Name: an externally-heated diamond anvil cell for synthesis and single-crystal elasticity determination of ice-vii at high pressure-temperature conditions
Uploaded: 2020-06-18T14:45:00
Description: Watch this Scientific Journal Video about An Externally-Heated Diamond Anvil Cell for Synthesis and Single-Crystal Elasticity Determination of Ice-VII at High Pressure-Temperature Conditions at JoVE.c

我们感谢王思恒、王琴霞、高静、刘英新对实验的帮助。这项研究使用了美国能源部（DOE）科学用户设施办公室根据合同第1号为能源部科学办公室运营的先进光子源（APS）的资源。DE-AC02-06CH11357。地球土壤科学（第13区）由NSF地球科学（EAR-1128799）和能源地球科学部（DE-FG02-94ER14466）支持。EHDAC的发展得到了外部加热的钻石铁锤细胞实验（EH-DANCE）项目的支持，该项目由国家自然科学基金委员会根据NSF合作协议EE-1606856向陈先生提供教育外展和基础设施发展（EOID）项目。十、赖昌星感谢中国地质大学（武汉）创业基金（第162301202618号）的支持。B. 陈感谢美国国家科学基金会（EAR-1555388）和 EAR-1829273的支持。 J.S. Zhang 感谢美国 NSF 的支持（EAR-1664471、EAR-1646527 和 EAR-1847707）。

1. 环形加热器制备
<ol><li>制造环形加热器底座<ol>
<li>利用基于设计的三元模型的丙烷基机，用计算机数控（CNC）铣床制造环形加热器底座。加热器的外径为 22.30 mm ，内径为 8.00 mm，厚度为 2.25 mm。将加热器底座在 1523 K 下烧结 20 小时。</li>
	</ol>
</li>
	<li>布线<ol>
<li>将 Pt 10 wt% Rh 线（直径：0.01 英寸）切割成 3 条等长导线（每根约 44 厘米）。</li>
		<li>小心地将每根 Pt/Rh 导线穿过加热器底座的孔，将...

