B. Tiss , D. Martínez-Martínez , C. Mansilla , J.R. Gomes , C.S. Abreu , N. Pereira , L. Cunha
{"title":"Protective coatings for complex organic flexible materials I: characterization and tribological performance of TiO2 and ZnO films deposited by magnetron sputtering on cork","authors":"B. Tiss , D. Martínez-Martínez , C. Mansilla , J.R. Gomes , C.S. Abreu , N. Pereira , L. Cunha","doi":"10.1016/j.apsadv.2025.100753","DOIUrl":"10.1016/j.apsadv.2025.100753","url":null,"abstract":"<div><div>The escalating imperative to combat the climate change has generated sustainability trends, leading to a rising demands for eco-friendly products. Cork and rubber are versatile materials based or derived from natural sources with various industrial uses and applications. This work represents the first part of a comprehensive investigation focusing on cork, with rubber being the subject of a subsequent paper. Cork shows unique properties which make it attractive for many applications beyond wine stoppers, such as bags, flooring, walls lining and aerospace components. Nevertheless, cork suffers from strong wearing when subjected to friction and mechanical wear. The objective of this work is to improve the tribological performance of cork by deposition of a protective oxide layer, while preserving its original appearance. As such, optically transparent TiO<sub>2</sub> and ZnO thin films were deposited onto silicon and cork substrates using magnetron sputtering. The TiO<sub>2</sub> thin films exhibited an amorphous structure while the ZnO films displayed texture along the (002) direction of hexagonal wurtzite structure of zinc oxide. ZnO-coated cork showed lower coefficient of friction against 100Cr6 stainless steel balls than uncoated cork, while TiO<sub>2</sub> coatings did not reveal any relevant improvement. The wear rate of the samples was evaluated using a novel method based on the analysis of energy dispersive spectra. All coated samples demonstrated an improvement regarding wear resistance, although ZnO films seem to be more effective, in line with the reduction of friction coefficient up to 38 % respect uncoated cork. The detection of metallic oxide coatings within the wear track after the tribotests indicates a strong adhesion of both coatings to the cork substrate, which is supported by tensile tests.</div></div>","PeriodicalId":34303,"journal":{"name":"Applied Surface Science Advances","volume":"27 ","pages":"Article 100753"},"PeriodicalIF":7.5,"publicationDate":"2025-04-26","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143873616","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Klaus Zimmer , Joachim Zajadacz , Martin Ehrhardt , Pierre Lorenz , Tamás Smausz , Béla Hopp
{"title":"Transfer of photolithographic patterns by excimer laser ablation of polymers","authors":"Klaus Zimmer , Joachim Zajadacz , Martin Ehrhardt , Pierre Lorenz , Tamás Smausz , Béla Hopp","doi":"10.1016/j.apsadv.2025.100754","DOIUrl":"10.1016/j.apsadv.2025.100754","url":null,"abstract":"<div><div>Pattern transfer of lithographically produced patterns is a key technology in microelectronics and other micro- and nanotechnologies. This approach has been perfected continuously to meet the requirements for size and quality, but vacuum processes are required for pattern transfer into microelectronic materials. Here an atmospheric pressure approach of pattern transfer by laser ablation is proposed and demonstrated. Similar plasma-based pattern transfer laser beams provide a directed energy impact to the exposed material, but the resulting material reactions are different as distinct primary processes govern the material removal mechanism by ablation. The laser ablation-based pattern transfer mechanism comprises (i) optical effects such as laser photon absorption and scattering processes, (ii) thermal processes such as material heating and melting, and (iii) laser ablation processes of the masking and the substrate materials. These characteristics cause topographical effects of laser-based pattern transfer (LiPT) process that results in a specific sidewall angle of the transferred pattern due to cone formation effects, trench formation related to diffraction and reflection at the patterns and surrounding wavy pattern due to laser beam diffraction. The ablation rate ratio determines the selectivity for laser-based pattern transfer and therewith the limit in depth. The pattern transfer can be achieved locally with varying parameters including different inclination angles. The results pave the way to a new approach for sustainable economic fabrication processes that do not need vacuum and reactive gases.</div></div>","PeriodicalId":34303,"journal":{"name":"Applied Surface Science Advances","volume":"27 ","pages":"Article 100754"},"PeriodicalIF":7.5,"publicationDate":"2025-04-26","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143873617","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
