Synthesis of BiVO 4 nanostructures via Hydrothermal Synthesis: Evaluation of its Electrochemical Lithium ion battery performance

Synthesis of BiVO 4 nanostructures via Hydrothermal Synthesis: Evaluation of its Electrochemical Lithium ion battery 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 Synthesis of BiVO 4 nanostructures via Hydrothermal Synthesis: Evaluation of its Electrochemical Lithium ion battery performance Harini R, Sunil T D, Pooja K R, Manjanna J, Nagaraju Gm This is a preprint; it has not been peer reviewed by a journal. https://doi.org/ 10.21203/rs.3.rs-7931892/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 work, bismuth vanadate (BiVO 4 ) NPs were prepared by a low temperature hydrothermal route and were well characterized to assess their electrochemical performances as an anode material for lithium-ion battery (LIB). X-ray diffraction (XRD) established the development of single monoclinic phase with a mean crystallite size of 67 nm. Fourier-transform infrared (FTIR) and Raman spectroscopy studies confirmed the occurrence of Bi-O and V-O vibrational modes, confirming the structural composition of the material synthesized. UV-Vis diffuse reflectance spectroscopy (DRS) confirmed an optical band gap of around 2.2 eV. Electrochemical performance investigations indicated that the BiVO 4 electrode provided an initial discharge capacity of 198 mAh g − 1 at 0.1C (C/10), which decreased gradually to 104 mAh g − 1 at 54 cycles while retaining a Coulombic efficiency of about 98%. In addition, at a current density of 50 mA g − 1 , the electrode retained a stable capacity of 100 mAh g − 1 even at 500 cycles. The synergized structural stability, high lithium storage capacity, and superior cycling life highlight the promise of BiVO 4 as a good anode material for future lithium-ion batteries. BiVO4 NPs Anode Li ion battery Photoluminescence Figures Figure 1 Figure 2 Figure 3 Figure 4 Figure 5 Figure 6 1.0. Introduction The growing global demand for energy is one of the critical challenges of the twenty-first century, making energy research a highly prioritized field. Although technology has improved, non-renewable energy sources such as coal, oil, and natural gas still dominate energy production, which makes up a significant portion of the world's energy consumption[ 1 ]. It is alarming that reports indicate that the world's oil reserves will be depleted in the next 40 years. This scenario calls for urgent development of clean, cost-effective, and environmentally sustainable energy storage and conversion devices. Fuel cells, solar cells, supercapacitors, and lithium-ion batteries (LIBs) are emerging as promising solutions to these challenges [ 2 , 3 ]. Among them, LIBs are promising energy storage technologies for a variety of applications, including mobile devices, portable electronics, hybrid electric vehicles, backup power systems, and military equipment. They are highly appealing because of their high power density, extended cycle life, and rapid charge-discharge capabilities[ 4 , 5 ]. Traditionally, noble-metal-based electrode materials have been widely used in both aqueous and non-aqueous LIBs due to their affordability, excellent energy performance, and remarkable cycling stability. Some other advanced materials explored for improvement in energy density and cyclic stability include metal oxides, hydroxides, binary transition metal oxides, conducting polymers, and metal chalcogenides. These materials, for instance, include metal oxides, such as V 2 O 5 [ 6 ], BiVO 4 , and SiO 2 [ 7 ], which are receiving attention in the application of LIB due to their interesting properties, which include affordability, a larger surface area, and good redox activity. Unfortunately, the limiting factors such as low rate capability and cyclic stability limit its practical application. Researchers have increasingly focused on binary