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Powder Diffraction Laboratory

Description

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The powder diffraction laboratory aims at the analysis of polycrystalline samples (powders and bulk), at room temperature, with the high resolution powder diffractometer, as well as at high temperature (up to 1600 °C). We also perform analysis for industries, various laboratories for quality check and for environmental evaluations.

It is possible to ask for qualitative, quantitative analyses, but also just for data collection.

Contacts

Equipment

  • Philips X’pert MPD with high temperature chamber 
  • High resolution X-ray powder diffractometer Panalytical X’pert Pro

Equipment

Main specifications

It's a theta/theta diffractometer, with a double detector system: a proportional counter and a position sensitive detector are present. The diffractometer is equipped with a high-temperature chamber (AHT-PAP 1600), with a maximum temperature of 1600°C. 
The diffractometer is fully computer-integrated, with incident and anti-scatter opticsc ompletely programmable. The two detectors can be used for different purposes: for structural analyses the former, and for fast reaction kinetics the latter.  
The AHT hot chamber is equipped with a stepper motor, that moves the sample downwards as a function of the thermal expansion of the sample holder, in order to keep the sample in the ideal diffraction position. The sample, at the same time, can be spinned for a better counting statistics and temperature uniformity. Temperature oscillations inside the chamber are never bigger than 1°C, even at the highest attainable temperature (1600°C), and for temperatures lower than 1200°C are within 0.2°. The data quality is therefore particularly good, and data collected with this instrument can be used for structure refinement at high temperature.

Main specifications

It’s a high-resolution powder diffractomer, equipped with an incident beam monochromator, that separates the Ka1 and the Ka2, allowing the measurements to be performed with the Ka1 only. 
The diffractometer can work with the usual Bragg Brentano geometry (divergent beam) as well as with a parallel beam geometry. The latter allows the use of rough samples, of samples not perfectly positioned on the goniometer circle, and has a particularly good signal-to-noise ratio. The detector X’Celerator completes the instrument, allowing very fast data collection (for a qualitative analysis the data collection time is of the order of minutes), together with an excellent signal-to-noise ratio.
A 15 positions sample changer is also mounted on the instrument.

Research activities

High resolution powder diffraction, qualitative and quantitative analyses, 
structural refinements with the Rietveld method, in-situ high temperature experiments

Location

Via Botticelli 23 - 20133 Milano