Characterization of NiOAg thin film applicated as photocatalytic degradation of methylene blue dye waste in Yogyakarta textile factory

Characterization of NiOAg thin film applicated as photocatalytic degradation of methylene blue dye waste in Yogyakarta textile factory | 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 Characterization of NiOAg thin film applicated as photocatalytic degradation of methylene blue dye waste in Yogyakarta textile factory Trimarji Atmono, Agus Purwadi, Taxwim Taxwim, Asih Melati, Usman Sudjadi This is a preprint; it has not been peer reviewed by a journal. https://doi.org/ 10.21203/rs.3.rs-3611170/v1 This work is licensed under a CC BY 4.0 License Status: Posted Version 1 posted You are reading this latest preprint version Abstract Thin films NiOAg were growth onto glass substrates by RF sputtering technique at the Radio Frequency of 13.56 MHz with variation of oxygen pressure. The research was conducted about preparation and characterization of NiOAg thin films, applicated as a photocatalyst degradation of methylene blue. XRD analysis showed stronger intensity (111) and (200) planes at peak 2θ of 37.66 0 and 43,23 0 . EDX analysis showed the following composition, Ni = 40.45%, Ag = 13.01%, and O = 46.53%. Based on UV-Vis, it was found the band gap energy of 2.8 eV, 3.1 eV and 3.2 eV, for oxygen pressure 0.05; 0.1 and 0.15 x 10 − 2 mbar, respectively. From the experiment of degradation of methylene blue, that was taken from textile factory dye waste in Yogyakarta/Indonesia, it was obtained the best value of degradation by 91.96%. RF-sputtering NiO/Ag methylene blue oxygen partial band gap energy Figures Figure 1 Figure 2 Figure 3 Figure 4 Figure 5 Figure 6 Figure 7 INTRODUCTION Textile dye waste contributes significantly to air pollution if it is not treated. In addition to the air ecosystem, textile substances can also reduce environmental aesthetics, cause unpleasant odors, and interfere with the use of air in human activities. Liquid waste from the textile industry contains reactive, toxic residues, hazardous chemicals and substances that are difficult to degrade [ 1 – 3 ]. One example of a dye that is often used is methylene blue which is a synthetic dye commonly used in textile dyeing. The use of methylene blue in addition to its cheap price, this compound is easy to obtain, easy to use and produces good colors. It is a hydrocarbon compound containing benzene which is difficult to degrade and canonical dye with strong adsorption power [ 4 ]. This dye waste results in excessive amounts of pollutants. Methylene blue dye is one of the most famous water contaminants that cause many health problems such as abdominal disorders, respiratory distress, skin sensitization, and blindness [ 5 – 7 ]. Also, methylene blue dye adversely affects the environment and damages the balance of the ecosystem. It blocks light permeation for aquatic organisms and thus threatens their life. Thus, the removal of this dye from water is foremost for keeping up the environment [ 8 ]. The degradation of methylene blue compounds with high concentrations is slower than its accumulation. So that the dye will be more easily accumulated to the bottom of the water than degraded [ 9 ]. Several methods have been developed for removing methylene blue dye, for example, adsorption, coagulation or flocculation, membrane filtration [ 10 ]. Adsorption is one of the popular methods in the community. However, this method has not been effective in reducing textile dyestuff pollution. The adsorption method is simple, easy, and efficient. Materials, which were utilized for the adsorption technique, such as zeolite, activated carbon, multiwalled carbon nanotubes, and polymers are characterized by high cost due to the consumption of energy and expensive chemicals during their preparation [ 11 , 12 ]. The use of relatively expensive materials and residual substances color that still accumulates in the absorbent, causing new problems. According to Chen [ 13 ], the use of semiconductors as photocatalysts in waste treatment has advantages, including being environmentally friendly because the reagents are electrons and holes that come from the excitation process that occurs in oxide semiconductors due to exposure to ultraviolet photon radiation, as well as being flexible where electrons and holes can react. With pollutants in the form of liquid or gas, the time required is relatively short, does not require complicated analysis and does not leave residue. Among the many semiconductors used, Nickel Oxide (NiO) has a good capacity because it has the ability to remove dye contamination physically and chemically which is environmentally friendly. NiO is a semiconductor with a wide band gap between the valence and conduction bands [ 14 ]. NiO has a band gap of 3.4-4.0 eV, which is similar to TiO2, resulting in higher quantum efficiencies (the ratio of electron-pair holes caused by photons) and effective photocatalytic [ 15 ]. The use of NiO as a photocatalyst can increase the water decomposition reaction, where hydrogen gas is formed on the surface of nickel oxide while oxygen gas is released from the surface of the photocatalyst. In the process NiO is expected to degrade pollutants such as dyes, organic waste, bacteria and so on into environmentally friendly compounds such as H 2 O or CO 2 [ 16 ]. NiO has advantages such as having a slow oxidation rate, non-toxicity, and chemical stability [ 17 ]. In several studies, NiO is widely used to treat various wastes, such as phenol waste, water pollution, paper-making waste, and so on. The degradation activity of the dye waste can be increased by the addition of dopants on the semiconductor NiO. The addition of dopants selected materials that have a reduction potential that is not an electron acceptor, can improve charge separation, and inhibits electron and hole recombination. Silver (Ag) has these characteristics as a dopant. NiOAg semiconductor material can be deposited into a layer, both chemically and physically. Several thin layer deposition techniques include chemical bath deposition, Sol-Gel and sputtering techniques [ 18 ]. In this study, the RF sputtering technique was used. Rf sputtering is an effective method for depositing high quality thin films of oxides, carbides and nitrides of metals and Semiconductors [ 19 ]. The process is capable of obtaining high quality thin films with high deposition rates, good adhesion, uniformity in surface morphology, ease of operation and economical for depositing even large areas at room temperature without the need for melting as in thermal spraying [ 20 ]. Layer/sample deposition by utilizing RF waves has several advantages such as being able to deposit insulating materials, the adhesive power of sputtered materials is stronger and can deposit thin films more homogeneously [ 21 , 22 ]. Finally, the tested thin layer was used as a photocatalyst for the degradation of methylene blue dye using UV radiation for 4 hours for each variation of oxygen pressure. METHODS OF EXPERIMENT Preparation of NiOAg thin layer was carried out onto glass substrate, using the RF-sputtering method at a frequency of 13.56 MHz, vacuum pressure of 3x10 − 6 mbar, with a bias voltage of -700 V, corresponding to 65 watts of power. The pressure of argon (as sputter gas) was held constant at 3.0x10 − 2 mbar, while the pressure of oxygen was variated at (0.5; 1.0 and 1.5) x10⁻ ² mbar. An Ag plate with a size of 15 mm x 1.5 mm, put on the Ni material having diameter of 75 mm, forming a mosaic target arrangement, installed as cathode. SEM/EDX characterization aims to determine the crystalline and composition of the thin films, while