この作品は中国の国家自然科学基金 (21674018)、キー研究と開発中国プログラム (2016YFA0201702/2016YFA0201700) と上海教育開発でサポートされている「曙光プログラム」主催財団と上海市教育委員会 (15SG30)、デュ区別若い教授プログラム (A201302)、中央大学と 111 プロジェクト (No.111-2-04) のための基礎的研究資金です。

警告: 使用前にすべての関連の製品安全データシートを参照してください。成形品の準備に使用される化学物質のいくつかは、急性毒性です。個人用保護具 (保護メガネ、手袋、白衣、フルの長さのズボン、閉じてつま先の靴) を使用してください。
 1 マイクロ RSF 回転水溶液 <ol><li>水溶液のドープを回転の RSF の準備 4 , 15 , 16。 <ol><li>Degumming カイコの 30 分ごとに、100 ° C で <ol><li>Degum Na 2 CO 3 水溶液 (水 0.5 wt %) で 2 回 カイコ が繭を繭し、削除する脱イオン水でシルクを洗う、セリシン</li>。
		</ol></li> <li>ガム繭の解消 <ol><li>乾燥空気でガム繭シルク; 1:10 (w/v) 40 ° C で 2 時間の比率は 9.0 M 臭化リチウム水溶液中でガム繭シルクを解散。たとえば、1 グラム絹 ( 図 1 a) あたり 10 mL 臭化リチウムを追加します</li>。
		</ol></li> <li>Centrifuging とフィルタ リング <ol><li>脱イオン水による 1.5 倍 RSF 溶液を希釈します。遠心分離機、不純物を除去するためのフィルター。1,234.8 x g に 10 分間遠心 4 ° C で 250 mL ボトルで RSF ソリューションは、20 μ m フィルターと真空ポンプを用いた RSF ソリューションをフィルター処理します。ダブル フィルター ペーパー ベッド実験効果を考慮したをお勧めします</li>。
		</ol></li> <li>Dialyzing <ol><li>セルロースの半透膜を利用した 3 日間の 5 ° C で脱イオン水で RSF ソリューションを Dialyze (MWCO: 14,000 ± 2,000)。国境なき記者団のソリューションの容量は約 1 L、4 透析バッグに読み込まれています。これらの透析袋をバケツに入れて、10 L の逆浸透 (RO) で満ちている脱イオン水 。
			注: 脱イオン水の pH 値は濃度プロセス中にゲル化を避けるためには、6 より高くなければなりません。脱イオン水の pH がこのプロトコルの調整を必要としない</li>。
		</ol></li> <li>集中 <ol><li>1.0 ミリ モル/g Ca 2 + 最終濃度; 国境なき記者団の解決策に 5 ° c. を追加 3 M CaCl 2 水溶液で強制換気によって 20 wt % 水溶液 RSF を凝縮し、強制空気で集中38 47 wt % へのフロー</li>。
			<li>スライド ガラスに一滴 RSF ソリューションの重量を量るし、105 のオーブンで 2 時間乾燥 ° C 
			注: 重量パーセント、残りの固体蛋白質および CaCl 2 の濃度は、乾燥する前にドロップの重量と比較して。国境なき記者団の濃度は、CaCl 2 の質量を控除後派生します。少なくとも 4 繰り返し測定を行った。以前, Ca 2 + 濃度は、レオロジー特性と国境なき記者団の水溶液の曳糸性に大きく影響します。一方、Ca 2 + 添加では、β シートの限定の形成と国境なき記者団 17 凝集を求めるメッセージが表示。ネイティブの回転ドープ CaCl 2 回転前にゲル化を避けるために麻薬を回転の貯蔵の間に重要な役割を果たすことと見なされます。 18</li></ol></li></ol></li> <li>マイクロ流体チップの準備 8 , 19 <ol><li>フォトマスクを準備する <ol><li>のマイクロ チャンネルを設計、CAD プログラム。 19 高解像度の透明性を生成する CAD ファイルを印刷します</li>。
		</ol></li> <li>金型の準備 <ol><li>スライド ガラスをクリーニング <ol><li>化学フードで濃硫酸の混合液で 30 巻 % 過酸化水素溶液 (10:1) 20 分間ホット プレート上のガラス スライドを沸騰します 。
				注意: 硫酸と過酸化水素蒸気は非常に有毒な</li>。
			</ol></li> <li>スライド ガラスを洗う <ol><li>脱イオン水を使用してスライド ガラスを洗浄し、高純度窒素ブローします</li>。
			</ol></li> <li>塗膜 <ol><li>コート コーティング バーの下面とガラスの上面間 100 μ m ギャップでの特注コーティング装置でスライド ガラス上の SU 8 フォトレジスト</li>。
			</ol></li> <li>スピン コーティング <ol><li>30 40.3 x g でスピン塗布装置を使用して均一な膜を形成するガラス スライド上のフォトレジストを広める s。均一な膜の厚さは約 85 μ m.</li>
			</ol></li> <li>凝固 <ol><li>プログラムを制御する温度でオーブンでフォトレジストを固めます。温度を室温から 65 ° C 2 ° C/分に昇格させる 65 ° C 2 分続行で熱 65 の ° C から 95 ° C からを押しながら部屋に自然を 95 ° C 15 分ターン オーブンとクールで押しオーブンで温度</li>。
			</ol></li> <li>紫外線露光 <ol><li>ガラスの側面に 12 の紫外線フォトレジストとスライド公開フォトマスクとして透明度を用いたフォトリソグラフィ 19 s 。
				注: 紫外光の波数は 365 nm と照射エネルギー量は 273.6 mJ/cm 2. 
				注意: はオーブンや紫外線で作業しながら適切な安全措置を取ます</li>。
			</ol></li> <li>1.2.2.5 の手順で説明するように、フォトレジストを固めるです</li>。
			<li>開発途上 <ol><li>開発者向け 30 s. 洗浄イソプロパノールおよび開発者は、2 つは、スライド ガラス上の沈殿物がなくなるまで交互にスライド ガラスの超音波フォトレジストをきれいします</li>。
			</ol></li> <li>プログラムを制御する温度でオーブンでフォトレジストを固めます。温度を常温から 170 ° C で 2 ° C/分に昇格させる押し 30 分ターン オーブンとクールな 170 ° C で当然オーブンで部屋の温度にします</li>。
		</ol></li> <li>ソフト ・ リソグラフィー <ol><li>金型と 65 ° C で 30 分間の治療上 8.8 g 液体ポリジメチルシロキサン (PDMS) 前ポリマーを注ぎ、80 ° c. 液体 PDMS 前ポリマーで 15 分は、PDMS と硬化剤 (通常は 10:1 (w/w) で構成されています</li>。
