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High Temperature XRD Phase Transformation Analysis
Requirement
As part of the PRISM research programme, there was a need to develop advanced analytical capability for studying phase transformations at elevated temperatures.
Many industrial and academic clients required in-situ XRD analysis from room temperature up to 1600°C to understand how materials such as ceramics, slags, and alloys change structure under thermal conditions.
The existing platinum (Pt) hot stage was limited by deformation and eutectic Pt-Si formation at high temperatures, making reliable analysis above 1400°C difficult. A more stable and durable solution was therefore required.
Solution
A new tantalum (Ta)-based hot stage was developed at the Materials Processing Institute within the Characterisation & Analysis Department.
The original platinum strip with a melting point of 1768°C was replaced with a tantalum strip with a significantly higher melting point of 3017°C, ensuring excellent thermal stability at high temperatures.
An annealed tantalum foil was added to protect the strip from contamination and to reduce maintenance.
Samples were milled to 120µm and compacted into 1mm pellets under a 7-tonne press to prevent movement or deformation under vacuum during heating.
The hot stage was programmed with heating rates between 5°C and 50°C per minute, allowing controlled temperature ramps and hold points (e.g., 1100°C, 1200°C) for phase analysis before cooling to room temperature.
Outcome
The new tantalum-based hot stage enabled accurate and repeatable XRD measurements up to 1600°C, allowing precise monitoring of phase transformations during heating and cooling.
Sample integrity was maintained throughout the process, and results showed clear, well-defined changes in crystalline phases at elevated temperatures.
This development met the requirements of the PRISM Programme and has significantly expanded the Materials Processing Institute’s capability to support clients with advanced high-temperature materials characterisation.
Prism
PRISM is a Programme of Research and Innovation for the UK Steel and Metals sectors to support innovation in:
- Decarbonisation
- Digital technologies
- Circular economy
The programme is being delivered by the Materials Processing Institute with funding from Innovate UK, part of UK Research and Innovation.
Advanced Materials Characterisation Centre
The Advanced Materials Characterisation Centre is an international centre for steel and metals characterisation and investigation, including failure analysis and forensic analysis, along with research, development and innovation.
More about our Advanced Materials Characterisation Centre
For advice and support contact us at enquiries@mpiuk.com
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