<ol>
	<li>Shen, G., Mao, H. K., Hemley, R. J. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Laser-heated+diamond+anvil+cell+technique:+double-sided+heating+with+multimode+Nd:+YAG+laser.">Laser-heated diamond anvil cell technique: double-sided heating with multimode Nd: YAG laser.</a> Computer. 1, 2 (1996).</li><li>Zhang, J. S., Bass, J. D., Zhu, G. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Single-crystal+Brillouin+spectroscopy+with+CO2+laser+heating+and+variable+q.">Single-crystal Brillouin spectroscopy with CO2 laser heating and variable q.</a> Review of Scientific Instruments. 86 (6), 063905 (2015).</li><li>Benedetti, L. R., Loubeyre, P. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Temperature+gradients,+wavelength-dependent+emissivity,+and+accuracy+of+high+and+very-high+temperatures+measured+in+the+laser-heated+diamond+cell.">Temperature gradients, wavelength-dependent emissivity, and accuracy of high and very-high temperatures measured in the laser-heated diamond cell.</a> High Pressure Research. 24 (4), 423-445 (2004).</li><li>Goncharov, A. F., Crowhurst, J. C. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Pulsed+laser+Raman+spectroscopy+in+the+laser-heated+diamond+anvil+cell.">Pulsed laser Raman spectroscopy in the laser-heated diamond anvil cell.</a> Review of Scientific Instruments. 76 (6), 063905 (2005).</li><li>Meng, Y., Hrubiak, R., Rod, E., Boehler, R., Shen, G. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=New+developments+in+laser-heated+diamond+anvil+cell+with+in+situ+synchrotron+x-ray+diffraction+at+High+Pressure+Collaborative+Access+Team.">New developments in laser-heated diamond anvil cell with in situ synchrotron x-ray diffraction at High Pressure Collaborative Access Team.</a> Review of Scientific Instruments. 86 (7), 072201 (2015).</li><li>Prakapenka, V., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Advanced+flat+top+laser+heating+system+for+high+pressure+research+at+GSECARS:+application+to+the+melting+behavior+of+germanium.">Advanced flat top laser heating system for high pressure research at GSECARS: application to the melting behavior of germanium.</a> High Pressure Research. 28 (3), 225-235 (2008).</li><li>Du, Z., Miyagi, L., Amulele, G., Lee, K. K. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Efficient+graphite+ring+heater+suitable+for+diamond-anvil+cells+to+1300+K.">Efficient graphite ring heater suitable for diamond-anvil cells to 1300 K.</a> Review of Scientific Instruments. 84 (2), 024502 (2013).</li><li>Bassett, W. A., Shen, A., Bucknum, M., Chou, I. M. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=A+new+diamond+anvil+cell+for+hydrothermal+studies+to+2.5+GPa+and+from-+190+to+1200&#176;+C.">A new diamond anvil cell for hydrothermal studies to 2.5 GPa and from- 190 to 1200&#176; C.</a> Review of Scientific Instruments. 64 (8), 2340-2345 (1993).</li><li>Kantor, I., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=BX90:+A+new+diamond+anvil+cell+design+for+X-ray+diffraction+and+optical+measurements.">BX90: A new diamond anvil cell design for X-ray diffraction and optical measurements.</a> Review of Scientific Instruments. 83 (12), 125102 (2012).</li><li>Dubrovinsky, L., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Stability+of+ferropericlase+in+the+lower+mantle.">Stability of ferropericlase in the lower mantle.</a> Science. 289 (5478), 430-432 (2000).</li><li>Komabayashi, T., Hirose, K., Sata, N., Ohishi, Y., Dubrovinsky, L. S. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Phase+transition+in+CaSiO3+perovskite.">Phase transition in CaSiO3 perovskite.</a> Earth and Planetary Science Letters. 260 (3-4), 564-569 (2007).</li><li>Datchi, F., Loubeyre, P., LeToullec, R. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Extended+and+accurate+determination+of+the+melting+curves+of+argon,+helium,+ice+(H+2+O),+and+hydrogen+(H+2).">Extended and accurate determination of the melting curves of argon, helium, ice (H 2 O), and hydrogen (H 2).</a> Physical Review B. 61 (10), 6535 (2000).</li><li>Lai, X., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=The+high-pressure+anisotropic+thermoelastic+properties+of+a+potential+inner+core+carbon-bearing+phase,+Fe7C3,+by+single-crystal+X-ray+diffraction.">The high-pressure anisotropic thermoelastic properties of a potential inner core carbon-bearing phase, Fe7C3, by single-crystal X-ray diffraction.</a> American Mineralogist. 103 (10), 1568-1574 (2018).</li><li>Yang, J., Mao, Z., Lin, J. F., Prakapenka, V. B. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Single-crystal+elasticity+of+the+deep-mantle+magnesite+at+high+pressure+and+temperature.">Single-crystal elasticity of the deep-mantle magnesite at high pressure and temperature.</a> Earth and Planetary Science Letters. 392, 292-299 (2014).</li><li>Zhang, D., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=High+pressure+single+crystal+diffraction+at+PX^+2.">High pressure single crystal diffraction at PX^ 2.</a> Journal of Visualized Experiments. (119), e54660 (2017).</li><li>Sinogeikin, S., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Brillouin+spectrometer+interfaced+with+synchrotron+radiation+for+simultaneous+X-ray+density+and+acoustic+velocity+measurements.">Brillouin spectrometer interfaced with synchrotron radiation for simultaneous X-ray density and acoustic velocity measurements.</a> Review of Scientific Instruments. 77 (10), 103905 (2006).</li><li>Dubrovinskaia, N., Dubrovinsky, L. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Whole-cell+heater+for+the+diamond+anvil+cell.">Whole-cell heater for the diamond anvil cell.</a> Review of Scientific Instruments. 74 (7), 3433-3437 (2003).</li><li>Fan, D., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=A+simple+external+resistance+heating+diamond+anvil+cell+and+its+application+for+synchrotron+radiation+X-ray+diffraction.">A simple external resistance heating diamond anvil cell and its application for synchrotron radiation X-ray diffraction.</a> Review of Scientific Instruments. 81 (5), 053903 (2010).</li><li>Jenei, Z., Cynn, H., Visbeck, K., Evans, W. J. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=High-temperature+experiments+using+a+resistively+heated+high-pressure+membrane+diamond+anvil+cell.">High-temperature experiments using a resistively heated high-pressure membrane diamond anvil cell.</a> Review of Scientific Instruments. 84 (9), 095114 (2013).</li><li>Shinoda, K., Noguchi, N. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=An+induction+heating+diamond+anvil+cell+for+high+pressure+and+temperature+micro-Raman+spectroscopic+measurements.">An induction heating diamond anvil cell for high pressure and temperature micro-Raman spectroscopic measurements.</a> Review of Scientific Instruments. 79 (1), 015101 (2008).</li><li>Zha, C. S., Mao, H. -. k., Hemley, R. J., Duffy, T. S. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Recent+progress+in+high-pressure+Brillouin+scattering:+olivine+and+ice.">Recent progress in high-pressure Brillouin scattering: olivine and ice.</a> The Review of High Pressure Science and Technology. 7, 739-741 (1998).</li><li>Zhang, J. S., Hao, M., Ren, Z., Chen, B. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=The+extreme+acoustic+anisotropy+and+fast+sound+velocities+of+cubic+high-pressure+ice+polymorphs+at+Mbar+pressure.">The extreme acoustic anisotropy and fast sound velocities of cubic high-pressure ice polymorphs at Mbar pressure.</a> Applied Physics Letters. 114 (19), 191903 (2019).</li></ol>

