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Herein, we systematically investigate the effect of synthesis pH (2, 4, and 6) on the structural, morphological, electronic, and photocatalytic properties of Nb2O5 nanoparticles prepared via two hydrothermal routes. pH variation in Route 1 promotes a phase transition from pseudohexagonal TT-Nb2O5 (pH 2) to hydrated Nb2O5nH2O (pH 4\u20136), accompanied by pronounced morphological evolution from nanoneedles to lamellar structures. In contrast, Route 2 preserves the TT-Nb2O5 phase regardless of post-treatment pH, highlighting its structural stability. In organic pollutant degradation, all samples were active toward Rhodamine B and amiloride, where mechanistic studies revealed a hole-dominated oxidation pathway with secondary involvement of superoxide radicals. Hydrated Nb2O5\u00b7nH2O phases exhibited strong adsorption capacity, whereas TT-Nb2O5 showed higher intrinsic photocatalytic efficiency. Stability tests confirmed sustained activity over four cycles. TT-Nb2O5 materials also exhibited superior charge-transfer properties and were active in H2 evolution, achieving up to 4104.5 \u03bcmol g\u20131 after 8 h (Nb2O5-AP2). Optimization of Pt loading revealed an optimal cocatalyst content of 0.5 wt %, while long-term assays confirmed stable H2 production over 24 h of operation. Photoluminescence results indicated that recombination suppression contributes to performance enhancement but does not solely govern activity. These findings demonstrate that synthesis pH governs phase formation, surface chemistry, and charge-carrier dynamics in Nb2O5, providing fundamental insights into the rational design of niobium-based photocatalysts tailored for integrated environmental and energy applications.<\/jats:p>","DOI":"10.1021\/acsphyschemau.5c00132","type":"journal-article","created":{"date-parts":[[2026,3,18]],"date-time":"2026-03-18T16:55:38Z","timestamp":1773852938000},"page":"1018-1030","source":"Crossref","is-referenced-by-count":3,"title":["pH-Controlled\nSynthesis of Nb2O5 Nanoparticles with Enhanced\nPerformance for Photodegradation of\nOrganic Pollutants and H2 Production"],"prefix":"10.1021","volume":"6","author":[{"given":"Carolina X. J.","family":"Silva","sequence":"first","affiliation":[{"name":"Federal University of Uberla\u0302ndia (IQUFU) , , Avenue Joa\u0303o Naves de A\u0301vila, 2121, Santa Monica , , ,","place":["Uberla\u0302ndia, Minas Gerais, Brazil, 38400-902"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0001-7788-8034","authenticated-orcid":true,"given":"Marcela","family":"Piassi Bernardo","sequence":"additional","affiliation":[{"name":"Federal University of Uberla\u0302ndia (IQUFU) , , Avenue Joa\u0303o Naves de A\u0301vila, 2121, Santa Monica , , ,","place":["Uberla\u0302ndia, Minas Gerais, Brazil, 38400-902"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"suffix":"Jr.","given":"Ivan Jose\u0301","family":"Silva","sequence":"additional","affiliation":[{"name":"Federal University of Uberla\u0302ndia (IQUFU) , , Avenue Joa\u0303o Naves de A\u0301vila, 2121, Santa Monica , , ,","place":["Uberla\u0302ndia, Minas Gerais, Brazil, 38400-902"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Sheila Cristina","family":"Canobre","sequence":"additional","affiliation":[{"name":"Federal University of Uberla\u0302ndia (IQUFU) , , Avenue Joa\u0303o Naves de A\u0301vila, 2121, Santa Monica , , ,","place":["Uberla\u0302ndia, Minas Gerais, Brazil, 38400-902"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0003-2077-4583","authenticated-orcid":true,"given":"Osmando F.","family":"Lopes","sequence":"additional","affiliation":[{"name":"Federal University of Uberla\u0302ndia (IQUFU) , , Avenue Joa\u0303o Naves de A\u0301vila, 2121, Santa Monica , , ,","place":["Uberla\u0302ndia, Minas Gerais, Brazil, 38400-902"]}],"role":[{"vocabulary":"crossref","role":"author"}]}],"member":"316","published-online":{"date-parts":[[2026,3,18]]},"reference":[{"key":"2026092310065605200_cit1","doi-asserted-by":"publisher","first-page":"143586","DOI":"10.1016\/j.electacta.2023.143586","article-title":"Effective Photoelectrocatalysis of\nLevofloxacin Antibiotic with Ti\/IrO2Nb2O5 in Environmental Samples","volume":"475","author":"Fernandes","year":"2024","journal-title":"Electrochim. Acta"},{"issue":"5","key":"2026092310065605200_cit2","doi-asserted-by":"publisher","first-page":"1277","DOI":"10.1016\/S1872-2067(21)63976-1","article-title":"Engineering Piezoelectricity and\nStrain Sensitivity in CdS to Promote Piezocatalytic Hydrogen Evolution","volume":"43","author":"Wang","year":"2022","journal-title":"Chin. J. Catal."},{"issue":"9","key":"2026092310065605200_cit3","doi-asserted-by":"publisher","first-page":"9919","DOI":"10.1021\/cr5001892","article-title":"Understanding\nTiO2 Photocatalysis:\nMechanisms and Materials","volume":"114","author":"Schneider","year":"2014","journal-title":"Chem. Rev."},{"key":"2026092310065605200_cit4","doi-asserted-by":"publisher","first-page":"117732","DOI":"10.1016\/j.jelechem.2023.117732","article-title":"Using a Novel Gas\nDiffusion Electrode Based on Vulcan\nXC-72 Carbon Modified with Nb2O5 Nanorods for Enhancing H2O2 Electrogeneration","volume":"946","author":"Trench","year":"2023","journal-title":"J. Electroanal. Chem."},{"key":"2026092310065605200_cit5","doi-asserted-by":"publisher","first-page":"125807","DOI":"10.1016\/j.chemosphere.2019.125807","article-title":"Degradation\nof Antibiotic Ciprofloxacin by Different AOP Systems Using Electrochemically\nGenerated Hydrogen Peroxide","volume":"247","author":"Lima","year":"2020","journal-title":"Chemosphere"},{"key":"2026092310065605200_cit6","doi-asserted-by":"publisher","first-page":"182237","DOI":"10.1016\/j.jallcom.2025.182237","article-title":"Stepwise Hydrothermal\nSynthesis of Bi2S3\/PbBiO2Cl S-Scheme\nHeterojunction for Synergistic Piezo-Photocatalytic Dyes Degradation","volume":"1037","author":"Zheng","year":"2025","journal-title":"J. Alloys Compd."},{"issue":"5","key":"2026092310065605200_cit7","doi-asserted-by":"publisher","first-page":"118386","DOI":"10.1016\/j.jece.2025.118386","article-title":"Ultrasound-Driven S-Scheme\ng-C3N5\/Bi4Ti3O12 Heterojunctions for Enhanced Piezocatalytic Degradation\nof Organic Dyes","volume":"13","author":"Xu","year":"2025","journal-title":"J. Environ. Chem. Eng."},{"key":"2026092310065605200_cit8","doi-asserted-by":"publisher","first-page":"146189","DOI":"10.1016\/j.jclepro.2025.146189","article-title":"Harvesting Vibration Energy for Efficiently Piezocatalytic\nDegradation of Organic Dyes by Bi11VO19 Nanosheets","volume":"521","author":"Zhou","year":"2025","journal-title":"J. Cleaner Prod."},{"issue":"19","key":"2026092310065605200_cit9","doi-asserted-by":"publisher","first-page":"18037","DOI":"10.1021\/acsnano.5c02660","article-title":"Unveiling\nMechanically\nDriven Catalytic Processes: Beyond Piezocatalysis to Synergetic Effects","volume":"19","author":"Jiang","year":"2025","journal-title":"ACS Nano"},{"issue":"15","key":"2026092310065605200_cit10","doi-asserted-by":"publisher","first-page":"8927","DOI":"10.1021\/acsomega.0c00699","article-title":"Easy Synthesis of BiVO4 for Photocatalytic\nOverall Water Splitting","volume":"5","author":"Chen","year":"2020","journal-title":"ACS Omega"},{"issue":"88","key":"2026092310065605200_cit11","doi-asserted-by":"publisher","first-page":"37517","DOI":"10.1016\/j.ijhydene.2021.10.139","article-title":"Structure-Mechanism\nRelationship