The long-standing collaboration with Chang-Beom Eom at the University of Wisconsin-Madison, who provided the LAO/STO samples, is gratefully acknowledged. Video editing assistance from Christopher Solis is greatly appreciated. This work is supported by NSF (DMR-1104191, DMR-1124131), ARO (W911NF-08-1-0317), and AFOSR (FA9550-10-1-0524, FA9550-12-1-0268, FA9550-12-1-0057).

1. LAO / STO 헤테로를 얻 <ol><li> 티오이 종료 STO 기판에 펄스 레이저 증착법에 의해 성장 LAO의 3.4 단위 전지로 구성된 산화물 헤테로 구조를 얻습니다. 샘플 성장의 세부 사항 참조. 22에 설명되어 있습니다. </li></ol> 샘플 2. 포토 리소그래피 처리 칩 캐리어에 배선 캔버스를위한 본딩 패드와 LAO / STO 인터페이스에 전기 접점을 만듭니다. 개별 처리 단계는 아래에 상세히 설명된다. <ol><li> 스핀 포토 레지스트 <ol><li> 다음 30 초 동안 4,000 rpm에서 5 초 동안 600 rpm에서 샘플에 포토 레지스트를 스핀. 포토 레지스트 층은 약 2 μm의 두께 일 것이다. 1 분 동안 95 ° C에서 샘플을 굽는다. </li></ol></li><li> 5 mW의 / ㎠의 복용량 100 초 동안 320 nm의 빛을 마스크 얼 라이너를 사용하여 포토 레지스트를 노출합니다. </li><li> fo를 포토 레지스트 개발에 포토 레지스트를 개발1 분 R. </li><li> 이온 밀링 <ol><li> 포토 레지스트에 포함되지 분야에서 15 소재의 뉴 멕시코 (LAO와 STO)를 제거하기 위해 아르곤 + 이온 밀을 사용합니다. 들어오는 아르곤 + 이온 빔에 수직 인 방향으로 22.5 ° 각도로 샘플을 놓습니다. 아르곤 + 에칭 속도가 보정되지 않은 경우, 재료의 정확한 양이 제거 될 수 있도록 교정 실행을 수행합니다. AFM 또는 이에 상응하는 profilmetry를 사용하여 식각 깊이를 결정합니다. </li></ol></li><li> TI와 금의 DC 스퍼터링 <ol><li> 입금 4 nm의 TI는 다음의 Au 노출 STO 층과 전기적으로 접촉을 시료 위에 25 nm의 금하게되도록. 스퍼터링 압력 범위 2-6 X 10-7 토르이며, 스퍼터링은 RT에서 샘플로 이루어진다. TI는 셔터와 함께 10 분 동안 열린 셔터 후, 100 W로 마감 전 스퍼터 완료되면 100 W.에서 20 초 동안 스퍼터, 바로 50 W에서 1 분 동안 금을 미리 스퍼터 다음에 샘플을 30 초 동안 금을 스퍼터 50 W. 칼리소망의 Ti와 두께의 Au를 생성하는 시간을 브레이트. </li></ol></li><li> 이륙 <ol><li> 샘플의 표면에서 포토 레지스트를 제거하기 위해 아세톤 / IPA 초음파 세척을 사용합니다. </li></ol></li><li> 두 번째 층 <ol><li> 4 단계 (예. 제외 이온 밀링)을 제외하고 두 번째 리소그래피 공정은, 각각의 본딩 패드에 골드 와이어 연결을 작성하는 데 사용됩니다. 두 가지 패턴들은 전기 단락을 생성하지 않도록 잘 정렬되어야합니다. </li></ol></li><li> 플라즈마 세정. <ol><li> IPC 배럴 에처는 트렌치 패턴에 포토 레지스트 잔류 물을 제거하기 위해 사용된다. 1 분 동안 100 W, 1 Torr의 아르곤에서 사용 계측기 </li></ol></li></ol> 3. 와이어 본드 샘플 쓰기를 준비하는 <ol><li> 28 사용 가능한 핀 칩 캐리어 (그림 2A)에 LAO / STO 샘플을 장착합니다. </li><li> 와이어 결합 구조 </li></ol> 참고 : 전기 C를 만들기 위해 와이어 본더를 사용샘플에 본딩 패드와 칩 캐리어 사이 onnections. 전기 접점 및 칩 캐리어 사이에 1 밀 (25 마이크로 미터) 골드 와이어를 연결합니다. 나노 쓰기 4. 나노 구조를 쓰기 <ol><li> 전도성 나노 구조 (그림 3A)의 비공식 스케치를 만듭니다. </li><li> 확장 가능한 벡터 그래픽 (SVG) 편집기 (그림 3B)를 엽니 다. <ol><li> 템플릿을 사용하거나 AFM 이미지의 일치하도록 창 크기를 정의합니다. </li><li> SVG 편집기에 시료의 AFM 이미지를로드합니다. </li><li> AFM 이미지에 중첩 나노 구조 요소를 만듭니다. </li></ol></li><li> 나노 리소그래피 프로그램에 SVG 파일을로드합니다. </li><li> 전도성 나노 구조를 만들 수 리소그래피 소프트웨어를 실행합니다. <ol><li> 사용 V 팁 = +10 나노 구조를 만들 수있는 V 및 V 팁 = 나노 구조를 지울 -10 V. </li><li> 범위의 속도로 C-AFM 팁을 이동 202 μM / 초의 0 ㎚ / 초. </li></ol></li></ol> 5. 장치를 냉각 및 측정을 수행 <ol><li> 모두 흰색 조명을 끄고 빨간색 필터 / 라이트 소스를 사용합니다. </li><li> AFM 시스템에서 샘플을 추출합니다. </li><li> 희석 냉장고 (A)에 샘플을로드합니다. </li><li> 샘플이 냉각으로 온도 (B) 대 저항을 측정합니다. </li><li> 낮은 온도 (C)에 전송 특성을 측정한다. </li></ol>