J.G. Cuadra , S. Molina-Prados , Gladys Mínguez-Vega , L.A. Abderrahim , J. Colombari , J.B. Carda , Nuno P.F. Gonçalves , R.M. Novais , J.A. Labrincha
{"title":"Generation of Schottky heterojunction (SnO2-Au NPs) transparent thin film for ciprofloxacin photodegradation","authors":"J.G. Cuadra , S. Molina-Prados , Gladys Mínguez-Vega , L.A. Abderrahim , J. Colombari , J.B. Carda , Nuno P.F. Gonçalves , R.M. Novais , J.A. Labrincha","doi":"10.1016/j.apsadv.2025.100751","DOIUrl":"10.1016/j.apsadv.2025.100751","url":null,"abstract":"<div><div>In this study, transparent Schottky heterojunction thin films composed of SnO₂ and Au nanoparticles (Au NPs) were developed and applied for the photocatalytic degradation of ciprofloxacin (CIP) under UV light. The SnO₂-Au NPs films achieved a 75 % degradation of CIP and 70 % total organic carbon (TOC) mineralization within 180 min using only 0.02 g/L of catalyst, highlighting their exceptional efficiency compared to conventional powder-based systems. The incorporation of Au NPs significantly enhanced charge separation and reduced electron-hole recombination, as confirmed by structural and optical analyses. Optimal photocatalytic activity was observed at pH 7, following pseudo-first-order kinetics. Scavenger tests and fluorescence probing confirmed that hydroxyl radicals (•OH) and superoxide radicals (O₂•−) were the primary active species. QTOF-MS identified five degradation intermediates, suggesting mechanisms involving defluorination, hydroxylation, and ring cleavage. In silico toxicity assessments showed reduced toxicity for most transformation products. The catalyst exhibited high stability and reusability over four cycles without detectable leaching, indicating strong potential for sustainable water treatment applications.</div></div>","PeriodicalId":34303,"journal":{"name":"Applied Surface Science Advances","volume":"27 ","pages":"Article 100751"},"PeriodicalIF":7.5,"publicationDate":"2025-04-25","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143868226","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Byeong Jun Cha , Sang Ju Lee , Chang Min Choi , Cheolho Jeon , Young Dok Kim , Myoung Choul Choi
{"title":"Effect of CO2 addition to Ar on gas cluster ion beam sputtering of a Si wafer: An in-situ XPS study","authors":"Byeong Jun Cha , Sang Ju Lee , Chang Min Choi , Cheolho Jeon , Young Dok Kim , Myoung Choul Choi","doi":"10.1016/j.apsadv.2025.100750","DOIUrl":"10.1016/j.apsadv.2025.100750","url":null,"abstract":"<div><div>Many recent studies showed mixing CO<sub>2</sub> with the Ar gas source improves the secondary ionization yield of an Ar gas cluster ion beam (GCIB) with enhanced depth resolution. However, the impact of CO<sub>2</sub> addition on the surface chemical structure remains unclear. In the present work, we studied the effect of CO<sub>2</sub> addition to Ar on the GCIB sputtering behavior of a Si wafer surface using an <em>in-situ</em> GCIB & X-ray photoelectron spectroscopy (XPS) combined system. During preferential sputtering with Ar GCIB, substoichiometric SiO<sub>x</sub> (<em>x</em> < 2) forms, leaving unstable Si species on the surface. These species could interact with surface carbon impurities, leading to the formation of SiC. In addition, a slight distortion of Si lattice could increase its amorphous character. Mixing CO<sub>2</sub> with Ar significantly reduces these structural changes without specific carbon contamination.</div></div>","PeriodicalId":34303,"journal":{"name":"Applied Surface Science Advances","volume":"27 ","pages":"Article 100750"},"PeriodicalIF":7.5,"publicationDate":"2025-04-23","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143865095","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Ionela-Cristina Petcu , Raluca Negrea , Ana T.S.C. Brandão , Cosmin Romanitan , Oana Brincoveanu , Nikolay Djourelov , Iuliana Mihalache , L. Monica Veca , Gabriela Isopencu , Carlos M. Pereira , Liana Anicai , Cristina Busuioc , Sabrina State (Rosoiu)