XRD observations were to analyze the crystal structure/the corresponding planes. The degradation test for methylene blue was carried out using a UV-Vis spectrophotometer by measuring the solution with concentrations of 0; 2; 4; 6; 8 and 10 ppm. The maximum wavelength was determined by measuring a standard solution of 10 ppm at a wavelength of 300–800 nm using UV-Vis spectrophotometry. The wavelength that gives the highest absorbance value is the maximum wavelength. The standard curve is made by measuring absorbance value of each concentration at the maximum wavelength of methylene blue solution. The photodegradation test was carried out to determine the activity of the NiOAg photocatalyst against 10 ppm methylene blue dye. The sample was taken from textile factory dye waste in Yogyakarta/Indonesia. The degradation process requires three main components of a light source (photons), a target compound, and a photocatalyst. In this study, the light source came from a UV lamp with a wavelength of 385 nm and a power of 60 watts used to evaluate the process. The target compound is a solution of methylene blue and a photocatalyst NiOAg. Determination of methylene blue degradation using a thin layer of NiOAg and UV irradiation for 4 hours. After the degradation process of the methylene blue solution was successful, the absorbance was measured using UV-Vis spectroscopy at a wavelength of 663 nm. The simple illustration of the degradation process mechanism can be observed in Fig. 2 . RESULT/DISCUSSION The X-ray diffraction pattern of a thin layer NiOAg sputtered onto a glass substrate with oxygen pressure of 0.1 × 10 − 2 mbar which was deposited for 15 minutes, resulted in a thicker layer, so that when characterized by using XRD can be diffracted perfectly. The result of the XRD analysis is shown in Fig. 3 (a). It is compatible with data sheet no. 96-101-0096 and 96-901-3048 on the Match3 app. Based on the analysis of the crystal structure of the thin layer, two peaks were observed, at 37.660 o and 43.320 o which is the peak of Ag and NiO, respectively, these peaks correspond to (111) and (200) which are part of the face center cubic (FCC) crystal structure [ 23 , 24 ]. Based on the graph, the grain size (D) based on the Scherrer formula has a D value of 90.045 nm and 91.61 nm. It is reported that there is a decrease in peak intensity (200) with increasing oxygen pressure in the chamber [ 18 ]. According to research states that high oxygen pressure will result in crystal defects. These crystal defects will affect the nucleation and growth of the thin film. In this research, the SEM-EDX test was carried out on samples of the NiOAg that was sputtered at oxygen pressure of 0.15 × 10 − 2 mbar with a deposition time of 15 minutes. The longer the deposition time, the thicker the layer deposited on the substrate, and the atomic arrangement will be closer together so that by the characterization using SEM and EDX the light source can be perfectly reflected, nevertheless the length of deposition time does not significantly affect the percentage of elements that are sputtered [ 13 , 25 ]. The morphological structure can be clearly revealed, the analysis was carried out with a magnification of 50,000 times. SEM characterization sample micrograph is presented in Fig. 3 (b). At the magnification of 50,000 times, it has showed that the NiOAg particles form clusters with a regular structure as a result of deposition using RF sputtering which has the property of being able to deposit a more homogeneous thin layer. In this case, the ordered particles are formed through the process of deposition, in which the target material is bombarded by high-energy atoms of argon as an inert gas in the sputtering process. Analysis with a higher magnification result in blurry, unclear and discharge occurs when the test is carried out, there are particles that are not homogeneous and appear larger than the other homogeneous particles. Based on measurements by XRD, it follows that the particles have an average size of 50.8 nm, as shown in Fig. 4 . EDX analysis is used to complete the quantitative test in identifying the elements. The results of the EDX test is shown quantitatively in Table 1 below. Table 1 E lements contains in NiOAg Element Weight % Atomic % O K 46,53 74,68 Ag L 13,01 2,89 Ni K 40,45 22,43 Based on the results of EDX characterization, it is known that the microstructure of the NiOAg thin film sample with the effect of 0.15 × 10 − 2 mbar oxygen pressure on RF sputtering contains elements of Ni, Ag, O, Mg, Ca, Si. The element Si has the highest percentage in the chemical composition because it has a high absorption but emits little energy. The percentage of Si has the highest amount because the substrate used as a place for molecular condensation comes from glass preparations containing Si, Ca, and Mg, it means that the element Si is an impurity material. The sputtered oxygen particles also condense to form crystal grains on the substrate. Therefore, according Berrios [ 26 ] it is said that the presence of sputtered oxygen pressure affects the decrease in the deposition rate. The deposition rate will gradually be low because the oxygen pressure is high, and the deposition rate will be high at low oxygen pressure. The pressure of oxygen flowing in the plasma chamber causes a change in the chemical composition of the thin film. Optical Properties of NiOAg Thin Layer Figure. 5(a) shows UV-Vis spectrophotometric characterization, from which it can be seen the relationship between wavelength and the transmittance of the thin film. In this research, a UV-Vis test was carried out on samples of the NiOAg thin film with variations in oxygen pressure when it was deposited by RF sputtering. It shows that the greater the oxygen pressure, the more transparent the thin layer, because the pressure of oxygen flowing into the sputter chamber will affect the sputtering process, the firing using argon ions towards the target surface will be inhibited. So, the transmittance of the layer will be even greater. This is because the more transparent a layer is, the sparser distance of the constituent atoms are, as well as the collisions of used light with atoms of thin film, the fewer collisions of light particles with atoms, making it easier for light to pass through the layer. The thickness of the coating affects several optical properties of the material, including absorbance and transmittance. The more transparent the layer, the smaller the absorbance value and the greater the transmittance value. The results of testing the optical properties of the NiOAg thin film show that the increase in transmittance occurs when exposed to the UV light spectrum at a wavelength of 300–400 nm. However, at 0.15×10 − 2 mbar oxygen pressure there is a deviation in the increase in the transmittance value. A significant increase occurs in the UV to visible light range at a wavelength of 300–480 nm, because there are several phenomena that affect the analysis process. The transmittance value at oxygen pressure of 0.05×10 − 2 mbar and 0.1×10 − 2 mbar does not increase drastically because visible light has a wavelength value of ± 400–800 nm. At a wavelength of 400 nm visible light emitted will be slightly passed by the material, so that only light with a certain wavelength will be absorbed. The high optical transmittance is caused by the homogeneity of the structural properties and crystallinity, while the low optical band is caused by irregular crystallinity, resulting in a lot of light scattering. If light with a various wavelength (polychromatic light) hits a sample, a certain wavelength will be absorbed. In molecules, valence electrons