계약 DE-AC52-07NA27344에서 로렌스 리버모어 국립 연구소에 의해 미국 에너지 국의 후원하에 수행이 작품.

1. 솔루션 준비 <ol><li> 주사기 및 0.20 μm의 주사기 필터를 사용하여 에틸 락 테이트 60 g의 필터. 에틸 락 테이트에 정식 폴리 비닐 0.3 g을 넣고. 4 시간 동안 50 ℃의 오븐에 솔루션을 놓습니다. 중합체가 완전히 용해되지 않았는지 유리 병을 가볍게 흔들어. <ol><li> 이 솔루션은 흐린 또는 아직도 광 비균질성을 표시하는 경우, 다른 2 시간 동안 오븐에 유리 병을 반환합니다. 이 레시피는 통상적으로 막 두께 약 30 nm의 사용되는 0.5 중량 %의 중합체 용액에 대한 것이다. 높은 중합체 중량 함량이 해법은 두꺼운 막에 사용될 수있다. </li></ol></li><li> 20 ㎖ 용량 플라스크에 PDAC 시약 1.0 g의 무게와 탈 (DI) 물 측정 라인에 플라스크를 작성하여 PDAC 솔루션을 준비합니다. 부드럽게 저장 용기로 전환하기 전에 용액 소용돌이 친다. </li></ol> 2. 기판 준비 <ol><li> 주의. 진한 황산 60ml를 붓고깨끗하고 250 mL의 비커에 산. 천천히 30 % 과산화수소 20 ㎖를 추가한다. 가라 발연, 부드럽게 솔루션을 소용돌이 때까지 기다립니다. 용액 및 비이커는 매우 뜨거워 질 것이며, 혼합물은 부식성. </li><li> 핫 플레이트에 150mm 페트리 접시를 놓고 접시에 산을 붓는다. 100 ℃로 핫 플레이트를 설정합니다. <ol><li> 연마면을 위로 산에 4 &#39;실리콘 웨이퍼를 놓습니다. 부드럽게 표면 전체가 침수되어 있는지 확인하기 위해 핀셋 한 쌍의 중간에 웨이퍼를 아래로 밀어 넣습니다. 30 분 동안 산에 웨이퍼를 남겨주세요. </li></ol></li><li> 핀셋으로 산에서 웨이퍼를 제거하고 전면을 씻어 내고 다시 웨이퍼의 철저하게 탈 이온수와 함께 물총 병에서. 물은 규칙적인 패턴으로 시트를 해제해야합니다. 클린 벤치에서 웨이퍼를 건조. </li><li> 필터를 장착, 주사기에 액체를 그림으로써 PDAC 용액으로 한 후 3 ㎖의 일회용 주사기 및 DI 워터와 제 0.2 ㎛의 필터 및 린스 및N 필터를 통해 액체를 밀어. </li><li> 스핀 코터의 청소 웨이퍼를 탑재합니다. 주사기에 PDAC 솔루션의 최대 1.0-1.2 ml의를 그리고 웨이퍼의 중간 위에 필터 비록 분배. 15 초 동안 4,000 rpm에서 스핀 후 (50 ° C로 예열) 핫 플레이트에 웨이퍼를 전송하고 30 초 동안 앉아 보자. </li><li> 탈 이온수로 건조 PDAC 층을 씻어 클린 벤치에서 웨이퍼를 건조하게 할 수 있습니다. </li></ol> 3. 영화 제작 <ol><li> 스핀 코터에 건조 PDAC 처리 된 웨이퍼를 놓습니다. </li><li> 3 ㎖의 일회용 주사기 및 2.4의 절차를 사용하여 에틸 락 테이트 용액)을 0.45 ㎛의 필터를 헹군다. </li><li> 입금 후 200 rpm에서 10 초 동안 웨이퍼와 스핀의 중간에 주사기 필터를 통해 에틸 락 테이트 용액 2.5 ml를, 1,700 RPM (원하는 필름 두께에 따라 다름)에 3 초 동안. 웨이퍼에 균일 한 액체 필름이 있어야한다. </li><li> 스핀 코터의 필름 건조하자은 (일반적으로 10 ~ 15 분) 눈에 띄게 건조 될 때까지, 다음 10 분 동안 (50 ° C로 예열) 열판에 놓습니다. </li><li> , 리프트 오프를 위해 일반적으로 2cm × 2 ㎝의 작은 사각형으로 필름을 주사위, 그러나 사용 필름 홀더 (3.5.1-3.5.2)의 크기에 따라 커질 수있다. 또한, 웨이퍼 크기의 필름 (3.5.3)을 탈착하는 두 서기관을합니다. 