이 작품은 독일 연구 재단 (DFG) (계약 CH 943/2-1)에 의해 설립된다. 저자는이 작품에 대한 CIGS 흡수층를 준비 젠트 FÜR Sonnenenergie - 싶게 Wasserstoff-Forschung 바덴 뷔 르템 베르크에서 볼프강 Dittus, 그리고 스테판 Paetel에게 감사의 말씀을 전합니다.

1. CIGS 층 증착 <ol><li> 3 mm 두께의 소다 석회 유리 기판 (SLG) 위에 몰리브덴 스퍼터링 예금 500 나노 미터 (다시 접촉 층). </li><li> 인라인 다단 CIGS 공정 24 CIGS 2 μm의 공동 증발. 레이어 모 다시 접촉에 입금 얻은 CIGS는 그림 1에 표시됩니다. </li><li> X-선 형광 분석기 (XRF)에 의한 CIGS 층의 통합 구성을 측정합니다. 얻어진 CIGS의 조성은 표 1에 나타나있다. </li></ol> 2. APT 분석을위한 특정 사이트 샘플 제작 <ol><li> 나중에 표본에 대한 지원되고, 여러 핀의 행을 얻기 위해 두 개의 반쪽으로 TEM 모 격자를 잘라. 5 중량의 전해 연마에 의해 핀의 끝 홀더와 테이퍼에 반 그리드 TEM을 설치합니다. 아래 팁 직경 &lt;2 μm의 % NaOH를합니다. 이 과정은 입체경을 사용하여 제어 합리적 할 수 있습니다. 그런 다음 다른 홀더 티셔츠 위에 전해 그리드를 탑재모자는 순차적 FIB, TEM, EBSD, 그리고 APT 특성에​​ 최적화되어 있습니다. </li><li> 공장 CIGS 박막에 두 개의 참호를 얻을 수 언더컷 (그림 2A).를 FIB를 사용하여 청크의 왼쪽에있는 첫 번째 프리 컷하십시오. </li><li> 이온 빔에 의한 화학 기상 증착법에 의해 백금 용접을 증착하여 덩어리로 micromanipulator에 연결합니다. 그런 다음 확인 최종 반대 사이트와 리프트 아웃 무료 서 덩어리 (그림 2B)에서 프리 컷. </li><li> 추출 된 청크에 대한 좋은 공동을 갖는 쐐기 (직경 2-3 μm의) 지금 TEM 모 반 그리드의 날카로운 핀을 잘라. 백금 증착 (그림 2C)를 사용하여 핀에 덩어리를 장착합니다. 이 프리 컷 마침내 모 핀의 상단에있는 덩어리의 작은 부분 만 (2 μm의 주위에) 얻을 수 있도록. 그 후 거꾸로 그리드 홀더를 탑재하고 모 핀과 백금에 장착 된 조각 사이의 간격을 입력합니다. 남은 청크와 동일한 절차를 추구한다. 리프트 아웃에 대한 자세한 내용은절차 판독기는 다음을 참조 1:18을 참조 할 수 있습니다. </li><li> 수직 그리드를 배치하고 FIB의 낮은 가속 전압과 전류 빔 (5 kV의 및 &lt;50 PA)를 사용하여 덩어리의 단면 (얇은 백금 용접과 함께 사이트를 선택) 청소합니다. 따라서 하나의 매끄러운 표면 및 EBSD 측정에 필요한 가인 + 주입으로 인해 더 적은 오염을 가져옵니다. </li><li> 단면에서 수행 EBSD 측정의 관심 GB를 선택합니다. GB의 방향을 토론 부분에서 자세히 더 설명하는 지역 확대 효과 26를 줄이기 위해 원자 탐침 (Z 축)의 분석 방향에 대해 직각으로하는 것이 바람직하다. GB와 해당 영역은 그림 2 차원으로 강조 표시됩니다. </li><li> 예리한 끝을 형성하는 단계 2.6)에서 선택한 GB의 지역에있는 고리 모양의 밀링을 수행합니다. 곡률 반경은 더 TEM investigat을 위해 충분히 작은 (&lt;100 nm의)해야한다이온. 이 목표를 도달하는 단계 (그림 2E)로 환상 밀링 패턴 단계의 내부 직경을 줄이고 병용 이차 전자 (SE)에 의해 형성 끝을 시각화. 따라서 하나의 빔 변화를 수정하거나 서로 다른 효과 등 그림자, 수율을 스퍼터에서 발생하는 물질의 리플 또는 재 부착 등 첨단에 부정을 제거하는 밀링 패턴을 조정할 수 있습니다. </li><li> CIGS GB를이 SEM에 표시되지 않은 다른 물질 (초 내열 합금 등)에 비해 것을 알고, TEM 도구 (그림 2F 참조)를 사용하여 팁의 정점에 대하여 GB를의 정확한 위치를 집중. </li><li> GB는 APT 끝에서의 위치를​​ 정확하게 알고, FIB로 시험편을 전송하고 팁의 꼭대기 아래에 최대 200 nm에서 GB를 놓다 공장 샘플로 진행합니다. 이 단계에서, 밀링 매우 낮은 kV의 (5 kV의) 및 저 전류 (&lt;50 PA)에서 이루어집니다. 