Thin Film Structured Superior Anode Material Based N-Graphene Supported Coupled NiO/TiO2 Hollow Nanospheres and Their Cyclic Voltammetry Performance

Thin Film Structured Superior Anode Material Based N-Graphene Supported Coupled NiO/TiO2 Hollow Nanospheres and Their Cyclic Voltammetry Performance | 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 Thin Film Structured Superior Anode Material Based N-Graphene Supported Coupled NiO/TiO2 Hollow Nanospheres and Their Cyclic Voltammetry Performance Thamrin Azis, Lintan Ashari, Muhammad Zakir Muzakkar, Muhammad Nurdin, and 2 more This is a preprint; it has not been peer reviewed by a journal. https://doi.org/ 10.21203/rs.3.rs-3338252/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 In this research, we succeeded in designing a new strategy to synthesize a unique thin film structured of nitrogen doped graphene (NGr) composite combined with coupled NiO/TiO 2 hollow nanospheres using a synergistic hydrothermal method. The NGr@NiO/TiO 2 composite characteristics are demonstrated by several rational characterization techniques such as the morphological shape of NiO/TiO 2 hollow nanospheres which are evenly distributed on the surface of N-graphene with particle distribution in the range 79.78-362.13 nm with an average diameter of 130 nm. In addition, the crystal structures of carbon from NGr, NiO, and TiO 2 (anatase and rutile) have been confirmed and proven by spectra showing the presence of C-N stretching primary amides (1400 cm − 1 ), Ni-O stretching (700 cm − 1 ) and Ti-O-Ti bond (425 cm − 1 ), respectively. The electrochemical test was carried out by optimizing the performance of cyclic voltammetry (CV) through parameters such as the influence of composition, scan rate, and cycle with the best conditions, namely composite ratio 80:10:10 (wt%), scan rate 50 mV/s, condition stable cycle and also calculated the high specific capacity value of 839.83 F/g. Based on this, it is revealed that NGr@NiO/TiO 2 composites can explore the potential and be fully applied in the development of alkaline metal ion (AIB) batteries such as Li/Na/K. Battery N-Graphene NiO-TiO2 cyclic voltammetry specific capacitance Figures Figure 1 Figure 2 Figure 3 Figure 4 Figure 5 Figure 6 1 Introduction In today's world, batteries and other electrochemical energy storage technologies are crucial for transitioning from a fossil fuel-based economy to a sustainable one. This has led to a growing demand for energy storage in electric vehicles, portable devices, and grid or plant scale storage. As a result, researchers are focused on developing cleaner and more efficient electrochemical energy conversion systems (Cui et al., 2017 ; He et al., 2023 ; Olsson et al., 2021 ; Tang et al., 2019 ). One type of power source that is becoming more popular is the alkaline metal-ion battery (AIB), including the Li-ion battery (LIB) (Yao et al., 2022 ), Na-ion battery (NIB) (C. Xu et al., 2022 ) dan K-ion battery (KIB) (Kang et al., 2022 ). These batteries are attracting attention because they have a high power density, excellent cycle performance, and long cycle life. As a result, the development of AIBs is ongoing to meet increasing energy storage demands (He et al., 2023 ; Olsson et al., 2021 ; Tang et al., 2019 ). The performance of batteries is dependent on the electrode materials used, specifically the anode and cathode. To achieve high performance, optimization of these materials is necessary. Carbonaceous materials, such as graphite, are commonly used as anodes for LIBs but are not suitable for NIBs due to their inability to store large amounts of Na + (less than 35 mAh g − 1 ) and have a low reversible capacity of ~ 260 mAh g − 1 in KIB. Graphene materials have shown promising results as NIB anodes and have also demonstrated good performance for LIBs and KIBs (Dou et al., 2019 ; Jian et al., 2015 ; Y. Li et al., 2019 ; Olsson et al., 2021 ; Stevens & Dahn, 2001 ; Sun et al., 2021 ). Graphene, a one-atom-thick layer with a two-dimensional architecture of carbon materials, has received great attention because of its superior electrical, mechanical, and chemical properties (G. Li et al., 2017 ). More extraordinary, nitrogen-doped graphene (NGr) is becoming increasingly popular due to its high-performance electrochemical properties in comparison to pure graphene. The addition of N atoms in the graphene network creates activated regions where they are next to carbon atoms. Moreover, N atoms can also function as binding sites for metal ions. When combined with other active material, high-quality NGr provides excellent electrical conductivity. Therefore, NGr unique properties make it a highly sought-after material for enhancing electrochemical capabilities in metal oxide matrices (Kamal et al., 2022 ; Kaur et al., 2018 ; Miao et al., 2019 ; Naveenkumar et al., 2023 ). To enhance the electrochemical performance of anode materials, we utilize a research strategy that involves incorporating NGr composites with the help of metal oxide nanoparticles. This is achieved through a two-step hydrothermal method. Our approach involves using selected metal oxides such as NiO and TiO 2 , which are highly effective modifiers with fast and reversible faradaic redox processes. These metal oxides interact with ions and electrons in their charge storage mechanisms, making them ideal for our research objectives (Al Kiey et al., 2022 ; Tang et al., 2019 ). NiO is a popular choice for AIB anode material due to its cost-effectiveness, high theoretical capacity, and non-toxicity. However, the anode made of pure NiO particles has poor initial Coulomb efficiency and cycle performance. To improve NiO performance as an anode, several attempts have been made to incorporate nanostructures such as nanoparticles (Natsir et al., 2021 ; L. Zhang et al., 2016 ; Y. Zhang et al., 2021 ). On the other hand, TiO 2 is a zero-strain embedding material, which makes it highly reversible, safe, and stable during electrochemical processes. Despite its excellent properties, TiO 2 practical development for commercial use is limited due to its low theoretical capacity (Chen et al., 2023 ; Long et al., 2018 ; Wang et al., 2021 ). The purpose of this study is to analyze the performance of NGr@NiO/TiO 2 hollow nanosphere anodes using cyclic voltammetry (CV), which is a fundamental electrochemical analysis technique. This method helps to identify the oxidation or reduction voltage, detect impurities, and ensure that the reaction occurs correctly. The goal is to determine if NGr@NiO/TiO 2 hollow nanosphere anodes are suitable as superior anode candidates for AIB (Huang et al., 2019 ; Kim et al., 2020 ). Miao et al. (Miao et al., 2019 ) synthesized a TiO 2 /N-graphene/Si-MCP composite for LIB with the redox peaks observed in the 2nd and 3rd cycles overlapping each other implying high reversibility and stability. Porous NiO hollow quasi-nanospheres showing the first three CV profiles of the NiO electrode at a voltage of 0–3 V with a scan rate of 0.2mVs − 1 (J. Xu et al., 2017 ). As a NIB anode, TiO 2 /NRGO shows four CV profiles at 0.1 mV s − 1 (0.01-3V). An irreversibly reduced peak was observed at 1.2 V during the initial cathodic sweep, which was caused by electrolyte decomposition and SEI formation. Based on this, it is very important to understand the electrochemical properties of NGr@NiO/TiO2 composites with CV so that it becomes the main basis for developing anodes in the future. 