semiconducting metal oxides due to their better electrical conductivity, thermal stability, and higher active surface area as compared to single-component oxides that can solve the above issues[ 8 , 9 ]. Multi objective utilization of materials, such as BiVO 4 and V 2 O 5 in terms of desirable attributes, such as a small bandgap, onset potential, high redox behavior, and long-time stability, also finds application for the treatment of wastewater, catalysis[ 10 ], and energy storage applications. For example, LIBs-based on V 2 O 5 exhibit improved electrochemical performance arising from its structure with layered lattice and variable oxidation states. Similarly, n-type semiconductor BiVO 4 boasts a low optical bandgap in the range 2.2–2.5 eV, excellent reduction potential, superb light absorption ability, and a large capacitive capability. Crystalline forms of BiVO 4 include three forms: zircon-structured tetragonal, scheelite-structured tetragonal, and scheelite-structured monoclinic. Among these, the monoclinic crystal structure exhibits outstanding photocatalytic and electrochemical properties because of its unique lattice distortions, particularly between the BiO 6 octahedra and VO 4 tetrahedra, making it an ideal material for energy storage and conversion applications[ 11 ]. 2.0. Experimental 2.1 Chemicals and electrode materials The following chemicals are procured from Merck: bismuth nitrate pentahydrate [Bi(NO 3 ) 3 ·5H 2 O], ammonium metavanadate (NH 4 VO 3 ), nitric acid (HNO 3 ) All chemicals are analytical in grade and are used without purification. 2.3 Synthesis of BiVO 4 NPs Bismuth vanadate (BiVO 4 ) NPs were synthesized using a hydrothermal method. First, 1 mmol of bismuth nitrate pentahydrate [Bi(NO 3 ) 3 ·5H 2 O] was dispersed in 35 mL of 0.5 M nitric acid (HNO 3 ) solution and stirred for 30 minutes to ensure complete dissolution. In a separate step, 1 mmol of ammonium metavanadate (NH 4 VO 3 ) was dissolved in 35 mL of distilled water and stirred under heat for 30 minutes until a clear solution was obtained. The clear solution was then added dropwise to the bismuth nitrate solution while stirring continuously. The resulting mixture, a brick-red suspension, was stirred for another 30 minutes. This suspension was then transferred to a 75 mL autoclave, sealed, and heated to 160°C for 42 hours. After the hydrothermal reaction, the brownish-yellow solid product was collected and washed three times with deionized water and ethanol. Finally, the product was dried at 80°C for 3 hours to obtain the BiVO 4 NPs. 3.0. Characterization The crystal structure and the size of BiVO 4 NPs were analysed using Rigaku martlab X- Ray diffractometer (XRD) with monochromatized CuKα radiation (1.5418Å) in 2θ range 10–70. Functional group Bi-Oand V-O bond of BiVO 4 were analysed using FTIR (Bruker Alpha P-spectrophotometer) in the wavenumber range 350 to 4000 cm − 1 . The optical properties of the NPs were evaluated using Agilent technology Cary-60 UV-Vis diffuse reflectance spectrophotometer (UV-Vis DRS) in the range of 200 to 800 nm. Morphological properties, elemental analysis, and size of the nano materials were identified using a scanning electron microscope, energy dispersive X-ray spectrometer (TESCAN Vega 3LMU. Horiba Xplora Plus Raman microscope was used to check Raman measurements. Biologics instrument was employed to study electrochemical properties. 