have an important role that can move (excitation), spin (rotate) and vibrate (vibrate) when they get an energy from outside. From this event, electrons will move from the ground state to the excited state. These phenomena are used to determine the optical properties and values of the band gap. The relationship between the direct band gap (αhʋ) and the photon energy (hʋ) determined from the Swanepoel equation [ 27 ] is then connected to the Tauc relationship for the energy width of band gap (E g ) as shown in Eqs. 1 and 2 \(\alpha =A\frac{{(hv-E)}^{1/2}}{hv}\) (Eq. 1) \(\left(\alpha hv\right)=A{(hv-{E}_{g})}^{1/2}\) (Eq;2) A is a constant, and \(\alpha\) obtained from the relationship as shown in Eq. 3. \(\alpha =(1 /d)\text{ln}\left(T\right)\) (Eq. 3) (𝛼 is the absorption coefficient (cm −1 ), T is the transmittance and d is the layer thickness) The absorbance value decreases for a larger wavelength because at a larger wavelength it is the wavelength range of visible light, which has a photon energy smaller than the photon energy possessed by UV light. The decrease is also an absorption characteristic of the semiconductor. This is because the more transparent a sample means the more layers formed; the more NiOAg molecules involved in light absorption. Measurement of the energy band gap of a semiconductor material is determined by drawing a line from the relationship (𝛼ℎ𝑣) 2 as shown in Fig. 5 (b). It shows that oxygen pressure affects the width of the band gap energy of the NiOAg thin film. The greater the oxygen pressure, the smaller the energy band gap of the thin film. The smallest slit width is indicated by an oxygen pressure of 0.15×10 − 2 mbar followed by a pressure of 0.1×10 − 2 mbar, and 0.05×10 − 2 mbar. The decrease in the energy band gap with increasing oxygen pressure can be caused by the quality of the thin film produced in the sputtering process. Band gap energy shows the movement of electrons across the valence band to the conduction band, the absorption value increases so that the energy absorbed by the material increases and causes the band gap energy value to decrease. The absorbance of methylene blue solution using a UV-Vis spectrophotometer at a wavelength of 300–800 nm is shown in Fig. 6 (a) below. Measurements were taken at 0; 1; 2; 3 and 4 hours. The maximum wavelength of 663 nm was obtained. The wavelength value is almost close to the reference which has a wavelength of 665 nm [ 28 ]. The calibration of methylene blue was determined by measuring the absorbance of the standard solution at a wavelength of 663 nm with a concentration of 0; 2; 4; 6; 8; 10 ppm. So that the resulting regression equation from the curve is y = bx - a. In Fig. 6 (b), it can be seen that the regression equation for the resulting methylene blue standard curve is y = 0.1288x-0.0606 and the relation coefficient (R 2 ) is 0.9913 which shows a linear curve. The regression equation was used to determine the concentration of the methylene blue solution after being degraded. The value (y) is the absorbance of the solution while the value (x) is the concentration obtained. The degradation results shown in Fig. 7 state that methylene blue experienced an increase in the percentage (%) of degradation along with increasing irradiation time. At 0.15 × 10 − 2 mbar oxygen pressure, the degradation was 91.96%. It does provide a significant value in degradation of methylene blue dye waste, although the effect of variations in oxygen pressure is not very visible. When the semiconductor is exposed to light with the appropriate energy, there will be e-mobility activity from the valence band to the conduction band, resulting in h + in the valence band. Most of these e − and h + pairs will recombine, both on the particle surface and in the NiOAg catalyst. Meanwhile, some e − and h + pairs will carry out oxidation and reduction reactions around the semiconductor surface [ 15 ]. When there is absorption of photons whose energy exceeds the band gap energy difference, there will be a release of heat energy due to the recombination of e − and h + in the semiconductor, so that the surface is stable due to trapping of e − and h + . Most photodegradation reactions use the power of h + to oxidize, so to maintain the charge it is necessary to add other species that can be reduced by electrons [ 13 ]. The charge carrier can be activated by adding doping, namely metal elements [ 13 ]. One of them is Ag metal doping, that will cause a change in the distribution of electrons which results in a change in properties. In this context, metal doping is able to modulate the electronic structure of the catalyst material. The combination of the two materials results therefore in the formation of clusters to increase the efficiency of the photocatalyst reaction [ 29 ]. CONCLUSION The NiOAg thin layers were successfully prepared by means of RF sputtering technique at 13, 56 MHz, followed by characterization using XRD, SEM, EDX, UV-Vis, and proven to be able to degrade methylene blue on the textile fabric. By utilizing ultraviolet light, where layer prepared with oxygen pressure of 0.15 × 10 − 2 mbar has the highest percentage capable of degrading methylene blue by 91.96%. Although the effect of variations in oxygen pressure is not very significant, it does provide a significant value in degradation of methylene blue dye waste of textile factory in Yogyakarta. Declarations ACKNOWLEDGMENT The authors would like to acknowledge KEMENRISTEKDIKTI for the research financial support. CONFLICT OF INTEREST The authors declare that they have no conflict of interest. CREDIT AUTHORSHIP CONTRIBUTION STATEMENT Trimarji Atmono : Investigation, methodology, conceptualization, formal analysis, data curation, writing -original draft; writing -review & editing. Agus Purwadi: conceptualization, formal analysis, methodology, writing -review & editing.Taxwim: methodology, data curation. Asih Melati: writing – review & supervision. INFORMED CONSENT All Authors involved in this study provided written informed consent prior to their inclusion. The informed consent process included detailed information about the study's purpose, procedures, potential risks, and the voluntary nature of participation. Additionally, participants were explicitly informed about the use of their data for publication purposes, and written consent to publish their anonymized results was obtained. The study protocol, including the consent forms, was reviewed and approved by the The National Research Agency of Republic Indonesia and Islamic state University Sunan Kalijaga Yogyakarta. DATA AVAILABILITY The Authors confirm that the data supporting the findings of the study are available within the article. 