2 Experimental Method 2.1 Preparation of N-Graphene (NG) Preparation and synthesis of NG were started with graphene oxide powder prepared according to the Hummers method referring to our previous studies (Nurdin et al., 2022 ; Wibowo et al., 2020 ). The graphene powder obtained was reduced by hydrothermal addition of nitrogen. Then, 70 mg of graphene was dispersed in 30 mL of deionized water by ultrasonication for 3 hours and a certain amount of urea was added to the graphene solution. The suspension was ultrasonicated again for 1 hour. The resulting mixture was transferred into a Teflon-lined autoclave and heated at 180 ºC for 12 hours. The black product is obtained by centrifugation. And finally, the precipitate was washed several times with deionized water to remove impurities and then dried at 60 ºC in an oven for 24 hours (Ramezani & Dehghani, 2019 ). 2.2 Synthesis of NiO and TiO 2 Nanoparticles Synthesis of NiO nanoparticles were prepared by incorporating 250 mL of 1.2 M NaOH solution into a 1000 mL burette and then added to 250 mL of 0.5 M NiSO 4 solution drop by drop until used up while stirring using a magnetic stirrer at 1000 rpm at room temperature. The formed Ni(OH) 2 precipitate was separated and washed until it was free of sulfate and the filtrate had a neutral pH. The content of sulfate impurities in the filtrate was tested by adding BaCl 2 solution to the filtrate until no white precipitate formed. Then the cleaned Ni(OH) 2 solid was dried in an oven at 70 ºC for 24 hours. The dried solids were then calcined at 800 ºC for 2 hours. For the next step, TiO 2 nanoparticles was prepared using the annealing method which was initiated by dissolving 10 g of TiO 2 Degussa and dissolving it with distilled water and ethanol (1:1). Then the suspension was ultrasonicated for 1 hour at 80 ºC. Then the suspension was filtered and dried at 500 ºC using a closed container for 3 hours (Lal et al., 2022 ; Salim et al., 2023 ). 2.3 Preparation of NG@NiO-TiO 2 Electrode NGr@NiO/TiO 2 was prepared with the composition of NiO, TiO 2 , and NGr with a composite mass ratio of 15:5:80, 10:10:80, and 5:15:80 (wt%) which was dissolved in 50 mL of deionized water mixture, then ultrasonicated for 1 hour. After that, the suspension mixture was transferred into a 100 mL Teflon-coated stainless steel autoclave at 200°C for 6 hours. After the reaction was complete, the autoclave was allowed to stand until room temperature, the product obtained was washed several times with deionized water and ethanol and dried at 60°C for 24 hours. Furthermore, the product obtained was annealed at 350 ºC for 2 hours. Next, prepare the electrode by homogenizing a mixture of 0.05 g NGr@NiO/TiO 2 nanocomposite and 0.3 paraffin oil which is stirred at 400 rpm for 15 minutes while heated at 80 ℃. Then the NGr@NiO/TiO 2 paste was put into a 3 mm diameter glass tube, pressed gently, smoothed on the surface, and connected to a copper wire. Finally, composite comparators were made, each labeled NG, NGr@TiO 2 and NG@NiO. 2.4 Electrochemical Properties Measurements The electrochemical properties of the prepared samples were measured in a mixture of K 3 [Fe(CN) 6 ] solution and 1 M KOH electrolyte using a three-electrode system. The three-electrode system includes a counter electrode (platinum electrode), a reference electrode (Ag/AgCl), and a working electrode (prepared sample). Next, electrodes are measured based on composition variations (NGr composite, NGr@TiO 2 , NGr@NiO, and NGr@NiO/TiO 2 (80:10:10, 80:5:15, and 80:15:10), scan rate variations (5- 100 mV/s) and cycle variations (1–5 cycles). 2.5 Characterizations The morphology of the electrode was characterized using Xray diffraction, XRD (Shimadzu 6000) at 2θ = 20-80o with Cu-Kα = 1.54060). The morphology of the nanocomposites was characterized using scanning electron microscopy, SEM (HITACHI SU3500). To identify chemical bonds and functional groups, Fourier transforms infrared (FT-IR) spectra was used (Shimadzu Varian 4300 spectrophotometer). The electrochemical properties of the nanocomposites were characterized by cyclic voltammetry techniques using a DY2100 potentiostat. 3 Result and Discussion 3.1 Morphological and Structure of NG@NiO/TiO 2 Nanocomposite The production of N-Graphene (NG) involves utilizing urea to react with graphene oxide obtained via the Hummer method. This crucial step aids in the reduction of various functional groups, such as phenol, ketone, epoxy, carboxyl, and carbonyl groups. These groups arise and attach to the graphene during the oxidation process of graphite, eventually resulting in the formation of graphene oxide. The substitution of these functional groups is made possible by the introduction of N atoms from urea (Nurdin et al., 2022 ; Wibowo et al., 2020 ). The modification uses a combination of NiO and TiO 2 nanoparticle pairs with several different concentrations, including NGr (100:0:0), NGr@NiO (80:20:0), NGr@TiO 2 (80:0:20), NGr @NiO/TiO 2 (80:10:10, 80:5:15, and 80:15:5) (wt%) where we have identified the morphology, crystal structure and bonds formed in this composite material. The nanocomposite XRD pattern is presented in Fig. 1 . The graphene peak is located at 2θ=26.4°, which is consistent with previous studies by Dong et al. (Dong et al., 2019 ) and Wibowo et al. (Wibowo et al., 2022 ) that showed the layered graphene structure obtained from XRD spectra. Additionally, NiO diffraction peaks at 37.2◦, 43.3◦, and 64.44◦ were observed and can be Miller Indexed to the (111), (200), and (220) planes of NiO nanoparticles' structure, as reported in JCPDS 47-1049. Moreover, TiO2 is dominated by anatase crystals compared to JCPDS 21-1272. At 2θ = 25.5°, 37.9°, 39.39°, 48.1°, 56.7°, the diffraction peaks were observed and indexed to the (101), (103), (112), (200), and (105) planes. Additionally, rutile crystals were identified at 2θ = 27.74°, 56.56°, and 64.20°, with index positions to the (110), (201), and (002) planes, compared to JCPDS 21-1276. Furthermore, the Scherrer formula is used to obtain an average crystal size for particles of 19.66 nm. To confirm the findings of the XRD analysis, SEM characterization was conducted. The results revealed the presence of a mixture of NiO/TiO2 nanoparticles on the surface of the graphene material. Figure 2 a provides a clear view of the distinctive thin layer structure of this composite and highlights the distribution of the nano hollow NiO/TiO 2 on the NGr surface, which has been previously documented (J. Xu et al., 2017 ). n Fig. 2 b, the spherical nanoparticles are shown to cover almost the entire surface of the graphene layer. To determine the diameter size of the NiO/TiO 2 particles on the thin layer composites, SEM characterization results were processed using image-J software with the "analyze particles" feature. The size distribution of NiO/TiO 2 particle diameters on the NGr surface ranged from 79.78 to 362.13 nm, with an average diameter of 130 nm and an R square value of 0.94212, indicating good data (Fig. 2 c). The