在这项工作中，我们描述了为高压研究准备EHDAC的协议。电池组件包括微型加热器和热绝缘层和电气绝缘层。以前，有多种电阻式加热器的设计，用于不同类型的DAC或实验配置7，17，18，19，20。大多数加热器由个别调查人员加工或从行业购买，通常为其他目的设计。在普通机...

金刚石铁锤细胞（DAC）是高压研究的重要工具之一。结合基于同步加速器和传统的分析方法，它被广泛用于研究行星材料在多兆巴压力和宽温度范围内的特性。大多数行星内部都同时在高压和高温 （HPHT） 条件下。因此，在原位高压下对 DAC 中的压缩样品进行加热，以研究行星内部的物理和化学特性至关重要。研究行星材料的相变关系和热力学特性不仅需要高温，还有助于缓解压力梯度，促进相变和化学反应，加快扩散和再结晶。两种方法通常用于加热DAC中的样品：激光加热和内部/外部电阻加热方法。
激光加热DAC技术已应用于行星内部1、2的高压材料科学和矿物物理研究。虽然越来越多的实验室能够使用这项技术，但它通常需要大量开发和维护工作。激光加热技术已用于达到高达7000K3的温度。然而，在激光加热实验中，长期稳定加热和温度测量一直是一个长期存在的问题。激光加热期间的温度通常会波动，但可以通过热发射和激光功率之间的反馈耦合来降低。更具挑战性的是控制和确定不同激光吸光度多个相的装配温度。温度也有相当大的梯度和不确定性（数百K），虽然最近的技术开发努力已经用于缓解这个问题4，5，6。加热样品区的温度梯度有时可能进一步引入扩散、重新分割或部分熔化引起的化学异质性。此外，如果没有红外波长范围内灵敏度高的定制探测器，通常无法精确测量低于 1100 K 的温度。
EHDAC 使用垫片/座椅周围的电阻电线或铝箔加热整个样品室，使样品加热至 +900 K，而不具有保护性气氛（如 Ar/H2气体），在保护气氛为 7 的 +1300 K 中加热至+900K。在较高温度下，钻石的氧化和石墨化限制了可达到的最高温度。虽然温度范围与激光加热相比有限，但它在较长持续时间内提供更稳定的加热和更小的温度梯度8，非常适合与各种检测和诊断方法相结合，包括光学显微镜、X射线衍射（XRD）、拉曼光谱、布里卢因光谱和四边变换红外光谱9。因此，EHDAC已成为研究HHT条件下各种材料特性的有用工具，例如相位稳定性和过渡10、11、熔化曲线12、状态13的热方程和弹性14。
BX-90型DAC是新开发的活塞式DAC，最大孔径（最大90°），用于XRD和激光光谱测量9，具有安装微型电阻加热器的空间和开口。气缸侧的 U 形切口还提供空间来释放活塞和气缸侧之间由温度梯度引起的应力。因此，它最近被广泛用于粉末或单晶XRD和布里卢因测量与外部加热设置。在这项研究中，我们描述了制备EHDC的可重复和标准化协议，并演示了单晶XRD以及使用EHDAC在11.2GPa和300-500K下合成单晶冰VII的布里卢因光谱测量。