for Enhancing Photocatalytic H2 Production","volume":"47","author":"Zhang","year":"2022","journal-title":"Int. J. Hydrogen Energy"},{"key":"2026092310065605200_cit12","doi-asserted-by":"publisher","first-page":"101715","DOI":"10.1016\/j.surfin.2021.101715","article-title":"A Novel Understanding\nof Morphological Anisotropy Features\nof Nanorod Units in Brookite Dominated Triphase Mesoporous TiO2 and\nIts Excellent Photocatalytic Activity in Phenol Decomposition: The\nRole of Synthesis PH and Surface Hydroxylation","volume":"29","author":"Seal","year":"2022","journal-title":"Surf. Interfaces"},{"issue":"19","key":"2026092310065605200_cit13","doi-asserted-by":"publisher","first-page":"23731","DOI":"10.1007\/s11356-020-11262-5","article-title":"Nb2O5 Nanoparticles\nDecorated with Magnetic Ferrites for Wastewater Photocatalytic Remediation","volume":"28","author":"Paris","year":"2021","journal-title":"Environ. Sci. Pollut. Res."},{"issue":"1","key":"2026092310065605200_cit14","doi-asserted-by":"publisher","first-page":"126","DOI":"10.3390\/catal10010126","article-title":"Recent\nAdvances in Niobium-Based Materials for Photocatalytic Solar Fuel\nProduction","volume":"10","author":"Nunes","year":"2020","journal-title":"Catalysts"},{"key":"2026092310065605200_cit15","doi-asserted-by":"publisher","first-page":"1","DOI":"10.1016\/j.pmatsci.2016.02.001","article-title":"Niobium Oxides and Niobates Physical\nProperties: Review and Prospects","volume":"80","author":"Nico","year":"2016","journal-title":"Prog. Mater.\nSci."},{"issue":"1","key":"2026092310065605200_cit16","doi-asserted-by":"publisher","first-page":"106","DOI":"10.5935\/0100-4042.20140280","article-title":"O\u0301xidos de Nio\u0301bio:\nUma Visa\u0303o Sobre\na Si\u0301ntese Do Nb2O5 e Sua Aplicac\u0327a\u0303o Em Fotocata\u0301lise\nHeteroge\u0302nea","volume":"38","author":"Lopes","year":"2014","journal-title":"Quim. Nova"},{"issue":"9","key":"2026092310065605200_cit17","doi-asserted-by":"publisher","first-page":"14719","DOI":"10.1016\/j.ceramint.2023.01.068","article-title":"The\nRole of Oxygen Vacancies in TT-Nb2O5\nNanoparticles for the Photoconversion of Glycerol into Solketal","volume":"49","author":"Gomes","year":"2023","journal-title":"Ceram. Int."},{"key":"2026092310065605200_cit18","doi-asserted-by":"publisher","first-page":"138271","DOI":"10.1016\/j.cplett.2020.138271","article-title":"Influence of Nb2O5 Crystal Structure\non Photocatalytic Efficiency","volume":"764","author":"U\u0308cker","year":"2021","journal-title":"Chem. Phys. Lett."},{"key":"2026092310065605200_cit19","doi-asserted-by":"publisher","first-page":"115580","DOI":"10.1016\/j.jcat.2024.115580","article-title":"Niobium\nOxides: The Key Role of Hydroxylated Surface on Photocatalytic Driven\nC\u2013C Reductive Coupling of Acetophenone","volume":"436","author":"Filho","year":"2024","journal-title":"J. Catal."},{"key":"2026092310065605200_cit20","doi-asserted-by":"publisher","first-page":"494","DOI":"10.1016\/j.jssc.2018.10.018","article-title":"A Review\non Effect of Synthesis Conditions on the Formation of Layered Double\nHydroxides","volume":"269","author":"Bukhtiyarova","year":"2019","journal-title":"J. Solid State Chem."},{"key":"2026092310065605200_cit21","doi-asserted-by":"publisher","first-page":"144058","DOI":"10.1016\/j.apsusc.2019.144058","article-title":"Synthesis\nand Characterization of TiO2 Nanorods by\nHydrothermal Method with Different PH Conditions and Their Photocatalytic\nActivity","volume":"500","author":"Santhi","year":"2020","journal-title":"Appl. Surf. Sci."