Highly efficient photocatalytic degradation of organic polluants over Cu 2 AlSnS 4 (CATS) thin films: synthesis, chracterization and photocataysis Approch

Highly efficient photocatalytic degradation of organic polluants over Cu 2 AlSnS 4 (CATS) thin films: synthesis, chracterization and photocataysis Approch | Research Square window.SnipcartSettings = { analytics: { enabled: false } }; (function() { var accessVector = localStorage.getItem('access_vector') || ''; window.dataLayer = window.dataLayer || []; if (accessVector) { window.dataLayer.push({ user: { profile: { profileInfo: { snid: accessVector } } } }); } })(); (function(w,d,s,l,i){w[l]=w[l]||[];w[l].push({'gtm.start':new Date().getTime(),event:'gtm.js'});var f=d.getElementsByTagName(s)[0],j=d.createElement(s),dl=l!='dataLayer'?'&l='+l:'';j.async=true;j.src='https://www.googletagmanager.com/gtm.js?id='+i+dl;f.parentNode.insertBefore(j,f);})(window,document,'script','dataLayer','GTM-K279D39R'); Browse Preprints In Review Journals COVID-19 Preprints AJE Video Bytes Research Tools Research Promotion AJE Professional Editing AJE Rubriq About Preprint Platform In Review Editorial Policies Our Team Advisory Board Help Center Sign In Submit a Preprint Cite Share Download PDF Research Article Highly efficient photocatalytic degradation of organic polluants over Cu 2 AlSnS 4 (CATS) thin films: synthesis, chracterization and photocataysis Approch A. Timoumi, N. El Guesmi, S. N. Alamri, O. H. Alsalmi, S. A. Ahmed This is a preprint; it has not been peer reviewed by a journal. https://doi.org/ 10.21203/rs.3.rs-2517839/v1 This work is licensed under a CC BY 4.0 License Status: Published Journal Publication published 01 Apr, 2023 Read the published version in Journal of Inorganic and Organometallic Polymers and Materials → Version 1 posted 7 You are reading this latest preprint version Abstract Cu 2 AlSnS 4 (CATS) was generated through directly fusing of extremely pure elements. Powder show a tetragonal crystal system belongs to the space group Fd3m and the CATS film displays narrow and weak diffraction peaks corresponding to the CZTS structure of pure kesterite without secondary phase. The surface appearance and chemical content films exposed their homogenous character. The optical analysis displayed good visible-range optical absorption and optical direct band gap of 1.30–1.65 eV with excellent transmission. CATS showed high photocatalytic efficacy to degrade methylene blue ( MB ) completely under UV-light irradiation. These results will open the opportunity for using this new material as talented candidate in solar cells and removing organic pollutants from aqueous solutions. Cu2AlSnS4 thin films inorganic materials catalysis vapor deposition Figures Figure 1 Figure 2 Figure 3 Figure 4 Figure 5 Figure 6 Figure 7 Figure 8 Figure 9 Figure 10 Figure 11 Figure 12 Figure 13 Figure 14 1. Introduction Considering the richness of its components on earth, inexpensive and non-toxic, Cu 2 ZnSnS 4 (CZTS) compound has conventional the greatest courtesy in investigations. In general, the quaternary semiconductor compound Cu 2 ZnSnS 4 [ 1 ] has emerged as one of the most promising contenders, thanks to its p-type conductivity, good optoelectronic capabilities, non-toxicity, and availability of all its constituent elements in the earth's crust [ 2 , 3 ]. Having a direct gap energy of 1.4 to 1.5 eV and a high absorption coefficient (10 4 cm − 1 ), CZTS constitute an appropriate material for the conversion of solar energy [ 4 , 5 ]. Interestingly, solar cells made from CZTS conversion efficiency expanded from 2.3% in 1997 to 11.1% in 2012 [ 6 ]. Therefore, investigation of new materials that resemble CZTS-like Cu 2 AlSnS 4 in terms of structure (CZTS) are highly recommended. It is worth mentioning that there are two physical characteristics of CZTS that exhibit excellent optical parameters with tunable direct bandgap energy as well as high absorption coefficient. Because of these unique characteristics, CATS represents a serious candidate and can be exploitable as an absorber layer in inexpensive solar cells. The synthesis of such quaternary compounds have been adopted using a various range of techniques [ 9 – 14 ]. From the above-mentioned techniques, each technique has advantages and limitations as well. Vacuum thermal evaporation has acquired the most affection of these techniques due to a large variety of factors into consideration. Thus, it is a practical way to deposit a wide range of thin layers. In addition, compared to the procedures mentioned above, which are typically convoluted and time-consuming, is supposed of as a straightforward, reasonable, and environmentally friendly methodology. Quaternary Cu 2 XSnS 4 (X = Ni , Zn , Fe ,… etc.) compound have, nevertheless, been found to be deposited [ 15 , 16 ]. Based on previous [ 17 – 20 ] work and in continuation of our research interest, the present study is carried out to establish firstly an exclusive physical synthesis of new CATS quaternary compound using direct fusion process. After that exploiting the vacuum deposition technique for obtaining thin films, that exhibits a noticeable change in physical properties as a result of the substrate temperature. However, as far as we are aware, no research has been centered on the structural, morphological, optical of CATS thin films as well their photocatalytic activities. Thus, the aim of the present research work is to study the synthesis and the consequences of growth temperature on the morphological, the structural, and the optical characteristics of CATS-based thin layers as well their photocatalytic degradation efficacy toward organic pollutant in particular aqueous methylene blue (MB) solution exposed to UV light. 2. Experimental Strategies 2.1. Cu 2 AlSnS 4 powder Synthesis: The 99.999% pure elements copper (Cu), aluminum (Al), tin (Sn), and sulfur were combined in stoichiometric quantities to form the quaternary Cu 2 AlSnS 4 material. A quartz tube was used to seal the mixture while operating at a high vacuum of 10 − 4 Torr. The tube is placed within a horizontal furnace of the Nabertherm (B 180) design with the arrangement of the tube being horizontal. The quartz tube was progressively heated (100°C/h) to a temperature of 1100°C in order to prevent explosions caused by sulfur vapor pressure. By maintaining the melt at 1100°C for roughly 4 hours to make good element interdiffusion, a complete homogeneity could be attained. The obtained material was then appropriately crystallized by admitting the tube to innately cool to ambient temperature. This procedure has given the desired synthesized material a black ingot-shaped substance. The ingot is then ground into a fine powder that is utilized as the basic material for creating thin films for thermal evaporation. The schematic of thermal profile adopted for the synthesis, the CATS ingot and the powder are portrayed in Fig. 1 . 2.2. Thin film preparation: Cu 2 AlSnS 4 powder was expended to create evaporated thin films (Fig. 2 ). The huge radiant-heat loads and lack of vacuum materials and procedures that could tolerate the heat, predominantly in a demountable system, hindered its development. A graphite made crucible holds the CATS powder that has been crushed. The use of thermal evaporation sources, which allow us to control the powder, has been carried out. Prior to deposition, the chamber was evacuated to a pressure of less than 10 − 6 Torr. Approximately 15 centimetres alienated the substrate from the crucible. The temperature of the crucible was retained to control the thermal evaporation sources. The substrates were maintained at four different temperatures, ranging from 25°C, 100°C, 200°C, and 300°C. To produce the same film thicknesses, the bulk of the added powder, which weighs approximately 0.2 g, was left unchanged. The films thicknesses found to be between 500 and 600 nm. 2.3. Thin film characterizations: The crystalline film structure was examined by X-ray diffraction using (Shimadzu XRD-6000 X-ray diffractometer supplied with a Cu-K radiation source of 1.5418 Å). AFM using a Veeco CP-II in contact mode with Si tips with a 1 Hz scan rate, was exploited to analyze the thin-film surface morphology while scanning-electron microscopy (SEM, Shimadzu Superscan SSX-550) was employed to study EDS analysis. The homogenous as-grown films adhered adequately to the substrate glass surface and had no pinholes or crashes on their surface. At normal incidence and room temperature, the optical transmittance T (λ) and reflectance R (λ) spectra over the wavelength range of 200–2500 nm were measured with a 0.1 nm resolution (Shimadzu Solid Spec-3700 UV-visible spectrophotometer with an integrating sphere). The thickness of the film layer was assessed using stylus displacement (Veeco Dektak 150 profilometer). 