The authors acknowledge financial support from the Engineering and Physical Sciences Research Council, UK under the Program Grant 'Supercritical Fluid Electrodeposition' (EP/J016276/1). J.S. and R.J.K. are indebted to the Warwick Centre for Analytical Science (EPSRC funded Grant EP/F034210/1). Additionally, we are indebted to Drs. Zheng Liu and Kazu Suenaga who provided the top right part of Panel d of Figure 1, which originally appeared in Microsc. Semicond. Mater. 2008, 120, 213-216 (used with permission).

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The authors have nothing to disclose.

연구의 거대한 양의 나노 와이어에 완료되었습니다 동안 가장 작은 직경의 근본적인 제한이 가능, 극단적 인 나노 와이어를 나노 와이어, 거의 탐구 없습니다. 예들은 자신의 모재의 완전히 새로운 결정형을 나타낼 수 있으며, 이미 이러한 나노 와이어의 특성도 약간 큰 직경의 나노 와이어와 연속체를 형성하지 않는 것이 밝혀졌다. 각 부모 가능한 모재의 그 다수를 고려하면 물리 거대 많은 이상의 극단적 인 나노 와이어를 수 나노 와이어의 폭을 생산할 수있다. 이들의 제조 방법은 잘 확립되어 있지 않으므로 극단적 나노 와이어 연구가 여전히 초기 단계에 있다는 사실은 아니다. 이 논문에 제시된 용융 침투 과정은 신뢰성과 용융 침투가 특정 작성을위한 최적이 아닌 경우 사용할 수있는 여러 그룹 및 승화 작성 등의 다른 방법으로 사용되어왔다. 부분에서필드 비파괴 극단적 나노 와이어의 특성을 비교적 간단하고 광범위하게 적용 가능한 방법의 부족에 의해 다시 유지된다. 카본 나노 튜브의 필드는 임의의 가이드 인 경우, 라만 분광법이 문제를 해결하기위한 선택의 방법이라는 좋은 기회를 가진다. 극단적 나노 유용한 라만 스펙트럼을 얻기위한 키가 라만 산란의 다른 1D 공진 시스템 강화와 공통 것을 인식하는 것은 임의의 산란을 관찰하기위한 필요 조건이다. 특정 샘플 형태의 전체의 공진 동작이 측정을 빠르게 할 시료의 특성에 라만 대부분의 애플리케이션에 고정 공진 여기 에너지를 사용하여 비용을 절감 할 수있다,이 프로토콜에서 제시된 방법을 사용하여 결정되면 라만 시스템 요구. 이 논문에 제시된 결과에 나타낸 바와 같이 극단적 인 나노 와이어에 높은 품질의 공명 라만 결과를 얻는 중요한 문제입니다재현 고정밀 며칠 동안 가변 레이저의 빔을 다시 정렬 할 필요가있다. 이 실험에서 가장 중요한 세부 실험 시스템 및 관심 특히 수정을 요구; 정확한 광학 시스템의 초점 현미경 대물 시료 중 횡 이동을 정확하게 교정 할 수있는 능력 상에 레이저 빔의 정확한 정렬. 기술은이 양식이 논문의 기초를 달성하기 위해 개발했다. 기타 벌크 및 양자 우물 시스템 광범위한 기술을 적용한 예로서 M. 카르 도나 선구자 포함 공진 라만 실험의 재현성을 개선하기위한 방법 및 시스템을 개발 하였다. 우리의 기술은 M. Dresselhaus (21)를 포함하는 탄소 나노 튜브의 라만의 개척자의 일에 작성합니다. 그러나 여기에 제시된 프로토콜은 극단적 나노 와이어 공명 라만 실험에 특히 적합하다. 의 S의 핵심프로토콜 uccess는도 10에 도시 된 실험 시스템의 개발이었다. 도면은 프로토콜에 설명 된 라만 실험에서 사용한 광 셋업의 평면도를 보여준다. 레이저 광은 프로토콜에 따라 그라 이오 스탯에 밀봉 된 샘플시 50X 목표 (라벨 OB)를 통해 초점을 맞추고 있습니다. 이 저온 유지 장치는 재배치 및 포커싱을 위해 샘플의 3 차원 적 움직임을 허용하는 XYZ 스테이지 상에 장착된다. 레이저 광이 A 및 B (a 펌프 소스 및 Ti 인 : 각각 사파이어)를 통해 생성되고, 레이저의 정확한 세부 사항은 제공되는 재료 문헌에 언급되어있다. 상업적인 레이저 라인 필터를 사용하는 경우 (성분 C)의 레이저 광은 조리개 (1) 및 (2) 시준 렌즈를 사용하여도 1 및 2 (L1 및 L2)의 중앙을 통해 지향된다. 광은 프로토콜에 설명 된대로, 1/2 파장 판 및 편광판 (HWP1 및 POL1) PM2에 편광 레이저 파워 입사면을 제어하기 위해 통과한다. 레이저 빛이 통과가변 필터, C, 및 거울 M1 및 M2를 사용을 통해, 그것은 대물 (OB)의 배면에 수직 및 카메라 C1 및 C2를 중심으로되도록 정확한 광로 상 스티어링. ND 필터는 집중 절차 (단계 9.9)을 수행 할 수 있도록, 전력 미터, PM1 상 대물로부터 다시 반사 된 빔을 위치시키기 위해 사용된다. 샘플로부터 위로 산란광 수집 및 분석 장치에 3 렌즈 (L3) 및 슬릿 (1)를 통해 전달된다. 렌즈의 슬릿 폭과 위치를 조정하면, 레이저 파장, 레이저 선 벗어나면 프로토콜 8 항에 설명 된대로, 라만 신호를 최대화하는 것이 중요하다 필터링 동작 범위, 볼륨 브래그 설치 섹션 8.2에 따라 이용해야 .1-8.2.3. 이 광학 셋업은도 10에 따라, 검은 색 점선에 따라 변경되고, 미러 M3 경로에서 제거하는 것이 중요하다. 편광 의존하는 실험에 착수하면 마지막으로, 그것은 중요하다편광을 제어하고 분광계 입력 편광 유지, 이것은도 10에서 보라색 점선으로 강조 셋업에 추가 될 프로토콜과 구성 요소 (12)에 대해서 설명한다. 청색은도 10에 점선은 구성 요소를 지시 프로토콜 부 (14)로 나타낸 바와 같이, 시료의 라이브 영상을 허용했다. 모든 실험 방법과 마찬가지로 공명 라만 산란는 한계가있다. 특히, 가능한 파장 가변 레이저 소스 및 검출기는 적외선 내로 연장하지만 상기 스펙트럼 범위에서 수행 할 350-1,000 나노 훨씬 용이하고 UV 가능하다는 것을 의미한다. 조정 가능한 소스와 라만 산란을 수행하는 데 필요한 실험 시스템은 합리적인 추정이 발행 당시 £ 200-300k되는 저렴한 없습니다. 또한 필요한 시스템의 복잡성은 광에 익숙를 필요로한다는 것을 의미분광법은 성공적으로 작동합니다. 그러나 라만 산란은 다른 기술로 수득하기 어려운 정보의 조합을 제공한다. 놀랍게도 아직 임의의 다른 기술에 의해 달성 될 수있는 개별 단일 벽 탄소 나노 튜브의 라만 산란, 따라서 진동 에너지를 얻을 수있다. 이제 나노 와이어의 공명이 라만 산란의 가능한 정보의 범위를 열어 결정하기 시작하고있다. 우리의 의견 확장자는 전기 화학적으로 이들 물질을 이해하는데 중요한 것이다 전하 밀도의 넓은 범위의 나노 와이어에 대한 측정을 허용 4 36 K까지 온도가 극단적 나노 와이어 (20)를 게이트한다. 마지막으로 더욱 제조 할 수있는 샘플의 품질을 최적화시킬 수있는 극단적 인 나노 와이어의 구조 및 용융 전이를 이해하는 라만 산란을 이용하여.