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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-3611170","acceptedTermsAndConditions":true,"allowDirectSubmit":true,"archivedVersions":[],"articleType":"Research Article","associatedPublications":[],"authors":[{"id":254735222,"identity":"8e3162f3-1d84-4722-a3c0-e701af723d80","order_by":0,"name":"Trimarji 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Agency/BRIN","correspondingAuthor":false,"submittingAuthor":false,"prefix":"","firstName":"Agus","middleName":"","lastName":"Purwadi","suffix":""},{"id":254735227,"identity":"93266a5d-8df8-4b93-9e4d-ccb2dbf7fd6a","order_by":2,"name":"Taxwim Taxwim","email":"","orcid":"","institution":"National Research and Innovation Agency/BRIN","correspondingAuthor":false,"submittingAuthor":false,"prefix":"","firstName":"Taxwim","middleName":"","lastName":"Taxwim","suffix":""},{"id":254735230,"identity":"78f7f541-6bd3-4167-9033-8069a6d87591","order_by":3,"name":"Asih Melati","email":"","orcid":"","institution":"Universitas Islam Negeri /UIN Sunan Kalijaga","correspondingAuthor":false,"submittingAuthor":false,"prefix":"","firstName":"Asih","middleName":"","lastName":"Melati","suffix":""},{"id":254735232,"identity":"3a044931-e2db-4cda-8f81-c0e7ef71d319","order_by":4,"name":"Usman Sudjadi","email":"","orcid":"","institution":"National Research and Innovation Agency/BRIN","correspondingAuthor":false,"submittingAuthor":false,"prefix":"","firstName":"Usman","middleName":"","lastName":"Sudjadi","suffix":""}],"badges":[],"createdAt":"2023-11-14 15:59:22","currentVersionCode":1,"declarations":"","doi":"10.21203/rs.3.rs-3611170/v1","doiUrl":"https://doi.org/10.21203/rs.3.rs-3611170/v1","draftVersion":[],"editorialEvents":[],"editorialNote":"","failedWorkflow":false,"files":[{"id":47469458,"identity":"ea93b408-54b9-46c3-a026-a47496264744","added_by":"auto","created_at":"2023-12-02 01:55:07","extension":"png","order_by":1,"title":"Figure 1","display":"","copyAsset":false,"role":"figure","size":313789,"visible":true,"origin":"","legend":"\u003cp\u003eRF Sputtering system for preparation of NiOAg layer\u003c/p\u003e","description":"","filename":"1.png","url":"https://assets-eu.researchsquare.com/files/rs-3611170/v1/84e657eff6b206ea4ec2f640.png"},{"id":47469456,"identity":"6c00b213-404d-4c3b-8db1-080f02913314","added_by":"auto","created_at":"2023-12-02 01:55:07","extension":"png","order_by":2,"title":"Figure 2","display":"","copyAsset":false,"role":"figure","size":67029,"visible":true,"origin":"","legend":"\u003cp\u003eSimple illustration of experimental to degrade the methylene blue.\u003c/p\u003e","description":"","filename":"2.png","url":"https://assets-eu.researchsquare.com/files/rs-3611170/v1/1d8207b52d455d6c64cf8e43.png"},{"id":47469934,"identity":"e971dc48-1943-4baa-b869-daf81c796993","added_by":"auto","created_at":"2023-12-02 02:03:07","extension":"png","order_by":3,"title":"Figure 3","display":"","copyAsset":false,"role":"figure","size":461739,"visible":true,"origin":"","legend":"\u003cp\u003eXRD, SEM and EDX characterization of NiOAg\u003c/p\u003e","description":"","filename":"3.png","url":"https://assets-eu.researchsquare.com/files/rs-3611170/v1/9b6d10a5685d88e16cd80196.png"},{"id":47469461,"identity":"4202011b-fd81-4525-b7fb-07f0baa08194","added_by":"auto","created_at":"2023-12-02 01:55:07","extension":"png","order_by":4,"title":"Figure 4","display":"","copyAsset":false,"role":"figure","size":250287,"visible":true,"origin":"","legend":"\u003cp\u003eGraph of the average pore diameter of the NiOAg\u003c/p\u003e","description":"","filename":"4.png","url":"https://assets-eu.researchsquare.com/files/rs-3611170/v1/94986a46460785f391545f1d.png"},{"id":47469933,"identity":"42be2602-635a-47ae-ae74-6bb2e959eda7","added_by":"auto","created_at":"2023-12-02 02:03:07","extension":"png","order_by":5,"title":"Figure 5","display":"","copyAsset":false,"role":"figure","size":212671,"visible":true,"origin":"","legend":"\u003cp\u003e\u003cstrong\u003e(a)\u003c/strong\u003e Graph of the relationship between wavelength (nm) and % transmittance.\u003c/p\u003e\n\u003cp\u003e\u003cstrong\u003e(b)\u003c/strong\u003e Band gap as function of photon energy.\u003c/p\u003e","description":"","filename":"5.png","url":"https://assets-eu.researchsquare.com/files/rs-3611170/v1/c6d6d2313b86f29d58f6bd38.png"},{"id":47469460,"identity":"3213c3ee-a931-49e1-b1f4-fe57d5317a8f","added_by":"auto","created_at":"2023-12-02 01:55:07","extension":"png","order_by":6,"title":"Figure 6","display":"","copyAsset":false,"role":"figure","size":268639,"visible":true,"origin":"","legend":"\u003cp\u003e\u003cstrong\u003e(a)\u003c/strong\u003e Spectra of methylene blue dye from UV-Vis analysis.\u003c/p\u003e\n\u003cp\u003e\u003cstrong\u003e(b)\u003c/strong\u003eLinear regression of methylene blue standard solution.\u003c/p\u003e","description":"","filename":"6.png","url":"https://assets-eu.researchsquare.com/files/rs-3611170/v1/fba6d89e9205ffa2b9017818.png"},{"id":47469457,"identity":"dbbb5c4b-0c48-4448-b8a6-8f9769074815","added_by":"auto","created_at":"2023-12-02 01:55:07","extension":"png","order_by":7,"title":"Figure 7","display":"","copyAsset":false,"role":"figure","size":82518,"visible":true,"origin":"","legend":"\u003cp\u003eOptimization of methylene blue degradation.\u003c/p\u003e","description":"","filename":"7.png","url":"https://assets-eu.researchsquare.com/files/rs-3611170/v1/4a412ccef23c5f5e37ea7fa5.png"},{"id":47570403,"identity":"551e0a1c-123c-4cca-a007-d1308e00a5c1","added_by":"auto","created_at":"2023-12-04 17:14:42","extension":"pdf","order_by":0,"title":"","display":"","copyAsset":false,"role":"manuscript-pdf","size":1699929,"visible":true,"origin":"","legend":"","description":"","filename":"manuscript.pdf","url":"https://assets-eu.researchsquare.com/files/rs-3611170/v1/627583de-4dd8-4f41-8808-03b7c27c9429.pdf"}],"financialInterests":"No competing interests reported.","formattedTitle":"Characterization of NiOAg thin film applicated as photocatalytic degradation of methylene blue dye waste in Yogyakarta textile factory","fulltext":[{"header":"INTRODUCTION","content":"\u003cp\u003eTextile dye waste contributes significantly to air pollution if it is not treated. In addition to the air ecosystem, textile substances can also reduce environmental aesthetics, cause unpleasant odors, and interfere with the use of air in human activities. Liquid waste from the textile industry contains reactive, toxic residues, hazardous chemicals and substances that are difficult to degrade [\u003cspan additionalcitationids=\"CR2\" citationid=\"CR1\" class=\"CitationRef\"\u003e1\u003c/span\u003e\u0026ndash;\u003cspan citationid=\"CR3\" class=\"CitationRef\"\u003e3\u003c/span\u003e]. One example of a dye that is often used is methylene blue which is a synthetic dye commonly used in textile dyeing. The use of methylene blue in addition to its cheap price, this compound is easy to obtain, easy to use and produces good colors. It is a hydrocarbon compound containing benzene which is difficult to degrade and canonical dye with strong adsorption power [\u003cspan citationid=\"CR4\" class=\"CitationRef\"\u003e4\u003c/span\u003e]. This dye waste results in excessive amounts of pollutants. Methylene blue dye is one of the most famous water contaminants that cause many health problems such as abdominal disorders, respiratory distress, skin sensitization, and blindness [\u003cspan additionalcitationids=\"CR6\" citationid=\"CR5\" class=\"CitationRef\"\u003e5\u003c/span\u003e\u0026ndash;\u003cspan citationid=\"CR7\" class=\"CitationRef\"\u003e7\u003c/span\u003e]. Also, methylene blue dye adversely affects the environment and damages the balance of the ecosystem. It blocks light permeation for aquatic organisms and thus threatens their life. Thus, the removal of this dye from water is foremost for keeping up the environment [\u003cspan citationid=\"CR8\" class=\"CitationRef\"\u003e8\u003c/span\u003e]. The degradation of methylene blue compounds with high concentrations is slower than its accumulation. So that the dye will be more easily accumulated to the bottom of the water than degraded [\u003cspan citationid=\"CR9\" class=\"CitationRef\"\u003e9\u003c/span\u003e].