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MgO and Mg(OH)2 thin films prepared by the SILAR method and their CO2 photocatalytic performance

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Abstract

CO2 photoconversion to solar fuels requires materials with a high affinity to the acidic CO2, and MgO and Mg(OH)2 films represent good candidates due to their basic sites are highly active for CO2 capture in a wide interval of temperatures. However, the deposition of MgO and Mg(OH)2 as thin film is difficult to obtain by traditional methods. As an alternative, in this work, the successive ionic layer adsorption and reaction (SILAR) method is proposed to obtain MgO/Mg(OH)2 mixtures over glass substrates at significantly lower temperatures (200–400 °C). The films were tested as photocatalysts in the CO2 photoconversion to solar fuels (HCOOH and CH3OH) under UV–visible-NIR irradiation. The as-prepared films exhibited the hexagonal structure of the Mg(OH)2 phase. As the temperature increased, XRD and XPS analysis confirmed the presence of orthorhombic MgO, while the morphology remains with similar grains with an estimated size of 1 µm. The annealing temperatures change the chemical species (Mg–O, Mg–OH, and Mg–CO3) on the films affected their photocatalytic activity. The films exhibited high affinity for CO2 due to the presence of defects (F and F+ centers) in both phases. The photocatalytic behavior was directly related to OH species present in each sample. According to the results, it seems that fewer hydroxides and defects on the films favored higher efficiencies for the CO2 photoconversion. In addition, the films were exposed to accelerated weathering tests to evaluate their efficiency for more extended periods. The results indicated that the aged films still have activity for CO2 photoconversion.

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References

  1. Güneya H, İskenderoğlu D (2018) Synthesis of MgO thin films grown by SILAR technique. Ceram Int 44(7788):7793

    Google Scholar 

  2. Feng H, Shiyong Wu, Huang S, Youqing Wu, Gao J (2015) Regenerable magnesium-based sorbent for high-pressure and moderate-temperature CO2 capture: physicochemical structures and capture performances. Fuel 159(559):569

    Google Scholar 

  3. Kato K, Omoto H, Takamatsu A, Tomioka T (2011) Crystal growth of MgO thin films deposited on ZnO underlayers by magnetron sputtering. J Cryst Growth 333(59):65

    Google Scholar 

  4. Cáceres D, Vergara I, González R (2003) Microstructural characterization of MgO thin films grown by radio-frequency sputtering. Target and substrate-temperature effect. J Appl Phys 93(4300):4305

    Google Scholar 

  5. Li M, Wang X, Li H, Di H, Xiaoguo Wu, Fang C, Yan B (2013) Preparation of photoluminescent single crystalline MgO nanobelts by DC arc plasma jet CVD. Appl Surf Sci 274(188):194

    Google Scholar 

  6. Suárez-Campos G, Cabrera-German D, García-Valenzuela JA, Cota-Leal M, Fuentes-Ríos JL, Martínez-Gil M, Hu H, Sotelo-Lerma M (2019) Controlled synthesis of Mg(OH)2 thin films by chemical solution deposition and their thermal transformation to MgO thin films. Ceram Int 45(10356):10363

    Google Scholar 

  7. Garza-Hernández R, Lugo-Loredo S, Aguirre-Tostado FS (2020) The role of copper during the growth of stoichiometric Cu2ZnSnS4 by successive ionic layer adsorption and reaction method. Ceram Int 46(5185):5192

    Google Scholar 

  8. Arora S (2020) ZnO/MgO/ITO structured thin film transistor for ultraviolet photo detector application. Mater Today Proc 30(150):152

    Google Scholar 

  9. Khaleel WA, Sadeq SA, Alani IAM, Ahmed MHM (2019) Magnesium oxide (MgO) thin film as saturable absorber for passively mode locked erbium-doped fiber laser. Opt Laser Technol 115(331):336

    Google Scholar 

  10. Taşer A, Güldüre ME, Güney H (2021) Fe doping effects in MgO thin films grown with SILAR technique. Mater Chem Phys 272:124993

    Article  Google Scholar 

  11. Taşer A, Güldüre ME, Güney H (2021) Tuning PL emission energy and bandgap with Ni dopant of MgO thin films. Ceram Int 47(15792):15800

    Google Scholar 

  12. Alfaro Cruz MR, Garza-Hernández R, Horley PP, Mata-Ramírez J, Martínez-G E, Aguirre-Tostado FS (2018) Low temperature ZnO films grown by successive ionic layer adsorption and reaction method. Thin Solid Films 663(49):55

    Google Scholar 

  13. Nicolau YF (1985) Solution deposition of thin solid compound films by a successive ionic layer absorption and reaction process. Appl Surf Sci 22(1061):1074

    Google Scholar 

  14. Zheng Y, Cao L, Xing G, Bai Z, Huang J, Zhang Z (2019) Microscale flower-like magnesium oxide for highly efficient photocatalytic degradation of organic dyes in aqueous solution. RSC Adv 9:7338

    Article  CAS  Google Scholar 

  15. Mageshwari K, Sathyamoorthy R (2012) Studies on photocatalytic performance of MgO nanoparticles prepared by wet chemical method. Trans Indian Inst Met 65(49):55

