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Currently, the development of highly active photocatalytic additives for self-cleaning cement materials is a topical direction of building materials science. Mixed transition metal oxides are one of the effective types of photocatalysts, because they have improved functional characteristics compared to monometallic compounds. The purpose of this study was to establish the effects of synthesis conditions on the structure parameters and photocatalytic activity of zinc-titanium layered double hydroxide (Zn-Ti LDH) with Zn2+/Ti4+ molar ratio of 2/1, as well as its calcination products in the form of zinc-titanium mixed metal oxides (Zn-Ti MMOs). It was found that the mixing temperature of solutions of precursor salts and precipitators, as well as the temperature of sediment aging, were the main synthesis parameters that had the greatest impact on the phase composition and crystallite size of layered double hydroxide.
The research results showed differences in the kinetics of photodestruction of methylene blue (MB) in solution under UV radiation in the presence of Zn-Ti layered double hydroxide and Zn-Ti mixed metal oxides. The photocatalytic process involving Zn-Ti MMOs, corresponding to a pseudo-first order reaction kinetic, proceeded in a diffusion mode with limiting step in the form of dye adsorption on the surface of photocatalyst. The photodegradation of MB in the presence of Zn-Ti LDH, which was more accurately described by a pseudo-second order model, occurred in a kinetic regime, where the photocatalytic reaction was the limiting stage.
Mixed metal oxides of zinc and titanium had significantly higher functional characteristics compared to their Zn-Ti LDH precursor. The calcination of Zn-Ti layered double hydroxide at 200–500 °C allowed to achieve the highest photocatalytic activity of Zn-Ti MMO, which was due to phase transformations occurring during thermal treatment. The decomposition of Zn-Ti LDH at 200–250 °C resulted in the formation of a crystalline phase of zinc oxide (ZnO), which had a hexagonal wurtzite crystal structure with the ability to effectively absorb radiation from almost the entire UV spectral region. The rise of the Zn-Ti LDH calcination temperature to 500 °C led to an increase in the crystallinity degree of ZnO.
The research results showed differences in the kinetics of photodestruction of methylene blue (MB) in solution under UV radiation in the presence of Zn-Ti layered double hydroxide and Zn-Ti mixed metal oxides. The photocatalytic process involving Zn-Ti MMOs, corresponding to a pseudo-first order reaction kinetic, proceeded in a diffusion mode with limiting step in the form of dye adsorption on the surface of photocatalyst. The photodegradation of MB in the presence of Zn-Ti LDH, which was more accurately described by a pseudo-second order model, occurred in a kinetic regime, where the photocatalytic reaction was the limiting stage.
Mixed metal oxides of zinc and titanium had significantly higher functional characteristics compared to their Zn-Ti LDH precursor. The calcination of Zn-Ti layered double hydroxide at 200–500 °C allowed to achieve the highest photocatalytic activity of Zn-Ti MMO, which was due to phase transformations occurring during thermal treatment. The decomposition of Zn-Ti LDH at 200–250 °C resulted in the formation of a crystalline phase of zinc oxide (ZnO), which had a hexagonal wurtzite crystal structure with the ability to effectively absorb radiation from almost the entire UV spectral region. The rise of the Zn-Ti LDH calcination temperature to 500 °C led to an increase in the crystallinity degree of ZnO.