{"title":"Pulsed reverse electrochemical synthesis of Ag-TiO2 composites from deep eutectic solvents: Photocatalytic and antibacterial behaviour","authors":"Ionela-Cristina Petcu , Raluca Negrea , Ana T.S.C. Brandão , Cosmin Romanitan , Oana Brincoveanu , Nikolay Djourelov , Iuliana Mihalache , L. Monica Veca , Gabriela Isopencu , Carlos M. Pereira , Liana Anicai , Cristina Busuioc , Sabrina State (Rosoiu)","doi":"10.1016/j.apsadv.2025.100749","DOIUrl":"10.1016/j.apsadv.2025.100749","url":null,"abstract":"<div><div>This study presents an environmentally friendly approach for synthesis Ag-TiO<sub>2</sub> composite using pulsed reverse current (PRC) electrodeposition from green electrolytes, specifically deep eutectic solvents (DESs). The combination of PRC and DESs offers better control over nanoparticle synthesis while eliminating the need for toxic or expensive precursors, representing a significant advancement in sustainable nanomaterial synthesis. Different electrochemical parameters were adjusted, and their influence on the structure and morphology of the composite was investigated using X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), scanning electron microscopy (SEM) and transmission electron microscopy (TEM). TEM analysis revealed that silver nanoparticles (Ag NPs) are attached to TiO<sub>2</sub> nanopowder, with the coexistence of TiO<sub>2</sub> and Ag further confirmed by XRD and XPS. The recorded UV–Vis diffuse reflectance spectra (DRS) displayed a broad peak in the range of 400 – 650 nm, associated with the localized surface plasmon resonance (LSPR) of Ag NPs on the semiconductor’s surface. The photocatalytic activity of TiO<sub>2</sub> nanopowder and Ag-TiO<sub>2</sub> composite was evaluated based on the degradation of methyl orange (MO) dye under UV and visible light illumination. Our findings clearly demonstrated that the incorporation of Ag improved the photocatalytic efficiency. The mechanism of MO dye degradation was explored by using various scavengers, revealing that superoxide radicals (•<span><math><msubsup><mi>O</mi><mn>2</mn><mo>−</mo></msubsup></math></span>) play a dominant role. Furthermore, the incorporation of Ag NPs significantly enhanced the antimicrobial activity of the oxide against both Gram-positive (<em>B. subtilis</em>) and Gram-negative (<em>E.coli</em>) strains.</div></div>","PeriodicalId":34303,"journal":{"name":"Applied Surface Science Advances","volume":"27 ","pages":"Article 100749"},"PeriodicalIF":7.5,"publicationDate":"2025-04-21","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143851346","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
{"title":"Ultrafast laser nanostructuring and its application in electrochemical deposition of metal microstructures with high density and robust bonding strength","authors":"Jinlong Xu , Wanfei Ren , Aobo Zhang , Fuliang Wang , Jinkai Xu , Guodong Zhang , Guanghua Cheng","doi":"10.1016/j.apsadv.2025.100748","DOIUrl":"10.1016/j.apsadv.2025.100748","url":null,"abstract":"<div><div>Ultrafast laser direct writing technology, with its capacity to efficiently and conveniently induce micro-nano structures on material surfaces, has opened up new avenues for precision material processing and the preparation of functional devices. In this study, we investigate the potential application of laser nanostructuring for surface functionalization and therefore localized electrochemical deposition. The surface skin-layer nano-relief structures induced by ultrafast laser are demonstrated to provide localized field enhancement and create attachment sites for electrochemical reactions, thereby enabling equivalent parallel localized electrochemical deposition under standard plating conditions. Furthermore, these nano-relief structures form a unique interdigitating junction structure between the depositor and the substrate, significantly enhancing the bond strength between the depositor and the substrate. The shear test results indicating the bond strengths can be up to 100 MPa, significantly exceeding that of conventional localized electrochemical deposition techniques. With the incorporation of electrochemical additives, crystalline growth during electrochemical deposition is regulated, realizing efficient and controllable deposition of high-density copper microstructures. The hardness and elastic modulus of the deposited copper were tested to be 0.95 GPa and 67.99 GPa, respectively, approaching those of forged copper. For microstructure arrays on a centimeter scale, the electrodeposition time can be reduced from hundreds of hours to tens of minutes. This method is not only applicable to metallic conductive substrates but can also be extended to localized electrochemical deposition on semiconductor materials, offering promising prospects for the high-efficiency, high-performance, and practical manufacturing of metallic complex structured devices.</div></div>","PeriodicalId":34303,"journal":{"name":"Applied Surface Science Advances","volume":"27 ","pages":"Article 100748"},"PeriodicalIF":7.5,"publicationDate":"2025-04-18","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143843927","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