3.1. Electrochemical Measurements Electrochemical studies of BiVO 4 NPs were done for LIB anode applications. The electrochemical properties were studied in coin cell arrangement (CR2032) with lithium metal as both reference and counter electrode. The working electrode consisted of active material, acetylene black and polyvinylidene fluoride (PVDF) in the ratio 80:15:5. The materials were taken in the above ratio in an agate mortar and ground well. Further, a small quantity of N-methylpyrrolidine (NMP) was added to acquire slurry. The slurry was uniformly coated on pre-treated copper foil and subjected to drying at 110⁰C for 12 hours in a vacuum oven. The pretreatment of Cu foil was done by etching the foils in 5 N HNO 3 and then washings them abundantly with DD water, followed by acetone and finally air dried. Argon filled glove box assembled coin cells by dissolving 1 M LiPF 6 in ethylene carbonate, diethyl carbonate and dimethyl carbonate (2:1:2 v/v) as electrolyte and a porous polypropylene membrane as a separator. Charge/discharge tests are carried out on Biologic battery tester at room temperature at diverse current rates and respective voltage ranges [ 12 ]. 4.0. Results and discussion 4.1. XRD analysis X-ray diffraction (XRD) analysis was used to verify the hydrothermally produced BiVO 4 NPs phase purity and crystalline structure, as shown in Fig. 1 (a). The XRD pattern's diffraction peaks are in good agreement with standard data (JCPDS card number. 14–0688) and the monoclinic phase of BiVO 4 (space group: I2/a)[ 13 ]. It was discovered that the lattice parameters were a = 5.195 nm, b = 11.701 nm, and c = 5.092 nm. The Scherrer equation was used to determine the BiVO 4 NPs average crystallite size: D = Kλ/βCos θ Where θ is the Bragg angle, β is the full width at half maximum (FWHM) of the diffraction peak, λ is the X-ray wavelength of the Cu Kα source (1.54 Å), and D is the crystallite size. The average crystallite size was calculated to be roughly 67 nm using this method. 4.2. FTIR studies The characteristic peaks in the FTIR spectrum of the synthesized BiVO 4 NPs (Fig. 2 (b)) are in good agreement with those found in the literature. The stretching vibrations of the terminal V = O bonds are identified by a noticeable band at 1025 cm − 1 [14 ] .The antisymmetric stretching of bridging oxygen atoms between two vanadium center (V–O–V connections) is linked to the peaks seen at 830 cm − 1 and 720 cm − 1 . Furthermore, the symmetric stretching vibrations of the V–O–V units are represented by a band that emerges at 412 cm − 1 . The bending mode of adsorbed water molecules on the surface of the nanoparticle is responsible for a prominent peak at 1614 cm − 1 [ 15 , 16 ]. 4.3. UV-Vis analysis The BiVO 4 NPs optical characteristics were examined through the technique of UV-Visible Diffuse Reflectance Spectroscopy (UV-DRS). The material's photocatalytic capacity under visible illumination was demonstrated by the recorded spectrum's significant absorption edge in the visible light band. Using the Kubelka–Munk function on the reflectance data, the optical band gap was calculated and plotted as a Tauc plot, [(F(R)hv) 2 ], versus photon energy (hν), assuming a direct allowed transition. An optical band gap of roughly 2.2 eV was obtained by extrapolating the linear part of the curve from the Tauc plot to the photon energy axis as shown in Fig. 1 (c). This value validates the suitability of monoclinic BiVO 4 as a visible-light-responsive photocatalyst and is in good agreement with previously published data[ 17 ]. 4.4. Raman Studies The symmetric stretching vibration mode of the vanadate group (VO 4 3− ) is characterized by a clear and powerful peak centered about 827 cm − 1 in the Raman spectra of BiVO 4 nanoparticles, as seen in the Fig. 1 (d). Given that similar vibrational modes are commonly seen in this phase, this strong and sharp peak validates the creation of the monoclinic scheelite structure of BiVO 4 . Furthermore, the bending and asymmetric stretching modes of the VO 4 units are responsible for the smaller peaks seen in the lower wavenumber region. The produced BiVO 4 NPs phase purity and structural stability are further demonstrated by the lack of notable extra peaks or shifts. All things considered, the Raman study confirms that monoclinic BiVO 4 with distinct vibrational properties was successfully formed [ 18 ]. 