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[9] Amor F., Baudys M., Racova Z., Scheinherrová L., Ingrisova L., Hajek P. Contribution of TiO2 and ZnO nanoparticles to the hydration of Portland cement and photocatalytic properties of High Performance Concrete. Case Studies in Construction Materials. 2022. 16. Art. no. e00965. https://doi.org/10.1016/j.cscm.2022.e00965
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[17] Peng D., Zhang Y. Engineering of mixed metal oxides photocatalysts derived from transition-metal-based layered double hydroxide towards selective oxidation of cyclohexane under visible light. Applied Catalysis A: General. 2023. 653. Art. no. 119067. https://doi.org/10.1016/j.apcata.2023.119067
[18] Jiménez A., Trujillano R., Rives V., Vicente M.A. Mixed–metal–oxide photocatalysts generated by high–temperature calcination of CaAlFe, hydrocalumite–LDHs prepared from an aluminum salt–cake. Catalysis Today. 2023. 423. Art. no. 114008. https://doi.org/10.1016/j.cattod.2023.01.015
[19] Boumeriame H., Da Silva E.S., Cherevan A.S. Layered double hydroxide (LDH)-based materials: A mini-review on strategies to improve the performance for photocatalytic water splitting. Journal of Energy Chemistry. 2022. 64. P. 406 – 431. https://doi.org/10.1016/j.jechem.2021.04.050
[20] Yang Z.Z., Zhang C., Zeng G.M., Tan X.F., Huang D.L., Zhou J.W., Fang Q.Z., Yang K.H., Wang H., Wei J., Nie K. State-of-the-art progress in the rational design of layered double hydroxide based photocatalysts for photocatalytic and photoelectrochemical H2/O2 production. Coordination Chemistry Reviews. 2021. 446. Art. no. 214103. https://doi.org/10.1016/j.ccr.2021.214103
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[22] Seftel E.M., Niarchos M., Vordos N., Nolan J.W., Mertens M., Mitropoulos A.Ch., Vansant E.F., Cool P. LDH and TiO2/LDH-type nanocomposite systems: A systematic study on structural characteristics. Microporous and Mesoporous Materials. 2015. 203. P. 208 – 215. https://doi.org/10.1016/j.micromeso.2014.10.029
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[24] Al-Aani H.M.S., Trandafir M.M., Fechete I., Leonat L.N., Badea M., Negrilă C., Popescu I., Florea M., Marcu, I.-C. Highly Active Transition Metal-Promoted CuCeMgAlO Mixed Oxide Catalysts Obtained from Multicationic LDH Precursors for the Total Oxidation of Methane. Catalysts. 2020. 10 (6). Art. no. 613. https://doi.org/10.3390/catal10060613
[25] Puscasu C.M., Seftel E.M., Mertens M., Cool P., Carja G. ZnTiLDH and the Derived Mixed Oxides as Mesoporous Nanoarchitectonics with Photocatalytic Capabilities. Journal of Inorganic and Organometallic Polymers and Materials. 2015. 25. P. 259 – 266. https://doi.org/10.1007/s10904-014-0132-y
[26] Sahu R.K., Mohanta B.S., Das N.N. Synthesis, characterization and photocatalytic activity of mixed oxides derived from ZnAlTi ternary layered double hydroxides. Journal of Physics and Chemistry of Solids. 2013. 74 (9). P. 1263 – 1270. https://doi.org/10.1016/j.jpcs.2013.04.002
[27] Bukhtiyarova M.V., Bulavchenko O.A., Bukhtiyarov A.V., Nuzhdin A.L., Bukhtiyarova G.A. Selective Hydrogenation of 5-Acetoxymethylfurfural over Cu-Based Catalysts in a Flow Reactor: Effect of Cu-Al Layered Double Hydroxides Synthesis Conditions on Catalytic Properties. Catalysts. 2022. 12 (8). Art. no. 878. https://doi.org/10.3390/catal12080878
[28] Bulyga D.V., Evstropiev S.K. Kinetics of adsorption and photocatalytic decomposition of a diazo dye by nanocomposite ZnO–MgO. Optics and Spectroscopy. 2022. 130 (9). P. 1176. https://doi.org/10.21883/eos.2022.09.54839.3617-22
[29] Syuleiman Sh.A., Yakushova N.D., Pronin I.A., Kaneva N.V., Bojinova A.S., Papazova K.I., Gancheva M.N., Dimitrov D.Tz., Averin I.A., Terukov E.I., Moshnikov V.A. Study of the photodegradation of brilliant green on mechanically activated powders of zinc oxide. Technical Physics. 2017. 62 (11). P. 1709 – 1713. https://doi.org/10.1134/S1063784217110287
[30] Man H., Wen C., Luo W., Bian J., Wang W., Li C. Simultaneous deSOx and deNOx of marine vessels flue gas on ZnO-CuO/rGO: Photocatalytic oxidation kinetics. Journal of Industrial and Engineering Chemistry. 2020. 92. P. 77 – 87. https://doi.org/10.1016/j.jiec.2020.08.022
[31] Fatimah I., Yahya A., Iqbal R.M., Tamyiz M., Doong R.-a., Sagadevan S., Oh W.-C. Enhanced Photocatalytic Activity of Zn-Al Layered Double Hydroxides for Methyl Violet and Peat Water Photooxidation. Nanomaterials. 2022. 12 (10). Art. no. 1650. https://doi.org/10.3390/nano12101650
[32] Irani M., Mohammadi T., Mohebbi S. Photocatalytic Degradation of Methylene Blue with ZnO Nanoparticles; a Joint Experimental and Theoretical Study. Journal of the Mexican Chemical Society. 2016. 60 (4). P. 218 – 225.
