우리는 고급 소재의 니케 연구소, 흐로 닝언 대학의 재정 지원을 인정합니다.

두 Gyroid 형태론 1. 준비 및 PS-B-P4VP의 특성 (PDP) 단지 <ol><li> 달다 폴리스티렌 - 블록 - 폴리 (4 - 비닐 피리딘) (PS-B-P4VP)과 pentadecylphenol (PDP, M의 R = 304.51 g / 몰). 되어야 gyroid 형태를 얻기 위해서 신중 PDP의 양을 선택 ((P4VP (PDP) f)는 CA되어야 P4VP (PDP) 블록의 중량 분율. 0.6 직선 AB 디 블록 공중 합체의 상태도에 따라). 보통, PS-B-P4VP의 0.15-0.2 g의 (단계 1.3에서 사용되는 배양 접시의 직경 5 ~ 6 cm입니다 주어진) PS-B-P4VP 50 ~ 100 μm의 두께 (PDP) 필름에 이르게한다. 다음의 식에 따른 PDP의 양을 계산한다 : <img alt="식 (1)" src="/files/ftp_upload/50673/50673eq1.jpg" /> <img alt="식 2" src="/files/ftp_upload/50673/50673eq2.jpg" /> <img alt="식 3" src="/files/ftp_upload/50673/50673eq3.jpg" /><br/&gt; <img alt="식 4" src="/files/ftp_upload/50673/50673eq4.jpg" /></li><li> 클로로포름에 PS-B-P4VP와 PDP를 녹이고 실온에서 몇 시간 동안 저어. 균질 복합체 형성을 보장하기 위해 2 중량 % 이하의 중합체 농도를 유지한다. </li><li> 유리 페트리 접시에 솔루션을 붓는다. </li><li> 포화 클로로포름 분위기에 접시를 놓습니다. </li><li> 일주일 정도 후, 페트리 접시를 꺼내. 초분자 복합체의 막이 형성된다. </li><li> 하룻밤 30 ° C에서 진공 필름을 건조시킵니다. </li><li> 특수 제작 된 용기에 필름을 배치, 컨테이너에서 공기를 제거하고 질소로 채 웁니다. 1 바 과압와 N 2 분위기에서 120 ° C 오븐에서 4 일 동안 필름을 어닐링. </li><li> 에폭시에 포함 된 영화의 작은 조각을 잘라 40 ℃에서 하룻밤 치료 </li><li> 실온에서 다이아몬드 나이프를 사용하여 약 80 nm의 두께로 샘플을 마이크로톰. 일전자 microtomed 부분은 물에 뜰 것이다. 을 들고 구리 그리드에 배치합니다. </li><li> 요오드와 항아리에 microtomed 섹션을 포함하는 그리드를 넣습니다. 45 분 샘플 스테인드 및 투과 전자 현미경에 대한 준비가되면. </li><li> 120 kV의 및 이미지 샘플의 가속 전압에서 동작하는 투과 전자 현미경 스테인드 섹션과 구리 그리드를 삽입합니다. </li><li> 소각 X-선 산란 용 샘플 홀더에 (단계 1.7 후에 얻어진) 필름의 조각을 넣고 캡톤 테이프로 고정한다. SAXS의 기계로 제조 된 샘플 홀더를 배치합니다. X-선 셔터를 열고 2D 산란 패턴을 취득. 얻어진 2 차원 패턴을 통합하고 1D 패턴에서 피크의 위치를​​ 분석한다. </li></ol> 다공성 구조의 2. 생성 및 특성 <ol><li> 에탄올 (단계 1.7 후의) 필름의 조각을 넣어 사흘 동안 보관. </li><li> 샘플을 건조시킵니다. </li><li> 사전1 H NMR 측정을위한 샘플을 깎다. PDP 파우더, PS-B-P4VP 분말을 CDCl3에 (단계 2.2 이후) 초분자 복합체 PS-B-P4VP (PDP) (단계 1.7 이후), 다공성 필름을 용해. 실온에서 기록 된 1 H NMR 스펙트럼. </li><li> PS-B-P4VP 분말을 분석, 초분자 복합체 PS-B-P4VP (PDP) (단계 1.7 이후) 및 시차 주사 열량계에 의한 다공성 필름 (단계 2.2 이후). 1 ° C / 분의 가열 / 냉각 속도, 0.5 ° C의 진동 진폭, 60 초 진동주기와 변조 모드를 사용합니다. -30 ° C에서 샘플을 평형, 열 180 ° C에, -30 ° C로 냉각 한 다음 180 ℃로 다시 가열 C. 