4.5. SEM Analysis Surface morphology and elemental analysis of the produced BiVO 4 NPs were carried out by scanning electron microscopy (SEM) and energy-dispersive X-ray spectroscopy (EDS), respectively, as presented in Fig. 2 .The low-magnification SEM image (Figure. 2(a)) indicates that the BiVO 4 particles exhibit a spherical hierarchical structure, that are spherical aggregates with an average size in the micrometer range. At increased magnification (Fig. 2 (b-c)), the morphology is resolved into ultrathin nanosheets emanating from a central core, indicating anisotropic growth and self-assembled architecture. Such a porous and layered morphology is beneficial in baterry applications. The EDS spectrum (Fig. 2 (d)) identifies the presence of bismuth (Bi), vanadium (V), and oxygen (O), with typical peaks including Bi-M, Bi-L, V-K, and O-K, which confirm the successful formation of stoichiometric and phase-pure BiVO 4 free of detectable impurities [ 19 ]. 4.6. TEM Studies TEM and HRTEM images verify the nanoscale morphology and crystallinity of the resultant BiVO 4 NPs. Figure.4(a) exhibits aggregated, semi-spherical particles with dimensions of 20–80 nm. Figure.4(b) depicts more distinct particles with smoother surfaces, with an average size of 15–30 nm.Figure.4(c) is a closer image, with clear particle boundaries and verifying their nanocrystalline character. The HRTEM Figure.4(d) exhibits distinct lattice fringes, reflecting high crystallinity.The interplanar spacing observed is corresponding to the (001) plane, as depicted in the inset.This indicates a well-defined structure of scheelite-type for BiVO 4 . These characteristics render BiVO 4 appropriate for energy applications. 4.6. Photoluminescence Studies In electronic components, PL spectroscopy is frequently used to ascertain details such as the presence of surface defects, oxygen vacancies, and the effectiveness of charge-carrier trapping and transfer. This is explained by the fact that the recombination of photoexcited charges is the cause of the PL emission of BiVO 4 [ 20 ]. The recombination of the hole formed from the hybrid orbitals of Bi 6s and O 2p and the electron generated from the V 3d orbitals are responsible for the strong emission centred at 546 nm and the excitation at 340 nm, respectively, observed in the PL spectrum of BiVO 4 nanoparticles [ 21 ] (Fig. 4a-b). 5.0. Electrochemical properties of BiVO nanoparticles The electrochemical properties of the enhanced BiVO 4 electrode were thoroughly examined via galvanostatic charge–discharge (GCD) experiments, prolonged cycling, and Coulombic efficiency testing, as illustrated in Fig. 4. As apparent from Fig. 5 (a), the BiVO 4 electrode attained an initial discharge capacity of 198 mAh g − 1 with a current density of C/10 (0.1C) in the voltage range 1.0–2.5 V. The high initial capacity is because of the lithium intercalation/deintercalation reaction achieved by the porous nature and large surface area of the BiVO 4 nanomaterial. Yet, upon repeated cycling, the capacity decreased progressively, to 104 mAh g − 1 after 54 cycles, showing a 48% capacity fade. This loss could be caused by active material degradation, structural instability, or SEI formation with time[ 22 , 23 ]. Figure 5 (b) shows the stable long-term cycling performance at increased current density of 50 mA g − 1 , for which the BiVO 4 electrode still exhibits a fixed capacity of about 100 mAh g − 1 even after 500 cycles, illustrating great cycling stability and rate ability. Such reliable long-term stability suggests great high-rate application prospect of BiVO 4 electrode material. In the Fig. 5 (c) indicates the capacity and Coulombic efficiency trends after 54 cycles. While the discharge capacity continuously drops, the Coulombic efficiency is always high at about 98%, reflecting superior charge/discharge reversibility and small side reactions. This high efficiency