[33] Khamizov R.Kh. A Pseudo-Second Order Kinetic Equation for Sorption Processes. Russian Journal of Physical Chemistry A. 2020. 94 (1). P. 171 – 176. https://doi.org/10.1134/S0036024420010148
[2] Tayeh B.A., Akeed M.H., Qaidi S., Bakar B.H.A. Ultra-high-performance concrete: Impacts of steel fibre shape and content on flowability, compressive strength and modulus of rupture. Case Studies in Construction Materials. 2022. 17. Art. no. e01615. https://doi.org/10.1016/j.cscm.2022.e01615
[3] Klyuev S., Fediuk R., Ageeva M., Fomina E., Klyuev A., Shorstova E., Zolotareva S., Shchekina N., Shapovalova A., Sabitov L. Phase formation of mortar using technogenic fibrous materials. Case Studies in Construction Materials. 2022. 16. P. e01099.
[4] Nizina T.A., Balykov A.S., Korovkin D.I., Volodin V.V. Physical and mechanical properties of modified fine-grained fibre-reinforced concretes containing carbon nanostructures. International Journal of Nanotechnology. 2019. 16. P. 496 – 509. https://doi.org/10.1504/IJNT.2019.106621
[5] Fediuk R., Amran M., Klyuev S., Klyuev A. Increasing the performance of a fiber-reinforced concrete for protective facilities. Fibers. 2021. 9 (11). Art. no. 64. https://doi.org/10.3390/fib9110064
[6] Balykov A.S., Nizina T.A., Volodin S.V. Optimization of technological parameters for obtaining mineral additives based on calcined clays and carbonate rocks for cement systems. Nanotechnologies in Construction. 2022. 14 (2). P. 145 – 155. https://doi.org/10.15828/2075-8545-2022-14-2-145-155
[7] Klyuev S., Fediuk R., Ageeva M., Fomina E., Klyuev A., Shorstova E., Sabitov L., Radaykin O., Anciferov S., Kikalishvili D., de Azevedo Afonso R.G., Vatin N. Technogenic fiber wastes for optimizing concrete. Materials. 2022. 15 (14). P. 5058.
[8] Balykov A.S., Nizina T.A., Kyashkin V.M., Volodin S.V. Evaluation of the effectiveness of mineral additives in cement systems in the development of “core – shell” photocatalytic compositions. Nanotechnologies in Construction. 2022. 14 (5). P. 405 – 418. https://doi.org/10.15828/2075-8545-2022-14-5-405-418
[9] Amor F., Baudys M., Racova Z., Scheinherrová L., Ingrisova L., Hajek P. Contribution of TiO2 and ZnO nanoparticles to the hydration of Portland cement and photocatalytic properties of High Performance Concrete. Case Studies in Construction Materials. 2022. 16. Art. no. e00965. https://doi.org/10.1016/j.cscm.2022.e00965
[10] Balykov A.S., Nizina T.A., Kyashkin V.M., Chugunov D.B. Siliceous rocks as modifiers of structure of photocatalytic self-cleaning concrete. Impact assessment on phase composition of cement stone. Nanotechnologies in Construction. 2024. 16 (2). P. 158 – 169. https://doi.org/10.15828/2075-8545-2024-16-2-158-169
[11] Janczarek M., Klapiszewski Ł., Jędrzejczak P., Klapiszewska I., Ślosarczyk A., Jesionowski T. Progress of functionalized TiO2-based nanomaterials in the construction industry: A comprehensive review. Chemical Engineering Journal. 2022. 430 (3). Art. no. 132062. https://doi.org/10.1016/j.cej.2021.132062
[12] Yang L., Hakki A., Wang F., Macphee D.E. Photocatalyst efficiencies in concrete technology: The effect of photocatalyst placement. Applied Catalysis B: Environmental. 2018. 222. P. 200 – 208. https://doi.org/10.1016/j.apcatb.2017.10.013
[13] Amran M., Fediuk R., Klyuev S., Qader D.N. Sustainable development of basalt fiber-reinforced high-strength eco-friendly concrete with a modified composite binder. Case Studies in Construction Materials. 2022. 17. e01550.