사실, 목표는 가까이 t GB를 지역​​화 할뿐만 아니라팁의 정점 O를, 또한 가인 +이 절차를 수행하는 동안 APT 팁의 피해를 최소화 할 수 있습니다. 병용 낮은 kV의 밀링에, SEM의 APT 팁의 형상을 시각화하고 팁의 정점 (그림 2G)에서 제거해야 재료의 양을 제어합니다. </li><li> TEM 다시 시험편을 전송하고 팁의 꼭대기에 관하여 GB의 위치를​​ 확인합니다. GB 위치, 시편 직경의 진화와 반 정강이 각도에 대한 정확한 지식을 얻기 위해 시편의 개요 이미지 (그림 2H)합니다. 이 APT 데이터의 최적의 재건을 달성하기 위해 필요합니다. 또한, 전자 빔에 의한 손상 및 APT 측정에서 높은 실패율로 이어질 수 C 오염을 최소화하기 위해 낮은 배율 및 감소 된 노출 시간을 사용합니다. </li></ol> 3. CAMECA의 LEAP 3000X HR 시스템에서 APT 분석 <ol><li> APT 보류에 시료를 장착어. 그런 다음, 사용 가능한 네 개의 회전 목마 중 하나의 표본 퍽을 장착합니다. </li><li> 로드 록 내부의 시편 퍽을 포함하는 회전 목마를 삽입하고로드 잠금을 펌핑 시작합니다. 로드 록 내부의 진공 ~ 10 -7 Torr의 경우, 버퍼 챔버 내부에 회전 목마를 삽입합니다. </li><li> 캘리포니아 대기 후. 버퍼 챔버 (~ 7X10 -9 Torr의)의 진공을 복원하는 1 시간은 버퍼 챔버에서 주 분석 챔버에 시험편을 전송합니다. 이 수동 작동 장치 수평 이동 막대와 함께 이루어집니다. </li><li> 60 K.에 온도 아래 APT, 시원한 내부 측정을 시작하기 전에이 낮은 온도는 분석 중에 시편의 표면에서 원자의 확산을 방지합니다. 우리는 60 K가 설정 온도가 아닌 시편의 레이저 열로 인해 더해야 APT 끝에서 측정 한 실제 온도는 것을 여기에서주의한다. 로 켈로그 등으로 제안했다. 27 일이 온도는진짜야이 계정에 상대적 충전 상태 비율을 복용하여 추정 할 수있다. CIGS 재료의 필드 증발 알 수 없기 때문에 불행히도,이 연구에서 팁의 실제 온도는 주로 계산 할 수 없습니다. </li><li> APT 실험은 532 nm의 12 PSEC 펄스 길이의 파장 녹색 레이저를 이용한 레이저 모드에서 수행됩니다. </li></ol> 4. APT 데이터의 재건 <ol><li> CAMECA의 통합 된 시각화 및 분석 소프트웨어 (IVAS 3.6.2)은 일반적으로 3D지도를 재구성하는 데 28.와 RHIT 파일 (원시 데이터를 직접 APT 측정 한 후 얻어진)를 엽니 다 </li><li> 다음과 같은 여덟 단계 28를 사용하여 3D지도의 재건을 수행합니다 : <ol><li> 1 단계 - 모든 특성에 대한 자세한 내용 및 선택한 연구의 내용을 제공하는 읽기 전용 창입니다 설치. </li><li> 2 단계 - 선택 이온 시퀀스 범위. 이 단계는 표본에 비해 이온 시퀀스 범위를 정의전압은 재구성 데이터를 선택할 수 있습니다. </li><li> 3 단계 - 선택 검출기 ROI. 이 단계는 발견 ROI (검출기 이벤트 히스토그램에 검은 타원) 외부에있는 이온을 제거 할 수있는 기회를 제공합니다. </li><li> 4 단계 - TOF의 수정. 이 단계는 비행 시간 (TOF), 전압을 계산하고 분석 검출기의 평탄도 ( &#39;는 그릇 수정&#39;) 수정. </li><li> 5 단계 - 질량 교정. 분석 질량 스펙트럼에서 측정 된 피크 위치가 알려진 동위 원소 / 충전 상태로 교정됩니다. </li><li> 6 단계 - 이온 할당였다. 이 단계에서 질량 스펙트럼의 피크 요소 동위 원소 범위에 할당됩니다. </li><li> 7 단계 - 재건축. 전압 방법, 정강이 각도 방법이나 팁 프로파일 방법 :이 단계는 획득 한 데이터에 세 가지 재건 방법 중 하나를 적용합니다. 마지막 하나는 우리의 3 차원지도를 재구성하는 현재의 연구에 사용됩니다. 이 방법은 TI의 SEM이나 TEM 이미지가 필요P는 그림의 2G와 그림 하반기에 표시. 재건의 어떤 시점에서 팁 반경은 SEM 이미지에서 정의 된 일련의 점 사이의 선형 보간에 의해 정의됩니다. </li><li> 8 단계 - 확인. 이 단계에서는 복원 탭에서 생성 된 미리보기가 저장된 분석으로 변환됩니다. </li></ol></li></ol>

