저자는 회계 SMhardBi (프로젝트 번호 200021_150088/1)를 위한 스위스 국립 과학 재단을 인정 합니다. SANS 실험은 스위스 spallation 중성자 소스 SINQ, 폴 Scherrer Instute, Villigen, 스위스에서 수행 했다. 따뜻하게 저자 박사 요 아 킴 Kohlbrecher SAN 실험과 함께 그의 지도 감사합니다. 높은 자기장에서 복굴절 측정 설치 높은 분야 자석 실험실 HFML, Nijmegen, 네덜란드에서 기존 설치에서 영감을 했다. 우리는 브루노 Pfister 복굴절 설치의 전자 제품 개발에 그의 도움에 대 한, 1 월 Corsano와 다니엘 Kiechl, 레이저의 정밀 하 고 손쉬운 맞춤을 허용 하는 프레임 워크를 구축 및 지속적인 기술 지원에 대 한 박사 베른하르트 콜 러 감사 합니다.

<ol>
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저자는 공개 없다.

복굴절 측정 했다 SAN과 함께에서 사용 하는 방법의 세부 계정을 생성 높은 자석으로 응답 Ln3 + 어셈블리 Isabettini 외 에 인지질 킬레이트 화 하기 위한 방법을 평가 하 실험 23 제안 된 제조 프로토콜은 또한 더 긴 DPPC와 DPPE DTPA 인지질으로 구성 하는 어셈블리에 대 한 또는 그들의 bilayer에 화학적 조작된 스테로이드 유도체를 포함에 대 한 적용 됩니다. 1...