<table>
	<tbody>
		<tr>
			<td>Au</td>
			<td>N/A</td>
			<td>N/A</td>
			<td>for pressure calibration</td>
		</tr>
		<tr>
			<td>Deionized water</td>
			<td>Fisher Scientific</td>
			<td>7732-18-5</td>
			<td>for the starting material of ice-VII synthesis</td>
		</tr>
		<tr>
			<td>Diamond anvil cell</td>
			<td>SciStar, Beijing</td>
			<td>N/A</td>
			<td>for generating high pressure</td>
		</tr>
		<tr>
			<td>K-type thermocouple</td>
			<td>Omega</td>
			<td>L-0044K</td>
			<td>for measuring high temperature</td>
		</tr>
		<tr>
			<td>Mica</td>
			<td>Spruce Pine Mica Company</td>
			<td>N/A</td>
			<td>for electrical insulation</td>
		</tr>
		<tr>
			<td>Pt 10wt%Rh</td>
			<td>Alfa Aesar</td>
			<td>10065</td>
			<td>for heater</td>
		</tr>
		<tr>
			<td>Pyrophyllite</td>
			<td>McMaster-Carr</td>
			<td>8479K12</td>
			<td>for fabricating the heater base</td>
		</tr>
		<tr>
			<td>Re</td>
			<td>Sigma-Aldrich</td>
			<td>267317</td>
			<td>for the gasket of diamond anvil cell</td>
		</tr>
		<tr>
			<td>Resbond 919 Ceramic Adhesive</td>
			<td>Cotronics Corp</td>
			<td>Resbond 919-1</td>
			<td>for insulating heating wires and mounting diamonds on seats</td>
		</tr>
		<tr>
			<td>Ruby</td>
			<td>N/A</td>
			<td>N/A</td>
			<td>for pressure calibration</td>
		</tr>
		<tr>
			<td>Ultra-Temp 2300F ceramic tape</td>
			<td>McMaster Carr Supply</td>
			<td>390-23M</td>
			<td>for thermal insulation</td>
		</tr>
	</tbody>
</table>

an externally-heated diamond anvil cell for synthesis and single-crystal elasticity determination of ice-vii at high pressure-temperature conditions

外部加热的金刚石铁锤电池 （EHDAC） 可用于同时生成地球和行星内部中的高压和高温条件。在这里，我们描述了 EHDAC 组件和附件的设计和制造，包括环电阻加热器、热绝缘层和电气绝缘层、热电偶放置，以及使用这些部件准备 EHDAC 的实验方案。EHDAC 可用于在露天产生兆巴压力和高达 900 K 的温度，在保护性大气中可能升高至 ±1200 K（即 Ar 与 1% H2 混合）。与达到通常温度的激光加热方法相比，外部加热可以轻松实现，并在 ≤900 K 和更少的温度梯度下提供更稳定的温度。我们展示了EHDAC在单晶冰-VII合成中的应用，并研究了其单晶弹性特性，利用同步加速器基X射线衍射和布里卢因散射在高压高压条件下。

在这份报告中，我们使用制造的电阻式微型加热器和BX-90 DAC进行EHDAC实验（图1和图2）。图 1显示了环形加热器的加工和制造过程。加热器底座的标准尺寸为外径 22.30 mm，内径 8.00 mm，厚度 2.25 mm。可调整环形加热器的尺寸，以适应各种类型的座位和钻石。
我们在EHDAC中加热压缩的H2O样品，在6GPa高达850K?...

Watch this Scientific Journal Video about An Externally-Heated Diamond Anvil Cell for Synthesis and Single-Crystal Elasticity Determination of Ice-VII at High Pressure-Temperature Conditions at JoVE.c

An Externally-Heated Diamond Anvil Cell for Synthesis and Single-Crystal Elasticity Determination of Ice-VII at High Pressure-Temperature Conditions

本工作侧重于用于制备外部加热金刚石铁锤电池 （EHDAC） 以产生高压和高温 （HPHT） 条件的标准协议。EHDAC 用于研究极端条件下地球和行星内部的材料，这些材料也可用于固态物理和化学研究。

在高压-温度条件下用于冰-VII合成和单晶弹性的外热金刚石铁锤细胞

The externally-heated diamond anvil cell (EHDAC) can be used to generate simultaneously high-pressure and high-temperature conditions found in ...