참고 : 표준 필름 홀더는 중간에 13mm 직경의 원형 개구, 19 X 19mm이다. 웨이퍼 크기의 필름을 위해, &quot;웨이퍼 (1)보다도 작은 직경 인 와이어 후프 (원형으로 형성된 예를 들어, 스테인레스 스틸 와이어)를 사용한다. 필름은 일반적으로 리프트 오프 팽윤 중에 수분을 흡수하기 때문에 원형 개구부가 선택된다. 필름 홀더에 건조 된 바와 같이, 물을 제거하고, 필름은 수축한다. 원형 개방 스트레스도 배포 할 수 있습니다. <ol><li> 절단 템플릿에 웨이퍼를 놓습니다. 바로 전자를 방지하기 위해 모든 가장자리가 웨이퍼보다 키가되는 사각형 템플릿을 사용DGE는 웨이퍼에 접촉 크라이 빙 동안 블레이드를 안내하는 데 사용됩니다. 다이 싱시 직선 에지의 배치를 안내하기 위해 2cm 간격으로 가장자리를 표시한다. 그것을 정렬이 가장자리에 웨이퍼를 밀어 넣습니다. </li><li> 두 정렬 마크를 따라 직선을 배치, 필름을 스크라이브하는 직선 가장자리를 따라 조심스럽게 면도날을 그립니다. 필름을 표시하기에 충분한 압력을 적용하지만, 너무 많이하지 웨이퍼 자체를 표시하고 입자를 생성 할 수 있습니다. 두꺼운 필름에서 절단 선이 명확하게 볼 수 있습니다. </li><li> 웨이퍼에서 한 장에 영화를 발사하기 위해, 면도날과 웨이퍼 가장자리를 스크라이브. 웨이퍼상의 두 플랫 사이 랙 - 피니언 상에 웨이퍼를 클램핑 충분히 넓은 스트립을 스크라이브. </li></ol></li><li> 탈 이온수와 190 X 100mm 배양 접시를 채우십시오. 틸트 스테이지에 장착 된 랙과 피니언에 의한 대형 평면 웨이퍼 클램프 천천히 DI 워터로 저하. 이 영화는 물 라인에서 웨이퍼로부터 분리해야한다. <ol><li> 웹 애플리케이션 방화벽을 낮추는 계속오히려 물 선 아래 리프트 오프 (lift-off) 인터페이스를 추진하는 것보다, 웨이퍼로부터 분리 필름 충분한 시간을 제공하는 속도로 어. 제곱의 첫 번째 행이 웨이퍼로부터 분리하고 표면 상에 부유 할 때, 웨이퍼의 저하를 일시. 필름이 완전히 분리 될 때까지 웨이퍼 크기의 필름의 경우, 웨이퍼를 침지 계속한다. </li><li> 물에 필름 홀더의 머리를 담그고 필름 아래로 이동합니다. 필름 가장자리 중 하나 후프의 손잡이 끝을 라인과 필름 후프를 터치합니다. 성공하면,이 영화는 후프에 충실 할 것이다. <ol><li> 웨이퍼 크기의 필름, 멀리 가장자리에서 스 크라이 빙 섹션 아래에 와이어 후프, 단지 센티미터를 놓습니다. 후프, 캡처를 시작하는 영화는 후프 감싸는 자체에 다시 접을 수 있도록 필름 가장자리와 후프 가장자리 사이에 약간의 거리를 유지하기 전에 필름 아래 중앙에 있는지 확인합니다. </li></ol></li><li> 에서 물에서 천천히 후프 후퇴35 °의 각도. 아주 천천히 물 밖으로 필름을 들어 올립니다. 주 : 필름의 약 절반 (물 표면에, 즉, 표준)이 거의 90 °로 물에서 뽑은 후 20nm 이하 후막 들어, 홀더를 통해 필름을 당기는 피하기 위해 각도를 증가시킨다. 리프트 아웃 각도를 변경하는 경우, 후프를 통해 필름을 당겨 피하기 위해 천천히 않습니다. </li><li> 후프가 완전히 수축되면, 건조 옆에 놓습니다. 확인 후프의 바닥이 아래로 후프를 놓기 전에 상품이 없는지 확인하고, 후프와 표면 사이에 액체 밀봉을 만들지 않도록 (예 : 웨이퍼 트레이 등) 곡면을 사용합니다. </li><li> 더 스크라이브 사각형 웨이퍼 상에 남아있는 경우, 물에 웨이퍼를 낮추는 단계를 계속 반복 3.6.1-3.6.4 상기 나머지에 대한 제곱. </li><li> 필름을 건조 O / N을 보자. </li></ol></li></ol>