Bicelles는 수많은 지질 혼합물에서 얻은 디스크 모양의 polymolecular 어셈블리. 1 , 2 , 3 , 4 , 5 그들은 널리 NMR 분광학에 의해 생체 막의 구조 특성에 대 한 사용 됩니다. 6 , 그러나 7 , 최근 노력 하고자 가능한 응용 프로그램의 필드를 확장 합니다. 5 , 8 , 9 가장 공부 bicelle 시스템은 1, 2의 혼합물의 구성 되어-dimyristoyl-sn-glycero-3-phosphocholine (DMPC), 구성 어셈블리 및 1, 2의 평면 부분-dihexanoyl-sn-glycero-3-phosphocholine (DHPC) 가장자리를 포함 하는 인지질. 1 , 2 , 3 인지질 bilayer 지시 자체 조립된 polymolecular 구조의 건축 구성의 분자 기하학. 4 , 5 DMPE-DTPA와 교체 DHPC 높은 자석으로 대답 하 고 조정할 수 있는 bicelle 시스템을 생성합니다. 10 , 11 DMPC/DMPE-DTPA/Ln3 + (어 금 니 비율 4:1:1) bicelles 연관 많은 더 많은 상자성 란타넘족 이온 (Ln3 +) 향상 된 자기 반응의 결과로 하는 bilayer의 표면에. 10 또한, 교체 수용 DHPC 분자 DMPE-DTPA/Ln3 + 수 희석 방지 bicelles의 형성 11
평면 polymolecular 어셈블리의 자석 alignability는 그들의 전반적인 자기 에너지에 의해 결정
<img alt="Equation 1" src="/files/ftp_upload/56812/56812eq1v2.jpg">(1)
B는 자기 필드 강도 <img alt="Equation 2" src="/files/ftp_upload/56812/56812eq2.jpg"> 자석 상수, n 집계 수와 <img alt="Equation 3" src="/files/ftp_upload/56812/56812eq3.jpg"> 는 bilayer를 구성 하는 지질 분자 diamagnetic 자화 율 이방성. 따라서, 자기장에 DMPC/DMPE-DTPA/Ln3 + bicelles의 응답은 그들의 크기 (집계 숫자 n)와 분자 diamagnetic 자화 율 이방성 Δχ에 의해 지어진 다. 후자는 쉽게 달성 chelated Ln3 +의 특성을 변경 하 여. 12 , 13 , 14 , 15 소개 콜레스테롤 (철-오) 또는 다른 스테로이드 유도체는 bilayer에 집계 숫자 n와 어셈블리의 자기 자화 율 Δχ 튜닝의 가능성을 제공 합니다. 11 , 16 , 17 , 18 , 19 주어진된 지질 구성에 대 한 큰 어셈블리 포함 더 많은 지질 E탄 창 (큰 집계 숫자 n)에 기여 가능 결과 더 alignable 종에. DMPC/DHPC bicelles의 크기 예를 들면, 전통적으로 구성 지질 비율이 나 총 농도의 최적화를 통해 제어 됩니다. 20 , 21 , 22 이 DMPC/DMPE-DTPA/Ln3 + bicelles에, 있지만 난방 제공 시 소포를 bicelle에서 그들의 열 가역 변환을 짓는 옵션 추가. 기계와 같은 멤브레인 필터를 통해 압출 수는 vesicles의 형성을 의미 합니다. 자석으로 alignable bicelles는 5 ° C에 냉각 시 재생성 하 고 그들의 크기 기 선구자에서 결정 됩니다. 11 여기, 우리가에 초점을 가진 DMPC/DMPE-DTPA/Tm3 + 기계 제조 절차의 잠재력 (어 금 니 비율 4:1:1) 또는 DMPC/철-오/DMPE-DTPA/Tm3 + (어 금 니 비율 16:4:5:5) 참조 시스템으로. 프로세스 작업 다른 Ln3 + 보다 Tm3 +비슷하게 작동 합니다. 이러한 기술에서 제공 하는 가능성의 넓은 범위는 그림 1 에서 강조 표시 하 고 광범위 하 게 다른 논의. 23
<img alt="Figure 1" class="xfigimg" src="/files/ftp_upload/56812/56812fig1.jpg"> 
그림 1: 가능한 제작 절차의 개요 개요. 공부 자석으로 alignable Ln3 + chelating polymolecular 어셈블리는 구성 중 DMPC/DMPE-DTPA/Tm3 + (어 금 니 비율 4:1:1) 또는 DMPC/철-오/DMPE-DTPA/Tm3 + (어 금 니 비율 16:4:5:5). 건조 지질 영화 7.4의 pH 값에 50 m m 인산 염 버퍼 화 이며 총 지질 농도 15 m m. 지질 영화의 효과적인 수 분 요구도 녹고 사이클 (피트) 또는 열 및 냉각 사이클을 동결 (H &#38; C). H &#38; C 사이클 마지막 동결 단계, 녹고 후 샘플을 다시 생성 하거나 압출 추가 없이 사용할 수 있다면 그들은 시간의 연장된 기간 동안 냉동 보관 하는 샘플을 다시 생성에 필요 하다. 이 단계는 Isabettini 외에 의해 광범위 하 게 논의 된다. 23 극대 alignable polymolecular 어셈블리 지질 구성에 따라 서로 다른 어셈블리 아키텍처를 제공 하는, 달성 된다. Bicelle 크기와 자석 alignability nanopore 멤브레인 필터를 통해 압출 (Ext)에 의해 가변 이다. 제시 정렬 요소 Af 800, 400, 200, 또는 100 통해 압출 DMPC/철-오/DMPE-DTPA/Tm3 + (어 금 니 비율 16:4:5:5) 샘플의 2D 작은 각 중성자 산란 (SANS) 패턴에서 계산 된 숨 구멍 nm. 측정 없이 더 자세히 여기에 적용 되지 것입니다 bicelle 정렬 측정의 보완 수단입니다. 11 , 16 는 Af 등방성 산란에 대 한 0-1 (병렬 중성자 산란 또는 자기장 방향 bicelles의 수직 정렬)에서 배열 한다.<a href="//ecsource.jove.com/files/ftp_upload/56812/56812fig1large.jpg" target="_blank">이 그림의 더 큰 버전을 보려면 여기를 클릭 하십시오.</a>
