C.R.C. would like to acknowledge the Ramsay Memorial Trust for funding.

의 CdSe /의 ZnS 코어 / 쉘 양자 점의 1. 준비 <ol><li> 트리 옥틸 포스 핀의 제조 (TOP) -se 솔루션 <ol><li> (8 ㎖를 일반적으로 0.4 g이 TOP 10 ㎖에 용해, 반응에 따라 필요) 질소 하에서 또는 글러브 박스에서 쉬 렌크 플라스크에 TOP에 셀레늄의 적절한 양을 혼합하여 TOP에 셀레늄의 0.5 M 용액을 준비합니다. </li><li> 상단 셀레늄 복잡 회색 용액 결과 1 시간 동안 선생을 용해 혼합물을 교반한다. </li><li> 이 솔루션은 동결 펌프 - 해동 5 회 탈기 한 후되어 있는지 확인합니다. 얻어진 원액 3 개월 동안 질소하에 저장 될 수있다. </li></ol></li><li> 의 CdSe 코어의 제조 <ol><li> 카드뮴 산화물 (51 ㎎, 0.4 밀리몰), TOP 옥사이드 (3.7 g, 9.6 밀리몰)를 달아, 헥사 데실 (1.93 g, 8 mmol) 및 1- dodecylphosphonic 산 (0.22 g, 0.88 mmol) 및 세 경부에 결합 (250) ml의 둥근 바닥 플라스크. 교반 막대를 추가합니다. </li><li> 격막 및 확인과 닫기를 두 목세 번째는 긴 환류 응축기 및 질소 / 진공 쉬 렌크 라인에 부착된다. 혼합물에 직접 하나 격막을 통해 가열 맨틀 온도 프로브를 삽입합니다. 다섯 번 / 펌프 질소 플라스크 리필. </li><li> 320 ° C까지 플라스크를 가열하고, 질소 분위기 하에서 1 시간 동안 용융 교반한다. </li><li> 질소로 큰 주사기와 넓은 구멍 바늘을 사용해서 5 회 탈기에 (20 ㎖, 3mm 구멍)를 270 ° C에 벽난로의 온도를 낮추고. </li><li> 위로 TOP-셀레늄 용액 (1.1 단계)의 8 mL를 취하여 격막을 통해 세 목 플라스크에 신중하지만 빠른 속도로 주입. </li><li> 생성 된 입자의 크기를 제어 할 분 30 초 내지 10 대 270 ℃에서 반응물을 교반한다. 적색 발광 (~ 600 ㎚)의 경우, 7-9 분에 적합하다. </li><li> 다음, 반응 혼합물 및 장소 (반응 용기의 절반을 잠수함하기에 충분히 큰) 끓는 물 그릇을 준비합니다. 반응 시간이 끝나면 신속 boili으로 반응을 냉각소용돌이 치는 물을 ng를. 주의 : 냉각은 플라스크 균열의 원인이 될 수 있습니다. 큰 관심을 가지고 두꺼운 불 침투성 장갑을 착용하십시오. </li><li> 일단 차가운, 모든 제품을 용해 플라스크에 클로로포름 10 ㎖를 주입하고, 두 개의 50 ㎖ 원심 분리 튜브의 혼합물을 분할. </li><li> 3,600 × g 10 분 각 튜브 최대의 EtOH 및 원심 분리기와 50 ㎖로 최고 최대 입자를 침전한다. 상층 액을 제거하고, n- 헥산 10 ㎖의 총 펠렛을 다시 분산. </li></ol></li><li> 의 CdSe 코어의의 ZnS 포격 : <ol><li> 100 ml의 헥산으로 코어를 추가 둥근 바닥 플라스크에 포함 된 아연 디 에틸 (0.5 g, 1.4 밀리몰), 올레 일 아민 (3 ㎖, 9.12 밀리몰), 트리 옥틸 포스 핀 (3 ㎖, 6.73 밀리몰) 및 1- 옥타 데센 (10 ㎖). 교반 막대를 추가합니다. 