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T. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Automated+Process+for+Improved+Uniformity+and+Versatility+of+Layer-by-Layer+Deposition.">Automated Process for Improved Uniformity and Versatility of Layer-by-Layer Deposition.</a> Langmuir. 23, 3137-3141 (2007).</li><li>Hall, D. B., Underhill, P., Torkelson, J. M. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Spin+coating+of+thin+and+ultrathin+polymer+films.">Spin coating of thin and ultrathin polymer films.</a> Polymer Engineering &amp; Science. 38, 2039-2045 (1998).</li></ol>

저자가 공개하는 게 없다.

PDAC 기판 처리는. 쉽게 부정적 (예를 들어, 실리콘 또는 유리) 충전이 제공 처리 할 수있는 크기의 기판을 의미, 자기 제한 정전 기적 ​​상호 작용을 기반으로 1-2 13cm까지 매우 큰 박막 (표시도됩니다 직경)만을 변화 사용한 시약의 부피로 되,이 프로토콜을 이용하여 제조. 궁극적 인 달성 크기에만 증착 및 박리 장치 또는 프리 스탠딩 구조를 제조하는데 사용되는 ...

프리 스탠딩 얇은 폴리머 필름은 5-8. 센서의 MEMS 1-3, 또는 촉매를 여과, 4 및 조직 공학을 포함한 다양한 애플리케이션에 사용된다 또한 한정하에 중합체의 기본적인 동작을 탐색 연구에 사용된다. 9- 13 프리 스탠딩 필름은 환형 링 또는 실리콘 웨이퍼 또는 유리 슬라이드 반대로 후프 같이 불연속 기판 상에지지되는 것이다. 이 작업은 큰 면적의 필름 또는 높은 처리량의 생산에 적합하다 초박막 독립 중합체 필름에 대한 간단한 반복적 인 제조 과정을 설명한다. 이 폴리 (비닐 형식), 폴리스티렌, 및 폴리 (메틸 메타 크릴 레이트)를 포함한 다른 중합체의 종류와 호환된다. 이는 13 cm의 직경만큼 클 또는 10 내지만큼 얇다 프리 스탠딩 필름을 제조하는데 사용될 수있다. 무료 서 중합체의 제조는 세 가지 기본 단계로 구성 : 1) D기존의 기판 상에 고분자 필름의 eposition 같은 지지체 상에 웨이퍼 또는 슬라이드, 2) 분리 또는 기판으로부터 막 발사, 얻어진 막의 3)로서 캡처. 이 논문은 우리가 다양한 릴리스 방법에 대한 이전 연구에서보고 된 방법에 대해 설명합니다. (14) 증착은 예컨대 스핀 코팅, 증착, 또는 딥 - 코팅과 같은 염기성 중합체 박막 기술의 임의의 수에 의해 달성 될 수있다. 이 작품에서 우리는 표준 스핀 코팅 기술을 사용한다. 기술 &quot;에 리프트 오프 플로트는&quot;적당한 용매 욕조에 몰입이 기술, 필름 및 기판에서 가장 흔한 그 기판에서 얇은 필름을 해제하는 방법. 15입니다. 용매가 필름을 팽윤하고, 필름을 해제하고 욕의 상단에 떠 있도록 자발적 박리를 유도한다. 최소 막 두께 수리프트를 사용하여 출시 오프 플로트 팽창에 의한 변형 에너지와 계면 박리 에너지의 균형에 의해 결정됩니다에 : 16 <img alt="식 (1)" src="/files/ftp_upload/52832/52832eq1.jpg" width="200" /> (1) L은 막 두께이고, ν의 f는 필름의 포아송 비, E는 필름의 영률이다, ξ는 막의 팽윤 율이고, γ는 박리 계면 에너지이다. 수학 식에 의해 부과 된 제한을 우회하는 전형적인 방법은 (1) 필름과 증착 기판 사이에 희생 층간을 증착하는 것이다. 17-20이 층간 용매 욕에 용해하는 경우, 필름은 해제되고 지지체 상에 캡처 할 수있다 . 관련된 방법은, 희생 층 (PR) 상으로 필름의 기계적 박리를 이용하는 희생 오버 방법이며용해에 IOR. (21) 희생 물질의 사용은 몇 개의 주요한 단점을 가지고있다. 첫째, 별도의 공정 단계 및 물질의 첨가는 최적의 막 제조 조건으로 희생 물질 처리 조건 간의 타협을 필요로 할 수있다. 두 번째로, 희생 재료는 최종 프리 스탠딩 필름의 기계적 특성이나 순도에 영향을주지 않으면 서 증착하기 어려울 수있다. 셋째, 희생 물질을 증착하기위한 프로세스 최적화 전체 프리 스탠딩 필름 제조에 대해 동작으로서 모니터되어야한다. (14) 이 작품에서 우리는 얇은 필름에 사용되는 오프 플로트 기술에 리프트를 가능하게, 계면 박리 에너지를 감소 표면 개질 기술에 대해 설명합니다. 퇴적 기판은, 폴리 양이온의 polydiallyldiammonium 클로라이드 (PDAC)의 자기 한정자가 최적화 가까운 조립 단분자층에 의해 수정된다. 때문에의폴리 양이온과 기판 사이의 결합 강도는, 이러한 표면 개질은 후속 공정 단계에 강하다. 거의 단층의 형성과 자기 - 제한자가 최적화 특성은 실질적으로 제로의 최적화가 필요하고 큰 영역에 용이하게 확장 가능하다. 제거 후, ​​영화는 후프와 같은 지원에 포착되는 용매 목욕의 정상에 수레. 현존 문헌에 많은 관심을 부여하는 것은 아니지만, 본 연구에서 우리는 찢어짐 또는 다른 손상을 막을 확률을 감소 지지부에 대 면적의 박막을 캡쳐하는 기술을 설명한다.