Bicelles의 구조는 다양 한 특성화 기법에 의해 광범위 하 게 연구 되었습니다. 13 자기 필드에 노출 하는 bicelles의 맞춤 NMR 분광학 또는 작은 각 중성자 산란 (SANS) 실험을 사용 하 여 측정할 되었습니다. 5 , 10 , 11 , 12 , 13 , 16 , 17 , 18 , 19 , 24 , 그러나 25 , 변화와 존재 Ln3 + 발생 NMR 봉우리의 확대는 메서드에 심각한 한계. 15 , 26 , 27 , 28 있지만 SAN 실험이이 제한, 대체에서 고통을 하지 않습니다 그리고 더 접근 기술 솔루션에서 어셈블리의 자석으로 유도 맞춤의 일상적인 정량화에 대 한 바람직한. 복굴절 측정 실용적이 고 비교적 간단한 대안입니다. 비슷하게 NMR 실험, 복굴절 측정 지질 재배열 및 지질 단계는 bilayer에 발생에 대 한 귀중 한 정보를 공개. 또한, 온도 같은 환경 조건 변경 polymolecular 어셈블리에서 발생 하는 기하학적 변환 모니터링 된다. 11 , 12 , 13 , 16 자기 유도 복굴절 Δn′ 인지질 시스템의 다양 한 유형을 공부에 사용 되었습니다. 13 , 29 , 30 는 자기장에서 위상 변조 기술에 따라 복굴절 측정 bicelles의 방향을 감지 하는 가능한 방법입니다. 12 , 16 , 18 , 29 , 31 , 32 35 T까지 높은 자기장에서 복굴절와 함께 bicelles를 조사 하는의 가능성 또한 M. Liebi 그 외 여러분 에 의해 입증 되었다 13
편광 이방성 물자 들어가면 일반 및 특별 한 파에서 굴절 됩니다. 11 두 파 다른 속도 있고 지체 δ에 의해 단계에서 이동 된다. 지체 δ의 정도 측정 하 고 복굴절 신호로 변환 <img alt="Equation 5" src="/files/ftp_upload/56812/56812eq5.jpg"> 는 소재를 사용 하 여 이방성의 정도 계량 하기
<img alt="Equation 6" src="/files/ftp_upload/56812/56812eq6.jpg">(2)
여기서 λ는 레이저와 d의 파장은 샘플의 두께입니다. 인지질은 광학 이방성 그리고 탄화수소 꼬리에 평행 하 게 그들의 긴 분자 축과 일치 하는 그들의 광 축. 11 , 12 는 인지질은 임의로 솔루션에서 지향 하는 경우 지체 없이 측정 됩니다. 지체는 인지질 서로 평행 정렬 됩니다 때 측정 된다. 자석으로 유도 복굴절 <img alt="Equation 5" src="/files/ftp_upload/56812/56812eq5.jpg"> ; 자기장에서 분자의 방향에 따라 양수 또는 음수 부호를 가질 수 있습니다 그림 2를 참조 하십시오. X 축에 평행 정렬 인지질 네거티브 귀 착될 것 이다 <img alt="Equation 5" src="/files/ftp_upload/56812/56812eq5.jpg"> </img>z 축을 따라 정렬 된 결과 긍정적인 그러나, <img alt="Equation 5" src="/files/ftp_upload/56812/56812eq5.jpg"> </img>. 아니 복굴절 때 광 축과 일치 빛 전파의 방향으로는 인지질 y 축에 평행 하 게 정렬 관찰 됩니다.
<img alt="Figure 2" class="xfigimg" src="/files/ftp_upload/56812/56812fig2.jpg"> 
그림 2: 맞춤 인지질 및 자기 유도 복굴절의 해당 표시의 <img alt="Equation 12" src="/files/ftp_upload/56812/56812eq12.jpg"> </img> . 측정된의 <img alt="Equation 12" src="/files/ftp_upload/56812/56812eq12.jpg"> 는 자기장에서 인지질의 방향에 따라 달라 집니다. 파선 분자의 광 축을 나타냅니다. 빛은 45 °에서 편광 하 고 y 방향으로 전파. 자기장 B z 방향에서입니다. 이 그림은 M. Liebi에서 수정 되었습니다. 11 <a href="//ecsource.jove.com/files/ftp_upload/56812/56812fig2large.jpg" target="_blank">이 그림의 더 큰 버전을 보려면 여기를 클릭 하십시오.</a>
Bicelles의 등방성 콜 로이드 정지, 경우는 bilayer에 인지질의 배열에 의해 유도 된 방향 지체 δ 비우기 손실 될 것입니다. Bicelles는 또한 편광된 빛의 지체 δ를 일으키는 그들의 bilayers에 광학 활성 인지질을 찾으시는 순서 정렬 해야 합니다. 따라서, 복굴절 polymolecular 어셈블리의 자석 alignability 계량 하는 중요 한 도구입니다. Bicelles 정렬 자기장에 수직 긍정적인 보장할 <img alt="Equation 5" src="/files/ftp_upload/56812/56812eq5.jpg"> </img>병렬 정렬 그 부정적인 항복 것입니다 하는 동안, <img alt="Equation 5" src="/files/ftp_upload/56812/56812eq5.jpg"> </img>. 서명 설정의 정렬에 따라 달라 집니다 그리고 참조 샘플을 확인할 수 있습니다.