2.4. Analysis of Photocatalytic Activity: The photocatalytic degradation efficacy of prepared Cu 2 AlSnS 4 was evaluated using MB in aqueous solution. The photocatalytic activity of the prepared photocatalyst Cu 2 AlSnS 4 was assessed by monitoring the degradation of (MB) pollutants throws decreasing its absorption. MB stock solution was prepared by dissolving it in distilled water at ~ 7 mg/L (2x10 − 5 mol/L) ~ 14 mg/L (4x10 − 5 mol/L) and into a 2 L volumetric flask. Then, different mass (15 mg, 25 mg and 50 mg) of Cu 2 AlSnS 4 photocatalysts (each in a separate experiment) were added into a photoreactor comprising 370 mL of MB solution (Fig. 3 ). The solutions were stirred with a magnetic stirrer in a dark environment for 30 min to ensure the adsorption/desorption equilibrium of MB on these photocatalysts. Then, the mixture was exposed to UV irradiation provided by a 125W UV -lamp vertically within the 500 ml intended photochemical reactor (Fig. 3 ). The solution's UV-vis absorption spectrum was found to be between 200 and 1000 nm using double-beam Shimadzu 1800 UV-VIS-NIR spectrophotometer. Eight samples were collected following UV radiation at predetermined intervals of 30 min, and their absorption spectra were recorded from its decreasing in absorption intensity corresponding to the progress of the photocatalytic degradation of MB indicator at the characteristic wavelength λ max = 664 nm. 3. Results And Discussion 3.1 Identification of the structure: The X-ray diffraction patterns of the pure CATS powder are displayed in Fig. 4 . The sample, according to the JCPDS (card No. 00-047-1343), is well crystalline. It shows twelve clearly defined XRD peaks that match the card's associated peaks. Because there are no further other phases, all of the sample's peaks are tetragonal in nature. The crystal structure's XRD patterns of CATS thin films was obtained using (Card JCPS, code 00-027-0980) as presented in Fig. 5 . At temperatures of 25, 100, and 200 degrees Celsius, one peak that correspond to the (111) orientations of CATS thin layers appear on the X-ray diffractogram at the angle of (2θ = 30°). However, at 300 degrees Celsius, two peaks that correspond to the (111) and (220) orientations of CATS thin layers appear on the X-ray diffractogram respectively at the angle of (2θ = 30°) and (2θ = 50°). No any other impurity phases were detected, specifying the stability of atoms at the substrate surface. Therefore, the deposition at 300°C increases crystallization and promotes the formation of further CATS kesterite peaks. 3.2 EDX analysis: Energy dispersive X-ray ( EDX ) analysis was employed to look into the samples' quantitative makeup. The outcomes of the sample's EDX of CATS powder elemental analysis are displayed in Fig. 6 . It has been confirmed that Cu, Al, Sn, and S are presented. At 2.4 keV, the sulphur (S) displays a higher intensity pic which represents the principle element. The findings of the CATS films numerous surface spots' EDX elemental analyses are shown in Fig. 7 . All samples have been found to include Cu , Al , Sn , and S . Due to the substrate being employed; a well-defined peak was seen in all films between 1.2 keV and 2 keV [ 21 ]. We may infer from the EDX analysis that each sample contains Cu , Al , Sn , and S . Thus, XRD analysis and atomic concentrations determined by EDX agree with the formula Cu 2 AlSnS 4 . 3.3 AFM analysis: Atomic force microscopy ( AFM ), was susscesfully used to assess the CATS films. In order to attain more surface data, contact AFM was implemented to evaluate the surface topography of CATS films (Fig. 8 ). All AFM micrographs had a same scan area. Based on the temperature of the substrate, the surfaces of the films have noticeably varying morphologies and roughness. The lengthened shape befitted more sphere-like at high substrate temperatures. Grain agglomeration, which results in irregular particle morphologies, is produced on by rising temperature. For films, the root mean square ( rms ) surface roughness was determined to be ranged between 13 to 24 nm. A higher substrate temperature may cause smaller crystals to fuse together which led to increasing roughness. As a result of AFM investigation, it has been determined that as temperature rises, CZTS film surface roughness and particle size both increase [ 22 ]. 3.4 UV-Visible spectroscopy analysis: The photon-matter interaction measurements were used to record the transmittance and the reflectance spectra with regard to the 200–2500 nm wavelength range (Fig. 9 ). Around 370 nm, all films transmittances began to decline. All films can block damaging UV radiation. The uniformity of the grains and variations in their height on the films surface have an impact on transmittance. However, as the surface roughness decreases, the transmittance significantly rises. Calculating the optical energy bandgap involves using Tauc's relationship (Eq. 1) [ 23 , 24 ]: (αhν) m = B (hν-Eg) (1) Where m defines whether an optical transition occurs directly or indirectly, α is the absorption coefficient, B is the constant, and hv is the incident photon energy. To evaluate the bandgap, plotting of (αhν) 2 vs photon energy (hν) is done (Fig. 10 ). Energy of the obtained band gap ranged from 1.65 eV to 1.30 eV. The direct bandgap energy of the CATS reaches 1.30 eV for 300° C as the substrate temperature rises. 3.5. Photocatalytic Activity: Figure 11 recording the photocatalytic degradation of MB by CATS after UV-light irradiation. It is noticeable that for UV-light irradiation, the absorbance intensity of the MB absorption peak (664 nm) progressively decreased in all samples. All samples demonstrated a stable adsorption-desorption equilibrium in MB solution for the first 30 min (dark adsorption test). The degradation of MB with a concentration of 2x10 − 5 M under UV-light was observed about 70%, 94%, 96% and 98% after 4 h when using different amounts of the catalyst CATS dosages of 40, 65, 95 and 130 mg/L, respectively (Fig. 11 ). Thus, a more pronounced decrease (of more than 90%) in the MB major absorption peak intensity was monitored using catalyst dosages ≥ 65 mg/L in UV-light. This indicates that Cu 2 AlSnS 4 represent an appropriate and efficient candidate for the photocatalytic degradation of MB dye. Additionally, to improve the experimental setup for the optimum photocatalytic efficiency of the Cu 2 AlSnS 4 , an efficient study was achieved to find the optimum CATS and MB concentrations for samples with excellent performance. Thus, for comparison, we investigated additionally the photocatalytic degradation of 4x10 − 5 M concentration of MB . A degradation of MB of 38%, 34% over 4 h was observed for a catalyst CATS dosages of 65 and 130 mg/L, respectively (Fig. 12 ). Consequently, and from the above results, the photocatalytic results when exposed to UV light in the presence of 65 mg/L of CATS showed a more rapid degradation of 2x10 − 5 M of MB (≈ 95%) as compared to other outcomes. On the other hand, under UV-irradiation for 240 minutes, the photodegradation of MB in the presence of photocatalyst CATS results in the transformation of nitrogen and sulfur atoms in MB molecules into inorganic ions and gasses. As reported, the mineralization and decomposition of MB were confirmed by the reduction of total organic carbon (TOC) followed by almost complete mineralization of carbon and of nitrogen and sulfur heteroatoms into CO 2 , ammonium NH 4 + , nitrate NO 3 − and sulfate SO 4 2− , respectively [ 25 , 26 ]. The C/C 0 vs degradation time plots are presented in Figs. 11 and 12 to provide a thorough understanding of the kinetic mechanism during the photocatalytic process. According to the results, the photodegradation progression proceeded gradually with irradiation time, with a much steeper decrease under UV-light irradiation for the CATS dosages of 65, 95 and 130 mg/L compared to that for 40 mg/L. The rate constants ( k ) for the degradation