This research was funded by the International Research Training Group (IRTG) &#8220;Diffusion in porous Materials&#8221;. We acknowledge the technical support from Gert Klotzsche and stimulating discussions with Steven Reichhardt, Thomas Meissner, Damian Rybicki, Tobias Herzig, Natalya Georgieva, Jonas Kohlrautz, and Michael Jurkutat.

1 설치 및 6H-SiC를 대형 콘 Boehler 형 모루의 조심 <ol><li> 장착 도구의 피스톤과 XY 판을 수정하고 휴식 공간에서 Boehler 형 받침대를 삽입합니다. </li><li> 확실히 각 받침대는 받침 플레이트에 단단히 앉아합니다. </li><li> (예 Stycast 1266)는, 자신에게 모두 좌석 앤빌 접착제, 에폭시 수지를 사용. RT에서 12 시간 또는 2 시간 동안 노에서 65 ºC위한 치료. </li><li> 충분한 모루 정렬의 경우, 백킹 플레이트를 정렬하고 두 받침대의 병렬 처리를 모니터하기 위해 M1 세트 스크류를 사용합니다. 앤빌은 비평 것으로 발견된다면, 에폭시 수지를 제거하고, 포인트 120에서 다시 시작. </li></ol> 2 가스켓 준비 <ol><li> 어닐링 구리 - 수의 칩으로 드릴 1mm 구멍 황동 가이드 핀 (% w 구리 (98)는, 2 중량 %, 0.5 mm의 두께로한다). </li><li> GUID의 역할을하는, 앤빌 따라 분포되는 구멍으로 세 5mm 1 mm 직경의 비 절연 된 구리 와이어의 긴 조각을 삽입구리가 되실 가스켓 전자 핀. </li><li> 가이드 핀과 세포체 사이의 적절한 접지를 확인합니다. 통상적으로, 약 0.1 Ω의 DC 저항은 바람직하다. 전도성 실버 소량의 응용 프로그램을 개선 할 수 있습니다. </li><li> 모이 사 나이트 모루 위에 구리가 되실 칩을 삽입하고 셀을 닫습니다. </li><li> 유압 프레스를 사용하여 극대화 된 작업의 안정성을 위해 culet 직경의 약 8 일에 가스켓 압력을. 마이크로 미터 캘리퍼스를 사용하여 들여 쓰기의 실제 두께를 모니터링합니다. </li><li> 들여 쓰기의 중심에 적절한 직경 (culet 직경의 ½)의 구멍을 뚫습니다. </li><li> 사전 들여 가스켓으로이 채널을 개척. 채널은 마이크로 코일 18 μm의 구리 와이어를 수용 할 수있을 정도로 충분히 깊게해야한다. </li><li> 강화로에서 2 시간 3에 대한 617 K에서 제조 된 가스켓. </li></ol> 3 준비 및 마이크로 코일의 로딩 <ol><li> 1mm 구리 와이어의 조각을 사용하여피스톤의 관통 구를 통해 스레드 ㄹ. 