Heinen Benedict J, Drewitt James W E, Walter Michael J, Clapham Charles, Qin Fei, Kleppe Annette K, Lord Oliver T
School of Earth Sciences, University of Bristol, Wills Memorial Building, Queens Road, Bristol BS81RJ, United Kingdom.
Earth and Planets Laboratory, Carnegie Institution for Science, 5241 Broad Branch Road NW, Washington, DC 20015, USA.
Rev Sci Instrum. 2021 Jun 1;92(6):063904. doi: 10.1063/5.0038917.
High pressure-temperature experiments provide information on the phase diagrams and physical characteristics of matter at extreme conditions and offer a synthesis pathway for novel materials with useful properties. Experiments recreating the conditions of planetary interiors provide important constraints on the physical properties of constituent phases and are key to developing models of planetary processes and interpreting geophysical observations. The laser-heated diamond anvil cell (DAC) is currently the only technique capable of routinely accessing the Earth's lower-mantle geotherm for experiments on non-metallic samples, but large temperature uncertainties and poor temperature stability limit the accuracy of measured data and prohibits analyses requiring long acquisition times. We have developed a novel internal resistive heating (IRH) technique for the DAC and demonstrate stable heating of non-metallic samples up to 3000 K and 64 GPa, as confirmed by in situ synchrotron x-ray diffraction and simultaneous spectroradiometric temperature measurement. The temperature generated in our IRH-DAC can be precisely controlled and is extremely stable, with less than 20 K variation over several hours without any user intervention, resulting in temperature uncertainties an order of magnitude smaller than those in typical laser-heating experiments. Our IRH-DAC design, with its simple geometry, provides a new and highly accessible tool for investigating materials at extreme conditions. It is well suited for the rapid collection of high-resolution P-V-T data, precise demarcation of phase boundaries, and experiments requiring long acquisition times at high temperature. Our IRH technique is ideally placed to exploit the move toward coherent nano-focused x-ray beams at next-generation synchrotron sources.
高压-高温实验提供了有关极端条件下物质的相图和物理特性的信息,并为具有有用特性的新型材料提供了合成途径。重现行星内部条件的实验对组成相的物理性质提供了重要限制,是开发行星过程模型和解释地球物理观测结果的关键。激光加热金刚石对顶砧(DAC)是目前唯一能够常规获取地球下地幔地热以用于非金属样品实验的技术,但较大的温度不确定性和较差的温度稳定性限制了测量数据的准确性,并禁止了需要长时间采集的分析。我们为DAC开发了一种新型内部电阻加热(IRH)技术,并通过原位同步加速器X射线衍射和同步光谱辐射温度测量证实,该技术能将非金属样品稳定加热到3000 K和64 GPa。我们的IRH-DAC产生的温度可以精确控制且极其稳定,在无需任何用户干预的情况下,数小时内温度变化小于20 K,导致温度不确定性比典型激光加热实验小一个数量级。我们的IRH-DAC设计几何结构简单,为在极端条件下研究材料提供了一种新的、易于使用的工具。它非常适合快速收集高分辨率P-V-T数据、精确划分相界以及在高温下需要长时间采集的实验。我们的IRH技术非常适合利用下一代同步加速器光源向相干纳米聚焦X射线束的发展趋势。