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. Montaj ve 6H-SiC Büyük Koni Boehler-tipi Anvils Hizalamalı <ol><li> Montaj araçları piston ve xy plaka düzeltmek ve oturma alanında Boehler-tipi anvils yerleştirin. </li><li> Tabii her örs sırt plakaları sıkıca oturur olun. </li><li> (Örneğin, Stycast 1266), kendi koltuk hem anvils tutkal, epoksi reçine kullanma. Oda sıcaklığında 12 saat ya da 2 saat boyunca bir fırın içinde 65 ° C &#39;için tedavi. </li><li> Yeterli bir örs uyum için, arka plakaları hizalayın ve hem de örsün paralelliği izlemek için M1 set vidaları kullanın. Örsler paralel olmayan olduğu bulunmuştur ise, epoksi reçinesi çıkarın ve yeniden başlatma alanına 1.2. </li></ol> 2. Conta Hazırlık <ol><li> Tavlı Cu-Be bir çip içine matkap, 1 mm delik pirinç kılavuz pinlerinin (w% Cu 98, ağırlıkça% 2, 0.5 mm kalınlığında olun). </li><li> GUID&#39;deki olarak hizmet etmek üzere, örs boyunca dağıtılmış olan delikler üç tane 5 mm ve çapı 1 mm olmayan izole edilmiş bakır telden uzun parçalar kaydedinCu-Be conta e pimleri. </li><li> Kılavuz pimleri ve hücre gövdesi arasında uygun topraklama için kontrol edin. Tipik haliyle, yaklaşık 0.1 Ω bir DC direnci arzu edilir. Iletken gümüş küçük bir miktarda bir uygulama ile geliştirin. </li><li> Moisanit örs üzerine Cu-Be çip yerleştirin ve hücre kapatın. </li><li> Bir hidrolik pres kullanarak, en üst düzeyde çalışma istikrar için culet çapının yaklaşık 1/8 inci conta basınç. Bir mikrometre kaliper kullanılarak girinti gerçek kalınlığının izleyin. </li><li> Girintinin merkezinde uygun çapın (culet çapının ½) bir delik delin. </li><li> Önceden girintili conta haline iki kanal bölmek. Kanallar mikro-bobinin 18 mikron bakır tel karşılamak için yeterince derin olmalı. </li><li> Harden fırında 2 saat 3 için 617 K&#39;de hazırlanmış conta. </li></ol> 3. hazırlanması ve Mikro-bobinin Yükleme <ol><li> 1 mm bakır tel an bölgesinin bir parça kullanınPistonun boydan boya besleme geçirmektir d. Epoksi reçine ile bakır tel Fix ve adım 1.3 göre bunu tedavi. </li><li> Mikro-coil için istenen çapa sahip bir bız (malzemelerin listesini görmek) seçin ve dönebilen ayna çeneleri bir çift arasında bunu düzeltmek. </li><li> Tutkal diğer ucunu tutarken, çeneleri üzerine 18 mikron bakır telin bir ucunu (SCB dan eg, vernik ile, malzemelerin listesini görmek) ve tel tığ üzerine sarılmış şekilde ayna çene döndürün. </li><li> Mikro bobin istenilen geometrinin olduğunda, hem de tutkal üzerine telin diğer ucunu sabitlemek. </li><li> Sargılarının üst kısmında küçük bir miktarın uygulanmasıyla bobini sabitlemek için seyreltilmiş vernik. </li><li> Teflon bant kullanarak tığ dikkatlice bobini çıkarın. </li><li> Contanın kanalları, herhangi bir katkı maddesi, bir epoksi reçinesi (noktası 1.3) yerleştirin. </li><li> Numune odasının içine mikro-coil yerleştirin ve kanallar içine uçlarını sabitleyin. </li><li> Epox Curey reçine göre 1.3 adıma. </li><li> Sıcak tel mikro bobini ve bir kılavuz pimi diğer bir kurşun lehim. </li><li> Her kavşak üstüne bazı gümüş iletken macun ekleyin. Tipik Kür birkaç dakika sürer. </li><li> Epoksi reçinenin küçük bir miktarı ile, her iki kavşaklar Seal. </li><li> 1.3 aşamasına göre epoksi Cure. </li><li> Şimdi, her adımdan sonra bobinin DC direnci kontrol edin. </li><li> Mikro bobinindeki numuneyi. Gereksiz fiziksel temas bobini yok olabileceğini unutmayın. </li><li> Basınç kalibrasyon için numuneye ince öğütülmüş yakut toz ekleyin. </li><li> Son olarak, uygun bir basınç ortam maddesi ile numune haznesi sel. 9 GPa kadar neredeyse-hidrostatik koşulları sağlamak için parafin yağı kullanın. </li><li> Dikkatli bir şekilde hücre kapatın. </li></ol> 4. Uygulama ve Basınç İzleme <ol><li> İlk başta biraz M3 Allen gömme vidayı sıkın. </li><li> Basınçlandırma için bir mengene hücreyi düzeltmek. Şimdi, sıkınİki karşıt vida ikili. </li><li> Bir hücre tutucuya basınçlı hücre yerleştirin. </li><li> Lazer ışını, numune odasına ulaşır, böylece hücrenin pozisyonunu ayarlar. </li><li> Lazer ışını yakut tozu odaklanmak için ince ayar tablosunu kullanın. </li><li> İlgili spektrometre yazılımını kullanarak yakut fotolüminesans spektrumunu izleyin. </li><li> Yakut R1 ve R2 hatlarının gözlenen tayf kayması örnek boşluğunda gerçek basıncı ayıklayın. </li><li> NMR ölçümleri çalıştırılmadan önce en az 12 saat boyunca basınçlı hücre dengelenmesi. </li></ol> 5. Sahne NMR Deneyleri <ol><li> Tipik NMR sonda üzerine basınç hücresi monte edin. Mekanik atölye uygun hücre taşıyıcıların imalatı. </li><li> Sondaya sıcak tel lehim. Hücre ve sonda arasında uygun elektrik teması kontrol edin. </li><li> Şimdi, standart NMR deneyleri gerçekleştirmek. Mikro-bobin ver olduğu gerçeğine dikkat çekmekuygulanan radyo frekansı gücüne karşı duyarlı y. </li></ol>

