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

Summary

This work focuses on the standard protocol for preparing the externally-heated diamond anvil cell (EHDAC) for generating high-pressure and high-temperature (HPHT) conditions. The EHDAC is employed to investigate materials in Earth and planetary interiors under extreme conditions, which can be also used in solid state physics and chemistry studies.

Abstract

The externally-heated diamond anvil cell (EHDAC) can be used to generate simultaneously high-pressure and high-temperature conditions found in Earth’s and planetary interiors. Here we describe the design and fabrication of the EHDAC assemblies and accessories, including ring resistive heaters, thermal and electrical insulating layers, thermocouple placement, as well as the experimental protocol for preparing the EHDAC using these parts. The EHDAC can be routinely used to generate megabar pressures and up to 900 K temperatures in open air, and potentially higher temperatures up to ~1200 K with a protective atmosphere (i.e., Ar mixed with 1% H₂). Compared with a laser-heating method for reaching temperatures typically >1100 K, external heating can be easily implemented and provide a more stable temperature at ≤900 K and less temperature gradients to the sample. We showcased the application of the EHDAC for synthesis of single crystal ice-VII and studied its single-crystal elastic properties using synchrotron-based X-ray diffraction and Brillouin scattering at simultaneously high-pressure high-temperature conditions.

Introduction

The diamond anvil cell (DAC) is one of the most important tools for high pressure research. Coupled with synchrotron-based and conventional analytical methods, it has been widely used to study properties of planetary materials up to multi-megabar pressures and at wide ranges of temperatures. Most planetary interiors are under both high-pressure and high-temperature (HPHT) conditions. It is thus essential to heat the compressed samples in a DAC at high pressures in situ to study the physics and chemistry of planetary interiors. High temperatures are not only required for the investigations of phase and melting relationships and thermodynamic properties of planetary mat....

Protocol

1. Ring heater preparation

1. Fabricating the ring heater base
   1. Fabricate the ring heater base by a computer numerical control (CNC) milling machine using pyrophyllite based on the designed 3D model. The dimensions of the heater are 22.30 mm in outer diameter (OD), 8.00 mm in inner diameter (ID) and 2.25 mm in thickness. Sinter the heater base in the furnace at 1523 K for >20 hours.
2. Wiring
   1. Cut Pt 10 wt% Rh wire (diameter: 0.01 inch) into 3 equal-length wires (about 44 cm each).
   2. Carefully wind each Pt/Rh wire through the holes in the heater base, leave about 10 cm wire outside of the heater base for....

Results

In this report, we used the fabricated resistive micro-heater and BX-90 DAC for the EHDAC experiment (Figure 1 and Figure 2). Figure 1 shows the machining and fabrication processes of the ring heaters. The standard dimensions of the heater base are 22.30 mm in outer diameter, 8.00 mm in inner diameter and 2.25 mm in thickness. The dimensions of the ring heater can be adjusted to accommodate various types of seats and diamonds.<.......

Discussion

In this work, we described the protocol of preparing the EHDAC for high pressure research. The cell assemblies including a micro-heater and thermal and electrical insulating layers. Previously, there are multiple designs of resistive heaters for different types of DACs or experimental configurations^{7,17,18,19,20}. Most of the heaters are machined by individual .......

Materials

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