에폭시 수지와 구리 와이어를 고정하여 단계 1.3에 따라 치료. </li><li> 마이크로 코일 원하는 직경이 송곳 (물질의 목록 참조)을 선택하고 회전 척 - 한 쌍의 죠 (jaw) 사이에 고정합니다. </li><li> 접착제 다른 쪽 끝을 잡고, 척 턱 위에 18 μm의 구리 와이어의 한쪽 끝 (SCB에서 예를 들면, 니스와 함께, 물질의 목록 참조)와 와이어가 송곳에 코일되도록 척 턱을 돌립니다. </li><li> 마이크로 코일을 원하는 형상의 경우뿐만 아니라, 접착제에 와이어의 타단을 고정한다. </li><li> 권선 위에 소량을인가함으로써 상기 코일을 고정하기 위해 희석 된 바니쉬를 사용한다. </li><li> 테프론 테이프를 사용하여 송곳에서 신중하게 코일을 제거합니다. </li><li> 개스킷의 채널에서, 어떠한 첨가물없이, 일부 에폭시 수지 (1.3 포인트 참조) 놓는다. </li><li> 샘플 챔버 내부의 마이크로 코일을 배치하고 채널로 리드를 고정합니다. </li><li> EPOX을 치료Y 수지있어서 1.3로 진행한다. </li><li> 열선에 마이크로 코일과 가이드 핀에 다른 하나의 리드를 납땜. </li><li> 각 접합의 상단에 약간은 도전성 페이스트를 추가합니다. 일반적으로 치료하는 것은 어떤 분 정도 소요됩니다. </li><li> 에폭시 수지의 양쪽과 소량의 접합부를 밀봉. </li><li> 130 단계에있어서, 에폭시 경화. </li><li> 이제, 각 단계 후에 코일의 DC 저항을 확인. </li><li> 마이크로 코일의 샘플을 놓습니다. 불필요한 신체 접촉은 코일을 파괴 할 수 있음을주의하십시오. </li><li> 압력 보정을위한 시료에 미세하게 분쇄 루비 파우더를 추가합니다. </li><li> 마지막으로, 적절한 압력 매체와 샘플 챔버 홍수. 9 GPa로까지 거의 - 수압 조건을 보장하기 위해 파라핀 오일을 사용합니다. </li><li> 조심스럽게 셀을 닫습니다. </li></ol> (4) 적용 및 압력 모니터링 <ol><li> 처음에는 약간 M3 육각 접시 머리 나사를 조입니다. </li><li> 가압은 바이스에 셀을 수정합니다. 이제, 조마주 보는 두 개의 나사 페어. </li><li> 적절한 셀 홀더에 압력 셀을 놓습니다. </li><li> 레이저 빔이 샘플 챔버에 도달 할 수 있도록 셀의 위치를​​ 조정한다. </li><li> 레이저 빔에 루비 파우더 초점을 미세 조정 테이블을 사용합니다. </li><li> 분광계 해당 소프트웨어를 사용하여 루비 광 발광 스펙트럼을 모니터한다. </li><li> 루비 R1과 R2 라인의 관찰 된 스펙트럼 변화에서 샘플 공동의 실제 압력의 압축을 풉니 다. </li><li> NMR 측정이 시작되기 전에 최소 12 시간 동안 세포를 가압 평형. </li></ol> 5 수행 NMR 실험 <ol><li> 일반적인 NMR 프로브에 압력 셀을 탑재합니다. 기계 작업장에서 적절한 셀 홀더 제조. </li><li> 프로브에 열선을 납땜. 셀과 프로브 사이의 적절한 전기적 접촉을 확인합니다. </li><li> 이제 표준 NMR 실험을 수행합니다. 마이크로 코일 VER 사실에주의를 집중인가 고주파 전력에 민감한 Y. </li></ol>