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The authors have nothing to disclose.

Giga-Pascal basınçlarında NMR gerçekleştirmek için, yeni ve umut verici bir yöntem tarif edilmiştir. Bu yöntem nedeniyle mükemmel hassasiyet ve çözünürlük NMR deneyleri geniş bir çeşitli kapı açılır. Bununla birlikte, protokol bölümünde açıklanan çeşitli adımlar deney sonucu için çok önemlidir. Özellikle, mikro-coil hazırlanması ve Cu-Be conta onun sabitleme çok zordur ve deneyim gerektirir. Aşağıda bununla ilgili bazı önemli ipuçları tekniğin bir birinci uygulama başarılı...

Geçen yüzyılın başında, yüksek hidrostatik basınç altında yoğunlaştırılmış madde Percy BRIDGMAN damgasını deneylerde bu yana, yüksek basınç fizik alanı hızla 1 gelişmiştir. Ilgi çekici fenomenlerin çok sayıda çeşitli GPa 2 basınçlar altında meydana geldiği bilinmektedir. Buna ek olarak, yüksek basınç yoğun madde sistemlerin yanıtı bize elektronik zemin ve uyarılmış hal 3,4 hakkında çok şey öğretti. Ne yazık ki, Giga-Pascal basınçlarında Yoğun madde elektronik özelliklerinin incelenmesi için teknikler x-ray ya da yolunu 5 önde gelen DC direnç ölçümleri ile nadirdir. Özellikle, elektron spin (ESR), ve nükleer manyetik rezonans (NMR) deneyleri, elektronik ya da nükleer Manyetik anlar üzerinde bir algılama gelen sinyali almak için gereken tipik bir yüksek basınçlı örs hücrelerde uygulanması neredeyse imkânsız olacağı kesindir küçük bir volume örs ve bir sızdırmaz contası tarafından konulan. Çeşitli gruplar, karmaşık düzenlemeler kullanarak bu sorunu çözmek için çalıştık, örneğin, iki bölünmüş çift radyo frekans (RF) bobinler örsün 6 yanları boyunca yara, bir tek veya çift döngü saç iğnesi rezonatörünü 7,8; . 1 gibi çekirdekler γ - ya da bir RF bobin tarafından 9, Şekil 1, bir çift olarak bölünmüş renyum conta Ne yazık ki, bu yaklaşım hala büyük için deneysel uygulamalar sınırlayan düşük bir sinyal-gürültü oranı (SNR) muzdarip H 10. 15 - İlgilenen okuyucu diğer yüksek basınçlı rezonans tank devresi deneyleri 11 ifade edilebilir. Pravica ve Silvera 16 rapor hidrojen orto-para dönüşüm incelenmiştir 12.8 GPa, NMR ile bir örs hücrede elde edilen en yüksek basınç. NMR uygulayarak büyük bir ilgi ilekuantum katıların özelliklerini incelemek için, bizim grup da yüksek basınçlar mevcut NMR olan ilgi oldu. Nihayet, 2009 yılında bir rezonansa radyo frekansı (RF) mikro-bobin örnek 17 çevreleyen yüksek basınç boşluğuna doğrudan yerleştirilir eğer yüksek hassasiyetli örs hücre NMR gerçekten mümkün olduğunu gösterdi olabilir. Bu tür bir yaklaşımda, NMR hassasiyeti, toz numuneleri üzerinde 17 A, NMR, örneğin daha da zor bir NMR deneyleri mümkün kılan, (RF bobini faktörü doldurulmasında çoğunlukla dramatik artışa bağlı olarak), birkaç büyüklük geliştirilir 7&#39;ye kadar 18 GPa yüksek-sıcaklık süper-iletken. Bu malzemeler içinde büyük ölçüde süper-iletkenlik basınç uygulanması ile amplifiye edilebilir ve bu süreçlere ilişkin temel fikir söz yerel elektronik sonda ile bu işlemi takip etmek mümkündür. Ne olduğunu, yüksek basınç altında NMR ve güç için bir başka örnek ortaya Believed rutin deneyler referans olması: - Basit alüminyum metal gelen yeni örs hücre NMR test etmek