of MB were determined from the well-known rate constant equation ln (C/C 0 ) = k t and plotted in Figs. 13 and 14 to better illustrate the degradation rates. Figures 13 and 14 shows that the degradation of MB followed first order kinetics that illustrates by linear plots. The rate of degradation constants ( k ) were obtained from the slope of linear plot and are 5.03x10 − 3 , 1.24x10 − 2 , 1.38x10 − 2 and 1.63x10 − 2 min − 1 for different catalyst (CATS) dosages of 40, 65, 95 and 130 mg/L, respectively (Fig. 10 ) in the presence of 2x10 − 5 M of MB . While for 4x10 − 5 M of MB, k is 2.08x10 − 3 and 1.77x10 − 3 min − 1 for different catalyst (CATS) dosages of 65 and 130 mg/L, respectively (Fig. 13 ). The CATS displayed higher photocatalytic activity more than three times from a dosage of 65 mg/L under UV-light than a dosage of CATS of 40 mg/L. The achieved results remain interesting compared literature, in which the photocatalytic degradation of MB , under UV light irradiation using polymeric membranes impregnated with ZnO nanoparticles, such as cellulose acetate/Zinc oxide [ 26 ] poly(methylmethacrylate) (PMMA)/Zinc oxide [ 27 ] and Polyaniline/Zinc oxide [ 28 ] as catalysts exhibited 30%, 60% and 79% of dye degradation in 300 minute. However, remains inferior to the photocatalytic efficiency of TiO 2 /AC (Activated Carbon) in which almost complete degradation of MB (98%) was achieved within only 90 min UV-light irradiation [ 29 ]. As well AgNPs/TiO 2 /Ti 3 C 2 Tx MXene composites [ 30 ] as efficient catalysts with exclusive degradation efficacy as the majority of the previously described photocatalysts in comparable experimental setups. 4. Conclusions In this study, the direct melting of the component elements and the vacuum thermal evaporation method was successfully used for manufacture and deposit a novel CATS quaternary material. The structural, the morphological and the optical characteristics of the layers were evaluated at various substrate temperatures between 25°C and 300°C. The X-ray diffractograms for CATS thin films demonstrate that the optimal orientations along the layers deposited at 300°C (111) and (220) planes. An XRD investigation showed that as substrate temperature rises, crystallinity also rises. Additionally, the CATS thin films have have Eg values for direct transitions in the range of 1.30–1.65 eV, rough, dense, and compact surface. The photocatalytic degradation of methylene blue (MB), similar renowned pollutants dye using CATS as catalysts was evaluated under UV-light irradiation condition. Indeed, CATS under UV-light achieved maximum degradation of 8 % of aqueous MB solution in 120 min without any scavenger. The obtained results will help of active CATS catalysts for the mineralization and photodegradation of other organic pollutants. Declarations Acknowledgments The authors would like to thank the Deanship of Scientific Research at Umm Al-Qura University for supporting this work (22UQU4331172-DSR01). Conflict of Interest: The authors declare that they are no conflict of interest. References M. Rahman, M. Bashar, & N. Islam, Optical and Structural Study of the CZTS Thin Film for Solar Cell Derived from the Chloride-Based sol-gel Precursor Solution. Dhaka University Journal of Science, 70 (1) (2022) 1–7. Y.M. Zhang, Z.J. Jia, Z.Y. Zhao, Secondary phases in Cu 2 ZnSnS 4 thin film solar cell: The role of interfaces, Physica B: Condensed Matter, 626 (2022) 413539 . H. Katagiri, N. Ishigaki, T. Ishida, Jpn. J. Appl. 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Cite Share Download PDF Status: Published Journal Publication published 01 Apr, 2023 Read the published version in Journal of Inorganic and Organometallic Polymers and Materials → Version 1 posted Editorial decision: Major revision 30 Jan, 2023 Reviews received at journal 29 Jan, 2023 Reviewers agreed at journal 29 Jan, 2023 Reviewers invited by journal 28 Jan, 2023 Editor assigned by journal 28 Jan, 2023 Submission checks completed at journal 26 Jan, 2023 First submitted to journal 26 Jan, 2023 You are reading this latest preprint version Research Square lets you share your work early, gain feedback from the community, and start making changes to your manuscript prior to peer review in a journal. As a division of Research Square Company, we’re committed to making research communication faster, fairer, and more useful. We do this by developing innovative software and high quality services for the global research community. Our growing team is made up of researchers and industry professionals working together to solve the most critical problems facing scientific publishing. Also discoverable on Platform About Our Team In Review Editorial Policies Advisory Board Help Center Resources Author Services Accessibility API Access RSS feed Manage Cookie Preferences © Research Square 2026 | ISSN 2693-5015 (online) Privacy Policy Terms of Service Do Not Sell My Personal Information {"props":{"pageProps":{"initialData":{"identity":"rs-2517839","acceptedTermsAndConditions":true,"allowDirectSubmit":false,"archivedVersions":[],"articleType":"Research Article","associatedPublications":[],"authors":[{"id":171025880,"identity":"8295ae65-4934-4e78-935a-7da353a648e3","order_by":0,"name":"A. 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El Guesmi","email":"","orcid":"","institution":"","correspondingAuthor":false,"submittingAuthor":false,"prefix":"","firstName":"N.","middleName":"El","lastName":"Guesmi","suffix":""},{"id":171025882,"identity":"cc76c2ba-289e-484b-81e8-bcafdd376787","order_by":2,"name":"S. N. Alamri","email":"","orcid":"","institution":"Taiba University","correspondingAuthor":false,"submittingAuthor":false,"prefix":"","firstName":"S.","middleName":"N.","lastName":"Alamri","suffix":""},{"id":171025883,"identity":"4a910fe0-62ed-4950-9f38-86993575fcb0","order_by":3,"name":"O. H. Alsalmi","email":"","orcid":"","institution":"Umm AL-Qura University","correspondingAuthor":false,"submittingAuthor":false,"prefix":"","firstName":"O.","middleName":"H.","lastName":"Alsalmi","suffix":""},{"id":171025884,"identity":"bb1206da-cb4d-4f7b-aad6-d632e3cc1378","order_by":4,"name":"S. A. Ahmed","email":"","orcid":"","institution":"","correspondingAuthor":false,"submittingAuthor":false,"prefix":"","firstName":"S.","middleName":"A.","lastName":"Ahmed","suffix":""}],"badges":[],"createdAt":"2023-01-26 16:29:23","currentVersionCode":1,"declarations":"","doi":"10.21203/rs.3.rs-2517839/v1","doiUrl":"https://doi.org/10.21203/rs.3.rs-2517839/v1","draftVersion":[],"editorialEvents":[{"content":"https://doi.org/10.1007/s10904-023-02582-3","type":"published","date":"2023-04-01T20:14:42+00:00"}],"editorialNote":"","failedWorkflow":false,"files":[{"id":32218152,"identity":"fc5b011c-5926-4cf4-abbd-eea479cf0261","added_by":"auto","created_at":"2023-01-30 16:06:39","extension":"jpg","order_by":1,"title":"Figure 1","display":"","copyAsset":false,"role":"figure","size":48329,"visible":true,"origin":"","legend":"\u003cp\u003e(a) A schematic of the experimental temperature profile used to create the compound Cu\u003csub\u003e2\u003c/sub\u003eAlSnS\u003csub\u003e4\u003c/sub\u003e, (b) a quartz tube filled with pure components, and (c) the finished CATS ingot.\u003c/p\u003e","description":"","filename":"1.jpg","url":"https://assets-eu.researchsquare.com/files/rs-2517839/v1/f0c965c20114dba8b9f89af1.jpg"},{"id":32218154,"identity":"405861f9-8379-4320-a93a-4a6f2d898acb","added_by":"auto","created_at":"2023-01-30 16:06:39","extension":"jpg","order_by":2,"title":"Figure 2","display":"","copyAsset":false,"role":"figure","size":39342,"visible":true,"origin":"","legend":"\u003cp\u003e(a) Synthetic \u003cem\u003eCATS \u003c/em\u003epowder and (b) a schematic representation of physical vapor deposition from a single source (\u003cem\u003ePVD\u003c/em\u003e).\u003c/p\u003e","description":"","filename":"2.jpg","url":"https://assets-eu.researchsquare.com/files/rs-2517839/v1/3ddce21fe50c50ac087d1822.jpg"},{"id":32218155,"identity":"f11d97f1-1a27-4c5c-b745-00da094a8d88","added_by":"auto","created_at":"2023-01-30 16:06:39","extension":"jpg","order_by":3,"title":"Figure 3","display":"","copyAsset":false,"role":"figure","size":68027,"visible":true,"origin":"","legend":"\u003cp\u003eExperimental setup of photocatalytic reactor for degradation of MB pollutant dye under UV-irradiation.