Insight into the Oxygen-Sensing Mechanisms of TiO<sub>2</sub>–CeO<sub>2</sub> Mixed Oxides Treated in a High-Energy Ball Mill: An XPS Analysis

This study explored the oxygen-sensing mechanism of CeO<sub>2</sub> modified with TiO<sub>2</sub> via high-energy ball milling at different speeds. Different characterization techniques were employed to investigate the obtained materials. Quantitative surface analysis by X-ra...

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Main Authors: Jelena N. Stevanović, Ana G. Silva, Nenad Bundaleski, Dana Vasiljević-Radović, Milija Sarajlić, Orlando M. N. D. Teodoro, Srđan P. Petrović
Format: Article
Language:English
Published: MDPI AG 2025-05-01
Series:Inorganics
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Online Access:https://www.mdpi.com/2304-6740/13/5/159
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author Jelena N. Stevanović
Ana G. Silva
Nenad Bundaleski
Dana Vasiljević-Radović
Milija Sarajlić
Orlando M. N. D. Teodoro
Srđan P. Petrović
author_facet Jelena N. Stevanović
Ana G. Silva
Nenad Bundaleski
Dana Vasiljević-Radović
Milija Sarajlić
Orlando M. N. D. Teodoro
Srđan P. Petrović
author_sort Jelena N. Stevanović
collection DOAJ
description This study explored the oxygen-sensing mechanism of CeO<sub>2</sub> modified with TiO<sub>2</sub> via high-energy ball milling at different speeds. Different characterization techniques were employed to investigate the obtained materials. Quantitative surface analysis by X-ray photoelectron spectroscopy was conducted to elucidate their sensitivity mechanisms and assess the impact of the introduction of TiO<sub>2</sub>. A comparable concentration of oxygen vacancies was found in the samples milled at 350 and 450 rpm. Electrical measurements conducted at temperatures lower than required for semiconductor gas sensors revealed the higher sensitivity of these two samples in comparison to pure CeO<sub>2</sub> at an oxygen concentration above 10%. In contrast, the samples derived from precursors milled at the highest speed exhibited the lowest sensitivity. This may be linked to a slight decrease in the vacancy concentration and the presence of a differentially charged carbon-containing phase. Eventually, the C 1s line provided significant insight into the surface characteristics of the materials. The uniform and non-uniform charging found for pure TiO<sub>2</sub> and CeO<sub>2</sub>, respectively, along with the high charging of CeO<sub>2</sub>, suggest that TiO<sub>2</sub> promotes the contact between the sensing layer and the overlayer. Sensor testing showed the significantly lower resistance of mixed oxides in comparison to CeO<sub>2</sub>, which increases the utility of metal oxide-based sensors.
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spelling doaj-art-e2550a7e524d46a98cf82bc59e9e5c222025-08-20T01:56:31ZengMDPI AGInorganics2304-67402025-05-0113515910.3390/inorganics13050159Insight into the Oxygen-Sensing Mechanisms of TiO<sub>2</sub>–CeO<sub>2</sub> Mixed Oxides Treated in a High-Energy Ball Mill: An XPS AnalysisJelena N. Stevanović0Ana G. Silva1Nenad Bundaleski2Dana Vasiljević-Radović3Milija Sarajlić4Orlando M. N. D. Teodoro5Srđan P. Petrović6Institute of Chemistry, Technology and Metallurgy, University of Belgrade, Njegoševa 12, 11000 Belgrade, SerbiaCeFiTec, Nova School of Science and Technology, New University of Lisbon, Campus da Caparica, 2829-516 Caparica, PortugalCeFiTec, Nova School of Science and Technology, New University of Lisbon, Campus da Caparica, 2829-516 Caparica, PortugalInstitute of Chemistry, Technology and Metallurgy, University of Belgrade, Njegoševa 12, 11000 Belgrade, SerbiaInstitute of Chemistry, Technology and Metallurgy, University of Belgrade, Njegoševa 12, 11000 Belgrade, SerbiaCeFiTec, Nova School of Science and Technology, New University of Lisbon, Campus da Caparica, 2829-516 Caparica, PortugalInstitute of Chemistry, Technology and Metallurgy, University of Belgrade, Njegoševa 12, 11000 Belgrade, SerbiaThis study explored the oxygen-sensing mechanism of CeO<sub>2</sub> modified with TiO<sub>2</sub> via high-energy ball milling at different speeds. Different characterization techniques were employed to investigate the obtained materials. Quantitative surface analysis by X-ray photoelectron spectroscopy was conducted to elucidate their sensitivity mechanisms and assess the impact of the introduction of TiO<sub>2</sub>. A comparable concentration of oxygen vacancies was found in the samples milled at 350 and 450 rpm. Electrical measurements conducted at temperatures lower than required for semiconductor gas sensors revealed the higher sensitivity of these two samples in comparison to pure CeO<sub>2</sub> at an oxygen concentration above 10%. In contrast, the samples derived from precursors milled at the highest speed exhibited the lowest sensitivity. This may be linked to a slight decrease in the vacancy concentration and the presence of a differentially charged carbon-containing phase. Eventually, the C 1s line provided significant insight into the surface characteristics of the materials. The uniform and non-uniform charging found for pure TiO<sub>2</sub> and CeO<sub>2</sub>, respectively, along with the high charging of CeO<sub>2</sub>, suggest that TiO<sub>2</sub> promotes the contact between the sensing layer and the overlayer. Sensor testing showed the significantly lower resistance of mixed oxides in comparison to CeO<sub>2</sub>, which increases the utility of metal oxide-based sensors.https://www.mdpi.com/2304-6740/13/5/159mixed oxideshigh-energy ball millingoxygen sensingmaterials characterization
spellingShingle Jelena N. Stevanović
Ana G. Silva
Nenad Bundaleski
Dana Vasiljević-Radović
Milija Sarajlić
Orlando M. N. D. Teodoro
Srđan P. Petrović
Insight into the Oxygen-Sensing Mechanisms of TiO<sub>2</sub>–CeO<sub>2</sub> Mixed Oxides Treated in a High-Energy Ball Mill: An XPS Analysis
Inorganics
mixed oxides
high-energy ball milling
oxygen sensing
materials characterization
title Insight into the Oxygen-Sensing Mechanisms of TiO<sub>2</sub>–CeO<sub>2</sub> Mixed Oxides Treated in a High-Energy Ball Mill: An XPS Analysis
title_full Insight into the Oxygen-Sensing Mechanisms of TiO<sub>2</sub>–CeO<sub>2</sub> Mixed Oxides Treated in a High-Energy Ball Mill: An XPS Analysis
title_fullStr Insight into the Oxygen-Sensing Mechanisms of TiO<sub>2</sub>–CeO<sub>2</sub> Mixed Oxides Treated in a High-Energy Ball Mill: An XPS Analysis
title_full_unstemmed Insight into the Oxygen-Sensing Mechanisms of TiO<sub>2</sub>–CeO<sub>2</sub> Mixed Oxides Treated in a High-Energy Ball Mill: An XPS Analysis
title_short Insight into the Oxygen-Sensing Mechanisms of TiO<sub>2</sub>–CeO<sub>2</sub> Mixed Oxides Treated in a High-Energy Ball Mill: An XPS Analysis
title_sort insight into the oxygen sensing mechanisms of tio sub 2 sub ceo sub 2 sub mixed oxides treated in a high energy ball mill an xps analysis
topic mixed oxides
high-energy ball milling
oxygen sensing
materials characterization
url https://www.mdpi.com/2304-6740/13/5/159
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