Metrological assurance of measurements of the dimensional parameters of nanoparticles and thin films by small-angle X-ray diffractometry methods

To assure the verification and calibration of small-angle X-ray diffractometers owned by many organizations of the national nanotechnology network, new technologically simple synthesis methods have been developed and standard reference samples (SRS) based on metal gold nanoparticles and semiconductor zinc oxide of a size of 2–10 nm have been fabricated. The SRS of multilayer thin films of fatty acid salts of a recurrence period of 4.9 nm on solid substrates have been obtained as well. A complex of techniques for the calculation and cross verification of dimensional parameters by methods of diffraction, high-resolution transmission and analytical electron microscopy, electronography, and X-ray phase analysis, as well as using synchrotron radiation, has been developed. The techniques and programs of determining the parameters of nanoparticle dispersion from the data of small-angle X-ray scattering from disordered systems based on stable numerical methods of solving the problem of searching for the size distribution have been improved. The software and techniques of calibration of the angle scale of small-angle diffractometers on the data of both scattering from standard samples with nanoparticles and reflectrometry from multilayer films samples have been developed. Techniques of the primary processing of the X-ray scattering data taking into account the peculiarities of the equipment in order to present measurements in a unified format have been developed as well. Examples of calibrating a laboratory small-angle diffractometer using the developed standards are provided.