\u003c/p\u003e","description":"","filename":"3.jpg","url":"https://assets-eu.researchsquare.com/files/rs-2517839/v1/e25a7ea5a3db2c64821de252.jpg"},{"id":32219714,"identity":"55472595-b021-4201-9e10-20fe02e5568a","added_by":"auto","created_at":"2023-01-30 16:22:39","extension":"jpg","order_by":4,"title":"Figure 4","display":"","copyAsset":false,"role":"figure","size":46895,"visible":true,"origin":"","legend":"\u003cp\u003e\u003cem\u003eXRD\u003c/em\u003e pattern of synthesized \u003cem\u003eCATS \u003c/em\u003epowder.\u003c/p\u003e","description":"","filename":"4.jpg","url":"https://assets-eu.researchsquare.com/files/rs-2517839/v1/3582ac8e7c6aa88373991100.jpg"},{"id":32219037,"identity":"1d9f9ae0-8fbd-44db-9244-2f827003324f","added_by":"auto","created_at":"2023-01-30 16:14:39","extension":"jpg","order_by":5,"title":"Figure 5","display":"","copyAsset":false,"role":"figure","size":59711,"visible":true,"origin":"","legend":"\u003cp\u003eX-ray diffractograms of CATS thin layers deposited at a) 25°C, b)100°C, c) 200°C,\u003csub\u003e \u003c/sub\u003eand d) 300°C, respectively.\u003c/p\u003e","description":"","filename":"5.jpg","url":"https://assets-eu.researchsquare.com/files/rs-2517839/v1/31d70d391ad3ccf72f96d1a7.jpg"},{"id":32218157,"identity":"1347a3d8-f6ce-41ae-80eb-3b5977b6778d","added_by":"auto","created_at":"2023-01-30 16:06:39","extension":"jpg","order_by":6,"title":"Figure 6","display":"","copyAsset":false,"role":"figure","size":37276,"visible":true,"origin":"","legend":"\u003cp\u003eEDX analysis of synthesized CATS powder.\u003c/p\u003e","description":"","filename":"6.jpg","url":"https://assets-eu.researchsquare.com/files/rs-2517839/v1/757a27c7cf5efbb3c947973a.jpg"},{"id":32218149,"identity":"d2d3943c-a55e-491b-84e2-703faad28e9c","added_by":"auto","created_at":"2023-01-30 16:06:39","extension":"jpg","order_by":7,"title":"Figure 7","display":"","copyAsset":false,"role":"figure","size":52779,"visible":true,"origin":"","legend":"\u003cp\u003eEDX analysis of \u003cem\u003eCATS\u003c/em\u003e thin films deposited at a) 25°C, b) 100°C, c) 200°C,\u003csub\u003e \u003c/sub\u003eand d) 300°C.\u003c/p\u003e","description":"","filename":"7.jpg","url":"https://assets-eu.researchsquare.com/files/rs-2517839/v1/9bfe8fc44b5f018d5b8a37ce.jpg"},{"id":32218156,"identity":"2d9bda7b-5eee-4184-8ab2-5d1fd6fb3b29","added_by":"auto","created_at":"2023-01-30 16:06:39","extension":"jpg","order_by":8,"title":"Figure 8","display":"","copyAsset":false,"role":"figure","size":493103,"visible":true,"origin":"","legend":"\u003cp\u003e\u003cem\u003e2D\u003c/em\u003e and \u003cem\u003e3D\u003c/em\u003e AFM surface patterns of \u003cem\u003eCATS\u003c/em\u003e thin films deposited at (a) 25°C, (b) 100°C, (c) 200°C,\u003csub\u003e \u003c/sub\u003eand (d) 300°C.\u003c/p\u003e","description":"","filename":"8.jpg","url":"https://assets-eu.researchsquare.com/files/rs-2517839/v1/7059bb8b99863d5bb951c401.jpg"},{"id":32218150,"identity":"5daaf51c-f991-46df-bea2-a6fbea1f4f1a","added_by":"auto","created_at":"2023-01-30 16:06:39","extension":"jpg","order_by":9,"title":"Figure 9","display":"","copyAsset":false,"role":"figure","size":53711,"visible":true,"origin":"","legend":"\u003cp\u003eR, T(%) spectra of \u003cem\u003eCATS\u003c/em\u003ethin films deposited at various temperatures.\u003c/p\u003e","description":"","filename":"9.jpg","url":"https://assets-eu.researchsquare.com/files/rs-2517839/v1/f548877d28d84fe357b7ee99.jpg"},{"id":32218148,"identity":"38cd5366-8e1f-4edb-8d5d-18cfd2e47e87","added_by":"auto","created_at":"2023-01-30 16:06:39","extension":"jpg","order_by":10,"title":"Figure 10","display":"","copyAsset":false,"role":"figure","size":45985,"visible":true,"origin":"","legend":"\u003cp\u003eVariation of (αhν)\u003csup\u003e2\u003c/sup\u003e\u0026nbsp;\u003cem\u003evs\u003c/em\u003e\u0026nbsp;(hν) of\u0026nbsp;\u003cem\u003eCATS\u003c/em\u003e\u0026nbsp;thin films deposited at different temperatures.\u003c/p\u003e","description":"","filename":"10.jpg","url":"https://assets-eu.researchsquare.com/files/rs-2517839/v1/236dce0fcd301b84f42e81dd.jpg"},{"id":32218162,"identity":"b27aceae-5355-4d17-80b5-dffc31de7b5c","added_by":"auto","created_at":"2023-01-30 16:06:39","extension":"jpg","order_by":11,"title":"Figure 11","display":"","copyAsset":false,"role":"figure","size":104212,"visible":true,"origin":"","legend":"\u003cp\u003ePhotocatalytic degradation of \u003cem\u003eMB\u003c/em\u003e (2x10\u003csup\u003e-5\u003c/sup\u003eM) under UV-light irradiaton by Cu\u003csub\u003e2\u003c/sub\u003eAlSnS\u003csub\u003e4\u003c/sub\u003e (CATS) with different dosages (\u003cstrong\u003ea\u003c/strong\u003e) 40 mg/L (\u003cstrong\u003eb\u003c/strong\u003e) 65 mg/L (\u003cstrong\u003ec\u003c/strong\u003e) 95 mg/L and (\u003cstrong\u003ed\u003c/strong\u003e) 130 mg/L.\u003c/p\u003e","description":"","filename":"11.jpg","url":"https://assets-eu.researchsquare.com/files/rs-2517839/v1/0104ac758a121430471f1d16.jpg"},{"id":32219035,"identity":"3b3d0a05-6bd5-4f0f-88e9-491c0ff58271","added_by":"auto","created_at":"2023-01-30 16:14:39","extension":"jpg","order_by":12,"title":"Figure 12","display":"","copyAsset":false,"role":"figure","size":77338,"visible":true,"origin":"","legend":"\u003cp\u003ePhotocatalytic degradation of \u003cem\u003eMB\u003c/em\u003e (4x10\u003csup\u003e-5\u003c/sup\u003eM) under UV-light irradiation by Cu\u003csub\u003e2\u003c/sub\u003eAlSnS\u003csub\u003e4\u003c/sub\u003e (CATS) with different dosages (\u003cstrong\u003ee\u003c/strong\u003e) 65 mg/L and (\u003cstrong\u003ef\u003c/strong\u003e) 130 mg/L.\u003c/p\u003e","description":"","filename":"12.jpg","url":"https://assets-eu.researchsquare.com/files/rs-2517839/v1/04ed8499bbd39bf4de69c600.jpg"},{"id":32219036,"identity":"8aae8b01-53f5-4307-bf5a-c8236519807f","added_by":"auto","created_at":"2023-01-30 16:14:39","extension":"jpg","order_by":13,"title":"Figure 13","display":"","copyAsset":false,"role":"figure","size":68449,"visible":true,"origin":"","legend":"\u003cp\u003ePlots of C/C\u003csub\u003e0\u003c/sub\u003e and ln (C/C\u003csub\u003e0\u003c/sub\u003e) \u003cem\u003evs\u003c/em\u003e. irradiation time\u003cstrong\u003e \u003c/strong\u003efor photocatalytic degradation of \u003cem\u003eMB \u003c/em\u003e(2x10\u003csup\u003e-5\u003c/sup\u003eM) under UV-light irradiation in the presence of \u003cem\u003eCATS\u003c/em\u003e utilizing various doses 40, 65, 95 and 130 mg/L.\u003c/p\u003e","description":"","filename":"13.jpg","url":"https://assets-eu.researchsquare.com/files/rs-2517839/v1/8aa1e2d9fd8699c1fefd7c60.jpg"},{"id":32218159,"identity":"4fa06e87-eab2-4336-aa93-4a569221114d","added_by":"auto","created_at":"2023-01-30 16:06:39","extension":"jpg","order_by":14,"title":"Figure 14","display":"","copyAsset":false,"role":"figure","size":56369,"visible":true,"origin":"","legend":"\u003cp\u003ePlots of C/C\u003csub\u003e0\u003c/sub\u003e and ln (C/C\u003csub\u003e0\u003c/sub\u003e) \u003cem\u003evs\u003c/em\u003e. irradiation time\u003cstrong\u003e \u003c/strong\u003efor photocatalytic degradation of \u003cem\u003eMB \u003c/em\u003e(4x10\u003csup\u003e-5\u003c/sup\u003eM) under the influence of UV light in the presence of \u003cem\u003eCATS\u003c/em\u003e with different dosages 65 and 130 mg/L.