<table>
	<tbody>
		<tr>
			<td>1,2-dimyristoyl-sn-glycero-3-phosphocholine (DMPC)</td>
			<td>Avanti Polar Lipids</td>
			<td>850345P</td>
			<td>&#62;99%</td>
		</tr>
		<tr>
			<td>1,2-dimyristoyl-sn-glycero-3-phospho-ethanolamine-diethylene triaminepentaacetate acid hexammonium salt (DMPE-DTPA)</td>
			<td>Avanti Polar Lipids</td>
			<td>790535P</td>
			<td>&#62;99%</td>
		</tr>
		<tr>
			<td>Thulium(III) chloride</td>
			<td>Sigma-Aldrich</td>
			<td>439649</td>
			<td>anhydrous, powder, 99.9% trace metals basis</td>
		</tr>
		<tr>
			<td>Dysprosium(III) chloride</td>
			<td>Sigma-Aldrich</td>
			<td>325546</td>
			<td>anhydrous, powder, 99.9% trace metals basis</td>
		</tr>
		<tr>
			<td>Ytterbium(III) chloride</td>
			<td>Sigma-Aldrich</td>
			<td>439614</td>
			<td>anhydrous, powder, 99.9% trace metals basis</td>
		</tr>
		<tr>
			<td>Chloroform</td>
			<td>Sigma-Aldrich</td>
			<td>319988</td>
			<td>contains ethanol as stabilizer, ACS reagent, &#8805;99.8%</td>
		</tr>
		<tr>
			<td>Methanol</td>
			<td>Sigma-Aldrich</td>
			<td>34860</td>
			<td>&#8805;99.9%</td>
		</tr>
		<tr>
			<td>Cholesterol</td>
			<td>Amresco</td>
			<td>433</td>
			<td>Ultra pure grade</td>
		</tr>
		<tr>
			<td>D2O</td>
			<td>ARMAR chemicals</td>
			<td>1410</td>
			<td>99.8 atom % D</td>
		</tr>
		<tr>
			<td>Ultrapure water</td>
			<td>Millipore</td>
			<td></td>
			<td>Synergy pak2 (SYPK0SIX2), Millipack GP (MPGP02001)</td>
		</tr>
		<tr>
			<td>electronic pH meter</td>
			<td>Metrohm</td>
			<td>17440010</td>
			<td></td>
		</tr>
		<tr>
			<td>Whatmann Nuclepore 25 mm 100nm membrane filter</td>
			<td>VWR</td>
			<td>515-2028</td>
			<td></td>
		</tr>
		<tr>
			<td>Whatmann Nuclepore 25 mm 200nm membrane filter</td>
			<td>VWR</td>
			<td>515-2029</td>
			<td></td>
		</tr>
		<tr>
			<td>Whatmann Nuclepore 25 mm 400nm membrane filter</td>
			<td>VWR</td>
			<td>515-2030</td>
			<td></td>
		</tr>
		<tr>
			<td>Whatmann Nuclepore 25 mm 800nm membrane filter</td>
			<td>VWR</td>
			<td>515-2032</td>
			<td></td>
		</tr>
		<tr>
			<td>Whatmann Filter paper</td>
			<td>VWR</td>
			<td>230600</td>
			<td></td>
		</tr>
		<tr>
			<td>25 ml round bottom flask</td>
			<td>VWR</td>
			<td>201-1352</td>
			<td>14/23 NS</td>
		</tr>
		<tr>
			<td>3 ml glass snap-cup</td>
			<td>VWR</td>
			<td>548-0554</td>
			<td>ND18, 18x30mm</td>
		</tr>
		<tr>
			<td>2.5 ml glass syringe</td>
			<td>Hamilton</td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>Sodium dihydrogen phosphate dihydrate</td>
			<td>Merk</td>
			<td>1.06342</td>
			<td>Salt used to make phosphate buffer</td>
		</tr>
		<tr>
			<td>di-Sodium hydrogen phosphate</td>
			<td>Merk</td>
			<td>1.06586</td>
			<td>Salt used to make phosphate buffer</td>
		</tr>
		<tr>
			<td>Liquid Nitrogen</td>
			<td>Carbagas</td>
			<td>-</td>
			<td></td>
		</tr>
		<tr>
			<td>Pressurized Nitrogen gas</td>
			<td>Carbagas</td>
			<td>-</td>
			<td>200 bar bottle</td>
		</tr>
		<tr>
			<td>Lipid Extruder 10 ml</td>
			<td>Lipex</td>
			<td>-</td>
			<td>Fully equipped with thermobarrel</td>
		</tr>
		<tr>
			<td>High-pressure PVC tube</td>
			<td>GR NETUM</td>
			<td>-</td>
			<td>must resist more than 4 MPa</td>
		</tr>
		<tr>
			<td>Serto adaptors</td>
			<td>Sertot</td>
			<td>-</td>
			<td></td>
		</tr>
		<tr>
			<td>Nitrile gloves</td>
			<td>VWR</td>
			<td>-</td>
			<td></td>
		</tr>
		<tr>
			<td>2 ml glass pipettes</td>
			<td>VWR</td>
			<td>612-1702</td>
			<td>230 mm long</td>
		</tr>
		<tr>
			<td>Diode Laser</td>
			<td>Newport</td>
			<td>LPM635-25C</td>
			<td></td>
		</tr>
		<tr>
			<td>DSP Dual Phase Lock-in Amplifier</td>
			<td>SRS</td>
			<td>SR830</td>
			<td></td>
		</tr>
		<tr>
			<td>Photodiode Detector</td>
			<td>Silonex Inc.</td>
			<td>SLSD-71N5</td>
			<td>5mm2, Silicon, photo-conductive</td>
		</tr>
		<tr>
			<td>5.5 T Cryogenic Magnetic</td>
			<td>Cryogenic/Oerlikon AG</td>
			<td>-</td>
			<td>12 bar He-cooled. RW4000/6000 compressor, RGD 5/100 TA cryo-head</td>
		</tr>
		<tr>
			<td>Second order low pass filter</td>
			<td>home-built</td>
			<td>-</td>
			<td>Linear power supply 24V DC, second order, Sallen Key, cut-off frequency 360 Hz, +/- 12V, max 10 mA</td>
		</tr>
		<tr>
			<td>Photoelastic modulator</td>
			<td>Hinds instruments</td>
			<td>PEM-90</td>
			<td></td>
		</tr>
		<tr>
			<td>Glan-Thompson Calcite Polarizer</td>
			<td>Newport</td>
			<td>10GT04</td>
			<td>25.4mm diameter</td>
		</tr>
		<tr>
			<td>Quartz sample cuvette</td>
			<td>Hellma</td>
			<td>165-10-40</td>
			<td>temperature controlled cell, 0.8 ml, 10mm path length</td>
		</tr>
		<tr>
			<td>Temperature probe</td>
			<td>Thermocontrol</td>
			<td>-</td>
			<td>Type K, 0.5mm diameter, Thermocoax</td>
		</tr>
		<tr>
			<td>Non-polarizing mirrors</td>
			<td>Newport</td>
			<td>50326-1002</td>
			<td>25.4mm</td>
		</tr>
		<tr>
			<td>RS 232 cables</td>
			<td>National Instruments</td>
			<td>189284-02</td>
			<td>For Connecting to the RS-232 Port on the front of Compact FieldPoint Controllers</td>
		</tr>
		<tr>
			<td>BNC 50 &#937; cable and connectors</td>
			<td>National Instruments</td>
			<td>763389-01</td>
			<td></td>
		</tr>
		<tr>
			<td>cFP-AI-110</td>
			<td>National Instruments</td>
			<td>777318-110</td>
			<td>8-Channel Analog Voltage and Current Input Module for Compact FieldPoint</td>
		</tr>
		<tr>
			<td>cFP-CB-1</td>
			<td>National Instruments</td>
			<td>778618-01</td>
			<td>Integrated Connector Block for Wiring to Compact FieldPoint I/O</td>
		</tr>
		<tr>
			<td>cFP-CB-3</td>
			<td>National Instruments</td>
			<td>778618-03</td>
			<td>Integrated Isothermal Connector Block for Wiring Thermocouples to the cFP-TC-120 Module</td>
		</tr>
		<tr>
			<td>cFP-TC-120</td>
			<td>National Instruments</td>
			<td>777318-120</td>
			<td>8-Channel Thermocouple Input Module for Compact FieldPoint</td>
		</tr>
		<tr>
			<td>cFP-1804</td>
			<td>National Instruments</td>
			<td>779490-01</td>
			<td>Ethernet/Serial Interface for NI Compact FieldPoint</td>
		</tr>
		<tr>
			<td>LabView 2010</td>
			<td>National Instruments</td>
			<td>-</td>
			<td></td>
		</tr>
		<tr>
			<td>Industrial power supply</td>
			<td>Traco Power</td>
			<td>TCL 060-124</td>
			<td>100-240V AC</td>
		</tr>
		<tr>
			<td>Waterbath</td>
			<td>Julabo</td>
			<td>FP40-HE</td>
			<td>refrigerated/Heating Circulator</td>
		</tr>
	</tbody>
</table>