implies that the electrode maintains structural integrity and stable electrochemical kinetics throughout cycling. In total, the findings confirm that the well-separated BiVO 4 electrode exhibits good electrochemical and structural stability, which is a promising anode material for high-rate lithium-ion battery applications. The high initial capacity, great Coulombic efficiency, and long-term cycling stability at various current densities confirm its appropriateness for energy storage technology[ 24 , 25 ]. The cyclic voltammetry curve of BiVO 4 as a lithium-ion battery anode material was obtained in the potential window of 0.01–3.0 V at 0.5 mV/s scan rate in the Fig. 5 d. The CV profile shows well-defined redox peaks, validating the reversible lithiation and delithiation characteristics of BiVO 4 . During the first cathodic scan, a prominent reduction peak at 0.5 V is due to the conversion reaction of BiVO 4 with lithium ions to produce metallic Bi and Li 2 O, followed by dealloying of Bi with Li to produce Li x Bi phases. The anodic peaks corresponding to these near 1.5-2.0 V are due to the dealloying of Li x Bi and the partial re-formation of BiVO 4 , reflecting good electrochemical reversibility. The stable and almost overlapped curves in following cycles indicate superior cyclic stability and good electrode kinetics, which means that BiVO 4 retains structural integrity throughout repeated lithiation/delithiation cycles. In summary, the CV response validates the efficient redox activity and reversible Li + storage ability of BiVO 4 as a great anode material for lithium-ion batteries. 5.1. Impedance Spectra The impedance plots of BiVO 4 NPs, as evident from the Nyquist plot (Fig. 6 ), are rich in information regarding their electrical conductivity and charge transfer mechanism. The plot consists of a high-frequency semicircular arc followed by a low-frequency linear tail. Appearance of the semicircle signifies the charge transfer resistance (R ct ) at the electrode–electrolyte interface, which is equivalent to the bulk resistance and interfacial phenomena of the material. The steep straight line at low frequencies indicates the Warburg impedance, which is generally related to ion diffusion inside the electrode material. The comparably small semicircle diameter suggests low charge transfer resistance, implying that the BiVO 4 nanoparticles are electrically conductive and support rapid charge transport. Such activity is favorable for electrochemical device applications, such as photocatalysis and energy storage, where rapid electron mobility and minimized recombination losses are essential. 6.0. Conclusion In summary, BiVO 4 NPs were effectively synthesized and methodically analyzed for their structural, optical, vibrational, and electrochemical characteristics. The monoclinic nature of the phase with a crystallite size of 67 nm was ensured through XRD analysis. The existence of distinctive vibrational modes relating to Bi–O and V–O bonds was ensured by FTIR and Raman spectroscopy, which confirmed the structural integrity of the material obtained. UV-Vis DRS was used to calculate the optical band gap of about 2.2 eV, and it was deemed appropriate for use in visible-light-driven applications. Electrochemical characterization showed that the optimized BiVO 4 electrode had a maximum initial discharge capacity of 198 mAh g − 1 at C/10, with 104 mAh g − 1 being retained after 54 cycles at a Coulombic efficiency of around 98%. Even at a high current density of 50 mA g⁻¹, the electrode retained 100 mAh g − 1 capacity after 500 cycles, exhibiting good rate capability and cycling stability. These results indicate that BiVO 4 is a good candidate anode material for high-performance lithium-ion batteries due to its stable structure, efficient redox behavior, and long-term durability. Declarations Declaration of Competing Interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper. Credit Authorship R: Writing – original draft, Method ology, Formal analysis, Data curation. K R: Writing – review & editing, Conceptualization. T D: Data curation. J: Resources, Data curation. G : Supervision, writing and reviewing. Author Contribution R: Writing – original draft, Method ology, Formal analysis, Data curation. K R: Writing – review & editing, Conceptualization. T D: Data curation. J: Resources, Data curation. G : Supervision, writing and reviewing. Acknowledgement Pooja K. R. gratefully acknowledges the Department of Science and Technology KSTePS Fellowship (Award No: CHE-02/2024-25) for the financial support. One of the author G. Nagaraju acknowledges VGST-K-FIST 9GRD 950/2020–2021), Govt. of Karnataka for financial support. Data availability Data will be made available on request. References C. Ayoo, Towards energy security for the twenty-first century, Energy policy (2020) 15-40. R. Hafezi, M. Alipour, Renewable energy sources: traditional and modern-age technologies, Affordable and clean energy, Springer2021, pp. 1085-1099. R. Asghar, M.H. Sulaiman, Z. Mustaffa, N. Ullah, W. 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09:29:37","extension":"xml","order_by":19,"title":"","display":"","copyAsset":false,"role":"acdc-reference","size":68611,"visible":true,"origin":"","legend":"","description":"","filename":"8bd0053ed40d4c42ad62d47d9d9fb9a31structuring.xml","url":"https://assets-eu.researchsquare.com/files/rs-7931892/v1/289a9d70b872a9f05da367f6.xml"},{"id":97468917,"identity":"e1994814-8b7f-4271-b5d3-22714df967c8","added_by":"auto","created_at":"2025-12-04 17:16:12","extension":"html","order_by":20,"title":"","display":"","copyAsset":false,"role":"acdc-reference","size":73998,"visible":true,"origin":"","legend":"","description":"","filename":"earlyproof.html","url":"https://assets-eu.researchsquare.com/files/rs-7931892/v1/32f047596a6449c5b4714088.html"},{"id":97468889,"identity":"854b044d-2f1c-4306-90e5-e021dd1b25c0","added_by":"auto","created_at":"2025-12-04 17:16:12","extension":"png","order_by":1,"title":"Figure 1","display":"","copyAsset":false,"role":"figure","size":199232,"visible":true,"origin":"","legend":"\u003cp\u003eXRD pattern Inset: Crystal structure of BiVO\u003csub\u003e4\u003c/sub\u003e, (b) FTIR spectrum, (c) DRS UV–Visible spectrum (d) Raman Spectrum of BiVO\u003csub\u003e4\u003c/sub\u003e NPs\u003c/p\u003e","description":"","filename":"1.png","url":"https://assets-eu.researchsquare.com/files/rs-7931892/v1/769459c7be624cc9d8274ad5.png"},{"id":97468892,"identity":"dcda5892-7752-4d29-b4f9-6f9ee88b2fb9","added_by":"auto","created_at":"2025-12-04 17:16:12","extension":"png","order_by":2,"title":"Figure 2","display":"","copyAsset":false,"role":"figure","size":261505,"visible":true,"origin":"","legend":"\u003cp\u003eFE-SEM image (a-b), EDX spectrum (c) of BiVO\u003csub\u003e4\u003c/sub\u003e NPs\u003c/p\u003e","description":"","filename":"2.png","url":"https://assets-eu.researchsquare.com/files/rs-7931892/v1/9c07b789989bdefdd13c328f.png"},{"id":97468899,"identity":"155c0368-efac-426c-9992-a132ceb34e4b","added_by":"auto","created_at":"2025-12-04 17:16:12","extension":"png","order_by":3,"title":"Figure 3","display":"","copyAsset":false,"role":"figure","size":48103,"visible":true,"origin":"","legend":"\u003cp\u003ePhotoluminescence (a) excitation spectra, (b) emission spectra of BiVO\u003csub\u003e4\u003c/sub\u003e NPs\u003c/p\u003e","description":"","filename":"3.png","url":"https://assets-eu.researchsquare.com/files/rs-7931892/v1/92b88384b7e1b7edd67bf0bc.png"},{"id":97468894,"identity":"c831b30b-3d28-43db-9021-d21faf719859","added_by":"auto","created_at":"2025-12-04 17:16:12","extension":"png","order_by":4,"title":"Figure 4","display":"","copyAsset":false,"role":"figure","size":267604,"visible":true,"origin":"","legend":"\u003cp\u003e(a) exhibits aggregated, semi-spherical