外部加热的金刚石铁锤细胞可以同时产生高压和高温，以模拟我们和其他行星内部的条件。该技术的主要优点是，它可以与各种光谱技术相结合，如光学显微镜、X射线衍射、拉曼光谱学和布里卢因散射。这项技术用于研究岩石行星和月球的内部。它还可用于研究固态物理和化学极端条件下的材料特性。该协议最具挑战性的部分是将热对钻石的放置和夹具固定。执行这些步骤时，必须仔细遵循说明。该协议涉及许多操作步骤，因为演示至关重要，以便为观众提供足够的详细信息。首先将铂金线切割成三个相等的长度，每个长度约为 44 厘米。小心地将每根导线穿过加热器底座的孔，将加热器底座外约 10 厘米的导线与电源连接。确保导线低于底座的排水沟。如果它高于排水沟，请使用适当的平头螺丝刀向下按压。风更多的电线在10厘米的延长线，以减少电阻。使用两个小陶瓷绝缘套保护导线，延伸至环形加热器底座外。将水泥胶粘剂与水混合，比例为 100 比 13，并使用混合物将这些管子固定到环形加热器底座上。然后让水泥固化。用胶粘剂将一个云母环连接到加热器的每一侧，使导线电绝缘。使用安装夹具将钻石与背座对齐。然后用黑色环氧树脂将钻石粘在后排座椅上。黑色环氧树脂应低于钻石的腰带，为高温水泥留有空间。要对座椅和金刚石铁锤电池或 DAC 进行热绝缘，请将云母胶上或将云母环放在座椅下。将带钻石的座椅放入 BX90 DAC 中。在光学显微镜下对齐两颗钻石。将气垫片放在两颗钻石之间，轻轻拧紧 DAC 的四个螺钉，使垫片预缩至约 30 至 45 微米。使用放电机或激光微钻机在压痕中心钻孔。将两小块云母与水泥混合物放在 DAC 活塞侧的座椅上，使热组与座椅进行电气绝缘。将两个 K 型或 R 型热对贴到 DAC 的活塞侧，确保热型对触的金刚石靠近金刚石。然后，使用高温水泥混合物固定热对子位置，并覆盖 DAC 两侧的黑色环氧树脂。使用二氧化碳激光钻孔机切割 2300 华氏度的陶瓷胶带，形成加热器底座的形状，并把它放在 DAC 的两侧，必要时用粘合推杆固定。将加热器放在 BX90 DAC 的活塞侧，并使用一些陶瓷胶带来填补加热器和 DAC 壁之间的间隙。用针清洁垫片的样品室孔，清除钻孔引入的金属碎片。然后使用超声波清洁剂清洁垫片 5 至 10 分钟。在 DAC 活塞侧的金刚石周围放两个小球的胶粘剂，以支持垫片。然后在光学显微镜下对齐垫片的样品室孔，以匹配玻璃的中心。将一个或多个红宝石球和一块金块装入样品室。然后在样品室中装一滴蒸馏水。通过拧紧四个螺钉，关闭 DAC 并压缩 DAC。使用拉曼光谱仪测量红宝石球体的荧光，确定样品的压力。转动四个螺钉，小心地压缩样品。并监测压力，直到它到达冰七号的稳定性场。目标压力通常在 300 开尔文时在 2 到 10 千兆帕卡尔之间。将外部加热 DAC 置于光学显微镜下，将摄像机连接到计算机。使用显微镜级对 DAC 进行热绝缘，而不会阻塞显微镜的透射光路径。将热对连接到温度计，然后将加热器连接到直流电源。监测冰七晶的熔化，加热到高于高压冰七的熔化温度。淬火样品室，使液态水结晶。然后提高温度，直到一些较小的冰晶熔化。重复加热和冷却循环几次，直到样品室中仅保留一个或几个较大的颗粒。压缩水样品被加热到外部加热的DAC约6千兆帕卡，高达850开尔文，使一个单一的水晶冰VII。经过多次加热和冷却，合成了一个大的单晶。合成的单结晶VII用于在高压和高温下同步加速器X射线衍射和布里卢因光谱。确定了温度功率关系。晶体的晶格应力很小，压缩加热后保持了良好的质量。如基于同步加速器的单晶X射线衍射图像的尖锐布拉格衍射峰值所示。衍射模式可以使用立方结构进行索引。通过高压和高温布里鲁因散射测量，获得了声速和弹性模组。在尝试此协议时，热夫妻的放置非常重要。热夫妻应在座椅和 DAC 周围进行电气绝缘，并且应靠近钻石的铜孔。外加热金刚石铁锤电池通常与拉面、FTIR和众多同步辐射光谱方法（如 X 射线衍射）相结合，并结合高温条件下高压下材料的原位特性。对于那些熟悉金刚石铁锤细胞的人，这种技术可以很容易地学习，使性能不仅在高压，而且在高温测量在未来的研究。