질소 분위기 하에서 반응을 교환한다. </li><li> 70 ° C까지 부분적인 진공 하에서 3.3 ° C / 분에서 핫 플레이트 - 교반기의 반응을 가열하고, 쉬 렌크 줄을 사용하여 헥산을 제거합니다. </li&gt; <li> 질소로 분위기를 전환하고 120 ° C까지이 속도로 가열을 계속한다. 2 시간 동안 120 ℃에서 교반 하였다. </li><li> 반응이 냉각 할 수 있도록 허용하고, 2 × 50 ML의 원심 분리기 튜브 사이의 혼합물을 분리. 튜브는 10 분 동안 3,600 × g에서 입자와 원심 분리기를 침전 EtOH로 50 ㎖까지 얹어되어 있는지 확인합니다. </li><li> 상층 액을 제거하고, n- 헥산 10 ㎖의 총 펠렛을 다시 분산. </li><li> 최대 3 개월 동안 질소 대기 하에서 냉장고 (4 ℃)에서 원심 분리 용액 (3,600 × g으로 10 분간) 샘플 튜브로 경사지기 전에, 임의의 불용성 불순물을 제거하기 위해 다시 한 번, 그리고 매장. </li></ol></li></ol> PDMS에 나노 입자의 2 붓기 캡슐화 <ol><li> 솔루션 준비 붓기 : <ol><li> 4 (합성 등)의 CdSe QD 분산액 ㎖의 n- 헥산 36 ml에 혼합 한 CdSe 양자점의 스톡 용액을 준비하고 자기 용액을 교반 하였다. &lt;/ 리&gt; <li> 별도로 두 바이알 지정 팽윤 용액으로 원액 9 mL를 함유 각각 설정한다. </li><li> QD의 농도를 변화시키는 상기 팽윤 용액의 제조 원액의 나머지 부분을 사용한다. 66 % (v / v) 용액, 50 % 용액, 33 % 용액을 수득 원액을 희석함으로써 감소 QD 농도 세 팽윤 용액을 준비한다. <ol><li> n- 헥산 3 mL로 한 CdSe QD 스톡 용액 6 ml를 혼합하여 66 % (v / v)의 용액을 제조 하였다. 완전한 혼합을 보장하기 위해 자기 용액을 교반한다. </li><li> 4.5 ㎖의 n- 헥산으로 한 CdSe QD 원액 4.5 ml를 혼합하여 50 % (v / v)의 용액을 제조 하였다. 완전한 혼합을 보장하기 위해 자기 용액을 교반한다. </li><li> n- 헥산 6 mL로 한 CdSe QD 스톡 용액 3 ㎖를 혼합하여 33 % (v / v)의 용액을 제조 하였다. 완전한 혼합을 보장하기 위해 자기 용액을 교반한다. </li></ol></li><li> 실온에서, 어두운 조건에서 QD 솔루션을 모두 저장합니다. &lt;/ 리&gt; </ol></li><li> 고분자 제조 및 QD 법인은 - 붓기 솔루션의 QD 농도를 변화 : <ol><li> 신선한 메스 블레이드를 사용하여 네 개의 의료용 실리콘 사각형 (11mm X 11mm)을 잘라. </li><li> %의 QD 농도 변화의 네 팽윤 용액 각각 의료용 실리콘 사각형 담가 : 스톡 용액, 66 % (V / V), 50 % (v / v)의 33 % (V / V). 중합체 샘플이 암 조건 하에서 24 시간 동안 팽창을 허용하고, 실온에서 첨가 하였다. </li><li> 잔류 용매의 증발과 폴리머는 다시 초기 크기로 축소이 기간 동안 48 시간에 대한 어두운 조건에서 팽창 솔루션 및 공기 건조 각각의 부어 폴리머 샘플을 제거합니다. </li><li> 어떤 표면 결합 물질을 제거하는 탈 이온수로 철저하게 QD-통합 샘플을 씻으십시오. </li></ol></li><li> 중합체 제조 및 QD 혼입 - 팽윤 중합체 용액에 노출 시간을 변화 : </strong&gt; <ol><li> 2.2.1에서 언급 한 바와 같이, 네 더 의료용 