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，安装和6H-SiC的大锥伯勒尔型砧的对齐<ol><li>修正了在安装工具活塞和XY板插入伯勒尔型砧的休息区。 </li><li>确保每个砧坐在稳稳的背板。 </li><li>采用环氧树脂，（ 例如 ，STYCAST 1266），胶砧均向自己的座位上。固化在室温下12小时，或65ºC在炉中2小时。 </li><li>为了有足够的铁砧对齐，用货币供应量M1止动螺钉对齐背板和监控两个砧的并行性。如果被发现的砧块是不平行的，除去环氧树脂和重新启动点1.2处。 </li></ol> 2垫片准备<ol><li>钻头1毫米的孔进入退火铜成为一个芯片（铜98瓦特％，为2％（重量），厚度为0.5mm）的黄铜导销。 </li><li>插入三个长5mm条直径为1毫米的非绝缘铜线插入孔中，这是沿着砧分布，以作为GUIDË引脚的铜要垫片。 </li><li>检查之间的导销和胞体正确接地。通常情况下，约0.1Ω的直流电阻是理想的。改善与少量的导电银的应用。 </li><li>广场上的莫桑石砧顶部的铜成为芯片和关闭的单元格。 </li><li>使用油压机，加压垫片约1/8底尖直径为最大化的工作稳定性。监控用千分尺卡尺压痕的实际厚度。 </li><li>钻适当的直径（底尖直径为½）在压痕中心的孔。 </li><li>中分两个通道进入预凹垫圈。信道应足够深以容纳微线圈的18微米的铜导线。 </li><li>硬化的炉中所制备的衬垫在617 K表示2至3小时。 </li></ol> 3，准备和微线圈的加载<ol><li>采用了一块1毫米铜线的d至馈通在活塞的螺纹它。固定铜线用环氧树脂和根据步骤1.3治愈它。 </li><li>选择锥子（见材料清单），其具有用于将微线圈的所需直径和固定它的一对可旋转的卡盘夹爪之间。 </li><li>胶（ 如与清漆从SCB，见材料清单）的18微米的铜导线的一端上的卡盘爪，同时保持，另一端与旋转的卡盘爪，使得导线被卷绕到锥子。 </li><li>当微线圈是所期望的几何形状，固定金属丝的另一端部上的胶为好。 </li><li>使用稀释的清漆通过在绕组的顶部施加少量固定线圈。 </li><li>使用铁氟龙胶带锥子小心地取出线圈。 </li><li>放置一些环氧树脂（见点1.3），无任何添加剂，在密封垫的频道。 </li><li>将微线圈的样品室内部并固定在引线进入通道。 </li><li>治愈的磐英根据Ÿ树脂步骤1.3。 </li><li>焊料的微线圈的热丝，另一个导销的一个引线。 </li><li>添加一些银导电浆料每个结顶。固化过程通常需要几分钟。 </li><li>用少量环氧树脂密封两个结。 </li><li>治疗根据步骤1.3环氧树脂。 </li><li>现在，检查该线圈的直流电阻的每一步之后。 </li><li>放置在微线圈的样品。要知道，任何不必要的身体接触可能会破坏线圈。 </li><li>加入精细研磨的红宝石粉末样品的压力校准。 </li><li>最后，水灾与适当的压力介质的样品室中。用石蜡油，以确保近静水条件下可达9 GPA。 </li><li>小心合上电池。 </li></ol> 4，应用和监控压力<ol><li>起初，稍微收紧货币供应M3六角沉头螺钉。 </li><li>对于加压固定在台钳细胞。现在，拧紧两个对立的螺丝配对。 </li><li>将加压的细胞在适当的细胞支架。 </li><li>调整单元的位置，以使激光束到达样品室。 </li><li>使用精细调节表聚焦红宝石粉末在激光束。 </li><li>显示器采用相应的光谱仪软件红宝石光致发光光谱。 </li><li>提取在从红宝石R1和R2线所观察到的光谱位移的样品腔的实际压力。 </li><li>平衡加压的细胞至少12小时NMR测量前。 </li></ol> 5，执行NMR实验<ol><li>安装压力盒上典型的核磁共振探头。制造一个机械车间相应的单元格持有人。 </li><li>焊接热丝到探针。检查细胞和探针之间的适当的电接触。 </li><li>现在，执行标准NMR实验。提请注意的事实是，微线圈是版y以所施加的射频功率敏感。 </li></ol>

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The authors have nothing to disclose.

