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X-ray Crystallography

X-ray Crystallography

The size of the unit cell and the arrangement of atoms in a crystal may be determined from measurements of the diffraction of X-rays by the crystal, termed X-ray crystallography.
Diffraction
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$X-ray Diffraction of Biological Samples$ 01:10

X-ray Diffraction of Biological Samples

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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Related Experiment Video

Updated: Dec 14, 2025

$On-Chip Crystallization and Large-Scale Serial Diffraction at Room Temperature$

On-Chip Crystallization and Large-Scale Serial Diffraction at Room Temperature

Published on: March 11, 2022

X-ray diffraction using focused-ion-beam-prepared single crystals.

Tina Weigel¹, Claudia Funke¹, Matthias Zschornak¹

¹Institute of Experimental Physics, Technische Universität Bergakademie Freiberg, Leipziger Strasse 23, 09596 Freiberg, Germany.

Journal of Applied Crystallography

|July 21, 2020

Summary

This summary is machine-generated.

A new focused ion beam method creates precisely shaped lithium niobate (LiNbO3) single crystals for X-ray diffraction. This technique minimizes data ambiguities and improves the reliability of crystal structure and electron density analysis.

Keywords:

X-ray diffraction focused ion beams sample preparation

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Area of Science:

Crystallography
Materials Science
Solid State Physics

Background:

High-quality single crystals are crucial for accurate X-ray diffraction (XRD) data.
Crystal shape significantly impacts absorption corrections, especially for high-absorbing materials like lithium niobate (LiNbO3).
Existing preparation methods can introduce ambiguities and damage delicate samples.

Purpose of the Study:

To present and evaluate a focused ion beam (FIB) method for preparing regularly shaped single crystals.
To assess the impact of FIB preparation on XRD data quality and structural analysis.
To compare FIB-prepared crystals with those prepared using conventional methods.

Main Methods:

Utilized a focused ion beam (FIB) to precisely cut LiNbO3 single crystals.
Performed single-crystal X-ray diffraction (SCXRD) measurements using a laboratory diffractometer.
Compared data reduction, structure refinement, and electron density reconstruction for crystals prepared via different methods.

Main Results:

FIB preparation yielded reproducibly shaped LiNbO3 crystals with minimal splintering.
XRD data from FIB-prepared crystals showed reduced extinction effects compared to conventionally prepared ones.
Structure refinement and electron density reconstruction yielded qualitatively similar results across all preparation methods, but with enhanced reliability for FIB samples.

Conclusions:

Focused ion beam (FIB) milling is a highly effective, minimally invasive technique for preparing single crystals for XRD.
This method enhances the reliability of structural parameters and electron density maps, particularly for susceptible or complex materials.
FIB preparation is recommended for samples requiring precise shape control, minimal damage, or extraction from specific material regions.