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The authors have nothing to disclose.

Successful creation of nanostructures depends on several critical steps. It is important that the LAO/STO samples are grown with a thickness that is known to be at the boundary between the insulating and conductive phase. (Details of sample growth fall outside the scope of this paper, but are crucial for overall success.) Second, it is important to have relative humidity within the range 25-45% for successful c-AFM writing. Values below 25% are unlikely to produce conductive nanostructures, while too high humidity will generally produce uncontrollably large features. Also, temperature control of the AFM is important if the c-AFM tip needs to achieve precise registry over long periods of time. Once the nanostructures are created, they must be placed in a vacuum environment if experiments lasting longer than a few hours are to be performed. For the experiments described here, the structure is created and within minutes transferred to a vacuum environment.
It is recommend before writing that a &#8220;writing test&#8221; be performed on all relevant electrodes. In such a test, two virtual electrodes are first created, and a single nanowire is written while simultaneously monitoring the conductance. A similar test of erasure can be performed by &#8220;cutting&#8221; the nanowire shortly afterwards. If the nanostructure is decaying rapidly, the issue is most likely due either to the interfacial contacts or the canvas itself. To distinguish between these two effects, a four-terminal measurement of the conductance should be performed, and the two-terminal conductance should be compared with the four-terminal conductance as a function of time. If the two-terminal conductance is decaying more rapidly than the four-terminal conductance, then the issue is related to the electrical contacts to the interface. If the four-terminal conductance is decaying at a comparable rate, then most likely the canvas is not suitable and should be replaced.
There are natural limitations of the current method for creating nanostructures. Specifically, the writing speed for the smallest devices is limited to a few hundred nanometers per second. Speeds far above that value lead to unpredictable results. Use of parallel writing techniques are possible27,28, but are not highly developed and have their own drawbacks. The size of nanostructures that can be created is naturally limited by the scan range of the AFM being used. A high-quality AFM with closed-loop feedback in the two scan directions is highly recommended. Tracking of point-like objects on the sample surface should be performed to monitor temporal drift of the sample.
Once creation of conductive nanostructures at oxide interfaces has been mastered, there are a wide range of experimental directions that can be explored. Using this technique, a wide variety of nanostructures and devices have already been demonstrated, including nanowires18, tunnel barriers29, rectifying junctions30, field-effect transistors18, single-electron transistors31, superconducting nanowires32, nanoscale optical detectors33, and nanoscale THz emitters and detectors34.