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F., Gorman, B. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=In+situ+site-specific+specimen+preparation+for+atom+probe+tomography.">In situ site-specific specimen preparation for atom probe tomography.</a> Ultramicroscopy. 107 (2-3), 131-139 (2007).</li><li>Cadel, E., Barreau, N., Kessler, J., Pareige, P. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Atom+probe+study+of+sodium+distribution+in+polycristalline+Cu(In,Ga)Se2+thin+film.">Atom probe study of sodium distribution in polycristalline Cu(In,Ga)Se2 thin film.</a> Acta Material. 58, 2634-2637 (2010).</li><li>Schlesiger, R., Oberdorfer, C., W&#252;rz, R., Greiwe, G., Stender, P., Artmeier, M., Pelka, P., Spaleck, F., Schmitz, G. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Design+of+a+laser-assisted+tomographic+atom+probe+at+M&#252;nster+University.">Design of a laser-assisted tomographic atom probe at M&#252;nster University.</a> Rev. Sci. Instr. 81, 043703 (2010).</li><li>Cojocaru-Mir&#233;din, O., Choi, P., Abou-Ras, D., Schmidt, S. S., Caballero, R., Raabe, D. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Characterization+of+grain+boundaries+in+Cu(In,Ga)Se2+films+using+atom-probe+tomography.">Characterization of grain boundaries in Cu(In,Ga)Se2 films using atom-probe tomography.</a> IEEE J. Photovolt. 1 (2), 207-212 (2011).</li><li>Cojocaru-Mir&#233;din, O., Choi, P., Wuerz, R., Raabe, D. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Atomic-scale+characterization+of+the+CdS/CuInSe2+interface+in+thin-film+solar+cells.">Atomic-scale characterization of the CdS/CuInSe2 interface in thin-film solar cells.</a> Appl. Phys. Lett. 98, 103504-1-103504-3 (2011).</li><li>Couzinie-Devy, F., Cadel, E., Barreau, N., Arzel, L., Pareige, P. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Atom+probe+study+of+Cu-poor+to+Cu-rich+transition+during+Cu(In,Ga)Se2+growth.">Atom probe study of Cu-poor to Cu-rich transition during Cu(In,Ga)Se2 growth.</a> Appl. Phys. Lett. 99, 232108-1-232108-3 (2011).</li><li>Voorwinden, G., Jackson, P., Kniese, R., Powalla, M. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=In-line+Cu(In,Ga)Se2+co-evaporation+process+on+30+cm+x+30+cm+substrates+with+multiple+deposition+stages.">In-line Cu(In,Ga)Se2 co-evaporation process on 30 cm x 30 cm substrates with multiple deposition stages.</a> , 2115-2118 (2007).</li><li>Miller, M. K., Russell, K. F., Thompson, K., Alvis, R., Larson, D. 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H., Zunger, A., Katayama-Yoshida, H. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Defect+physics+of+the+CuInSe2+chalcopyrite+semiconductor.">Defect physics of the CuInSe2 chalcopyrite semiconductor.</a> Phys. Rev. B. 57, 9642-9656 (1998).</li><li>Cahn, J. W., Johnson, W. C., Blakely, J. M. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=.">.</a> Interfacial Segregation. , 3-23 (1979).</li><li>Miller, M. K., Jayaram, R. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Some+factors+affecting+analysis+in+atom+probe.">Some factors affecting analysis in atom probe.</a> Surf. 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Sci. 116, 273-301 (1982).</li><li>Letellier, L. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=.">.</a> Etude des joints de grains et interphases dans les superalliages Astroloy par microscopie electronique et tomographie atomique [dissertation]. , (1994).</li><li>Hoummada, I., Mangelinck, K., Chow, D., Lee, J., Bernardini, <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Original+methods+for+diffusion+measurements+in+polycrystalline+thin-films.">Original methods for diffusion measurements in polycrystalline thin-films.</a> Defect and Diffusion Forum. 322, 129-150 (2012).</li></ol>

<p class="jove_content"&gt; 저자는 공개 아무것도 없어.</p&gt;

현재 작업에서, 우리는 CIGS 태양 광 응용 프로그램에 사용되는 화합물 반도체 재료의 임의의 HAGB에 APT 결과를 발표했다. 또한, 우리는 또한 EBSD 및 TEM과 같은 보완 기술,와 함께 APT는 CIGS 태양 전지 구조 구성 속성 관계를 해명하는 강력한 도구입니다 것으로 나타났습니다. 첫째, EDX / 뱀장어는​​ 입자 경계에서 낮은 나와 O의 농도를 감지하고 둘째, EDX / EELS, 특히 모든 요소에 민감하지 않는 충분?...