		</ol></li> <li>パンチ <ol><li>ドリルによって、チャネルの先頭に PDMS レプリカに穴をパンチします。ドリルの直径は 1.2 mm です</li>。
		</ol></li> <li>シール <ol><li>2 つの PDMS 層表面に酸素プラズマ処理によるパターンがないフラット PDMS 層へのチャネルに PDMS レプリカをシールします 。
			注: チップの準備プロセス全体は約 72 h</li>
		</ol></li></ol></li> <li>作製の RSF 繊維 <ol><li>回転して麻薬の注射 <ol><li>注入シリンジ ポンプで 2 μ L/分でマイクロに麻薬を回転 RSF</li>。
		</ol></li> <li>環境規制 <ol><li>40 ± 5 に相対湿度を調整する RH % または 50 ± 5 %rh の加湿器を使います。常温 40 ± 5% として紡糸繊維凝固に比べ 50 ± 5 %rh</li>。
		</ol></li> <li>国境なき記者団の生産繊維 <ol><li>マイクロ流路の出口にピンポイントで RSF ドロップをタッチ、空気中に RSF 繊維を描画し、その後 ( 図 1b 3 cm/秒の速度で 10 cm エアー ギャップをローラーの上にリール).</li>
		</ol></li> <li>24 時間の密封されたデシケータで RSF 繊維を格納</li>
		<li>繊維後処理 <ol><li>に描画として紡糸繊維 4 回 80 vol % エタノで 0.9 mm s -1特注マシンと描かれた繊維を見続ける l ソリューションは固定、1 h のためのソリューションで繊維を浸します。この治療のため、繊維の長さは当初 15 mm から 60 mm に変更されました</li>。
		</ol></li> <li>特性評価用サンプルを準備する <ol><li>紙フレームに 10 mm ゲージ長さでポスト処理繊維を固定します。少なくとも 20 の繊維は、引張試験、SEM、FTIR、広角でを含む測定の必要性です。 図 1 は、10 μ m に 5 から後描かれた繊維の範囲の直径は、繊維の生産および広角の特性の概略図を示しています。国境なき記者団繊維の機械的性質は、材料試験装置 (25 ± 2) ° C と (45 ± 5) % 相対湿度によって検討しました。拡張レートし、ゲージ長 2 mm/分と 1 cm であった</li>。
		</ol></li></ol></li></ol> 2。放射特性の結晶構造の RSF 繊維 <ol><li>放射特性 4 , 13 , 17 <ol><li>ビームライン <ol><li>の調整は、それぞれ波長 x 線と 0.07746 の nm と 3 x 2 μ m 2、スポット サイズを調整します 。
			メモ: プロトコルは上海のシンクロトロン放射光施設で BL15U1 ビームラインを使用して実行されます</li>。
		</ol></li> <li>X 線のスポットの場所 <ol><li>x 線のスポットの場所を検索します 。
			注: シンクロトロン放射光施設で検査技師による x 線のスポットの位置を調節します</li>。
		</ol></li> <li>標準試料の評価: 二酸化セリウム (CeO 2) <ol><li>標準サンプル CeO 2 粉末をテストします。円の中心およびサンプルから検出器までの距離を計算する特徴付けられた CeO 2 粉</li>。
		</ol></li> <li>試料調製 <ol><li>紙フレームに互いと並行して 10 mm ゲージと RSF フィラメントを修正します。テスト段階で紙フレームに接着します 。
			注: は、繊維を水平に保ちます</li>。
		</ol></li> <li>SR 広角のテスト <ol><li>シャッターを開く <ol><li>部屋で人がないことを確認した後共用ビーム ステーションのドアを閉じます。X 線ビーム源のシャッターを開く</li>。
			</ol></li> <li>中心 <ol><li>少しがフォーカスされるまでの繊維を移動します。X、y、z 方向 ( 図 1 c) ソフトウェアを介してリモートに沿って光ファイバーの位置を調整します</li>。
			</ol></li> <li>露出のサンプル <ol><li>上下繊維リモート ソフトウェアを介してそれは x 線のスポットまで。20 x 線ビームラインに繊維を公開するソフトウェアのスタート ボタンを押します ( 図 1 c) s.</li>
			</ol></li> <li>回折の背景 <ol><li>ソフトウェアを介してリモートで 20 s. 移動 x 線のスポットから繊維の露光時間と空気背景の回折をテストします。プレス、&#34; 開始 &#34; に x 線ビームラインを公開するソフトウェアのボタン &#34; 空気中 &#34; 20 の s.</li>
			</ol></li></ol></li></ol></li> <li>SR 広角データ処理 13 <ol><li>ソフトウェアのキャリブレーション <ol><li>FIT2D (V12.077) を用いた広角データを処理します。円の中心とのサンプル-検出 CeO 2 粉末回折データを用いた距離調整します</li>。
		</ol></li> <li>2 D 回折パターン <ol><li>FIT2D (V12.077) を使用して繊維の回折パターンから空気背景を減算します</li>。
		</ol></li> <li>結晶化度と結晶子サイズ <ol><li>散乱角 2 θ の関数としての回折強度を統合します。自動ピーク分離ソフトウェア (バージョン 4.12) 12 強度統合のデコンボリューションを実行します。C、x、結晶化度の関係から推定された: <img alt="Equation"src="/files/ftp_upload/56271/56271eq1.jpg"/> 、どこで私 c は結晶のピークの積分強度の合計 アモルファス ヘイロー 4 , 11 の統合の強さです。広角パターンの統合 [200] のピーク幅を示した、[020] [002] 反射。これらのピークの半値幅は、に沿って結晶子サイズを決定に使用された、b、および c 軸シェラーを使用して &#39; s 式 4</li>。
		</ol></li> <li>、配向の測定 <ol><li>、結晶の向きを計算して、ピーク 11 (020) の方位角の統合および (210) によると非晶質。ハーマンによると結晶の配向性を定量的計算できます &#39; s 向き。ここでは、両方の (020) (210) のピークは、2 つのガウス機能装備があったとします。狭いものは、結晶方位と指向の非晶質材料 13 他のより広範なもの。ここでは、RSF 繊維の結晶方位は方位統合 (002) ピークの半値幅の全幅を使用して比較した</li>。
		</ol>
		</li>
	</ol>
	</li>
</ol>

