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X-ray diffraction or XRD is an analytical tool that utilizes X-rays to study ordered structures such as crystalline organic and inorganic samples, polycrystalline materials, proteins, carbohydrates, and drugs.
According to Bragg's law, when X-rays strike the sample positioned on a stage, the rays are  scattered by the electron clouds around the sample atoms. The  X-ray diffraction or scattering is caused by constructive interference of the X-ray waves that reflect off the internal...
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Benchmarking 3D-ΔPDF analysis using in-house X-ray sources.

Karl O R Juul1, Kristoffer A H Støckler1, Bo B Iversen1

  • 1Center for Integrated Materials Research, Department of Chemistry and iNANO, Aarhus University, Aarhus, DK-8000, Denmark.

Acta Crystallographica. Section A, Foundations and Advances
|May 19, 2025
PubMed
Summary

Modern in-house X-ray sources can analyze diffuse scattering and three-dimensional difference pair-distribution function (3D-ΔPDF) data, yielding conclusions similar to synchrotron data. However, subtle details may be obscured, requiring additional analysis for in-house datasets.

Keywords:
3D-ΔPDFcorrelated disorderdiffuse scatteringpair-distribution function

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Area of Science:

  • Crystallography and Materials Science
  • X-ray Diffraction Analysis
  • Condensed Matter Physics

Background:

  • Advances in detector technology have improved in-house X-ray diffractometer data quality.
  • Previous studies compared in-house and synchrotron data for electron density details using multipole models.
  • Synchrotron sources offer higher resolution for subtle electron density features in organic crystals.

Purpose of the Study:

  • To benchmark the quality of weak diffuse scattering and 3D-ΔPDF analysis using in-house X-ray sources against synchrotron data.
  • To evaluate the applicability of 3D-ΔPDF analysis for in-house X-ray sources on selected material systems.
  • To provide a general description of the 3D-ΔPDF analysis pipeline.

Main Methods:

  • Comparison of X-ray diffraction data quality from in-house sources and synchrotron radiation.
  • Application and analysis of three-dimensional difference pair-distribution function (3D-ΔPDF) on Cu1.95Se, Nb1-xCoSb, and InTe.
  • Detailed analysis of correlated disorder and structural features from both in-house and synchrotron datasets.

Main Results:

  • In-house 3D-ΔPDF analysis successfully determined the 2D superstructure in Cu1.95Se, comparable to synchrotron data, though requiring additional modeling arguments.
  • Vacancy ordering and lattice relaxation effects in Nb1-xCoSb were observable and assignable using in-house 3D-ΔPDF.
  • For InTe, some diffuse scattering features were visible with in-house data, but obscured details prevented full correlated disorder modeling due to weaker signal and higher temperature.

Conclusions:

  • Many conclusions from synchrotron data analysis are achievable with in-house X-ray sources for diffuse scattering and 3D-ΔPDF.
  • In-house data may require additional assumptions or postulates to fully interpret results, especially for complex disorder.
  • Subtle crystallographic details can be less interpretable in in-house data due to lower signal-to-noise ratios and limited scattering vector range.