{"title":"Highly thermostable and visibly transparent Cu-thin-film planar heaters","authors":"Chankyoung Lee , Jaewoo Park , Dooho Choi","doi":"10.1016/j.apsadv.2025.100747","DOIUrl":"10.1016/j.apsadv.2025.100747","url":null,"abstract":"<div><div>Transparent heaters (THs) are widely used in applications such as deicing, defogging, and thermal management, requiring high transparency, low sheet resistance and structural durability. This study investigates the design, fabrication, and performance of ZnO/Cu/SiO₂ (ZCS) THs, with a particular focus on thermostability. By employing a dielectric/metal/dielectric configuration with Cu as the metallic layer, ZCS heaters offer a cost-effective alternative to indium tin oxide and Ag-based THs. The optimized ZCS structure, comprising ZnO (20 nm)/Cu (6 nm)/SiO₂ (80 nm), demonstrates exceptional performance, achieving high visible transparency (maximum of 94.8 % and average of 86.3 %), low sheet resistance (∼10 Ω/sq or less), and rapid thermal response. The heaters exhibit excellent stability during prolonged operation and repeated on-off cycling at elevated temperatures of ∼200 °C due to the planar structure of heating element. This remarkable thermostability far exceeds that of THs consisting of network-structured Cu nanowires, which fail at temperatures below 90 °C. Under bias voltage sweeping, the ZCS TH with an 8-nm-thick Cu layer undergoes gradual and irreversible structural degradation, beginning with localized void formation and progressing to full-scale solid-state dewetting and agglomeration of Cu layer, ultimately failing at ∼ 330 °C. These findings establish ZCS heaters as versatile and cost-efficient alternatives for high-performance transparent heating in demanding environments and present a pathway for further structural enhancement.</div></div>","PeriodicalId":34303,"journal":{"name":"Applied Surface Science Advances","volume":"27 ","pages":"Article 100747"},"PeriodicalIF":7.5,"publicationDate":"2025-04-15","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143828764","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Kun Woong Lee , Dong Su Kim , Su Yeon Jung , Joohoon Kang , Hyung Koun Cho
{"title":"Oxygen network formation for efficient charge transport and durable BiVO4 photoanodes with ultra-thin TiO2 layer in solar water splitting","authors":"Kun Woong Lee , Dong Su Kim , Su Yeon Jung , Joohoon Kang , Hyung Koun Cho","doi":"10.1016/j.apsadv.2025.100737","DOIUrl":"10.1016/j.apsadv.2025.100737","url":null,"abstract":"<div><div>Bismuth vanadate (BiVO<sub>4</sub>) has emerged as a prominent oxide semiconductor in solar water splitting investigations owing to facile synthesis and favorable band-alignment with the water oxidation level. Oxygen and oxygen vacancies (V<sub>O</sub>) within the BiVO<sub>4</sub> exhibit multifaceted roles across bulk, surface, and interface. This study presents a method for selectively regulating the surface and bulk V<sub>O</sub> in BiVO<sub>4</sub> through facile chemical redox reactions. A large amount of V<sub>O</sub> on the BiVO<sub>4</sub> surface enables the formation of a robust networking interface with oxide-based protection overlayers, whereas V<sub>O</sub> in bulk region must be effectively suppressed. A significant amount of V<sub>O</sub> can be specifically formed on the BiVO<sub>4</sub> surface via a controlled surface chemical reduction reaction (SCR) at the atomic level, precisely controlling the presence of O<sup>2-</sup> and OH<sup>-</sup> ions. Here, we quantitatively and qualitatively analyze V<sub>O</sub> changes and the impact of V<sub>O</sub> on photoelectrochemical operation. As a result, The SCR process allows for the strategic control of the BiVO<sub>4</sub> surface into a V<sub>O</sub>-rich surface. The controlled surface enhances the charge kinetic by promoting the conformal coating of a n-TiO<sub>2</sub> protective layer and decreasing the charge loss in the interface junction with ensuring stability. Furthermore, the SCR-BiVO<sub>4</sub>/TiO<sub>2</sub>/CoPi photoanodes exhibit a highly stable photocurrent density of 3.9 mA cm<sup>−2</sup> at 1.23 V<sub>RHE</sub>. Surface modification and understanding of the oxygen-end network can be broadly applied to photoelectrodes that require oxide-based overlays.</div></div>","PeriodicalId":34303,"journal":{"name":"Applied Surface Science Advances","volume":"27 ","pages":"Article 100737"},"PeriodicalIF":7.5,"publicationDate":"2025-04-11","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143816614","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