continuous NGr phase, as reported by Chen et al. (Chen et al., 2019 ), can effectively improve the structural stability of the NGr@NiO/TiO 2 nanocomposite during the charge-discharge process. Using FTIR analysis, we were able to identify the chemical processes that occur during nanocomposite formation, including the development of chemical bonds and coordination. The results are presented in Fig. 3 . Figure 3 a displays the NGr spectrum, which shows peaks of epoxy groups and C-O stretching at around 1125 cm − 1 . Heating NGr during formation causes a peak at around 2874 cm − 1 to appear, indicating the presence of aliphatic C-H groups. Furthermore, the formation of NGr is confirmed by the observation of N–H stretching as a hump at around 3078 cm − 1 . In Fig. 3 b, the C-N bond stretching around 1400 cm − 1 is identified as a characteristic of NGr, and Ni-O is identified at an absorption peak of 700 cm − 1 . TiO 2 absorption peaks are also observed at wave numbers 1638 cm − 1 and 425 cm − 1 , caused by Ti-O vibrations. As a result, the nanocomposite process's new coordination chemistry maintains the intrinsic properties of the individual elements. Any changes to this process's performance can be directly linked to the electrochemical properties of these nanocomposites. 3.2 Cyclic Voltammetry Performance Scan Rate and Cyclic Variation Six different variations of the NG@NiO/TiO2 nanocomposite anode were tested to find the best composition. The electrodes included NGr, NGr@TiO2, NGr@NiO, and three variations of NGr@NiO/TiO2. Each electrode was tested in an electrochemical cell with a 0.01 M K3(Fe(CN)6) solution and 1 M KOH electrolyte. The voltammogram curves of the K3[Fe(CN)6] solution were measured using a scan rate of 5-100 mV/s over a potential range of -0.8 to 0.8 V/s. Adding metal oxide to the K 3 [Fe(CN) 6 ] solution improved its measurement results compared to NGr due to the presence of nano-hollow NiO and TiO 2 doping. The reactions in the Fe(CN) 6 3− /Fe(CN) 6 4− system were reversible, and NGr and NGr@TiO 2 were good electrodes with clear current peaks. NGr@NiO and NGr@NiO/TiO 2 electrodes tended to form voltammograms resembling a rectangle. A slower scan rate resulted in a thicker diffusion layer, causing a reduction in the current generated (Brownson & Banks, 2014 ). Determining the stability of an electrode involves taking multiple measurements. By analyzing the formation of oxidation and reduction peaks and producing a stable voltammogram, we can determine the repeatability and reversibility of the electrode. After conducting 5 cycles of measurements on the NGr electrode, we found that it has good stability. Additionally, the voltammogram produced during the repetition process was consistently stable. The NGr@TiO 2 electrode also showed good potential after undergoing a repeatability test for 5 cycles. Furthermore, the NGr@NiO electrode maintained good stability during the 5th cycle, as shown in the accompanying image (Fig. 4 b, d, f). Based Fig. 5 NGr@NiO/TiO 2 electrode's cyclic voltammetric results showed good stability after 5 cycles using 0.01 M K 3 (Fe(CN) 6 ) and 1 M KOH solutions. The NGr@NiO/TiO 2 80:15:5 (wt%) electrode had the best stability and successful electron transfer. Nitrogen doping increases wettability and binding energy, allowing for more ion movement and higher capacitance. NiO/TiO 2 nanoparticles play a crucial role. Specific Capacity Measurement Kapasitansi spesifik bahan elektroda NGr@NiO/TiO 2 beserta anoda pembandingnya dihitung dari kurva CV yaitu Gambar 4a, c, d dan Gambar 5a, c, d seperti yang ditunjukkan pada Gambar 6. Berdasarkan Gambar 6a memperlihatkan kapasitas spesifik NGr, NGr@TiO 2 and NGr@NiO composite berbanding terbalik dengan scan rate 5-100 mV/s dengan nilai masing-masing yaitu NGr (135.38, 73.95, 48.69, 29.43, 20.46 F/g), NGr@TiO2 (287.11, 203.58, 128.02, 62.53, 31.26 F/g) dan NGr@NiO (1959.71, 979.85, 541.38, 262.77, 131.38 F/g). Sedangkan Gambar 6b memperlihatkan kapasitas spesifik dari NGr@NiO/TiO 2 sesuai komposisi diantaranya 80:10:10 (741.02, 376.76, 188.86, 85.28, 48.36 F/g), 80:5:15 (408.53, 234.13, 131.78, 60.76, 40.89 F/g) and 80:15:5 (839.84, 440.93, 238.88, 111.04, 60.35 F/g). Gambar 6 juga menunjukkan bahwa nilai kapasitansi spesifik menurun dengan meningkatnya kecepatan pemindaian. 3 Conclusions Based on the results and discussion that have been described, it can be concluded that the NGr@NiO/TiO 2 nanocomposite has been successfully synthesized with NGr thin films by hydrothermally combining NiO/TiO 2 hollow nanospheres. In addition, the unique structure of the material is supported by XRD, SEM and FTIR characterization data with crystallinity, morphology and bonds directly confirming the success of this synthesis. Electrochemical tests were carried out by optimizing cyclic voltammetry (CV) performance through parameters such as the influence of composition, scan rate and cycle with the best conditions, namely a composite ratio of 80:10:10 (wt%), scan rate of 50 mV/s, the most stable cycle conditions and also taking into account the high specific capacity value of 839.83 F/g. Based on this, it is revealed that the NGr@NiO/TiO 2 composite is very suitable for application in alkali metal ion batteries (AIB). Declarations Author Contributions T.A. and L.A. performed all the experiments. M.Z.M coordinated the study. M.N. and L.O.M.Z.M. writing the manuscript. L.O.M.Z.M and A.A.U. processed the research data. 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Electron. 31 (17), 14375–14383 (2020). https://doi.org/10.1007/s10854-020-03996-2 C. Xu, J. Wang, K. Wu, G. Xi, X. Hu, L. Qiu, CuFeS2 anchored in ethylenediamine-modified reduced graphene oxide as an anode material for sodium ion batteries. Mater. Lett. 308 , 131164 (2022) J. Xu, H. Tang, T. Xu, D. Wu, Z. Shi, Y. Tian, X. Li, Porous NiO hollow quasi-nanospheres derived from a new metal-organic framework template as high-performance anode materials for lithium ion batteries. Ionics. 23 , 3273–3280 (2017) L.-H. Yao, J.-G. Zhao, Q.-L. Pan, X.-Y. Li, B.-Y. Xing, S. Jiang, J. Song, M.-J. Pang, Tailoring NiO@ NiFe2O4/CNTs triphase hybrids towards high-performance anode for lithium-ion batteries. J. Alloys Compd. 912 , 165209 (2022) L. Zhang, J. Mu, Z. Wang, G. Li, Y. Zhang, Y. He, One-pot synthesis of NiO/C composite nanoparticles as anode materials for lithium-ion batteries. J. Alloys Compd. 