X-ray Scattering

The term X-ray Scattering encompasses a number of techniques. X-ray diffraction (XRD), Small (SAXS) and Wide (WAXS) angle X-ray scattering, and X-ray fluorescence (XRF) are three types of X-ray scattering measurements that MCL offers to characterize materials. The term XRD has traditionally been applied to well-ordered crystalline materials for determination of crystal structures, identification of phase composition, stress measurements, and preferred orientation and crystallinity determination, whereas the terms SAXS and WAXS have been applied to the characterization of non- or semi-crystalline materials. SAXS experiments can study electron density structures in materials on size scales greater than the electron density contrast due to atomic ordering observed in diffraction from crystalline materials and can provide information on size, shape, and distribution of electron density contrasted domains. Diffuse scattering to wide angles (WAXS) can study atomic structure in non-crystalline materials. X-ray fluorescence (XRF) is commonly used to identify the elemental composition of materials.

A variety of samples can be measured including bulk specimens, powders, thin films, liquids, gels, emulsions and more. In situ capabilities include the ability to work with wet or air sensitive specimens, at temperatures from -196 to 1600 C, in air, vacuum, or a variety of gases and at pressures up to 100 bar. These capabilities are summarized in the table below.

An image of a technical poster about the Characterization of Coatings and Thin Films by X-Ray Diffraction
XRD / SAXS-WAXS Technical Poster
Instrument Source Goniometer Optics Focus Mode Detector Applications
Malvern Panalytical Empyrean II Cu, Co, Mo 3-axis cradle micro-diffraction, para-focusing, BBHD line/point reflection GaliPIX and X'Celerator powder, bulk, metals, polymers, many others, sample changer, non-ambient (Anton Paar HTK1200N and 2000N)
Malvern Panalytical Empyrean III Cu theta-theta multi-core line or microbeam reflection PIXcel 3D powder, bulk, metals, polymers, many others, sample changer
Malvern Panalytical Empyrean IV Cu theta-theta multi-core line or microbeam reflection PIXcel 3D and 1Der powder, bulk, metals, polymers, many others, sample changer
Malvern Panalytical - MRD Cu, Cr 4-circle high resolution, para-focusing, focusing lens line/point reflection PIXcel 3D and Xe proportional bulk/thin films, Anton Paar DHS900 domed heating stage, in-plane, XRR, residual stress, pole figures
XENOCS Xeuss 2.0 SAXS/WAXS Cu none collimation scatterless slits - point focus transmission and GIXRD Dectris Pilatus 200K polymers, nanoparticles, nanocomposites, etc. Linkam HFSX350, CSS450 and MFS with Xenocs humidity control stage
Multiwire Laue W - white radiation 3-axis; Bond Barrel collimation point back-reflection multiwire area single crystal

In situ XRD
In situ XRD of a NiTi shape memory alloy showing a phase change from martentsitic to austenitic.
XRD Instrument (Radiation sources) Non-ambient Stage Temp. Range Environment Sample Size Limitations Angle Limitations
Emp 1 (Mo) Anton Paar HPC900 25 to 900 °C He, from 1 to 100 bar Alumina or Inconel cups: 10 mm diameter, 0.8 mm depth 0 to 160 ° 2θ
25 to 500 °C Air, Nitrogen, CO2, from 1 to 100 bar
Emp2 (Cu, Co, Mo, Ag) Anton Paar HTK1200N 25 to 1200 °C Vacuum (10^-4 mbar), air, inert gases max. 16 mm diameter 0 to 164 ° 2θ
Anton Paar HTK2000N 25 to 1600 °C Vacuum (10^-4 mbar), air, inert gases ~1cm^2 powder 4 to 164 ° 2θ
MRD (Cu, Cr) Anton Paar DHS900 25 to 900 °C Vacuum (10^-1 mbar), air, inert gases, nitrogen max. 25 mm diameter 0 to 166 ° 2θ
0 to 85 °ψ (psi)
0 to 360 ° φ (phi)
Xuess SAXS/WAXS (Cu) Linkam HFSX350 -196 to 350 °C vacuum Capillaries up to 1.7 mm diam. / bulk ~5 mm 0.0040 - 2.88 A-1
Linkam CSS450 -50 to 450 °C vacuum 30 mm 0.0040 - 2.88 A-1
Linkam MFS with Xenocs Humidity Control -196 to 350 °C compression and tensile force; relative humidity (in air only) from 10-90% for temperatures 25-60 °C varies widely with setup 0.0040 - 2.88 A-1
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