라만 분광법과 공명 라만 분광법 널리 과학적 및 기술적으로 악용되어 잘 확립 된 기술이다. 1928 제 1 라만 스스로보고 동안 라만 분광기의 광범위한 보급 이용에 키 고강도, 협 대역 여기 소스를 제공하는 레이저 라만 공명의 경우 가변 파장 레이저의 개발이었다. 공명 라만 산란이 ~ 1-5 원자의 직경, 예를 들어 나노 와이어를 기본 물리학을 조사하고 일반 및 극단적 인 나노 와이어에 1D 시스템의 샘플을 특성화를위한 특히 중요한 방법입니다 왜이 논문은 제시한다. 또한 라만 분광법 등 나노 와이어 및 이들 극복함으로써, 이러한 시스템에서의 라만 산란 효율의 레이저 에너지 의존성 높은 반복 측정을 달성 할 수 있도록하는 프로토콜의 특별한 어려움을 설명한다. exte 다양한가연구와 응용 프로그램을 사용할 수 또한 나노 와이어로 알려진 nded, 결정 1D 양자 시스템. 이 증기 - 액체 - 고체 성장 된 반도체 나노 와이어 2, 리소그래피 정의 나노 와이어 (3), 양극 알루미나를 포함하고 에칭 막 템플릿 나노 와이어 (4) 다른 사람을 추적 할 수 있습니다. 이러한 시스템에 대한 관심이 중요한 이유는 구성에 따라 자유롭게 이동하는 전자와 다른 음원 정보 능력 큰 양자 구속 효과를 결합한다는 것이다. 어떤면에서, 나노 와이어 인해 자유 전하 (5) 전자파 차단 등을 감소 상위 재료는 상당히 상이하고, 어떤 경우에는 탄도 수송 6 선도 전자 산란을 감소시켰다. 그러나, 많은 점에서 나노 와이어는 여전히 로컬 본딩 결정 구조 예와 같은 일괄되고, 거의 항상 원자 수준에서 전자파 함수의 기본적인 품질을 약하게하므로 대량 ​​비해 수정봉투 근사 것을 7 유효합니다. 밀폐 방향의 치수가 몇 원자 감소하지만 같은 완전히 새로운 결합을 가진 나노 와이어는 결코 이전에 본 적이 동소체 8-10을 형성 발생할 수 있습니다. 이 나노 와이어는이 감각의 극단적; 그들은 단면 11 ~ 13의 수 감소의 극단적 인 한계 그리고 그들은 극단적 인 특성 10,13,14 있습니다. 공명 라만 분광법에 착수하기 전에, 극단적 인 나노 와이어 샘플을 생성하기 위해 필요하다. 이러한 나노 와이어를 생성하기 위해 본 논문에 제시된 방법론은 단일 벽 탄소 나노 튜브로 재료의 용융 침투입니다. 용해 침투하면 가장 최근에 (즉, 풀러렌) 일부 이진 염을 연속적으로 충전 단층 카본 나노 튜브 (SWNT), 일부 분자의 도입에 대한 인기가 다른 하나의 승화를 얻기 위해 사용되는 두 고 수율 충전 프로토콜 중 하나 인 한 CsI (13). 후자의 방법은 정량 충전 근처 생성하지만,이 재료는 크게 SWNT로 도입 될 수 충전재의 수와 유형을 제한해야하는 쉽게 승화를 도입하는 것을 제한한다. 용융 침투 충전 프로토콜 조심 정량 충전 (15) 근방에 생성하기 위해 사용되며, 승화 프로토콜보다 적은 제약을 보유 할 수있다. 이들 재료가 호스트 벽 탄소 나노 튜브의 손상을 방지하기 위해, 표면 장력보다 낮은 100 ~ 200 백만 m -1 내지 약 1300 K 이하의 용융 온도를 가져야한다. 16 투과 전자 현미경 (TEM)을 카본 나노 튜브의 충전 품질을 특성화하고 생성 된 나노 극도의 결정 구조 또는 구조들을 식별하는 가장 좋은 방법이다. HRTEM 이미지에서 SWNT 매립 결정 단편의 구조를 해결하는 시험 결정 단편 모드에서 이미지 시뮬레이션 사이의 시행 착오 비교를 포함ELS와 실험적으로 얻어진 이미지의 대비. 이 논문은 자신의 분광 특성에 대한 서두로서 HRTEM 이미지 시뮬레이션에 의한 SWNT 샘플의 극단적 인 나노 와이어 모티브의 미세 구조를 확인하기위한 프로토콜을 설명합니다. 공명 라만 분광기 (17)가 이상적인 도구 모두 공진 에너지는 나노 와이어 샘플의 종류와 품질을 특성화를 위해 결정되고 나면 극단적 나노 와이어의 기본 물리학 및 이해를위한. 기본적으로, 공명 라만는 모두 광학 및 진동 여기 에너지 (17)의 직접적인 결정을 할 수 있습니다. 공진의 광자 에너지 의존성을 추가로 모델링는 전자 포논 상호 작용 (17)을 계량 할 수있다. 