\u003c/p\u003e \u003cp\u003eSeveral methods have been developed for removing methylene blue dye, for example, adsorption, coagulation or flocculation, membrane filtration [\u003cspan citationid=\"CR10\" class=\"CitationRef\"\u003e10\u003c/span\u003e]. Adsorption is one of the popular methods in the community. However, this method has not been effective in reducing textile dyestuff pollution. The adsorption method is simple, easy, and efficient. Materials, which were utilized for the adsorption technique, such as zeolite, activated carbon, multiwalled carbon nanotubes, and polymers are characterized by high cost due to the consumption of energy and expensive chemicals during their preparation [\u003cspan citationid=\"CR11\" class=\"CitationRef\"\u003e11\u003c/span\u003e, \u003cspan citationid=\"CR12\" class=\"CitationRef\"\u003e12\u003c/span\u003e]. The use of relatively expensive materials and residual substances color that still accumulates in the absorbent, causing new problems. According to Chen [\u003cspan citationid=\"CR13\" class=\"CitationRef\"\u003e13\u003c/span\u003e], the use of semiconductors as photocatalysts in waste treatment has advantages, including being environmentally friendly because the reagents are electrons and holes that come from the excitation process that occurs in oxide semiconductors due to exposure to ultraviolet photon radiation, as well as being flexible where electrons and holes can react. With pollutants in the form of liquid or gas, the time required is relatively short, does not require complicated analysis and does not leave residue.\u003c/p\u003e \u003cp\u003eAmong the many semiconductors used, Nickel Oxide (NiO) has a good capacity because it has the ability to remove dye contamination physically and chemically which is environmentally friendly. NiO is a semiconductor with a wide band gap between the valence and conduction bands [\u003cspan citationid=\"CR14\" class=\"CitationRef\"\u003e14\u003c/span\u003e]. NiO has a band gap of 3.4-4.0 eV, which is similar to TiO2, resulting in higher quantum efficiencies (the ratio of electron-pair holes caused by photons) and effective photocatalytic [\u003cspan citationid=\"CR15\" class=\"CitationRef\"\u003e15\u003c/span\u003e]. The use of NiO as a photocatalyst can increase the water decomposition reaction, where hydrogen gas is formed on the surface of nickel oxide while oxygen gas is released from the surface of the photocatalyst. In the process NiO is expected to degrade pollutants such as dyes, organic waste, bacteria and so on into environmentally friendly compounds such as H\u003csub\u003e2\u003c/sub\u003eO or CO\u003csub\u003e2\u003c/sub\u003e [\u003cspan citationid=\"CR16\" class=\"CitationRef\"\u003e16\u003c/span\u003e]. NiO has advantages such as having a slow oxidation rate, non-toxicity, and chemical stability [\u003cspan citationid=\"CR17\" class=\"CitationRef\"\u003e17\u003c/span\u003e]. In several studies, NiO is widely used to treat various wastes, such as phenol waste, water pollution, paper-making waste, and so on. The degradation activity of the dye waste can be increased by the addition of dopants on the semiconductor NiO. The addition of dopants selected materials that have a reduction potential that is not an electron acceptor, can improve charge separation, and inhibits electron and hole recombination. Silver (Ag) has these characteristics as a dopant.\u003c/p\u003e \u003cp\u003eNiOAg semiconductor material can be deposited into a layer, both chemically and physically. Several thin layer deposition techniques include chemical bath deposition, Sol-Gel and sputtering techniques [\u003cspan citationid=\"CR18\" class=\"CitationRef\"\u003e18\u003c/span\u003e]. In this study, the RF sputtering technique was used. Rf sputtering is an effective method for depositing high quality thin films of oxides, carbides and nitrides of metals and Semiconductors [\u003cspan citationid=\"CR19\" class=\"CitationRef\"\u003e19\u003c/span\u003e]. The process is capable of obtaining high quality thin films with high deposition rates, good adhesion, uniformity in surface morphology, ease of operation and economical for depositing even large areas at room temperature without the need for melting as in thermal spraying [\u003cspan citationid=\"CR20\" class=\"CitationRef\"\u003e20\u003c/span\u003e]. Layer/sample deposition by utilizing RF waves has several advantages such as being able to deposit insulating materials, the adhesive power of sputtered materials is stronger and can deposit thin films more homogeneously [\u003cspan citationid=\"CR21\" class=\"CitationRef\"\u003e21\u003c/span\u003e, \u003cspan citationid=\"CR22\" class=\"CitationRef\"\u003e22\u003c/span\u003e]. Finally, the tested thin layer was used as a photocatalyst for the degradation of methylene blue dye using UV radiation for 4 hours for each variation of oxygen pressure.\u003c/p\u003e"},{"header":"METHODS OF EXPERIMENT","content":"\u003cp\u003ePreparation of NiOAg thin layer was carried out onto glass substrate, using the RF-sputtering method at a frequency of 13.56 MHz, vacuum pressure of 3x10\u003csup\u003e\u0026minus;\u0026thinsp;6\u003c/sup\u003e mbar, with a bias voltage of -700 V, corresponding to 65 watts of power. The pressure of argon (as sputter gas) was held constant at 3.0x10\u003csup\u003e\u0026minus;\u0026thinsp;2\u003c/sup\u003e mbar, while the pressure of oxygen was variated at (0.5; 1.0 and 1.5) x10⁻ \u0026sup2; mbar. An Ag plate with a size of 15 mm x 1.5 mm, put on the Ni material having diameter of 75 mm, forming a mosaic target arrangement, installed as cathode.\u003c/p\u003e \u003cp\u003e \u003c/p\u003e \u003cp\u003eSEM/EDX characterization aims to determine the crystalline and composition of the thin films, while XRD observations were to analyze the crystal structure/the corresponding planes. The degradation test for methylene blue was carried out using a UV-Vis spectrophotometer by measuring the solution with concentrations of 0; 2; 4; 6; 8 and 10 ppm. The maximum wavelength was determined by measuring a standard solution of 10 ppm at a wavelength of 300\u0026ndash;800 nm using UV-Vis spectrophotometry. The wavelength that gives the highest absorbance value is the maximum wavelength. The standard curve is made by measuring absorbance value of each concentration at the maximum wavelength of methylene blue solution.\u003c/p\u003e \u003cp\u003eThe photodegradation test was carried out to determine the activity of the NiOAg photocatalyst against 10 ppm methylene blue dye. The sample was taken from textile factory dye waste in Yogyakarta/Indonesia. The degradation process requires three main components of a light source (photons), a target compound, and a photocatalyst. In this study, the light source came from a UV lamp with a wavelength of 385 nm and a power of 60 watts used to evaluate the process. The target compound is a solution of methylene blue and a photocatalyst NiOAg. Determination of methylene blue degradation using a thin layer of NiOAg and UV irradiation for 4 hours. After the degradation process of the methylene blue solution was successful, the absorbance was measured using UV-Vis spectroscopy at a wavelength of 663 nm. The simple illustration of the degradation process mechanism can be observed in Fig.\u0026nbsp;\u003cspan refid=\"Fig2\" class=\"InternalRef\"\u003e2\u003c/span\u003e.\u003c/p\u003e "},{"header":"RESULT/DISCUSSION","content":"\u003cdiv id=\"Sec3\" class=\"Section2\"\u003e \u003cp\u003eThe X-ray diffraction pattern of a thin layer NiOAg sputtered onto a glass substrate with oxygen pressure of 0.1 \u0026times; 10\u0026thinsp;\u0026minus;\u0026thinsp;2 mbar which was deposited for 15 minutes, resulted in a thicker layer, so that when characterized by using XRD can be diffracted perfectly. The result of the XRD analysis is shown in Fig.