671 , 60–65 (2016) Y. Zhang, M. Xie, Y. He, Y. Zhang, L. Liu, T. Hao, Y. Ma, Y. Shi, Z. Sun, N. Liu, Hybrid NiO/Co3O4 nanoflowers as high-performance anode materials for lithium-ion batteries. Chem. Eng. J. 420 , 130469 (2021) Additional Declarations No competing interests reported. Cite Share Download PDF Status: Posted Version 1 posted 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-3338252","acceptedTermsAndConditions":true,"allowDirectSubmit":true,"archivedVersions":[],"articleType":"Research Article","associatedPublications":[],"authors":[{"id":231927469,"identity":"b6328b4c-15f1-44bb-bb2a-eff0db6f1017","order_by":0,"name":"Thamrin Azis","email":"data:image/png;base64,iVBORw0KGgoAAAANSUhEUgAAAZAAAAAyAQMAAABI0h/eAAAABlBMVEX///8AAABVwtN+AAAACXBIWXMAAA7EAAAOxAGVKw4bAAAA/UlEQVRIiWNgGAWjYDACCRBhAMTMDAwHEipsgCzGxgP4dPAgaWF88OFMGkhLAxFaIIDZcGbLYTALrxZ76eanmysK7sjLt7M/k+ZtOG+3tv0w0JYam2ictsgcM7t5xuCZYWMzj5k0747bydvOJAK1HEvLbcDpsASzmw0GhxmbmXnYpHnP3E42OwDUwthwGI+W9G8gLfZtzCCHtZ1LNjv/kJCWHLAtiT3MDMaGM9sO2JndIGTLjZwykJbkGcw8hsBATk4wuwG0JQGPX9hnpG+72fDnsO38/uMPgFFpZ292Pv3hgw81Nji1YIBEsMoEYpWDgD0pikfBKBgFo2BkAAArVmXUqAwWMgAAAABJRU5ErkJggg==","orcid":"","institution":"Universitas Halu Oleo","correspondingAuthor":true,"prefix":"","firstName":"Thamrin","middleName":"","lastName":"Azis","suffix":""},{"id":231927470,"identity":"126a7c49-05ea-44d3-b699-b3cd7f73d15b","order_by":1,"name":"Lintan Ashari","email":"","orcid":"","institution":"Universitas Halu Oleo","correspondingAuthor":false,"prefix":"","firstName":"Lintan","middleName":"","lastName":"Ashari","suffix":""},{"id":231927472,"identity":"805f779d-58e8-495f-8ce5-9671a430c028","order_by":2,"name":"Muhammad Zakir Muzakkar","email":"","orcid":"","institution":"Universitas Halu Oleo","correspondingAuthor":false,"prefix":"","firstName":"Muhammad","middleName":"Zakir","lastName":"Muzakkar","suffix":""},{"id":231927473,"identity":"3bc36472-24f5-43af-b8a5-b74f63e52fa9","order_by":3,"name":"Muhammad Nurdin","email":"","orcid":"","institution":"Universitas Halu Oleo","correspondingAuthor":false,"prefix":"","firstName":"Muhammad","middleName":"","lastName":"Nurdin","suffix":""},{"id":231927475,"identity":"635ca6ac-b375-495f-ae08-e04bc72257fd","order_by":4,"name":"Muhammad Zuhdi Mulkiyan","email":"","orcid":"","institution":"Universitas Halu Oleo","correspondingAuthor":false,"prefix":"","firstName":"Muhammad","middleName":"Zuhdi","lastName":"Mulkiyan","suffix":""},{"id":231927477,"identity":"635105f4-fda4-4ecf-9ace-0ab4613cdcad","order_by":5,"name":"Akrajas Ali Umar","email":"","orcid":"","institution":"Universiti Kebangsaan Malaysia, UKM","correspondingAuthor":false,"prefix":"","firstName":"Akrajas","middleName":"Ali","lastName":"Umar","suffix":""}],"badges":[],"createdAt":"2023-09-08 16:14:20","currentVersionCode":1,"declarations":"","doi":"10.21203/rs.3.rs-3338252/v1","doiUrl":"https://doi.org/10.21203/rs.3.rs-3338252/v1","draftVersion":[],"editorialEvents":[],"editorialNote":"","failedWorkflow":false,"files":[{"id":43078836,"identity":"a3b369ce-94d3-4f5a-b32d-6ff408680987","added_by":"auto","created_at":"2023-09-13 15:22:18","extension":"png","order_by":1,"title":"Figure 1","display":"","copyAsset":false,"role":"figure","size":84764,"visible":true,"origin":"","legend":"\u003cp\u003eXRD pattern of NGr@NiO/TiO\u003csub\u003e2 \u003c/sub\u003enanocomposite\u003c/p\u003e","description":"","filename":"floatimage1.png","url":"https://assets-eu.researchsquare.com/files/rs-3338252/v1/94ee6bd2da69d96e10d8397b.png"},{"id":43078839,"identity":"dc3281a0-ad82-4503-b308-f56d16dd7831","added_by":"auto","created_at":"2023-09-13 15:22:18","extension":"jpeg","order_by":2,"title":"Figure 2","display":"","copyAsset":false,"role":"figure","size":233766,"visible":true,"origin":"","legend":"\u003cp\u003e(a-b) SEM image and (c) particles size distribution of NGr@NiO/TiO\u003csub\u003e2 \u003c/sub\u003enanocomposite\u003c/p\u003e","description":"","filename":"floatimage2.jpeg","url":"https://assets-eu.researchsquare.com/files/rs-3338252/v1/6aae835200956275e3a5be83.jpeg"},{"id":43078838,"identity":"b7510ce1-b91d-4bee-9107-1525bfd4f33f","added_by":"auto","created_at":"2023-09-13 15:22:18","extension":"jpeg","order_by":3,"title":"Figure 3","display":"","copyAsset":false,"role":"figure","size":147478,"visible":true,"origin":"","legend":"\u003cp\u003eFTIR spectra of (a) NG@NiO/TiO\u003csub\u003e2\u003c/sub\u003e nanocomposite and (b) C-N, Ni-O, and Ti-O-Ti bond.\u003c/p\u003e","description":"","filename":"floatimage3.jpeg","url":"https://assets-eu.researchsquare.com/files/rs-3338252/v1/f36f501b827eb86505c224b7.jpeg"},{"id":43079931,"identity":"a7d380fa-8dbb-4fa6-a028-5d790e8a7ab2","added_by":"auto","created_at":"2023-09-13 15:30:18","extension":"jpeg","order_by":4,"title":"Figure 4","display":"","copyAsset":false,"role":"figure","size":432747,"visible":true,"origin":"","legend":"\u003cp\u003eThe voltammogram of scan rate and cyclic variation of NGr [a-b], NGr@TiO\u003csub\u003e2\u003c/sub\u003e [c-d], and NGr@TiO\u003csub\u003e2\u003c/sub\u003e [e-f] composite\u003c/p\u003e","description":"","filename":"floatimage4.jpeg","url":"https://assets-eu.researchsquare.com/files/rs-3338252/v1/a9fb25a409a5f835ab6fbf52.jpeg"},{"id":43078841,"identity":"c019fd46-6f58-401d-96ee-e739ee14a167","added_by":"auto","created_at":"2023-09-13 15:22:18","extension":"jpeg","order_by":5,"title":"Figure 5","display":"","copyAsset":false,"role":"figure","size":437109,"visible":true,"origin":"","legend":"\u003cp\u003eThe voltammogram of scan rate and cyclic variation of NGr@NiO/TiO\u003csub\u003e2\u003c/sub\u003e composite with compositions, 80:10:10 [a-b], 80:5:15 [c-d], and 80:15:5 (wt%) [e-f]\u003c/p\u003e","description":"","filename":"floatimage5.jpeg","url":"https://assets-eu.researchsquare.com/files/rs-3338252/v1/83ab8b570de352954bd3eebc.jpeg"},{"id":43078837,"identity":"16cda26e-d4f1-473f-8f67-09b288fbe759","added_by":"auto","created_at":"2023-09-13 15:22:18","extension":"jpeg","order_by":6,"title":"Figure 6","display":"","copyAsset":false,"role":"figure","size":124764,"visible":true,"origin":"","legend":"\u003cp\u003eThe specific capacity as a function of [a] NGr, NGr@TiO2 and NGr@NiO composite, and [b] NGr@NiO/TiO\u003csub\u003e2\u003c/sub\u003e composite with compositions 80:10:10, 80:5:15, and 80:15:5 (wt%) by scan rate 5-100 mV/s.\u003c/p\u003e","description":"","filename":"floatimage6.jpeg","url":"https://assets-eu.researchsquare.com/files/rs-3338252/v1/7a66c4b283fa3503959cede5.jpeg"},{"id":43148919,"identity":"e81227e5-9653-4d82-9678-87cf4728069e","added_by":"auto","created_at":"2023-09-14 17:37:33","extension":"pdf","order_by":0,"title":"","display":"","copyAsset":false,"role":"manuscript-pdf","size":998019,"visible":true,"origin":"","legend":"","description":"","filename":"manuscript.pdf","url":"https://assets-eu.researchsquare.com/files/rs-3338252/v1/6c9e434f-7371-416f-9634-cfe43d445dbc.pdf"}],"financialInterests":"No competing interests reported.","formattedTitle":"Thin Film Structured Superior Anode Material Based N-Graphene Supported Coupled NiO/TiO2 Hollow Nanospheres and Their Cyclic Voltammetry Performance","fulltext":[{"header":"1 Introduction","content":"\u003cp\u003eIn today's world, batteries and other electrochemical energy storage technologies are crucial for transitioning from a fossil fuel-based economy to a sustainable one. This has led to a growing demand for energy storage in electric vehicles, portable devices, and grid or plant scale storage. As a result, researchers are focused on developing cleaner and more efficient electrochemical energy conversion systems (Cui et al., \u003cspan citationid=\"CR5\" class=\"CitationRef\"\u003e2017\u003c/span\u003e; He et al., \u003cspan citationid=\"CR8\" class=\"CitationRef\"\u003e2023\u003c/span\u003e; Olsson et al., \u003cspan citationid=\"CR23\" class=\"CitationRef\"\u003e2021\u003c/span\u003e; Tang et al., \u003cspan citationid=\"CR28\" class=\"CitationRef\"\u003e2019\u003c/span\u003e). One type of power source that is becoming more popular is the alkaline metal-ion battery (AIB), including the Li-ion battery (LIB) (Yao et al., \u003cspan citationid=\"CR34\" class=\"CitationRef\"\u003e2022\u003c/span\u003e), Na-ion battery (NIB) (C. Xu et al., \u003cspan citationid=\"CR32\" class=\"CitationRef\"\u003e2022\u003c/span\u003e) dan K-ion battery (KIB) (Kang et al., \u003cspan citationid=\"CR12\" class=\"CitationRef\"\u003e2022\u003c/span\u003e). These batteries are attracting attention because they have a high power density, excellent cycle performance, and long cycle life. As a result, the development of AIBs is ongoing to meet increasing energy storage demands (He et al., \u003cspan citationid=\"CR8\" class=\"CitationRef\"\u003e2023\u003c/span\u003e; Olsson et al., \u003cspan citationid=\"CR23\" class=\"CitationRef\"\u003e2021\u003c/span\u003e; Tang et al., \u003cspan citationid=\"CR28\" class=\"CitationRef\"\u003e2019\u003c/span\u003e).