공명 에너지는 특히 극단적 인 나노 결정 되었으면, 나노 와이어의 라만 스펙트럼은 18 변형을 추적하는데 사용될 수 있고 구조적 위상 인해 19 변경온도, 수압 또는 와이어의 굽힘. 아직 입증하는 동안, 몇 가지 자기 극단적 인 나노 와이어에서 가진에 그들을 탐색 할 수 있도록 라만 산란으로 이어질 것 스핀 가능성이 높습니다. spectroelectrochemical 셀에 유지 샘플 라만 산란 연장 극단적 나노 튜브와 호스트 (20) 사이의 전하 전송을 검사하는데 사용될 수있다. 특성화 도구로서 라만 분광법은 나노 와이어 종류와 품질 (21)의 비접촉, 비파괴 측정하는 방법을 제공한다. 그것은 제조 및 / 또는 정제 후 샘플을 특성화하기위한 도구로서 이용 될 수있는 나노 와이어 트랜지스터 또는 적어도 부분적으로 투명 필요한 광자 에너지에있다 복합체와 같은 장치에 포함 된 경우에도. 공명 라만 산란 (RRS)에 대한 직접적인 대안을 제공 할 수있는 하나의 기술은 없다; 그러나 일부 ASPE 중첩 다른 기술의 범위에있다기능의 캐럿이 방법. 극단적 나노 UV-VIS-NIR 흡수 측정 22 쿠폰보다 간단한 기술의 광학 천이 에너지를 결정하는 조건이다. 그러나 특정 구조와 연관된 세트로 다른 광학 기능을 분리 할 수​​있는 다른 구조의 흡광의 앙상블 샘플이다. 공명 라만 산란 광과 진동 스펙트럼의 연결이 때문에 달성 할 수있다. 자외선 VIS-NIR 흡수 측정 하이라이트 공명 라만 에너지 타겟팅 된 두 기술의 조합은 상당히 전체 공정을 단축 할 수있다. 여기 광 발광 스펙트럼 (PLE) (23)는 하나의 샘플에서 상이한 광학 전이를 연결하는 기능을 제공하며; 그러나는 특히 비 - 금속 나노 와이어 일부 작동하며 RRS보다 수행 약간 덜 복잡하며 일반적으로 ENVIRO으로부터 보호 단 분산 샘플을 필요nment 완전히 성공합니다. PLE는 달리, 공명 라만 분광법은 번들과 단 분산 샘플과 동일하게 작동하기 때문에 작은 샘플 준비가 필요합니다. 아직 약간의 사용 동안, 투과 전자 현미경 (TEM) 연구 스펙트럼 범위 내에서 와이어의 광 여기 에너지를 모두 파악하고, 특정 나노 와이어 구조를 식별 할 수있는 나노 와이어의 구조를 분석 하였다 개별 나노 와이어 (24)의 레일리 산란 분광법 . 그러나,이 기술은 RRS와 가능한 진동 에너지 정보를 제공하지 않는다; 수행하는 것은 매우 도전 결코 일반적인 특성 도구로 적합 할 것 없습니다. 진동 에너지 정보의 관점에서 유일하게 현재 가능한 대안은 그러나이 진동 에너지의 다른 세트를 조사함으로써 보완이 아닌 경쟁하기 때문에 선택 규칙에, 가능성이 IR 분광법 (25)이다. 또한 IR은이야pectroscopy는 UV-VIS-NIR 흡수 측정과 같은 앙상블 샘플과 같은 문제에서 겪게됩니다. 이미 설명한 바와 같이 라만 분광법 과학 내의 광범위한 문제에 적용되어왔다. 분자 시스템에서는 재료의 조성을 분석하는 핑거 프린팅 기법으로도 진동 스펙트럼을 결정하고 대한 IR 스펙트럼을 보완하기 위해 사용된다. 그것은 널리 예를 들어 결정 시스템에 이용 된 책의 솔리드 시리즈의 광산란은 구 볼륨이 포함됩니다. 3D 및 2D 시스템의 경우, 공진 여진 표준 선택 규칙의 붕괴와 상호 작용을 정량화하는 능력 선도 라만 프로세스 내의 특정 광학 전이의 기여를 향상시키기위한 전체 산란 강도 등을 향상시키기위한 이하 사용 특정 전자 상태와 라만 스펙트럼에서 관찰의 기진. 보다 최근 라만 분광법이있다 중앙 t카본 나노 튜브, 특히 단일 벽 탄소 나노 튜브의 연구 O. 카본 나노 튜브 연구 21 (1D) 시스템의 공진이 여기 차원 및 3 차원 시스템에 대한 라만 대부분의 애플리케이션대로 선택적 아니지만 반드시 필요하다는 점을 강조하고있다. 비 공진 라만 산란이 관찰되기에 너무 약한 여진 특별히 1D 시스템의 특징있는 상태의 광학 밀도의 강한 반 호브 특이성, 공진 때만 그 때문, 임의 라만 스펙트럼 그 관찰 될 수있다. 따라서, 극단적 인 나노 와이어의 경우에는 라만 분광기의 사용은 라만 분광법이 물질을 연구에 적용되기 전에 샘플의 나노 와이어 모두의 공진을 찾기 위해 전체 공명 라만 측정을 필요로한다.