<table border="0" cellpadding="0" cellspacing="0">
	<tbody>
		<tr>
			<td>Vinylec E</td>
			<td>SPI</td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>ethyl lactate, &#62;98%, FCC, FG,</td>
			<td>Sigma-Aldrich</td>
			<td>W244007-1KG-K</td>
			<td></td>
		</tr>
		<tr>
			<td>4&#34; silicon wafers &#60;100&#62;, Single side polished</td>
			<td>International Wafer Service</td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>sulfuric acid, 98%, ACS reagent grade</td>
			<td>Sigma-Aldrich</td>
			<td>320501-6X500ML</td>
			<td></td>
		</tr>
		<tr>
			<td>hydrogen peroxide, 30%, semiconductor grade</td>
			<td>Sigma-Aldrich</td>
			<td>316989-3.7L</td>
			<td></td>
		</tr>
		<tr>
			<td>isopropanol, ACS grade, 4 L</td>
			<td>Fisher Scientific</td>
			<td>A464-4</td>
			<td></td>
		</tr>
		<tr>
			<td>dichloromethane, ACS grade</td>
			<td>Alfa-Aesar</td>
			<td>22917</td>
			<td></td>
		</tr>
		<tr>
			<td>deionized water , distilled</td>
			<td></td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>PDAC reagent (Sigma-Aldrich 409014)</td>
			<td>Sigma-Aldrich</td>
			<td>409014</td>
			<td></td>
		</tr>
		<tr>
			<td>Spin Coater</td>
			<td>Laurell Technologies&#160;</td>
			<td>WS-650-23</td>
			<td></td>
		</tr>
		<tr>
			<td>Barnstead/Thermolyne Super Nuova explosion-proof hot plate&#160;</td>
			<td></td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>explosion-proof forced air oven</td>
			<td>VWR&#160;</td>
			<td>1330 FMS&#160;</td>
			<td></td>
		</tr>
		<tr>
			<td>balance with a range of 1 mg to 1020 g</td>
			<td>Mettler Toledo</td>
			<td>MS1003S</td>
			<td></td>
		</tr>
		<tr>
			<td>reflectance spectrometer</td>
			<td>Filmetrics</td>
			<td>F20-UV</td>
			<td></td>
		</tr>
		<tr>
			<td>manipulator consisting of a Klinger tilt stage, a Brinkman rack-and-pinion and a lab jack&#160;</td>
			<td></td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>Cutting tool/template, LLNL-built, no drawings</td>
			<td></td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>straight edge, LLNL, no drawings</td>
			<td></td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>Tent hoop, LLNL</td>
			<td></td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>culture dish 190 mm x 100 mm, Pyrex</td>
			<td>VWR</td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>20 ml beaker, Pyrex</td>
			<td>VWR</td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>250 ml beaker, Pyrex</td>
			<td>VWR</td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>1000 ml beaker, Pyrex</td>
			<td>VWR</td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>60 ml glass vial with plastic stopper&#160;</td>
			<td>VWR</td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>petri dish, 150 mm diameter x2, Pyrex</td>
			<td>VWR</td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>600 ml beaker x2, Pyrex</td>
			<td>VWR</td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>tweezers, stainless steel</td>
			<td></td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>cutting blade</td>
			<td>Exacto</td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>clean room wipes</td>
			<td>Contec&#160;</td>
			<td>PNHS-99</td>
			<td></td>
		</tr>
		<tr>
			<td>polyester knit 9/91 IPA/DI water wipes</td>
			<td>Contec&#160;</td>
			<td>Prosat&#160;</td>
			<td></td>
		</tr>
		<tr>
			<td>Fluoroware wafer trays</td>
			<td>Ted Pella</td>
			<td>1395-40</td>
			<td></td>
		</tr>
		<tr>
			<td>Nylon Micro fiber (camel hair)</td>
			<td></td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>Disposable BD 3-mL plastic syringe</td>
			<td>VWR</td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>0.2 um&#160; Luer-lock PTFE filters</td>
			<td>Acrodisc&#160;</td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>0.45 um&#160; Luer-lock PTFE filters</td>
			<td>Acrodisc&#160;</td>
			<td></td>
			<td></td>
		</tr>
	</tbody>
</table>

fabrication of large-area free-standing ultrathin polymer films

This procedure describes a method for the fabrication of large-area and ultrathin free-standing polymer films. Typically, ultrathin films are prepared using either sacrificial layers, which may damage the film or affect its mechanical properties, or they are made on freshly cleaved mica, a substrate that is difficult to scale. Further, the size of ultrathin film is typically limited to a few square millimeters. In this method, we modify a surface with a polyelectrolyte that alters the strength of adhesion between polymer and deposition substrate. The polyelectrolyte can be shown to remain on the wafer using spectroscopy, and a treated wafer can be used to produce multiple films, indicating that at best minimal amounts of the polyelectrolyte are added to the film. The process has thus far been shown to be limited in scalability only by the size of the coating equipment, and is expected to be readily scalable to industrial processes. In this study, the protocol for making the solutions, preparing the deposition surface, and producing the films is described.