fabrication procedures and birefringence measurements for designing magnetically responsive lanthanide ion chelating phospholipid assemblies

Bicelles는 조정 디스크 같은 polymolecular 어셈블리 지질 혼합물의 큰 다양성에서 형성. 응용 프로그램 범위에서 핵 자기 공명 (NMR)에 의해 막 단백질 구조 연구 nanotechnological 개발 광학 활성 및 자석으로 전환 젤의 형성을 포함 하 여. 이러한 기술 어셈블리 크기, 자석 응답 및 열저항의 높은 관리가 필요합니다. 1, 2의 혼합물-dimyristoyl-sn-glycero-3-phosphocholine (DMPC)와 인지질 공액, 1, 2를 킬레이트 화는 란타넘족 이온 (Ln3 +)-dimyristoyl-sn-glycero-3-인-방법-신 triaminepentaacetate ( DMPE-DTPA), DMPC/DMPE-DTPA/Ln3 + 같은 높은 자석으로 응답 어셈블리에 조립 (어 금 니 비율 4:1:1) bicelles. 콜레스테롤 (철-오)과 독특한 physico-화학 특성을 제공 하는 어셈블리의 다른 세트에서 bilayer 결과에 스테로이드 파생 상품의 소개. 주어진된 지질 구성에 대 한 자석 alignability bicelle 크기에 비례 이다. Ln3 + 의 complexation 크기 및 정렬 방향 측면에서 전례 없는 자석 응답에 있는 결과. 난방 시 소포에 디스크와 같은 구조의 온도 가역 붕괴 정의 된 기 공 크기와 멤브레인 필터를 통해 압출 하 여 어셈블리의 치수의 조정 수 있습니다. 자석으로 alignable bicelles 기 선구자에 의해 정의 하는 어셈블리 차원에서 발생 하는 5 ° C에 냉각 하 여 다시 생성 됩니다. 여기, 그리고 어셈블리의 자석 alignability 5.5 T 자기장에서 복굴절 측정 하 여 정량이 제작 절차 설명 했다. 인지질 bilayer에서 발생 한 복굴절 신호는 더는 bilayer에서 발생 하는 polymolecular 변경 모니터링 수 있습니다. 이 간단한 기술은 이다 bicelles 하 고용 일반적으로 NMR 실험을 보완.

압출 비 DMPC/DMPE-DTPA/Tm3 + 의 복굴절 신호 (어 금 니 비율 4:1:1) 샘플 난방 및 냉각 주기 5에서 ~ 40 ° C 및 1 ° C/min (그림 6)의 속도로 다시 동안 5.5 T 자기장에서 모니터링 했습니다. 복굴절 결과 1.5 x 10-5, 배나 강한 보고 압출 시스템의 값이 있는 5 ° C에서 높은 자기 정렬 확인. 6 , 7 , <sup ...

Watch this Scientific Journal Video about Fabrication Procedures and Birefringence Measurements for Designing Magnetically Responsive Lanthanide Ion Chelating Phospholipid Assemblies at JoVE.com

Fabrication Procedures and Birefringence Measurements for Designing Magnetically Responsive Lanthanide Ion Chelating Phospholipid Assemblies

자석으로 높은 반응 란타넘족 이온 킬레이트 화 polymolecular 어셈블리에 대 한 제작 절차 되 게 됩니다. 마그네틱 응답 nanopore 세포 막을 통해 밀어 남에 의해 맞게 어셈블리 크기에 의해 결정 됩니다. 어셈블리의 마그네틱 alignability 및 구조적인 변화 온도 유도 된 복굴절 측정, 핵 자기 공명 및 작은 각 중성자 뿌리기 무료 기법에 의해 감시 된다.

제작 절차 및 복굴절 측정 자석으로 응답 란타넘족 이온 킬레이트 화 인지질 어셈블리 설계에 대 한

Bicelles are tunable disk-like polymolecular assemblies formed from a large variety of lipid mixtures. Applications range from membrane protein structural ...

fabrication-procedures-birefringence-measurements-for-designing

Research

JoVE Journal

Engineering

7.1K 조회수.  ETH Zurich. 자석으로 높은 반응 란타넘족 이온 킬레이트 화 polymolecular 어셈블리에 대 한 제작 절차 되 게 됩니다. 마그네틱 응답 nanopore 세포 막을 통해 밀어 남에 의해 맞게 어셈블리 크기에 의해 결정 됩니다. 어셈블리의 마그네틱 alignability 및 구조적인 변화 온도 유도 된 복굴절 측정, 핵 자기 공명 및 작은 각 중성자 뿌리기 무료 기법에 의해 감시 된다.

비디오: Fabrication Procedures and Birefringence Measurements for Designing Magnetically Responsive Lanthanide Ion Chelating Phospholipid Assemblies

Construction and Testing of Coin Cells of Lithium Ion Batteries

Rechargeable lithium ion batteries have wide applications in electronics, where customers always demand more capacity and longer lifetime. Lithium ion batteries have also been considered to be used in electric and hybrid vehicles1 or even electrical grid stabilization systems2. All these applications simulate a dramatic increase in the research and development of battery materials3-7, including new materials3,8, doping9, nanostructuring10-13, coatings or surface modifications14-17 and novel binders18. Consequently, an increasing number of physicists, chemists and materials scientists have recently ventured into this area. Coin cells are widely used in research laboratories to test new battery materials; even for the research and development that target large-scale and high-power applications, small coin cells are often used to test the capacities and rate capabilities of new materials in the initial stage. 
 In 2010, we started a National Science Foundation (NSF) sponsored research project to investigate the surface adsorption and disordering in battery materials (grant no. DMR-1006515). In the initial stage of this project, we have struggled to learn the techniques of assembling and testing coin cells, which cannot be achieved without numerous help of other researchers in other universities (through frequent calls, email exchanges and two site visits). Thus, we feel that it is beneficial to document, by both text and video, a protocol of assembling and testing a coin cell, which will help other new researchers in this field. This effort represents the "Broader Impact" activities of our NSF project, and it will also help to educate and inspire students.
In this video article, we document a protocol to assemble a CR2032 coin cell with a LiCoO2 working electrode, a Li counter electrode, and (the mostly commonly used) polyvinylidene fluoride (PVDF) binder. To ensure new learners to readily repeat the protocol, we keep the protocol as specific and explicit as we can. However, it is important to note that in specific research and development work, many parameters adopted here can be varied. First, one can make coin cells of different sizes and test the working electrode against a counter electrode other than Li. Second, the amounts of C black and binder added into the working electrodes are often varied to suit the particular purpose of research; for example, large amounts of C black or even inert powder were added to the working electrode to test the "intrinsic" performance of cathode materials14. Third, better binders (other than PVDF) have also developed and used18. Finally, other types of electrolytes (instead of LiPF6) can also be used; in fact, certain high-voltage electrode materials will require the uses of special electrolytes7.