분석을 위해 제 2 가열 사이클에서 데이터를 사용한다. </li><li> 70 ° C에서 상온에서 8 시간 동안 18 시간 동안 (단계 2.2 이후) 다공성 샘플을 배출 가스 77 K.에서 질소 흡착 측정을 수행 </li><li> 적절한 소프트웨어 (예 WinAD를 사용P) 및 수득 등온선을 분석하는 모델. </li><li> 2 시간 동안 0.5 파의 실내 온도와 압력에서 8 시간 및 가스 제거를 위해 50 ° C에서 (단계 2.2 이후) 다공성 샘플을 건조시킵니다. </li><li> 수은 압 입법을 수행합니다. </li></ol> 폴리머 템플릿 3. 삽입 니켈 <ol><li> 염화 주석 (SnCl 2, M의 R = 189.60 g / 몰)을 밖으로 달아 수용액 (0.1 M SnCl 2 / 0.1 M 염산, 1.896 g SnCl 2, 0.8 ㎖의 염산, 100 ml의 H 2 O)를 준비합니다. SnCl 2의 완전한 해체를 보장하기 위해 셰이커 하룻밤에 솔루션을 넣습니다. </li><li> 염화 팔라듐 (의 PdCl 2, M의 R = 177.33 g / 몰)을 밖으로 달아 수용액 (0.0014 M의 PdCl 2 / 0.25 M 염산, 0.025 g의의 PdCl 2, 2 ㎖의 염산 100 ㎖의 H 2 O)를 준비합니다. </li><li> 니켈 도금 욕의 Part 1을 준비 중 6.78 g의 황산 니켈 수화물의 무게 (니소 4 • 6H 2 O, M의 R = 2620.85 g / mol) 및 2g 소듐 시트 레이트 (나 3 C 6 H 5 O 07 M의 R = 258.06 g / mol) 및 물 80 ㎖에 이들을 용해. 828 ㎕의 85 % 젖산 (C 3 H 6 O 3, M의 R = 90.08 g / 몰)를 추가합니다. </li><li> 니켈 도금 욕의 부분이 준비 : 축소 중량 0.2 g 보란 디메틸 아민 착체 ((CH 3) 2 NHBH 3, M의 R = 58.92 g / mol) 및 물 20 ㎖에 녹여. 보란 디메틸 아민 단지는 통풍이 잘되는 흄 후드에서 처리되어야한다. </li><li> 1 시간 동안 염화 주석 (단계 3.1)의 수용액에 다공질 막 (단계 2.2 이후)을 담근다. </li><li> 탈 이온수로 철저하게 필름을 씻어. </li><li> 1 시간 동안 염화 팔라듐 (단계 3.2)의 수용액에 필름을 담근​​다. </li><li> 탈 이온수로 철저하게 필름을 씻어. </li><li> 파트 1 (3.3) 및 니켈 도금 욕의 파트 2 (3.4)을 섞는다. 수산화 암모늄을 사용하여 7.0으로 산도를 조정합니다. </li><li> 1 시간 동안 니켈 도금 욕에 필름을 담근​​다. </li><li> 탈 이온수로 철저하게 필름을 씻어. </li><li> 샘플을 건조시킵니다. </li><li> 단계 1.8-1.9에 설명 된대로 전자 현미경의 도금 샘플을 준비합니다. </li><li> 이미지 단계 1.11에 설명 된대로 샘플. </li><li> 고분해능 투과형 전자 현미경에 도금 샘플의 섹션을 포함하는 구리 그리드입니까. 고해상도 TEM 현미경 사진을 획득. 현미경으로 샘플을 관찰하고 EDX (X-광선의 에너지 분산 분석)에 의한 원소 분석의 영역을 선택합니다. 선택 영역의 EDX 분석을 수행하고 얻어진 패턴을 분석 할 수 있습니다. </li></ol> 역 Gyroid 니켈 거품 4. 노출 <ol><li> 350 ° C의 오븐에서 니켈 도금 필름 (단계 3.12 이후)를 넣어 4 일 1 시간까지에서 보관. </li><li> 은 페이스트를 사용하여 샘​​플 홀더에 샘플을 연결합니다. </li><li> 주사 전자 마이크에 샘플을 삽입roscope. 샘플의 여러 이미지를 획득. </li><li> 주사 전자 현미경으로 샘플을 삽입합니다. 현미경으로 샘플을 관찰하고 EDX에 의한 원소 분석의 영역을 선택합니다. 선택 영역의 EDX 분석을 수행하고 얻어진 패턴을 분석 할 수 있습니다. </li></ol>

