X-ray diffraction platform

X-ray Diffraction (XRD) is a powerful non-destructive technique for characterizing crystalline materials in many different solid materials (organic, inorganic, and metallorganic). While most other analytical techniques provide elemental or molecular information from a sample, XRD is unique in providing a wide range of information on structures, crystalline phases, lattice parameters preferred crystal orientations, and other structural parameters such as, particle size, strain, stress, and crystal defects. The ICN2 x-ray diffraction facility is dedicated to support the research activities of ICN2 groups, the surrounding research community or private companies. The facility has the suitable equipment and knowledge for dealing with nanopowders and thin films materials. Samples usually come from the fields of Chemistry, Physics, and Material Science. The XRD facility is equipped with two versatile and advanced Malvern PANalytical diffractometers: a Multipurpose Diffractometer (MPD) for powder materials and a Materials Research Diffractometer (MRD) for thin films. The instruments allow to perform routinary powder analysis and phase identification, to more sophisticated measurements, including grazing angle diffraction, X-ray reflectometry, diffuse scattering studies in nanopowders (SAXS), high-resolution analysis and reciprocal space mapping in epitaxial films, in-plane diffraction, as well as diffraction under non-ambient conditions (High temperature and controlled atmosphere).

Facility

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Malvern PANalytical X’pert Pro MPD

The MPD (Materials Powder Diffractometer) is suitable for the analysis of polycrystalline samples at room temperature. This diffractometer has a vertical theta-theta goniometer (240 mm radius), where the sample stage is fixed and does not rotate around omega axis as in ω-2θ diffractometers.

Malvern PANalytical X’pert Pro MPD - Bragg-Brentano Geometry

The main powder analysis applications for the Bragg-Brentano Geometry are:

  • Identification of crystalline phases in organic and inorganic compounds.

  • Quantitative phase analysis in organic and inorganic compounds.

  • Particle size determination.

  • Crystal structure determination performing Rietveld refinements.

Malvern PANalytical X’pert Pro MPD - Transmission Geometry - Vertical Configuration

Available capillaries in the facility are (Diameter): 0.3mm, 0.5mm, 0.7mm. Material: Borosilicate

Advantages of transmission-mode powder diffraction

Transmission geometry requires samples that are sufficiently transparent for the type of X-rays used. The incident X-ray beam fully penetrates, and is transmitted through, the sample with only moderate attenuation.

The advantages of transmission geometry in powder diffraction are detailed:

  • Generally, transmission mode is good for low density samples or weakly absorbing materials; i.e. pharmaceutical substances, proteins, synthetic polymers (foils and fibers) and other organic materials.

  • Small amounts of sample are sufficient. We can transfer the sample into a thin capillary or in horizontal sample holders in our setup.

  • Fluids; i.e. liquid dispersions can be measured.

  • Air-sensitive samples can be sealed in a capillary or between kapton foils.

  • Reduction of the preferred orientation effects in powder samples.

  • To obtain accurate Rietveld refinements. Using this geometry the data resolution is increased due to much quantity of sample is illuminated by X-rays and as a consequence it enhances statistics.

Malvern PANalytical X’pert Pro MPD - Transmission Geometry - Capillary Configuration

Available capillaries in the facility are (Diameter): 0.3mm, 0.5mm, 0.7mm. Material: Borosilicate

Advantages of transmission-mode powder diffraction

Transmission geometry requires samples that are sufficiently transparent for the type of X-rays used. The incident X-ray beam fully penetrates, and is transmitted through, the sample with only moderate attenuation.

The advantages of transmission geometry in powder diffraction are detailed:

  • Generally, transmission mode is good for low density samples or weakly absorbing materials; i.e. pharmaceutical substances, proteins, synthetic polymers (foils and fibers) and other organic materials.

  • Small amounts of sample are sufficient. We can transfer the sample into a thin capillary or in horizontal sample holders in our setup.

  • Fluids; i.e. liquid dispersions can be measured.