<html> 흡수 물질로 황동광 구조의 화합물 반도체 구리 (, 조지아) 괜찮다 2 (CIGS)에 따라 박막 태양 전지 때문에 그들의 높은 효율, 방사선 경도, 장기 안정의 두 개 이상의 수십 년 동안 개발되었습니다 성능 및 낮은 생산 1-3 듭니다. 이러한 태양 전지 즉 CIGS 흡수층의 유리한 광학 특성, 직접 밴드 갭과 높은 흡수 계수 1,2로 인한에만 약간의 재료 소비량으로 제작 될 수 있습니다. 두께 몇 마이크로 미터의 흡수 필름​​은 높은 광전류를 생성하기에 충분합니다. 전극 photogenerated 전하 캐리어의 확산 경로가 상대적으로 짧은 있기 때문에, CIGS 흡수는 다결정 형태로 생성 할 수있다. 구리의 최대 효율 (조지아에서) 괜찮다 2까지 달성 (CIGS) 태양 전지는 모든 박막 태양 전지 중 가장 높은 값이 20.4 % 4입니다. ove_content &quot;&gt; 추가를 모두 생산 비용의 감소와 태양 전지 효율의 향상이 필수적이다. 후자는 CIGS 흡수층의 미세 화학 조성에 크게 의존한다. 내부 인터페이스, CIGS 박막 태양 광 기술을 확립하기 위해, 흡수기 내에서 특정 결정립 경계 (GB를), 그들은 photogenerated 전하 캐리어의 이동에 영향을 미칠 수 있으므로 중추적 인 역할을한다. CIGS 태양 전지와 관련된 주요 해결되지 않은 문제 중 하나는 CIGS GB를의 양성 본질, 즉 다결정 CIGS 흡수 필름 GB를하고 격자 결함 밀도에도 불구하고 뛰어난 전지 효율을 얻을 수 있습니다. 몇몇 저자들은 전기적 특성 5,6, 캐릭터와 misorientation 7-9뿐만 아니라 불순물 분리 10-13에 대하여 태양 급 CIGS 박막에서 GB를을 공부했다. 이 properti 사이 그러나 명확한 링크가 없습니다ES 지금까지 구축 할 수 있습니다. 특히, 지역의 화학 조성 및 GB를의 불순물 함량에 대한 정보의 상당한 부족이있다. 지난 20 년 동안, 아톰 프로브 단층 촬영 (APT) 유망 나노 분석 기술 14 ~ 17 중 하나로 떠오르고있다. 최근까지 태양 전지 APT 연구는 주로 샘플 준비 과정에서 어려움과 기존의 펄스 전압 원자 프로브를 사용하여 반도체 재료 분석의 제한된 기능에 의해 제한되었다. 이러한 제한은 대부분의 개발로 극복 한 &#39;리프트 아웃 방식&#39;에 초점을 맞춘 이온 빔 (FIB) 밀링 18, 16 APT 펄스 레이저의 도입에 따라. CIGS 태양 전지의 APT 특성에 대한 여러 논문을 강하게 자세한 조사를 위해 권장되는, 19-23 출판되었습니다. 본 논문에서는 나는 내부 연구 방법의 가이드 라인을 제공원자 탐침 단층 촬영 기술에 의한 CIGS의 nterfaces 박막 태양 전지.

atom probe tomography studies on the cu(in,ga)se2 grain boundaries

존재하지 않는 기술과 비교, 원자 탐침 단층 촬영 화학적 나노에서 세 차원의 내부 인터페이스를 특징 할 수 독특한 기술입니다. 사실, APT 높은 감도 (PPM의 순서대로)과 높은 공간 해상도 (이하 NM)를 보유하고있다. 상당한 노력이 알려진 구조를 원하는 입자 경계를 포함하는 APT 팁을 준비하기 위해 여기를 수행 하였다. 실제로, 사이트 별 샘플 준비하여 초점을 맞 춥니 이온 빔, 전자 후방 산란 회절 및 투과 전자 현미경 결합 된이 작품에 제시되어있다. 이 방법은 구리의 알려진 구조와 위치 (, 조지아) 괜찮다 원자 탐침 단층 촬영 연구 할 2 박막와 선택 입계 수 있습니다. 마지막으로, 우리는 구리의 그레인 경계 (조지아에서) 괜찮다 2 박막 태양 전지를 연구하는 원자 탐침 단층 촬영 기술을 사용의 장점과 단점에 대해 설명합니다.

그림 3은 사이드 뷰 (XZ 조각) 임의의 높은 각도 GB (HAGB) 28.5 원소지도를 보여줍니다 ° - &lt;511&gt; 새끼 사이트 별 준비 방법으로 그림 2에서 선택. CIGS HAGB에 나, K, 및 O의 공동 분리는 주로 APT 사용하여 매핑된다. 이러한 불순물은 대부분 ~ 600 ° C.에 CIGS 층의 증착시 흡수층으로 SLG 기판에서 확산 그림 4A 그림 3에 표시된 GB에 걸쳐있?...