<ol>
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Y., 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=Inorganic+Gyroid+with+Exceptionally+Low+Refractive+Index+from+Block+Copolymer+Templating.">Inorganic Gyroid with Exceptionally Low Refractive Index from Block Copolymer Templating.</a> Nano Lett. 10, 4994-5000 (2010).</li><li>Hsueh, H. -. Y., Ho, R. -. M. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Bicontinuous+Ceramics+with+High+Surface+Area+from+Block+Copolymer+Templates.">Bicontinuous Ceramics with High Surface Area from Block Copolymer Templates.</a> Langmuir. 28, 8518-8529 (2012).</li><li>Riedel, W. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=.">.</a> Electroless Nickel Plating. , (1991).</li><li>Mallory, G. O., Hajdu, J. B. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Electroless+Plating:+Fundamentals+and+Applications.">Electroless Plating: Fundamentals and Applications.</a> American Electroplaters and Surface Finishers Society. , (1992).</li><li>Djoki&#263;, S. S. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=.">.</a> Modern Aspects of Electrochemistry. , (2002).</li><li>Djoki&#263;, S. S., Cavallotti, P. L. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=.">.</a> Modern Aspects of Electrochemistry. , (2010).</li><li>Crossland, E. J. W., Ludwigs, S., Hillmyer, M. A., Steiner, U. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Control+of+gyroid+forming+block+copolymer+templates:+effects+of+an+electric+field+and+surface+topography.">Control of gyroid forming block copolymer templates: effects of an electric field and surface topography.</a> Soft Matter. 6, 670-676 (2010).</li><li>Hsueh, H. Y., 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=Nanoporous+Gyroid+Nickel+from+Block+Copolymer+Templates+via+Electroless+Plating.">Nanoporous Gyroid Nickel from Block Copolymer Templates via Electroless Plating.</a> Adv. Mater. 23, 3041-3046 (2011).</li><li>Vukovic, I., 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=Supramolecular+Route+to+Well-Ordered+Metal+Nanofoams.">Supramolecular Route to Well-Ordered Metal Nanofoams.</a> ACS Nano. 5, 6339-6348 (2011).</li><li>Mao, H., Hillmyer, M. A. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Macroscopic+samples+of+polystyrene+with+ordered+three-dimensional+nanochannels.">Macroscopic samples of polystyrene with ordered three-dimensional nanochannels.</a> Soft Matter. 2, 57-59 (2006).</li><li>Kobayashi, Y., Tadaki, Y., Nagao, D., Konno, M. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Deposition+of+Gold+Nanoparticles+on+Polystyrene+Spheres+by+Electroless+Metal+Plating+Technique.">Deposition of Gold Nanoparticles on Polystyrene Spheres by Electroless Metal Plating Technique.</a> J. Phys. Conf. Ser. 61, 582-586 (2007).</li><li>Finnefrock, A. C., Ulrich, R., Toombes, G. E., Gruner, S. M., Wiesner, U. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=The+plumber's+nightmare:+a+new+morphology+in+block+copolymer-ceramic+nanocomposites+and+mesoporous+aluminosilicates.">The plumber's nightmare: a new morphology in block copolymer-ceramic nanocomposites and mesoporous aluminosilicates.</a> J. Am. Chem. Soc. 125, 13084-13093 (2003).</li><li>Tyler, C. A., Morse, D. C. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Orthorhombic+Fddd+network+in+triblock+and+diblock+copolymer+melts.">Orthorhombic Fddd network in triblock and diblock copolymer melts.</a> Phys. Rev. Lett. 94, 208-302 (2005).</li><li>Ranjan, A., Morse, D. C. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Landau+theory+of+the+orthorhombic+Fddd+phase.">Landau theory of the orthorhombic Fddd phase.</a> Phys. Rev. E. 74, 011803 (2006).</li><li>Kim, M. I., 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=Stability+of+the+Fddd+Phase+in+Diblock+Copolymer+Melts.">Stability of the Fddd Phase in Diblock Copolymer Melts.</a> Macromolecules. 41, 7667-7670 (2008).</li></ol>