\u003c/p\u003e","description":"","filename":"14.jpg","url":"https://assets-eu.researchsquare.com/files/rs-2517839/v1/2deeeb4b4894a18159184523.jpg"},{"id":44724054,"identity":"9bfcf862-0bdc-4b87-97dd-c077dd8e95bd","added_by":"auto","created_at":"2023-10-16 20:23:58","extension":"pdf","order_by":0,"title":"","display":"","copyAsset":false,"role":"manuscript-pdf","size":1019386,"visible":true,"origin":"","legend":"","description":"","filename":"manuscript.pdf","url":"https://assets-eu.researchsquare.com/files/rs-2517839/v1/c999a548-af83-434e-8d0e-7fc9a6d3a9b9.pdf"}],"financialInterests":"No competing interests reported.","formattedTitle":"Highly efficient photocatalytic degradation of organic polluants over Cu 2 AlSnS 4 (CATS) thin films: synthesis, chracterization and photocataysis Approch","fulltext":[{"header":"1. Introduction","content":"\u003cp\u003eConsidering the richness of its components on earth, inexpensive and non-toxic, Cu\u003csub\u003e2\u003c/sub\u003eZnSnS\u003csub\u003e4\u003c/sub\u003e (CZTS) compound has conventional the greatest courtesy in investigations. In general, the quaternary semiconductor compound Cu\u003csub\u003e2\u003c/sub\u003eZnSnS\u003csub\u003e4\u003c/sub\u003e [\u003cspan citationid=\"CR1\" class=\"CitationRef\"\u003e1\u003c/span\u003e] has emerged as one of the most promising contenders, thanks to its p-type conductivity, good optoelectronic capabilities, non-toxicity, and availability of all its constituent elements in the earth's crust [\u003cspan citationid=\"CR2\" class=\"CitationRef\"\u003e2\u003c/span\u003e, \u003cspan citationid=\"CR3\" class=\"CitationRef\"\u003e3\u003c/span\u003e]. Having a direct gap energy of 1.4 to 1.5 eV and a high absorption coefficient (10\u003csup\u003e4\u003c/sup\u003e cm\u003csup\u003e\u0026minus;\u0026thinsp;1\u003c/sup\u003e), \u003cem\u003eCZTS\u003c/em\u003e constitute an appropriate material for the conversion of solar energy [\u003cspan citationid=\"CR4\" class=\"CitationRef\"\u003e4\u003c/span\u003e, \u003cspan citationid=\"CR5\" class=\"CitationRef\"\u003e5\u003c/span\u003e]. Interestingly, solar cells made from \u003cem\u003eCZTS\u003c/em\u003e conversion efficiency expanded from 2.3% in 1997 to 11.1% in 2012 [\u003cspan citationid=\"CR6\" class=\"CitationRef\"\u003e6\u003c/span\u003e]. Therefore, investigation of new materials that resemble CZTS-like Cu\u003csub\u003e2\u003c/sub\u003eAlSnS\u003csub\u003e4\u003c/sub\u003e in terms of structure (CZTS) are highly recommended. It is worth mentioning that there are two physical characteristics of \u003cem\u003eCZTS\u003c/em\u003e that exhibit excellent optical parameters with tunable direct bandgap energy as well as high absorption coefficient. Because of these unique characteristics, CATS represents a serious candidate and can be exploitable as an absorber layer in inexpensive solar cells. The synthesis of such quaternary compounds have been adopted using a various range of techniques [\u003cspan additionalcitationids=\"CR10 CR11 CR12 CR13\" citationid=\"CR9\" class=\"CitationRef\"\u003e9\u003c/span\u003e\u0026ndash;\u003cspan citationid=\"CR14\" class=\"CitationRef\"\u003e14\u003c/span\u003e]. From the above-mentioned techniques, each technique has advantages and limitations as well. Vacuum thermal evaporation has acquired the most affection of these techniques due to a large variety of factors into consideration. Thus, it is a practical way to deposit a wide range of thin layers. In addition, compared to the procedures mentioned above, which are typically convoluted and time-consuming, is supposed of as a straightforward, reasonable, and environmentally friendly methodology. Quaternary Cu\u003csub\u003e2\u003c/sub\u003eXSnS\u003csub\u003e4\u003c/sub\u003e (X\u0026thinsp;=\u0026thinsp;\u003cem\u003eNi\u003c/em\u003e, \u003cem\u003eZn\u003c/em\u003e, \u003cem\u003eFe\u003c/em\u003e,\u0026hellip; etc.) compound have, nevertheless, been found to be deposited [\u003cspan citationid=\"CR15\" class=\"CitationRef\"\u003e15\u003c/span\u003e, \u003cspan citationid=\"CR16\" class=\"CitationRef\"\u003e16\u003c/span\u003e]. Based on previous [\u003cspan additionalcitationids=\"CR18 CR19\" citationid=\"CR17\" class=\"CitationRef\"\u003e17\u003c/span\u003e\u0026ndash;\u003cspan citationid=\"CR20\" class=\"CitationRef\"\u003e20\u003c/span\u003e] work and in continuation of our research interest, the present study is carried out to establish firstly an exclusive physical synthesis of new CATS quaternary compound using direct fusion process. After that exploiting the vacuum deposition technique for obtaining thin films, that exhibits a noticeable change in physical properties as a result of the substrate temperature.\u003c/p\u003e \u003cp\u003eHowever, as far as we are aware, no research has been centered on the structural, morphological, optical of \u003cem\u003eCATS\u003c/em\u003e thin films as well their photocatalytic activities. Thus, the aim of the present research work is to study the synthesis and the consequences of growth temperature on the morphological, the structural, and the optical characteristics of CATS-based thin layers as well their photocatalytic degradation efficacy toward organic pollutant in particular aqueous methylene blue (MB) solution exposed to UV light.\u003c/p\u003e"},{"header":"2. Experimental Strategies","content":"\u003cdiv id=\"Sec3\" class=\"Section2\"\u003e \u003ch2\u003e2.1. Cu\u003csub\u003e2\u003c/sub\u003eAlSnS\u003csub\u003e4\u003c/sub\u003e powder Synthesis:\u003c/h2\u003e \u003cp\u003eThe 99.999% pure elements copper (Cu), aluminum (Al), tin (Sn), and sulfur were combined in stoichiometric quantities to form the quaternary Cu\u003csub\u003e2\u003c/sub\u003eAlSnS\u003csub\u003e4\u003c/sub\u003e material. A quartz tube was used to seal the mixture while operating at a high vacuum of 10\u003csup\u003e\u0026minus;\u0026thinsp;4\u003c/sup\u003e Torr. The tube is placed within a horizontal furnace of the Nabertherm (B 180) design with the arrangement of the tube being horizontal. The quartz tube was progressively heated (100\u0026deg;C/h) to a temperature of 1100\u0026deg;C in order to prevent explosions caused by sulfur vapor pressure. By maintaining the melt at 1100\u0026deg;C for roughly 4 hours to make good element interdiffusion, a complete homogeneity could be attained. The obtained material was then appropriately crystallized by admitting the tube to innately cool to ambient temperature. This procedure has given the desired synthesized material a black ingot-shaped substance. The ingot is then ground into a fine powder that is utilized as the basic material for creating thin films for thermal evaporation. The schematic of thermal profile adopted for the synthesis, the \u003cem\u003eCATS\u003c/em\u003e ingot and the powder are portrayed in Fig.\u0026nbsp;\u003cspan refid=\"Fig1\" class=\"InternalRef\"\u003e1\u003c/span\u003e.\u003c/p\u003e \u003cp\u003e \u003c/p\u003e \u003c/div\u003e \u003cdiv id=\"Sec4\" class=\"Section2\"\u003e \u003ch2\u003e2.2. Thin film preparation:\u003c/h2\u003e \u003cp\u003eCu\u003csub\u003e2\u003c/sub\u003eAlSnS\u003csub\u003e4\u003c/sub\u003e powder was expended to create evaporated thin films (Fig.\u0026nbsp;\u003cspan refid=\"Fig2\" class=\"InternalRef\"\u003e2\u003c/span\u003e). The huge radiant-heat loads and lack of vacuum materials and procedures that could tolerate the heat, predominantly in a demountable system, hindered its development. A graphite made crucible holds the \u003cem\u003eCATS\u003c/em\u003e powder that has been crushed. The use of thermal evaporation sources, which allow us to control the powder, has been carried out. Prior to deposition, the chamber was evacuated to a pressure of less than 10\u003csup\u003e\u0026minus;\u0026thinsp;6\u003c/sup\u003e Torr. Approximately 15 centimetres alienated the substrate from the crucible. The temperature of the crucible was retained to control the thermal evaporation sources. The substrates were maintained at four different temperatures, ranging from 25\u0026deg;C, 100\u0026deg;C, 200\u0026deg;C, and 300\u0026deg;C. To produce the same film thicknesses, the bulk of the added powder, which weighs approximately 0.2 g, was left unchanged. The films thicknesses found to be between 500 and 600 nm.\u003c/p\u003e \u003cp\u003e \u003c/p\u003e \u003c/div\u003e \u003cdiv id=\"Sec5\" class=\"Section2\"\u003e \u003ch2\u003e2.3. Thin film characterizations:\u003c/h2\u003e \u003cp\u003eThe crystalline film structure was examined by X-ray diffraction using (Shimadzu XRD-6000 X-ray diffractometer supplied with a Cu-K radiation source of 1.5418 \u0026Aring;). AFM using a Veeco CP-II in contact mode with Si tips with a 1 Hz scan rate, was exploited to analyze the thin-film surface morphology while scanning-electron microscopy (SEM, Shimadzu Superscan SSX-550) was employed to study \u003cem\u003eEDS\u003c/em\u003e analysis. The homogenous as-grown films adhered adequately to the substrate glass surface and had no pinholes or crashes on their surface. At normal incidence and room temperature, the optical transmittance \u003cem\u003eT (λ)\u003c/em\u003e and reflectance \u003cem\u003eR (λ)\u003c/em\u003e spectra over the wavelength range of 200\u0026ndash;2500 nm were measured with a 0.1 nm resolution (Shimadzu Solid Spec-3700 UV-visible spectrophotometer with an integrating sphere). The thickness of the film layer was assessed using stylus displacement (Veeco Dektak 150 profilometer).