<ol>
	<li>Asakura, T., 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=Some+observations+on+the+structure+and+function+of+the+spinning+apparatus+in+the+silkworm+Bombyx+mori.">Some observations on the structure and function of the spinning apparatus in the silkworm Bombyx mori.</a> Biomacromolecules. 8 (1), 175-181 (2007).</li><li>Vollrath, F., Knight, D. P. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Liquid+crystalline+spinning+of+spider+silk.">Liquid crystalline spinning of spider silk.</a> Nature. 410 (6828), 541-548 (2001).</li><li>Zhou, G. Q., Shao, Z. Z., Knight, D. P., Yan, J. P., Chen, X. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Silk+Fibers+Extruded+Artificially+from+Aqueous+Solutions+of+Regenerated+Bombyx+mori+Silk+Fibroin+are+Tougher+than+their+Natural+Counterparts.">Silk Fibers Extruded Artificially from Aqueous Solutions of Regenerated Bombyx mori Silk Fibroin are Tougher than their Natural Counterparts.</a> Adv Mater. 21 (3), 366-370 (2009).</li><li>Sun, M. J., Zhang, Y. P., Zhao, Y. M., 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=The+structure-property+relationships+of+artificial+silk+fabricated+by+dry-spinning+process.">The structure-property relationships of artificial silk fabricated by dry-spinning process.</a> J Mater Chem. 22 (35), 18372-18379 (2012).</li><li>Martel, A., 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=Silk+Fiber+Assembly+Studied+by+Synchrotron+Radiation+SAXS/WAXS+and+Raman+Spectroscopy.">Silk Fiber Assembly Studied by Synchrotron Radiation SAXS/WAXS and Raman Spectroscopy.</a> J Am Chem Soc. 130 (50), 17070-17074 (2008).</li><li>Rammensee, S., Slotta, U., Scheibel, T., Bausch, A. R. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Assembly+mechanism+of+recombinant+spider+silk+proteins.">Assembly mechanism of recombinant spider silk proteins.</a> P Natl Acad Sci USA. 105 (18), 6590-6595 (2008).</li><li>Kinahan, M. 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>