},{"key":"2026092310065605200_cit22","doi-asserted-by":"publisher","first-page":"349","DOI":"10.1016\/j.apcatb.2018.10.017","article-title":"Acidic Surface Niobium Pentoxide\nIs Catalytic Active for CO2 Photoreduction","volume":"242","author":"da Silva","year":"2019","journal-title":"Appl. Catal., B"},{"key":"2026092310065605200_cit23","doi-asserted-by":"publisher","first-page":"3642","DOI":"10.1016\/j.jmrt.2023.06.178","article-title":"Promoting the Performance of Nb2O5 by Doping Transition\nMetal Oxide for Catalytic Degradation of Monochlorobenzene and Toluene","volume":"25","author":"Liu","year":"2023","journal-title":"J. Mater. Res. Technol."},{"issue":"43","key":"2026092310065605200_cit24","doi-asserted-by":"publisher","first-page":"14859","DOI":"10.1039\/C7DT02611K","article-title":"Nanostructured N-Doped\nOrthorhombic Nb2O5 as an Efficient Stable Photocatalyst for Hydrogen\nGeneration under Visible Light","volume":"46","author":"Kulkarni","year":"2017","journal-title":"Dalton Trans."},{"issue":"8","key":"2026092310065605200_cit25","doi-asserted-by":"publisher","first-page":"7629","DOI":"10.1021\/acsaem.0c01047","article-title":"CuO Decoration Controls Nb2O5Photocatalyst\nSelectivity in CO2Reduction","volume":"3","author":"Nogueira","year":"2020","journal-title":"ACS Appl. Energy\nMater."},{"issue":"4","key":"2026092310065605200_cit26","doi-asserted-by":"publisher","first-page":"3521","DOI":"10.1016\/j.ceramint.2016.11.063","article-title":"Synthesis\nof G-C3N4\/Nb2O5 Heterostructures and Their Application in the Removal\nof Organic Pollutants under Visible and Ultraviolet Irradiation","volume":"43","author":"Carvalho","year":"2017","journal-title":"Ceram. Int."},{"key":"2026092310065605200_cit27","doi-asserted-by":"publisher","first-page":"220","DOI":"10.1016\/j.cej.2016.11.135","article-title":"Enhanced Cr(VI) Photoreduction\nin Aqueous Solution Using Nb2O5\/CuO Heterostructures under UV and\nVisible Irradiation","volume":"312","author":"Nogueira","year":"2017","journal-title":"Chem. Eng. J."},{"key":"2026092310065605200_cit28","doi-asserted-by":"publisher","first-page":"131418","DOI":"10.1016\/j.cej.2021.131418","article-title":"Anchoring Dye onto\n1D Nb2O5 in Cooperation with TEMPO for the Selective Photocatalytic\nAerobic Oxidation of Amines","volume":"426","author":"Ma","year":"2021","journal-title":"Chem. Eng. J."},{"key":"2026092310065605200_cit29","doi-asserted-by":"publisher","first-page":"800","DOI":"10.1016\/j.apcatb.2013.08.031","article-title":"Synthesis of Nb2O5\nNanoparticles\nthrough the Oxidant Peroxide Method Applied to Organic Pollutant Photodegradation:\nA Mechanistic Study","volume":"144","author":"Lopes","year":"2014","journal-title":"Appl. Catal., B"},{"key":"2026092310065605200_cit30","doi-asserted-by":"publisher","DOI":"10.21577\/0103-5053.20240137","article-title":"Sustainable\nRecycling of Spent Li-Ion Batteries and Iron Ore Tailings for Cobalt\nFerrite Synthesis and Its Dual Applications as a Photocatalyst in\nSolar Photo-Fenton Process and an Electrochemical Sensor","volume":"36","author":"Almeida","year":"2025","journal-title":"J. Braz. Chem. Soc."},{"key":"2026092310065605200_cit31","doi-asserted-by":"publisher","first-page":"112429","DOI":"10.1016\/j.optmat.2022.112429","article-title":"Visible-Light-Driven Hierarchical Porous CeO2 Derived\nfrom Wood for Effective Photocatalytic Degradation of Methylene Blue","volume":"129","author":"Cheng","year":"2022","journal-title":"Opt. Mater."