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However, the selective and reversible detection of trace concentrations of H<jats:sub>2<\/jats:sub>S (\u22480.1\u00a0ppm) in high humidity conditions (exhaled breath) is challenging because of irreversible H<jats:sub>2<\/jats:sub>S adsorption\/desorption at the surface of chemiresistors. The study reports the synthesis of Fe\u2010doped CuO hollow spheres as H<jats:sub>2<\/jats:sub>S gas\u2010sensing materials via spray pyrolysis. 4 at.% of Fe\u2010doped CuO hollow spheres exhibit high selectivity (response ratio \u2265 34.4) over interference gas (ethanol, 1\u00a0ppm) and reversible sensing characteristics (100% recovery) to 0.1\u00a0ppm of H<jats:sub>2<\/jats:sub>S under high humidity (relative humidity 80%) at 175 \u00b0C. The effect of multi\u2010valent transition metal ion doping into CuO on sensor reversibility is confirmed through the enhancement of recovery kinetics by doping 4 at.% of Ti\u2010 or Nb ions into CuO sensors. Mechanistic details\u00a0of these excellent H<jats:sub>2<\/jats:sub>S sensing characteristics are also investigated by analyzing the redox reactions and the catalytic activity change of the Fe\u2010doped CuO sensing materials. The selective and reversible detection of H<jats:sub>2<\/jats:sub>S using the Fe\u2010doped CuO sensor suggested in this work opens a new possibility for halitosis self\u2010monitoring.<\/jats:p>","DOI":"10.1002\/smll.202308963","type":"journal-article","created":{"date-parts":[[2024,3,10]],"date-time":"2024-03-10T19:56:07Z","timestamp":1710100567000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":20,"title":["Highly Selective and Reversible Detection of Simulated Breath Hydrogen Sulfide Using Fe\u2010Doped CuO Hollow Spheres: Enhanced Surface Redox Reaction by Multi\u2010Valent Catalysts"],"prefix":"10.1002","volume":"20","author":[{"given":"Ki Beom","family":"Kim","sequence":"first","affiliation":[{"name":"Department of Materials Science and Engineering Korea University  Seoul 02841 Republic of Korea"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Myung 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