<table>
	<tbody>
		<tr>
			<td>Carbon Nanotubes</td>
			<td>Nanointegris</td>
			<td>NI96</td>
			<td></td>
		</tr>
		<tr>
			<td>Carbon Nanotubes</td>
			<td>Private</td>
			<td></td>
			<td>Synthesis described in Eurasian Chem.-Technol. J. 2005, 5, 7-18.</td>
		</tr>
		<tr>
			<td>Mercury Telluride</td>
			<td>VMR</td>
			<td></td>
			<td>99.999% metals basis</td>
		</tr>
		<tr>
			<td>Silica Quartz Tubing</td>
			<td>H. Baumbach &#38; Co.&#160;</td>
			<td></td>
			<td>Various diameters and lengths used - typically 1 cm OD, 0.8 cm ID and 8cm long.&#160;</td>
		</tr>
		<tr>
			<td>Tube furnace</td>
			<td>Carbolite</td>
			<td>&#160;MTF-12/38/250</td>
			<td></td>
		</tr>
		<tr>
			<td>JEOL ARM 200F&#160;</td>
			<td>JEOL&#160;</td>
			<td></td>
			<td>200 kV High Resolution TEM Operated at 80 kV and equipped with&#160;</td>
		</tr>
		<tr>
			<td></td>
			<td></td>
			<td></td>
			<td>CEOS hardware spherical aberation (Cs) imaging corrector. Cs corrected&#160;</td>
		</tr>
		<tr>
			<td></td>
			<td></td>
			<td></td>
			<td>to 0.001 mm.</td>
		</tr>
		<tr>
			<td>SC1000 ORIUS camera</td>
			<td>Gatan</td>
			<td></td>
			<td>Size of CCD 4008 x 2672</td>
		</tr>
		<tr>
			<td>Digital Micrograph Suite 2.31</td>
			<td>Gatan</td>
			<td></td>
			<td>64 bit version</td>
		</tr>
		<tr>
			<td>XMax X-ray Microanalysis&#160;</td>
			<td>Oxford Instruments</td>
			<td></td>
			<td>This detector uses the silicon drift detection (SDD) principle. 1 nm diameter electron probe.</td>
		</tr>
		<tr>
			<td></td>
			<td></td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>Crystalmaker Ver 8.7</td>
			<td>Crystalmaker</td>
			<td></td>
			<td>Used for assembling crystal fragments for image simulations</td>
		</tr>
		<tr>
			<td>Nanotube Modeler</td>
			<td colspan="2">JCrystalSoft &#169;2015-2015</td>
			<td>Used for generating Nanotube models</td>
		</tr>
		<tr>
			<td>SimulaTEM</td>
			<td>Private</td>
			<td></td>
			<td>Ultramicroscopy, 2010, 110, 95-104.</td>
		</tr>
		<tr>
			<td></td>
			<td></td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>Verdi V8 Pump</td>
			<td>Coherent</td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>Mira 900 Ti:Sapphire</td>
			<td>Coherent</td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>Volume Bragg Grating</td>
			<td>Optigrate</td>
			<td></td>
			<td>Specfication between 680-720nm</td>
		</tr>
		<tr>
			<td>Photonetc TLS 850 LLTF&#160;</td>
			<td>Photonetc</td>
			<td></td>
			<td>Tunable between 700-1000nm</td>
		</tr>
		<tr>
			<td>LMPLAN IR50x MircoscopeObjective</td>
			<td>Olympus</td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>Cryostat</td>
			<td>Oxford Instruments</td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>Triple Raman Spectrometers</td>
			<td>Princeton Instruments</td>
			<td></td>
			<td>triple 600nm using gratings 900, 900, 1800 lines/mm</td>
		</tr>
		<tr>
			<td>CCD</td>
			<td>Princeton Instruments</td>
			<td></td>
			<td>deep depleted, UV enchanced liquid N2 Cooled Silicon CCD</td>
		</tr>
	</tbody>
</table>