  • Air-sensitive samples can be sealed in a capillary or between kapton foils.

  • Reduction of the preferred orientation effects in powder samples.

  • To obtain accurate Rietveld refinements. Using this geometry the data resolution is increased due to much quantity of sample is illuminated by X-rays and as a consequence it enhances statistics.

Malvern PANalytical X’pert Pro MRD

The MRD (Materials Research Diffractometer) is suitable for the structural characterization in thin-films materials at room and high temperature. This diffractometer has a horizontal ω-2θ goniometer (320 mm radius) in a four-circle geometry and it works with a ceramic X-ray tube with Cu Kα anode (λ=1.540 Å). This diffractometer is equipped with different incident and diffracted optics which can be interchanged depending on the application required (i.e. a parabolic mirror, a hybrid monochromator, a Ge(440) four-crystal monochromator, a parallel plate collimator, and a polycapillary lens).

Malvern PANalytical X’pert Pro MPD - SAXS Geometry

Advantages of SAXS measurements

This technique allows sensitive measurements of the X-rays that are just barely scattered by the sample (scattering angle < 6°) using a transmission geometry. The length scale of d(Å) is inversely proportional to the scattering angle, therefore, small angles represent larger features in the samples.

This angular range contains information about the shape and size of nanoparticles and porous materials, characteristic distances of partially ordered materials, and pore sizes distributions. SAXS is capable of delivering structural information of macromolecules between 5 and 25 nm, of repeated distances in partially ordered systems of up to 150 nm.

Applications

The most common applications for these measurements are:

  • Nanoparticle size distribution

  • Particle shape

  • Specific surface area

  • Pore size distribution

Malvern PANalytical X’pert Pro MRD - Equipment

The MRD (Materials Research Diffractometer) is suitable for the structural characterization in thin-films materials at room and high temperature. This diffractometer has a horizontal ω-2θ goniometer (320 mm radius) in a four-circle geometry and it works with a ceramic X-ray tube with Κα anode (λ=1.540 Å). This diffractometer is equipped with different incident and diffracted optics which can be interchanged depending on the application required (i.e. a parabolic mirror, a hybrid monochromator, a Ge(440) four-crystal monochromator, a parallel plate collimator, and a polycapillary lens). The detector used is a PIXcel which is a fast X-ray detector based on Medipix2 technology with a 256x256 pixels array.

Provisional Contacts

Jessica Padilla Pantoja | X-Ray Diffraction Facilities Research Technician |  jessica.padilla@icn2.cat  | 937 372 638 |  ORCID 

Jessica Padilla Pantoja |  jessica.padilla@icn2.cat  | 937 372 638 |  ORCID 

Gustavo Ceballos | Head of Research Support Division - Instrumentation Unit |  gustavo.ceballos@icn2.cat  |  ORCID 

CERCA Institutes

Cerdanyola del Vallès, Spain

2004

Institut Català de Nanociència i Nanotecnologia (ICN2)

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https://icn2.cat/en/x-ray-diffraction-facility-overview

Equipments & Services Offered

Malvern PANalytical X’pert Pro MPD The MPD (Materials Powder Diffractometer) is suitable for the analysis of polycrystalline samples at room temperature. This diffractometer has a vertical theta-theta goniometer (240 mm radius), where the sample stage is fixed and does not rotate around omega axis as in ω-2θ diffractometers. Malvern PANalytical X’pert Pro MRD The MRD (Materials Research Diffractometer) is suitable for the structural characterization in thin-films materials at room and high temperature. This diffractometer has a horizontal ω-2θ goniometer (320 mm radius) in a four-circle geometry and it works with a ceramic X-ray tube with Cu Kα anode (λ=1.540 Å). This diffractometer is equipped with different incident and diffracted optics which can be interchanged depending on the application required (i.e. a parabolic mirror, a hybrid monochromator, a Ge(440) four-crystal monochromator, a parallel plate collimator, and a polycapillary lens).

Case studies and examples on the facility website

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