<ol>
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The authors have nothing to disclose.

기가 파스칼 압력에서 NMR을 수행 할 수있는 새로운 유망 방법에 대하여 설명 하였다. 이 방법으로 인해 우수한 감도와 해상도로 NMR 실험의 폭 넓은 다양한 문을 엽니 다. 그럼에도 불구하고, 프로토콜 절에 설명 된 여러 단계의 실험 결과에 결정적이다. 특히, 마이크로 코일의 준비 및 구리 되실 가스켓에서의 고정이 매우 어렵고 경험이 필요합니다. 다음에, 몇 가지 중요한 팁은 기술의 최초의 성?...

지난 세기의 시작 부분에서 높은 수압 압력에서 응축 물질의 퍼시 브리지 먼의 특징 실험 이후, 고압 물리학의 분야는 급속 한 발전했다. 흥미로운 현상의 많은 여러 GPa로 (2)의 압력에 따라 발생하는 것으로 알려져있다. 또한, 고압으로 응축 물질 시스템의 응답은 우리에게 자신의 전자 지상과 흥분 상태 3,4에 대해 많은 것을 가르쳤다. 불행하게도, 기가 파스칼의 압력에서 응축 물질의 전기적 성질의 조사 기술은 X 선이나 방법 5를 선도 DC 저항 측정으로 드물다. 특히, 전자 스핀 (ESR) 또는 핵 자기 공명 (NMR) 실험으로 전자 또는 핵 자기 모멘트의 검출은 하나의 신호를 검색 할 필요 전형적인 고압 앤빌 세포에서 구현하는 것은 거의 불가능할 수밖에 작은 Volume 받침대 및 밀봉 가스켓에 안치. 몇몇 그룹이 복소 배열을 사용하여이 문제를 해결하는 시도 등이 분할 한 쌍의 무선 주파수 (RF) 코일은 받침대 (6)의 측면을 따라 감겨, 단일 또는 이중 루프 머리 핀 공진기 7,8; . 예컨대 1과 핵 γ - 또는 RF 픽업 코일 (9),도 1 참조 심지어 분할 레늄 가스켓 불행히도, 그러한 접근법은 여전히 대형까지 실험 응용을 제한, 낮은 신호 대 잡음비 (SNR)을 앓고 H 10. 15 - 관심있는 독자는 다른 고압 공진 탱크 회로 실험 11 지칭 될 수있다. Pravica 및 Silvera 16 보고서 수소의 오르토 - 파라 변환을 공부 12.8 GPa로와 NMR에 대한 앤빌 셀에 달성 된 가장 높은 압력. NMR을 적용에 큰 관심과 함께양자 고체의 특성을 연구하기 위해, 우리 그룹뿐만 아니라, 높은 압력에서 사용할 수 NMR 데에 관심이 있었다. 마지막으로, 2009 년에이를 공명 무선 주파수 (RF) 마이크로 코일 (17)을 둘러싸는 샘플 고압 캐비티에 직접 배치되는 경우 고감도 앤빌 셀 NMR 정말로 가능하다는 것을 입증 할 수 있었다. 이러한 접근법에서, NMR 감도의 분말 샘플에 대해 17 O NMR 예 더욱 도전 NMR 실험을 가능하게, (RF 코일의 계수를 채우기에 주로 기인 극적인 증가) 수십배에 의해 향상된다 최대 7 GPa로 (18)에서 고온 초전도체. 이들 재료의 초전도 크게 압력의인가에 의해 증폭 될 수 있으며, 프로세스에 지배 근본적인 통찰력을 약속 로컬 전자 탐침이 프로세스를 수행하는 것이 가능하다. 무엇인지 고압 NMR의 힘에 대한 또 다른 예는 등장 believED 루틴 퍼런 실험으로 : - 단순 알루미늄 금속을 도입 새로운 앤빌 셀 NMR을 테스트하기 위해, 잘 알려진 물질 중 하나를 측정 하였다. 