一个新的，有前途的方法，以千兆帕斯卡的压力进行核磁共振被描述。这种方法开启了大门，各种各样的NMR实验，由于其出色的灵敏度和分辨率。然而，在该协议部分中所述的几个步骤是至关重​​要的实验的结果。特别是，在制备微线圈和其在所述Cu-成为垫圈固定是非常困难的，并且需要一定的经验。在下文中，一些重要的提示被给出，这将有助于该技术的第一次成功应用。 <p class="jove_conte...

由于在上个世纪初高静水压力凝聚态珀西·布里奇曼的标志性实验，高压物理学领域已经发展迅速1。大量的有趣的现象是已知的下几个GPA 2的压力下发生。此外，凝聚态系统的高压反应已经告诉我们很多关于他们的电子基态和激发态3,4。 不幸的是，技术的凝聚态的千兆帕斯卡压力的电子性质的研究并不多见，与X射线或直流电阻测量一路领先5。特别地，电子或核磁矩与电子自旋（ESR）或核磁共振（NMR）实验中，检测被绑定到几乎不可能在一个典型的高压砧座单元，其中一个需要从检索的信号来实现一个小v通过砧座和密封垫圈olume供奉。 几个小组已尝试通过使用复杂的安排，要解决这个问题，例如，两个分割线对射频（RF）线圈沿砧块6的侧面缠绕;单或双环流发针谐振器7,8; 。甚至分裂铼垫圈作为RF拾取线圈9， 见图1不幸的是，这些方法仍然从低信号对噪声比（SNR）遭遇，限制了实验应用到大- γ核如1 H 10。有兴趣的读者可以称作其它高压谐振电路实验11 - 15。 Pravica和Silvera 16报告后的核磁共振砧细胞与12.8 GPA，谁研究了邻对位氢转换的最高压力。 随着应用核磁共振极大的兴趣研究量子固体的性质，我们集团很感兴趣，有核磁共振可在高压下，也是如此。最后，在2009年它可以证实高灵敏度砧细胞NMR的确是可能的，如果谐振无线电频率（RF）微线圈是在高压腔包围的样品17直接放置。在这样的方法中，NMR灵敏度是由几个数量级的（主要是由于急剧增加填充的RF线圈的因子），其变得更加具有挑战性NMR实验可能的， 例如在粉末样品的提高，17 O NMR高温超导体在长达7 GPA 18。超导这些材料可以通过施加压力大大放大了，现在就可以按照这个过程与当地的电子探头，承诺根本的洞察管理流程。另一实例为核磁共振高压下的功率从出现什么是believ编为常规参考实验：为了测试引入新砧细胞核磁共振，最著名的材料中的一种测定 - 简单的铝金属。随着压力的增加，从人们所期望的自由电子系统的NMR位移的一个意想不到的偏差被发现。增加下压力的反复实验，也表明新的结果确实是可靠的。最后，与带结构的计算然后将其发现的结果是，铝的费米表面，而无法通过计算年前被检测到的拓扑过渡的表现形式，在计算能力低。的调查结果的环境条件推断表明，这种金属的使用几乎无处不在的特性是由这个特殊的电子状态的影响。 为了追求许多不同的应用的特殊设计的砧座单元（前细胞已经从Cavend进口ISH实验室改造核磁共振）已经制定出来。目前，所使用自制的底盘是能够使用对800微米的底尖刻6H-SiC的砧块到达压力高至25京帕。核磁共振实验，成功地进行了高达10.1 GPa时为止。这种新的细胞的NMR性能被证明是优良19。其主要成分是钛铝（6）-Vanadium（4）与超低间隙水平（等级23），提供约800屈服强度MPa 20。由于它的非磁特性（磁化率χ是约5ppm）它是用于在砧座单元机架的适当材料。引入细胞（ 见图2中的所有自制的压腔设计概述）的整体尺寸小到足以放入普通标准孔核磁共振磁体。最小的设计中，LAC-TM1，这是只有20毫米高和1​​7毫米的直径，也符合典型的小，冷孔磁铁（30毫米孔直径）。第lAC-TM2，这是最新的底盘作者设计，使用四个M4内六角沉头螺栓（做出来的相同的合金作为电池机箱）作为压力驱动机构，允许在内部压力的平稳控制（安装在蓝图补充部分）。 通常情况下，金刚石砧使用，以便产生上述为100GPa最高压力。许茂和21 - 23已经证明，莫桑石砧提供高压的研究具有成本效益的替代方案，高达约60 GPA的压力。因此，碳硅石砧块被用于引入GPA NMR方法。最好的结果是用自Charles＆科尔瓦德的砧座部定制大锥6H-SiC的砧块。与这些细胞中，压力达10.1 GPa时使用800微米的底尖刻砧被发现导致非常好的NMR灵敏度。为了进行比较，李等人报道的1 SNR核为1 H NM自来水中的R，而引入微线圈的方法的SNR显示出25的值对于其体积的七分之一，即使在稍微较低的磁场。 有了这项新措施，以高灵敏度压腔核磁共振可以追求的承诺令人兴奋的新洞察现代材料的物理和化学多种应用。然而，一如既往的灵敏度和分辨率最终限制NMR的应用，特别是，如果一个人的爱好有高得多的压力需要小型的底尖大小。然后，人们不仅以优化电池设计具有更小的RF线圈，而且还考虑增加核极化方法。

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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.