Watch this Scientific Journal Video about Atom Probe Tomography Studies on the CuIn,GaSe2 Grain Boundaries at JoVE.com

Atom Probe Tomography Studies on the CuIn,GaSe2 Grain Boundaries

이 작품에서 우리는 CIGS 태양 전지의 광 흡수층의 곡물 경계를 공부 원자 탐침 단층 촬영 기술의 사용을 설명합니다. 알려진 구조로 원하는 입자 경계를 포함하는 원자 프로브 팁을 준비하는 새로운 접근 방식도 여기에 표시됩니다.

구리의 원자 조사 단층 촬영 연구 (, 조지아) 괜찮다<sub&gt; 2</sub&gt; 곡물 경계

Compared with the existent techniques, atom probe tomography is a unique technique able to chemically characterize the internal interfaces at the ...

atom-probe-tomography-studies-on-the-cu-inga-se2-grain-boundaries

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Atom Probe Tomography Studies on the Cu(In,Ga)Se2 Grain Boundaries

12.7K 조회수.  Max-Planck-Institut für Eisenforschung GmbH. 이 작품에서 우리는 CIGS 태양 전지의 광 흡수층의 곡물 경계를 공부 원자 탐침 단층 촬영 기술의 사용을 설명합니다. 알려진 구조로 원하는 입자 경계를 포함하는 원자 프로브 팁을 준비하는 새로운 접근 방식도 여기에 표시됩니다.

비디오: Atom Probe Tomography Studies on the CuIn,GaSe2 Grain Boundaries

In Situ Time-dependent Dielectric Breakdown in the Transmission Electron Microscope: A Possibility to Understand the Failure Mechanism in Microelectronic Devices

The time-dependent dielectric breakdown (TDDB) in on-chip interconnect stacks is one of the most critical failure mechanisms for microelectronic devices. The aggressive scaling of feature sizes, both on devices and interconnects, leads to serious challenges to ensure the required product reliability. Standard reliability tests and post-mortem failure analysis provide only limited information about the physics of failure mechanisms and degradation kinetics. Therefore it is necessary to develop new experimental approaches and procedures to study the TDDB failure mechanisms and degradation kinetics in particular. In this paper, an in situ experimental methodology in the transmission electron microscope (TEM) is demonstrated to investigate the TDDB degradation and failure mechanisms in Cu/ULK interconnect stacks. High quality imaging and chemical analysis are used to study the kinetic process. The in situ electrical test is integrated into the TEM to provide an elevated electrical field to the dielectrics. Electron tomography is utilized to characterize the directed Cu diffusion in the insulating dielectrics. This experimental procedure opens a possibility to study the failure mechanism in interconnect stacks of microelectronic products, and it could also be extended to other structures in active devices.

In Situ Time-dependent Dielectric Breakdown in the Transmission Electron Microscope: A Possibility to Understand the Failure Mechanism in Microelectronic Devices

The time-dependent dielectric breakdown (TDDB) in on-chip interconnect stacks is one of the most critical failure mechanisms for microelectronic devices. This paper demonstrates the procedure of an in situ TDDB experiment in the transmission electron microscope, which opens a possibility to study the failure mechanism in microelectronic products.

투과 전자 현미경에서 제자리 시간에 따른 절연 파괴에 : 가능성은 마이크로 전자 장치의 고장 메커니즘을 이해하기

The time-dependent dielectric breakdown (TDDB) in on-chip interconnect stacks is one of the most critical failure mechanisms for microelectronic devices. ...

연구

공학

Electron Channeling Contrast Imaging for Rapid III-V Heteroepitaxial Characterization

Misfit dislocations in heteroepitaxial layers of GaP grown on Si(001) substrates are characterized through use of electron channeling contrast imaging (ECCI) in a scanning electron microscope (SEM). ECCI allows for imaging of defects and crystallographic features under specific diffraction conditions, similar to that possible via plan-view transmission electron microscopy (PV-TEM). A particular advantage of the ECCI technique is that it requires little to no sample preparation, and indeed can use large area, as-produced samples, making it a considerably higher throughput characterization method than TEM. Similar to TEM, different diffraction conditions can be obtained with ECCI by tilting and rotating the sample in the SEM. This capability enables the selective imaging of specific defects, such as misfit dislocations at the GaP/Si interface, with high contrast levels, which are determined by the standard invisibility criteria. An example application of this technique is described wherein ECCI imaging is used to determine the critical thickness for dislocation nucleation for GaP-on-Si by imaging a range of samples with various GaP epilayer thicknesses. Examples of ECCI micrographs of additional defect types, including threading dislocations and a stacking fault, are provided as demonstration of its broad, TEM-like applicability. Ultimately, the combination of TEM-like capabilities &#8211; high spatial resolution and richness of microstructural data &#8211; with the convenience and speed of SEM, position ECCI as a powerful tool for the rapid characterization of crystalline materials.