압력이 증가함에 따라, 하나는 자유 전자 시스템에 대해 무엇을 기대에서 NMR 변화의 예기치 않은 편차가 발견되었다. 증가 된 압력에 따라 또한, 실험을 반복, 새로운 결과가 참으로 신뢰할 수있는 것으로 나타났다. 컴퓨팅 파워가 낮을 때 마지막 밴드 구조 계산으로는, 결과 년전 계산에 의해 검출 될 수없는 알루미늄 페르미 표면의 위상 전이의 표현 인 것으로 밝혀졌다. 주변 조건에 대한 연구 결과의 외삽은 거의 모든 곳에서 사용이 금속의 성질이 특별한 전자 조건에 의해 영향을받는 것으로 나타났다. 서로 다른 응용 프로그램의 수를 추구하기 위해 특별히 디자인 된 앤빌 셀 (이전 셀은 Cavend에서 수입했다NMR을 위해 개조 틱 연​​구소와) 개발되었다. 현재 사용되는 조립식 섀시는 800 μM의 culet 6H-SiC를 앤빌의 쌍을 사용하여 25 GPa의 최대 압력에 도달 할 수있다. NMR 실험은 성공적 지금까지, 10.1 GPa로까지 수행 하였다. 이 새로운 셀 NMR 성능은 19 우수한 것으로 나타났다. 주성분은 티타늄 - 알루미늄 (6) -Vanadium (4)에 대한 (800)의 항복 강도가 20 MPa로 제공 여분 낮은 격자 간 레벨 (등급 23)와. 인해 비 자기 특성 (자기 자화율 χ 약 5 ppm의 경우)는 앤빌 셀 섀시의 적절한 소재이다. 도입 된 세포 (모든 조립식 앤빌 셀 설계의 개요를 그림 2 참조)의 전체 크기는 일반 표준 구멍 NMR 자석에 들어갈 정도로 작다. 높이 만 20mm, 직경 17mm 인 작은 디자인, LAC-TM1은 또한 전형적인 작은 냉간 구멍 자석 (30mm 구멍 직경)에 적합합니다. L저자 설계된 최신 섀시 인 AC-TM2는 (내부 압력의 매끄러운 제어에 부착 청사진을 허용 압력 구동 메커니즘 (셀 섀시와 같은 합금으로 만들어진) 사 M4 육각 카운터 싱크 볼트를 사용 보충 절). 통상적으로, 다이아몬드 앤빌 100 GPa의 전술의 최고 압력을 생성하기 위해 사용된다. 쑤 마오 21-23 moissanite의 앤빌은 약 60 GPa의 압력의 최대 고압 연구 비용 효율적인 대안을 제공하는 것을 보여 주었다. 따라서, 모이 사 나이트 모루는 도입 GPa의 NMR 방법을 사용 하였다. 가장 좋은 결과는 찰스 &amp; Colvard의 모루 부서의 사용자 정의 대형 콘 6H-SiC를 모루 달성 하였다. 그 세포로, 1​​0.1 GPa의 최대 압력에 대해, 800 μM의 culet 앤빌의 사용은 아주 좋은 NMR 감도가 낮아 밝혀졌다. 비교를 위해, Lee 등은 알. 1 H NM 1의 SNR을보고도입 마이크로 코일 방식의 SNR에도 약간 낮은 자기장에서의 7.2 부피에 대해 25의 값을 보였다 수돗물 R,. 현대 물질의 물리와 화학에 흥미 진진한 새로운 통찰력을 약속 많은 응용 프로그램을 추구 할 수 고감도 세포와 모루 NMR의 일에이 새로운 접근 방식. 하나는 작은 크기 culet 요구 훨씬 높은 압력 관심 경우에는 항상 같은 감도 및 해상도는 궁극적으로, 특히, NMR의 적용을 제한한다. 그런 다음, 하나는 더 작은 RF 코​​일과 셀 설계를 최적화뿐만 아니라, 핵 분극을 증가시키기위한 방법에 대해 생각뿐만 아니라 있습니다.