图3示出了如何在完全组装压力盒，布线和安装到一个典型的NMR探针样子。在下文中，几个实验进行审查，应使读者能够收集有关的优点和引入的技术的范围广泛的概述。 <img alt="图1" src="/files/ftp_upload/52243/52243fig1highres.jpg" /> 图1：不同的方法适用于高压核磁共振：（一）拆分对线圈围绕砧侧面，以及从Bertani 等?...

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.

高灵敏度核磁共振的千兆帕斯卡压力：一种新的工具，用于极端条件下探测电子和化工凝聚态的性质

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

SCIENTISTS IN ACTION

11.5K 次观看.  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.

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

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.

在极端的压力和温度的合成和Microdiffraction

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

科研

工程学

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.

火焰在实验的先进光源：全新洞察烟灰形成过程

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.

原位中子衍射用特制的锂离子电池

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.

至尊纳米线和其他维系统的共振拉曼光谱

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 ...

Use of a Multi-compartment Dynamic Single Enzyme Phantom for Studies of Hyperpolarized Magnetic Resonance Agents

Imaging of hyperpolarized substrates by magnetic resonance shows great clinical promise for assessment of critical biochemical processes in real time. Due to fundamental constraints imposed by the hyperpolarized state, exotic imaging and reconstruction techniques are commonly used. A practical system for characterization of dynamic, multi-spectral imaging methods is critically needed. Such a system must reproducibly recapitulate the relevant chemical dynamics of normal and pathological tissues. The most widely utilized substrate to date is hyperpolarized [1-13C]-pyruvate for assessment of cancer metabolism. We describe an enzyme-based phantom system that mediates the conversion of pyruvate to lactate. The reaction is initiated by injection of the hyperpolarized agent into multiple chambers within the phantom, each of which contains varying concentrations of reagents that control the reaction rate. Multiple compartments are necessary to ensure that imaging sequences faithfully capture the spatial and metabolic heterogeneity of tissue. This system will aid the development and validation of advanced imaging strategies by providing chemical dynamics that are not available from conventional phantoms, as well as control and reproducibility that is not possible in vivo.

A multi-compartment dynamic phantom is used to simulate some biology of interest for metabolic studies using hyperpolarized magnet resonance agents.

一个多腔动态单一酶幻影超极化磁共振剂研究的用途

Imaging of hyperpolarized substrates by magnetic resonance shows great clinical promise for assessment of critical biochemical processes in real time. Due ...

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.

在油样品的相行为在炼油工艺条件的原位可视化

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.

一种新型双轴试验设备的成形极限的下烫印条件的决定

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.

由界面润湿片的热力学生长触发的液晶中的定向转变

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.

全电子纳秒分辨扫描隧道显微镜: 促进单一掺杂剂电荷动力学的研究

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

Electric-field Control of Electronic States in WS2 Nanodevices by Electrolyte Gating

A method of carrier number control by electrolyte gating is demonstrated. We have obtained WS2 thin flakes with atomically flat surface via scotch tape method or individual WS2 nanotubes by dispersing the suspension of WS2 nanotubes. The selected samples have been fabricated into devices by the use of the electron beam lithography and electrolyte is put on the devices. We have characterized the electronic properties of the devices under applying the gate voltage. In the small gate voltage region, ions in the electrolyte are accumulated on the surface of the samples which leads to the large electric potential drop and resultant electrostatic carrier doping at the interface. Ambipolar transfer curve has been observed in this electrostatic doping region. When the gate voltage is further increased, we met another drastic increase of source-drain current which implies that ions are intercalated into layers of WS2 and electrochemical carrier doping is realized. In such electrochemical doping region, superconductivity has been observed. The focused technique provides a powerful strategy for achieving the electric-filed-induced quantum phase transition.

Electric-field Control of Electronic States in WS2 Nanodevices by Electrolyte Gating

Here, we present a protocol to control the carrier number in solids by using the electrolyte.

用电解质浇注法对 WS2纳米器件电子态的电场控制

A method of carrier number control by electrolyte gating is demonstrated. We have obtained WS2 thin flakes with atomically flat surface via scotch tape ...