resonance raman spectroscopy of extreme nanowires and other 1d systems

This paper briefly describes how nanowires with diameters corresponding to 1 to 5 atoms can be produced by melting a range of inorganic solids in the presence of carbon nanotubes. These nanowires are extreme in the sense that they are the limit of miniaturization of nanowires and their behavior is not always a simple extrapolation of the behavior of larger nanowires as their diameter decreases. The paper then describes the methods required to obtain Raman spectra from extreme nanowires and the fact that due to the van Hove singularities that 1D systems exhibit in their optical density of states, that determining the correct choice of photon excitation energy is critical. It describes the techniques required to determine the photon energy dependence of the resonances observed in Raman spectroscopy of 1D systems and in particular how to obtain measurements of Raman cross-sections with better than 8% noise and measure the variation in the resonance as a function of sample temperature. The paper describes the importance of ensuring that the Raman scattering is linearly proportional to the intensity of the laser excitation intensity. It also describes how to use the polarization dependence of the Raman scattering to separate Raman scattering of the encapsulated 1D systems from those of other extraneous components in any sample.

Watch this Scientific Journal Video about Resonance Raman Spectroscopy of Extreme Nanowires and Other 1D Systems at JoVE.com

Resonance Raman Spectroscopy of Extreme Nanowires and Other 1D Systems

The paper describes a method for producing extreme nanowires by melt infiltration into carbon nanotubes and how 1D systems may be characterized and investigated using Resonance Raman Spectroscopy to determine vibrational and optical excitation energies.

극단적 인 나노 와이어 및 기타 1D 시스템의 공명 라만 분광법

This paper briefly describes how nanowires with diameters corresponding to 1 to 5 atoms can be produced by melting a range of inorganic solids in the ...

resonance-raman-spectroscopy-of-extreme-nanowires-and-other-1d-systems

Research

JoVE Journal

Engineering

15.0K 조회수.  University of Southampton. The paper describes a method for producing extreme nanowires by melt infiltration into carbon nanotubes and how 1D systems may be characterized and investigated using Resonance Raman Spectroscopy to determine vibrational and optical excitation energies.

비디오: Resonance Raman Spectroscopy of Extreme Nanowires and Other 1D Systems

Synthesis and Microdiffraction at Extreme Pressures and Temperatures

High pressure compounds and polymorphs are investigated for a broad range of purposes such as determine structures and processes of deep planetary interiors, design materials with novel properties, understand the mechanical behavior of materials exposed to very high stresses as in explosions or impacts. Synthesis and structural analysis of materials at extreme conditions of pressure and temperature entails remarkable technical challenges. In the laser heated diamond anvil cell (LH-DAC), very high pressure is generated between the tips of two opposing diamond anvils forced against each other; focused infrared laser beams, shined through the diamonds, allow to reach very high temperatures on samples absorbing the laser radiation. When the LH-DAC is installed in a synchrotron beamline that provides extremely brilliant x-ray radiation, the structure of materials under extreme conditions can be probed in situ. LH-DAC samples, although very small, can show highly variable grain size, phase and chemical composition. In order to obtain the high resolution structural analysis and the most comprehensive characterization of a sample, we collect diffraction data in 2D grids and combine powder, single crystal and multigrain diffraction techniques. Representative results obtained in the synthesis of a new iron oxide, Fe4O5 1 will be shown.

The laser heated diamond anvil cell combined with synchrotron micro-diffraction techniques allows researchers to explore the nature and properties of new phases of matter at extreme pressure and temperature (PT) conditions. Heterogeneous samples can be characterized in situ under high pressure by 2D mapping and combined powder, single-crystal and multigrain diffraction approaches.

극단적 인 압력과 온도에서 합성 부위 회절

High pressure compounds and polymorphs are investigated for a broad range of purposes such as determine structures and processes of deep planetary ...

연구

공학

Ultrahigh Density Array of Vertically Aligned Small-molecular Organic Nanowires on Arbitrary Substrates

In recent years &pi;-conjugated organic semiconductors have emerged as the active material in a number of diverse applications including large-area, low-cost displays, photovoltaics, printable and flexible electronics and organic spin valves. Organics allow (a) low-cost, low-temperature processing and (b) molecular-level design of electronic, optical and spin transport characteristics. Such features are not readily available for mainstream inorganic semiconductors, which have enabled organics to carve a niche in the silicon-dominated electronics market. The first generation of organic-based devices has focused on thin film geometries, grown by physical vapor deposition or solution processing. However, it has been realized that organic nanostructures can be used to enhance performance of above-mentioned applications and significant effort has been invested in exploring methods for organic nanostructure fabrication.	
A particularly interesting class of organic nanostructures is the one in which vertically oriented organic nanowires, nanorods or nanotubes are organized in a well-regimented, high-density array. Such structures are highly versatile and are ideal morphological architectures for various applications such as chemical sensors, split-dipole nanoantennas, photovoltaic devices with radially heterostructured "core-shell" nanowires, and memory devices with a cross-point geometry. Such architecture is generally realized by a template-directed approach. In the past this method has been used to grow metal and inorganic semiconductor nanowire arrays. More recently &pi;-conjugated polymer nanowires have been grown within nanoporous templates. However, these approaches have had limited success in growing nanowires of technologically important &pi;-conjugated small molecular weight organics, such as tris-8-hydroxyquinoline aluminum (Alq3), rubrene and methanofullerenes, which are commonly used in diverse areas including organic displays, photovoltaics, thin film transistors and spintronics.	
Recently we have been able to address the above-mentioned issue by employing a novel "centrifugation-assisted" approach. This method therefore broadens the spectrum of organic materials that can be patterned in a vertically ordered nanowire array. Due to the technological importance of Alq3, rubrene and methanofullerenes, our method can be used to explore how the nanostructuring of these materials affects the performance of aforementioned organic devices. The purpose of this article is to describe the technical details of the above-mentioned protocol, demonstrate how this process can be extended to grow small-molecular organic nanowires on arbitrary substrates and finally, to discuss the critical steps, limitations, possible modifications, trouble-shooting and future applications.