\u003c/p\u003e \u003cp\u003eThe performance of batteries is dependent on the electrode materials used, specifically the anode and cathode. To achieve high performance, optimization of these materials is necessary. Carbonaceous materials, such as graphite, are commonly used as anodes for LIBs but are not suitable for NIBs due to their inability to store large amounts of Na\u003csup\u003e+\u003c/sup\u003e (less than 35 mAh g\u003csup\u003e\u0026minus;\u0026thinsp;1\u003c/sup\u003e) and have a low reversible capacity of ~\u0026thinsp;260 mAh g\u003csup\u003e\u0026minus;\u0026thinsp;1\u003c/sup\u003e in KIB. Graphene materials have shown promising results as NIB anodes and have also demonstrated good performance for LIBs and KIBs (Dou et al., \u003cspan citationid=\"CR7\" class=\"CitationRef\"\u003e2019\u003c/span\u003e; Jian et al., \u003cspan citationid=\"CR10\" class=\"CitationRef\"\u003e2015\u003c/span\u003e; Y. Li et al., \u003cspan citationid=\"CR17\" class=\"CitationRef\"\u003e2019\u003c/span\u003e; Olsson et al., \u003cspan citationid=\"CR23\" class=\"CitationRef\"\u003e2021\u003c/span\u003e; Stevens \u0026amp; Dahn, \u003cspan citationid=\"CR26\" class=\"CitationRef\"\u003e2001\u003c/span\u003e; Sun et al., \u003cspan citationid=\"CR27\" class=\"CitationRef\"\u003e2021\u003c/span\u003e). Graphene, a one-atom-thick layer with a two-dimensional architecture of carbon materials, has received great attention because of its superior electrical, mechanical, and chemical properties (G. Li et al., \u003cspan citationid=\"CR16\" class=\"CitationRef\"\u003e2017\u003c/span\u003e). More extraordinary, nitrogen-doped graphene (NGr) is becoming increasingly popular due to its high-performance electrochemical properties in comparison to pure graphene. The addition of N atoms in the graphene network creates activated regions where they are next to carbon atoms. Moreover, N atoms can also function as binding sites for metal ions. When combined with other active material, high-quality NGr provides excellent electrical conductivity. Therefore, NGr unique properties make it a highly sought-after material for enhancing electrochemical capabilities in metal oxide matrices (Kamal et al., \u003cspan citationid=\"CR11\" class=\"CitationRef\"\u003e2022\u003c/span\u003e; Kaur et al., \u003cspan citationid=\"CR13\" class=\"CitationRef\"\u003e2018\u003c/span\u003e; Miao et al., \u003cspan citationid=\"CR19\" class=\"CitationRef\"\u003e2019\u003c/span\u003e; Naveenkumar et al., \u003cspan citationid=\"CR21\" class=\"CitationRef\"\u003e2023\u003c/span\u003e).\u003c/p\u003e \u003cp\u003eTo enhance the electrochemical performance of anode materials, we utilize a research strategy that involves incorporating NGr composites with the help of metal oxide nanoparticles. This is achieved through a two-step hydrothermal method. Our approach involves using selected metal oxides such as NiO and TiO\u003csub\u003e2\u003c/sub\u003e, which are highly effective modifiers with fast and reversible faradaic redox processes. These metal oxides interact with ions and electrons in their charge storage mechanisms, making them ideal for our research objectives (Al Kiey et al., \u003cspan citationid=\"CR1\" class=\"CitationRef\"\u003e2022\u003c/span\u003e; Tang et al., \u003cspan citationid=\"CR28\" class=\"CitationRef\"\u003e2019\u003c/span\u003e). NiO is a popular choice for AIB anode material due to its cost-effectiveness, high theoretical capacity, and non-toxicity. However, the anode made of pure NiO particles has poor initial Coulomb efficiency and cycle performance. To improve NiO performance as an anode, several attempts have been made to incorporate nanostructures such as nanoparticles (Natsir et al., \u003cspan citationid=\"CR20\" class=\"CitationRef\"\u003e2021\u003c/span\u003e; L. Zhang et al., \u003cspan citationid=\"CR35\" class=\"CitationRef\"\u003e2016\u003c/span\u003e; Y. Zhang et al., \u003cspan citationid=\"CR36\" class=\"CitationRef\"\u003e2021\u003c/span\u003e). On the other hand, TiO\u003csub\u003e2\u003c/sub\u003e is a zero-strain embedding material, which makes it highly reversible, safe, and stable during electrochemical processes. Despite its excellent properties, TiO\u003csub\u003e2\u003c/sub\u003e practical development for commercial use is limited due to its low theoretical capacity (Chen et al., \u003cspan citationid=\"CR4\" class=\"CitationRef\"\u003e2023\u003c/span\u003e; Long et al., \u003cspan citationid=\"CR18\" class=\"CitationRef\"\u003e2018\u003c/span\u003e; Wang et al., \u003cspan citationid=\"CR29\" class=\"CitationRef\"\u003e2021\u003c/span\u003e).\u003c/p\u003e \u003cp\u003eThe purpose of this study is to analyze the performance of NGr@NiO/TiO\u003csub\u003e2\u003c/sub\u003e hollow nanosphere anodes using cyclic voltammetry (CV), which is a fundamental electrochemical analysis technique. This method helps to identify the oxidation or reduction voltage, detect impurities, and ensure that the reaction occurs correctly. The goal is to determine if NGr@NiO/TiO\u003csub\u003e2\u003c/sub\u003e hollow nanosphere anodes are suitable as superior anode candidates for AIB (Huang et al., \u003cspan citationid=\"CR9\" class=\"CitationRef\"\u003e2019\u003c/span\u003e; Kim et al., \u003cspan citationid=\"CR14\" class=\"CitationRef\"\u003e2020\u003c/span\u003e). Miao et al. (Miao et al., \u003cspan citationid=\"CR19\" class=\"CitationRef\"\u003e2019\u003c/span\u003e) synthesized a TiO\u003csub\u003e2\u003c/sub\u003e/N-graphene/Si-MCP composite for LIB with the redox peaks observed in the 2nd and 3rd cycles overlapping each other implying high reversibility and stability. Porous NiO hollow quasi-nanospheres showing the first three CV profiles of the NiO electrode at a voltage of 0\u0026ndash;3 V with a scan rate of 0.2mVs\u0026thinsp;\u0026minus;\u0026thinsp;1 (J. Xu et al., \u003cspan citationid=\"CR33\" class=\"CitationRef\"\u003e2017\u003c/span\u003e). As a NIB anode, TiO\u003csub\u003e2\u003c/sub\u003e/NRGO shows four CV profiles at 0.1 mV s\u0026thinsp;\u0026minus;\u0026thinsp;1 (0.01-3V). An irreversibly reduced peak was observed at 1.2 V during the initial cathodic sweep, which was caused by electrolyte decomposition and SEI formation. Based on this, it is very important to understand the electrochemical properties of NGr@NiO/TiO2 composites with CV so that it becomes the main basis for developing anodes in the future.