산화물 헤테로 1-5 전시 과학적으로 흥미로운 응용 프로그램 4 잠재적으로 유용한 응급 물리적 현상의 매우 다양한 종류. 특히, LaAlO3는 (LAO) 및 3 된 SrTiO3 (STO) (6) 사이의 인터페이스는 8 강유전체 조 및 강자성 구 동작 7 초전도, 전도성, 절연성을 나타낼 수있다. 2006 년 틸 등이 LAO 층의 두께와 같은 날카로운 절연체 - 금속 전이가 있음을 보여 주었다 (10)은 4 단위 셀 (4uc)의 임계 두께에 따라 증가한다. 그것은 이후 3uc-LAO/STO 구조가 전도성 원자 힘 현미경 (C-AFM) 탐침 (11)와 로컬로 제어 할 수있는 이력 전환을 나타내는 것으로 나타났다. 예컨대 LaAlO3는 / 3 된 SrTiO3 등의 산화물 인터페이스의 특성은 도전성의 부재 또는 존재에 의존계면에서 전자. 이 전자가 위로 게이트 전극 (12, 13), 게이트 (10)를 사용하여 제어 할 수 있습니다, 표면 (14) 흡착, 강유전체 층 (15, 16)과 C-AFM 리소그래피 11. C-AFM 리소그래피의 독특한 기능은 매우 작은 나노 기능을 생성 할 수 있다는 것입니다. 두 차원 감금과 함께 전기 톱 게이트는 종종 III-V 반도체 (17) 양자 도트를 만드는 데 사용됩니다. 대안 적으로, 준 일차원 반도체 나노 와이어는 전기적으로 근접하여 게이팅 될 수있다. 이러한 구조의 제조 방법은 시간 소모적이고, 일반적으로 비가 역적이다. 대조적으로, C-AFM 리소그래피 기술은 나노 구조물이 한 실험에 대해 생성 한 다음, (화이트 보드와 유사한) &quot;소거&quot;될 수 있다는 점에서 가역적이다. 삭제, 동안 일반적으로, C-AFM 쓰기는 AFM 팁에 적용 양의 전압으로 수행음의 전압을 사용하여 수행된다. 특정한 구조를 생성하는 데 필요한 시간은 디바이스의 복잡성에 의존하지만, 일반적으로 30 분 미만이고; 그 시간의 대부분은 캔버스를 삭제 소요됩니다. 일반적인 공간 해상도는 약 10 나노 미터입니다 만, 2 나노 미터 (18)를 생성 할 수있는 적절한 튜닝은 작은 있습니다. 나노 제조 절차의 상세한 설명은 다음과 같다. 여기에 제공된 내용은 비슷한 실험이 관심이 연구자에 의해 수행 될 수 있도록 충분해야한다. 여기에 설명 된 방법은 반도체에 전자 나노 구조를 만드는 데 사용되는 기존의 리소그래피 방법에 비해 많은 장점을 가지고 있습니다. 여기에 기재된 C-AFM 리소그래피 방법은 주사 양극 산화 (19), 딥 - 펜 나노 리소그래피 (20), 압전 패터닝 등 스캐닝 프로브 기반 리소그래피 노력의 훨씬 광범위한 클래스의 일부인21, 등등. 신규 산화물 인터페이스의 사용과 함께 여기에 설명 C-AFM 기술은, 물성의 전례 다양한 높은 정밀도의 전자 구조의 일부를 생성 할 수있다.

<table border="0" cellpadding="0" cellspacing="0" width="889">
	<tbody>
		<tr height="20">
			<td height="20" style="height:20px;width:165px;">Name</td>
			<td style="width:169px;">Company</td>
			<td style="width:108px;">Catalog Number</td>
			<td style="width:447px;">Comments</td>
		</tr>
		<tr height="20">
			<td height="20" style="height:20px;">Equipment</td>
			<td></td>
			<td></td>
			<td></td>
		</tr>
		<tr height="20">
			<td height="20" style="height:20px;">Contact Aligner</td>
			<td>Karl-Suss</td>
			<td>MA6</td>
			<td></td>
		</tr>
		<tr height="20">
			<td height="20" style="height:20px;">Spinner</td>
			<td>Solitec</td>
			<td>5110C</td>
			<td></td>
		</tr>
		<tr height="20">
			<td height="20" style="height:20px;">Ion Mill</td>
			<td>Commonwealth Scientific</td>
			<td>8C</td>
			<td></td>
		</tr>
		<tr height="20">
			<td height="20" style="height:20px;">Sputtering System</td>
			<td>Leybold-Heraeus</td>
			<td>Z-650</td>
			<td></td>
		</tr>
		<tr height="20">
			<td height="20" style="height:20px;">Barrel Etcher</td>
			<td>Branson/IPC</td>
			<td>3000C</td>
			<td></td>
		</tr>
		<tr height="20">
			<td height="20" style="height:20px;">Wire Bonder</td>
			<td>Westbond</td>
			<td>7700E</td>
			<td></td>
		</tr>
		<tr height="20">
			<td height="20" style="height:20px;">AFM</td>
			<td>Asylum Research</td>
			<td>MFP-3D</td>
			<td></td>
		</tr>
		<tr height="20">
			<td height="20" style="height:20px;">Dilution Refrigerator</td>
			<td>Quantum Design</td>
			<td>P850</td>
			<td></td>
		</tr>
		<tr height="20">
			<td height="20" style="height:20px;">Ultrasonic Wash Machine</td>
			<td>Fisher Scientific</td>
			<td>15-335-6</td>
			<td></td>
		</tr>
		<tr height="20">
			<td height="20" style="height:20px;">Current Amplifier</td>
			<td>Femto</td>
			<td>DLPCA-200</td>
			<td></td>
		</tr>
		<tr height="20">
			<td height="20" style="height:20px;"></td>
			<td></td>
			<td></td>
			<td></td>
		</tr>
		<tr height="20">
			<td height="20" style="height:20px;">Materials</td>
			<td></td>
			<td></td>
			<td></td>
		</tr>
		<tr height="20">
			<td height="20" style="height:20px;">LaAlO3/SrTiO3</td>
			<td>Prof. Chang-Beom Eom</td>
			<td>N/A</td>
			<td>5mm x 1mm with ~3.4 unit cells of LAO (See Reference 18)</td>
		</tr>
		<tr height="20">
			<td height="20" style="height:20px;">Photoresist</td>
			<td>AZ Electronic Materials</td>
			<td>P4210</td>
			<td></td>
		</tr>
		<tr height="20">
			<td height="20" style="height:20px;">Developer</td>
			<td>AZ Electronic Materials</td>
			<td>400K</td>
			<td></td>
		</tr>
		<tr height="20">
			<td height="20" style="height:20px;">Acetone</td>
			<td>Fisher Scientific</td>
			<td>A929SK-4</td>
			<td></td>
		</tr>
		<tr height="20">
			<td height="20" style="height:20px;">Isopropyl Alcohol</td>
			<td>Fisher Scientific</td>
			<td>A459-1</td>
			<td></td>
		</tr>
		<tr height="20">
			<td height="20" style="height:20px;">Deionized Water</td>
			<td>Fisher Scientific</td>
			<td>23-290-065</td>
			<td></td>
		</tr>
		<tr height="20">
			<td height="20" style="height:20px;">Gold Wire</td>
			<td>DuPont</td>
			<td>5771</td>
			<td>1 mil diameter</td>
		</tr>
		<tr height="20">
			<td height="20" style="height:20px;">Chip Carrier</td>
			<td>NTK Technologies</td>
			<td>IRK28F1-5451D</td>
			<td></td>
		</tr>
	</tbody>
</table>