    Google Scholar 

  16. Akbari S, Moussavi G, Giannakis S (2021) Efficient photocatalytic degradation of ciprofloxacin under UVA-LED, using S, N-doped MgO nanoparticles: synthesis, parametrization and mechanistic interpretation. J Mol Liq 324:114831

    Article  CAS  Google Scholar 

  17. Chang X, Wang T, Gong J (2016) CO2 photo-reduction: insights into CO2 activation and reaction on surfaces of photocatalysts. Energy Environ Sci 9(2177):2196

    Google Scholar 

  18. Mahmodi G, Sharifnia S, Madani M, Vatanpour V (2013) Photoreduction of carbon dioxide in the presence of H2, H2O and CH4 over TiO2 and ZnO photocatalysts. Sol Energy 97(186):194

    Google Scholar 

  19. Habisreutinger SN, Schmidt-Mende L, Stolarczyk JK (2013) Photocatalytic reduction of CO2 on TiO2 and other semiconductors. Chem Int Ed 52(7372):7408

    Google Scholar 

  20. Yang C, Tan Q, Li Q, Zhou J, Fan J, Li B, Sun J, Lv K (2020) 2D/2D Ti3C2 Xene/g-C3N4 nanosheets heterojunction for high efficient CO2 reduction photocatalyst: dual effects of urea. Appl Catal 268:118738

    Article  CAS  Google Scholar 

  21. Li J, Li K, Tan Q, Li Q, Fan J, Chao Wu, Lv K (2022) Facile preparation of highly active CO2 reduction (001)TiO2/Ti3C2Tx photocatalyst from Ti3AlC2 with less fluorine. Catalysts 12:785

    Article  Google Scholar 

  22. Xiong X, Zhao Y, Shi R, Yin W, Zhao Y, Waterhouse GIN, Zhang T (2020) Selective photocatalytic CO2 reduction over Zn-based layered double hydroxides containing tri or tetravalent metals. Sci Bull 65:987–994

    Article  CAS  Google Scholar 

  23. Zhao Y, Chen G, Bian T, Zhou C, Waterhouse GIN, Li-Zhu Wu, Tung C-H, Smith LJ, O’Hare D, Zhang T (2015) Defect-rich ultrathin ZnAl-layered double hydroxide nanosheets for efficient photoreduction of CO2 to CO with water. Adv Mater 27:7824–7831

    Article  CAS  Google Scholar 

  24. Shuqi Wu, Wang J, Li Q, Huang Z, Rao Z, Zhou Y (2021) Bi/BiOCl nanosheets enriched with oxygen vacancies to enhance photocatalytic CO2 reduction. Trans Tianjin Univ 27:155–164

    Article  Google Scholar 

  25. An W, Tian L, Jinshan Hu, Liu Li, Cui W, Liang Y (2020) Efficient degradation of organic pollutants by catalytic ozonation and photocatalysis synergy system using double-functional MgO/g-C3N4 catalyst. Appl Surf Sci 534:147518

    Article  CAS  Google Scholar 

  26. ASTM International. Standard Guide to Charge Control and Charge Referencing Techniques in X-Ray Photoelectron Spectroscopy. Designation: E1523-15. https://www.astm.org/

  27. Wang L, Wei B, Dong P, Miao Q, Liu Z, Fubiao Xu, Jingjie Wu, Lou J, Vajtai R, Fei W (2016) Large-scale synthesis of few-layer graphene from magnesium and different carbon sources and its application in dye-sensitized solar cells. Mater Des 92(462):470

    Google Scholar 

  28. NIST X-ray photoelectron spectroscopy database. NIST Standard Reference Database 20, Version 4.1

  29. Chen M, Chen Y, Zhang W, Zhao S, Wang J, Mao J, Li W, Zhao Y, Huang N, Wan G (2016) Controlling the corrosion rate and behavior of biodegradable magnesium by a surface immobilized ultrathin 1-hydroxyethylidene-1,1-diphosphonic acid (HEDP) film. RSC Adv 6(15247):15259

    Google Scholar 

  30. Luévano-Hipólito E, Torres Martínez LM (2018) Mg(OH)2 films prepared by ink-jet printing and their photocatalytic activity in CO2 Reduction and H2O Conversion. Top Catal 61(1574):1584

    Google Scholar 

  31. Feliu S, Maffiotte C, Galván JC, Pardo A, Merino MC, Arrabal R (2011) The application of X-ray photoelectron spectroscopy in understanding corrosion mechanisms of magnesium and Mg–Al alloys. Open Surf Sci J 3(1):14

    Google Scholar 

  32. Zhang H, Cao T, Cheng Yi (2014) Synthesis of nanostructured MgO powders with photoluminescence by plasma-intensified pyrohydrolysis process of bischofite from brine. Green Process Synth 3(215):222

    Google Scholar 

  33. Latha Kumari WZ, Li CH, Vannoy RM, Leblanc DZW (2009) Synthesis, characterization and optical properties of Mg(OH)2 micro-/nanostructure and its conversion to MgO. Ceram Int 35(3355):3364