The use of electron channeling contrast imaging in a scanning electron microscope to characterize defects in III-V/Si heteroexpitaxial thin films is described. This method yields similar results to plan-view transmission electron microscopy, but in significantly less time due to lack of required sample preparation.

빠른 III-V 족 이종 특성에 대한 전자 채널링 대비 이미징

Misfit dislocations in heteroepitaxial layers of GaP grown on Si(001) substrates are characterized through use of electron channeling contrast imaging ...

Energy Dispersive X-ray Tomography for 3D Elemental Mapping of Individual Nanoparticles

Energy dispersive X-ray spectroscopy within the scanning transmission electron microscope (STEM) provides accurate elemental analysis with high spatial resolution, and is even capable of providing atomically resolved elemental maps. In this technique, a highly focused electron beam is incident upon a thin sample and the energy of emitted X-rays is measured in order to determine the atomic species of material within the beam path. This elementally sensitive spectroscopy technique can be extended to three dimensional tomographic imaging by acquiring multiple spectrum images with the sample tilted along an axis perpendicular to the electron beam direction.
Elemental distributions within single nanoparticles are often important for determining their optical, catalytic and magnetic properties. Techniques such as X-ray tomography and slice and view energy dispersive X-ray mapping in the scanning electron microscope provide elementally sensitive three dimensional imaging but are typically limited to spatial resolutions of &gt; 20 nm. Atom probe tomography provides near atomic resolution but preparing nanoparticle samples for atom probe analysis is often challenging. Thus, elementally sensitive techniques applied within the scanning transmission electron microscope are uniquely placed to study elemental distributions within nanoparticles of dimensions 10-100 nm.
Here, energy dispersive X-ray (EDX) spectroscopy within the STEM is applied to investigate the distribution of elements in single AgAu nanoparticles. The surface segregation of both Ag and Au, at different nanoparticle compositions, has been observed.

The use of energy dispersive X-ray tomography in the scanning transmission electron microscope to characterize elemental distributions within single nanoparticles in three dimensions is described.

개별 나노 입자의 3D 원소 매핑에 대한 에너지 분산 X 선 단층 촬영

Energy dispersive X-ray spectroscopy within the scanning transmission electron microscope (STEM) provides accurate elemental analysis with high spatial ...

Epitaxial Growth of Perovskite Strontium Titanate on Germanium via Atomic Layer Deposition

Atomic layer deposition (ALD) is a commercially utilized deposition method for electronic materials. ALD growth of thin films offers thickness control and conformality by taking advantage of self-limiting reactions between vapor-phase precursors and the growing film. Perovskite oxides present potential for next-generation electronic materials, but to-date have mostly been deposited by physical methods. This work outlines a method for depositing SrTiO3 (STO) on germanium using ALD. Germanium has higher carrier mobilities than silicon and therefore offers an alternative semiconductor material with faster device operation. This method takes advantage of the instability of germanium's native oxide by using thermal deoxidation to clean and reconstruct the Ge (001) surface to the 2&#215;1 structure. 2-nm thick, amorphous STO is then deposited by ALD. The STO film is annealed under ultra-high vacuum and crystallizes on the reconstructed Ge surface. Reflection high-energy electron diffraction (RHEED) is used during this annealing step to monitor the STO crystallization. The thin, crystalline layer of STO acts as a template for subsequent growth of STO that is crystalline as-grown, as confirmed by RHEED. In situ X-ray photoelectron spectroscopy is used to verify film stoichiometry before and after the annealing step, as well as after subsequent STO growth. This procedure provides framework for additional perovskite oxides to be deposited on semiconductors via chemical methods in addition to the integration of more sophisticated heterostructures already achievable by physical methods.

This work details the procedures for the growth and characterization of crystalline SrTiO3 directly on germanium substrates by atomic layer deposition. The procedure illustrates the ability of an all-chemical growth method to integrate oxides monolithically onto semiconductors for metal-oxide semiconductor devices.

원자 층 증착을 통해 게르마늄에 페 로브 스카이 스트론튬 티탄의 에피 택셜 성장

Atomic layer deposition (ALD) is a commercially utilized deposition method for electronic materials. ALD growth of thin films offers thickness control and ...

화학

Comprehensive Characterization of Extended Defects in Semiconductor Materials by a Scanning Electron Microscope

Extended defects such as dislocations and grain boundaries have a strong influence on the performance of microelectronic devices and on other applications of semiconductor materials. However, it is still under debate how the defect structure determines the band structure, and therefore, the recombination behavior of electron-hole pairs responsible for the optical and electrical properties of the extended defects. The present paper is a survey of procedures for the spatially resolved investigation of structural and of physical properties of extended defects in semiconductor materials with a scanning electron microscope (SEM). Representative examples are given for crystalline silicon. The luminescence behavior of extended defects can be investigated by cathodoluminescence (CL) measurements. They are particularly valuable because spectrally and spatially resolved information can be obtained simultaneously. For silicon, with an indirect electronic band structure, CL measurements should be carried out at low temperatures down to 5 K due to the low fraction of radiative recombination processes in comparison to non-radiative transitions at room temperature. For the study of the electrical properties of extended defects, the electron beam induced current (EBIC) technique can be applied. The EBIC image reflects the local distribution of defects due to the increased charge-carrier recombination in their vicinity. The procedure for EBIC investigations is described for measurements at room temperature and at low temperatures. Internal strain fields arising from extended defects can be determined quantitatively by cross-correlation electron backscatter diffraction (ccEBSD). This method is challenging because of the necessary preparation of the sample surface and because of the quality of the diffraction patterns which are recorded during the mapping of the sample. The spatial resolution of the three experimental techniques is compared.

