Name: microfluidic dry-spinning and characterization of regenerated silk fibroin fibers
Uploaded: 2017-09-04T14:00:00
Description: Watch this Scientific Journal Video about Microfluidic Dry-spinning and Characterization of Regenerated Silk Fibroin Fibers at JoVE.com

这项工作由中国国家自然科学基金 (21674018)、中国国家重点研究开发项目 (2016YFA0201702/2016YFA0201700) 和上海教育发展支持的 "曙光计划" 赞助。基金会和上海市教育委员会 (15SG30), 东华大学杰出青年教授项目 (A201302), 为中央大学的基础研究基金, 和111项目 (no. 111-2-04)。

警告: 请在使用前查阅所有相关的材料安全数据表。用于制备成型的几种化学药剂具有剧毒。请使用个人防护用品 (安全眼镜, 手套, 实验室大衣, 全长长裤, 和脚趾鞋). 
 1. 微流体纺丝 RSF 水溶液 <ol> <li> RSF 水纺涂料的制备 4 , 15 , 16 <ol> <li> 蚕茧脱胶 <ol> <li> 脱胶在 Na 2 CO 3 </...

<ol>
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E., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Tunable+silk:+using+microfluidics+to+fabricate+silk+fibers+with+controllable+properties.">Tunable silk: using microfluidics to fabricate silk fibers with controllable properties.</a> Biomacromolecules. 12 (5), 1504-1511 (2011).</li><li>Luo, J., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Tough+silk+fibers+prepared+in+air+using+a+biomimetic+microfluidic+chip.">Tough silk fibers prepared in air using a biomimetic microfluidic chip.</a> Int J Biol Macromol. 66, 319-324 (2014).</li><li>Peng, Q. F., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Recombinant+spider+silk+from+aqueous+solutions+via+a+bio-inspired+microfluidic+chip.">Recombinant spider silk from aqueous solutions via a bio-inspired microfluidic chip.</a> Sci Rep. 6, (2016).</li><li>Peng, Q. F., Shao, H. L., Hu, X. C., Zhang, Y. P. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Role+of+humidity+on+the+structures+and+properties+of+regenerated+silk+fibers.">Role of humidity on the structures and properties of regenerated silk fibers.</a> Prog Nat Sci-Matter. 25 (5), 430-436 (2015).</li><li>Sampath, S., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=X-ray+diffraction+study+of+nanocrystalline+and+amorphous+structure+within+major+and+minor+ampullate+dragline+spider+silks.">X-ray diffraction study of nanocrystalline and amorphous structure within major and minor ampullate dragline spider silks.</a> Soft Matter. 8 (25), 6713-6722 (2012).</li><li>Martel, A., Burghammer, M., Davies, R. J., Riekel, C. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Thermal+Behavior+of+Bombyx+mori+silk:+Evolution+of+crystalline+parameters,+molecular+structure,+and+mechanical+properties.">Thermal Behavior of Bombyx mori silk: Evolution of crystalline parameters, molecular structure, and mechanical properties.</a> Biomacromolecules. 8 (11), 3548-3556 (2007).</li><li>Pan, H., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Nanoconfined+crystallites+toughen+artificial+silk.">Nanoconfined crystallites toughen artificial silk.</a> J Matter Chem B. 2 (10), 1408-1414 (2014).</li><li>Zhang, C., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Microstructural+evolution+of+regenerated+silk+fibroin/graphene+oxide+hybrid+fibers+under+tensile+deformation.">Microstructural evolution of regenerated silk fibroin/graphene oxide hybrid fibers under tensile deformation.</a> Rsc Adv. 7 (6), 3108-3116 (2017).</li><li>Wei, W., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Bio-inspired+capillary+dry+spinning+of+regenerated+silk+fibroin+aqueous+solution.">Bio-inspired capillary dry spinning of regenerated silk fibroin aqueous solution.</a> Mat Sci Eng C-Mater. 31 (7), 1602-1608 (2011).</li><li>Jin, Y., Zhang, Y. P., Hang, Y. C., Shao, H. L., Hu, X. C. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=A+simple+process+for+dry+spinning+of+regenerated+silk+fibroin+aqueous+solution.">A simple process for dry spinning of regenerated silk fibroin aqueous solution.</a> J Mater Res. 28 (20), 2897-2902 (2013).</li><li>Jin, Y., Hang, Y. C., Zhang, Y. P., Shao, H. L., Hu, X. C. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Role+of+Ca2++on+structures+and+properties+of+regenerated+silk+fibroin+aqueous+solutions+and+fibres.">Role of Ca2+ on structures and properties of regenerated silk fibroin aqueous solutions and fibres.</a> Mater Res Innov. 18, 113-116 (2014).</li><li>Koh, L. D., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Structures,+mechanical+properties+and+applications+of+silk+fibroin+materials.">Structures, mechanical properties and applications of silk fibroin materials.</a> Prog Polym Sci. 46, 86-110 (2015).</li><li>McDonald, J. C., Whitesides, G. M. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Poly(dimethylsiloxane)+as+a+material+for+fabricating+microfluidic+devices.">Poly(dimethylsiloxane) as a material for fabricating microfluidic devices.</a> Accounts Chem Res. 35 (7), 491-499 (2002).</li><li>Knight, D. P., Vollrath, F. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Liquid+crystals+and+flow+elongation+in+a+spider's+silk+production+line.">Liquid crystals and flow elongation in a spider's silk production line.</a> P Roy Soc B-Biol Sci. 266 (1418), 519-523 (1999).</li></ol>

