X-ray diffraction and fluorescence analysis at TU Delft

General Information

X-RAY FACILITIES at the department of Materials Science & Engineering, Delft University of Technology, Netherlands

Department of Materials Science and Engineering, Rooms 34J-1-420/070, Mekelweg 2, Delft; tel (+31 15-27)89459/82243

Dr. Amarante Böttger (A.J.Bottger@tudelft.nl),

Richard Huizenga (R.M.Huizenga@tudelft.nl),

Ruud Hendrikx (R.W.A.Hendrikx@tudelft.nl),

The X-ray facilities are available for TU Delft students and staff.

Main application:

X-ray diffraction is a versatile, non-destructive technique that can be used to investigate the structure of materials. X-ray diffraction patterns can be used to determine the crystal structure and crystalline compounds present in a sample. More advanced applications are (1) the determination of texture or crystallite orientations, (2) the analysis of the state of stress through measuring the lattice-spacing changes caused by external or internal forces and (3) estimating the crystallite size and dislocation densities by full diffraction profile analysis.

X-ray fluorescence (XRF) is the emission of characteristic "secondary" (or fluorescent) X-rays from a material that has been excited by bombarding with high-energy X-rays. The phenomenon is used for elemental analysis of solids, powders or liquids.

Instrument specification

1. D8-Discover diffractometer system with Eulerian cradle and diffracted beam monochromator.

The tilt and rotation angles of the Eulerian cradle in combination with the parallel beam geometry, obtained by a poly-capillary optics, makes this system especially suited for crystallographic texture and stress determination. The sample stage includes computer controlled X, Y and Z movements. The X-ray wavelength is 0.179 nm (Co Kα).

2. D8- Advance theta/2theta vertically mounted diffractometer system with Vantec position sensitive detector and diffracted beam monochromator.

Due to the high counting efficiency of the Vantec position sensitive detector, short measurement times are possible. The home-made diffracted beam monochromator diminishes the contribution of fluorescence radiation. The X-ray wavelength is 0.179 nm (Co Kα), making this diffractometer especially suited for iron samples.

3. D8- Advance theta/theta vertically mounted diffractometer system with Lynxeye position sensitive detector.

Due to the high counting efficiency of the Lynxeye position sensitive detector, short measurement times are possible. This instrument has an excellent angular resolution combined with a high counting efficiency; ideal for phase identification as well as for detailed analysis of the diffraction maxima. It is equipped with a 90 positions sample changer. In this instrument, the sample stage remains in a fixed horizontal position during scanning. The X-ray wavelength is 0.154 nm (Cu Kα).

4. D8 theta/theta vertically mounted diffractometer system with Anton-Paar XRK900 reaction chamber and Lynxeye XE-T position sensitive detector

Also in this instrument, the sample stage remains in a fixed horizontal position during scanning. A temperature chamber is mounted that makes it possible to measure in the range from room temperature up to 900 ^oC in various atmospheres. The X-ray wavelength is 0.154 nm (Cu Kα).

5. D8-Discover theta/theta vertically mounted diffractometer with a 2D Eiger2 detector.

This equipment combines a high-brightness micro-focus X-ray source with a 2D detector, enabling fast in-situ texture and stress measurements. Beam size ranges from 1 to 0.1 mm diameter allowing local analysis; X,Y-scanning over a larger area of (100x100 mm) is possible. The sample stage allows dedicated appliances like high-temperature chamber or tensile device and large objects with a maximum weight of 5 kg to be mounted.

Useful information

The diffractometers are manufactured by Bruker-AXS. They can be equipped with various attachments for special applications. Special sample holders and sample preparation methods are available. A tensile device for in-situ stress measurements can be mounted.

The irradiated area on the specimen is usually about 10 x 15 mm2, but can be made as small as 1 x 1 mm2. The effective penetration depth depends on the material and the wavelength used and falls in the range of 2 - 20 μm.

Specimen requirements:

For powder material, the minimum amount needed to make a specimen is about 10 mg.

Specimens made from bulk materials should fit within a circle of 50 mm diameter and should not be thicker than 10 mm; the surface should be as flat as possible.

5. PANalytical Axios ^Max sequential wavelength dispersive X-ray Fluorescence Spectrometer.

(Semi)-quantitative multi-element analysis (F-U) of metals, minerals, soils, ceramics, glass etc.

Data evaluation is done with SuperQ and Omnian software.

Specimen requirements:

Solid samples should be flat and fit into a 50 mm diameter sample holder. Dry powders are pressed into pellets, minimum amount ca. 2 grams.

Opening hours:

Mondays-Fridays:8:00-17:00