[14] Klyuev S., Klyuev A., Fediuk R., Ageeva M., Fomina E., Amran M., Murali G. Fresh and mechanical properties of low-cement mortars for 3D printing. Construction and Building Materials. 2022. № 338. P. 127644. DOI:10.1016/j.conbuildmat.2022.127644
[15] Janani F.Z., Khiar H., Taoufik N., Elhalil A., Sadiq M., Puga A.V., Mansouri S., Barka N. ZnO–Al2O3–CeO2–Ce2O3 mixed metal oxides as a promising photocatalyst for methyl orange photocatalytic degradation. Materials Today Chemistry. 2021. 21. Art. no. 100495. https://doi.org/10.1016/j.mtchem.2021.100495
[16] Al Miad A., Saikat S.P., Alam Md.K., Hossain Md. S., Bahadur N.M., Ahmed S. Metal oxide-based photocatalysts for the efficient degradation of organic pollutants for a sustainable environment: a review. Nanoscale Advances. 2024. 6 (19). P. 4781 – 4803. https://doi.org/10.1039/d4na00517a
[17] Peng D., Zhang Y. Engineering of mixed metal oxides photocatalysts derived from transition-metal-based layered double hydroxide towards selective oxidation of cyclohexane under visible light. Applied Catalysis A: General. 2023. 653. Art. no. 119067. https://doi.org/10.1016/j.apcata.2023.119067
[18] Jiménez A., Trujillano R., Rives V., Vicente M.A. Mixed–metal–oxide photocatalysts generated by high–temperature calcination of CaAlFe, hydrocalumite–LDHs prepared from an aluminum salt–cake. Catalysis Today. 2023. 423. Art. no. 114008. https://doi.org/10.1016/j.cattod.2023.01.015
[19] Boumeriame H., Da Silva E.S., Cherevan A.S. Layered double hydroxide (LDH)-based materials: A mini-review on strategies to improve the performance for photocatalytic water splitting. Journal of Energy Chemistry. 2022. 64. P. 406 – 431. https://doi.org/10.1016/j.jechem.2021.04.050
[20] Yang Z.Z., Zhang C., Zeng G.M., Tan X.F., Huang D.L., Zhou J.W., Fang Q.Z., Yang K.H., Wang H., Wei J., Nie K. State-of-the-art progress in the rational design of layered double hydroxide based photocatalysts for photocatalytic and photoelectrochemical H2/O2 production. Coordination Chemistry Reviews. 2021. 446. Art. no. 214103. https://doi.org/10.1016/j.ccr.2021.214103
[21] Taoufik N., Sadiq M., Abdennouri M., Qourzal S., Khataee A., Sillanpää M., Barka N. Recent advances in the synthesis and environmental catalytic applications of layered double hydroxides-based materials for degradation of emerging pollutants through advanced oxidation processes. Materials Research Bulletin. 2022. 154. Art. no. 111924. https://doi.org/10.1016/j.materresbull.2022.111924
[22] Seftel E.M., Niarchos M., Vordos N., Nolan J.W., Mertens M., Mitropoulos A.Ch., Vansant E.F., Cool P. LDH and TiO2/LDH-type nanocomposite systems: A systematic study on structural characteristics. Microporous and Mesoporous Materials. 2015. 203. P. 208 – 215. https://doi.org/10.1016/j.micromeso.2014.10.029
[23] Ludvíková J., Jirátová K., Kovanda F. Mixed oxides of transition metals as catalysts for total ethanol oxidation. Chemical Papers. 2012. 66 (6). P. 589 – 597. https://doi.org/10.2478/s11696-011-0127-x