\u003c/p\u003e"},{"header":"2 Experimental Method","content":"\u003cdiv id=\"Sec3\" class=\"Section2\"\u003e \u003ch2\u003e2.1 Preparation of N-Graphene (NG)\u003c/h2\u003e \u003cp\u003ePreparation and synthesis of NG were started with graphene oxide powder prepared according to the Hummers method referring to our previous studies (Nurdin et al., \u003cspan citationid=\"CR22\" class=\"CitationRef\"\u003e2022\u003c/span\u003e; Wibowo et al., \u003cspan citationid=\"CR31\" class=\"CitationRef\"\u003e2020\u003c/span\u003e). The graphene powder obtained was reduced by hydrothermal addition of nitrogen. Then, 70 mg of graphene was dispersed in 30 mL of deionized water by ultrasonication for 3 hours and a certain amount of urea was added to the graphene solution. The suspension was ultrasonicated again for 1 hour. The resulting mixture was transferred into a Teflon-lined autoclave and heated at 180 \u0026ordm;C for 12 hours. The black product is obtained by centrifugation. And finally, the precipitate was washed several times with deionized water to remove impurities and then dried at 60 \u0026ordm;C in an oven for 24 hours (Ramezani \u0026amp; Dehghani, \u003cspan citationid=\"CR24\" class=\"CitationRef\"\u003e2019\u003c/span\u003e).\u003c/p\u003e \u003c/div\u003e \u003cdiv id=\"Sec4\" class=\"Section2\"\u003e \u003ch2\u003e2.2 Synthesis of NiO and TiO\u003csub\u003e2\u003c/sub\u003e Nanoparticles\u003c/h2\u003e \u003cp\u003eSynthesis of NiO nanoparticles were prepared by incorporating 250 mL of 1.2 M NaOH solution into a 1000 mL burette and then added to 250 mL of 0.5 M NiSO\u003csub\u003e4\u003c/sub\u003e solution drop by drop until used up while stirring using a magnetic stirrer at 1000 rpm at room temperature. The formed Ni(OH)\u003csub\u003e2\u003c/sub\u003e precipitate was separated and washed until it was free of sulfate and the filtrate had a neutral pH. The content of sulfate impurities in the filtrate was tested by adding BaCl\u003csub\u003e2\u003c/sub\u003e solution to the filtrate until no white precipitate formed. Then the cleaned Ni(OH)\u003csub\u003e2\u003c/sub\u003e solid was dried in an oven at 70 \u0026ordm;C for 24 hours. The dried solids were then calcined at 800 \u0026ordm;C for 2 hours.\u003c/p\u003e \u003cp\u003eFor the next step, TiO\u003csub\u003e2\u003c/sub\u003e nanoparticles was prepared using the annealing method which was initiated by dissolving 10 g of TiO\u003csub\u003e2\u003c/sub\u003e Degussa and dissolving it with distilled water and ethanol (1:1). Then the suspension was ultrasonicated for 1 hour at 80 \u0026ordm;C. Then the suspension was filtered and dried at 500 \u0026ordm;C using a closed container for 3 hours (Lal et al., \u003cspan citationid=\"CR15\" class=\"CitationRef\"\u003e2022\u003c/span\u003e; Salim et al., \u003cspan citationid=\"CR25\" class=\"CitationRef\"\u003e2023\u003c/span\u003e).\u003c/p\u003e \u003c/div\u003e \u003cdiv id=\"Sec5\" class=\"Section2\"\u003e \u003ch2\u003e2.3 Preparation of NG@NiO-TiO\u003csub\u003e2\u003c/sub\u003e Electrode\u003c/h2\u003e \u003cp\u003eNGr@NiO/TiO\u003csub\u003e2\u003c/sub\u003e was prepared with the composition of NiO, TiO\u003csub\u003e2\u003c/sub\u003e, and NGr with a composite mass ratio of 15:5:80, 10:10:80, and 5:15:80 (wt%) which was dissolved in 50 mL of deionized water mixture, then ultrasonicated for 1 hour. After that, the suspension mixture was transferred into a 100 mL Teflon-coated stainless steel autoclave at 200\u0026deg;C for 6 hours. After the reaction was complete, the autoclave was allowed to stand until room temperature, the product obtained was washed several times with deionized water and ethanol and dried at 60\u0026deg;C for 24 hours. Furthermore, the product obtained was annealed at 350 \u0026ordm;C for 2 hours. Next, prepare the electrode by homogenizing a mixture of 0.05 g NGr@NiO/TiO\u003csub\u003e2\u003c/sub\u003e nanocomposite and 0.3 paraffin oil which is stirred at 400 rpm for 15 minutes while heated at 80 ℃. Then the NGr@NiO/TiO\u003csub\u003e2\u003c/sub\u003e paste was put into a 3 mm diameter glass tube, pressed gently, smoothed on the surface, and connected to a copper wire. Finally, composite comparators were made, each labeled NG, NGr@TiO\u003csub\u003e2\u003c/sub\u003e and NG@NiO.\u003c/p\u003e \u003c/div\u003e \u003cdiv id=\"Sec6\" class=\"Section2\"\u003e \u003ch2\u003e2.4 Electrochemical Properties Measurements\u003c/h2\u003e \u003cp\u003eThe electrochemical properties of the prepared samples were measured in a mixture of K\u003csub\u003e3\u003c/sub\u003e[Fe(CN)\u003csub\u003e6\u003c/sub\u003e] solution and 1 M KOH electrolyte using a three-electrode system. The three-electrode system includes a counter electrode (platinum electrode), a reference electrode (Ag/AgCl), and a working electrode (prepared sample). Next, electrodes are measured based on composition variations (NGr composite, NGr@TiO\u003csub\u003e2\u003c/sub\u003e, NGr@NiO, and NGr@NiO/TiO\u003csub\u003e2\u003c/sub\u003e (80:10:10, 80:5:15, and 80:15:10), scan rate variations (5- 100 mV/s) and cycle variations (1\u0026ndash;5 cycles).\u003c/p\u003e \u003c/div\u003e \u003cdiv id=\"Sec7\" class=\"Section2\"\u003e \u003ch2\u003e2.5 Characterizations\u003c/h2\u003e \u003cp\u003eThe morphology of the electrode was characterized using Xray diffraction, XRD (Shimadzu 6000) at 2θ\u0026thinsp;=\u0026thinsp;20-80o with Cu-Kα\u0026thinsp;=\u0026thinsp;1.54060). The morphology of the nanocomposites was characterized using scanning electron microscopy, SEM (HITACHI SU3500). To identify chemical bonds and functional groups, Fourier transforms infrared (FT-IR) spectra was used (Shimadzu Varian 4300 spectrophotometer). The electrochemical properties of the nanocomposites were characterized by cyclic voltammetry techniques using a DY2100 potentiostat.\u003c/p\u003e \u003c/div\u003e"},{"header":"3 Result and Discussion","content":"\u003cdiv id=\"Sec9\" class=\"Section2\"\u003e \u003ch2\u003e3.1 Morphological and Structure of NG@NiO/TiO\u003csub\u003e2\u003c/sub\u003e Nanocomposite\u003c/h2\u003e \u003cp\u003eThe production of N-Graphene (NG) involves utilizing urea to react with graphene oxide obtained via the Hummer method. This crucial step aids in the reduction of various functional groups, such as phenol, ketone, epoxy, carboxyl, and carbonyl groups. These groups arise and attach to the graphene during the oxidation process of graphite, eventually resulting in the formation of graphene oxide. The substitution of these functional groups is made possible by the introduction of N atoms from urea (Nurdin et al., \u003cspan citationid=\"CR22\" class=\"CitationRef\"\u003e2022\u003c/span\u003e; Wibowo et al., \u003cspan citationid=\"CR31\" class=\"CitationRef\"\u003e2020\u003c/span\u003e). The modification uses a combination of NiO and TiO\u003csub\u003e2\u003c/sub\u003e nanoparticle pairs with several different concentrations, including NGr (100:0:0), NGr@NiO (80:20:0), NGr@TiO\u003csub\u003e2\u003c/sub\u003e (80:0:20), NGr @NiO/TiO\u003csub\u003e2\u003c/sub\u003e (80:10:10, 80:5:15, and 80:15:5) (wt%) where we have identified the morphology, crystal structure and bonds formed in this composite material.