writing and low-temperature characterization of oxide nanostructures

Oxide nanoelectronics is a rapidly growing field which seeks to develop novel materials with multifunctional behavior at nanoscale dimensions. Oxide interfaces exhibit a wide range of properties that can be controlled include conduction, piezoelectric behavior, ferromagnetism, superconductivity and nonlinear optical properties. Recently, methods for controlling these properties at extreme nanoscale dimensions have been discovered and developed. Here are described explicit step-by-step procedures for creating LaAlO3/SrTiO3 nanostructures using a reversible conductive atomic force microscopy technique. The processing steps for creating electrical contacts to the LaAlO3/SrTiO3 interface are first described. Conductive nanostructures are created by applying voltages to a conductive atomic force microscope tip and locally switching the LaAlO3/SrTiO3 interface to a conductive state. A versatile nanolithography toolkit has been developed expressly for the purpose of controlling the atomic force microscope (AFM) tip path and voltage. Then, these nanostructures are placed in a cryostat and transport measurements are performed. The procedures described here should be useful to others wishing to conduct research in oxide nanoelectronics.

결과는 여기에 도시 된 나노 구조물이 클래스에 의해 발휘된다 반송 동작을 대표하며 그 밖에 23-26 상세히 설명되었다. 이 예에서, 나노 와이어 캐비티는 3.3 단위 셀 LAO / STO 헤테로 구조에서 (도 4)를 구성하고있다. 실험 11 &quot;절단&quot;나노 와이어에 의해 결정 (녹색으로 표시) 도전은 넓은 일반적으로 10 ㎚이다. 팁 쓰기 속도는 각 세그먼트의 끝 속도와 전압, 리소그래피 전면 패널 (그림 4B)에서 독립적으로 구성 할 수 있습니다. &quot;가상 전극는&quot;계면 연락처와 해당 인터페이스는 나노 구조에 전도성이 높은 전기 연결이 있는지 확인합니다. 나노 구조가 기록 된 후에는 희석 냉동기로 전달된다. 550 나노 미터 이하에서 빛에 대한 노출은 원치 않는 광전도를 생성합니다, 그래서 꼬마 도깨비ortant 어둠 또는 빨간색 &quot;암실&quot;빛 (그림 5A)의 도움으로 장치를 전송합니다. 전기 연결은 RT에서 수행되어야하고, 극저온에서 전기 연결을 변경할 때 대부분의 반도체 나노 구조와 같은 큰주의를 기울여야합니다. 장치가 정전기 방전을 실시하면, 가장 가능성이 절연 될 것이다. 현저하게, 디바이스 기능은 &quot;순환&quot;300 K까지 온도를 다시 냉각하여 회수 할 수있다. 쿨 다운 동안, 2 단자의 저항을 모니터링하는 루틴, 심지어 4 단자 저항, 온도의 함수로서. AC 전류는 트랜스 임피던스 증폭기를 사용하여 측정되는 동안 이러한 측정을 위해 AC 전압 (일반적으로 1 ~ MV)는, 전극들 중 하나에 저주파 (&lt;10 헤르쯔)에인가된다. 복조 잠금 및 필터링은 집에서 개발 한 잠금 앰프를 사용하여 수행됩니다. 교류 세제곱rrent는 온도의 함수 (그림 5B)로 감시된다. 장치가 희석 냉장고 (50 mK의)의베이스 온도로 냉각되면, 4 단자 전송 측정 (도 5c)이 수행된다. 장치를 통해 전압을 동시에 측정하는 동안 이러한 측정의 경우, 현재는 장치의 기본 채널을 통해 공급된다. 대신 잠금 앰프, 전체 전류 - 전압 측정의 (IV) 추적을 측정한다. 이 방법은 더 많은 정보를 포함하고 차동 도통 수치 분화를 통해 계산 될 수있다. 특정 장치, 차동 도통 사이드 게이트 전압 V에 SG의 함수로서 측정된다. 이 게이트 디바이스의 화학 전위가 변화 될 수있다. 장치를 통해 전송은 쿨롱 봉쇄 작은 값을 발생하고, 스트로크 엔진을하는 영역을 나타내는 강력한 단순하지 않은 의존성을 보여줍니다V의 SG의 큰 값을 초전도 겨. 