StoRIES Infrastructures: NIC research infrastructure

National Insitute of Chemistry (NIC) research infrastructure in Ljubljana combines infrastructure of 2 Departments at National Institute of Chemistry.

State of the art: in-situ/operando approach for determination of structure, PDF analysis (inhomogeneous distribution of active sites/defects, distribution of the bonding distances of the studied atoms with adjacent atoms), electrochemical cell for in-situ batteries testing, high pressure reaction cells, gravimetric high-resolution isotherms and kinetic adsorption profiles, UV-Vis in-situ/operando characterization up to 900oC, developing new methods.

Services currently offered by the infrastructure: structural and chemical characterizations of materials for thermochemical and electrochemical ES, in situ and ex situ examination of materials` thermal, hydrothermal, structural stability and storage performance.

  1. Powder X-Ray Diffractometers: determination of phase purity and composition, identification of crystalline materials, particle size calculation, in-situ studies of thermal stability of compounds, PDF analysis of local and middle-range order, in-situ studies of materials under reaction conditions;

  • PANalytical X'Pert PRO MPD diffractometer: high-resolution images with only Kα1 part of the X-ray spectrum, for multiphase samples, crystalline samples with low cell symmetry, air or moisture sensitive samples (capillary)
  • PANalytical X'Pert PRO (HTK) diffractometer: high-resolution and high-temperature measurements up to 1200 oC in different ambient conditions (vacuum, different gasses up to 1 bar).
  • EMPYREAN X-ray powder diffractometer with three wavelengths (Cu, Mo, and Ag) enabling PDF analysis and integrated in-situ measurement cells: electrochemical cell for batteries testing and high pressure reaction cell; PDF analysis of the inhomogeneous distribution of active sites/defects, also for partially crystalline or amorphous materials.

2. Gas adsorption analyser: gas adsorption capacity, kinetic measurements, cycling stability, durability;

  • IMI-HTP1 (volumetric), gas adsorption analyser for the adsorption of CO2, N2, CH4, H2 in the pressure range from 10-6 to 100 bar from 77 to 773 K.
  • IGA-100 (gravimetric) water / ethanol adsorption analyser: 10-7 - 1 bar, 20 - 70 o
  • IGAsorpXT (gravimetric); dynamic water vapor analyzer for high-temperature measurements of sorption isotherms (up to 300 °C) via active partial water pressure regulation, isothermal, isobaric and temperature-program experiments.

3. Surface area and porosity analyser (volumetric): determination of structural and textural properties of porous materials: specific surface area, pore volume, pore size distribution (0.4 - 300 nm). Adsorption of argon, nitrogen, carbon dioxide, krypton, oxygen; pressure range from 10-7 bar up to 1 bar and from 77K to room temperature.

4. UV/VIS-DR spectrophotometer: determination of coordination and oxidation state of metal cations, presence of oxides; in-situ and operando characterization of solid materials at wavelengths from 200 to 900 nm in a wide temperature range (up to 900 oC) and atmospheric pressure at defined conditions (i.e. temperature, inert/oxidative/reductive atmosphere).

5. TPR/TPO/TPD chemisorption analyser: determination of active metal area, crystallite size, active metal dispersion by means of dynamic chemisorption method using various probe molecules such as carbon monoxide, hydrogen, methane, nitrogen oxides, ammonia, determination of acidic/basic properties of catalysts and other solids, determination of heat of adsorption by using various adsorbates such as CO, CO2, H2, water vapour, saturated and unsaturated hydrocarbons (e.g., benzene, toluene, pyridine)

https://www.ki.si/en/departments/d09-department-of-inorganic-chemistry-and-technology/equipment/

6. AR STEM: examination of solid samples, observes columns of atom, determine the crystal structure, structure of nanoparticles, crystal boundaries, two dimensional defects, the local bonding, coordination and valence state of the atoms, crystal boundaries, two dimensional defects, reconstruction of 3D shape of the particles or macromolecules, determination of pore arrangement of porous materials, in situ experiments at temperatures from -180 up to 1200 °C and samples can be electrically biased in the potential range of +/- 50 V, obtaining electric fields up to 100 kV/cm. Biasing at temperature up to 1000 °C are also possible, measurements of atom column displacements below 5 pm, single atom detection of N, O, F on graphene layer. It enables atomic resolution (sub-angstrom resolution, typically below 0,8 Å also at 80 kV).

https://www.ki.si/en/departments/d10-department-of-materials-chemistry/electron-microscopy-and-catalysts/