실리콘 사각형 (11mm X 11mm)를 준비합니다. </li><li> 시간 기간을 변화시키는 재고 팽윤 액 중의 의료용 실리콘 사각형 담가 1 시간, 3 시간, 6 시간, 24 시간이. </li><li> 팽윤 용액으로부터 제거 후, ​​공기는​​ 샘플이 다시 이전 크기로 축소하도록 48 시간 동안 어두운 조건에서 부어 폴리머 샘플을 건조. </li><li> 어떤 표면 결합 물질이나 잔류 용매를 제거하는 탈 이온수로 철저하게 QD-통합 샘플을 씻으십시오. </li></ol></li></ol> 나노 입자의 3 시각화 PDMS로 캡슐화 스웰 <ol><li> 실리콘 샘플 준비 : <ol><li> 신선한 메스 블레이드 (5.5 mm X 11mm) 두 개의 실리콘 사각형을 잘라. 이 실리콘 샘플의 내부 표면을 노출 있는지 확인합니다. </li></ol></li><li> 형광 이미징 : <ol><li> microsco에 실리콘 샘플을 배치폴리머의 갓 잘라면이 유리 슬라이드 전체 접촉을 보장 이미징을위한 체육 슬라이드. 현미경 슬라이드와 부드러운 접촉을 보장하기 위해 가볍게 실리콘 부분을 아래로 누릅니다. 현미경의 무대에서 샘플을 놓습니다. </li><li> 20 MHz 또는 유사한 속도로 5 PSEC 펄스로 이루어지는 488 nm의 스펙트럼을 여과 레이저 라인을 사용하여 전체 수명 형광 측정. (23)를 사용하여 음향 광학 가변 필터에있어서, 상기 레이저 출력에 직접 커플 488을 생성하기 위해서 nm의 레이저 라인. 샘플에 다음 10X 대물 렌즈의 배면 개구로 익 미러 (488 ㎚)에 의해 반사되는 맞춤형 레이저 스캐닝 유닛 (부가 정보를 참조)를 사용하여 레이저 빔을 초점. <ol><li> 다음 동일한 다이크로 익 미러를 통과 동일한 목적으로 형광 방출을 수집한다. 단일 광자 계수 모드에서 작동 눈사태 포토 다이오드를 향해이 빛을 직접. 프로세스 lifeti<html> 시간 상관 단일 광자 계산 (TCSPC) 보드를 사용하여 나 측정. (23) </li></ol></li><li> 처음에 장비 응답 함수 (IRF) 각 실험 세션 종료를 기록한다. (23) 주 : TCSPC 실험에서 기록 된 신호는 상기 검출기에서의 광자의 도착 이후의 레이저 펄스의 제조 사이의 시간 지연을 표시한다. 이 시간 지연 그러나, 측정 장치의 IRF와 컨벌루션한다. 따라서, IRF는 쓸모 응답에 비해 매우 짧은 수명 (~ 100 PSEC)이 100 nm의 오라 민 O, 악기의 응답으로서 측정된다. </li><li> 형광 강도의 감쇠 지수의 비선형 피팅에 의해 수명을 추출하여 최대 우도 추정기 (MLE) 알고리즘을 사용하여 25-27 IRF 에서이 deconvolute. MLE (γ의 J)는 다음과 같이 계산된다 eq1.jpg &quot;/&gt; N (I)이 채널 I의 광자 카운트 수이고, k는 각 형광 감쇠 용 채널 (또는 빈들)의 수이고, p는 I (j)는 광자의 그룹 입자가 나는 경우 채널 내에 속하는 확률은 수명은 J 및 N은 소정의 감쇠에 대한 계수의 총 수이다. </li><li> 크기가 512 × 512 픽셀 (264)의 이미지로 구성된 연속 스캔을 만드는 5 분간 각 시료의 형광 강도 및 수명 데이터를 기록한다. 이러한 150 광자 임계 공정이 사용 MATLAB으로 계산 MLE와 이차원 형광 강도, 수명 및 강도 가중 수명지도를 제공하기 위해 결합한다. </li></ol></li></ol>