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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.

그림 3은 일반적인 NMR 프로브 상에 완전히 조립 된 압력 셀, 배선 및 설치가 같이 방법을 보여줍니다. 다음에 몇 가지 실험 이점과 도입 기술의 한계에 대한 광범위한 개요를 수집하는 독자를 활성화해야하는 검토 될 것이다. <img alt="그림 1" src="/files/ftp_upload/52243/52243fig1highres.jpg" /> 그림 고압 NMR에 대한 다양한 접근 방법 1 :</s...

Watch this Scientific Journal Video about High-Sensitivity Nuclear Magnetic Resonance at Giga-Pascal Pressures: A New Tool for Probing Electronic and Chemical Properties of Condensed Matter under Extr

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 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 ...

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Principles of Nuclear Magnetic Resonance

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11.5K 조회수.  University of Leipzig. 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.

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

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 ...

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공학

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 ...

Measuring Material Microstructure Under Flow Using 1-2 Plane Flow-Small Angle Neutron Scattering

A new small-angle neutron scattering (SANS) sample environment optimized for studying the microstructure of complex fluids under simple shear flow is presented. The SANS shear cell consists of a concentric cylinder Couette geometry that is sealed and rotating about a horizontal axis so that the vorticity direction of the flow field is aligned with the neutron beam enabling scattering from the 1-2 plane of shear (velocity-velocity gradient, respectively). This approach is an advance over previous shear cell sample environments as there is a strong coupling between the bulk rheology and microstructural features in the 1-2 plane of shear. Flow-instabilities, such as shear banding, can also be studied by spatially resolved measurements. This is accomplished in this sample environment by using a narrow aperture for the neutron beam and scanning along the velocity gradient direction. Time resolved experiments, such as flow start-ups and large amplitude oscillatory shear flow are also possible by synchronization of the shear motion and time-resolved detection of scattered neutrons. Representative results using the methods outlined here demonstrate the useful nature of spatial resolution for measuring the microstructure of a wormlike micelle solution that exhibits shear banding, a phenomenon that can only be investigated by resolving the structure along the velocity gradient direction. Finally, potential improvements to the current design are discussed along with suggestions for supplementary experiments as motivation for future experiments on a broad range of complex fluids in a variety of shear motions.

A shear cell is developed for small-angle neutron scattering measurements in the velocity-velocity gradient plane of shear and is used to characterize complex fluids. Spatially resolved measurements in the velocity gradient direction are possible for studying shear-banding materials. Applications include investigations of colloidal dispersions, polymer solutions, and self-assembled structures.

1-2 평면 흐름 - 작은 각 중성자 산란을 이용하여 재료 미세 조직에서 유량을 측정

A new small-angle neutron scattering (SANS) sample environment optimized for studying the microstructure of complex fluids under simple shear flow is ...

Flame Experiments at the Advanced Light Source: New Insights into Soot Formation Processes

The following experimental protocols and the accompanying video are concerned with the flame experiments that are performed at the Chemical Dynamics Beamline of the Advanced Light Source (ALS) of the Lawrence Berkeley National Laboratory1-4. This video demonstrates how the complex chemical structures of laboratory-based model flames are analyzed using flame-sampling mass spectrometry with tunable synchrotron-generated vacuum-ultraviolet (VUV) radiation. This experimental approach combines isomer-resolving capabilities with high sensitivity and a large dynamic range5,6. The first part of the video describes experiments involving burner-stabilized, reduced-pressure (20-80 mbar) laminar premixed flames. A small hydrocarbon fuel was used for the selected flame to demonstrate the general experimental approach. It is shown how species&#8217; profiles are acquired as a function of distance from the burner surface and how the tunability of the VUV photon energy is used advantageously to identify many combustion intermediates based on their ionization energies. For example, this technique has been used to study gas-phase aspects of the soot-formation processes, and the video shows how the resonance-stabilized radicals, such as C3H3, C3H5, and i-C4H5, are identified as important intermediates7. The work has been focused on soot formation processes, and, from the chemical point of view, this process is very intriguing because chemical structures containing millions of carbon atoms are assembled from a fuel molecule possessing only a few carbon atoms in just milliseconds. The second part of the video highlights a new experiment, in which an opposed-flow diffusion flame and synchrotron-based aerosol mass spectrometry are used to study the chemical composition of the combustion-generated soot particles4. The experimental results indicate that the widely accepted H-abstraction-C2H2-addition (HACA) mechanism is not the sole molecular growth process responsible for the formation of the observed large polycyclic aromatic hydrocarbons (PAHs).

Gas sampling from laboratory-scale flames with online analysis of all species by mass spectrometry is a powerful method to investigate the complex mixture of chemical compounds occurring during combustion processes. Coupled with tunable soft ionization via synchrotron-generated vacuum-ultraviolet radiation, this technique provides isomer-resolved information and potentially fragment-free mass spectra.

고급 광원 불꽃 실험 : 그을음 형성 프로세스에 새로운 통찰력

The following experimental protocols and the accompanying video are concerned with the flame experiments that are performed at the Chemical Dynamics ...