We report a simple method for fabricating an ultrahigh density array of vertically ordered small-molecular organic nanowires. This method allows for synthesis of complex heterostructured hybrid nanowire geometries, which can be inexpensively grown on arbitrary substrates. These structures have potential applications in organic electronics, optoelectronics, chemical sensing, photovoltaics and spintronics.

임의 기판에 수직으로 정렬 작은 분자 유기 나노 와이어의 초 밀도 배열

In  recent years &pi;-conjugated  organic semiconductors have emerged as the active material in a number of  diverse applications including large-area, ...

Monolayer Contact Doping of Silicon Surfaces and Nanowires Using Organophosphorus Compounds

Monolayer Contact Doping (MLCD) is a simple method for doping of surfaces and nanostructures1. MLCD results in the formation of highly controlled, ultra shallow and sharp doping profiles at the nanometer scale. In MLCD process the dopant source is a monolayer containing dopant atoms.
In this article a detailed procedure for surface doping of silicon substrate as well as silicon nanowires is demonstrated. Phosphorus dopant source was formed using tetraethyl methylenediphosphonate monolayer on a silicon substrate. This monolayer containing substrate was brought to contact with a pristine intrinsic silicon target substrate and annealed while in contact. Sheet resistance of the target substrate was measured using 4 point probe. Intrinsic silicon nanowires were synthesized by chemical vapor deposition (CVD) process using a vapor-liquid-solid (VLS) mechanism; gold nanoparticles were used as catalyst for nanowire growth. The nanowires were suspended in ethanol by mild sonication. This suspension was used to dropcast the nanowires on silicon substrate with a silicon nitride dielectric top layer. These nanowires were doped with phosphorus in similar manner as used for the intrinsic silicon wafer. Standard photolithography process was used to fabricate metal electrodes for the formation of nanowire based field effect transistor (NW-FET). The electrical properties of a representative nanowire device were measured by a semiconductor device analyzer and a probe station.

A detailed procedure for surface doping of Silicon interfaces is provided. The ultra-shallow surface doping is demonstrated by using phosphorus containing monolayers and rapid annealing process. The method can be used for doping of macroscopic area surfaces as well as nanostructures.

유기 화합물을 사용하여 실리콘 표면과 나노 와이어의 단층 연락 도핑

Monolayer Contact Doping (MLCD) is a simple method for doping of surfaces and nanostructures1. MLCD results in the formation of highly controlled, ultra ...

Evaluating Plasmonic Transport in Current-carrying Silver Nanowires

Plasmonics is an emerging technology capable of simultaneously transporting a plasmonic signal and an electronic signal on the same information support1,2,3. In this context, metal nanowires are especially desirable for realizing dense routing networks4. A prerequisite to operate such shared nanowire-based platform relies on our ability to electrically contact individual metal nanowires and efficiently excite surface plasmon polaritons5 in this information support. In this article, we describe a protocol to bring electrical terminals to chemically-synthesized silver nanowires6 randomly distributed on a glass substrate7. The positions of the nanowire ends with respect to predefined landmarks are precisely located using standard optical transmission microscopy before encapsulation in an electron-sensitive resist. Trenches representing the electrode layout are subsequently designed by electron-beam lithography. Metal electrodes are then fabricated by thermally evaporating a Cr/Au layer followed by a chemical lift-off. The contacted silver nanowires are finally transferred to a leakage radiation microscope for surface plasmon excitation and characterization8,9. Surface plasmons are launched in the nanowires by focusing a near infrared laser beam on a diffraction-limited spot overlapping one nanowire extremity5,9. For sufficiently large nanowires, the surface plasmon mode leaks into the glass substrate9,10. This leakage radiation is readily detected, imaged, and analyzed in the different conjugate planes in leakage radiation microscopy9,11. The electrical terminals do not affect the plasmon propagation. However, a current-induced morphological deterioration of the nanowire drastically degrades the flow of surface plasmons. The combination of surface plasmon leakage radiation microscopy with a simultaneous analysis of the nanowire electrical transport characteristics reveals the intrinsic limitations of such plasmonic circuitry.

Silver nanowires can simultaneously transport electrons and optical information in the form of surface plasmons. A procedure is described here to realize such a shared circuitry and the limitations at propagating both information carriers are evaluated.

Plasmonics is an emerging technology capable of simultaneously transporting a plasmonic signal and an electronic signal on the same information ...