著者が明らかに何もありません。

RSF ソリューションの透析中に pH 値は次の濃度処理にとって重要です。脱イオン水の pH 値が 6 よりも小さい場合、RSF ソリューションはゲル濃度プロセスの間に容易になります。ゲル化を避けるためには、CaCl2は、国境なき記者団のソリューションに追加されます。CaCl2の濃度は、国境なき記者団の重量あたり 1 モルです。
我々 の以前の仕事は、国境なき?...

蜘蛛や蚕は、周囲温度と圧力で水溶液中のタンパク質溶液から卓越した絹繊維を作り出すことができます。せん断と伸張流れは絹糸腺1液晶テクスチャの形成を誘導することができます。近年、高強度人工繊維を生成するためにスパイダーの回転プロセスを模倣することに大きな関心があった。ただし、効率的かつ経済的には共食いによりクモを農業でクモ絹タンパク質の大量の作成ができません。家蚕絹のかなりの量は、農耕によって簡単に取得できます。そうでなければ、カイコとクモと同様回転プロセスとアミノ酸組成があります。したがって、カイコ絹フィブロインは多くの研究者によって動物の人工シルクをスピンする代替として選択されます。
クモとカイコは、空気中の繊維に彼らの回転の管を通して蛋白質の解決を押し出します。最も可能性の高い回転管に沿って発生した高い応力力より拡張された構造2絹フィブロイン分子をストレッチします。人工シルクの繊維は、従来の湿式紡糸とドライ回転プロセス3,4を考慮していないを使用してスピンされているアカウント回転ダクト内流体力。
まず、マイクロのアプローチは、シルクプロテイン5,6のアセンブリを調査する使用されました。国境なき記者団のマイクロ加工をせん断と引張りの力7、8をモデリングによって調べた。ヤング係数と国境なき記者団繊維の繊維径をマイクロ湿式紡糸で調整できますが、描かれた繊維の引張強度は未満 100 MPa7。最後に、国境なき記者団の高強度繊維をマイクロ ドライ回転法を用いた正常に調製が繊維の径は 2 μ m8でだけ。最近では、マイクロ流体湿式紡糸は正常に高強度組換えスパイダー シルク繊維の生産で使用されました。人工繊維9の表面および内部欠陥を改善空気の後回転描画します。
この研究では、国境なき記者団繊維の紡糸改良されたマイクロが登場です。それは家蚕絹、せん断力、及びドライ紡糸紡績ドープを含むの回転プロセスを模倣するように目指しています。この回転メソッドは、高強度人工シルク繊維を作り出すことができるだけでなく、繊維の直径を調整することができますも。まず、ドープを回転国境なき記者団はせん断され第 2 順序の指数関数的減衰で biomimic チャンネルで細長い。第二に、マイクロ ドライ回転プロセス10繊維形態と性質に及ぼす相対湿度 (RH) の影響を調べた。従来回転スピナレットと比較して、マイクロ流体システムは非常に模倣と湿式紡糸法または乾燥による周囲温度でのソリューションから高強度繊維を生成する使用ことができます。
高解像度、高輝度、高エネルギー放射光マイクロ x 線のため直径数 μ m4,11の単一繊維の微細構造の特性評価に使用することができます。,12,13,14します。 ここでは、SR 広角技術は、結晶、結晶子サイズと RSF 線維の配向性の計算に使用されました。

<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

プロトコルは、カイコの回転プロセスを模倣するためのメソッドを示します。ネイティブ紡糸契約紡績ダクトは小型・せん断・伸長力によって順序付けられた絹蛋白質を使用できます。ここでは、生体模倣マイクロ流路は、カイコの回転管の特定の形状を模倣するように設計されました。高濃度ドープした再生絹フィブロイン (RSF) 回転は周囲温度および圧力でドライ スピン繊維マイクロ チャネルを通じて押し出されます。ポスト処理プロセスでとして紡糸繊維が描画され、エタノール水溶液に保存されています。シンクロトロン放射光 (SR 広角) 広角 x 線回折技術は、国境なき記者団の光軸を通常の x 線マイクロビームでサンプル ホルダーに固定された単一の RSF 繊維の微細構造を調査に使用されました。結晶、結晶子サイズと繊維の配向性は、広角のデータから計算されました。広角の 2次元パターンの赤道付近の回折円弧は、ポスト処理の RSF 繊維が高配向度を持っていることを示します。

国境なき記者団の高強度繊維は、紡糸法マイクロを使用して正常に生産されました。応力-ひずみ曲線と伸ばされた国境なき記者団繊維 C44R40 の SEM 像は図 2のとおりです。少なくとも 10 の繊維は、引張試験で測定しました。応力-ひずみ曲線は、繊維の破断応力の平均値によると選ばれました。繊維の広角データは図 3のと?...