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The authors have nothing to disclose.

Cross-sectional fluorescence imaging allows for direct visualization of nanoparticles during swell encapsulation. The kinetics of encapsulation has been shown, with the drive toward a high nanoparticle surface concentration demonstrated. The extent of nanoparticle incorporation is shown to vary with swell encapsulation time (described in section 2.3), with the total amount of incorporated nanoparticles increasing as this time is extended, with the particle concentration localized at the surface if the polymer samples are...

나노 물질의 응용 프로그램이 긴 새로운 기술에 대한 관심을 증가의 영역을 역임했다. 1-3이 화장품, 의류, 포장 및 전자 제품을 포함한 일상 항목에서 나노 입자의 성장 사용을 포함하고있다. 4-6 나노 입자를 사용하는 방향으로 주요 드라이브 기능성 물질의 입자 크기의 변화에 의해 튜닝 특성 능력 이외에 재료 그들의 높은 반응성 상대로부터 유래한다. 7 한 다른 이점은 같은 호스트 매트릭스에 중요한 특성을 도입하기 쉽게 복합 재료를 형성 할 수있는 능력이다 촉매 기능, 재료 강화 및 전기적 특성의 조정. 8-12 나노 입자 고분자 복합 재료 기술의 범위를 통해 달성 될 수 있고, 간단한있는 호스트 매트릭스의 제조 동안에 원하는 나노 직접 통합이다. (13, 14)이 R나노 입자에 걸쳐 재료의 균일 한 간격이 균일 한 재료 esults. 그러나 대부분의 응용 프로그램은 나노 복합 재료의 외부 인터페이스에 존재하는 활성 물질을 필요로한다. 재료의 벌크를 통해 많은 나노 폐기물이있는 한 결과, 직접 혼입 때때로 값 비싼 나노 물질의 효율적인 이용을 초래하지 않는다. (15, 16)를 직접 결합을 달성하기 위해, 나노 입자는 호스트 매트릭스의 형성과 호환되어야한다. 이는 특히 통상적으로 고 활성 인 나노 입자에 의해 영향을받을 수있는 금속 착체 촉매 메커니즘에 의해 촉진되는 열경화성 플라스틱의 경우와 같이 다면적 반응을 필요로 합성에 도전 할 수있다. (14) 중합체 합성시에 직접 나노 혼입과 연관된 상당한 단점이 나노 incorporati을 제한 할 목적으로 기술 개발을 이끌었다표면에 층. 17-21 스웰 캡슐화 중합체 벌크 제한 소모와 높은 표면 나노 입자의 농도를 달성하기 위해, 문헌에보고 된 가장 성공적인 전략이다. 17-19 기술은 중합체의 용매 구동 팽창을 이용한다 매트릭스 분자 종의 나노 입자의 침입을 허용. 팽윤 용매를 제거하면, 매트릭스 내에서의 종이 표면에 국부적 종의 높은 농도와 함께 제자리에 고정된다. 현재까지 팽창 캡슐화의보고 사용의 대부분은 (는) 활성제는 재료 표면에 있는지 중요 항균 고분자의 제조,에 관한 것이다. 이러한 보고서 많은 향상된 항균 활성을 나타내는 반면, 정확한 표면 나노 입자 조성물의 거의 상세히 프로빙 않는다. 크릭 등 알. 최근에 중요한 INSI을 제공하는 나노 입자 침입의 직접 시각화하는 방법을 시연팽윤 밀봉함으로써 달성 동력학 표면 나노 입자의 농도에 GHT. 22 이 작업은 카드뮴 셀레 나이드 양자점 (QD), 폴리 디메틸 실록산 (PDMS)과 형광 이미징을 사용하여 혼입 직접적인 시각화에 자신 팽윤 밀봉 합성 세부. 팽윤 액에 팽윤 밀봉 시간 및 나노 입자의 농도를 변화시키는 효과를 탐구한다. 형광의 시각화 기법은 PDMS에 나노 입자 침입 직접 이미징을 허용하고 양자점의 가장 높은 농도는 재료 표면에있는 것을 보여준다.

<table border="0" cellpadding="0" cellspacing="0" width="573">
	<tbody>
		<tr height="21">
			<td height="21" style="height:21px;width:216px;">Polydimethylsiloxane sheets</td>
			<td style="width:71px;">NuSil</td>
			<td style="width:119px;">-</td>
			<td style="width:167px;">Medical Grade</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:216px;">Oleylamine</td>
			<td style="width:71px;">Sigma Aldrich</td>
			<td style="width:119px;">O7805</td>
			<td>Technical Grade</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:216px;">Trioctylphosphine</td>
			<td style="width:71px;">Sigma Aldrich</td>
			<td style="width:119px;">117854</td>
			<td>Technical Grade</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:216px;">Trioctylphosphine oxide</td>
			<td style="width:71px;">Sigma Aldrich</td>
			<td style="width:119px;">346187</td>
			<td>Technical Grade</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:216px;">1-Octadecene</td>
			<td style="width:71px;">Sigma Aldrich</td>
			<td style="width:119px;">O806</td>
			<td>Technical Grade</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:216px;">Zinc diethyldithiocarbamate</td>
			<td style="width:71px;">Sigma Aldrich</td>
			<td style="width:119px;">329703</td>
			<td>-</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:216px;">Oleic acid</td>
			<td style="width:71px;">Sigma Aldrich</td>
			<td style="width:119px;">364525</td>
			<td>Technical Grade</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:216px;">Triethylamine</td>
			<td style="width:71px;">Sigma Aldrich</td>
			<td style="width:119px;">471283</td>
			<td>-</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:216px;">Cadmium oxide</td>
			<td style="width:71px;">Alfa Aesar</td>
			<td style="width:119px;">33235</td>
			<td>-</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:216px;">Hexadecylamine</td>
			<td style="width:71px;">Alfa Aesar</td>
			<td style="width:119px;">B22459</td>
			<td>Technical Grade</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:216px;">1-Dodecylphosphonic acid</td>
			<td style="width:71px;">Alfa Aesar</td>
			<td style="width:119px;">H26259</td>
			<td>-</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:216px;">Selenium powder</td>
			<td style="width:71px;">Acros</td>
			<td style="width:119px;">19807</td>
			<td>-</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:216px;">Chloroform</td>
			<td style="width:71px;">Sigma Aldrich</td>
			<td style="width:119px;">366919</td>
			<td>-</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:216px;">n-Hexane</td>
			<td style="width:71px;">Sigma Aldrich</td>
			<td style="width:119px;">208752</td>
			<td>-</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:216px;">Microscope slides</td>
			<td style="width:71px;">VWR</td>
			<td style="width:119px;">631-0137</td>
			<td>Thickness No. 1</td>
		</tr>
	</tbody>
</table>

advanced compositional analysis of nanoparticle-polymer composites using direct fluorescence imaging