için, en iyi bilinen malzemelerin bir ölçülmüştür. Basınç arttıkça, tek bir serbest elektron sistemi için beklediğiniz gelen NMR kayması beklenmedik bir sapma tespit edildi. Daha yüksek basınç altında da, deney tekrarlandı, yeni sonuçlar gerçekten de güvenilir olduğunu göstermektedir. Işlem gücü düşük olduğunda Nihayet, bant yapısı hesaplamaları ile daha sonra, sonuçları yıl önce hesaplamalar tarafından tespit edilemeyen alüminyum Fermi yüzeyinin, bir topolojik geçiş tezahürü olduğu tespit edilmiştir. Ortam koşullarına bulguların ekstrapolasyonunda hemen hemen her yerde kullanılır bu metalin özellikleri bu özel elektronik durumun etkili olduğunu gösterdi. Farklı uygulamalar bir dizi takip etmek için özel olarak tasarlanmış örs hücreleri (önceki hücreleri Cavend ithal edilmiştiNMR sonradan ish Laboratuar ve) geliştirilmiştir. Şu anda, ikinci ev yapımı taşıyıcı 800 um culet 6H-SiC örsün çifti kullanılarak 25 GPa kadar basınç ulaşma kabiliyetine sahiptir. NMR deneyleri başarıyla bugüne kadar, 10.1 GPa kadar yapılmıştır. Bu yeni hücre NMR performansı 19 çok iyi olduğu gösterilmiştir. Ana bileşen Titanyum-Alüminyum (6) -vanadyum (4) yaklaşık 800 akma mukavemeti MPa 20 sağlayan bir ekstra düşük interstisyel düzeyde (sınıf 23), ile. Sayesinde manyetik olmayan özellikleri (manyetik duyarlılık χ yaklaşık 5 ppm) o örs hücre şasi için yeterli bir malzeme olduğundan. Tanıttı hücreler (tüm ev inşa örs hücre tasarımları bir bakış için bakınız Şekil 2) genel ölçüler normal standart delik NMR mıknatıslar içine sığacak kadar küçük. Yüksekliği sadece 20 mm ve 17 mm küçük tasarım, LAC-TM1, aynı zamanda tipik bir küçük kalibreli soğuk mıknatıslar (30 mm delik çapı) uyar. LYazarlar tasarlanmış en son şasi AC TM2, (iç basınç düzgün bir kontrolü için bağlanmış mavi baskı sağlayan basınç tahrik mekanizması olarak (ki bu hücre şasi ile aynı alaşımdan yapılmış) dört adet M4 Allen havşa civatalar kullanır ek bölüm). Tipik olarak, elmas örsler 100 GPa üzerinde en yüksek basınçlar oluşturmak için kullanılır. Xu Mao 21-23 moisanit örsler yaklaşık 60 GPa basınçlara kadar, yüksek basınçlı araştırma maliyetli bir alternatif temin olduğunu göstermiştir. Bu nedenle moisanit örsler katılan GPa NMR yaklaşım kullanılmıştır. En iyi sonuçlar Charles &amp; Colvard bir örs bölümünden özelleştirilmiş büyük koni 6H-SiC örs ile elde edilmiştir. Bu hücreler sayesinde, 10.1 GPa kadar basınçlar için 800 um culet örsün kullanımı çok iyi NMR duyarlılık ile sonuçlandığı bulunmuştur. Karşılaştırma için, Lee ve ark. 1H NM 1 bir SNR raporTanıtılan mikro bobin yaklaşımın SNR hatta biraz daha düşük manyetik alan, kendi hacminin 1/7 için 25 değerini gösterirken musluk suyu R,. Modern malzeme fiziği ve kimyası heyecan verici yeni bir bakış açısı söz birçok uygulama takip edebilirsiniz yüksek hassasiyetli örs hücre NMR birine bu yeni yaklaşım ile. Bir küçük culet boyutlarını talep çok daha yüksek basınçlar ilgilenen Ancak, her zaman olduğu gibi, hassasiyet ve çözünürlük sonuçta, özellikle, NMR uygulamasını sınırlamak. Sonra, bir daha küçük RF bobinleri ile hücre tasarımı optimize değil, aynı zamanda nükleer kutuplaşmayı arttırmak için yöntemler düşünmek sadece vardır.