\u003c/p\u003e \u003cp\u003eThe nanocomposite XRD pattern is presented in Fig.\u0026nbsp;\u003cspan refid=\"Fig1\" class=\"InternalRef\"\u003e1\u003c/span\u003e. The graphene peak is located at 2θ=26.4\u0026deg;, which is consistent with previous studies by Dong et al. (Dong et al., \u003cspan citationid=\"CR6\" class=\"CitationRef\"\u003e2019\u003c/span\u003e) and Wibowo et al. (Wibowo et al., \u003cspan citationid=\"CR30\" class=\"CitationRef\"\u003e2022\u003c/span\u003e) that showed the layered graphene structure obtained from XRD spectra. Additionally, NiO diffraction peaks at 37.2◦, 43.3◦, and 64.44◦ were observed and can be Miller Indexed to the (111), (200), and (220) planes of NiO nanoparticles' structure, as reported in JCPDS 47-1049. Moreover, TiO2 is dominated by anatase crystals compared to JCPDS 21-1272. At 2θ\u0026thinsp;=\u0026thinsp;25.5\u0026deg;, 37.9\u0026deg;, 39.39\u0026deg;, 48.1\u0026deg;, 56.7\u0026deg;, the diffraction peaks were observed and indexed to the (101), (103), (112), (200), and (105) planes. Additionally, rutile crystals were identified at 2θ\u0026thinsp;=\u0026thinsp;27.74\u0026deg;, 56.56\u0026deg;, and 64.20\u0026deg;, with index positions to the (110), (201), and (002) planes, compared to JCPDS 21-1276. Furthermore, the Scherrer formula is used to obtain an average crystal size for particles of 19.66 nm.\u003c/p\u003e \u003cp\u003e \u003c/p\u003e \u003cp\u003eTo confirm the findings of the XRD analysis, SEM characterization was conducted. The results revealed the presence of a mixture of NiO/TiO2 nanoparticles on the surface of the graphene material. Figure\u0026nbsp;\u003cspan refid=\"Fig2\" class=\"InternalRef\"\u003e2\u003c/span\u003ea provides a clear view of the distinctive thin layer structure of this composite and highlights the distribution of the nano hollow NiO/TiO\u003csub\u003e2\u003c/sub\u003e on the NGr surface, which has been previously documented (J. Xu et al., \u003cspan citationid=\"CR33\" class=\"CitationRef\"\u003e2017\u003c/span\u003e). n Fig.\u0026nbsp;\u003cspan refid=\"Fig2\" class=\"InternalRef\"\u003e2\u003c/span\u003eb, the spherical nanoparticles are shown to cover almost the entire surface of the graphene layer. To determine the diameter size of the NiO/TiO\u003csub\u003e2\u003c/sub\u003e particles on the thin layer composites, SEM characterization results were processed using image-J software with the \"analyze particles\" feature. The size distribution of NiO/TiO\u003csub\u003e2\u003c/sub\u003e particle diameters on the NGr surface ranged from 79.78 to 362.13 nm, with an average diameter of 130 nm and an R square value of 0.94212, indicating good data (Fig.\u0026nbsp;\u003cspan refid=\"Fig2\" class=\"InternalRef\"\u003e2\u003c/span\u003ec). The continuous NGr phase, as reported by Chen et al. (Chen et al., \u003cspan citationid=\"CR3\" class=\"CitationRef\"\u003e2019\u003c/span\u003e), can effectively improve the structural stability of the NGr@NiO/TiO\u003csub\u003e2\u003c/sub\u003e nanocomposite during the charge-discharge process.\u003c/p\u003e \u003cp\u003e \u003c/p\u003e \u003cp\u003eUsing FTIR analysis, we were able to identify the chemical processes that occur during nanocomposite formation, including the development of chemical bonds and coordination. The results are presented in Fig.\u0026nbsp;\u003cspan refid=\"Fig3\" class=\"InternalRef\"\u003e3\u003c/span\u003e. Figure\u0026nbsp;\u003cspan refid=\"Fig3\" class=\"InternalRef\"\u003e3\u003c/span\u003ea displays the NGr spectrum, which shows peaks of epoxy groups and C-O stretching at around 1125 cm\u003csup\u003e\u0026minus;\u0026thinsp;1\u003c/sup\u003e. Heating NGr during formation causes a peak at around 2874 cm\u003csup\u003e\u0026minus;\u0026thinsp;1\u003c/sup\u003e to appear, indicating the presence of aliphatic C-H groups. Furthermore, the formation of NGr is confirmed by the observation of N\u0026ndash;H stretching as a hump at around 3078 cm\u003csup\u003e\u0026minus;\u0026thinsp;1\u003c/sup\u003e. In Fig.\u0026nbsp;\u003cspan refid=\"Fig3\" class=\"InternalRef\"\u003e3\u003c/span\u003eb, the C-N bond stretching around 1400 cm\u003csup\u003e\u0026minus;\u0026thinsp;1\u003c/sup\u003e is identified as a characteristic of NGr, and Ni-O is identified at an absorption peak of 700 cm\u003csup\u003e\u0026minus;\u0026thinsp;1\u003c/sup\u003e. TiO\u003csub\u003e2\u003c/sub\u003e absorption peaks are also observed at wave numbers 1638 cm\u003csup\u003e\u0026minus;\u0026thinsp;1\u003c/sup\u003e and 425 cm\u003csup\u003e\u0026minus;\u0026thinsp;1\u003c/sup\u003e, caused by Ti-O vibrations. As a result, the nanocomposite process's new coordination chemistry maintains the intrinsic properties of the individual elements. Any changes to this process's performance can be directly linked to the electrochemical properties of these nanocomposites.\u003c/p\u003e \u003cp\u003e \u003c/p\u003e \u003c/div\u003e \u003cdiv id=\"Sec10\" class=\"Section2\"\u003e \u003ch2\u003e3.2 Cyclic Voltammetry Performance\u003c/h2\u003e \u003cp\u003e \u003cb\u003eScan Rate and Cyclic Variation\u003c/b\u003e \u003c/p\u003e \u003cp\u003eSix different variations of the NG@NiO/TiO2 nanocomposite anode were tested to find the best composition. The electrodes included NGr, NGr@TiO2, NGr@NiO, and three variations of NGr@NiO/TiO2. Each electrode was tested in an electrochemical cell with a 0.01 M K3(Fe(CN)6) solution and 1 M KOH electrolyte. The voltammogram curves of the K3[Fe(CN)6] solution were measured using a scan rate of 5-100 mV/s over a potential range of -0.8 to 0.8 V/s.\u003c/p\u003e \u003cp\u003eAdding metal oxide to the K\u003csub\u003e3\u003c/sub\u003e[Fe(CN)\u003csub\u003e6\u003c/sub\u003e] solution improved its measurement results compared to NGr due to the presence of nano-hollow NiO and TiO\u003csub\u003e2\u003c/sub\u003e doping. The reactions in the Fe(CN)\u003csub\u003e6\u003c/sub\u003e\u003csup\u003e3\u0026minus;\u003c/sup\u003e/Fe(CN)\u003csub\u003e6\u003c/sub\u003e\u003csup\u003e4\u0026minus;\u003c/sup\u003e system were reversible, and NGr and NGr@TiO\u003csub\u003e2\u003c/sub\u003e were good electrodes with clear current peaks. NGr@NiO and NGr@NiO/TiO\u003csub\u003e2\u003c/sub\u003e electrodes tended to form voltammograms resembling a rectangle. A slower scan rate resulted in a thicker diffusion layer, causing a reduction in the current generated (Brownson \u0026amp; Banks, \u003cspan citationid=\"CR2\" class=\"CitationRef\"\u003e2014\u003c/span\u003e).\u003c/p\u003e \u003cp\u003e \u003c/p\u003e \u003cp\u003eDetermining the stability of an electrode involves taking multiple measurements. By analyzing the formation of oxidation and reduction peaks and producing a stable voltammogram, we can determine the repeatability and reversibility of the electrode. After conducting 5 cycles of measurements on the NGr electrode, we found that it has good stability. Additionally, the voltammogram produced during the repetition process was consistently stable. The NGr@TiO\u003csub\u003e2\u003c/sub\u003e electrode also showed good potential after undergoing a repeatability test for 5 cycles. Furthermore, the NGr@NiO electrode maintained good stability during the 5th cycle, as shown in the accompanying image (Fig.\u0026nbsp;\u003cspan refid=\"Fig4\" class=\"InternalRef\"\u003e4\u003c/span\u003eb, d, f).