저자는 더 경쟁 재정적 이익을 선언하지 않습니다.

초분자 복합체가 성공적으로 잘 정렬 된 금속 nanofoams 전구체로 적용됩니다. 이 방법에서 중요한 단계는 gyroid 형태와 템플릿 즉, 적절한 템플릿을 취득하는 것이다. 블록 공중 합체의 상태도에서 gyroid 영역은 매우 작은이며 타겟팅 다소 어렵다. 이것은 종래의 블록 공중 합체를 출발 원료로서 사용하는 경우, 매우 정교한 합성 gyroid 형태학을 초래 원하는 조성, 도달 할 때까지 반복되어야한?...

금속 nanofoams의 준비를 위해 사용할 수있는 몇 가지 방법이 있습니다 : 1-3 탈 합금, 졸 - 겔은 6,7 nanosmelting, 4,5 접근 및 연소 합성 8. 탈 합금 과정에서, 출발 물질은 일반적으로 예를 들어 이진 합금,은과 금의 합금이다. 적은 귀금속,이 경우 실버, 화학적으로 또는 전기 화학적으로 나노 크기의 인대와 무질서 다공성 골드 폼의 결과를 제거 할 수 있습니다. 연소 합성에서, 금속은 그 분해 중에 에너지를 해제하고, 메탈 nanofoam (8)의 형성을 구동 정력 전구체와 혼합된다. 발포 금속의 기계적 행동에 대한 연구는 무질서 아키텍처에서 응력이 전체 대용량 9-11에 인대 나노에서 효율적으로 전송 될 수 있음을 나타냅니다. 따라서 잘 정렬 된 금속 nanofoams가에 비해 우수한 기계적 특성을 가질 것으로 예상된다무질서 것. 여기에 표현 된 아이디어는 금속 nanofoams에 선구자로 주문 나노 구조로 자기 조립 블록 공중 합체를 사용하는 것이다. 구형, 원통형, 층상 이중 gyroid, 육방 천공 라멜라, 외 12-14 : 블록 공중 합체, 단량체 단위의 총 수와 화학적으로 연결된 블록 간의 반발력 정도의 조성에 따라 다양한 모폴로지 같은 나타나는 . 또한, 중합체 블록은 나노 다공성 물질 (15)로 이어지는 선택적으로 분해 될 수있다. 가장 일반적인 방법은 다음을 포함한다 : 오존 분해 16-18, UV 조사 19, 반응성 이온 식각 20-22, 용해 23-26. 생성 된 다공성 구조는 다양한 무기 재료 채워서 할 수 있습니다. 금속 산화물 (예 : 그런가 2, 티오 2) 일반적으로 템플릿의 채널 27 ~ 29에 졸 - 겔 (sol-gel) 법을 통해 도입된다. 엘ectrochemical과 무전 해 도금은 일반적으로 30 ~ 33에 또는 템플릿에 금속을 증착하는 데 사용됩니다. 마지막으로, 나머지 중합체는 열분해 등이 용해 34,35, UV 열화 28,29 통해 고분자 / 무기 나노 하이브리드로부터 제거 될 수있다 우리의 접근 방식에서 우리는 폴리스티렌 - 블록 - 폴리 (4 - 비닐 피리딘)의 초분자 복합체 (PS-B-P4VP) 블록 공중 합체 및 양친 pentadecylphenol (PDP) 분자에서 시작합니다. 이 복합체는 PDP 및 피리딘 고리 (도 1A) 사이의 수소 결합의 결과이다. 시작 블록 공중 합체의 조성 및 첨가 PDP의 양은 그러한 방식으로 선택되는 PS 네트워크와 P4VP (PDP) 행렬 bicontinuous 이중 gyroid 형태에서 얻어진 시스템 자체 조립한다 (도 1B). PDP 분자를 선택적으로 PS 네트워크 (에 에탄올과 P4VP 체인 붕괴에 용해 될그림 1C). 이어서, 무전 해 도금법을 사용하여, 니켈은 ​​템플릿 (도 1D)의 기공에 증착된다. 열분해를 통해 나머지 중합체의 제거 후, 잘 정돈 gyroid 니켈 nanofoam는 (도 1E)를 얻을 수있다.

<table border="1">
 <tbody>
 <tr>
 <td>REAGENTS:</td>
 <td></td>
 <td></td>
 <td></td>
 </tr>
 <tr>
 <td>PS-b-P4VP, CAS: 26222-40-2</td>
 <td>Polymer Source Inc.</td>
 <td>P9009-S4VP 
 P136-S4VP 
 P5462-S4VP 
 P3912-S4VP</td>
 <td>additional information are provided in a separate table</td>
 </tr>
 <tr>
 <td>PDP</td>
 <td>Aldrich</td>
 <td>P4402-100G-A</td>
 <td>recrystallized twice from petroleum ether</td>
 </tr>
 <tr>
 <td>SnCl2</td>
 <td>Acros Organics</td>
 <td>196981000</td>
 <td></td>
 </tr>
 <tr>
 <td>PdCl2</td>
 <td>Aldrich</td>
 <td>76050</td>
 <td></td>
 </tr>
 <tr>
 <td>NiSO4 x H2O</td>
 <td>Sigma-Aldrich</td>
 <td>227676</td>
 <td></td>
 </tr>
 <tr>
 <td>lactic acid</td>
 <td>Aldrich</td>
 <td>W261106</td>
 <td></td>
 </tr>
 <tr>
 <td>citric acid trisodium salt</td>
 <td>Sigma-Aldrich</td>
 <td>C3674</td>
 <td></td>
 </tr>
 <tr>
 <td>borane dimethyl amine complex</td>
 <td>Aldrich</td>
 <td>180238</td>
 <td></td>
 </tr>
 <tr>
 <td>PS-b-P4VP catalogue number</td>
 <td>Mn (PS), g/mol</td>
 <td>Mn(P4VP), g/mol</td>
 <td>PDI</td>
 </tr>
 <tr>
 <td>P9009-S4VP</td>
 <td>24000</td>
 <td>9500</td>
 <td>1.1</td>
 </tr>
 <tr>
 <td>P136-S4VP</td>
 <td>31900</td>
 <td>13200</td>
 <td>1.08</td>
 </tr>
 <tr>
 <td>P5462-S4VP</td>
 <td>37500</td>
 <td>16000</td>
 <td>1.3</td>
 </tr>
 <tr>
 <td>P3912-S4VP</td>
 <td>41500</td>
 <td>17500</td>
 <td>1.07</td>
 </tr>
 </tbody>
</table>