在 RSF 溶液的透析过程中, pH 值对以下浓度过程至关重要。如果去离子水的 pH 值小于 6, RSF 溶液在浓缩过程中会更容易凝胶。为了避免凝胶, CaCl2被添加到 RSF 解决方案中。CaCl2的浓度是每重量 RSF 的1摩尔。
我们以前的工作证明了微流控 RSF 水溶液干纺的可能性8。微流控通道的几何形状是一个简化的单级指数函数。对于蜘蛛和蚕, 纺纱兴奋剂是?...

在环境温度和压力下, 蜘蛛和蚕可以从水蛋白溶液中生产出优异的蚕丝纤维。剪切和伸展流动可诱导丝腺中的液晶纹理的形成1。近年来, 为了生产高强度的人造纤维, 模拟蜘蛛的纺丝工艺有着很大的兴趣。然而, 大量的蜘蛛丝蛋白不能生产效率和经济的养殖蜘蛛由于食人。大量的蚕丝绸可以通过耕作容易获得。否则, 蚕和蜘蛛有类似的纺纱工艺和氨基酸组成。因此, 蚕丝丝素被许多研究者选为人工动物丝的替代品。
蜘蛛和蚕通过他们的旋转导管挤出蛋白质溶液到空气中的纤维。沿着纺丝管道产生的高应力力很可能将丝素分子拉伸到更长的构象2。采用传统的湿纺和干纺工艺纺制了人造蚕丝纤维,3,4, 不考虑纺丝管产生的流体力。
首先, 采用微流控方法对蚕丝蛋白的组装进行了研究5,6。然后, 通过对剪切和伸展力的建模, 研究了 RSF 的微流体制备7,8。RSF 纤维的杨氏模量和直径可通过微流控湿纺纱进行调谐, 但拉伸纤维的抗拉强度小于100兆帕斯卡7。最后, 用微流控干纺法成功地制备了高强度 RSF 纤维, 但其直径仅2µm8。近年来, 微流控湿纺在高强度重组蜘蛛丝纤维生产中得到了成功的应用。空气中的 post-spinning 图改善了人造纤维的表面和内部缺陷9。
本文介绍了改进的微流控纺丝工艺在 RSF 光纤中的应用。它的目的是模仿蚕丝的纺纱过程, 包括纺纱涂料, 剪切力, 和干纺工艺。这种纺纱方法不仅可以生产高强度的人造蚕丝纤维, 而且可以调节纤维的直径。首先, 在具有二阶指数衰减的仿生通道中, RSF 纺涂料被剪切和拉长。其次, 研究了微流控干法纺丝过程中相对湿度 (RH) 对纤维形貌和性能的影响10。与传统的纺丝喷相比, 我们的微流控系统具有高度的仿生性, 可以用干湿纺法在室温下从溶液中产生高强度纤维。
由于同步辐射微 X 射线的高分辨率、亮度和高能性, 可以用来表征单个纤维的显微结构, 其直径为数微米4,11,12,13,14. 用 SR WAXD 技术计算了 RSF 纤维的结晶度、晶粒尺寸和晶体取向。