The fabrication of polymer-nanoparticle composites is extremely important in the development of many functional materials. Identifying the precise composition of these materials is essential, especially in the design of surface catalysts, where the surface concentration of the active component determines the activity of the material. Antimicrobial materials which utilize nanoparticles are a particular focus of this technology. Recently swell encapsulation has emerged as a technique for inserting antimicrobial nanoparticles into a host polymer matrix. Swell encapsulation provides the advantage of localizing the incorporation to the external surfaces of materials, which act as the active sites of these materials. However, quantification of this nanoparticle uptake is challenging. Previous studies explore the link between antimicrobial activity and surface concentration of the active component, but this is not directly visualized. Here we show a reliable method to monitor the incorporation of nanoparticles into a polymer host matrix via swell encapsulation. We show that the surface concentration of CdSe/ZnS nanoparticles can be accurately visualized through cross-sectional fluorescence imaging. Using this method, we can quantify the uptake of nanoparticles via swell encapsulation and measure the surface concentration of encapsulated particles, which is key in optimizing the activity of functional materials.

양자점은 약 600 nm의 람다 최대로 적색의 형광을 나타냈다. 22,28 적색 발광 크기 치수 강한 한정 체제 내에 양자로드하여 여기자의 제한 때문이었다. 리 등이. 양자 봉 들면 발광 변화의 폭 또는로드의 길이 중 하나의 증가와 에너지를 낮추는 것으로 나타났다. 그들은 상기 발광은 주로로드의 폭이 강한 한정 체제에서와 같이 해당 소재의 보어 반지름보다 작?...

Watch this Scientific Journal Video about Advanced Compositional Analysis of Nanoparticle-polymer Composites Using Direct Fluorescence Imaging at JoVE.com

Advanced Compositional Analysis of Nanoparticle-polymer Composites Using Direct Fluorescence Imaging

Here we present a reliable method to monitor the incorporation of nanoparticles into a polymer host matrix via swell encapsulation. We show that the surface concentration of cadmium selenide quantum dots can be accurately visualized through cross-sectional fluorescence imaging.

직접 형광 이미징을 사용하여 나노 입자 - 고분자 복합 재료의 고급 성분 분석

The fabrication of polymer-nanoparticle composites is extremely important in the development of many functional materials. Identifying the precise ...

advanced-compositional-analysis-nanoparticle-polymer-composites-using

Research

JoVE Journal

Engineering

7.6K 조회수.  Imperial College London. Here we present a reliable method to monitor the incorporation of nanoparticles into a polymer host matrix via swell encapsulation. We show that the surface concentration of cadmium selenide quantum dots can be accurately visualized through cross-sectional fluorescence imaging.

비디오: Advanced Compositional Analysis of Nanoparticle-polymer Composites Using Direct Fluorescence Imaging

Preparation and Evaluation of Hybrid Composites of Chemical Fuel and Multi-walled Carbon Nanotubes in the Study of Thermopower Waves

When a chemical fuel at a certain position in a hybrid composite of the fuel and a micro/nanostructured material is ignited, chemical combustion occurs along the interface between the fuel and core materials. Simultaneously, dynamic changes in thermal and chemical potentials across the micro/nanostructured materials result in concomitant electrical energy generation induced by charge transfer in the form of a high-output voltage pulse. We demonstrate the entire procedure of a thermopower wave experiment, from synthesis to evaluation. Thermal chemical vapor deposition and the wet impregnation process are respectively employed for the synthesis of a multi-walled carbon nanotube array and a hybrid composite of picric acid/sodium azide/multi-walled carbon nanotubes. The prepared hybrid composites are used to fabricate a thermopower wave generator with connecting electrodes. The combustion of the hybrid composite is initiated by laser heating or Joule-heating, and the corresponding combustion propagation, direct electrical energy generation, and real-time temperature changes are measured using a high-speed microscopy system, an oscilloscope, and an optical pyrometer, respectively. Furthermore, the crucial strategies to be adopted in the synthesis of hybrid composite and initiation of their combustion that enhance the overall thermopower wave energy transfer are proposed.

A protocol for conducting thermopower wave experiments is presented. The synthesis of hybrid composites of a chemical fuel and micro/nanostructured material, manufacturing of a thermopower wave generator, and methods for measuring the corresponding physical phenomena are described.

열 전력 (thermopower) 파도의 연구에서 화학 연료 및 다중 벽 탄소 나노 튜브의 하이브리드 복합 재료의 제조 및 평가

When a chemical fuel at a certain position in a hybrid composite of the fuel and a micro/nanostructured material is ignited, chemical combustion occurs ...

