LABORATORY ON OPERANDO MEHODS OF STUDY
PROJECT BG05M2OP001-1.001-0008 | NATIONAL CENTER OF MECHATRONICS AND CLEAN TECHNOLOGIES
Manager: Prof. PhD Mihail Mihaylov (IGIC-BAS),
Prof. PhD Tatyana Tabakova (IC-BAS)
E-mail: misho@svr.igic.bas.bg
Tel. (+359 2) 9796312
E-mail: tabakova@ic.bas.bg
Tel. (+359 2) 9792528
The laboratory performs operando and in-situ measurements with Fourier transform infrared (FTIR) spectroscopy, which are a powerful tool for detailed study of the mechanism of adsorption and catalytic processes. The results of these studies can be used as a foundation in the design of efficient materials for clean technologies (gas separation, purification, storage, sensing, catalysis, etc.). Potential partners and clients in the laboratory can be research teams and business representatives with interests in the field.
ACTIVITIES
- Characterization of surface centers (nature, acidity, oxidation, coordination state, etc.) using adsorption of infrared (IR) probe molecules (CO, NO, N2, CD3CN, CH3OH …);
- Elucidation of the nature and structure of surface species with isotope-labeled molecules (13CO, 15NO, 18O2, D2, D2O…);
- Study of the changes in the surface properties after various thermal and redox treatments;
- Study of the adsorption of CO2 and H2 in porous materials;
- Study of catalytic processes (e.g., conversion of nitrogen oxides, methanol decomposition) with simultaneous monitoring of surface species and reaction products.
SERVICES
- Recording of IR spectra of powdered materials (in the form of thin pellets, without dilution in KBr) after activation treatment under controlled conditions. Characterization of surface hydroxyl groups and impurities;
- Recording of IR spectra of adsorbed probe molecules such as CO on activated samples. Characterization of Brønsted and Lewis surface acid sites and determination of the nature, oxidation and coordination state of metal sites;
- Recording of IR spectra of surface compounds during adsorption and catalytic conversion under controlled conditions. Molecular level understanding of processes.
EQUIPMENT
SYSTEM FOR OPERANDO/IN SITU SPECTROSCOPY
The system includes:
– FTIR spectrometer Thermo Scientific Nicolet iS50R (fast scan, MCT-A detector);
– IR reaction cells from Harrick Scientific for in-situ/operando measurements: (i) high temperature transmission cell and (ii) high temperature diffusion reaction chamber, used in conjunction with the Praying Mantis accessory;
– Exhaust gas analyzers: (i) gas chromatograph Thermo Scientific Trace 1300 Series and (ii) mass spectrometer Hiden Analytical HPR-20 R&D;
– Gas flow set-up: Bronkhorst EL-FLOW Prestige mass-flow controllers, gas lines, valves.
Operando methodology allows spectroscopic characterization of materials during their operation in various processes, e.g. in catalytic processes with simultaneous measurement of catalytic activity and selectivity. On the contrary, in-situ spectroscopy deals with the analysis under controlled environment.