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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.

Şekil 3, tipik bir NMR sonda üzerine tamamen monte edilmiş basınçlı hücre, kablo ve montaj gibi gösterir. Aşağıda, çeşitli deneyler faydaları ve tanıttı tekniğinin sınırları hakkında geniş bir bakış toplamak için okuyucunun hangi gözden geçirilecektir. <img alt="Şekil 1" src="/files/ftp_upload/52243/52243fig1highres.jpg" /> Şekil yüksek basınç NMR 1. Çeşitli Yaklaşımlar: örs kana...

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.

Aşırı Koşullarında Yoğun Madde Elektronik ve Kimyasal Özellikler Probing için Yeni Bir Aracı: Giga Pascal Baskılara yüksek-Hassasiyet Nükleer Manyetik Rezonans

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 Görüntüleme.  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.

Video: 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.

Katı Oksit Yakıt Hücreleri Elektrot Yüzeyler Sondalama ve Haritalama

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

Mühendislik

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.

Aşırı basınç ve Sıcaklıklarda sentezi ve mikrodifraksiyon

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 Düzlem Flow-Küçük Açı Nötron Saçılma kullanma Malzeme Mikroyapı altında Akış Ölçme

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.

İleri Işık Source Alev Deneyler: İs Oluşumu Süreçlerinin içine Yeni Trendleri

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.

Yerinde Nötron Toz Kırınım olarak Ismarlama Lityum-iyon Piller kullanma

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.

Aşırı Nanotel ve Diğer 1D Sistemleri Rezonans Raman Spektroskopisi

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.

Rafineri Süreci Koşullarında Petrol Örneklerinin Faz Davranışının Yerinde Görselleştirme

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.

Sıcak Baskı Koşullarında Şekillendirme Limit belirlemesi için yeni bir iki eksenli Test Aparatı

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.

Yüzey Islatma Levhalarının Termodinamik Büyümesi ile tetiklenen Sıvı Kristalde Oryantasyon Geçişi

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.

Tüm elektronik Nanosecond çözüldü tarama tünelleme mikroskobu: tek Dopant şarj Dynamics incelenmesi kolaylaştırılması

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