도 1은 대 면적 독립 얇은 폴리머 필름의 예를 나타낸다. 이 55 nm 두께의 폴리 비닐 포르 막이 여기에 설명 된 절차와 13-cm 직경의 강철 후프에 장착하여 제조 하였다. 라미네이션 필름 찢어 이어질 결함을 도입하지 않고 넓은 영역에 걸쳐 발생한다. 따라서, 폴리 비닐 포르의 극한 강도는 매우 얇은 막에 대해서도 이용 될 수있다.도 2는 중&gt; 3 × 5 배 질량 무게 시?...

Watch this Scientific Journal Video about Fabrication of Large-area Free-standing Ultrathin Polymer Films at JoVE.com

Fabrication of Large-area Free-standing Ultrathin Polymer Films

We describe a method for the fabrication of large-area (up to 13 cm diameter) and ultrathin (as thin as 8 nm) polymer films. Instead of using a sacrificial interlayer to delaminate the film from its substrate, we use a self-limiting surface treatment suitable for arbitrarily large areas.

대 면적의 제작은 초박막 고분자 필름을 무료 서

This procedure describes a method for the fabrication of large-area and ultrathin free-standing polymer films.  Typically, ultrathin films are prepared ...

fabrication-of-large-area-free-standing-ultrathin-polymer-films

Research

JoVE Journal

Chemistry

15.2K 조회수.  Lawrence Livermore National Laboratory. We describe a method for the fabrication of large-area (up to 13 cm diameter) and ultrathin (as thin as 8 nm) polymer films. Instead of using a sacrificial interlayer to delaminate the film from its substrate, we use a self-limiting surface treatment suitable for arbitrarily large areas.

비디오: Fabrication of Large-area Free-standing Ultrathin Polymer Films

Towards Biomimicking Wood: Fabricated Free-standing Films of Nanocellulose, Lignin, and a Synthetic Polycation

Woody materials are comprised of plant cell walls that contain a layered secondary cell wall composed of structural polymers of polysaccharides and lignin. Layer-by-layer (LbL) assembly process which relies on the assembly of oppositely charged molecules from aqueous solutions was used to build a freestanding composite film of isolated wood polymers of lignin and oxidized nanofibril cellulose (NFC). To facilitate the assembly of these negatively charged polymers, a positively charged polyelectrolyte, poly(diallyldimethylammomium chloride) (PDDA), was used as a linking layer to create this simplified model cell wall. The layered adsorption process was studied quantitatively using quartz crystal microbalance with dissipation monitoring (QCM-D) and ellipsometry. The results showed that layer mass/thickness per adsorbed layer increased as a function of total number of layers. The surface coverage of the adsorbed layers was studied with atomic force microscopy (AFM). Complete coverage of the surface with lignin in all the deposition cycles was found for the system, however, surface coverage by NFC increased with the number of layers. The adsorption process was carried out for 250 cycles (500 bilayers) on a cellulose acetate (CA) substrate. Transparent free-standing LBL assembled nanocomposite films were obtained when the CA substrate was later dissolved in acetone. Scanning electron microscopy (SEM) of the fractured cross-sections showed a lamellar structure, and the thickness per adsorption cycle (PDDA-Lignin-PDDA-NC) was estimated to be 17 nm for two different lignin types used in the study. The data indicates a film with highly controlled architecture where nanocellulose and lignin are spatially deposited on the nanoscale (a polymer-polymer nanocomposites), similar to what is observed in the native cell wall.

The objective of this research was to form synthetic plant cell wall tissue using layer-by-layer assembly of nanocellulose fibrils and isolated lignin assembled from dilute aqueous suspensions.&#160; Surface measurement techniques of quartz crystal microbalance and atomic force microscopy were used to monitor the formation of the polymer-polymer nanocomposite material.

Nanocellulose, 리그닌의 날조 된 자립형 필름, 및 합성 폴리 양이온 : Biomimicking 나무를 향하여

Woody materials are comprised of plant cell walls that contain a layered secondary cell wall composed of structural polymers of polysaccharides and ...