\u0026nbsp;\u003cspan refid=\"Fig3\" class=\"InternalRef\"\u003e3\u003c/span\u003e(a). It is compatible with data sheet no. 96-101-0096 and 96-901-3048 on the Match3 app. Based on the analysis of the crystal structure of the thin layer, two peaks were observed, at 37.660\u003csup\u003eo\u003c/sup\u003e and 43.320\u003csup\u003eo\u003c/sup\u003e which is the peak of Ag and NiO, respectively, these peaks correspond to (111) and (200) which are part of the face center cubic (FCC) crystal structure [\u003cspan citationid=\"CR23\" class=\"CitationRef\"\u003e23\u003c/span\u003e, \u003cspan citationid=\"CR24\" class=\"CitationRef\"\u003e24\u003c/span\u003e]. Based on the graph, the grain size (D) based on the Scherrer formula has a D value of 90.045 nm and 91.61 nm. It is reported that there is a decrease in peak intensity (200) with increasing oxygen pressure in the chamber [\u003cspan citationid=\"CR18\" class=\"CitationRef\"\u003e18\u003c/span\u003e]. According to research states that high oxygen pressure will result in crystal defects. These crystal defects will affect the nucleation and growth of the thin film.\u003c/p\u003e \u003cp\u003eIn this research, the SEM-EDX test was carried out on samples of the NiOAg that was sputtered at oxygen pressure of 0.15 \u0026times; 10\u003csup\u003e\u0026minus;\u0026thinsp;2\u003c/sup\u003e mbar with a deposition time of 15 minutes. The longer the deposition time, the thicker the layer deposited on the substrate, and the atomic arrangement will be closer together so that by the characterization using SEM and EDX the light source can be perfectly reflected, nevertheless the length of deposition time does not significantly affect the percentage of elements that are sputtered [\u003cspan citationid=\"CR13\" class=\"CitationRef\"\u003e13\u003c/span\u003e, \u003cspan citationid=\"CR25\" class=\"CitationRef\"\u003e25\u003c/span\u003e]. The morphological structure can be clearly revealed, the analysis was carried out with a magnification of 50,000 times. SEM characterization sample micrograph is presented in Fig.\u0026nbsp;\u003cspan refid=\"Fig3\" class=\"InternalRef\"\u003e3\u003c/span\u003e(b). At the magnification of 50,000 times, it has showed that the NiOAg particles form clusters with a regular structure as a result of deposition using RF sputtering which has the property of being able to deposit a more homogeneous thin layer. In this case, the ordered particles are formed through the process of deposition, in which the target material is bombarded by high-energy atoms of argon as an inert gas in the sputtering process. Analysis with a higher magnification result in blurry, unclear and discharge occurs when the test is carried out, there are particles that are not homogeneous and appear larger than the other homogeneous particles. Based on measurements by XRD, it follows that the particles have an average size of 50.8 nm, as shown in Fig.\u0026nbsp;\u003cspan refid=\"Fig4\" class=\"InternalRef\"\u003e4\u003c/span\u003e.\u003c/p\u003e \u003cp\u003eEDX analysis is used to complete the quantitative test in identifying the elements. The results of the EDX test is shown quantitatively in Table\u0026nbsp;\u003cspan refid=\"Tab1\" class=\"InternalRef\"\u003e1\u003c/span\u003e below.\u003c/p\u003e \u003cp\u003e \u003cdiv class=\"gridtable\"\u003e\u003ctable float=\"Yes\" id=\"Tab1\" border=\"1\"\u003e \u003ccaption language=\"En\"\u003e \u003cdiv class=\"CaptionNumber\"\u003eTable 1\u003c/div\u003e \u003cdiv class=\"CaptionContent\"\u003e \u003cp\u003e\u003cb\u003eE\u003c/b\u003elements contains in NiOAg\u003c/p\u003e \u003c/div\u003e \u003c/caption\u003e \u003ccolgroup cols=\"3\"\u003e \u003cdiv align=\"left\" class=\"colspec\" colname=\"c1\" colnum=\"1\"\u003e\u003c/div\u003e \u003cdiv align=\"char\" char=\".\" class=\"colspec\" colname=\"c2\" colnum=\"2\"\u003e\u003c/div\u003e \u003cdiv align=\"char\" char=\".\" class=\"colspec\" colname=\"c3\" colnum=\"3\"\u003e\u003c/div\u003e \u003cthead\u003e \u003ctr\u003e \u003cth align=\"left\" colname=\"c1\"\u003e \u003cp\u003eElement\u003c/p\u003e \u003c/th\u003e \u003cth align=\"left\" colname=\"c2\"\u003e \u003cp\u003eWeight %\u003c/p\u003e \u003c/th\u003e \u003cth align=\"left\" colname=\"c3\"\u003e \u003cp\u003eAtomic %\u003c/p\u003e \u003c/th\u003e \u003c/tr\u003e \u003c/thead\u003e \u003ctbody\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003eO K\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c2\"\u003e \u003cp\u003e46,53\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c3\"\u003e \u003cp\u003e74,68\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003eAg L\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c2\"\u003e \u003cp\u003e13,01\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c3\"\u003e \u003cp\u003e2,89\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003eNi K\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c2\"\u003e \u003cp\u003e40,45\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c3\"\u003e \u003cp\u003e22,43\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003c/tbody\u003e \u003c/colgroup\u003e \u003c/table\u003e\u003c/div\u003e \u003c/p\u003e \u003cp\u003eBased on the results of EDX characterization, it is known that the microstructure of the NiOAg thin film sample with the effect of 0.15 \u0026times; 10\u0026thinsp;\u0026minus;\u0026thinsp;2 mbar oxygen pressure on RF sputtering contains elements of Ni, Ag, O, Mg, Ca, Si. The element Si has the highest percentage in the chemical composition because it has a high absorption but emits little energy. The percentage of Si has the highest amount because the substrate used as a place for molecular condensation comes from glass preparations containing Si, Ca, and Mg, it means that the element Si is an impurity material. The sputtered oxygen particles also condense to form crystal grains on the substrate. Therefore, according Berrios [\u003cspan citationid=\"CR26\" class=\"CitationRef\"\u003e26\u003c/span\u003e] it is said that the presence of sputtered oxygen pressure affects the decrease in the deposition rate. The deposition rate will gradually be low because the oxygen pressure is high, and the deposition rate will be high at low oxygen pressure. The pressure of oxygen flowing in the plasma chamber causes a change in the chemical composition of the thin film.\u003c/p\u003e \u003c/div\u003e \u003cdiv id=\"Sec4\" class=\"Section2\"\u003e \u003ch2\u003eOptical Properties of NiOAg Thin Layer\u003c/h2\u003e \u003cp\u003eFigure. 5(a) shows UV-Vis spectrophotometric characterization, from which it can be seen the relationship between wavelength and the transmittance of the thin film. In this research, a UV-Vis test was carried out on samples of the NiOAg thin film with variations in oxygen pressure when it was deposited by RF sputtering. It shows that the greater the oxygen pressure, the more transparent the thin layer, because the pressure of oxygen flowing into the sputter chamber will affect the sputtering process, the firing using argon ions towards the target surface will be inhibited. So, the transmittance of the layer will be even greater. This is because the more transparent a layer is, the sparser distance of the constituent atoms are, as well as the collisions of used light with atoms of thin film, the fewer collisions of light particles with atoms, making it easier for light to pass through the layer. The thickness of the coating affects several optical properties of the material, including absorbance and transmittance. The more transparent the layer, the smaller the absorbance value and the greater the transmittance value.