\u003c/p\u003e \u003cp\u003e \u003c/p\u003e \u003cp\u003eBased Fig.\u0026nbsp;\u003cspan refid=\"Fig5\" class=\"InternalRef\"\u003e5\u003c/span\u003e NGr@NiO/TiO\u003csub\u003e2\u003c/sub\u003e electrode's cyclic voltammetric results showed good stability after 5 cycles using 0.01 M K\u003csub\u003e3\u003c/sub\u003e(Fe(CN)\u003csub\u003e6\u003c/sub\u003e) and 1 M KOH solutions. The NGr@NiO/TiO\u003csub\u003e2\u003c/sub\u003e 80:15:5 (wt%) electrode had the best stability and successful electron transfer. Nitrogen doping increases wettability and binding energy, allowing for more ion movement and higher capacitance. NiO/TiO\u003csub\u003e2\u003c/sub\u003e nanoparticles play a crucial role.\u003c/p\u003e \u003cp\u003e \u003cb\u003eSpecific Capacity Measurement\u003c/b\u003e \u003c/p\u003e \u003cp\u003eKapasitansi spesifik bahan elektroda NGr@NiO/TiO\u003csub\u003e2\u003c/sub\u003e beserta anoda pembandingnya dihitung dari kurva CV yaitu Gambar 4a, c, d dan Gambar 5a, c, d seperti yang ditunjukkan pada Gambar 6. Berdasarkan Gambar 6a memperlihatkan kapasitas spesifik NGr, NGr@TiO\u003csub\u003e2\u003c/sub\u003e and NGr@NiO composite berbanding terbalik dengan scan rate 5-100 mV/s dengan nilai masing-masing yaitu NGr (135.38, 73.95, 48.69, 29.43, 20.46 F/g), NGr@TiO2 (287.11, 203.58, 128.02, 62.53, 31.26 F/g) dan NGr@NiO (1959.71, 979.85, 541.38, 262.77, 131.38 F/g). Sedangkan Gambar 6b memperlihatkan kapasitas spesifik dari NGr@NiO/TiO\u003csub\u003e2\u003c/sub\u003e sesuai komposisi diantaranya 80:10:10 (741.02, 376.76, 188.86, 85.28, 48.36 F/g), 80:5:15 (408.53, 234.13, 131.78, 60.76, 40.89 F/g) and 80:15:5 (839.84, 440.93, 238.88, 111.04, 60.35 F/g). Gambar 6 juga menunjukkan bahwa nilai kapasitansi spesifik menurun dengan meningkatnya kecepatan pemindaian.\u003c/p\u003e \u003cp\u003e \u003c/p\u003e \u003c/div\u003e"},{"header":"3 Conclusions","content":"\u003cp\u003eBased on the results and discussion that have been described, it can be concluded that the NGr@NiO/TiO\u003csub\u003e2\u003c/sub\u003e nanocomposite has been successfully synthesized with NGr thin films by hydrothermally combining NiO/TiO\u003csub\u003e2\u003c/sub\u003e hollow nanospheres. In addition, the unique structure of the material is supported by XRD, SEM and FTIR characterization data with crystallinity, morphology and bonds directly confirming the success of this synthesis. Electrochemical tests were carried out by optimizing cyclic voltammetry (CV) performance through parameters such as the influence of composition, scan rate and cycle with the best conditions, namely a composite ratio of 80:10:10 (wt%), scan rate of 50 mV/s, the most stable cycle conditions and also taking into account the high specific capacity value of 839.83 F/g. Based on this, it is revealed that the NGr@NiO/TiO\u003csub\u003e2\u003c/sub\u003e composite is very suitable for application in alkali metal ion batteries (AIB).\u003c/p\u003e"},{"header":"Declarations","content":"\u003cp\u003e\u003cstrong\u003eAuthor Contributions\u003c/strong\u003e\u003c/p\u003e\n\u003cp\u003eT.A. and L.A. performed all the experiments.\u0026nbsp;M.Z.M coordinated the study. M.N. and L.O.M.Z.M. writing the manuscript. L.O.M.Z.M and A.A.U. processed the research data. All authors have read and agreed to the published version of the manuscript\u003c/p\u003e\n\u003cp\u003e\u003cstrong\u003eAcknowledgments\u003c/strong\u003e\u003c/p\u003e\n\u003cp\u003eWe are grateful for financial support from the DRPM-Ministry of Research, Technology, and Higher Education of the Republic of Indonesia under Fundamental Research Grant No. DIPA-023.17.1.690523/2023, 48/UN29.20/PG/2023. Also, an acknowledgment to the Titania Research Group (TRG) and Department of Chemistry-Universitas Halu Oleo (UHO) for providing the facilities to conduct experimental work and lab testing.\u0026nbsp;\u003c/p\u003e"},{"header":"References","content":"\u003col\u003e\u003cli\u003e\u003cspan\u003eS.A. Al Kiey, R. Ramadan, M.M. 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J. \u003cb\u003e420\u003c/b\u003e, 130469 (2021)\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":"Battery, N-Graphene, NiO-TiO2, cyclic voltammetry, specific capacitance","lastPublishedDoi":"10.21203/rs.3.rs-3338252/v1","lastPublishedDoiUrl":"https://doi.org/10.21203/rs.3.rs-3338252/v1","license":{"name":"CC BY 4.0","url":"https://creativecommons.org/licenses/by/4.0/"},"manuscriptAbstract":"\u003cp\u003eIn this research, we succeeded in designing a new strategy to synthesize a unique thin film structured of nitrogen doped graphene (NGr) composite combined with coupled NiO/TiO\u003csub\u003e2\u003c/sub\u003e hollow nanospheres using a synergistic hydrothermal method. The NGr@NiO/TiO\u003csub\u003e2\u003c/sub\u003e composite characteristics are demonstrated by several rational characterization techniques such as the morphological shape of NiO/TiO\u003csub\u003e2\u003c/sub\u003e hollow nanospheres which are evenly distributed on the surface of N-graphene with particle distribution in the range 79.78-362.13 nm with an average diameter of 130 nm. In addition, the crystal structures of carbon from NGr, NiO, and TiO\u003csub\u003e2\u003c/sub\u003e (anatase and rutile) have been confirmed and proven by spectra showing the presence of C-N stretching primary amides (1400 cm\u003csup\u003e\u0026minus;\u0026thinsp;1\u003c/sup\u003e), Ni-O stretching (700 cm\u003csup\u003e\u0026minus;\u0026thinsp;1\u003c/sup\u003e) and Ti-O-Ti bond (425 cm\u003csup\u003e\u0026minus;\u0026thinsp;1\u003c/sup\u003e), respectively. The electrochemical test was carried out by optimizing the performance of cyclic voltammetry (CV) through parameters such as the influence of composition, scan rate, and cycle with the best conditions, namely composite ratio 80:10:10 (wt%), scan rate 50 mV/s, condition stable cycle and also calculated the high specific capacity value of 839.83 F/g. Based on this, it is revealed that NGr@NiO/TiO\u003csub\u003e2\u003c/sub\u003e composites can explore the potential and be fully applied in the development of alkaline metal ion (AIB) batteries such as Li/Na/K.\u003c/p\u003e","manuscriptTitle":"Thin Film Structured Superior Anode Material Based N-Graphene Supported Coupled NiO/TiO2 Hollow Nanospheres and Their Cyclic Voltammetry Performance","msid":"","msnumber":"","nonDraftVersions":[{"code":1,"date":"2023-09-13 15:22:13","doi":"10.21203/rs.3.rs-3338252/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":"3700f9d3-cc4d-47a8-a697-f77d7ec71f41","owner":[],"postedDate":"September 13th, 2023","published":true,"recentEditorialEvents":[],"rejectedJournal":[],"revision":"","amendment":"","status":"posted","subjectAreas":[],"tags":[],"updatedAt":"2023-09-14T17:29:26+00:00","versionOfRecord":[],"versionCreatedAt":"2023-09-13 15:22:13","video":"","vorDoi":"","vorDoiUrl":"","workflowStages":[]},"version":"v1","identity":"rs-3338252","journalConfig":"researchsquare"},"__N_SSP":true},"page":"/article/[identity]/[[...version]]","query":{"redirect":"/article/rs-3338252","identity":"rs-3338252","version":["v1"]},"buildId":"J0_U0BvcaRcwD8yVFaRlm","isFallback":false,"isExperimentalCompile":false,"dynamicIds":[84888],"gssp":true,"scriptLoader":[]}