\u003c/p\u003e \u003c/div\u003e \u003cdiv id=\"Sec6\" class=\"Section2\"\u003e \u003ch2\u003e2.4. Analysis of Photocatalytic Activity:\u003c/h2\u003e \u003cp\u003eThe photocatalytic degradation efficacy of prepared Cu\u003csub\u003e2\u003c/sub\u003eAlSnS\u003csub\u003e4\u003c/sub\u003e was evaluated using \u003cem\u003eMB\u003c/em\u003e in aqueous solution. The photocatalytic activity of the prepared photocatalyst Cu\u003csub\u003e2\u003c/sub\u003eAlSnS\u003csub\u003e4\u003c/sub\u003e was assessed by monitoring the degradation of (MB) pollutants throws decreasing its absorption. \u003cem\u003eMB\u003c/em\u003e stock solution was prepared by dissolving it in distilled water at ~\u0026thinsp;7 mg/L (2x10\u003csup\u003e\u0026minus;\u0026thinsp;5\u003c/sup\u003e mol/L)\u0026thinsp;~\u0026thinsp;14 mg/L (4x10\u003csup\u003e\u0026minus;\u0026thinsp;5\u003c/sup\u003e mol/L) and into a 2 L volumetric flask. Then, different mass (15 mg, 25 mg and 50 mg) of Cu\u003csub\u003e2\u003c/sub\u003eAlSnS\u003csub\u003e4\u003c/sub\u003e photocatalysts (each in a separate experiment) were added into a photoreactor comprising 370 mL of \u003cem\u003eMB\u003c/em\u003e solution (Fig.\u0026nbsp;\u003cspan refid=\"Fig3\" class=\"InternalRef\"\u003e3\u003c/span\u003e). The solutions were stirred with a magnetic stirrer in a dark environment for 30 min to ensure the adsorption/desorption equilibrium of MB on these photocatalysts. Then, the mixture was exposed to \u003cem\u003eUV\u003c/em\u003e irradiation provided by a 125W \u003cem\u003eUV\u003c/em\u003e-lamp vertically within the 500 ml intended photochemical reactor (Fig.\u0026nbsp;\u003cspan refid=\"Fig3\" class=\"InternalRef\"\u003e3\u003c/span\u003e). The solution's UV-vis absorption spectrum was found to be between 200 and 1000 nm using double-beam Shimadzu 1800 UV-VIS-NIR spectrophotometer. Eight samples were collected following \u003cem\u003eUV\u003c/em\u003e radiation at predetermined intervals of 30 min, and their absorption spectra were recorded from its decreasing in absorption intensity corresponding to the progress of the photocatalytic degradation of \u003cem\u003eMB\u003c/em\u003e indicator at the characteristic wavelength λ\u003csub\u003emax\u003c/sub\u003e\u0026thinsp;=\u0026thinsp;664 nm.\u003c/p\u003e \u003cp\u003e \u003c/p\u003e \u003c/div\u003e"},{"header":"3. Results And Discussion","content":"\u003cdiv id=\"Sec8\" class=\"Section2\"\u003e \u003ch2\u003e3.1 Identification of the structure:\u003c/h2\u003e \u003cp\u003eThe X-ray diffraction patterns of the pure \u003cem\u003eCATS\u003c/em\u003e powder are displayed in Fig.\u0026nbsp;\u003cspan refid=\"Fig4\" class=\"InternalRef\"\u003e4\u003c/span\u003e. The sample, according to the \u003cem\u003eJCPDS\u003c/em\u003e (card No. 00-047-1343), is well crystalline. It shows twelve clearly defined XRD peaks that match the card's associated peaks. Because there are no further other phases, all of the sample's peaks are tetragonal in nature.\u003c/p\u003e \u003cp\u003eThe crystal structure's XRD patterns of \u003cem\u003eCATS\u003c/em\u003e thin films was obtained using (Card JCPS, code 00-027-0980) as presented in Fig.\u0026nbsp;\u003cspan refid=\"Fig5\" class=\"InternalRef\"\u003e5\u003c/span\u003e. At temperatures of 25, 100, and 200 degrees Celsius, one peak that correspond to the (111) orientations of \u003cem\u003eCATS\u003c/em\u003e thin layers appear on the X-ray diffractogram at the angle of (2θ\u0026thinsp;=\u0026thinsp;30\u0026deg;). However, at 300 degrees Celsius, two peaks that correspond to the (111) and (220) orientations of \u003cem\u003eCATS\u003c/em\u003e thin layers appear on the X-ray diffractogram respectively at the angle of (2θ\u0026thinsp;=\u0026thinsp;30\u0026deg;) and (2θ\u0026thinsp;=\u0026thinsp;50\u0026deg;). No any other impurity phases were detected, specifying the stability of atoms at the substrate surface. Therefore, the deposition at 300\u0026deg;C increases crystallization and promotes the formation of further CATS kesterite peaks.\u003c/p\u003e \u003c/div\u003e \u003cdiv id=\"Sec9\" class=\"Section2\"\u003e \u003ch2\u003e3.2 EDX analysis:\u003c/h2\u003e \u003cp\u003eEnergy dispersive X-ray (\u003cem\u003eEDX\u003c/em\u003e) analysis was employed to look into the samples' quantitative makeup. The outcomes of the sample's EDX of CATS powder elemental analysis are displayed in Fig.\u0026nbsp;\u003cspan refid=\"Fig6\" class=\"InternalRef\"\u003e6\u003c/span\u003e. It has been confirmed that Cu, Al, Sn, and S are presented. At 2.4 keV, the sulphur (S) displays a higher intensity pic which represents the principle element.\u003c/p\u003e \u003cp\u003e \u003c/p\u003e \u003cp\u003eThe findings of the \u003cem\u003eCATS\u003c/em\u003e films numerous surface spots' EDX elemental analyses are shown in Fig.\u0026nbsp;\u003cspan refid=\"Fig7\" class=\"InternalRef\"\u003e7\u003c/span\u003e. All samples have been found to include \u003cem\u003eCu\u003c/em\u003e, \u003cem\u003eAl\u003c/em\u003e, \u003cem\u003eSn\u003c/em\u003e, and \u003cem\u003eS\u003c/em\u003e. Due to the substrate being employed; a well-defined peak was seen in all films between 1.2 keV and 2 keV [\u003cspan citationid=\"CR21\" class=\"CitationRef\"\u003e21\u003c/span\u003e]. We may infer from the EDX analysis that each sample contains \u003cem\u003eCu\u003c/em\u003e, \u003cem\u003eAl\u003c/em\u003e, \u003cem\u003eSn\u003c/em\u003e, and \u003cem\u003eS\u003c/em\u003e. Thus, XRD analysis and atomic concentrations determined by EDX agree with the formula Cu\u003csub\u003e2\u003c/sub\u003eAlSnS\u003csub\u003e4\u003c/sub\u003e.\u003c/p\u003e \u003cp\u003e \u003c/p\u003e \u003c/div\u003e \u003cdiv id=\"Sec10\" class=\"Section2\"\u003e \u003ch2\u003e3.3 AFM analysis:\u003c/h2\u003e \u003cp\u003eAtomic force microscopy (\u003cem\u003eAFM\u003c/em\u003e), was susscesfully used to assess the \u003cem\u003eCATS\u003c/em\u003e films. In order to attain more surface data, contact \u003cem\u003eAFM\u003c/em\u003e was implemented to evaluate the surface topography of \u003cem\u003eCATS\u003c/em\u003e films (Fig.\u0026nbsp;\u003cspan refid=\"Fig8\" class=\"InternalRef\"\u003e8\u003c/span\u003e). All \u003cem\u003eAFM\u003c/em\u003e micrographs had a same scan area. Based on the temperature of the substrate, the surfaces of the films have noticeably varying morphologies and roughness. The lengthened shape befitted more sphere-like at high substrate temperatures. Grain agglomeration, which results in irregular particle morphologies, is produced on by rising temperature. For films, the root mean square (\u003cem\u003erms\u003c/em\u003e) surface roughness was determined to be ranged between 13 to 24 nm. A higher substrate temperature may cause smaller crystals to fuse together which led to increasing roughness. As a result of AFM investigation, it has been determined that as temperature rises, \u003cem\u003eCZTS\u003c/em\u003e film surface roughness and particle size both increase [\u003cspan citationid=\"CR22\" class=\"CitationRef\"\u003e22\u003c/span\u003e].\u003c/p\u003e \u003cp\u003e \u003c/p\u003e \u003c/div\u003e \u003cdiv id=\"Sec11\" class=\"Section2\"\u003e \u003ch2\u003e3.4 UV-Visible spectroscopy analysis:\u003c/h2\u003e \u003cp\u003eThe photon-matter interaction measurements were used to record the transmittance and the reflectance spectra with regard to the 200\u0026ndash;2500 nm wavelength range (Fig.\u0026nbsp;\u003cspan refid=\"Fig9\" class=\"InternalRef\"\u003e9\u003c/span\u003e). Around 370 nm, all films transmittances began to decline. All films can block damaging \u003cem\u003eUV\u003c/em\u003e radiation. The uniformity of the grains and variations in their height on the films surface have an impact on transmittance. However, as the surface roughness decreases, the transmittance significantly rises.\u003c/p\u003e \u003cp\u003e \u003c/p\u003e \u003cp\u003eCalculating the optical energy bandgap involves using Tauc's relationship (Eq.\u0026nbsp;1) [\u003cspan citationid=\"CR23\" class=\"CitationRef\"\u003e23\u003c/span\u003e, \u003cspan citationid=\"CR24\" class=\"CitationRef\"\u003e24\u003c/span\u003e]:\u003c/p\u003e \u003cp\u003e \u003cem\u003e(αhν)\u003c/em\u003e \u003csup\u003e \u003cem\u003em\u003c/em\u003e \u003c/sup\u003e \u003cem\u003e= B (hν-Eg)\u003c/em\u003e (1)\u003c/p\u003e \u003cp\u003eWhere \u003cem\u003em\u003c/em\u003e defines whether an optical transition occurs directly or indirectly, \u003cem\u003eα\u003c/em\u003e is the absorption coefficient, \u003cem\u003eB\u003c/em\u003e is the constant, and \u003cem\u003ehv\u003c/em\u003e is the incident photon energy. To evaluate the bandgap, plotting of (αhν)\u003csup\u003e2\u003c/sup\u003e \u003cem\u003evs\u003c/em\u003e photon energy (hν) is done (Fig.