장치의이 클래스에 대한 물리적 해석에 대한 자세한 내용은 다른 곳에서 설명한다. <img alt="그림 1" src="/files/ftp_upload/51886/51886fig1highres.jpg" /> ..도 1 포토 리소그래피 공정 단계 단계 1 : 스핀 포토 레지스트. 2 단계 : 마스크 얼 라이너를 사용하여 포토 레지스트를 노출합니다. 3 단계 : 포토 레지스트를 개발한다. 4 단계 : 이온 밀링. 5 단계 : DC는 티타늄과 금을 증착하는 스퍼터링. 6 단계 : 리프트 오프 (lift-off). 7 단계 : 두 번째 층을 증착. 8 단계 : 플라즈마 세정. <img alt="그림 2" src="/files/ftp_upload/51886/51886fig2highres.jpg" /> 그림 2. 리소그래피 패터닝 LAO / STO 헤테로의 이미지. 칩 캐리어에 결합는 5mm X 5mm는 샘플 와이어를 보여주는 (A) 이미지. (B)<html> 본딩 패드와 캔버스 중 하나를 보여주는 광학 이미지. (C) 하나의 캔버스의 근접입니다. <a href="https://www.jove.com/files/ftp_upload/51886/51886fig2highres.jpg" target="_blank">이 그림의 더 큰 버전을 보려면 여기를 클릭하십시오.</a> <img alt="그림 3" src="/files/ftp_upload/51886/51886fig3highres.jpg" /> 그림 3. LAO / STO 나노 구조의 (A) 비공식 디자인. (B) 오픈 소스 확장 가능한 벡터 그래픽 (SVG) 편집기를 사용하여 나노 구조의 정확한 레이아웃입니다. <img alt="그림 4" src="/files/ftp_upload/51886/51886fig4highres.jpg" /> 그림 4. C-AFM의 패터닝 (A) 리소그래피 전면 패널. (B) 3 차원 시뮬레이터의 스크린 샷 위치와 C-AFM 팁의 전압을 표시합니다.w.jove.com/files/ftp_upload/52058/52058fig4large.jpg &quot;대상 =&quot;_blank &quot;&gt;이 그림의 더 큰 버전을 보려면 여기를 클릭하십시오. <img alt="그림 5" src="/files/ftp_upload/51886/51886fig5highres.jpg" /> 도 5. (A) LAO / STO 나노 구조물이 희석 냉동기에 삽입된다. (B) 시료의 저항의 모니터링이 50 mK의 300 내지 K로부터 냉각 될 때. 장치의 4 단자 차분 컨덕턴스 (C) 모니터링의 함수 장치 (V4t)에서 사이드 게이트 전압를 Vsg 전압. 지멘스 (S)의 단위 및 전압에 표시 강도 그래프는 볼트 (V) 단위로 표시됩니다.

Watch this Scientific Journal Video about Writing and Low-Temperature Characterization of Oxide Nanostructures at JoVE.com

Writing and Low-Temperature Characterization of Oxide Nanostructures

Oxide nanostructures provide new opportunities for science and technology. The interfacial conductivity between LaAlO3 and SrTiO3 can be controlled with near-atomic precision using a conductive atomic force microscopy technique. The protocol for creating and measuring conductive nanostructures at LaAlO3/SrTiO3 interfaces is demonstrated.

작성 및 산화물 나노 구조의 저온 특성

Oxide nanoelectronics is a rapidly growing field which seeks to develop novel materials with multifunctional behavior at nanoscale dimensions.  Oxide ...

writing-and-low-temperature-characterization-of-oxide-nanostructures

Research

JoVE Journal

Engineering

9.9K 조회수.  University of Pittsburgh. Oxide nanostructures provide new opportunities for science and technology. The interfacial conductivity between LaAlO3 and SrTiO3 can be controlled with near-atomic precision using a conductive atomic force microscopy technique. The protocol for creating and measuring conductive nanostructures at LaAlO3/SrTiO3 interfaces is demonstrated.