\u003c/p\u003e \u003cp\u003eThe results of testing the optical properties of the NiOAg thin film show that the increase in transmittance occurs when exposed to the UV light spectrum at a wavelength of 300\u0026ndash;400 nm. However, at 0.15\u0026times;10\u003csup\u003e\u0026minus;\u0026thinsp;2\u003c/sup\u003e mbar oxygen pressure there is a deviation in the increase in the transmittance value. A significant increase occurs in the UV to visible light range at a wavelength of 300\u0026ndash;480 nm, because there are several phenomena that affect the analysis process. The transmittance value at oxygen pressure of 0.05\u0026times;10\u003csup\u003e\u0026minus;\u0026thinsp;2\u003c/sup\u003e mbar and 0.1\u0026times;10\u003csup\u003e\u0026minus;\u0026thinsp;2\u003c/sup\u003e mbar does not increase drastically because visible light has a wavelength value of \u0026plusmn;\u0026thinsp;400\u0026ndash;800 nm. At a wavelength of 400 nm visible light emitted will be slightly passed by the material, so that only light with a certain wavelength will be absorbed. The high optical transmittance is caused by the homogeneity of the structural properties and crystallinity, while the low optical band is caused by irregular crystallinity, resulting in a lot of light scattering.\u003c/p\u003e \u003cp\u003eIf light with a various wavelength (polychromatic light) hits a sample, a certain wavelength will be absorbed. In molecules, valence electrons have an important role that can move (excitation), spin (rotate) and vibrate (vibrate) when they get an energy from outside. From this event, electrons will move from the ground state to the excited state. These phenomena are used to determine the optical properties and values of the band gap. The relationship between the direct band gap (αhʋ) and the photon energy (hʋ) determined from the Swanepoel equation [\u003cspan citationid=\"CR27\" class=\"CitationRef\"\u003e27\u003c/span\u003e] is then connected to the Tauc relationship for the energy width of band gap (E\u003csub\u003eg\u003c/sub\u003e) as shown in Eqs.\u0026nbsp;1 and 2\u003cdiv class=\"BlockQuote\"\u003e\u003cp\u003e \u003cspan class=\"InlineEquation\"\u003e \u003cspan class=\"mathinline\"\u003e\\(\\alpha =A\\frac{{(hv-E)}^{1/2}}{hv}\\)\u003c/span\u003e \u003c/span\u003e (Eq.\u0026nbsp;1)\u003c/p\u003e\u003cp\u003e \u003cspan class=\"InlineEquation\"\u003e \u003cspan class=\"mathinline\"\u003e\\(\\left(\\alpha hv\\right)=A{(hv-{E}_{g})}^{1/2}\\)\u003c/span\u003e \u003c/span\u003e (Eq;2)\u003c/p\u003e\u003c/div\u003e\u003c/p\u003e \u003cp\u003eA is a constant, and \u003cspan class=\"InlineEquation\"\u003e\u003cspan class=\"mathinline\"\u003e\\(\\alpha\\)\u003c/span\u003e\u003c/span\u003e obtained from the relationship as shown in Eq.\u0026nbsp;3.\u003c/p\u003e \u003cp\u003e \u003cspan class=\"InlineEquation\"\u003e \u003cspan class=\"mathinline\"\u003e\\(\\alpha =(1 /d)\\text{ln}\\left(T\\right)\\)\u003c/span\u003e \u003c/span\u003e (Eq.\u0026nbsp;3)\u003c/p\u003e \u003cp\u003e(\u0026#120572; is the absorption coefficient (cm\u003csup\u003e\u0026minus;1\u003c/sup\u003e), T is the transmittance and d is the layer thickness)\u003c/p\u003e \u003cp\u003eThe absorbance value decreases for a larger wavelength because at a larger wavelength it is the wavelength range of visible light, which has a photon energy smaller than the photon energy possessed by UV light. The decrease is also an absorption characteristic of the semiconductor. This is because the more transparent a sample means the more layers formed; the more NiOAg molecules involved in light absorption. Measurement of the energy band gap of a semiconductor material is determined by drawing a line from the relationship (\u0026#120572;ℎ\u0026#119907;)\u003csup\u003e2\u003c/sup\u003e as shown in Fig.\u0026nbsp;\u003cspan refid=\"Fig5\" class=\"InternalRef\"\u003e5\u003c/span\u003e(b).\u003c/p\u003e \u003cp\u003eIt shows that oxygen pressure affects the width of the band gap energy of the NiOAg thin film. The greater the oxygen pressure, the smaller the energy band gap of the thin film. The smallest slit width is indicated by an oxygen pressure of 0.15\u0026times;10\u003csup\u003e\u0026minus;\u0026thinsp;2\u003c/sup\u003e mbar followed by a pressure of 0.1\u0026times;10\u003csup\u003e\u0026minus;\u0026thinsp;2\u003c/sup\u003e mbar, and 0.05\u0026times;10\u003csup\u003e\u0026minus;\u0026thinsp;2\u003c/sup\u003e mbar. The decrease in the energy band gap with increasing oxygen pressure can be caused by the quality of the thin film produced in the sputtering process. Band gap energy shows the movement of electrons across the valence band to the conduction band, the absorption value increases so that the energy absorbed by the material increases and causes the band gap energy value to decrease.\u003c/p\u003e \u003cp\u003eThe absorbance of methylene blue solution using a UV-Vis spectrophotometer at a wavelength of 300\u0026ndash;800 nm is shown in Fig.\u0026nbsp;\u003cspan refid=\"Fig6\" class=\"InternalRef\"\u003e6\u003c/span\u003e(a) below. Measurements were taken at 0; 1; 2; 3 and 4 hours. The maximum wavelength of 663 nm was obtained. The wavelength value is almost close to the reference which has a wavelength of 665 nm [\u003cspan citationid=\"CR28\" class=\"CitationRef\"\u003e28\u003c/span\u003e].\u003c/p\u003e \u003c/div\u003e\n\u003cp\u003eThe calibration of methylene blue was determined by measuring the absorbance of the standard solution at a wavelength of 663 nm with a concentration of 0; 2; 4; 6; 8; 10 ppm. So that the resulting regression equation from the curve is y\u0026thinsp;=\u0026thinsp;bx - a. In Fig.\u0026nbsp;\u003cspan refid=\"Fig6\" class=\"InternalRef\"\u003e6\u003c/span\u003e(b), it can be seen that the regression equation for the resulting methylene blue standard curve is y\u0026thinsp;=\u0026thinsp;0.1288x-0.0606 and the relation coefficient (R\u003csup\u003e2\u003c/sup\u003e) is 0.9913 which shows a linear curve.\u003c/p\u003e \u003cp\u003eThe regression equation was used to determine the concentration of the methylene blue solution after being degraded. The value (y) is the absorbance of the solution while the value (x) is the concentration obtained.\u003c/p\u003e \u003cp\u003eThe degradation results shown in Fig.\u0026nbsp;\u003cspan refid=\"Fig7\" class=\"InternalRef\"\u003e7\u003c/span\u003e state that methylene blue experienced an increase in the percentage (%) of degradation along with increasing irradiation time.\u003c/p\u003e \u003cp\u003eAt 0.15 \u0026times; 10\u003csup\u003e\u0026minus;\u0026thinsp;2\u003c/sup\u003e mbar oxygen pressure, the degradation was 91.96%. It does provide a significant value in degradation of methylene blue dye waste, although the effect of variations in oxygen pressure is not very visible. When the semiconductor is exposed to light with the appropriate energy, there will be e-mobility activity from the valence band to the conduction band, resulting in h\u003csup\u003e+\u003c/sup\u003e in the valence band. Most of these e\u003csup\u003e\u0026minus;\u003c/sup\u003e and h\u003csup\u003e+\u003c/sup\u003e pairs will recombine, both on the particle surface and in the NiOAg catalyst. Meanwhile, some e\u003csup\u003e\u0026minus;\u003c/sup\u003e and h\u003csup\u003e+\u003c/sup\u003e pairs will carry out oxidation and reduction reactions around the semiconductor surface [\u003cspan citationid=\"CR15\" class=\"CitationRef\"\u003e15\u003c/span\u003e]. When there is absorption of photons whose energy exceeds the band gap energy difference, there will be a release of heat energy due to the recombination of e\u003csup\u003e\u0026minus;\u003c/sup\u003e and h\u003csup\u003e+\u003c/sup\u003e in the semiconductor, so that the surface is stable due to trapping of e\u003csup\u003e\u0026minus;\u003c/sup\u003e and h\u003csup\u003e+\u003c/sup\u003e. Most photodegradation reactions use the power of h\u003csup\u003e+\u003c/sup\u003e to oxidize, so to maintain the charge it is necessary to add other species that can be reduced by electrons [\u003cspan citationid=\"CR13\" class=\"CitationRef\"\u003e13\u003c/span\u003e]. The charge carrier can be activated by adding doping, namely metal elements [\u003cspan citationid=\"CR13\" class=\"CitationRef\"\u003e13\u003c/span\u003e]. One of them is Ag metal doping, that will cause a change in the distribution of electrons which results in a change in properties. In this context, metal doping is able to modulate the electronic structure of the catalyst material. The combination of the two materials results therefore in the formation of clusters to increase the efficiency of the photocatalyst reaction [\u003cspan citationid=\"CR29\" class=\"CitationRef\"\u003e29\u003c/span\u003e].