연구

공학

Failure Analysis of Batteries Using Synchrotron-based Hard X-ray Microtomography

Imaging morphological changes that occur during the lifetime of rechargeable batteries is necessary to understand how these devices fail. Since the advent of lithium-ion batteries, researchers have known that the lithium metal anode has the highest theoretical energy density of any anode material. However, rechargeable batteries containing a lithium metal anode are not widely used in consumer products because the growth of lithium dendrites from the anode upon charging of the battery causes premature cell failure by short circuit. Lithium dendrites can also form in commercial lithium-ion batteries with graphite anodes if they are improperly charged. We demonstrate that lithium dendrite growth can be studied using synchrotron-based hard X-ray microtomography. This non-destructive imaging technique allows researchers to study the growth of lithium dendrites, in addition to other morphological changes inside batteries, and subsequently develop methods to extend battery life.

Synchrotron-based hard X-ray microtomography is used to image the electrochemical growth of dendrites from a lithium metal electrode through a solid polymer electrolyte membrane.

싱크로 기반 하드 X 선 Microtomography를 사용하여 배터리의 실패 분석

Imaging morphological changes that occur during the lifetime of rechargeable batteries is necessary to understand how these devices fail. Since the advent ...

Advanced Experimental Methods for Low-temperature Magnetotransport Measurement of Novel Materials

Novel electronic materials are often produced for the first time by synthesis processes that yield bulk crystals (in contrast to single crystal thin film synthesis) for the purpose of exploratory materials research. Certain materials pose a challenge wherein the traditional bulk Hall bar device fabrication method is insufficient to produce a measureable device for sample transport measurement, principally because the single crystal size is too small to attach wire leads to the sample in a Hall bar configuration. This can be, for example, because the first batch of a new material synthesized yields very small single crystals or because flakes of samples of one to very few monolayers are desired. In order to enable rapid characterization of materials that may be carried out in parallel with improvements to their growth methodology, a method of device fabrication for very small samples has been devised to permit the characterization of novel materials as soon as a preliminary batch has been produced. A slight variation of this methodology is applicable to producing devices using exfoliated samples of two-dimensional materials such as graphene, hexagonal boron nitride (hBN), and transition metal dichalcogenides (TMDs), as well as multilayer heterostructures of such materials. Here we present detailed protocols for the experimental device fabrication of fragments and flakes of novel materials with micron-sized dimensions onto substrate and subsequent measurement in a commercial superconducting magnet, dry helium close-cycle cryostat magnetotransport system at temperatures down to 0.300 K and magnetic fields up to 12 T.

We describe the methodology of mechanical exfoliation and deposition of flakes of novel materials with micron-sized dimensions onto substrate, fabrication of experimental device structures for transport experimentation, and the magnetotransport measurement in a dry helium close-cycle cryostat at temperatures down to 0.300 K and magnetic fields up to 12 T.

소설 재료의 저온 Magnetotransport 측정을위한 고급 실험 방법

Novel electronic materials are often produced for the first time by synthesis processes that yield bulk crystals (in contrast to single crystal thin film ...

Ultrasonic Welding of Thermoplastic Composite Coupons for Mechanical Characterization of Welded Joints through Single Lap Shear Testing

This paper presents a novel straightforward method for ultrasonic welding of thermoplastic-composite coupons in optimum processing conditions. The ultrasonic welding process described in this paper is based on three main pillars. Firstly, flat energy directors are used for preferential heat generation at the joining interface during the welding process. A flat energy director is a neat thermoplastic resin film that is placed between the parts to be joined prior to the welding process and heats up preferentially owing to its lower compressive stiffness relative to the composite substrates. Consequently, flat energy directors provide a simple solution that does not require molding of resin protrusions on the surfaces of the composite substrates, as opposed to ultrasonic welding of unreinforced plastics. Secondly, the process data provided by the ultrasonic welder is used to rapidly define the optimum welding parameters for any thermoplastic composite material combination. Thirdly, displacement control is used in the welding process to ensure consistent quality of the welded joints. According to this method, thermoplastic-composite flat coupons are individually welded in a single lap configuration. Mechanical testing of the welded coupons allows determining the apparent lap shear strength of the joints, which is one of the properties most commonly used to quantify the strength of thermoplastic composite welded joints.

A straightforward procedure for ultrasonic welding of thermoplastic composite coupons for basic mechanical testing is described. Key characteristics of this ultrasonic welding process are the use of flat energy directors for simplified process preparation and the use of process data for the fast definition of optimum processing conditions.

단일 랩 전단 시험을 통해 용접 조인트의 기계적 특성에 대한 열가소성 복합 쿠폰의 초음파 용접

This paper presents a novel straightforward method for ultrasonic welding of thermoplastic-composite coupons in optimum processing conditions. The ...