gyroid nickel nanostructures from diblock copolymer supramolecules

나노 다공성 금속 폼 속성의 고유 한 조합을 가지고 - 그들은 열 및 전기 전도성, 촉매 활성, 그리고 또한, 다공성, 높은 표면 볼륨 및 비강도있다. 불행하게도, 금속 나노 구조의 준비를위한 일반적인 방법은 기계적 특성에 악영향을 미칠 수있는 매우 무질서 구조와 재질을 렌더링합니다. 블록 공중 합체 주문한 나노 구조로자가 조립하는 능력이 잘 정렬 된 금속 nanofoams 제조하기위한 템플릿으로 적용될 수있다. 여기에서 우리는 블록 공중 합체 기반의 초분자 복합체의 응용 프로그램을 설명 - 폴리스티렌 - 블록 - 폴리 (4 - 비닐 피리딘) (pentadecylphenol) PS-B-P4VP (PDP) - 잘 정돈 니켈 nanofoam의 전구체로. 초분자 복합체는 기존의 블록 공중 합체와 유사한 상 거동을 나타내고 bicontinuous gyroid 형태의 지혜로 자기 조립 수 있습니다P4VP (PDP) 매트릭스에 배치 H 두 개의 PS 네트워크. PDP는 금속 채워서 수 다공성 구조의 형성으로 이어지는 에탄올에 용해 될 수있다. 무전 해 도금 기술을 사용하여, 니켈 템플릿의 채널로 삽입 할 수있다. 마지막으로, 나머지 중합체는 역 gyroid 형태와 나노 다공성 니켈 폼에서 얻어진 중합체 / 무기 나노 하이브리드에서 열분해를 통해 제거 될 수있다.

. 초분자 복합체의 형태는 PS-B-P4VP (PDP) X는 TEM과 SAXS도 2a에 의해 검사되고 대표 초분자 복합체의 전형적인 gyroid 패턴 표시 2b에 : 더블 웨이브와 표현하는 것으로 알려진 수레 바퀴 패턴을 (211)를 통해 돌기 각각 gyroid 단위 셀 (111)면,. P4VP (PDP) X 블록 도메인이 때문에 요오드 염색을 어둡게 표시하면서 PS 블록 도메인은 밝게 나타납니다. 그림 2C는 주기성?...

Watch this Scientific Journal Video about Gyroid Nickel Nanostructures from Diblock Copolymer Supramolecules at JoVE.com

Gyroid Nickel Nanostructures from Diblock Copolymer Supramolecules

이 문서에서는 자기 조립 블록 공중 합체 기반 초분자에서 얻은 나노 다공성 템플릿 상에 무전 해 금속 증착을 통해 잘 정돈 니켈 nanofoams의 준비에 대해 설명합니다.

디 블록 공중 합체의 초분자에서 Gyroid 니켈 나노 구조

Nanoporous metal foams possess a unique combination of properties - they are catalytically active, thermally and electrically conductive, and furthermore, ...

gyroid-nickel-nanostructures-from-diblock-copolymer-supramolecules

Research

JoVE Journal

Chemistry

12.3K 조회수.  University of Groningen.  이 문서에서는 자기 조립 블록 공중 합체 기반 초분자에서 얻은 나노 다공성 템플릿 상에 무전 해 금속 증착을 통해 잘 정돈 니켈 nanofoams의 준비에 대해 설명합니다. 

비디오: Gyroid Nickel Nanostructures from Diblock Copolymer Supramolecules

Nucleoside Triphosphates - From Synthesis to Biochemical Characterization

The traditional strategy for the introduction of chemical functionalities is the use of solid-phase synthesis by appending suitably modified phosphoramidite precursors to the nascent chain. However, the conditions used during the synthesis and the restriction to rather short sequences hamper the applicability of this methodology. On the other hand, modified nucleoside triphosphates are activated building blocks that have been employed for the mild introduction of numerous functional groups into nucleic acids, a strategy that paves the way for the use of modified nucleic acids in a wide-ranging palette of practical applications such as functional tagging and generation of ribozymes and DNAzymes. One of the major challenges resides in the intricacy of the methodology leading to the isolation and characterization of these nucleoside analogues.
	
	In this video article, we present a detailed protocol for the synthesis of these modified analogues using phosphorous(III)-based reagents. In addition, the procedure for their biochemical characterization is divulged, with a special emphasis on primer extension reactions and TdT tailing polymerization. This detailed protocol will be of use for the crafting of modified dNTPs and their further use in chemical biology.

The protocol described herein aims to explain and abridge the numerous obstacles in the way of the intricate route leading to modified nucleoside triphosphates. Consequently, this protocol facilitates both the synthesis of these activated building-blocks and their availability for practical applications.