In Situ Neutron Powder Diffraction Using Custom-made Lithium-ion Batteries

Li-ion batteries are widely used in portable electronic devices and are considered as promising candidates for higher-energy applications such as electric vehicles.1,2 However, many challenges, such as energy density and battery lifetimes, need to be overcome before this particular battery technology can be widely implemented in such applications.3 This research is challenging, and we outline a method to address these challenges using in situ NPD to probe the crystal structure of electrodes undergoing electrochemical cycling (charge/discharge) in a battery. NPD data help determine the underlying structural mechanism responsible for a range of electrode properties, and this information can direct the development of better electrodes and batteries.
We briefly review six types of battery designs custom-made for NPD experiments and detail the method to construct the &#8216;roll-over&#8217; cell that we have successfully used on the high-intensity NPD instrument, WOMBAT, at the Australian Nuclear Science and Technology Organisation (ANSTO). The design considerations and materials used for cell construction are discussed in conjunction with aspects of the actual in situ NPD experiment and initial directions are presented on how to analyze such complex in situ data.

In Situ Neutron Powder Diffraction Using Custom-made Lithium-ion Batteries

We describe the design and construction of an electrochemical cell for the examination of electrode materials using in situ neutron powder diffraction (NPD). We briefly comment on alternate in situ NPD cell designs and discuss methods for the analysis of the corresponding in situ NPD data produced using this cell.

제자리 중성자 분말 회절에서 사용자 정의 - 만든 리튬 이온 배터리를 사용하여

Li-ion batteries are widely used in portable electronic devices and are considered as promising candidates for higher-energy applications such as electric ...

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.

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 ...

In Situ Visualization of the Phase Behavior of Oil Samples Under Refinery Process Conditions

To help address production issues in refineries caused by the fouling of process units and lines, we have developed a setup as well as a method to visualize the behavior of petroleum samples under process conditions. The experimental setup relies on a custom-built micro-reactor fitted with a sapphire window at the bottom, which is placed over the objective of an inverted microscope equipped with a cross-polarizer module. Using reflection microscopy enables the visualization of opaque samples, such as petroleum vacuum residues, or asphaltenes. The combination of the sapphire window from the micro-reactor with the cross-polarizer module of the microscope on the light path allows high-contrast imaging of isotropic and anisotropic media. While observations are carried out, the micro-reactor can be heated to the temperature range of cracking reactions (up to 450 &#176;C), can be subjected to H2 pressure relevant to hydroconversion reactions (up to 16 MPa), and can stir the sample by magnetic coupling. 
Observations are typically carried out by taking snapshots of the sample under cross-polarized light at regular time intervals. Image analyses may not only provide information on the temperature, pressure, and reactive conditions yielding phase separation, but may also give an estimate of the evolution of the chemical (absorption/reflection spectra) and physical (refractive index) properties of the sample before the onset of phase separation.

In Situ Visualization of the Phase Behavior of Oil Samples Under Refinery Process Conditions

This article describes a setup and method for the in situ visualization of oil samples under a variety of temperature and pressure conditions that aim to emulate refining and upgrading processes. It is primarily used for studying isotropic and anisotropic media involved in the fouling behavior of petroleum feeds.

정유 공정 조건에서 오일 샘플의 위상 행동 제자리 시각화에서

To help address production issues in refineries caused by the fouling of process units and lines, we have developed a setup as well as a method to ...

A Novel Biaxial Testing Apparatus for the Determination of Forming Limit under Hot Stamping Conditions

The hot stamping and cold die quenching process is increasingly used to form complex shaped structural components of sheet metals. Conventional experimental approaches, such as out-of-plane and in-plane tests, are not applicable to the determination of forming limits when heating and rapid cooling processes are introduced prior to forming for tests conducted under hot stamping conditions. A novel in-plane biaxial testing system was designed and used for the determination of forming limits of sheet metals at various strain paths, temperatures, and strain rates after heating and cooling processes in a resistance heating uniaxial testing machine. The core part of the biaxial testing system is a biaxial apparatus, which transfers a uniaxial force provided by the uniaxial testing machine to a biaxial force. One type of cruciform specimen was designed and verified for the formability test of aluminum alloy 6082 using the proposed biaxial testing system. The digital image correlation (DIC) system with a high-speed camera was used for taking strain measurements of a specimen during a deformation. The aim of proposing this biaxial testing system is to enable the forming limits of an alloy to be determined at various temperatures and strain rates under hot stamping conditions.