비디오: Writing and Low-Temperature Characterization of Oxide Nanostructures

A Method to Fabricate Disconnected Silver Nanostructures in 3D

The standard nanofabrication toolkit includes techniques primarily aimed at creating 2D patterns in dielectric media. Creating metal patterns on a submicron scale requires a combination of nanofabrication tools and several material processing steps. For example, steps to create planar metal structures using ultraviolet photolithography and electron-beam lithography can include sample exposure, sample development, metal deposition, and metal liftoff. To create 3D metal structures, the sequence is repeated multiple times. The complexity and difficulty of stacking and aligning multiple layers limits practical implementations of 3D metal structuring using standard nanofabrication tools. Femtosecond-laser direct-writing has emerged as a pre-eminent technique for 3D nanofabrication.1,2 Femtosecond lasers are frequently used to create 3D patterns in polymers and glasses.3-7 However, 3D metal direct-writing remains a challenge. Here, we describe a method to fabricate silver nanostructures embedded inside a polymer matrix using a femtosecond laser centered at 800 nm. The method enables the fabrication of patterns not feasible using other techniques, such as 3D arrays of disconnected silver voxels.8 Disconnected 3D metal patterns are useful for metamaterials where unit cells are not in contact with each other,9 such as coupled metal dot10,11or coupled metal rod12,13 resonators. Potential applications include negative index metamaterials, invisibility cloaks, and perfect lenses.
In femtosecond-laser direct-writing, the laser wavelength is chosen such that photons are not linearly absorbed in the target medium. When the laser pulse duration is compressed to the femtosecond time scale and the radiation is tightly focused inside the target, the extremely high intensity induces nonlinear absorption. Multiple photons are absorbed simultaneously to cause electronic transitions that lead to material modification within the focused region. Using this approach, one can form structures in the bulk of a material rather than on its surface.
Most work on 3D direct metal writing has focused on creating self-supported metal structures.14-16 The method described here yields sub-micrometer silver structures that do not need to be self-supported because they are embedded inside a matrix. A doped polymer matrix is prepared using a mixture of silver nitrate (AgNO3), polyvinylpyrrolidone (PVP) and water (H2O). Samples are then patterned by irradiation with an 11-MHz femtosecond laser producing 50-fs pulses. During irradiation, photoreduction of silver ions is induced through nonlinear absorption, creating an aggregate of silver nanoparticles in the focal region. Using this approach we create silver patterns embedded in a doped PVP matrix. Adding 3D translation of the sample extends the patterning to three dimensions.

Femtosecond-laser direct-writing is frequently used to create three-dimensional (3D) patterns in polymers and glasses. However, patterning metals in 3D remains a challenge. We describe a method for fabricating silver nanostructures embedded inside a polymer matrix using a femtosecond laser centered at 800 nm.

3D로 연결이 끊긴 실버 Nanostructures를 조작하는 방법

The standard nanofabrication toolkit includes  techniques primarily aimed at creating 2D patterns in dielectric media. Creating  metal patterns on a ...

연구

공학

Probing and Mapping Electrode Surfaces in Solid Oxide Fuel Cells

Solid oxide fuel cells (SOFCs) are potentially the most efficient and cost-effective solution to utilization of a wide variety of fuels beyond hydrogen 1-7. The performance of SOFCs and the rates of many chemical and energy transformation processes in energy storage and conversion devices in general are limited primarily by charge and mass transfer along electrode surfaces and across interfaces. Unfortunately, the mechanistic understanding of these processes is still lacking, due largely to the difficulty of characterizing these processes under in situ conditions. This knowledge gap is a chief obstacle to SOFC commercialization. The development of tools for probing and mapping surface chemistries relevant to electrode reactions is vital to unraveling the mechanisms of surface processes and to achieving rational design of new electrode materials for more efficient energy storage and conversion2. Among the relatively few in situ surface analysis methods, Raman spectroscopy can be performed even with high temperatures and harsh atmospheres, making it ideal for characterizing chemical processes relevant to SOFC anode performance and degradation8-12. It can also be used alongside electrochemical measurements, potentially allowing direct correlation of electrochemistry to surface chemistry in an operating cell. Proper in situ Raman mapping measurements would be useful for pin-pointing important anode reaction mechanisms because of its sensitivity to the relevant species, including anode performance degradation through carbon deposition8, 10, 13, 14 ("coking") and sulfur poisoning11, 15 and the manner in which surface modifications stave off this degradation16. The current work demonstrates significant progress towards this capability. In addition, the family of scanning probe microscopy (SPM) techniques provides a special approach to interrogate the electrode surface with nanoscale resolution. Besides the surface topography that is routinely collected by AFM and STM, other properties such as local electronic states, ion diffusion coefficient and surface potential can also be investigated17-22. In this work, electrochemical measurements, Raman spectroscopy, and SPM were used in conjunction with a novel test electrode platform that consists of a Ni mesh electrode embedded in an yttria-stabilized zirconia (YSZ) electrolyte. Cell performance testing and impedance spectroscopy under fuel containing H2S was characterized, and Raman mapping was used to further elucidate the nature of sulfur poisoning. In situ Raman monitoring was used to investigate coking behavior. Finally, atomic force microscopy (AFM) and electrostatic force microscopy (EFM) were used to further visualize carbon deposition on the nanoscale. From this research, we desire to produce a more complete picture of the SOFC anode.