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

マイクロ流体ドライ回転と再生絹フィブロイン繊維の特性

マイクロ流体回転再生絹フィブロイン モノフィラメントの微細構造キャラクタリゼーションのためのプロトコルが表示されます。

The protocol demonstrates a method for mimicking the spinning process of silkworm. In the native spinning process, the contracting spinning duct enables ...

microfluidic-dry-spinning-characterization-regenerated-silk-fibroin

Research

JoVE Journal

Chemistry

9.7K ビュー.  Donghua University. マイクロ流体回転再生絹フィブロイン モノフィラメントの微細構造キャラクタリゼーションのためのプロトコルが表示されます。

ビデオ: Microfluidic Dry-spinning and Characterization of Regenerated Silk Fibroin Fibers

Split-and-pool Synthesis and Characterization of Peptide Tertiary Amide Library

Peptidomimetics are great sources of protein ligands. The oligomeric nature of these compounds enables us to access large synthetic libraries on solid phase by using combinatorial chemistry. One of the most well studied classes of peptidomimetics is peptoids. Peptoids are easy to synthesize and have been shown to be proteolysis-resistant and cell-permeable. Over the past decade, many useful protein ligands have been identified through screening of peptoid libraries. However, most of the ligands identified from peptoid libraries do not display high affinity, with rare exceptions. This may be due, in part, to the lack of chiral centers and conformational constraints in peptoid molecules. Recently, we described a new synthetic route to access peptide tertiary amides (PTAs). PTAs are a superfamily of peptidomimetics that include but are not limited to peptides, peptoids and N-methylated peptides. With side chains on both &#945;-carbon and main chain nitrogen atoms, the conformation of these molecules are greatly constrained by sterical hindrance and allylic 1,3 strain. (Figure 1) Our study suggests that these PTA molecules are highly structured in solution and can be used to identify protein ligands. We believe that these molecules can be a future source of high-affinity protein ligands. Here we describe the synthetic method combining the power of both split-and-pool and sub-monomer strategies to synthesize a sample one-bead one-compound (OBOC) library of PTAs.

Peptide tertiary amides (PTAs) are a superfamily of peptidomimetics that include but are not limited to peptides, peptoids and N-methylated peptides. Here we describe a synthetic method which combines&#160;both split-and-pool and sub-monomer strategies to synthesize a one-bead one-compound library of PTAs.

ペプチド第三級アミドライブラリのスプリット·アンド·プールの合成とキャラクタリゼーション

Peptidomimetics are great sources of protein ligands. The oligomeric nature of these compounds enables us to access large synthetic libraries on solid ...

化学

Manufacturing of Three-dimensionally Microstructured Nanocomposites through Microfluidic Infiltration

Microstructured composite beams reinforced with complex three-dimensionally (3D) patterned nanocomposite microfilaments are fabricated via nanocomposite in&#64257;ltration of 3D interconnected microfluidic networks. The manufacturing of the reinforced beams begins with the fabrication of microfluidic networks, which involves layer-by-layer deposition of fugitive ink filaments using a dispensing robot, filling the empty space between filaments using a low viscosity resin, curing the resin and finally removing the ink.&#160;Self-supported 3D structures with other geometries and many layers (e.g.&#160;a few hundreds layers) could be built using this method. The resulting tubular micro&#64258;uidic networks are then infiltrated with thermosetting nanocomposite suspensions containing nanofillers (e.g.&#160;single-walled carbon nanotubes), and subsequently cured. The infiltration is done by applying a pressure gradient between two ends of the empty network (either by applying a vacuum or vacuum-assisted microinjection). Prior to the infiltration, the nanocomposite suspensions are prepared by dispersing nanofillers into polymer matrices using ultrasonication and three-roll mixing methods. The nanocomposites (i.e.&#160;materials infiltrated) are then solidified under UV exposure/heat cure, resulting in a 3D-reinforced composite structure. The technique presented here enables the design of functional nanocomposite macroscopic products for microengineering applications such as actuators and sensors.

Three-dimensional (3D) microstructured composite beams are fabricated through the directed and localized infiltration of nanocomposites into 3D porous microfluidic networks. The flexibility of this manufacturing method enables the utilization of different thermosetting materials and nanofillers in order to achieve a variety of functional 3D reinforced nanocomposite macroscopic products.