    Google Scholar 

  34. Yousefi S, Ghasemi B, Nikolova MP (2021) Opto-structural characterization of Mg(OH)2 and MgO nanostructures synthesized through a template-free sonochemical method. Appl Phys A 127:549

    Article  CAS  Google Scholar 

  35. Jacques J, Geoff T (2015) Defects at oxide surfaces. Springer, Cham

    Google Scholar 

  36. Wang K, Tao Wu, Congcong Wu, Rammohan Sriramdas Xu, Huang KW, Jiang Y, Liu H, Yan Y, Yang D, Ye T, Liu C, Xiaowen Hu, Jiang X, Priya S (2020) Nature of terrace edge states (TES) in lower dimensional halide perovskite. J Mater Chem A 8(7659):7670

    Google Scholar 

  37. Ki Young Kim (2010) Recent optical and photonic technologies. INTECH, Croatia, pp 450

  38. Nemade KR, Waghuley SA (2014) Synthesis of MgO nanoparticles by solvent mixed spray pyrolysis technique for optical investigation. Int J Met. https://doi.org/10.1155/2014/389416

    Article  Google Scholar 

  39. Habisreutinger SN, Schmidt-Mende L, Stolarczyk JK (2013) Photocatalytic reduction of CO2 on TiO2 and other semiconductors. Angew Chem Int Ed 52(7372):7408

    Google Scholar 

  40. Luévano-Hipólito E, Torres-Martínez LM (2022) CO2 photoreduction with H2O to C1 and C2 products over perovskite films of alkaline niobates ANbO3 (A = Li, Na, K). Fuel 320:123934

    Article  Google Scholar 

  41. Wang H, Cheng S, Cai X, Cheng L, Zhou R, Hou T, Li Y (2022) Photocatalytic CO2 reduction to HCOOH over core-shell Cu@Cu2O catalysts. Catal Commun 162:106372

    Article  CAS  Google Scholar 

  42. Henglein A, Gutiérrez M, Fischer C-H (1984) Photochemistry of colloidal metal sulfides 6. Kinetics of interfacial reactions at ZnS-particles. Ber Bunsenges Phys Chem 88(2):175

    Article  Google Scholar 

  43. Zhao X, Fan Y, Zhang W, Zhang X, Han D, Niu L, Ivaska A (2020) Nanoengineering construction of Cu2O nanowire arrays encapsulated with g-C3N4 as 3D spatial reticulation all-solid-state direct Zscheme photocatalysts for photocatalytic reduction of carbon dioxide. ACS Catal 10(6367):6376

    Google Scholar 

  44. Song H, Meng X, Wang S, Zhou W, Song S, Kako T, Ye J (2020) Selective photo-oxidation of methane to methanol with oxygen over dual-cocatalyst-modified titanium dioxide. ACS Catal 10(14318):14326

    Google Scholar 

  45. Yang C, Li Q, Xi Y, Lv K, Li M (2019) Enhanced visible-light photocatalytic CO2 reduction performance of Znln2S4 microspheres by using CeO2 as cocatalyst. Appl Surf Sci 464(388):395

    Google Scholar 

  46. Li K, Zhang S, Li Y, Fan J, Lv K (2021) MXenes as noble-metal-alternative co-catalysts in photocatalysis. Chin J Catal 42(1):14

    Article  CAS  Google Scholar 

  47. Li Y, Ren Z, Gu M, Duan Y, Zhang W, Lv K (2022) Synergistic effect of interstitial C doping and oxygen vacancies on the photoreactivity of TiO2 nanofibers towards CO2 reduction. Appl Catal B 317:121773

    Article  CAS  Google Scholar 

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Acknowledgements

The authors want to thank CONACYT for financial support for this research through the following projects: FC-2016-1725, Paradigmas y Fronteras de la Ciencia 320379, and Cátedras-CONACYT 363, and 1060. In addition, thanks are extended to the UANL for its financial support through the projects: PAYCIT: CE1771-21, IT1766-21, and 277-CE-2022. We also thank Dr. Alonso Concha Balderrama and M.C. Luis Gerardo Silva Vidaurri from CIMAV-Monterrey for his technical support in the XRD and XPS measurements.

Funding

Authors declare they have no financial interests. This work was supported by the following CONACYT projects: FC-2016-1725, Paradigmas y Fronteras de la Ciencia 320379, and Cátedras-CONACYT 363, and 1060. Also, UANL was supported part of the work with the projects: PAYCIT: CE1771-21, IT1766-21, 277-CE-2022.

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All authors contributed to the study conception and design of this work. MRAC and EL-H contributed to the conceptualization, methodology, investigation. MRAC, EL-H, and RG-H contributed to the writing—original draft, writing—review, and editing. While LMT-M contributed to the conceptualization, project administration, founding acquisition, resources, writing—review, and editing.

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Correspondence to Leticia M. Torres-Martínez.

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Cruz, M.R.A., Luévano-Hipólito, E., Garza-Hernández, R. et al. MgO and Mg(OH)2 thin films prepared by the SILAR method and their CO2 photocatalytic performance. J Mater Sci 57, 18739–18753 (2022). https://doi.org/10.1007/s10853-022-07837-x

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