X-Ray Diffraction (XRD)

X-ray diffraction (XRD) relies on the dual wave/particle nature of X-rays to obtain information about the structure of crystalline materials. A primary use of the technique is the identification and characterization of compounds based on their diffraction pattern.

The dominant effect that occurs when an incident beam of monochromatic X-rays interacts with a target material is scattering of those X-rays from atoms within the target material. In materials with regular structure (i.e. crystalline), the scattered X-rays undergo constructive and destructive interference. This is the process of diffraction. The diffraction of X-rays by crystals is described by Bragg’s Law, n(lambda) = 2d sin(theta). The directions of possible diffractions depend on the size and shape of the unit cell of the material. The intensities of the diffracted waves depend on the kind and arrangement of atoms in the crystal structure. However, most materials are not single crystals, but are composed of many tiny crystallites in all possible orientations called a polycrystalline aggregate or powder. When a powder with randomly oriented crystallites is placed in an X-ray beam, the beam will see all possible interatomic planes. If the experimental angle is systematically changed, all possible diffraction peaks from the powder will be detected.

The parafocusing (or Bragg-Brentano) diffractometer is the most common geometry for diffraction instruments.

This geometry offers the advantages of high resolution and high beam intensity analysis at the cost of very precise alignment requirements and carefully prepared samples. Additionally, this geometry requires that the source-to-sample distance be constant and equal to the sample-to-detector distance. Alignment errors often lead to difficulties in phase identification and improper quantification. A mis-positioned sample can lead to unacceptable specimen displacement errors. Sample flatness, roughness, and positioning constraints preclude in-line sample measurement. Additionally, traditional XRD systems are often based on bulky equipment with high power requirements as well as employing high powered X-ray sources to increase X-ray flux on the sample, therefore increasing the detected diffraction signals from the sample. These sources also have large excitation areas, which are often disadvantageous for the diffraction analysis of small samples or small sample features.

Polycapillary X-ray optics can be used to overcome many of these drawbacks and constraints to enhance XRD applications. Polycapillary collimating optics convert a highly divergent beam into a quasi-parallel beam with low divergence. They can be used to form a Parallel Beam XRD instrument geometry which greatly reduces and removes many sources of errors in peak position and intensity inherent to the parafocusing geometry, such as sample position, shape, roughness, flatness, and transparency. Polycapillary focusing optics collect X-rays from a divergent X-ray source and direct them to a small focused beam at the sample surface with diameters as small as tens of micrometers for micro X-ray diffraction applications of small samples or small specimen features. Both types of polycapillary optics direct very high X-ray intensities to the sample surface, such that XRD systems employing optics can use low power X-ray sources, reducing instrument size, cost, and power requirements.

X-ray diffraction using X-ray optics has been applied to many different types of applications including thin film analysis, sample texture evaluation, monitoring of crystalline phase and structure, and investigation of sample stress and strain.