연구

화학

Confocal Imaging of Confined Quiescent and Flowing Colloid-polymer Mixtures

The behavior of confined colloidal suspensions with attractive interparticle interactions is critical to the rational design of materials for directed assembly1-3, drug delivery4, improved hydrocarbon recovery5-7, and flowable electrodes for energy storage8. Suspensions containing fluorescent colloids and non-adsorbing polymers are appealing model systems, as the ratio of the polymer radius of gyration to the particle radius&#160;and concentration of polymer control the range and strength of the interparticle attraction, respectively. By tuning the polymer properties and the volume fraction of the colloids, colloid fluids, fluids of clusters, gels, crystals, and glasses can be obtained9.&#160;Confocal microscopy, a variant of fluorescence microscopy, allows an optically transparent and fluorescent sample to be imaged with high spatial and temporal resolution in three dimensions. In this technique, a small pinhole or slit blocks the emitted fluorescent light from regions of the sample that are outside the focal volume of the microscope optical system. As a result, only a thin section of the sample in the focal plane is imaged. This technique is particularly well suited to probe the structure and dynamics in dense colloidal suspensions at the single-particle scale: the particles are large enough to be resolved using visible light and diffuse slowly enough to be captured at typical scan speeds of commercial confocal systems10. Improvements in scan speeds and analysis algorithms have also enabled quantitative confocal imaging of flowing suspensions11-16,37.&#160;In this paper, we demonstrate confocal microscopy experiments to probe the confined phase behavior and flow properties of colloid-polymer mixtures. We first prepare colloid-polymer mixtures that are density- and refractive-index matched. Next, we report a standard protocol for imaging quiescent dense colloid-polymer mixtures under varying confinement in thin wedge-shaped cells. Finally, we demonstrate a protocol for imaging colloid-polymer mixtures during microchannel flow.

Confocal microscopy is used to image quiescent and flowing colloid-polymer mixtures, which are studied as model systems for attractive suspensions. Image analysis algorithms are used to calculate structural and dynamic metrics for the colloidal particles that measure changes due to geometric confinement.

밀폐 무부하 흐르는 콜로이드 중합체 혼합물의 공 촛점 이미징

The behavior of confined colloidal suspensions with attractive interparticle interactions is critical to the rational design of materials for directed ...

Preparation of Highly Porous Coordination Polymer Coatings on Macroporous Polymer Monoliths for Enhanced Enrichment of Phosphopeptides

We describe a protocol for the preparation of hybrid materials based on highly porous coordination polymer coatings on the internal surface of macroporous polymer monoliths. The developed approach is based on the preparation of a macroporous polymer containing carboxylic acid functional groups and the subsequent step-by-step solution-based controlled growth of a layer of a porous coordination polymer on the surface of the pores of the polymer monolith. The prepared metal-organic polymer hybrid has a high specific micropore surface area. The amount of iron(III) sites is enhanced through metal-organic coordination on the surface of the pores of the functional polymer support. The increase of metal sites is related to the number of iterations of the coating process.
The developed preparation scheme is easily adapted to a capillary column format. The functional porous polymer is prepared as a self-contained single-block porous monolith within the capillary, yielding a flow-through separation device with excellent flow permeability and modest back-pressure. The metal-organic polymer hybrid column showed excellent performance for the enrichment of phosphopeptides from digested proteins and their subsequent detection using matrix-assisted laser desorption/ionization time-of-flight mass spectrometry. The presented experimental protocol is highly versatile, and can be easily implemented to different organic polymer supports and coatings with a plethora of porous coordination polymers and metal-organic frameworks for multiple purification and/or separation applications.

A procedure for the preparation of porous hybrid separation media composed of a macroporous polymer monolith internally coated by a high surface area microporous coordination polymer is presented.

포스 포의 향상된 농축을위한 거대 다공성 고분자 모노리스에 다공성 조정 폴리머 코팅의 제조

We describe a protocol for the preparation of hybrid materials based on highly porous coordination polymer coatings on the internal surface of macroporous ...

Photodynamic Therapy with Blended Conducting Polymer/Fullerene Nanoparticle Photosensitizers

In this article a method for the fabrication and reproducible in-vitro evaluation of conducting polymer nanoparticles blended with fullerene as the next generation photosensitizers for Photodynamic Therapy (PDT) is reported. The nanoparticles are formed by hydrophobic interaction of the semiconducting polymer MEH-PPV (poly[2-methoxy-5-(2-ethylhexyloxy)-1,4-phenylenevinylene]) with the fullerene PCBM (phenyl-C61-butyric acid methyl ester) in the presence of a non-compatible solvent. MEH-PPV has a high extinction coefficient that leads to high rates of triplet formation, and efficient charge and energy transfer to the fullerene PCBM. The latter processes enhance the efficiency of the PDT system through fullerene assisted triplet and radical formation, and ultrafast deactivation of MEH-PPV excited stated. The results reported here show that this nanoparticle PDT sensitizing system is highly effective and shows unexpected specificity to cancer cell lines.

This protocol describes a method for the fabrication of conducting polymer nanoparticles blended with fullerene. These nanoparticles were investigated for their potential use as a next generation photosensitizers for Photodynamic Therapy (PDT).