This protocol proposes a novel biaxial testing system used on a resistance heating uniaxial tensile test machine in order to determine the forming limit diagram (FLD) of sheet metals under hot stamping conditions.

The hot stamping and cold die quenching process is increasingly used to form complex shaped structural components of sheet metals. Conventional ...

Orientational Transition in a Liquid Crystal Triggered by the Thermodynamic Growth of Interfacial Wetting Sheets

In liquid crystal (LC) physical chemistry, molecules near the surface play a great role in controlling bulk orientation. Thus far, mainly to achieve desired molecular orientation states in LC displays, the "static" surface property of LCs, so-called surface anchoring, has been intensively studied. As a rule of thumb, once the initial orientation of LCs is "locked" by specific surface treatments, such as rubbing or treatment with a specific alignment layer, it hardly changes with temperature. Here, we present a system exhibiting an orientational transition upon temperature variation, which conflicts with the consensus. Right on the transition, the bulk LC molecules experience the orientational rotation, with 90&#176; between the planar (P) orientation at high temperatures and the vertical (V) orientation at low temperatures in the first-order transitional manner. We have tracked thermodynamic surface anchoring behavior by means of polarizing optical microscopy (POM), dielectric spectroscopy (DS), high-resolution differential scanning calorimetry (HR-DSC), and grazing incidence X-ray diffraction (GI-XRD) and reached a plausible physical explanation: that the transition is triggered by a growth of surface wetting sheets, which impose the V orientation locally against the P orientation in the bulk. This landscape would provide a general link explaining how the equilibrium bulk orientation is affected by surface-localized orientation in many LC systems. In our characterization, POM and DS are advantageous by offering information on the spatial distribution of the orientation of LC molecules. HR-DSC gives information about the precise thermodynamic information on transitions, which cannot be addressed by conventional DSC instruments due to limited resolution. GI-XRD provides information on surface-specific molecular orientation and short-range orderings. The goal of this paper is to present a protocol for preparing a sample that exhibits the transition and to demonstrate how the thermodynamic structural variation, both in the bulk and on surfaces, can be analyzed through the abovementioned methods.

Here, we present a protocol to trigger an orientational transition of a liquid crystal in response to temperature. Methodologies are described for preparing a sample in order to observe the transition and the detailed transitional evolution.

계면 습윤지의 열역학적 성장에 의해 촉발 된 액정의 방향 전환

In liquid crystal (LC) physical chemistry, molecules near the surface play a great role in controlling bulk orientation. Thus far, mainly to achieve ...

All-electronic Nanosecond-resolved Scanning Tunneling Microscopy: Facilitating the Investigation of Single Dopant Charge Dynamics

The miniaturization of semiconductor devices to scales where small numbers of dopants can control device properties requires the development of new techniques capable of characterizing their dynamics. Investigating single dopants requires sub-nanometer spatial resolution, which motivates the use of scanning tunneling microscopy (STM). However, conventional STM is limited to millisecond temporal resolution. Several methods have been developed to overcome this shortcoming, including all-electronic time-resolved STM, which is used in this study to examine dopant dynamics in silicon with nanosecond resolution. The methods presented here are widely accessible and allow for local measurement of a wide variety of dynamics at the atomic scale. A novel time-resolved scanning tunneling spectroscopy technique is presented and used to efficiently search for dynamics.

We demonstrate an all-electronic method to observe nanosecond-resolved charge dynamics of dopant atoms in silicon with a scanning tunneling microscope.

모든 전자 나노초 해결 주사 터널링 현미경: 촉진 단일 불순물 충전 역학 조사

The miniaturization of semiconductor devices to scales where small numbers of dopants can control device properties requires the development of new ...