A protocol to construct and test coin cells of lithium ion batteries is described. The specific procedures of making a working electrode, preparing a counter electrode, assembling a cell inside a glovebox and testing the cell are presented.

건설과 리튬 이온 배터리의 동전 전지의 테스트

Rechargeable lithium ion batteries have wide applications in electronics, where customers always demand more capacity and longer lifetime.  Lithium ion ...

연구

공학

Concurrent Quantitative Conductivity and Mechanical Properties Measurements of Organic Photovoltaic Materials using AFM

Organic photovoltaic (OPV) materials are inherently inhomogeneous at the nanometer scale. Nanoscale inhomogeneity of OPV materials affects performance of photovoltaic devices. Thus, understanding of spatial variations in composition as well as electrical properties of OPV materials is of paramount importance for moving PV technology forward.1,2 In this paper, we describe a protocol for quantitative measurements of electrical and mechanical properties of OPV materials with sub-100 nm resolution. Currently, materials properties measurements performed using commercially available AFM-based techniques (PeakForce, conductive AFM) generally provide only qualitative information. The values for resistance as well as Young's modulus measured using our method on the prototypical ITO/PEDOT:PSS/P3HT:PC61BM system correspond well with literature data. The P3HT:PC61BM blend separates onto PC61BM-rich and P3HT-rich domains. Mechanical properties of PC61BM-rich and P3HT-rich domains are different, which allows for domain attribution on the surface of the film. Importantly, combining mechanical and electrical data allows for correlation of the domain structure on the surface of the film with electrical properties variation measured through the thickness of the film.

Organic photovoltaic (OPV) materials are inherently inhomogeneous at the nanometer scale. Nanoscale inhomogeneity of OPV materials affects performance of photovoltaic devices. In this paper, we describe a protocol for quantitative measurements of electrical and mechanical properties of OPV materials with sub-100 nm resolution.

동시 수량 전도성과 AFM을 사용하여 유기 태양 광 재료의 기계적 성질 측정

Organic photovoltaic  (OPV) materials are inherently inhomogeneous at the nanometer scale. Nanoscale  inhomogeneity of OPV materials affects performance ...

Characterization of Electrode Materials for Lithium Ion and Sodium Ion Batteries Using Synchrotron Radiation Techniques

Intercalation compounds such as transition metal oxides or phosphates are the most commonly used electrode materials in Li-ion and Na-ion batteries. During insertion or removal of alkali metal ions, the redox states of transition metals in the compounds change and structural transformations such as phase transitions and/or lattice parameter increases or decreases occur. These behaviors in turn determine important characteristics of the batteries such as the potential profiles, rate capabilities, and cycle lives. The extremely bright and tunable x-rays produced by synchrotron radiation allow rapid acquisition of high-resolution data that provide information about these processes. Transformations in the bulk materials, such as phase transitions, can be directly observed using X-ray diffraction (XRD), while X-ray absorption spectroscopy (XAS) gives information about the local electronic and geometric structures (e.g.&#160;changes in redox states and bond lengths). In situ experiments carried out on operating cells are particularly useful because they allow direct correlation between the electrochemical and structural properties of the materials. These experiments are time-consuming and can be challenging to design due to the reactivity and air-sensitivity of the alkali metal anodes used in the half-cell configurations, and/or the possibility of signal interference from other cell components and hardware. For these reasons, it is appropriate to carry out ex situ experiments (e.g.&#160;on electrodes harvested from partially charged or cycled cells) in some cases. Here, we present detailed protocols for the preparation of both ex situ and in situ samples for experiments involving synchrotron radiation and demonstrate how these experiments are done.

We describe the use of synchrotron X-ray absorption spectroscopy (XAS) and X-ray diffraction (XRD) techniques to probe details of intercalation/deintercalation processes in electrode materials for Li-ion and Na-ion batteries. Both in situ and ex situ experiments are used to understand structural behavior relevant to the operation of devices

방사광 기술을 사용하여 리튬 이온과 나트륨 이온 배터리 용 전극 재료의 특성

Intercalation compounds such as transition metal oxides or phosphates are the most commonly used electrode materials in Li-ion and Na-ion batteries. ...

Speciation and Bioavailability Measurements of Environmental Plutonium Using Diffusion in Thin Films

The biological uptake of plutonium (Pu) in aquatic ecosystems is of particular concern since it is an alpha-particle emitter with long half-life which can potentially contribute to the exposure of biota and humans. The diffusive gradients in thin films technique is introduced here for in-situ measurements of Pu bioavailability and speciation. A diffusion cell constructed for laboratory experiments with Pu and the newly developed protocol make it possible to simulate the environmental behavior of Pu in model solutions of various chemical compositions. Adjustment of the oxidation states to Pu(IV) and Pu(V) described in this protocol is essential in order to investigate the complex redox chemistry of plutonium in the environment. The calibration of this technique and the results obtained in the laboratory experiments enable to develop a specific DGT device for in-situ Pu measurements in freshwaters. Accelerator-based mass-spectrometry measurements of Pu accumulated by DGTs in a karst spring allowed determining the bioavailability of Pu in a mineral freshwater environment. Application of this protocol for Pu measurements using DGT devices has a large potential to improve our understanding of the speciation and the biological transfer of Pu in aquatic ecosystems.