Use of a Multi-compartment Dynamic Single Enzyme Phantom for Studies of Hyperpolarized Magnetic Resonance Agents

Imaging of hyperpolarized substrates by magnetic resonance shows great clinical promise for assessment of critical biochemical processes in real time. Due to fundamental constraints imposed by the hyperpolarized state, exotic imaging and reconstruction techniques are commonly used. A practical system for characterization of dynamic, multi-spectral imaging methods is critically needed. Such a system must reproducibly recapitulate the relevant chemical dynamics of normal and pathological tissues. The most widely utilized substrate to date is hyperpolarized [1-13C]-pyruvate for assessment of cancer metabolism. We describe an enzyme-based phantom system that mediates the conversion of pyruvate to lactate. The reaction is initiated by injection of the hyperpolarized agent into multiple chambers within the phantom, each of which contains varying concentrations of reagents that control the reaction rate. Multiple compartments are necessary to ensure that imaging sequences faithfully capture the spatial and metabolic heterogeneity of tissue. This system will aid the development and validation of advanced imaging strategies by providing chemical dynamics that are not available from conventional phantoms, as well as control and reproducibility that is not possible in vivo.

A multi-compartment dynamic phantom is used to simulate some biology of interest for metabolic studies using hyperpolarized magnet resonance agents.

과분극 자기 공명 에이전트의 연구 다중 구획 동적 단일 효소 팬텀의 사용

Imaging of hyperpolarized substrates by magnetic resonance shows great clinical promise for assessment of critical biochemical processes in real time. Due ...

Using Synchrotron Radiation Microtomography to Investigate Multi-scale Three-dimensional Microelectronic Packages

Synchrotron radiation micro-tomography (SR&#181;T) is a non-destructive three-dimensional (3D) imaging technique that offers high flux for fast data acquisition times with high spatial resolution. In the electronics industry there is serious interest in performing failure analysis on 3D microelectronic packages, many which contain multiple levels of high-density interconnections. Often in tomography there is a trade-off between image resolution and the volume of a sample that can be imaged. This inverse relationship limits the usefulness of conventional computed tomography (CT) systems since a microelectronic package is often large in cross sectional area 100-3,600 mm2, but has important features on the micron scale. The micro-tomography beamline at the Advanced Light Source (ALS), in Berkeley, CA USA, has a setup which is adaptable and can be tailored to a sample&#39;s properties, i.e., density, thickness, etc., with a maximum allowable cross-section of 36 x 36 mm. This setup also has the option of being either monochromatic in the energy range ~7-43 keV or operating with maximum flux in white light mode using a polychromatic beam. Presented here are details of the experimental steps taken to image an entire 16 x 16 mm system within a package, in order to obtain 3D images of the system with a spatial resolution of 8.7 &#181;m all within a scan time of less than 3 min. Also shown are results from packages scanned in different orientations and a sectioned package for higher resolution imaging. In contrast a conventional CT system would take hours to record data with potentially poorer resolution. Indeed, the ratio of field-of-view to throughput time is much higher when using the synchrotron radiation tomography setup. The description below of the experimental setup can be implemented and adapted for use with many other multi-materials.

For this study synchrotron radiation micro-tomography, a non-destructive three-dimensional imaging technique, is employed to investigate an entire microelectronic package with a cross-sectional area of 16 x 16 mm. Due to the synchrotron&#39;s high flux and brightness the sample was imaged in just 3 min&#160;with an 8.7 &#181;m spatial resolution.

멀티 스케일 3 차원 마이크로 전자 패키지를 조사하는 방사광 Microtomography 사용

Synchrotron radiation micro-tomography (SR&#181;T) is a non-destructive three-dimensional (3D) imaging technique that offers high flux for fast data ...

Nanostructured Ag-zeolite Composites as Luminescence-based Humidity Sensors

Small silver clusters confined inside zeolite matrices have recently emerged as a novel type of highly luminescent materials. Their emission has high external quantum efficiencies (EQE) and spans the whole visible spectrum. It has been recently reported that the UV excited luminescence of partially Li-exchanged sodium Linde type A zeolites [LTA(Na)] containing luminescent silver clusters can be controlled by adjusting the water content of the zeolite. These samples showed a dynamic change in their emission color from blue to green and yellow upon an increase of the hydration level of the zeolite, showing the great potential that these materials can have as luminescence-based humidity sensors at the macro and micro scale. Here, we describe the detailed procedure to fabricate a humidity sensor prototype using silver-exchanged zeolite composites. The sensor is produced by suspending the luminescent Ag-zeolites in an aqueous solution of polyethylenimine (PEI) to subsequently deposit a film of the material onto a quartz plate. The coated plate is subjected to several hydration/dehydration cycles to show the functionality of the sensing film.

A protocol for the synthesis of moisture-responsive luminescent Ag-zeolite composites is described in this report.

발광 기반 습도 센서와 같은 나노 구조 AG-제올라이트 복합

Small silver clusters confined inside zeolite matrices have recently emerged as a novel type of highly luminescent materials. Their emission has high ...