\u0026nbsp;\u003cspan refid=\"Fig10\" class=\"InternalRef\"\u003e10\u003c/span\u003e). Energy of the obtained band gap ranged from 1.65 eV to 1.30 eV. The direct bandgap energy of the \u003cem\u003eCATS\u003c/em\u003e reaches 1.30 eV for 300\u0026deg; C as the substrate temperature rises.\u003c/p\u003e \u003cp\u003e \u003c/p\u003e \u003c/div\u003e \u003cdiv id=\"Sec12\" class=\"Section2\"\u003e \u003ch2\u003e3.5. Photocatalytic Activity:\u003c/h2\u003e \u003cp\u003eFigure \u003cspan refid=\"Fig11\" class=\"InternalRef\"\u003e11\u003c/span\u003e recording the photocatalytic degradation of \u003cem\u003eMB\u003c/em\u003e by \u003cem\u003eCATS\u003c/em\u003e after UV-light irradiation. It is noticeable that for UV-light irradiation, the absorbance intensity of the MB absorption peak (664 nm) progressively decreased in all samples. All samples demonstrated a stable adsorption-desorption equilibrium in \u003cem\u003eMB\u003c/em\u003e solution for the first 30 min (dark adsorption test). The degradation of \u003cem\u003eMB\u003c/em\u003e with a concentration of 2x10\u003csup\u003e\u0026minus;\u0026thinsp;5\u003c/sup\u003e M under UV-light was observed about 70%, 94%, 96% and 98% after 4 h when using different amounts of the catalyst \u003cem\u003eCATS\u003c/em\u003e dosages of 40, 65, 95 and 130 mg/L, respectively (Fig.\u0026nbsp;\u003cspan refid=\"Fig11\" class=\"InternalRef\"\u003e11\u003c/span\u003e). Thus, a more pronounced decrease (of more than 90%) in the \u003cem\u003eMB\u003c/em\u003e major absorption peak intensity was monitored using catalyst dosages\u0026thinsp;\u0026ge;\u0026thinsp;65 mg/L in UV-light. This indicates that Cu\u003csub\u003e2\u003c/sub\u003eAlSnS\u003csub\u003e4\u003c/sub\u003e represent an appropriate and efficient candidate for the photocatalytic degradation of \u003cem\u003eMB\u003c/em\u003e dye.\u003c/p\u003e \u003cp\u003e \u003c/p\u003e \u003cp\u003eAdditionally, to improve the experimental setup for the optimum photocatalytic efficiency of the Cu\u003csub\u003e2\u003c/sub\u003eAlSnS\u003csub\u003e4\u003c/sub\u003e, an efficient study was achieved to find the optimum \u003cem\u003eCATS\u003c/em\u003e and \u003cem\u003eMB\u003c/em\u003e concentrations for samples with excellent performance. Thus, for comparison, we investigated additionally the photocatalytic degradation of 4x10\u003csup\u003e\u0026minus;\u0026thinsp;5\u003c/sup\u003e M concentration of \u003cem\u003eMB\u003c/em\u003e. A degradation of MB of 38%, 34% over 4 h was observed for a catalyst \u003cem\u003eCATS\u003c/em\u003e dosages of 65 and 130 mg/L, respectively (Fig.\u0026nbsp;\u003cspan refid=\"Fig12\" class=\"InternalRef\"\u003e12\u003c/span\u003e). Consequently, and from the above results, the photocatalytic results when exposed to \u003cem\u003eUV\u003c/em\u003e light in the presence of 65 mg/L of \u003cem\u003eCATS\u003c/em\u003e showed a more rapid degradation of 2x10\u003csup\u003e\u0026minus;\u0026thinsp;5\u003c/sup\u003eM of \u003cem\u003eMB\u003c/em\u003e (\u0026asymp;\u0026thinsp;95%) as compared to other outcomes.\u003c/p\u003e \u003cp\u003e \u003c/p\u003e \u003cp\u003eOn the other hand, under UV-irradiation for 240 minutes, the photodegradation of \u003cem\u003eMB\u003c/em\u003e in the presence of photocatalyst \u003cem\u003eCATS\u003c/em\u003e results in the transformation of nitrogen and sulfur atoms in \u003cem\u003eMB\u003c/em\u003e molecules into inorganic ions and gasses. As reported, the mineralization and decomposition of MB were confirmed by the reduction of total organic carbon (TOC) followed by almost complete mineralization of carbon and of nitrogen and sulfur heteroatoms into CO\u003csub\u003e2\u003c/sub\u003e, ammonium NH\u003csub\u003e4\u003c/sub\u003e\u003csup\u003e+\u003c/sup\u003e, nitrate NO\u003csub\u003e3\u003c/sub\u003e\u003csup\u003e\u0026minus;\u003c/sup\u003e and sulfate SO\u003csub\u003e4\u003c/sub\u003e\u003csup\u003e2\u0026minus;\u003c/sup\u003e, respectively [\u003cspan citationid=\"CR25\" class=\"CitationRef\"\u003e25\u003c/span\u003e, \u003cspan citationid=\"CR26\" class=\"CitationRef\"\u003e26\u003c/span\u003e].\u003c/p\u003e \u003cp\u003eThe C/C\u003csub\u003e0\u003c/sub\u003e \u003cem\u003evs\u003c/em\u003e degradation time plots are presented in Figs.\u0026nbsp;\u003cspan refid=\"Fig11\" class=\"InternalRef\"\u003e11\u003c/span\u003e and \u003cspan refid=\"Fig12\" class=\"InternalRef\"\u003e12\u003c/span\u003e to provide a thorough understanding of the kinetic mechanism during the photocatalytic process. According to the results, the photodegradation progression proceeded gradually with irradiation time, with a much steeper decrease under UV-light irradiation for the \u003cem\u003eCATS\u003c/em\u003e dosages of 65, 95 and 130 mg/L compared to that for 40 mg/L. The rate constants (\u003cem\u003ek\u003c/em\u003e) for the degradation of \u003cem\u003eMB\u003c/em\u003e were determined from the well-known rate constant equation ln (C/C\u003csub\u003e0\u003c/sub\u003e)\u0026thinsp;=\u0026thinsp;\u003cem\u003ek\u003c/em\u003et and plotted in Figs.\u0026nbsp;\u003cspan refid=\"Fig13\" class=\"InternalRef\"\u003e13\u003c/span\u003e and \u003cspan refid=\"Fig14\" class=\"InternalRef\"\u003e14\u003c/span\u003e to better illustrate the degradation rates. Figures\u0026nbsp;\u003cspan refid=\"Fig13\" class=\"InternalRef\"\u003e13\u003c/span\u003e and \u003cspan refid=\"Fig14\" class=\"InternalRef\"\u003e14\u003c/span\u003e shows that the degradation of \u003cem\u003eMB\u003c/em\u003e followed first order kinetics that illustrates by linear plots. The rate of degradation constants (\u003cem\u003ek\u003c/em\u003e) were obtained from the slope of linear plot and are 5.03x10\u003csup\u003e\u0026minus;\u0026thinsp;3\u003c/sup\u003e, 1.24x10\u003csup\u003e\u0026minus;\u0026thinsp;2\u003c/sup\u003e, 1.38x10\u003csup\u003e\u0026minus;\u0026thinsp;2\u003c/sup\u003e and 1.63x10\u003csup\u003e\u0026minus;\u0026thinsp;2\u003c/sup\u003e min\u003csup\u003e\u0026minus;\u0026thinsp;1\u003c/sup\u003e for different catalyst (CATS) dosages of 40, 65, 95 and 130 mg/L, respectively (Fig.\u0026nbsp;\u003cspan refid=\"Fig10\" class=\"InternalRef\"\u003e10\u003c/span\u003e) in the presence of 2x10\u003csup\u003e\u0026minus;\u0026thinsp;5\u003c/sup\u003e M of \u003cem\u003eMB\u003c/em\u003e. While for 4x10\u003csup\u003e\u0026minus;\u0026thinsp;5\u003c/sup\u003e M of MB, \u003cem\u003ek\u003c/em\u003e is 2.08x10\u003csup\u003e\u0026minus;\u0026thinsp;3\u003c/sup\u003e and 1.77x10\u003csup\u003e\u0026minus;\u0026thinsp;3\u003c/sup\u003e min\u003csup\u003e\u0026minus;\u0026thinsp;1\u003c/sup\u003e for different catalyst (CATS) dosages of 65 and 130 mg/L, respectively (Fig.\u0026nbsp;\u003cspan refid=\"Fig13\" class=\"InternalRef\"\u003e13\u003c/span\u003e). The \u003cem\u003eCATS\u003c/em\u003e displayed higher photocatalytic activity more than three times from a dosage of 65 mg/L under UV-light than a dosage of \u003cem\u003eCATS\u003c/em\u003e of 40 mg/L. The achieved results remain interesting compared literature, in which the photocatalytic degradation of \u003cem\u003eMB\u003c/em\u003e, under \u003cem\u003eUV\u003c/em\u003e light irradiation using polymeric membranes impregnated with ZnO nanoparticles, such as cellulose acetate/Zinc oxide [\u003cspan citationid=\"CR26\" class=\"CitationRef\"\u003e26\u003c/span\u003e] poly(methylmethacrylate) (PMMA)/Zinc oxide [\u003cspan citationid=\"CR27\" class=\"CitationRef\"\u003e27\u003c/span\u003e] and Polyaniline/Zinc oxide [\u003cspan citationid=\"CR28\" class=\"CitationRef\"\u003e28\u003c/span\u003e] as catalysts exhibited 30%, 60% and 79% of dye degradation in 300 minute. However, remains inferior to the photocatalytic efficiency of TiO\u003csub\u003e2\u003c/sub\u003e/AC (Activated Carbon) in which almost complete degradation of \u003cem\u003eMB\u003c/em\u003e (98%) was achieved within only 90 min UV-light irradiation [\u003cspan citationid=\"CR29\" class=\"CitationRef\"\u003e29\u003c/span\u003e]. As well AgNPs/TiO\u003csub\u003e2\u003c/sub\u003e/Ti\u003csub\u003e3\u003c/sub\u003eC\u003csub\u003e2\u003c/sub\u003eTx MXene composites [\u003cspan citationid=\"CR30\" class=\"CitationRef\"\u003e30\u003c/span\u003e] as efficient catalysts with exclusive degradation efficacy as the majority of the previously described photocatalysts in comparable experimental setups.