The optical, electrical, and structural properties of dislocations and of grain boundaries in semiconductor materials can be determined by experiments performed in a scanning electron microscope. Electron microscopy has been used to investigate cathodoluminescence, electron beam induced current, and diffraction of backscattered electrons.

Extended defects such as dislocations and grain boundaries have a strong influence on the performance of microelectronic devices and on other applications ...

A Novel Method for In Situ Electromechanical Characterization of Nanoscale Specimens

Electrically assisted deformation (EAD) is increasingly being used to improve the formability of metals during processes such as sheet metal rolling and forging. Adoption of this technique is proceeding despite disagreement concerning the underlying mechanism responsible for EAD. The experimental procedure described herein enables a more explicit study compared to previous EAD research by removing thermal effects, which are responsible for disagreement in interpreting previous EAD results. Furthermore, as the procedure described here enables EAD observation in situ and in real time in a transmission electron microscope (TEM), it is superior to existing post-mortem methods that observe EAD effects post-test. Test samples consist of a single crystal copper (SCC) foil having a free-standing tensile test section of nanoscale thickness, fabricated using a combination of laser and ion beam milling. The SCC is mounted to an etched silicon base that provides mechanical support and electrical isolation while serving as a heat sink. Using this geometry, even at high current density (~3,500 A/mm2), the test section experiences a negligible temperature increase (&#60;0.02 &#176;C), thus eliminating Joule heating effects. Monitoring material deformation and identifying the corresponding changes to microstructures, e.g. dislocations, are accomplished by acquiring and analyzing a series of TEM images. Our sample preparation and in situ experiment procedures are robust and versatile as they can be readily utilized to test materials with different microstructures, e.g., single and polycrystalline copper.

A Novel Method for In Situ Electromechanical Characterization of Nanoscale Specimens

Isolating electrical and thermal effects on electrically assisted deformation (EAD) is very difficult using macroscopic samples. Metallic sample micro- and nanostructures together with a custom test procedure have been developed to evaluate the impact of applied current on the formation without joule heating and evolution of dislocations on these samples.

에 대한 소설 방법<em&gt; 현장에서</em&gt; 나노 크기 시편의 전자 기계적 특성 분석

Electrically assisted deformation (EAD) is increasingly being used to improve the formability of metals during processes such as sheet metal rolling and ...

Atom Probe Tomography Analysis of Exsolved Mineral Phases

Element diffusion rates and temperature/pressure control a range of fundamental volcanic and metamorphic processes. Such processes are often recorded in lamellae exsolved from host mineral phases. Thus, the analysis of the orientation, size, morphology, composition and spacing of exsolution lamellae is an area of active research in the geosciences. The conventional study of these lamellae has been conducted by scanning electron microscopy (SEM) and transmission electron microscopy (TEM), and more recently with focused ion beam (FIB)-based nanotomography, yet with limited chemical information. Here, we explore the use of atom probe tomography (APT) for the nanoscale analysis of ilmenite exsolution lamellae in igneous titanomagnetite from ash deposits erupted from the active Soufri&#232;re Hills Volcano (Montserrat, British West Indies). APT allows the precise calculation of interlamellar spacings (14&#8211;29 &#177; 2 nm) and reveals smooth diffusion profiles with no sharp phase boundaries during the exchange of Fe and Ti/O between the exsolved lamellae and the host crystal. Our results suggest that this novel approach permits nanoscale measurements of lamellae composition and interlamellar spacing that may provide a means to estimate the lava dome temperatures necessary to model extrusion rates and lava dome failure, both of which play a key role in volcanic hazard mitigation efforts.

Analysis of the morphology, composition, and spacing of exsolution lamellae can provide essential information to understand geological processes related to volcanism and metamorphism. We present a novel application of APT for the characterization of such lamellae and compare this approach to the conventional use of electron microscopy and FIB-based nanotomography.

원자 프로브 단층 촬영 분석 의 Exsolved 광물 상

Element diffusion rates and temperature/pressure control a range of fundamental volcanic and metamorphic processes. Such processes are often recorded in ...

