XRD laboratory analysis: characterization and expertise of crystalline materials

XRD stands for X-ray diffraction, a laboratory method used for the structural characterization of crystalline materials, including powders, alloys, ceramics, coatings, and pharmaceutical products.

XRD is an analytical technique used to study the crystal structure of materials. It reveals the nature of the phases, their proportions, atomic arrangement, and any transformations resulting from a manufacturing process or thermal or mechanical stress.

X-ray diffraction is based on the interaction between an X-ray beam and the atomic planes of a crystallized material. When the Bragg conditions are met, the X-rays diffract and generate characteristic peaks, which make it possible to identify the crystal structure and the phases present.

XRD analysis consists of recording a diffractogram and then interpreting the resulting peaks to identify and quantify the crystalline phases present. This involves comparing peak positions and intensities with crystallographic databases and, where necessary, performing a Rietveld refinement to obtain precise structural parameters.

Yes, through Rietveld refinement, XRD can determine the proportions of crystalline phases and their structural parameters, helping to monitor the effectiveness of a heat treatment, synthesis, or formulation process.

XRD identifies crystalline phases and can also estimate the proportion of amorphous material when combined with an appropriate quantification method or complementary analysis.

Combining XRD with analysis such as SEM-EDS, DSC, or FTIR provides a comprehensive view of the material: crystal structure, composition, morphology, thermal transitions, and chemical interactions.

Yes, XRD can be applied to powders, granules, alloys, ceramics, catalysts, and coatings, using configurations adapted to the nature and size of the sample.

XRD is used in targeted applications across several industries where crystal structure plays a decisive role.

• In metallurgy, it is used to identify the phases present in steels and alloys, monitor carbide formation, quantify retained austenite, and assess internal stresses after heat treatment.

• In the pharmaceutical industry, XRD is used to control the polymorphism of active ingredients, verify crystal stability throughout the formulation stages, and monitor amorphization caused by milling and granulation.

• For chemistry and inorganic materials, it is used to characterize mineral powders, catalysts, fillers, and pigments by determining their crystal composition and the possible presence of secondary phases.

• In the field of advanced materials, such as technical ceramics, partially crystallized glasses, and composites, XRD is used to validate the structure obtained during synthesis, control crystallinity, and detect phase transformations that may influence mechanical, thermal, or functional properties.

In metallurgy, XRD can detect the presence of retained austenite, carbides, or precipitates. For polymers, it evaluates the degree of crystallinity and phase transitions, which are key factors in mechanical performance, thermal resistance, and dimensional stability.

XRD can be used to verify polymorphism, identify unexpected crystalline forms, monitor amorphization levels after milling or granulation, and ensure the structural conformity of APIs and excipients.

In the event of fracture, corrosion, or deformation, XRD helps detect the emergence of new phases, metallurgical transformations, or internal stresses resulting from poorly controlled heat treatment.

XRD is relevant for verifying the conformity of a raw material batch, validating the formation of an expected crystalline phase, or detecting unwanted phases that could impair material performance.

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