},{"issue":"28","key":"2026092310065605200_cit32","doi-asserted-by":"publisher","first-page":"15066","DOI":"10.1021\/acs.jpcc.0c04202","article-title":"Theoretical\nand Experimental Study on Exciton Properties of TT-, T-, and H-Nb2O5","volume":"124","author":"Jia","year":"2020","journal-title":"J. Phys. Chem. C"},{"issue":"7","key":"2026092310065605200_cit33","doi-asserted-by":"publisher","first-page":"1457","DOI":"10.1039\/b210055j","article-title":"Niobium Pentoxide Prepared by Soft\nChemical Routes:\nMorphology, Structure, Defects and Quantum Size Effect","volume":"5","author":"Brayner","year":"2003","journal-title":"Phys. Chem. Chem. Phys."},{"issue":"4","key":"2026092310065605200_cit34","doi-asserted-by":"publisher","DOI":"10.21577\/0103-5053.20230163","article-title":"Niobium Oxide Photocatalytically Oxidizes Ammonia in\nWater at Ambient Conditions","volume":"35","author":"Elias","year":"2024","journal-title":"J. Braz. Chem.\nSoc."},{"issue":"17","key":"2026092310065605200_cit35","doi-asserted-by":"publisher","first-page":"3271","DOI":"10.1557\/jmr.2017.93","article-title":"Microwave-Assisted Synthesis of Nb2O5\nfor Photocatalytic Application of Nanopowders and Thin Films","volume":"32","author":"Falk","year":"2017","journal-title":"J. Mater. Res."},{"issue":"3","key":"2026092310065605200_cit36","doi-asserted-by":"publisher","first-page":"218","DOI":"10.2298\/PAC1803218G","article-title":"The Effect of the Synthesis Conditions\non Structure and Photocatalytic Activity of Nb2O5 Nanostructures","volume":"12","author":"Go\u0301mez","year":"2018","journal-title":"Process. Appl. Ceram."},{"issue":"21","key":"2026092310065605200_cit37","doi-asserted-by":"publisher","first-page":"2658","DOI":"10.1016\/j.matlet.2004.03.041","article-title":"Sol-Gel Synthesis and Characterization\nof Nb2O5 Powders","volume":"58","author":"Ristic\u0301","year":"2004","journal-title":"Mater. Lett."},{"key":"2026092310065605200_cit38","doi-asserted-by":"publisher","first-page":"110408","DOI":"10.1016\/j.solmat.2020.110408","article-title":"Dependence of Photoactivity\nof Niobium Pentoxide (Nb2O5) on Crystalline Phase and Electrokinetic\nPotential of the Hydrocolloid","volume":"208","author":"Kumari","year":"2020","journal-title":"Sol. Energy Mater.\nSol. Cells"},{"issue":"3","key":"2026092310065605200_cit39","doi-asserted-by":"publisher","first-page":"1489","DOI":"10.1016\/j.apsusc.2006.02.035","article-title":"La 1-x\nCa x CoO 3 Perovskite-Type Oxides: Identification of the Surface Oxygen\nSpecies by XPS","volume":"253","author":"Merino","year":"2006","journal-title":"Appl. Surf. Sci."},{"key":"2026092310065605200_cit40","doi-asserted-by":"publisher","first-page":"288","DOI":"10.1016\/j.apcatb.2011.10.010","article-title":"Thermodecomposition\nSynthesis of WO 3\/H 2WO 4 Heterostructures with Enhanced Visible Light\nPhotocatalytic Properties","volume":"111\u2013112","author":"Cao","year":"2012","journal-title":"Appl. Catal., B"},{"key":"2026092310065605200_cit41","doi-asserted-by":"publisher","first-page":"160","DOI":"10.1016\/j.matchemphys.2019.02.062","article-title":"Zn-Doped Nb 2\nO 5 Photocatalysts Driven by Visible-Light: An Experimental and Theoretical\nStudy","volume":"228","author":"Oliveira","year":"2019","journal-title":"Mater. Chem. Phys."},{"issue":"1","key":"2026092310065605200_cit42","doi-asserted-by":"publisher","first-page":"861","DOI":"10.1016\/j.ceramint.2011.06.054","article-title":"Synthesis\nof Lamellar Niobic Acid\nNanorods via Proton-Exchange and Their Conversion to T-Nb2O5 Nanorods","volume":"38","author":"Xu","year":"2012","journal-title":"Ceram. Int."},{"issue":"1","key":"2026092310065605200_cit43","doi-asserted-by":"publisher","first-page":"254","DOI":"10.1039\/D1EE02664J","article-title":"A Niobium\nOxide with a Shear Structure and Planar Defects for High-Power\nLithium Ion Batteries","volume":"15","author":"Li","year":"2022","journal-title":"Energy Environ. 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