Non-Ambient X-Ray Diffraction

Significance of the Topic

Non-ambient X-ray diffraction (XRD) offers critical insights into how materials behave under controlled temperature, atmosphere and pressure. By enabling in situ monitoring of structural changes, thermal expansions, phase transitions and reaction kinetics, these techniques support both fundamental research and industrial quality control across sectors such as catalysis, energy materials, pharmaceuticals and ceramics.

Objectives and Overview

This review outlines a comprehensive portfolio of sample stages developed by Anton Paar for non-ambient XRD. It covers solutions spanning cryogenic cooling to ultra-high-temperature heating, various atmosphere controls (vacuum, inert, oxidizing, reducing, reactive gases and humidity), and compatibility with reflection, transmission and four-circle geometries. The goal is to demonstrate how tailored sample environments advance real-time structural analysis.

Methodology and Instrumentation

Heating and cooling strategies are classified into:

• Radiation heating (HTK 1500, HTK 1200N, XRK 900): homogeneous heating up to 1 500 °C (HTK 1500) or 1 200 °C (HTK 1200N), sample spinning for random grain orientation, inert holders, reflection/transmission modes and capillary extensions for powders.
• Direct filament heating (HTK 16N, HTK 2000N, DHS 1100): temperatures up to 2 300 °C under vacuum or gas, optimized for four-circle goniometers (DHS 1100) with minimal thermal gradients and rapid temperature ramps.
• Heating and cooling (TTK 600, CHC plus+, DCS 500, BTS 150/500): broad range from ‑190 °C to +600 °C (TTK 600) and controlled relative humidity (CHC plus+), as well as domed cooling stages (DCS 500) and compact benchtop attachments (BTS 150/500).

Main Results and Discussion

Each stage delivers precise temperature measurement via integrated sensors (thermocouples, Pt100) positioned near the sample. Homogeneity is achieved through optimized heater geometry and sample rotation. Atmosphere control ranges from high vacuum (~10⁻⁴ mbar) to pressurized gas (up to 10 bar) and defined humidity (5 %–95 % RH). These capabilities enable detailed studies of lattice parameter determination, phase diagrams, chemical reactions (annealing, sintering, calcination), texture analysis, catalytic gas-solid processes and kinetic investigations.

Benefits and Practical Applications

Key advantages include:

• Real-time phase and structural monitoring under realistic operating conditions.
• Enhanced data quality via sample spinning and minimal orientation effects.
• Flexibility to test powders, thin films, bulk materials and electrochemical cells.
• Efficient workflow through fast temperature ramps and easy sample exchange.

Future Trends and Potential Applications

Emerging directions involve integration of non-ambient XRD with complementary spectroscopic and imaging techniques, automation and high-throughput screening, advanced pressure cells for super-critical environments and AI-driven data analysis. Expanding humidity-controlled studies and micro-focused beam adapters will further broaden application fields.

Conclusion

Anton Paar’s modular non-ambient XRD stages cover an unrivaled range of temperature, atmosphere and geometry options, empowering researchers and industry to gain deeper structural insights and optimize material performance under real-world conditions.