The technique of diffusive gradients in thin films (DGT) is proposed for speciation studies of plutonium. This protocol describes diffusion experiments probing the behavior of Pu(IV) and Pu(V) in presence of organic matter. DGTs deployed in a karstic spring allow assessment of the bioavailability of Pu.

박막의 확산을 사용하여 환경 플루토늄의 분화 및 생체 이용률 측정

The biological uptake of plutonium (Pu) in aquatic ecosystems is of particular concern since it is an alpha-particle emitter with long half-life which can ...

Ohmic Contact Fabrication Using a Focused-ion Beam Technique and Electrical Characterization for Layer Semiconductor Nanostructures

Layer semiconductors with easily processed two-dimensional (2D) structures exhibit indirect-to-direct bandgap transitions and superior transistor performance, which suggest a new direction for the development of next-generation ultrathin and flexible photonic and electronic devices. Enhanced luminescence quantum efficiency has been widely observed in these atomically thin 2D crystals. However, dimension effects beyond quantum confinement thicknesses or even at the micrometer scale are not expected and have rarely been observed. In this study, molybdenum diselenide (MoSe2) layer crystals with a thickness range of 6-2,700 nm were fabricated as two- or four-terminal devices. Ohmic contact formation was successfully achieved by the focused-ion beam (FIB) deposition method using platinum (Pt) as a contact metal. Layer crystals with various thicknesses were prepared through simple mechanical exfoliation by using dicing tape. Current-voltage curve measurements were performed to determine the conductivity value of the layer nanocrystals. In addition, high-resolution transmission electron microscopy, selected-area electron diffractometry, and energy-dispersive X-ray spectroscopy were used to characterize the interface of the metal&#8211;semiconductor contact of the FIB-fabricated MoSe2 devices. After applying the approaches, the substantial thickness-dependent electrical conductivity in a wide thickness range for the MoSe2-layer semiconductor was observed. The conductivity increased by over two orders of magnitude from 4.6 to 1,500 &#937;&#8722;1 cm&#8722;1, with a decrease in the thickness from 2,700 to 6 nm. In addition, the temperature-dependent conductivity indicated that the thin MoSe2 multilayers exhibited considerably weak semiconducting behavior with activation energies of 3.5-8.5 meV, which are considerably smaller than those (36-38 meV) of the bulk. Probable surface-dominant transport properties and the presence of a high surface electron concentration in MoSe2 are proposed. Similar results can be obtained for other layer semiconductor materials such as MoS2 and WS2.

We describe the approaches for the device fabrication and electrical characterization of molybdenum diselenide (MoSe2) layer semiconductor nanostructures with different thicknesses. In addition, the fabrication of ohmic contacts for MoSe2-layer nanocrystals by the focused-ion beam deposition method using platinum (Pt) as a contact metal is described.

오믹 접촉 제조 집중 이온 빔 기술 및 전기 특성 계층 반도체 나노 구조를 위해 사용

Layer semiconductors with easily processed two-dimensional (2D) structures exhibit indirect-to-direct bandgap transitions and superior transistor ...

Synthesis and Functionalization of 3D Nano-graphene Materials: Graphene Aerogels and Graphene Macro Assemblies

Efforts to assemble graphene into three-dimensional monolithic structures have been hampered by the high cost and poor processability of graphene. Additionally, most reported graphene assemblies are held together through physical interactions (e.g., van der Waals forces) rather than chemical bonds, which limit their mechanical strength and conductivity. This video method details recently developed strategies to fabricate mass-producible, graphene-based bulk materials derived from either polymer foams or single layer graphene oxide. These materials consist primarily of individual graphene sheets connected through covalently bound carbon linkers. They maintain the favorable properties of graphene such as high surface area and high electrical and thermal conductivity, combined with tunable pore morphology and exceptional mechanical strength and elasticity. This flexible synthetic method can be extended to the fabrication of polymer/carbon nanotube (CNT) and polymer/graphene oxide (GO) composite materials. Furthermore, additional post-synthetic functionalization with anthraquinone is described, which enables a dramatic increase in charge storage performance in supercapacitor applications.

This video method describes the synthesis of high surface area, monolithic 3D graphene-based materials derived from polymer precursors as well as single layer graphene oxide.

합성 및 3D 나노 그래 핀 소재의 기능화 : 그래 핀 에어로젤과 그래 핀 매크로 어셈블리

Efforts to assemble graphene into three-dimensional monolithic structures have been hampered by the high cost and poor processability of graphene. ...

Synthesis of Ionic Liquid Based Electrolytes, Assembly of Li-ion Batteries, and Measurements of Performance at High Temperature

The chemical instability of the traditional electrolyte remains a safety issue in widely used energy storage devices such as Li-ion batteries. Li-ion batteries for use in devices operating at elevated temperatures require thermally stable and non-flammable electrolytes. Ionic liquids (ILs), which are non-flammable, non-volatile, thermally stable molten salts, are an ideal replacement for flammable and low boiling point organic solvent electrolytes currently used today. We herein describe the procedures to: 1) synthesize mono- and di-phosphonium ionic liquids paired with chloride or bis(trifluoromethane)sulfonimide (TFSI) anions; 2) measure the thermal properties and stability of these ionic liquids by differential scanning calorimetry (DSC) and thermal gravimetric analysis (TGA); 3) measure the electrochemical properties of the ionic liquids by cyclic voltammetry (CV); 4) prepare electrolytes containing lithium bis(trifluoromethane)sulfonamide; 5) measure the conductivity of the electrolytes as a function of temperature; 6) assemble a coin cell battery with two of the electrolytes along with a Li metal anode and LiCoO2 cathode; and 7) evaluate battery performance at 100 &#176;C. We additionally describe the challenges in execution as well as the insights gained from performing these experiments.

Here, we describe protocols to prepare phosphonium-based ionic liquid and lithium bis(trifluoromethane)sulfonimide salt electrolytes, and assemble a non-flammable and high temperature functioning lithium-ion coin cell battery.

