMAc into various coagulants was examined. The fiber was well formed in coagulants such as water/ethanol with a composition of 5/5, ethanol, and ethanol/isopropanol with a composition of 7/3 and 5/5. However, the PHA fiber spun in the water/ethanol mixture contained voids. After the fiber spun in ethanol was annealed at over $350^{\circ}C$, the ultimate stress and initial modulus of the fiber increased from 75.5 MPa and 3.22 GPa to 369 MPa and 29.5 GPa, respectively. These properties of the PHA fiber spun by the dry spinning method were also enhanced, attaining 154 MPa and 5.56 Gpa, respectivel.

• International Journal of Industrial Entomology and Biomaterials
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• 제16권2호
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• pp.61-66
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• 2008

In this paper, the regenerated silk fibroin (SF)/nylon 6 blend filaments were fabricated using wet spinning technique and the effect of coagulant on the post drawing and morphology of blend filaments was investigated. In the result of wet spinnability, methanol, acetone, DMF, and THF showed relatively good coagulation strength and fiber formation for the regenerated SF. On the contrary, they did not exhibit strong enough to produce a uniform nylon 6 filament due to the lack of coagulation strength. In the examination of post drawing performance, methanol showed the highest maximum draw ratio of the blend filament over all blend ratios. The maximum draw ratio of SF/nylon 6 blend filaments decreased with the reduction of SF content regardless of type of coagulant. SEM observation showed the consistent result with that of post-drawing performance. As SF content decreased, the uniform and regular structure was changed to irregular one. In particular, the severe macro-phase separation between SF and nylon 6 could be detected in the 50/50 SF/nylon 6 blend filaments coagulated in methanol and THF.

• 한국수산과학회지
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• 제9권4호
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• pp.293-298
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• 1976

관통형 그물감의 강도를 추정하기 위한 기초로서, 그물실의 강도가 관통마디에서 감소하는기구 및 주름을 주었을 때의 관통마디의 강도를 조사하고, 이들 강도를 매듭의 강도와 비교하였다. 실험에는 vinylidene(mono-f.), polyester(multi-f.) 및 nylon(multi-f.와 spun) 그물감이 사용되었으며, 관통마디의 시료는 이들 그물감을 계단하여 준비하였고, 또한 매듭은 이들 그물감의 다리로 만들어졌다. 실험 결과, 그물실의 강도가 관통마디에서 감소하는 원인은 마디에서의 편자사간의 마찰력으로 인해 마디의 첨단, 즉 마디와 다리와의 경계에 위치한 섬유들이 장력에 의해서 재분포하는데 마찰력만큼 저항을 받게 되고, 따라서 마찰력만큼 강도가 감소하는 것이라고 해석되었다. 그러나, 그 감소의 정도는 filament 그물실의 경우 $5\%$ 이내이고, spun 그물실의 경우는 $5\~10\%$ 정도여서, 마디의 감도는 근사적으로는 그물실의 강도로 표시해도 좋을 것 같았다. 주름을 주었을 애의 관통마디의 강도는 연접하는 두개의 다리가 이후는 각 $\varphi$가 $90^{\circ}$에서 최소치를 가지는 포물선상에서 변화하는 경향이었지만, 그 최소치는 강도의 감소가 가장 큰 습막의 spun 실에서 $\varphi$가 $0^{\circ}$때의 강도의 약 $94\%$이어서, filament 그물실의 관통마디의 강도는 $\varphi$의 변화에 관계없이 거의 일정하다고 간주해도 좋을 것으로 추찰되었다. 따라서, filament 그물실의 관통마디의 강도는 주름을 준 경우이거나 안준 경우거나를 불문하고, 그물실의 강도로 표시해도 좋을 것 같았다. 관통마디의 강도를 매듭의 강도와 비교한 결과, 매듭의 강도는 관통마디의 강도의 약 $70{\pm}5\%$로 나타났다.