We present a unique platform for characterizing electrode surfaces in solid oxide fuel cells (SOFCs) that allows simultaneous performance of multiple characterization techniques (e.g. in situ Raman spectroscopy and scanning probe microscopy alongside electrochemical measurements). Complementary information from these analyses may help to advance toward a more profound understanding of electrode reaction and degradation mechanisms, providing insights into rational design of better materials for SOFCs.

고체 산화물 연료 전지의 전극 표면을 탐색 및 매핑

Solid oxide fuel cells (SOFCs) are potentially the most efficient and cost-effective solution to utilization of a wide variety of fuels beyond hydrogen ...

Visible-light Induced Reduction of Graphene Oxide Using Plasmonic Nanoparticle

Present work demonstrates the simple, chemical free, fast, and energy efficient method to produce reduced graphene oxide (r-GO) solution at RT using visible light irradiation with plasmonic nanoparticles. The plasmonic nanoparticle is used to improve the reduction efficiency of GO. It only takes 30 min&#160;at RT by illuminating the solutions with Xe-lamp, the r-GO solutions can be obtained by completely removing gold nanoparticles through simple centrifugation step. The spherical gold nanoparticles (AuNPs) as compared to the other nanostructures is the most suitable plasmonic nanostructure for r-GO preparation. The reduced graphene oxide prepared using visible light and AuNPs was equally qualitative as chemically reduced graphene oxide, which was supported by various analytical techniques such as UV-Vis spectroscopy, Raman spectroscopy, powder XRD and XPS. The reduced graphene oxide prepared with visible light shows excellent quenching properties over the fluorescent molecules modified on ssDNA and excellent fluorescence recovery for target DNA detection. The r-GO prepared by recycled AuNPs is found to be of same quality with that of chemically reduced r-GO. The use of visible light with plasmonic nanoparticle demonstrates the good alternative method for r-GO synthesis.

A simple protocol for the preparation of reduced graphene oxide using visible light and plasmonic nanoparticle is described.

플라즈몬 나노 입자를 사용하여 그래 핀 산화물의 가시 광선 유도 감소

Present work demonstrates the simple, chemical free, fast, and energy efficient method to produce reduced graphene oxide (r-GO) solution at RT using ...

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 ...

Fabrication of Low Temperature Carbon Nanotube Vertical Interconnects Compatible with Semiconductor Technology

We demonstrate a method for the low temperature growth (350 &#176;C) of vertically-aligned carbon nanotubes (CNT) bundles on electrically conductive thin-films. Due to the low growth temperature, the process allows integration with modern low-&#954; dielectrics and some flexible substrates. The process is compatible with standard semiconductor fabrication, and a method for the fabrication of electrical 4-point probe test structures for vertical interconnect test structures is presented. Using scanning electron microscopy the morphology of the CNT bundles is investigated, which demonstrates vertical alignment of the CNT and can be used to tune the CNT growth time. With Raman spectroscopy the crystallinity of the CNT is investigated. It was found that the CNT have many defects, due to the low growth temperature. The electrical current-voltage measurements of the test vertical interconnects displays a linear response, indicating good ohmic contact was achieved between the CNT bundle and the top and bottom metal electrodes. The obtained resistivities of the CNT bundle are among the average values in the literature, while a record-low CNT growth temperature was used.

A method for the growth of low temperature vertically-aligned carbon nanotubes, and the subsequent fabrication of vertical interconnect electrical test structures using semiconductor fabrication is presented.

반도체 기술과 호환 저온 탄소 나노 튜브 수직 상호 연결의 제작

We demonstrate a method for the low temperature growth (350 &#176;C) of vertically-aligned carbon nanotubes (CNT) bundles on electrically conductive ...

Integration of Light Trapping Silver Nanostructures in Hydrogenated Microcrystalline Silicon Solar Cells by Transfer Printing

One of the potential applications of metal nanostructures is light trapping in solar cells, where unique optical properties of nanosized metals, commonly known as plasmonic effects, play an important role. Research in this field has, however, been impeded owing to the difficulty of fabricating devices containing the desired functional metal nanostructures. In order to provide a viable strategy to this issue, we herein show a transfer printing-based approach that allows the quick and low-cost integration of designed metal nanostructures with a variety of device architectures, including solar cells. Nanopillar poly(dimethylsiloxane) (PDMS) stamps were fabricated from a commercially available nanohole plastic film as a master mold. On this nanopatterned PDMS stamps, Ag films were deposited, which were then transfer-printed onto block copolymer (binding layer)-coated hydrogenated microcrystalline Si (&#181;c-Si:H) surface to afford ordered Ag nanodisk structures. It was confirmed that the resulting Ag nanodisk-incorporated &#181;c-Si:H solar cells show higher performances compared to a cell without the transfer-printed Ag nanodisks, thanks to plasmonic light trapping effect derived from the Ag nanodisks. Because of the simplicity and versatility, further device application would also be feasible thorough this approach.

A viable transfer printing-based methodology to introduce plasmonic metal nanostructures in solar cells is described. Using nanopillar poly(dimethylsiloxane) stamps, an Ag-based ordered nanodisk array was integrated with standard hydrogenated microcrystalline Si solar cells, which led to improved device performances due to plasmonic light trapping.