이온 성 액체 기반 전해질의 합성 리튬 이온 배터리의 조립 및 고온에서의 성능 측정

The chemical instability of the traditional electrolyte remains a safety issue in widely used energy storage devices such as Li-ion batteries. Li-ion ...

Magnetically Induced Rotating Rayleigh-Taylor Instability

Classical techniques for investigating the Rayleigh-Taylor instability include using compressed gasses1, rocketry2 or linear electric motors3 to reverse the effective direction of gravity, and accelerate the lighter fluid toward the denser fluid. Other authorse.g. 4,5,6 have separated a gravitationally unstable stratification with a barrier that is removed to initiate the flow. However, the parabolic initial interface in the case of a rotating stratification imposes significant technical difficulties experimentally. We wish to be able to spin-up the stratification into solid-body rotation and only then initiate the flow in order to investigate the effects of rotation upon the Rayleigh-Taylor instability. The approach we have adopted here is to use the magnetic field of a superconducting magnet to manipulate the effective weight of the two liquids to initiate the flow. We create a gravitationally stable two-layer stratification using standard flotation techniques. The upper layer is less dense than the lower layer and so the system is Rayleigh-Taylor stable. This stratification is then spun-up until both layers are in solid-body rotation and a parabolic interface is observed. These experiments use fluids with low magnetic susceptibility, |&#967;| ~ 10-6 - 10-5, compared to a ferrofluids. The dominant effect of the magnetic field applies a body-force to each layer changing the effective weight. The upper layer is weakly paramagnetic while the lower layer is weakly diamagnetic. When the magnetic field is applied, the lower layer is repelled from the magnet while the upper layer is attracted towards the magnet. A Rayleigh-Taylor instability is achieved with application of a high gradient magnetic field. We further observed that increasing the dynamic viscosity of the fluid in each layer, increases the length-scale of the instability.

We present a protocol for preparing a two-layer density-stratified liquid that can be spun-up into solid body rotation and subsequently induced into Rayleigh-Taylor instability by applying a gradient magnetic field.

Classical techniques for investigating the Rayleigh-Taylor instability include using compressed gasses1, rocketry2 or linear electric motors3 to reverse ...

Focused Ion Beam Fabrication of LiPON-based Solid-state Lithium-ion Nanobatteries for In Situ Testing

Solid-state electrolytes are a promising replacement for current organic liquid electrolytes, enabling higher energy densities and improved safety of lithium-ion (Li-ion) batteries. However, a number of setbacks prevent their integration into commercial devices. The main limiting factor is due to nanoscale phenomena occurring at the electrode/electrolyte interfaces, ultimately leading to degradation of battery operation. These key problems are highly challenging to observe and characterize as these batteries contain multiple buried interfaces. One approach for direct observation of interfacial phenomena in thin film batteries is through the fabrication of electrochemically active nanobatteries by a focused ion beam (FIB). As such, a reliable technique to fabricate nanobatteries was developed and demonstrated in recent work. Herein, a detailed protocol with a step-by-step process is presented to enable the reproduction of this nanobattery fabrication process. In particular, this technique was applied to a thin film battery consisting of LiCoO2/LiPON/a-Si, and has further been previously demonstrated by in situ cycling within a transmission electron microscope.

Focused Ion Beam Fabrication of LiPON-based Solid-state Lithium-ion Nanobatteries for In Situ Testing

A protocol for the fabrication of electrochemically active LiPON-based solid-state lithium-ion nanobatteries using a focused ion beam is presented.

집중 된 이온 빔 제작 현장에서 테스트 LiPON 기반 고체 리튬-이온 Nanobatteries

Solid-state electrolytes are a promising replacement for current organic liquid electrolytes, enabling higher energy densities and improved safety of ...

Three-electrode Coin Cell Preparation and Electrodeposition Analytics for Lithium-ion Batteries

As lithium-ion batteries find use in high energy and power applications, such as in electric and hybrid-electric vehicles, monitoring the degradation and subsequent safety issues becomes increasingly important. In a Li-ion cell setup, the voltage measurement across the positive and negative terminals inherently includes the effect of the cathode and anode which are coupled and sum to the total cell performance. Accordingly, the ability to monitor the degradation aspects associated with a specific electrode is extremely difficult because the electrodes are fundamentally coupled. A three-electrode setup can overcome this problem. By introducing a third (reference) electrode, the influence of each electrode can be decoupled, and the electrochemical properties can be measured independently. The reference electrode (RE) must have a stable potential that can then be calibrated against a known reference, for example, lithium metal. The three-electrode cell can be used to run electrochemical tests such as cycling, cyclic voltammetry, and electrochemical impedance spectroscopy (EIS). Three-electrode cell EIS measurements can elucidate the contribution of individual electrode impedance to the full cell. In addition, monitoring the anode potential allows the detection of electrodeposition due to lithium plating, which can cause safety concerns. This is especially important for the fast charging of Li-ion batteries in electric vehicles. In order to monitor and characterize the safety and degradation aspects of an electrochemical cell, a three-electrode setup can prove invaluable. This paper aims to provide a guide to constructing a three-electrode coin cell setup using the 2032-coin cell architecture, which is easy to produce, reliable, and cost-effective.

Three-electrode cells are useful in studying the electrochemistry of lithium-ion batteries. Such an electrochemical setup allows the phenomena associated with the cathode and anode to be decoupled and examined independently. Here, we present a guide for construction and use of a three-electrode coin cell with emphasis on lithium plating analytics.

3 전극 동전 전지 준비 및 Electrodeposition 리튬-이온 배터리에 대 한 분석

As lithium-ion batteries find use in high energy and power applications, such as in electric and hybrid-electric vehicles, monitoring the degradation and ...