뉴 클레오 사이드 트리 포스페이트 - 합성에서 생화학 적 특성에

The  traditional strategy for the introduction of chemical functionalities is the  use of solid-phase synthesis by appending suitably modified ...

연구

화학

Synthesis of Ligand-free CdS Nanoparticles within a Sulfur Copolymer Matrix

Aliphatic ligands are typically used during the synthesis of nanoparticles to help mediate their growth in addition to operating as high-temperature solvents. These coordinating ligands help solubilize and stabilize the nanoparticles while in solution, and can influence the resulting size and reactivity of the nanoparticles during their formation. Despite the ubiquity of using ligands during synthesis, the presence of aliphatic ligands on the nanoparticle surface can result in a number of problems during the end use of the nanoparticles, necessitating further ligand stripping or ligand exchange procedures. We have developed a way to synthesize cadmium sulfide (CdS) nanoparticles using a unique sulfur copolymer. This sulfur copolymer is primarily composed of elemental sulfur, which is a cheap and abundant material. The sulfur copolymer has the advantages of operating both as a high temperature solvent and as a sulfur source, which can react with a cadmium precursor during nanoparticle synthesis, resulting in the generation of ligand free CdS. During the reaction, only some of the copolymer is consumed to produce CdS, while the rest remains in the polymeric state, thereby producing a nanocomposite material. Once the reaction is finished, the copolymer stabilizes the nanoparticles within a solid polymeric matrix. The copolymer can then be removed before the nanoparticles are used, which produces nanoparticles that do not have organic coordinating ligands. This nascent synthesis technique presents a method to produce metal-sulfide nanoparticles for a wide variety of applications where the presence of organic ligands is not desired.

Herein we present a method to synthesize ligand-free cadmium sulfide (CdS) nanoparticles based on a unique sulfur copolymer. The sulfur copolymer operates as a high temperature solvent and a sulfur source during the nanoparticle synthesis and stabilizes the nanoparticles after the reaction.

황 합체 매트릭스 내의 자유 리간드의 CDS 나노 입자의 합성

Aliphatic ligands are typically used during the synthesis of nanoparticles to help mediate their growth in addition to operating as high-temperature ...

Anionic Polymerization of an Amphiphilic Copolymer for Preparation of Block Copolymer Micelles Stabilized by &#960;-&#960; Stacking Interactions

In this study, an amphiphilic copolymer that includes a core-forming block with phenyl groups was synthesized by living anionic polymerization of phenyl glycidyl ether (PheGE) on methoxy-polyethylene glycol (mPEG-b-PPheGE). Characterization of the copolymer revealed a narrow molecular distribution (PDI &#60; 1.03) and confirmed the degree of polymerization of mPEG122-b-(PheGE)15. The critical micelle concentration of the copolymer was evaluated using an established fluorescence method with the aggregation behavior evaluated by dynamic light scattering and transmission electronic microscopy. The potential of the copolymer for use in drug delivery applications was evaluated in a preliminary manner including in vitro biocompatibility, loading and release of the hydrophobic anti-cancer drug doxorubicin (DOX). A stable micelle formulation of DOX was prepared with drug loading levels up to 14% (wt%), drug loading efficiencies &#62; 60% (w/w) and sustained release of drug over 4 days under physiologically relevant conditions (acidic and neutral pH, presence of albumin). The high drug loading level and sustained release is attributed to stabilizing &#960;-&#960; interactions between DOX and the core-forming block of the micelles.

Anionic Polymerization of an Amphiphilic Copolymer for Preparation of Block Copolymer Micelles Stabilized by &amp;#960;-&amp;#960; Stacking Interactions

The key steps of living anionic polymerization of phenyl glycidyl ether (PheGE) on methoxy-polyethylene glycol (mPEG-b-PPheGE) are described. The resulting block copolymer micelles (BCMs) were loaded with doxorubicin 14% (wt%) and sustained release of drug over 4 days under physiologically relevant conditions was obtained.

π-π 스태킹 상호 작용에 의해 안정화 된 블록 공중 합체 미셀 준비하는 양친 매성 공중 합체의 음이온 중합

In this study, an amphiphilic copolymer that includes a core-forming block with phenyl groups was synthesized by living anionic polymerization of phenyl ...

Facet-to-facet Linking of Shape-anisotropic Colloidal Cadmium Chalcogenide Nanostructures

Here, we describe a protocol that allows for shape-anisotropic cadmium chalcogenide nanocrystals (NCs), such as nanorods (NRs) and tetrapods (TPs), to be covalently and site-specifically linked via their end facets, resulting in polymer-like linear or branched chains. The linking procedure begins with a cation-exchange process in which the end facets of the cadmium chalcogenide NCs are first converted to silver chalcogenide. This is followed by the selective removal of ligands at their surface. This results in cadmium chalcogenide NCs with highly reactive silver chalcogenide end facets that spontaneously fuse upon contact with each other, thereby establishing an interparticle facet-to-facet attachment. Through the judicious choice of precursor concentrations, an extensive network of linked NCs can be produced. Structural characterization of the linked NCs is carried out via low- and high-resolution transmission electron microscopy (TEM), as well as energy-dispersive X-ray spectroscopy, which confirm the presence of silver chalcogenide domains between chains of cadmium chalcogenide NCs.