Preparation and Use of Photocatalytically Active Segmented Ag|ZnO and Coaxial TiO2-Ag Nanowires Made by Templated Electrodeposition

Photocatalytically active nanostructures require a large specific surface area with the presence of many catalytically active sites for the oxidation and reduction half reactions, and fast electron (hole) diffusion and charge separation. Nanowires present suitable architectures to meet these requirements. Axially segmented Ag|ZnO and radially segmented (coaxial) TiO2-Ag nanowires with a diameter of 200 nm and a length of 6-20 &#181;m were made by templated electrodeposition within the pores of polycarbonate track-etched (PCTE) or anodized aluminum oxide (AAO) membranes, respectively. In the photocatalytic experiments, the ZnO and TiO2 phases acted as photoanodes, and Ag as cathode. No external circuit is needed to connect both electrodes, which is a key advantage over conventional photo-electrochemical cells. For making segmented Ag|ZnO nanowires, the Ag salt electrolyte was replaced after formation of the Ag segment to form a ZnO segment attached to the Ag segment. For making coaxial TiO2-Ag nanowires, a TiO2 gel was first formed by the electrochemically induced sol-gel method. Drying and thermal annealing of the as-formed TiO2 gel resulted in the formation of crystalline TiO2 nanotubes. A subsequent Ag electrodeposition step inside the TiO2 nanotubes resulted in formation of coaxial TiO2-Ag nanowires. Due to the combination of an n-type semiconductor (ZnO or TiO2) and a metal (Ag) within the same nanowire, a Schottky barrier was created at the interface between the phases. To demonstrate the photocatalytic activity of these nanowires, the Ag|ZnO nanowires were used in a photocatalytic experiment in which H2 gas was detected upon UV illumination of the nanowires dispersed in a methanol/water mixture. After 17 min&#160;of illumination, approximately 0.2 vol% H2 gas was detected from a suspension of ~0.1 g of Ag|ZnO nanowires in a 50 ml 80 vol% aqueous methanol solution.

Preparation and Use of Photocatalytically Active Segmented Ag|ZnO and Coaxial TiO2-Ag Nanowires Made by Templated Electrodeposition

Procedures are outlined to prepare segmented and coaxial nanowires via templated electrodeposition in nanopores. As examples, segmented nanowires consisting of Ag and ZnO segments, and coaxial nanowires consisting of a TiO2 shell and a Ag core were made. The nanowires were used in photocatalytic hydrogen formation experiments.

준비 및 광촉매 활성 분단 자세의 사용 | ZnO의 동축 티오<sub&gt; 2</sub템플릿 기반 전착에 의해 만들어진&gt; - 자세 나노 와이어

Photocatalytically active nanostructures require a large specific surface area with the presence of many catalytically active sites for the oxidation and ...

High-Sensitivity Nuclear Magnetic Resonance at Giga-Pascal Pressures: A New Tool for Probing Electronic and Chemical Properties of Condensed Matter under Extreme Conditions

Nuclear Magnetic Resonance (NMR) is one of the most important techniques for the study of condensed matter systems, their chemical structure, and their electronic properties. The application of high pressure enables one to synthesize new materials, but the response of known materials to high pressure is a very useful tool for studying their electronic structure and developing theories. For example, high-pressure synthesis might be at the origin of life; and understanding the behavior of small molecules under extreme pressure will tell us more about fundamental processes in our universe. It is no wonder that there has always been great interest in having NMR available at high pressures. Unfortunately, the desired pressures are often well into the Giga-Pascal (GPa) range and require special anvil cell devices where only very small, secluded volumes are available. This has restricted the use of NMR almost entirely in the past, and only recently, a new approach to high-sensitivity GPa NMR, which has a resonating micro-coil inside the sample chamber, was put forward. This approach enables us to achieve high sensitivity with experiments that bring the power of NMR to Giga-Pascal pressure condensed matter research. First applications, the detection of a topological electronic transition in ordinary aluminum metal and the closing of the pseudo-gap in high-temperature superconductivity, show the power of such an approach. Meanwhile, the range of achievable pressures was increased tremendously with a new generation of anvil cells (up to 10.1 GPa), that fit standard-bore NMR magnets. This approach might become a new, important tool for the investigation of many condensed matter systems, in chemistry, geochemistry, and in physics, since we can now watch structural changes with the eyes of a very versatile probe.

Nuclear magnetic resonance is one of the most important spectroscopic tools. Here, the development of a new approach under high pressure, currently up to 10.1 GPa, is presented. This opens a new window into condensed matter physics and chemistry, where high-pressure research is of great importance.

극한의 상황에서도 응집 물질의 전자 화학적 특성을 프로빙을위한 새로운 도구 : 기가 파스칼의 압력에서 고감도 핵 자기 공명

Nuclear Magnetic Resonance (NMR) is one of the most important techniques for the study of condensed matter systems, their chemical structure, and their ...

Surface Enhanced Raman Spectroscopy Detection of Biomolecules Using EBL Fabricated Nanostructured Substrates

Fabrication and characterization of conjugate nano-biological systems interfacing metallic nanostructures on solid supports with immobilized biomolecules is reported. The entire sequence of relevant experimental steps is described, involving the fabrication of nanostructured substrates using electron beam lithography, immobilization of biomolecules on the substrates, and their characterization utilizing surface-enhanced Raman spectroscopy (SERS). Three different designs of nano-biological systems are employed, including protein A, glucose binding protein, and a dopamine binding DNA aptamer. In the latter two cases, the binding of respective ligands, D-glucose and dopamine, is also included. The three kinds of biomolecules are immobilized on nanostructured substrates by different methods, and the results of SERS imaging are reported. The capabilities of SERS to detect vibrational modes from surface-immobilized proteins, as well as to capture the protein-ligand and aptamer-ligand binding are demonstrated. The results also illustrate the influence of the surface nanostructure geometry, biomolecules immobilization strategy, Raman activity of the molecules and presence or absence of the ligand binding on the SERS spectra acquired.