{"title":"A current review of TiO2 thin films: synthesis and modification effect to the mechanism and photocatalytic activity","authors":"D’ April Sabriantie Mulus , Muhamad Diki Permana , Yusi Deawati , Diana Rakhmawaty Eddy","doi":"10.1016/j.apsadv.2025.100746","DOIUrl":"10.1016/j.apsadv.2025.100746","url":null,"abstract":"<div><div>Photocatalysts in the form of thin films such as TiO<sub>2</sub> show great potential for various applications due to their ease of separation after use and their diverse synthesis processes. However, pure TiO<sub>2</sub> has some intrinsic limitations, such as a wide bandgap (∼3.2 eV) which lowers its visible-light absorption and fast recombination of electrons and holes. Thus, it is necessary to modify TiO<sub>2</sub> thin film to increase its photocatalysis efficiency and overcome these problems. This review examines reports over the past 10 years on TiO<sub>2</sub> thin-film modification strategies using metal and non-metal modifiers with detailed possible mechanisms of modified TiO<sub>2</sub> thin-film including optical modification and heterostructure formation. Recent advancements indicate that modifications can reduce the band gap 0.14–0.85 eV lower compared to pure TiO<sub>2</sub> and several modified photocatalysts can degrade >90 % of pollutant molecules. This review also highlights the effect of synthesis methods such as sol-gel, hydrothermal, magnetron sputtering, atomic layer, and chemical vapor deposition on the film properties. The different methods lead to different properties including morphology, defects, optical properties, crystal structure, and roughness. This review aims to provide a comprehensive understanding of synthesis methods, mechanisms, and performance enhancements, offering insights into the future design of high-efficiency TiO<sub>2</sub> thin film-based photocatalysts.</div></div>","PeriodicalId":34303,"journal":{"name":"Applied Surface Science Advances","volume":"27 ","pages":"Article 100746"},"PeriodicalIF":7.5,"publicationDate":"2025-04-11","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143816616","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Bartosz Zawadzki, Marta Valaskova, Alexandr Martaus, Jiri Pavlovsky, Kamila Koci
{"title":"Effect of sodium doping in NiO/Vermiculite composite on photocatalytic hydrogen production from methanol-water decomposition","authors":"Bartosz Zawadzki, Marta Valaskova, Alexandr Martaus, Jiri Pavlovsky, Kamila Koci","doi":"10.1016/j.apsadv.2025.100745","DOIUrl":"10.1016/j.apsadv.2025.100745","url":null,"abstract":"<div><div>This study investigates the efficiency of sodium-doped NiO/vermiculite (Vm) composites as photocatalysts for hydrogen production via methanol-water decomposition under UV irradiation. Using natural vermiculite as a support, NiO was introduced as a p-type semiconductor, and sodium doping was achieved using sodium hydroxide (NaOH) or sodium nitrate (NaNO<sub>3</sub>). Three synthesis methods - dry synthesis by milling, capillary impregnation, and wet impregnation were investigated for their influence on the structural, textural, optical, and electrical properties and the photocatalytic activity. Characterization techniques, including X-ray fluorescence, X-ray diffraction, atomic absorption spectrometry, photoluminescence, scanning electron microscopy with energy dispersive X-ray spectroscopy confirmed successful incorporation of NiO and sodium into the vermiculite matrix. Photocatalytic tests demonstrated that sodium doping enhances the stability and activity of the photocatalysts by reducing electron-hole recombination rates, with NaOH proving to be a more effective sodium source than NaNO<sub>3</sub>. Among the samples, those synthesized via capillary impregnation (NiO(OH)/Vm-C) and dry synthesis (NiO(OH)/Vm-M) showed the highest hydrogen yields (550 and 540 μmol/g cat., respectively) due to optimal crystallite size (∼22–23 nm) and defect-induced charge transfer efficiency. This is the first study to systematically investigate the role of sodium doping in NiO/clay-based photocatalysts and to reveal clear structure–property–activity correlations based on synthesis method and dopant type. The findings highlight the potential of Na-doped NiO/Vm composites as cost-effective and scalable photocatalysts for hydrogen production. The insights gained here lay the foundation for further development of layered, clay-supported photocatalysts beyond conventional oxide systems.</div></div>","PeriodicalId":34303,"journal":{"name":"Applied Surface Science Advances","volume":"27 ","pages":"Article 100745"},"PeriodicalIF":7.5,"publicationDate":"2025-04-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143808802","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}