혼합 폴리머 / 풀러렌 나노 입자 감광제를 실시와 광 역학 치료

In this article a method for the fabrication and reproducible in-vitro evaluation of conducting polymer nanoparticles blended with fullerene as the next ...

Cooling Rate Dependent Ellipsometry Measurements to Determine the Dynamics of Thin Glassy Films

This report aims to fully describe the experimental technique of using ellipsometry for cooling rate dependent Tg (CR-Tg) experiments. These measurements are simple high-throughput characterization experiments, which can determine the glass transition temperature (Tg), average dynamics, fragility and the expansion coefficient of the super-cooled liquid and glassy states for a variety of glassy materials. This technique allows for these parameters to be measured in a single experiment, while other methods must combine a variety of different techniques to investigate all of these properties. Measurements of dynamics close to Tg are particularly challenging. The advantage of cooling rate dependent Tg measurements over other methods which directly probe bulk and surface relaxation dynamics is that they are relatively quick and simple experiments, which do not utilize fluorophores or other complicated experimental techniques. Furthermore, this technique probes the average dynamics of technologically relevant thin films in temperature and relaxation time (&#964;&#945;) regimes relevant to the glass transition (&#964;&#945; &#62; 100 sec). The limitation to using ellipsometry for cooling rate dependent Tg experiments is that it cannot probe relaxation times relevant to measurements of viscosity (&#964;&#945; &#60;&#60; 1 sec). Other cooling rate dependent Tg measurement techniques, however, can extend the CR-Tg method to faster relaxation times. Furthermore, this technique can be used for any glassy system so long as the integrity of the film remains throughout the experiment.

Here, we present a protocol for cooling rate dependent ellipsometry experiments, which can determine the glass transition temperature (Tg), average dynamics, fragility and the expansion coefficient of the super-cooled liquid and glass for a variety of glassy materials.

속도 종속 엘립 소메 트리 측정 냉각 얇은 유리 필름의 역학을 확인하는

This report aims to fully describe the experimental technique of using ellipsometry for cooling rate dependent Tg (CR-Tg) experiments. These measurements ...

The Preparation and Properties of Thermo-reversibly Cross-linked Rubber Via Diels-Alder Chemistry

A method for using Diels Alder thermo-reversible chemistry as cross-linking tool for rubber products is demonstrated. In this work, a commercial ethylene-propylene rubber, grafted with maleic anhydride, is thermo-reversibly cross-linked in two steps. The pending anhydride moieties are first modified with furfurylamine to graft furan groups to the rubber backbone. These pendant furan groups are then cross-linked with a bis-maleimide via a Diels-Alder coupling reaction. Both reactions can be performed under a broad range of experimental conditions and can easily be applied on a large scale. The material properties of the resulting Diels-Alder cross-linked rubbers are similar to a peroxide-cured ethylene/propylene/diene rubber (EPDM) reference. The cross-links break at elevated temperatures (&#62; 150 &#176;C) via the retro-Diels-Alder reaction and can be reformed by thermal annealing at lower temperatures (50-70 &#176;C). Reversibility of the system was proven with infrared spectroscopy, solubility tests and mechanical properties. Recyclability of the material was also shown in a practical way, i.e., by cutting a cross-linked sample into small parts and compression molding them into new samples displaying comparable mechanical properties, which is not possible for conventionally cross-linked rubbers.

A simple two-step approach involving rubber modification and cross-linking yields fully reworkable, elastic rubber products.

열 가역적 가교 고무 통해 딜스 - 알더 화학의 준비 및 등록

A method for using Diels Alder thermo-reversible chemistry as cross-linking tool for rubber products is demonstrated. In this work, a commercial ...

Capillary Electrophoresis to Monitor Peptide Grafting onto Chitosan Films in Real Time

Free-solution capillary electrophoresis (CE) separates analytes, generally charged compounds in solution through the application of an electric field. Compared to other analytical separation techniques, such as chromatography, CE is cheap, robust and effectively requires no sample preparation (for a number of complex natural matrices or polymeric samples). CE is fast and can be used to follow the evolution of mixtures in real time (e.g., chemical reaction kinetics), as the signals observed for the separated compounds are directly proportional to their quantity in solution.
Here, the efficiency of CE is demonstrated for monitoring the covalent grafting of peptides onto chitosan films for subsequent biomedical applications. Chitosan&#39;s antimicrobial and biocompatible properties make it an attractive material for biomedical applications such as cell growth substrates. Covalently grafting the peptide RGDS (arginine - glycine - aspartic acid - serine) onto the surface of chitosan films aims at improving cell attachment. Historically, chromatography and amino acid analysis have been used to provide a direct measurement of the amount of grafted peptide. However, the fast separation and absence of sample preparation provided by CE enables equally accurate yet real-time monitoring of the peptide grafting process. CE is able to separate and quantify the different components of the reaction mixture: the (non-grafted) peptide and the chemical coupling agents. In this way the use of CE results in improved films for downstream applications.
The chitosan films were characterized through solid-state NMR (nuclear magnetic resonance) spectroscopy. This technique is more time-consuming and cannot be applied in real time, but yields a direct measurement of the peptide and thus validates the CE technique.