\u003c/p\u003e \u003cp\u003e \u003c/p\u003e \u003cp\u003e \u003c/p\u003e \u003c/div\u003e"},{"header":"4. Conclusions","content":"\u003cp\u003eIn this study, the direct melting of the component elements and the vacuum thermal evaporation method was successfully used for manufacture and deposit a novel \u003cem\u003eCATS\u003c/em\u003e quaternary material. The structural, the morphological and the optical characteristics of the layers were evaluated at various substrate temperatures between 25\u0026deg;C and 300\u0026deg;C. The X-ray diffractograms for \u003cem\u003eCATS\u003c/em\u003e thin films demonstrate that the optimal orientations along the layers deposited at 300\u0026deg;C (111) and (220) planes. An XRD investigation showed that as substrate temperature rises, crystallinity also rises. Additionally, the \u003cem\u003eCATS\u003c/em\u003e thin films have have \u003cem\u003eEg\u003c/em\u003e values for direct transitions in the range of 1.30\u0026ndash;1.65 eV, rough, dense, and compact surface. The photocatalytic degradation of methylene blue (MB), similar renowned pollutants dye using \u003cem\u003eCATS\u003c/em\u003e as catalysts was evaluated under UV-light irradiation condition. Indeed, \u003cem\u003eCATS\u003c/em\u003e under UV-light achieved maximum degradation of 8 % of aqueous \u003cem\u003eMB\u003c/em\u003e solution in 120 \u003cem\u003emin\u003c/em\u003e without any scavenger. The obtained results will help of active \u003cem\u003eCATS\u003c/em\u003e catalysts for the mineralization and photodegradation of other organic pollutants.\u003c/p\u003e"},{"header":"Declarations","content":"\u003cp\u003e\u003cstrong\u003eAcknowledgments\u003c/strong\u003e\u003c/p\u003e\n\u003cp\u003eThe authors would like to thank the Deanship of Scientific Research at Umm Al-Qura University for supporting this work (22UQU4331172-DSR01).\u003c/p\u003e\n\u003cp\u003e\u003cstrong\u003eConflict of Interest:\u0026nbsp;\u003c/strong\u003eThe authors declare that they are no conflict of interest.\u003c/p\u003e"},{"header":"References","content":"\u003col\u003e\n\u003cli\u003eM. Rahman, M. Bashar, \u0026amp; N. Islam, Optical and Structural Study of the CZTS Thin Film for Solar Cell Derived from the Chloride-Based sol-gel Precursor Solution. Dhaka University Journal of Science, 70 (1) (2022) 1\u0026ndash;7. \u003c/li\u003e\n\u003cli\u003eY.M. Zhang, Z.J. Jia, Z.Y. 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Mahmoud, Efficient Photocatalytic Degradation of Organic Dyes by AgNPs/TiO\u003csub\u003e2\u003c/sub\u003e/Ti\u003csub\u003e3\u003c/sub\u003eC\u003csub\u003e2\u003c/sub\u003eTx MXene Composites under UV and Solar Light, ACS Omega 6 (2021) 33325\u0026ndash;38.\u003c/li\u003e\n\u003c/ol\u003e"}],"fulltextSource":"","fullText":"","funders":[],"hasAdminPriorityOnWorkflow":false,"hasManuscriptDocX":true,"hasOptedInToPreprint":true,"hasPassedJournalQc":"","hasAnyPriority":false,"hideJournal":false,"highlight":"","institution":"","isAcceptedByJournal":true,"isAuthorSuppliedPdf":false,"isDeskRejected":"","isHiddenFromSearch":false,"isInQc":false,"isInWorkflow":false,"isPdf":false,"isPdfUpToDate":true,"isWithdrawnOrRetracted":false,"journal":{"display":true,"email":"[email protected]","identity":"journal-of-inorganic-and-organometallic-polymers-and-materials","isNatureJournal":false,"hasQc":true,"allowDirectSubmit":false,"externalIdentity":"joip","sideBox":"Learn more about [Journal of Inorganic and Organometallic Polymers and Materials](https://www.springer.com/journal/10904)","snPcode":"10904","submissionUrl":"https://submission.nature.com/new-submission/10904/3","title":"Journal of Inorganic and Organometallic Polymers and Materials","twitterHandle":"","acdcEnabled":true,"dfaEnabled":true,"editorialSystem":"em","reportingPortfolio":"Springer Hybrid","inReviewEnabled":true,"inReviewRevisionsEnabled":false},"keywords":"Cu2AlSnS4, thin films, inorganic materials, catalysis, vapor deposition","lastPublishedDoi":"10.21203/rs.3.rs-2517839/v1","lastPublishedDoiUrl":"https://doi.org/10.21203/rs.3.rs-2517839/v1","license":{"name":"CC BY 4.0","url":"https://creativecommons.org/licenses/by/4.0/"},"manuscriptAbstract":"\u003cp\u003eCu\u003csub\u003e2\u003c/sub\u003eAlSnS\u003csub\u003e4\u003c/sub\u003e (CATS) was generated through directly fusing of extremely pure elements. Powder show a tetragonal crystal system belongs to the space group \u003cem\u003eFd3m\u003c/em\u003e and the \u003cem\u003eCATS\u003c/em\u003e film displays narrow and weak diffraction peaks corresponding to the CZTS structure of pure kesterite without secondary phase. The surface appearance and chemical content films exposed their homogenous character. The optical analysis displayed good visible-range optical absorption and optical direct band gap of 1.30\u0026ndash;1.65 eV with excellent transmission. \u003cem\u003eCATS\u003c/em\u003e showed high photocatalytic efficacy to degrade methylene blue (\u003cem\u003eMB\u003c/em\u003e) completely under UV-light irradiation. These results will open the opportunity for using this new material as talented candidate in solar cells and removing organic pollutants from aqueous solutions.\u003c/p\u003e","manuscriptTitle":"Highly efficient photocatalytic degradation of organic polluants over Cu 2 AlSnS 4 (CATS) thin films: synthesis, chracterization and photocataysis Approch","msid":"","msnumber":"","nonDraftVersions":[{"code":1,"date":"2023-01-30 16:06:33","doi":"10.21203/rs.3.rs-2517839/v1","editorialEvents":[{"type":"communityComments","content":0},{"type":"decision","content":"Major revision","date":"2023-01-30T07:08:32+00:00","index":"","fulltext":""},{"type":"editorInvitedReview","content":"","date":"2023-01-30T01:48:27+00:00","index":"hide","fulltext":""},{"type":"reviewerAgreed","content":"876b9252-2a57-4000-832f-a693f52a3889","date":"2023-01-30T01:22:58+00:00","index":"hide","fulltext":""},{"type":"reviewersInvited","content":"","date":"2023-01-28T10:16:32+00:00","index":"","fulltext":""},{"type":"editorAssigned","content":"","date":"2023-01-28T09:37:33+00:00","index":"","fulltext":""},{"type":"checksComplete","content":"","date":"2023-01-27T04:10:54+00:00","index":"","fulltext":""},{"type":"submitted","content":"Journal of Inorganic and Organometallic Polymers and Materials","date":"2023-01-26T16:16:22+00:00","index":"","fulltext":""}],"status":"published","journal":{"display":true,"email":"[email protected]","identity":"journal-of-inorganic-and-organometallic-polymers-and-materials","isNatureJournal":false,"hasQc":true,"allowDirectSubmit":false,"externalIdentity":"joip","sideBox":"Learn more about [Journal of Inorganic and Organometallic Polymers and Materials](https://www.springer.com/journal/10904)","snPcode":"10904","submissionUrl":"https://submission.nature.com/new-submission/10904/3","title":"Journal of Inorganic and Organometallic Polymers and Materials","twitterHandle":"","acdcEnabled":true,"dfaEnabled":true,"editorialSystem":"em","reportingPortfolio":"Springer Hybrid","inReviewEnabled":true,"inReviewRevisionsEnabled":false}}],"origin":"","ownerIdentity":"80bf05cd-8f5f-4318-9f62-cc95a2dcb78f","owner":[],"postedDate":"January 30th, 2023","published":true,"recentEditorialEvents":[],"rejectedJournal":[],"revision":"","amendment":"","status":"published-in-journal","subjectAreas":[],"tags":[],"updatedAt":"2023-10-16T20:22:02+00:00","versionOfRecord":{"articleIdentity":"rs-2517839","link":"https://doi.org/10.1007/s10904-023-02582-3","journal":{"identity":"journal-of-inorganic-and-organometallic-polymers-and-materials","isVorOnly":false,"title":"Journal of Inorganic and Organometallic Polymers and Materials"},"publishedOn":"2023-04-01 20:14:42","publishedOnDateReadable":"April 1st, 2023"},"versionCreatedAt":"2023-01-30 16:06:33","video":"","vorDoi":"10.1007/s10904-023-02582-3","vorDoiUrl":"https://doi.org/10.1007/s10904-023-02582-3","workflowStages":[]},"version":"v1","identity":"rs-2517839","journalConfig":"researchsquare"},"__N_SSP":true},"page":"/article/[identity]/[[...version]]","query":{"redirect":"/article/rs-2517839","identity":"rs-2517839","version":["v1"]},"buildId":"ehx78VzkSd0WSzXnipQa-","isFallback":false,"isExperimentalCompile":false,"dynamicIds":[84888],"gssp":true,"scriptLoader":[]}