[24] Al-Aani H.M.S., Trandafir M.M., Fechete I., Leonat L.N., Badea M., Negrilă C., Popescu I., Florea M., Marcu, I.-C. Highly Active Transition Metal-Promoted CuCeMgAlO Mixed Oxide Catalysts Obtained from Multicationic LDH Precursors for the Total Oxidation of Methane. Catalysts. 2020. 10 (6). Art. no. 613. https://doi.org/10.3390/catal10060613
[25] Puscasu C.M., Seftel E.M., Mertens M., Cool P., Carja G. ZnTiLDH and the Derived Mixed Oxides as Mesoporous Nanoarchitectonics with Photocatalytic Capabilities. Journal of Inorganic and Organometallic Polymers and Materials. 2015. 25. P. 259 – 266. https://doi.org/10.1007/s10904-014-0132-y
[26] Sahu R.K., Mohanta B.S., Das N.N. Synthesis, characterization and photocatalytic activity of mixed oxides derived from ZnAlTi ternary layered double hydroxides. Journal of Physics and Chemistry of Solids. 2013. 74 (9). P. 1263 – 1270. https://doi.org/10.1016/j.jpcs.2013.04.002
[27] Bukhtiyarova M.V., Bulavchenko O.A., Bukhtiyarov A.V., Nuzhdin A.L., Bukhtiyarova G.A. Selective Hydrogenation of 5-Acetoxymethylfurfural over Cu-Based Catalysts in a Flow Reactor: Effect of Cu-Al Layered Double Hydroxides Synthesis Conditions on Catalytic Properties. Catalysts. 2022. 12 (8). Art. no. 878. https://doi.org/10.3390/catal12080878
[28] Bulyga D.V., Evstropiev S.K. Kinetics of adsorption and photocatalytic decomposition of a diazo dye by nanocomposite ZnO–MgO. Optics and Spectroscopy. 2022. 130 (9). P. 1176. https://doi.org/10.21883/eos.2022.09.54839.3617-22
[29] Syuleiman Sh.A., Yakushova N.D., Pronin I.A., Kaneva N.V., Bojinova A.S., Papazova K.I., Gancheva M.N., Dimitrov D.Tz., Averin I.A., Terukov E.I., Moshnikov V.A. Study of the photodegradation of brilliant green on mechanically activated powders of zinc oxide. Technical Physics. 2017. 62 (11). P. 1709 – 1713. https://doi.org/10.1134/S1063784217110287
[30] Man H., Wen C., Luo W., Bian J., Wang W., Li C. Simultaneous deSOx and deNOx of marine vessels flue gas on ZnO-CuO/rGO: Photocatalytic oxidation kinetics. Journal of Industrial and Engineering Chemistry. 2020. 92. P. 77 – 87. https://doi.org/10.1016/j.jiec.2020.08.022
[31] Fatimah I., Yahya A., Iqbal R.M., Tamyiz M., Doong R.-a., Sagadevan S., Oh W.-C. Enhanced Photocatalytic Activity of Zn-Al Layered Double Hydroxides for Methyl Violet and Peat Water Photooxidation. Nanomaterials. 2022. 12 (10). Art. no. 1650. https://doi.org/10.3390/nano12101650
[32] Irani M., Mohammadi T., Mohebbi S. Photocatalytic Degradation of Methylene Blue with ZnO Nanoparticles; a Joint Experimental and Theoretical Study. Journal of the Mexican Chemical Society. 2016. 60 (4). P. 218 – 225.
[33] Khamizov R.Kh. A Pseudo-Second Order Kinetic Equation for Sorption Processes. Russian Journal of Physical Chemistry A. 2020. 94 (1). P. 171 – 176. https://doi.org/10.1134/S0036024420010148
Balykov A.S., Nizina T.A., Chugunov D.B., Davydova N.S., Kyashkin V.M. Photocatalysts based on Zn-Ti layered double hydroxide and its calcination products for self-cleaning concretes: Structure formation and photocatalytic activity. Construction Materials and Products. 2025. 8 (1). 2. https://doi.org/10.58224/2618-7183-2025-8-1-2