A protocol detailing how shape-anisotropic colloidal cadmium chalcogenide nanocrystals can be covalently linked via their end facets is presented here.

면 대 면 모양 이방성 콜 로이드 카드뮴 칼코게나이드 Nanostructures의 연결

Here, we describe a protocol that allows for shape-anisotropic cadmium chalcogenide nanocrystals (NCs), such as nanorods (NRs) and tetrapods (TPs), to be ...

Synthesis of Platinum-nickel Nanowires and Optimization for Oxygen Reduction Performance

Platinum-nickel (Pt-Ni) nanowires were developed as fuel cell electrocatalysts, and were optimized for the performance and durability in the oxygen reduction reaction. Spontaneous galvanic displacement was used to deposit Pt layers onto Ni nanowire substrates. The synthesis approach produced catalysts with high specific activities and high Pt surface areas. Hydrogen annealing improved Pt and Ni mixing and specific activity. Acid leaching was used to preferentially remove Ni near the nanowire surface, and oxygen annealing was used to stabilize near-surface Ni, improving durability and minimizing Ni dissolution. These protocols detail the optimization of each post-synthesis processing step, including hydrogen annealing to 250 &#176;C, exposure to 0.1 M nitric acid, and oxygen annealing to 175 &#176;C. Through these steps, Pt-Ni nanowires produced increased activities more than an order of magnitude than Pt nanoparticles, while offering significant durability improvements. The presented protocols are based on Pt-Ni systems in the development of fuel cell catalysts. These techniques have also been used for a variety of metal combinations, and can be applied to develop catalysts for a number of electrochemical processes.

&#160; The protocol describes the synthesis and electrochemical testing of platinum-nickel nanowires. Nanowires were synthesized by the galvanic displacement of a nickel nanowire template. Post-synthesis processing, including hydrogen annealing, acid leaching, and oxygen annealing were used to optimize nanowire performance and durability in the oxygen reduction reaction.

백 금-니켈 나노 와이어 및 산소 감소 성능 최적화의 합성

Platinum-nickel (Pt-Ni) nanowires were developed as fuel cell electrocatalysts, and were optimized for the performance and durability in the oxygen ...

Chemical Precipitation Method for the Synthesis of Nb2O5 Modified Bulk Nickel Catalysts with High Specific Surface Area

We demonstrate a method for the synthesis of NixNb1-xO catalysts with sponge-like and fold-like nanostructures. By varying the Nb:Ni ratio, a series of NixNb1-xO nanoparticles with different atomic compositions (x = 0.03, 0.08, 0.15, and 0.20) have been prepared by chemical precipitation. These NixNb1-xO catalysts are characterized by X-ray diffraction, X-ray photoelectron spectroscopy, and scanning electron microscopy. The study revealed the sponge-like and fold-like appearance of Ni0.97Nb0.03O and Ni0.92Nb0.08O on the NiO surface, and the larger surface area of these NixNb1-xO catalysts, compared with the bulk NiO. Maximum surface area of 173 m2/g can be obtained for Ni0.92Nb0.08O catalysts. In addition, the catalytic hydroconversion of lignin-derived compounds using the synthesized Ni0.92Nb0.08O catalysts have been investigated.

Chemical Precipitation Method for the Synthesis of Nb2O5 Modified Bulk Nickel Catalysts with High Specific Surface Area

A protocol for the synthesis of sponge-like and fold-like Ni1-xNbxO nanoparticles by chemical precipitation is presented.

Nb2O5 의 합성을 위한 화학 강 수 방법을 수정할 높은 특정 표면 영역으로 대량 니켈 촉매

We demonstrate a method for the synthesis of NixNb1-xO catalysts with sponge-like and fold-like nanostructures. By varying the Nb:Ni ratio, a series of ...

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.

준비 및 C60/Graphene 하이브리드 Nanostructures의 특성화

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

Disentangling High Strength Copolymer Aramid Fibers to Enable the Determination of Their Mechanical Properties

