Jenei Zsolt, Cynn Hyunchae, Visbeck Ken, Evans William J
Lawrence Livermore National Laboratory, Livermore, California 94551, USA.
Rev Sci Instrum. 2013 Sep;84(9):095114. doi: 10.1063/1.4821622.
We describe a reliable high performance resistive heating method developed for the membrane diamond anvil cell. This method generates homogenous high temperatures at high pressure in the whole sample for extended operation period. It relies on two mini coil heaters made of Pt-Rh alloy wire mounted around the diamond anvils and gasket, while temperature is monitored by two K-type thermocouples mounted near the sample. The sample, diamonds, and tungsten-carbide seats are thermally insulated from the piston and cylinder keeping the cell temperature below 750 K while the sample temperature is 1200 K. The cell with the heaters is placed in a vacuum oven to prevent oxidation and unnecessary heat loss. This assembly allows complete remote operation, ideally suited for experiments at synchrotron facilities. Capabilities of the setup are demonstrated for in situ Raman and synchrotron x-ray diffraction measurements. We show experimental measurements from isothermal compression at 900 K and 580 K to 100 GPa and 185 GPa, respectively, and quasi-isobaric compression at 95 GPa over 1000 K.
我们描述了一种为膜状金刚石对顶砧池开发的可靠的高性能电阻加热方法。该方法能在整个样品的高压环境下产生均匀的高温,并能持续较长的运行时间。它依靠两个由铂铑合金丝制成的微型线圈加热器,安装在金刚石砧座和垫片周围,同时通过安装在样品附近的两个K型热电偶监测温度。样品、金刚石和硬质合金座与活塞和气缸隔热,使得池体温度保持在750 K以下,而样品温度可达1200 K。装有加热器的池体放置在真空炉中,以防止氧化和不必要的热损失。这种装置允许完全远程操作,非常适合在同步加速器设施进行实验。该装置的功能通过原位拉曼和同步加速器X射线衍射测量得到了证明。我们展示了分别在900 K和580 K下等温压缩至100 GPa和185 GPa,以及在95 GPa下超过1000 K的准等压压缩的实验测量结果。