<table>
	<tbody>
		<tr>
			<td>B. mori Cocoons</td>
			<td>Farmer in Tongxiang, Zhejiang Province, China</td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>Sodium carbonate, anhydrous, 99.8%</td>
			<td>Shanghai Lingfeng Chemical Reagent Co., Ltd., China</td>
			<td></td>
			<td>Analytically Pure</td>
		</tr>
		<tr>
			<td>Lithium bromide, 99.1%</td>
			<td>Shanghai China Lithium Industrial Co., Ltd., China</td>
			<td></td>
			<td>Analytically Pure</td>
		</tr>
		<tr>
			<td>Calcium chloride, anhydrous, 96.0%</td>
			<td>Shanghai Lingfeng Chemical Reagent Co., Ltd., China</td>
			<td></td>
			<td>Analytically Pure</td>
		</tr>
		<tr>
			<td>Ethanol, anhydrous, 99.7%</td>
			<td>Sinopharm Group Chemical Reagent Co.,Ltd., China</td>
			<td>10009218</td>
			<td>Analytically Pure</td>
		</tr>
		<tr>
			<td>SU-8 photoresist</td>
			<td>MicroChem Corp., USA</td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>Developing solution</td>
			<td>MicroChem Corp., USA</td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>Sylgard 184</td>
			<td>Dow Corning, USA</td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>Isopropanol</td>
			<td>Shanghai Lingfeng Chemical Reagent Co., Ltd., China</td>
			<td></td>
			<td>Analytically Pure</td>
		</tr>
		<tr>
			<td>Concentrated sulfuric acid</td>
			<td>Pinghu Chemical Reagent Factory, China</td>
			<td></td>
			<td>Analytically Pure</td>
		</tr>
		<tr>
			<td>30 vol% hydrogen peroxide</td>
			<td>Shanghai Jinlu Chemical reagent Co., Ltd., China</td>
			<td></td>
			<td>Analytically Pure</td>
		</tr>
		<tr>
			<td>Acetone</td>
			<td>Shanghai Zhengxing Chemical Reagent Factory, China</td>
			<td></td>
			<td>Analytically Pure</td>
		</tr>
		<tr>
			<td>Oxygen plasma treatment</td>
			<td>DT-01, Suzhou Omega Machinery Electronic Technology Co., Ltd., China</td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>Syringe pump</td>
			<td>&#160;KD Scientific, USA</td>
			<td></td>
			<td>KDS 200P</td>
		</tr>
		<tr>
			<td>Humidifier</td>
			<td>SEN electric</td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>Driller</td>
			<td>Hangzhou Bo Yang Machinery Co., Ltd., China</td>
			<td></td>
			<td>bench drilling machine Z406c</td>
		</tr>
		<tr>
			<td>Material testing system</td>
			<td>Instron, USA</td>
			<td></td>
			<td>Model: 5565</td>
		</tr>
		<tr>
			<td>PeakFit</td>
			<td>Systat Software, Inc., USA</td>
			<td></td>
			<td>Version 4.12</td>
		</tr>
	</tbody>
</table>

microfluidic dry-spinning and characterization of regenerated silk fibroin fibers

该协议展示了一种仿蚕纺纱过程的方法。在本机纺纱过程中, 收缩纺丝管使蚕丝蛋白具有紧凑和有序的剪切和伸长力。在此, 设计了一种仿生微流控通道, 模拟了蚕纺管的特定几何形状。以高浓度掺杂的再生蚕丝丝素 (RSF) 为原料, 在室温和压力下通过微通道向干纺纤维挤出。在 post-treated 过程中, 在乙醇水溶液中提取和贮存成纱纤维。采用同步辐射 wide-angle x 射线衍射 (SR WAXD) 技术对单 RSF 纤维的显微组织进行了研究, 并将其固定在与 X 射线微的 RSF 纤维轴垂直的试样持有者身上。从 WAXD 数据计算了纤维的结晶度、晶粒尺寸和晶体取向。two-dimensional WAXD 模式赤道附近的衍射弧表明, post-treated RSF 纤维具有很高的取向度。

采用微流控纺丝方法成功地制备了高强度 RSF 纤维。在图 2中显示了拉伸 RSF 光纤 C44R40 的应力-应变曲线和 SEM 图像。在拉伸试验中测量了至少10纤维。根据纤维断裂应力和应变的平均值选择应力应变曲线。光纤的 WAXD 数据显示在图 3中。根据 WAXD 数据计算了结晶度和结晶取向。对于样品的指定, 我们用 C 和 R 分别介绍了纺丝涂料?...

Watch this Scientific Journal Video about Microfluidic Dry-spinning and Characterization of Regenerated Silk Fibroin Fibers at JoVE.com

Microfluidic Dry-spinning and Characterization of Regenerated Silk Fibroin Fibers

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