\u003c/p\u003e"},{"header":"CONCLUSION","content":"\u003cp\u003eThe NiOAg thin layers were successfully prepared by means of RF sputtering technique at 13, 56 MHz, followed by characterization using XRD, SEM, EDX, UV-Vis, and proven to be able to degrade methylene blue on the textile fabric. By utilizing ultraviolet light, where layer prepared with oxygen pressure of 0.15 \u0026times; 10\u003csup\u003e\u0026minus;\u0026thinsp;2\u003c/sup\u003e mbar has the highest percentage capable of degrading methylene blue by 91.96%. Although the effect of variations in oxygen pressure is not very significant, it does provide a significant value in degradation of methylene blue dye waste of textile factory in Yogyakarta.\u003c/p\u003e"},{"header":"Declarations","content":"\u003cp\u003e\u003cstrong\u003eACKNOWLEDGMENT\u003c/strong\u003e\u003c/p\u003e\n\u003cp\u003eThe authors would like to acknowledge KEMENRISTEKDIKTI for the research financial support.\u0026nbsp;\u003c/p\u003e\n\u003cp\u003e\u003cstrong\u003eCONFLICT OF INTEREST\u003c/strong\u003e\u003c/p\u003e\n\u003cp\u003eThe authors declare that they have no conflict of interest.\u003c/p\u003e\n\u003cp\u003e\u003cstrong\u003eCREDIT AUTHORSHIP CONTRIBUTION STATEMENT\u003c/strong\u003e\u003c/p\u003e\n\u003cp\u003eTrimarji Atmono : Investigation, methodology, conceptualization, formal analysis, data curation, writing -original draft; writing -review \u0026amp; editing. Agus Purwadi: conceptualization, formal analysis, methodology, writing -review \u0026amp; editing.Taxwim: methodology, data curation. Asih Melati: writing \u0026ndash; review \u0026amp; supervision.\u0026nbsp;\u003c/p\u003e\n\u003cp\u003e\u003cstrong\u003eINFORMED CONSENT\u003c/strong\u003e\u003c/p\u003e\n\u003cp\u003eAll Authors involved in this study provided written informed consent prior to their inclusion. The informed consent process included detailed information about the study\u0026apos;s purpose, procedures, potential risks, and the voluntary nature of participation. Additionally, participants were explicitly informed about the use of their data for publication purposes, and written consent to publish their anonymized results was obtained. The study protocol, including the consent forms, was reviewed and approved by the The National Research Agency of Republic Indonesia and Islamic state University Sunan Kalijaga Yogyakarta.\u003c/p\u003e\n\u003cp\u003e\u003cstrong\u003eDATA AVAILABILITY\u003c/strong\u003e\u003c/p\u003e\n\u003cp\u003eThe Authors confirm that the data supporting the findings of the study are available within the article. The raw data that support the findings of this study are available from the corresponding author upon reasonable request. \u0026nbsp;\u003c/p\u003e"},{"header":"References","content":"\u003col\u003e\u003cli\u003e\u003cspan\u003eSonia, Kumari H, Suman, Chahal S, Devi S, Kumar S, et al. Spinel ferrites/metal oxide nanocomposites for waste water treatment. Appl Phys A. 2023;129:91.\u003c/span\u003e\u003c/li\u003e \u003cli\u003e\u003cspan\u003ePattnaik P, Dangayach GS, Bhardwaj AK. A review on the sustainability of textile industries wastewater with and without treatment methodologies. 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Journal of Environmental Management. 2022;308:114617.\u003c/span\u003e\u003c/li\u003e\u003c/ol\u003e"}],"fulltextSource":"","fullText":"","funders":[],"hasAdminPriorityOnWorkflow":false,"hasManuscriptDocX":true,"hasOptedInToPreprint":true,"hasPassedJournalQc":"","hasAnyPriority":false,"hideJournal":true,"highlight":"","institution":"","isAcceptedByJournal":false,"isAuthorSuppliedPdf":false,"isDeskRejected":"","isHiddenFromSearch":false,"isInQc":false,"isInWorkflow":false,"isPdf":false,"isPdfUpToDate":true,"isWithdrawnOrRetracted":false,"journal":{"display":true,"email":"[email protected]","identity":"researchsquare","isNatureJournal":false,"hasQc":true,"allowDirectSubmit":true,"externalIdentity":"","sideBox":"","snPcode":"","submissionUrl":"/submission","title":"Research Square","twitterHandle":"researchsquare","acdcEnabled":true,"dfaEnabled":false,"editorialSystem":"","reportingPortfolio":"","inReviewEnabled":false,"inReviewRevisionsEnabled":true},"keywords":"RF-sputtering, NiO/Ag, methylene blue, oxygen partial, band gap energy","lastPublishedDoi":"10.21203/rs.3.rs-3611170/v1","lastPublishedDoiUrl":"https://doi.org/10.21203/rs.3.rs-3611170/v1","license":{"name":"CC BY 4.0","url":"https://creativecommons.org/licenses/by/4.0/"},"manuscriptAbstract":"\u003cp\u003eThin films NiOAg were growth onto glass substrates by RF sputtering technique at the Radio Frequency of 13.56 MHz with variation of oxygen pressure. The research was conducted about preparation and characterization of NiOAg thin films, applicated as a photocatalyst degradation of methylene blue. XRD analysis showed stronger intensity (111) and (200) planes at peak 2θ of 37.66\u003csup\u003e0\u003c/sup\u003e and 43,23\u003csup\u003e0\u003c/sup\u003e. EDX analysis showed the following composition, Ni\u0026thinsp;=\u0026thinsp;40.45%, Ag\u0026thinsp;=\u0026thinsp;13.01%, and O\u0026thinsp;=\u0026thinsp;46.53%. Based on UV-Vis, it was found the band gap energy of 2.8 eV, 3.1 eV and 3.2 eV, for oxygen pressure 0.05; 0.1 and 0.15 x 10\u0026thinsp;\u0026minus;\u0026thinsp;2 mbar, respectively. From the experiment of degradation of methylene blue, that was taken from textile factory dye waste in Yogyakarta/Indonesia, it was obtained the best value of degradation by 91.96%.\u003c/p\u003e","manuscriptTitle":"Characterization of NiOAg thin film applicated as photocatalytic degradation of methylene blue dye waste in Yogyakarta textile factory","msid":"","msnumber":"","nonDraftVersions":[{"code":1,"date":"2023-12-02 01:55:02","doi":"10.21203/rs.3.rs-3611170/v1","editorialEvents":[{"type":"communityComments","content":0}],"status":"published","journal":{"display":true,"email":"[email protected]","identity":"researchsquare","isNatureJournal":false,"hasQc":true,"allowDirectSubmit":true,"externalIdentity":"","sideBox":"","snPcode":"","submissionUrl":"/submission","title":"Research Square","twitterHandle":"researchsquare","acdcEnabled":true,"dfaEnabled":false,"editorialSystem":"","reportingPortfolio":"","inReviewEnabled":false,"inReviewRevisionsEnabled":true}}],"origin":"","ownerIdentity":"b934e6da-e0cc-40e8-b0c9-9a109ee97a51","owner":[],"postedDate":"December 2nd, 2023","published":true,"recentEditorialEvents":[],"rejectedJournal":[],"revision":"","amendment":"","status":"posted","subjectAreas":[],"tags":[],"updatedAt":"2023-12-04T17:14:27+00:00","versionOfRecord":[],"versionCreatedAt":"2023-12-02 01:55:02","video":"","vorDoi":"","vorDoiUrl":"","workflowStages":[]},"version":"v1","identity":"rs-3611170","journalConfig":"researchsquare"},"__N_SSP":true},"page":"/article/[identity]/[[...version]]","query":{"redirect":"/article/rs-3611170","identity":"rs-3611170","version":["v1"]},"buildId":"FbvkV6FR0MCFSLy54lSbu","isFallback":false,"isExperimentalCompile":false,"dynamicIds":[84888],"gssp":true,"scriptLoader":[]}