Research

JoVE Journal

Chemistry

Rapid High Throughput Amylose Determination in Freeze Dried Potato Tuber Samples

快速高通量直链淀粉测定冻干马铃薯块茎样品

This protocol describes a high through put colorimetric method that relies on the formation of a complex between iodine and chains of glucose molecules in ...

科研

化学

Synthesis of Hypervalent Iodonium Alkynyl Triflates for the Application of Generating Cyanocarbenes

高价碘鎓炔基三氟甲磺酸酯的生成Cyanocarbenes的合成应用

The procedures described in this article involve the synthesis and isolation of hypervalent iodonium alkynyl triflates (HIATs) and their subsequent ...

Synthesis of Immunotargeted Magneto-plasmonic Nanoclusters

Immunotargeted的合成磁等离子团簇

Magnetic and plasmonic properties combined in a single nanoparticle provide a synergy that is advantageous in a number of biomedical applications ...

Synthesis, Characterization, and Functionalization of Hybrid Au/CdS and Au/ZnS Core/Shell Nanoparticles

合成，表征和混合金/硫化镉和Au / ZnS核/壳纳米颗粒功能化

Plasmonic nanoparticles are an attractive material for light harvesting applications due to their easily modified surface, high surface area and large ...

A Simple Method for the Size Controlled Synthesis of Stable Oligomeric Clusters of Gold Nanoparticles under Ambient Conditions

根据环境条件的金纳米粒子的稳定低聚簇的大小控制合成的一种简便方法

Reducing dilute aqueous HAuCl4 with sodium thiocyanate (NaSCN) under alkaline conditions produces 2 to 3 nm diameter nanoparticles. Stable grape-like ...

Protocol for the Synthesis of Ortho-trifluoromethoxylated Aniline Derivatives

Protocol for the Synthesis of Ortho-trifluoromethoxylated Aniline Derivatives

协议的合成<em&gt;邻</em&gt; -trifluoromethoxylated苯胺类化合物

Molecules bearing trifluoromethoxy (OCF3) group often show desired pharmacological and biological properties. However, facile synthesis of ...

Synthesis of a Water-soluble Metal&#8211;Organic Complex Array

Synthesis of a Water-soluble MetalÃƒÆ’Ã‚Â¢ÃƒÂ¢Ã¢â‚¬Å¡Ã‚Â¬ÃƒÂ¢Ã¢â€šÂ¬Ã…â€œOrganic Complex Array

一个水溶性金属 - 有机络合物阵列合成

We demonstrate a method for the synthesis of a water-soluble multimetallic peptidic array containing a predetermined sequence of metal centers such as ...

High Pressure Single Crystal Diffraction at PX^2

高压单晶衍射PX ^ 2

In this report we describe detailed procedures for carrying out single crystal X-ray diffraction experiments with a diamond anvil cell (DAC) at the ...

Synthesis of High Purity Nonsymmetric Dialkylphosphinic Acid Extractants

高纯度对称 Dialkylphosphinic 酸萃取的合成

We present the synthesis of (2,3-dimethylbutyl)(2,4,4&#39;-trimethylpentyl)phosphinic acid as an example to demonstrate a method for the synthesis of high ...