Small Angle X-ray Scattering

Structural & Morphology Characterization (X-ray analysis)

Small Angle X-ray Scattering is a non-destructive and highly versatile standard method to study at the nanoscale the structure of any type of material ranging from innovative nanostructured materials to biological macromolecules. With this technique, the in- homogeneities of the electron density in the samples are characterized, as a function of the scattering angle.

The investigated sample is irradiated with a monochromatic radiation, and scattered X-rays are typically collected in an angular range of 0 – 10° by a suitable detector (ie. CCD or imaging plate) and up to 60° (by using an imaging plate for the systems coupling SAXS and Wide Angle X-Ray Scattering, WAXS). By means of appropriate model fittings and reconstructions, SAXS data  deliver information on averaged particle sizes, shapes, distributions and materials' porosity.

SAXS allows structural studies in a dimension range typically between  1 and 100 nm; the dimension limits depend on the selected instrument. Samples can be probed in solution, solid, at the interface or in the gas phase;  with specially designed sample holders,  they can be measured under various conditions,  like at different temperature, humidity, high pressure and under mechanical stress/strain conditions.  Moreover, SAXS  can be used for time-resolved studies on fast structural transitions during chemical reactions or self-assembly process.

Grazing-incidence (GISAXS) measurements can be performed to study self-assembly processes on surfaces, as well as to perform structural characterisations of thin films.

At wider scattering angle (Wide Angle X-ray Scattering, WAXS), intramolecular dimensions, as well as the degree of crystallinity of the samples, can be probed.

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          provided at NFFA-Europe laboratories by:
TUG
Italy
CNR-DSCTM
Italy
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          provided at Large Scale Facilities by:
TUG
Italy
ALBA
Spain
SOLEIL
France
TUG
Italy
SAXS at TUG - Trieste
Low contrast solution scattering, grazing incidence surface diffraction, micro-spot scanning, x-ray fluorescence analysis, time-resolved studies (≥ 11 µs) and simultaneously performed Small- and Wide-Angle Measurements (SWAXS), Grazing Incidence Small Angle Scattering
Elettra Synchrotron Wiggler (NdFeB Hybrid), Critical Energy 4.27 keV; Radiation Power (9 mRad) 8.6 kW; Flux at sample 7.5 x 1012 ph/s (2 GeV, 300 mA, 8 keV)
2.0 or 2.4 GeV
Pilatus 1M (sensitive area 168.7 x 179.4 mm² ) and 100k (sensitive area 83.8 x 33.5 mm²) (Dectris, CH), single photon counting mode.
The SAXS Beamline accepts 2 discrete energies: 8 and 16 keV ( (1.54 and 0.77 Å).
Resolution in real space: 10-1400 Å (SAXS), 1- 9 Å (WAXS)
Gels, Liquid Crystals, (Bio)Polymers (solution, thin films, solid), Amorphous Materials, Fibers.
- Flow through cell for sample recirculation, eventually coupled with a thermostatable capillary holder (temperature range -30 – 150°C and 70 – 300°C). - Craddle for Grazing incidence SWAXS: Sample movement precision: rotation: 0.001 deg; translation : 5µm. - Domed hot stage for GISAXS: temperature range, 25 – 1100°C. - Stop flow: i) 4- syringe cell with 3 mixer modules for inorganic samples, and ii) 2-syringes, dedicated for biological samples. - High pressure cell system for transmission and grazing incidence experiments. Pressure range: 1-2500 Bar, Temperature range 0 – 80°C. - In-line Differential Scanning Calorimeter (DSC) for simultaneous time-resolved synchrotron X-ray diffraction as a function of the temperature and high sensitivity DSC from the same sample. Heating rate: 0.1 to 10 °C/min, with a 0.01 °C temperature resolution in the range -30/+130 °C. - Relative Humidity controlled cell for GISAXS. - Autosampler for automated processing of up to 480 liquid samples: required sample volume, 100 µl (approximately 20 µl/single measurement); cycle time (excluding measuring time): 35-50 s. - SEC-SAXS: Size Exclusion Chromatography system equipped with UV-Vis spectrometer, a Multi angle Light Scattering detector (MALS) and a Refractive Index refractometer (RI) installed in-line with the SAXS flowthrough cell.
CNR-DSCTM
Italy
SAXS - IPCB