Traditionally, soft body armor has been made from poly(p-phenylene terephthalamide) (PPTA) and ultra-high molecular weight polyethylene. However, to diversify the fiber choices in the United States body armor market, copolymer fibers based on the combination of 5-amino-2-(p-aminophenyl) benzimidazole (PBIA) and the more conventional PPTA were introduced. Little is known regarding the long-term stability of these fibers, but as condensation polymers, they are expected to have potential sensitivity to moisture and humidity. Therefore, characterizing the strength of the materials and understanding their vulnerability to environmental conditions is important for evaluating their use lifetime in safety applications. Ballistic resistance and other critical structural properties of these fibers are predicated on their strength. To accurately determine the strength of the individual fibers, it is necessary to disentangle them from the yarn without introducing any damage. Three aramid-based copolymer fibers were selected for the study. The fibers were washed with acetone followed by methanol to remove an organic coating that held the individual fibers in each yarn bundle together. This coating makes it difficult to separate single fibers from the yarn bundle for mechanical testing without damaging the fibers and affecting their strength. After washing, fourier transform infrared (FTIR) spectroscopy was performed on both washed and unwashed samples and the results were compared. This experiment has shown that there are no significant variations in the spectra of poly(p-phenylene-benzimidazole-terephthalamide-co-p-phenylene terephthalamide) (PBIA-co-PPTA1) and PBIA-co-PPTA3 after washing, and only a small variation in intensity for PBIA. This indicates that the acetone and methanol rinses are not adversely affecting the fibers and causing chemical degradation. Additionally, single fiber tensile testing was performed on the washed fibers to characterize their initial tensile strength and strain to failure, and compare those to other reported values. Iterative procedural development was necessary to find a successful method for performing tensile testing on these fibers.

The primary goal of the study is to develop a protocol to prepare consistent specimens for accurate mechanical testing of high strength copolymer aramid fibers, by removing a coating and disentangling the individual fiber strands without introducing significant chemical or physical degradation.

그들의 기계적 특성의 결정 수 있도록 고 강도 공중 합체 Aramid 섬유 disentangling

Traditionally, soft body armor has been made from poly(p-phenylene terephthalamide) (PPTA) and ultra-high molecular weight polyethylene. However, to ...

Stable DNA Motifs, 1D and 2D Nanostructures Constructed from Small Circular DNA Molecules

This article presents a detailed protocol for synthesis of small circular DNA molecules, annealing of circular DNA motifs, and construction of 1D and 2D DNA nanostructures. Over decades, the rapid development of DNA nanotechnology is attributed to the use of linear DNAs as the source materials. For example, the DAO (double crossover, antiparallel, odd half-turns) tile is well-known as a building block for construction of 2D DNA lattices; the core structure of DAO is made from two linear single-stranded (ss) oligonucleotides, like two ropes making a right hand granny&#160;knot. Herein, a new type of DNA tiles called cDAO (coupled DAO) are built using a small circular ss-DNA of c64nt or c84nt (circular 64 or 84 nucleotides) as the scaffold strand and several linear ss-DNAs as the staple strands. Perfect 1D and 2D nanostructures are assembled from cDAO tiles: infinite nanowires, nanospirals, nanotubes, nanoribbons; and finite nano-rectangles. Detailed protocols are described: 1) preparation by T4 ligase and purification by denaturing PAGE (polyacrylamide gel electrophoresis) of small circular oligonucleotides, 2) annealing of stable circular tiles, followed by native PAGE analysis, 3) assembling of infinite 1D nanowires, nanorings, nanospirals, infinite 2D lattices of nanotubes and nanoribbons, and finite 2D nano-rectangles, followed by AFM (Atomic Force Microscopy) imaging. The method is simple, robust, and affordable for most labs.

This article presents a detailed protocol for T4 ligation and denaturing PAGE purification of small circular DNA molecules, annealing and native PAGE analysis of circular tiles, assembling and AFM imaging of 1D and 2D DNA nanostructures, as well as agarose gel electrophoresis and centrifugation purification of finite DNA nanostructures.

안정적인 DNA 모티프, 1d와 2D Nanostructures 작은 원형 DNA 분자에서 건설

This article presents a detailed protocol for synthesis of small circular DNA molecules, annealing of circular DNA motifs, and construction of 1D and 2D ...

Gene-therapy Inspired Polycation Coating for Protection of DNA Origami Nanostructures

DNA origami nanostructures hold an immense potential to be used for biological and medical applications. However, low-salt conditions and nucleases in physiological fluids induce denaturation and degradation of self-assembled DNA nanostructures. In non-viral gene delivery, enzymatic degradation of DNA is overcome by the encapsulation of the negatively charged DNA in a cationic shell. Herein, inspired by gene delivery advancements, a simple, one-step and robust methodology is presented for the stabilization of DNA origami nanostructures by coating them with chitosan and linear polyethyleneimine. The polycation coating efficiently protects DNA origami nanostructures in Mg-depleted and nuclease-rich media. This method also preserves the full addressability of enzyme- and aptamer-based functionalization of DNA nanostructures.

Here, a protocol for the protection of DNA origami nanostructures in Mg-depleted and nuclease-rich media using natural cationic polysaccharide chitosan and synthetic linear polyethyleneimine (LPEI) coatings is presented.

유전자 치료 DNA 종이 접기 Nanostructures의 보호를 위한 Polycation 코팅을 영감

DNA origami nanostructures hold an immense potential to be used for biological and medical applications. However, low-salt conditions and nucleases in ...