Open AccessOxygen vacancies on Pd/TiO2 are detected at low pressures by ESR spectroscopy at ambient temperatures
Author(s) -
Deniz Üner,
Melis Yarar
Publication year - 2022
Publication title -
turkish journal of chemistry
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.239
H-Index - 46
eISSN - 1303-6130
pISSN - 1300-0527
DOI - 10.55730/1300-0527.3416
Subject(s) - electron paramagnetic resonance , chemistry , analytical chemistry (journal) , oxygen , torr , paramagnetism , spectrometer , hydrogen , saturation (graph theory) , spectroscopy , spectral line , nuclear magnetic resonance , optics , condensed matter physics , physics , mathematics , organic chemistry , chromatography , combinatorics , quantum mechanics , astronomy , thermodynamics
A low field benchtop electron spin resonance (ESR) (also referred to as electron paramagnetic resonance (EPR)) spectrometer is used to reveal paramagnetic centres such as oxygen vacancies and Ti +3 centres over 0.5%Pd/TiO 2 . The measurement was performed at room temperature after the sample was reduced in situ under mild hydrogen pressures and evacuated to P < 10 -6 Torr. The measurement was possible due to a T 1 compensation effect under vacuum: Correlation times at low pressures enabled sufficient line narrowing and detection of the ESR signal, justifying a method using benchtop spectrometers coupled to vacuum manifolds. The method justification was demonstrated using similar measurements performed on a reference compound, Mn(II) in plasticine: a measurement performed by saturation recovery technique revealed that T 1 of the signal due to Mn(II) was smaller in vacuum than its atmosphere exposed counterpart. By applying vacuum, the ESR spectra of 0.5%Pd/TiO 2 were collected at ambient temperatures, with features equivalent to the published data obtained at cryogenic temperatures.