전송 인쇄하여 수소 첨가 미세 결정 실리콘 태양 전지에 빛 트래핑 실버 나노 구조의 통합

One of the potential applications of metal nanostructures is light trapping in solar cells, where unique optical properties of nanosized metals, commonly ...

Writing Bragg Gratings in Multicore Fibers

Fiber Bragg gratings in multicore fibers can be used as compact and robust filters in astronomical and other research and commercial applications. Strong suppression at a single wavelength requires that all cores have matching transmission profiles. These gratings cannot be inscribed using the same method as for single-core fibers because the curved surface of the cladding acts as a lens, focusing the incoming UV laser beam and causing variations in exposure between cores. Therefore we use an additional optical element to ensure that the beam shape does not change while passing through the cross-section of the multicore fiber. This consists of a glass capillary tube which has been polished flat on one side, which is then placed over the section of the fiber to be inscribed. The laser beam enters the fiber through the flat surface of the capillary tube and hence maintains its original dimensions. This paper demonstrates the improvements in core-to-core uniformity for a 7-core fiber using this method. The technique can be generalized to larger multicore fibers.

We describe a technique for inscribing identical fiber Bragg gratings into each core of a multicore fiber. This is achieved by introducing an additional surface into the optical path to mitigate lensing by the curved surface of the fiber cladding.

멀티 코어 섬유에 브래그 격자를 작성

Fiber Bragg gratings in multicore fibers can be used as compact and robust filters in astronomical and other research and commercial applications. Strong ...

Iridium Oxide-reduced Graphene Oxide Nanohybrid Thin Film Modified Screen-printed Electrodes as Disposable Electrochemical Paper Microfluidic pH Sensors

A facile, controllable, inexpensive and green electrochemical synthesis of IrO2-graphene nanohybrid thin films is developed to fabricate an easy-to-use integrated paper microfluidic electrochemical pH sensor for resource-limited settings. Taking advantages from both pH meters and strips, the pH sensing platform is composed of hydrophobic barrier-patterned paper micropad (&#181;PAD) using polydimethylsiloxane (PDMS), screen-printed electrode (SPE) modified with IrO2-graphene films and molded acrylonitrile butadiene styrene (ABS) plastic holder. Repetitive cathodic potential cycling was employed for graphene oxide (GO) reduction which can completely remove electrochemically unstable oxygenated groups and generate a 2D defect-free homogeneous graphene thin film with excellent stability and electronic properties. A uniform and smooth IrO2 film in nanoscale grain size is anodically electrodeposited onto the graphene film, without any observable cracks. The resulting IrO2-RGO electrode showed slightly super-Nernstian responses from pH 2-12 in Britton-Robinson (B-R) buffers with good linearity, small hysteresis, low response time and reproducibility in different buffers, as well as low sensitivities to different interfering ionic species and dissolved oxygen. A simple portable digital pH meter is fabricated, whose signal is measured with a multimeter, using high input-impedance operational amplifier and consumer batteries. The pH values measured with the portable electrochemical paper-microfluidic pH sensors were consistent with those measured using a commercial laboratory pH meter with a glass electrode.

The study demonstrates the growth of iridium oxide-reduced graphene oxide (IrO2-RGO) nanohybrid thin films on irregular and rough screen-printed carbon substrate through a green electrochemical synthesis, and their implementation as a pH sensor with a patterned paper-fluidic platform.

일회용 전기 종이 마이크로 유체의 pH 센서와 같은 이리듐 산화물 환원 그래 핀 산화물 나노 하이브리드 박막 수정 스크린 인쇄 전극

A facile, controllable, inexpensive and green electrochemical synthesis of IrO2-graphene nanohybrid thin films is developed to fabricate an easy-to-use ...

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 ...

Method Development for Contactless Resonant Cavity Dielectric Spectroscopic Studies of Cellulosic Paper

The current analytical techniques for characterizing printing and graphic arts substrates are largely ex situ and destructive. This limits the amount of data that can be obtained from an individual sample and renders it difficult to produce statistically relevant data for unique and rare materials. Resonant cavity dielectric spectroscopy is a non-destructive, contactless technique which can simultaneously interrogate both sides of a sheeted material and provide measurements which are suitable for statistical interpretations. This offers analysts the ability to quickly discriminate between sheeted materials based on composition and storage history. In this methodology article, we demonstrate how contactless resonant cavity dielectric spectroscopy may be used to differentiate between paper analytes of varying fiber species compositions, to determine the relative age of the paper, and to detect and quantify the amount of post-consumer waste (PCW) recycled fiber content in manufactured office paper.

A protocol for the non-destructive analysis of the fiber content and relative age of paper.

비접촉식 공진성 유전체 분광연구용 셀룰로오스 종이 공진법 개발

The current analytical techniques for characterizing printing and graphic arts substrates are largely ex situ and destructive. This limits the amount of ...