환경과학

Processing of Bulk Nanocrystalline Metals at the US Army Research Laboratory

Given their potential for significant property improvements relative to their large grained counterparts, much work has been devoted to the continued development of nanocrystalline metals. Despite these efforts, the transition of these materials from the lab bench to actual applications has been blocked by the inability to produce large scale parts that retain the desired nanocrystalline microstructures. Following the development of a method proven to stabilize the nanosized grain structure to temperatures approaching that of the melting point for the given metal, the US Army Research Laboratory (ARL) has progressed to the next stage in the development of these materials - namely the production of large scale parts suitable for testing and evaluation in a range of relevant test environments. This report provides a broad overview of the ongoing efforts in the processing, characterization, and consolidation of these materials at ARL. In particular, focus is placed on the methodology used for producing the nanocrystalline metal powders, in both small and large-scale amounts, that are at the center of ongoing research efforts.

This paper provides a brief overview of the ongoing efforts at the Army Research Laboratory on the processing of bulk nanocrystalline metals with an emphasis on the methodologies used for the production of the novel metal powders.

미국 육군 연구소에서 대량 Nanocrystalline 금속 처리

Given their potential for significant property improvements relative to their large grained counterparts, much work has been devoted to the continued ...

Theoretical Calculation and Experimental Verification for Dislocation Reduction in Germanium Epitaxial Layers with Semicylindrical Voids on Silicon

Reduction of threading dislocation density (TDD) in epitaxial germanium (Ge) on silicon (Si) has been one of the most important challenges for the realization of monolithically integrated photonics circuits. The present paper describes methods of theoretical calculation and experimental verification of a novel model for the reduction of TDD. The method of theoretical calculation describes the bending of threading dislocations (TDs) based on the interaction of TDs and non-planar growth surfaces of selective epitaxial growth (SEG) in terms of dislocation image force. The calculation reveals that the presence of voids on SiO2 masks help to reduce TDD. Experimental verification is described by germanium (Ge) SEG, using an ultra-high vacuum chemical vapor deposition method and TD observations of the grown Ge via etching and cross-sectional transmission electron microscope (TEM). It is strongly suggested that the TDD reduction would be due to the presence of semicylindrical voids over the SiO2 SEG masks and growth temperature. For experimental verification, epitaxial Ge layers with semicylindrical voids are formed as the result of SEG of Ge layers and their coalescence. The experimentally obtained TDDs reproduce the calculated TDDs based on the theoretical model. Cross-sectional TEM observations reveal that both the termination and generation of TDs occur at semicylindrical voids. Plan-view TEM observations reveal a unique behavior of TDs in Ge with semicylindrical voids (i.e., TDs are bent to be parallel to the SEG masks and the Si substrate).

Theoretical calculation and experimental verification are proposed for a reduction of threading dislocation (TD) density in germanium epitaxial layers with semicylindrical voids on silicon. Calculations based on the interaction of TDs and surface via image force, TD measurements, and transmission electron microscope observations of TDs are presented.

실리콘에 반원통형 공극이 있는 게르마늄 에피택셜 층의 전위 감소에 대한 이론적 계산 및 실험적 검증

Reduction of threading dislocation density (TDD) in epitaxial germanium (Ge) on silicon (Si) has been one of the most important challenges for the ...

Sample Preparation and Experimental Design for In Situ Multi-Beam Transmission Electron Microscopy Irradiation Experiments

There is a need to understand materials exposed to overlapping extreme environments such as high temperature, radiation, or mechanical stress. When these stressors are combined there may be synergistic effects that enable unique microstructural evolution mechanisms to activate. Understanding of these mechanisms is necessary for the input and refinement of predictive models and critical for engineering of next generation materials. The basic physics and underlying mechanisms require advanced tools to be investigated. The in situ ion irradiation transmission electron microscope (I&#179;TEM) is designed to explore these principles.
To quantitatively probe the complex dynamic interactions in materials, careful preparation of samples and consideration of experimental design is required. Particular handling or preparation of samples can easily introduce damage or features that obfuscate the measurements. There is no one correct way to prepare a sample; however, many mistakes can be made. The most common errors and things to consider are highlighted within. The I&#179;TEM has many adjustable variables and a large potential experimental space, therefore it is best to design experiments with a specific scientific question or questions in mind.
Experiments have been performed on large number of sample geometries, material classes, and with many irradiation conditions. The following are a subset of examples that demonstrate unique in situ capabilities utilizing the I3TEM. Au nanoparticles prepared by drop casting have been used to investigate the effects of single ion strikes. Au thin films have been used in studies on the effects of multibeam irradiation on microstructure evolution. Zr films have been exposed to irradiation and mechanical tension to examine creep. Ag nanopillars were subjected to simultaneous high temperature, mechanical compression, and ion irradiation to study irradiation induced creep as well. These results impact fields including: structural materials, nuclear energy, energy storage, catalysis, and microelectronics in space environments.

Sample preparation techniques are outlined with specific considerations for in situ ion irradiation TEM experiments. Ion species, energy, and fluence are discussed with methods for how to select and compute them. Finally, procedures for conducting an experiment are described and accompanied by the representative results.

There is a need to understand materials exposed to overlapping extreme environments such as high temperature, radiation, or mechanical stress. When these ...

구리의 원자 조사 단층 촬영 연구 (, 조지아) 괜찮다

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