Synchrotron X-ray Microdiffraction and Fluorescence Imaging of Mineral and Rock Samples

In this report, we describe a detailed procedure for acquiring and processing&#160;x-ray microfluorescence (&#956;XRF), and Laue and powder microdiffraction two-dimensional (2D) maps at beamline 12.3.2 of the Advanced Light Source (ALS), Lawrence Berkeley National Laboratory. Measurements can be performed on any sample that is less than 10 cm x 10 cm x 5 cm, with a flat exposed surface. The experimental geometry is calibrated using standard materials (elemental standards for XRF, and crystalline samples such as Si, quartz, or Al2O3 for diffraction). Samples are aligned to the focal point of the x-ray microbeam, and raster scans are performed, where each pixel of a map corresponds to one measurement, e.g., one XRF spectrum or one diffraction pattern. The data are then processed using the in-house developed software XMAS, which outputs text files, where each row corresponds to a pixel position. Representative data from moissanite and an olive snail shell are presented to demonstrate data quality, collection, and analysis strategies.

We describe a beamline setup meant to carry out rapid two-dimensional x-ray fluorescence and x-ray microdiffraction mapping of single crystal or powder samples using either Laue (polychromatic radiation) or powder (monochromatic radiation) diffraction. The resulting maps give information about strain, orientation, phase distribution, and plastic deformation.

싱크 로트 론 엑스레이 Microdiffraction 및 광물 및 암석 샘플의 형광 이미징

In this report, we describe a detailed procedure for acquiring and processing&#160;x-ray microfluorescence (&#956;XRF), and Laue and powder ...

Expression of Cementitious Pore Solution and the Analysis of Its Chemical Composition and Resistivity Using X-ray Fluorescence

The goal of this method is to determine the chemical composition and electrical resistivity of cementitious pore solution expressed from a fresh paste sample. The pore solution is expressed from a fresh paste sample using a pressurized nitrogen gas system. The pore solution is then immediately transferred to a syringe to minimize evaporation and carbonation. After that, assembled testing containers are used for the X-ray fluorescence (XRF) measurement. These containers consist of two concentric plastic cylinders and a polypropylene film which seals one of the two open sides. The pore solution is added into the container immediately prior to the XRF measurement. The XRF is calibrated to detect the main ionic species in the pore solution, in particular, sodium (Na+), potassium (K+), calcium (Ca2+), and sulfide (S2-), to calculate sulfate (SO42-) using stoichiometry. The hydroxides (OH-) can be calculated from a charge balance. To calculate the electrical resistivity of the solution, the concentrations of the main ionic species and a model by Snyder et al. are used. The electrical resistivity of the pore solution can be used, along with the electrical resistivity of concrete, to determine the formation factor of concrete. XRF is a potential alternative to current methods to determine the composition of pore solution, which can provide benefits in terms of reduction in time and costs.

This protocol describes the procedure to express fresh pore solution from cementitious systems and the measurement of its ionic composition using X-ray fluorescence. The ionic composition can be used to calculate pore solution electrical resistivity, which can be used, together with concrete electrical resistivity, to determine the formation factor.

The goal of this method is to determine the chemical composition and electrical resistivity of cementitious pore solution expressed from a fresh paste ...

Excitation-Scanning Hyperspectral Imaging Microscopy to Efficiently Discriminate Fluorescence Signals

Several techniques rely on detection of fluorescence signals to identify or study phenomena or to elucidate functions. Separation of these fluorescence signals were proven cumbersome until the advent of hyperspectral imaging, in which fluorescence sources can be separated from each other as well as from background signals and autofluorescence (given knowledge of their spectral signatures). However, traditional, emission-scanning hyperspectral imaging suffers from slow acquisition times and low signal-to-noise ratios due to the necessary filtering of both excitation and emission light. It has been previously shown that excitation-scanning hyperspectral imaging reduces the necessary acquisition time while simultaneously increasing the signal-to-noise ratio of acquired data. Using commercially available equipment, this protocol describes how to assemble, calibrate, and use an excitation-scanning hyperspectral imaging microscopy system for separation of signals from several fluorescence sources in a single sample. While highly applicable to microscopic imaging of cells and tissues, this technique may also be useful for any type of experiment utilizing fluorescence in which it is possible to vary excitation wavelengths, including but not limited to: chemical imaging, environmental applications, eye care, food science, forensic science, medical science, and mineralogy.

Spectral imaging has become a reliable solution for identification and separation of multiple fluorescence signals in a single sample and can readily distinguish signals of interest from background or autofluorescence. Excitation-scanning hyperspectral imaging improves on this technique by decreasing the necessary image acquisition time while simultaneously increasing the signal-to-noise ratio.

형광 신호를 효율적으로 구별하기 위한 여기-스캐닝 하이퍼스펙트럼 이미징 현미경 검사법

Several techniques rely on detection of fluorescence signals to identify or study phenomena or to elucidate functions. Separation of these fluorescence ...