マイクロ流体浸透を通じて立体的微細構造ナノ複合材料の製造

Microstructured composite beams reinforced with complex three-dimensionally (3D) patterned nanocomposite microfilaments are fabricated via nanocomposite ...

Synthesis and Characterization of Functionalized Metal-organic Frameworks

Metal-organic frameworks have attracted extraordinary amounts of research attention, as they are attractive candidates for numerous industrial and technological applications. Their signature property is their ultrahigh porosity, which however imparts a series of challenges when it comes to both constructing them and working with them. Securing desired MOF chemical and physical functionality by linker/node assembly into a highly porous framework of choice can pose difficulties, as less porous and more thermodynamically stable congeners (e.g., other crystalline polymorphs, catenated analogues) are often preferentially obtained by conventional synthesis methods. Once the desired product is obtained, its characterization often requires specialized techniques that address complications potentially arising from, for example, guest-molecule loss or preferential orientation of microcrystallites. Finally, accessing the large voids inside the MOFs for use in applications that involve gases can be problematic, as frameworks may be subject to collapse during removal of solvent molecules (remnants of solvothermal synthesis). In this paper, we describe synthesis and characterization methods routinely utilized in our lab either to solve or circumvent these issues. The methods include solvent-assisted linker exchange, powder X-ray diffraction in capillaries, and materials activation (cavity evacuation) by supercritical CO2 drying. Finally, we provide a protocol for determining a suitable pressure region for applying the Brunauer-Emmett-Teller analysis to nitrogen isotherms, so as to estimate surface area of MOFs with good accuracy.

Synthesis, activation, and characterization of intentionally designed metal-organic framework materials is challenging, especially when building blocks are incompatible or unwanted polymorphs are thermodynamically favored over desired forms. We describe how applications of solvent-assisted linker exchange, powder X-ray diffraction in capillaries and activation via supercritical CO2 drying, can address some of these challenges.

官能化有機金属構造体の合成とキャラクタリゼーション

Metal-organic frameworks have attracted extraordinary amounts of research attention, as they are attractive candidates for numerous industrial and ...

Preparation and Characterization of SDF-1&#945;-Chitosan-Dextran Sulfate Nanoparticles

Chitosan (CS) and dextran sulfate (DS) are charged polysaccharides (glycans), which form polyelectrolyte complex-based nanoparticles when mixed under appropriate conditions. The glycan nanoparticles are useful carriers for protein factors, which facilitate the in vivo delivery of the proteins and sustain their retention in the targeted tissue. The glycan polyelectrolyte complexes are also ideal for protein delivery, as the incorporation is carried out in aqueous solution, which reduces the likelihood of inactivation of the proteins. Proteins with a heparin-binding site adhere to dextran sulfate readily, and are, in turn, stabilized by the binding. These particles are also less inflammatory and toxic when delivered in vivo. In the protocol described below, SDF-1&#945; (Stromal cell-derived factor-1&#945;), a stem cell homing factor, is first mixed and incubated with dextran sulfate. Chitosan is added to the mixture to form polyelectrolyte complexes, followed by zinc sulfate to stabilize the complexes with zinc bridges. The resultant SDF-1&#945;-DS-CS particles are measured for size (diameter) and surface charge (zeta potential). The amount of the incorporated SDF-1&#945; is determined, followed by measurements of its in vitro release rate and its chemotactic activity in a particle-bound form.

The objective of this protocol is to incorporate SDF-1&#945;, a stem cell homing factor, into dextran sulfate-chitosan nanoparticles. The resultant particles are measured for their size and zeta potential, as well as the content, activity, and in vitro release rate of SDF-1&#945; from the nanoparticles.

SDF-1α-キトサン硫酸デキストランナノ粒子の調製とキャラクタリゼーション

Chitosan (CS) and dextran sulfate (DS) are charged polysaccharides (glycans), which form polyelectrolyte complex-based nanoparticles when mixed under ...

Synthesis and Characterization of Supramolecular Colloids

Control over colloidal assembly is of utmost importance for the development of functional colloidal materials with tailored structural and mechanical properties for applications in photonics, drug delivery and coating technology. Here we present a new family of colloidal building blocks, coined supramolecular colloids, whose self-assembly is controlled through surface-functionalization with a benzene-1,3,5-tricarboxamide (BTA) derived supramolecular moiety. Such BTAs interact via directional, strong, yet reversible hydrogen-bonds with other identical BTAs. Herein, a protocol is presented that describes how to couple these BTAs to colloids and how to quantify the number of coupling sites, which determines the multivalency of the supramolecular colloids. Light scattering measurements show that the refractive index of the colloids is almost matched with that of the solvent, which strongly reduces the van der Waals forces between the colloids. Before photo-activation, the colloids remain well dispersed, as the BTAs are equipped with a photo-labile group that blocks the formation of hydrogen-bonds. Controlled deprotection with UV-light activates the short-range hydrogen-bonds between the BTAs, which triggers the colloidal self-assembly. The evolution from the dispersed state to the clustered state is monitored by confocal microscopy. These results are further quantified by image analysis with simple routines using ImageJ and Matlab. This merger of supramolecular chemistry and colloidal science offers a direct route towards light- and thermo-responsive colloidal assembly encoded in the surface-grafted monolayer.