Free solution capillary electrophoresis is a fast, cheap and robust analytical method that enables the quantitative monitoring of chemical reactions in real time. Its utility for rapid, convenient and precise analysis is demonstrated here through analysis of covalent peptide grafting onto chitosan films for improved cell adhesion.

모세관 전기 영동은 실시간으로 키토산 필름에 펩타이드 접목을 모니터링하는

Free-solution capillary electrophoresis (CE) separates analytes, generally charged compounds in solution through the application of an electric field. ...

Microfluidic Dry-spinning and Characterization of Regenerated Silk Fibroin Fibers

The protocol demonstrates a method for mimicking the spinning process of silkworm. In the native spinning process, the contracting spinning duct enables the silk proteins to be compact and ordered by shearing and elongation forces. Here, a biomimetic microfluidic channel was designed to mimic the specific geometry of the spinning duct of the silkworm. Regenerated silk fibroin (RSF) spinning doped with high concentration, was extruded through the microchannel to dry-spin fibers at ambient temperature and pressure. In the post-treated process, the as-spun fibers were drawn and stored in ethanol aqueous solution. Synchrotron radiation wide-angle X-ray diffraction (SR-WAXD) technology was used to investigate the microstructure of single RSF fibers, which were fixed to a sample holder with the RSF fiber axis normal to the microbeam of the X-ray. The crystallinity, crystallite size, and crystalline orientation of the fiber were calculated from the WAXD data. The diffraction arcs near the equator of the two-dimensional WAXD pattern indicate that the post-treated RSF fiber has a high orientation degree.

A protocol for the microfluidic spinning and microstructure characterization of regenerated silk fibroin monofilament is presented.

미세 드라이 회전 및 재생성된 실크 Fibroin 섬유의 특성

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

Time-resolved Photophysical Characterization of Triplet-harvesting Organic Compounds at an Oxygen-free Environment Using an iCCD Camera

Here, we present a sensible method of the acquisition and analysis of time-resolved photoluminescence using an ultrafast iCCD camera. This system enables the acquisition of photoluminescence spectra covering the time regime from nanoseconds up to 0.1 s. This enables us to follow the changes in the intensity (decay) and emission of the spectra over time. Using this method, it is possible to study diverse photophysical phenomena, such as the emission of phosphorescence, and the contributions of prompt and delayed fluorescence in molecules showing thermally activated delayed fluorescence (TADF). Remarkably, all spectra and decays are obtained in a single experiment. This can be done for solids (thin film, powder, crystal) and liquid samples, where the only limitations are the spectral sensitivity of the camera and the excitation wavelength (532 nm, 355 nm, 337 nm, and 266 nm). This technique is, thus, very important when investigating the excited state dynamics in organic emitters for their application in organic light-emitting diodes and other areas where triplet harvesting is of paramount importance. Since triplet states are strongly quenched by oxygen, emitters with efficient TADF luminescence, or those showing room temperature phosphorescence (RTP), must be correctly prepared in order to remove any dissolved oxygen from solutions and films. Otherwise, no long-lived emission will be observed. The method of degassing solid samples as presented in this work is basic and simple, but the degassing of liquid samples creates additional difficulties and is particularly interesting. A method of minimizing solvent loss and changing the sample concentration, while still enabling to remove oxygen in a very efficient and a repeatable manner, is presented in this work.

Here, we present a method of the spectroscopic characterization of organic molecules by means of time-resolved photoluminescence spectroscopy on the nanosecond-to-millisecond timescale in oxygen-free conditions. Methods to efficiently remove oxygen from the samples and, thus, limit luminescence quenching are also described.

Here, we present a sensible method of the acquisition and analysis of time-resolved photoluminescence using an ultrafast iCCD camera. This system enables ...

Raman and IR Spectroelectrochemical Methods as Tools to Analyze Conjugated Organic Compounds

In the presented work, two spectroelectrochemical techniques are discussed as tools for the analysis of the structural changes occurring in the molecule on the vibrational level of energy. Raman and IR spectroelectrochemistry can be used for advanced characterization of the structural changes in the organic electroactive compounds. Here, the step-by-step analysis by means of Raman and IR spectroelectrochemistry is shown. Raman and IR spectroelectrochemical techniques provide complementary information about structural changes occurring during an electrochemical process, i.e. allows for the investigation of redox processes and their products. The examples of IR and Raman spectroelectrochemical analysis are presented, in which the products of the redox reactions, both in solution and solid state, are identified.

A protocol of step-by-step Raman and IR spectroelectrochemical analysis is presented.

In the presented work, two spectroelectrochemical techniques are discussed as tools for the analysis of the structural changes occurring in the molecule ...