We describe the fabrication and characterization of nano-biological systems interfacing nanostructured substrates with immobilized proteins and aptamers. The relevant experimental steps involving lithographic fabrication of nanostructured substrates, bio-functionalization, and surface-enhanced Raman spectroscopy (SERS) characterization, are reported. SERS detection of surface-immobilized proteins, and probing of protein-ligand and aptamer-ligand binding is demonstrated.

표면 EBL 날조 된 나노 구조 기판을 사용하여 생체 분자의 라만 분광학 감지 강화

Fabrication and characterization of conjugate nano-biological systems interfacing metallic nanostructures on solid supports with immobilized biomolecules ...

Characterization of Nanocrystal Size Distribution using Raman Spectroscopy with a Multi-particle Phonon Confinement Model

Analysis of the size distribution of nanocrystals is a critical requirement for the processing and optimization of their size-dependent properties. The common techniques used for the size analysis are transmission electron microscopy (TEM), X-ray diffraction (XRD) and photoluminescence spectroscopy (PL). These techniques, however, are not suitable for analyzing the nanocrystal size distribution in a fast, non-destructive and a reliable manner at the same time. Our aim in this work is to demonstrate that size distribution of semiconductor nanocrystals that are subject to size-dependent phonon confinement effects, can be quantitatively estimated in a non-destructive, fast and reliable manner using Raman spectroscopy. Moreover, mixed size distributions can be separately probed, and their respective volumetric ratios can be estimated using this technique. In order to analyze the size distribution, we have formulized an analytical expression of one-particle PCM and projected it onto a generic distribution function that will represent the size distribution of analyzed nanocrystal. As a model experiment, we have analyzed the size distribution of free-standing silicon nanocrystals (Si-NCs) with multi-modal size distributions. The estimated size distributions are in excellent agreement with TEM and PL results, revealing the reliability of our model.

We demonstrate how to determine the size distribution of semiconductor nanocrystals in a quantitative manner using Raman spectroscopy employing an analytically defined multi-particle phonon confinement model. Results obtained are in excellent agreement with the other size analysis techniques like transmission electron microscopy and photoluminescence spectroscopy.

다중 입자 Phonon은 감금 모델 라만 분광학을 이용하여 나노 결정 크기 분포의 특성

Analysis of the size distribution of nanocrystals is a critical requirement for the processing and optimization of their size-dependent properties. The ...

A Fabrication Method for Highly Stretchable Conductors with Silver Nanowires

Stretchable electronics are identified as a key technology for electronic applications in the next generation. One of the challenges in fabrication of stretchable electronic devices is the preparation of stretchable conductors with great mechanical stability. In this study, we developed a simple fabrication method to chemically solder the contact points between silver nanowire (AgNW) networks. AgNW nanomesh was first deposited on a glass slide via spray coating method. A reactive ink composed of silver nanoparticle (AgNPs) precursors was applied over the spray coated AgNW thin films. After heating for 40 min, AgNPs were preferentially generated over the nanowire junctions to solder the AgNW nanomesh, and reinforced the conducting network. The chemically modified AgNW thin film was then transferred to polyurethane (PU) substrates by casting method. The soldered AgNW thin films on PU exhibited no obvious change in electrical conductivity under stretching or rolling process with elongation strains up to 120%.

A simple synthesis method is used to chemically solder silver nanowire thin film to fabricate highly stretchable and conductive metal conductors.

Stretchable electronics are identified as a key technology for electronic applications in the next generation. One of the challenges in fabrication of ...

High Resolution Phonon-assisted Quasi-resonance Fluorescence Spectroscopy

High resolution optical spectroscopy methods are demanding in terms of either technology, equipment, complexity, time or a combination of these. Here we demonstrate an optical spectroscopy method that is capable of resolving spectral features beyond that of the spin fine structure and homogeneous linewidth of single quantum dots (QDs) using a standard, easy-to-use spectrometer setup. This method incorporates both laser and photoluminescence spectroscopy, combining the advantage of laser line-width limited resolution with multi-channel photoluminescence detection. Such a scheme allows for considerable improvement of resolution over that of a common single-stage spectrometer. The method uses phonons to assist in the measurement of the photoluminescence of a single quantum dot after resonant excitation of its ground state transition. The phonon&#39;s energy difference allows one to separate and filter out the laser light exciting the quantum dot. An advantageous feature of this method is its straight forward integration into standard spectroscopy setups, which are accessible to most researchers.

The manuscript describes a method of phonon-assisted quasi-resonant fluorescence spectroscopy that incorporates both laser-limited resolution and photoluminescence (PL) spectroscopy. This method utilizes optical phonons to provide linewidth-limited resolution spectra of atom-like semiconductor structures in the energy domain. The method is also easily realized with a single spectrometer optical spectroscopy setup.

높은 해상도 포논 도움을 준 공명 형광 분광학

High resolution optical spectroscopy methods are demanding in terms of either technology, equipment, complexity, time or a combination of these. Here we ...