A protocol for the synthesis and characterization of colloids coated with supramolecular moieties is described. These supramolecular colloids undergo self-assembly upon the activation of the hydrogen-bonds between the surface-anchored molecules by UV-light.

超分子コロイドの合成とキャラクタリゼーション

Control over colloidal assembly is of utmost importance for the development of functional colloidal materials with tailored structural and mechanical ...

Highly Stable, Functional Hairy Nanoparticles and Biopolymers from Wood Fibers: Towards Sustainable Nanotechnology

Nanoparticles, as one of the key materials in nanotechnology and nanomedicine, have gained significant importance during the past decade. While metal-based nanoparticles are associated with synthetic and environmental hassles, cellulose introduces a green, sustainable alternative for nanoparticle synthesis. Here, we present the chemical synthesis and separation procedures to produce new classes of hairy nanoparticles (bearing both amorphous and crystalline regions) and biopolymers based on wood fibers. Through periodate oxidation of soft wood pulp, the glucose ring of cellulose is opened at the C2-C3 bond to form 2,3-dialdehyde groups. Further heating of the partially oxidized fibers (e.g., T = 80 &#176;C) results in three products, namely fibrous oxidized cellulose, sterically stabilized nanocrystalline cellulose (SNCC), and dissolved dialdehyde modified cellulose (DAMC), which are well separated by intermittent centrifugation and co-solvent addition. The partially oxidized fibers (without heating) were used as a highly reactive intermediate to react with chlorite for converting almost all aldehyde to carboxyl groups. Co-solvent precipitation and centrifugation resulted in electrosterically stabilized nanocrystalline cellulose (ENCC) and dicarboxylated cellulose (DCC). The aldehyde content of SNCC and consequently surface charge of ENCC (carboxyl content) were precisely controlled by controlling the periodate oxidation reaction time, resulting in highly stable nanoparticles bearing more than 7 mmol functional groups per gram of nanoparticles (e.g., as compared to conventional NCC bearing &#60;&#60; 1 mmol functional group/g). Atomic force microscopy (AFM), transmission electron microscopy (TEM), and scanning electron microscopy (SEM) attested to the rod-like morphology. Conductometric titration, Fourier transform infrared spectroscopy (FTIR), nuclear magnetic resonance (NMR), dynamic light scattering (DLS), electrokinetic-sonic-amplitude (ESA) and acoustic attenuation spectroscopy shed light on the superior properties of these nanomaterials.

Synthesis schemes to prepare highly stable wood fiber-based hairy nanoparticles and functional cellulose-based biopolymers have been detailed.

高安定、機能毛深いナノ粒子と木材繊維からバイオポリマー：持続可能なナノテクノロジーに向けて

Nanoparticles, as one of the key materials in nanotechnology and nanomedicine, have gained significant importance during the past decade. While ...

Low-energy Cathodoluminescence for (Oxy)Nitride Phosphors

Nitride and oxynitride (Sialon) phosphors are good candidates for the ultraviolet and visible emission applications. High performance, good stability and flexibility of their emission properties can be achieved by controlling their composition and dopants. However, a lot of work is still required to improve their properties and to reduce the production cost. A possible approach is to correlate the luminescence properties of the Sialon particles with their local structural and chemical environment in order to optimize their growth parameters and find novel phosphors. For such a purpose, the low-voltage cathodoluminescence (CL) microscopy is a powerful technique. The use of electron as an excitation source allows detecting most of the luminescence centers, revealing their luminescence distribution spatially and in depth, directly comparing CL results with the other electron-based techniques, and investigating the stability of their luminescence properties under stress. Such advantages for phosphors characterization will be highlighted through examples of investigation on several Sialon phosphors by low-energy CL.

Low-energy Cathodoluminescence for OxyNitride Phosphors

An excellent chemical and luminescence stabilities of (oxy)nitride phosphors present it as an promising alternative to currently used sulfide and oxide phosphors. In this paper, we present the way to investigate its local luminescence properties using low-energy cathodoluminescence (CL).

（オキシ）窒化物蛍光体のための低エネルギーのカソードルミネッセンス

Nitride and oxynitride (Sialon) phosphors are good candidates for the ultraviolet and visible emission applications. High performance, good stability and ...

Microfluidic-based Synthesis of Covalent Organic Frameworks (COFs): A Tool for Continuous Production of COF Fibers and Direct Printing on a Surface

Covalent Organic Frameworks (COFs) are a class of porous covalent materials which are frequently synthesized as unprocessable crystalline powders. The first COF was reported in 2005 with much effort centered on the establishment of new synthetic routes for its preparation. To date, most available synthetic methods for COF synthesis are based on bulk mixing under solvothermal conditions. Therefore, there is increasing interest in developing systematic protocols for COF synthesis that provide for fine control over reaction conditions and improve COF processability on surfaces, which is essential for their use in practical applications. Herein, we present a novel microfluidic-based method for COF synthesis where the reaction between two constituent building blocks, 1,3,5-benzenetricarbaldehyde (BTCA) and 1,3,5-tris(4-aminophenyl)benzene (TAPB), takes place under controlled diffusion conditions and at room temperature. Using such an approach yields sponge-like, crystalline fibers of a COF material, hereafter called MF-COF. The mechanical properties of MF-COF and the dynamic nature of the approach allow the continuous production of MF-COF fibers and their direct printing onto surfaces. The general method opens new potential applications requiring advanced printing of 2D or 3D COF structures on flexible or rigid surfaces.

Microfluidic-based Synthesis of Covalent Organic Frameworks COFs: A Tool for Continuous Production of COF Fibers and Direct Printing on a Surface

We present a novel microfluidic-based method for synthesis of covalent organic frameworks (COFs). We demonstrate how this approach can be used to produce continuous COF fibers, and also 2D or 3D COF structures on surfaces.

コバレント有機骨格（COF）のマイクロ流体ベースの合成：COF繊維の連続生産と表面への直接印刷のためのツール

Covalent Organic Frameworks (COFs) are a class of porous covalent materials which are frequently synthesized as unprocessable crystalline powders. The ...

Preparation and Characterization of C60/Graphene Hybrid Nanostructures

Physical thermal deposition in a high vacuum environment is a clean and controllable method for fabricating novel molecular nanostructures on graphene. We present methods for depositing and passively manipulating C60 molecules on rippled graphene that advance the pursuit of realizing applications involving 1D C60/graphene hybrid structures. The techniques applied in this exposition are geared towards high vacuum systems with preparation areas capable of supporting molecular deposition as well as thermal annealing of the samples. We focus on C60 deposition at low pressure using a homemade Knudsen cell connected to a scanning tunneling microscopy (STM) system. The number of molecules deposited is regulated by controlling the temperature of the Knudsen cell and the deposition time. One-dimensional (1D) C60 chain structures with widths of two to three molecules can be prepared via tuning of the experimental conditions. The surface mobility of the C60 molecules increases with annealing temperature allowing them to move within the periodic potential of the rippled graphene. Using this mechanism, it is possible to control the transition of 1D C60 chain structures to a hexagonal close packed quasi-1D stripe structure.

Preparation and Characterization of C60/Graphene Hybrid Nanostructures

Here we present a protocol for the fabrication of C60/graphene hybrid nanostructures by physical thermal evaporation. Particularly, the proper manipulation of deposition and annealing conditions allow the control over the creation of 1D and quasi 1D C60 structures on rippled graphene.

C60/Graphene ハイブリッド ナノ構造の作製と評価

Physical thermal deposition in a high vacuum environment is a clean and controllable method for fabricating novel molecular nanostructures on graphene. We ...

Microfluidic Preparation of Liquid Crystalline Elastomer Actuators

This paper focuses on the microfluidic process (and its parameters) to prepare actuating particles from liquid crystalline elastomers. The preparation usually consists in the formation of droplets containing low molar mass liquid crystals at elevated temperatures. Subsequently, these particle precursors are oriented in the flow field of the capillary and solidified by a crosslinking polymerization, which produces the final actuating particles. The optimization of the process is necessary to obtain the actuating particles and the proper variation of the process parameters (temperature and flow rate) and allows variations of size and shape (from oblate to strongly prolate morphologies) as well as the magnitude of actuation. In addition, it is possible to vary the type of actuation from elongation to contraction depending on the director profile induced to the droplets during the flow in the capillary, which again depends on the microfluidic process and its parameters. Furthermore, particles of more complex shapes, like core-shell structures or Janus particles, can be prepared by adjusting the setup. By the variation of the chemical structure and the mode of crosslinking (solidification) of the liquid crystalline elastomer, it is also possible to prepare actuating particles triggered by heat or UV-vis irradiation.

This article describes the microfluidic process and parameters to prepare actuating particles from liquid crystalline elastomers. This process allows the preparation of actuating particles and the variation of their size and shape (from oblate to strongly prolate, core-shell, and Janus morphologies) as well as the magnitude of actuation.

液晶エラストマーのアクチュエータのマイクロの準備

This paper focuses on the microfluidic process (and its parameters) to prepare actuating particles from liquid crystalline elastomers. The preparation ...