particles with dimensions of 20–80 nm. Figure.4(b) depicts more distinct particles with smoother surfaces, with an average size of 15–30 nm.Figure.4(c) is a closer image, with clear particle boundaries and verifying their nanocrystalline character. The HRTEM Figure.4(d)\u0026nbsp; exhibits distinct lattice fringes, reflecting high crystallinity.The interplanar spacing observed is corresponding to the (001) plane, as depicted in the inset.This indicates a well-defined structure of scheelite-type for BiVO\u003csub\u003e4\u003c/sub\u003e. These characteristics render BiVO\u003csub\u003e4\u003c/sub\u003e appropriate for energy applications.\u003c/p\u003e","description":"","filename":"4.png","url":"https://assets-eu.researchsquare.com/files/rs-7931892/v1/7399f40caa9cfed836a5ad31.png"},{"id":97669086,"identity":"0b932109-e780-40f2-b542-f3ba3ad7870a","added_by":"auto","created_at":"2025-12-08 09:27:11","extension":"png","order_by":5,"title":"Figure 5","display":"","copyAsset":false,"role":"figure","size":160147,"visible":true,"origin":"","legend":"\u003cp\u003e(a) Variation of specific and volumetric capacities with number of cycles at different current densities, (b) cycling performance of BiVO\u003csub\u003e4\u003c/sub\u003e electrode at 50 A g\u003csup\u003e-1\u003c/sup\u003e,(c) Cycling stability and Coulombic efficiency over 50 cycles showing excellent capacity retention, (d) Cyclic voltammetry \u0026nbsp;curves of the BiVO\u003csub\u003e4\u003c/sub\u003e anode\u003c/p\u003e","description":"","filename":"5.png","url":"https://assets-eu.researchsquare.com/files/rs-7931892/v1/3404b1d15e09096ce7996ced.png"},{"id":97468897,"identity":"62709d13-2cd5-4ca8-aa3a-3dabc8c70e28","added_by":"auto","created_at":"2025-12-04 17:16:12","extension":"png","order_by":6,"title":"Figure 6","display":"","copyAsset":false,"role":"figure","size":6183,"visible":true,"origin":"","legend":"\u003cp\u003eImpedance spectra of BiVO\u003csub\u003e4\u003c/sub\u003e NPs\u003c/p\u003e","description":"","filename":"6.png","url":"https://assets-eu.researchsquare.com/files/rs-7931892/v1/38caaeb27962743aba3acc93.png"},{"id":100360323,"identity":"0dd6bada-047e-4474-b35a-42f8b95e3e36","added_by":"auto","created_at":"2026-01-16 07:38:23","extension":"pdf","order_by":0,"title":"","display":"","copyAsset":false,"role":"manuscript-pdf","size":1498697,"visible":true,"origin":"","legend":"","description":"","filename":"manuscript.pdf","url":"https://assets-eu.researchsquare.com/files/rs-7931892/v1/f47f1e6c-6b78-4dc3-b628-3c07cd7af9e5.pdf"},{"id":97668837,"identity":"1eb2a9d0-d6ba-4f56-96b5-3e0b48e1b034","added_by":"auto","created_at":"2025-12-08 09:26:22","extension":"png","order_by":1,"title":"","display":"","copyAsset":false,"role":"supplement","size":110029,"visible":true,"origin":"","legend":"","description":"","filename":"Image.png","url":"https://assets-eu.researchsquare.com/files/rs-7931892/v1/3ddaf2abfd4a7983af487514.png"}],"financialInterests":"No competing interests reported.","formattedTitle":"Synthesis of BiVO 4 nanostructures via Hydrothermal Synthesis: Evaluation of its Electrochemical Lithium ion battery performance","fulltext":[{"header":"1.0. Introduction","content":"\u003cp\u003eThe growing global demand for energy is one of the critical challenges of the twenty-first century, making energy research a highly prioritized field. Although technology has improved, non-renewable energy sources such as coal, oil, and natural gas still dominate energy production, which makes up a significant portion of the world's energy consumption[\u003cspan citationid=\"CR1\" class=\"CitationRef\"\u003e1\u003c/span\u003e]. It is alarming that reports indicate that the world's oil reserves will be depleted in the next 40 years. This scenario calls for urgent development of clean, cost-effective, and environmentally sustainable energy storage and conversion devices. Fuel cells, solar cells, supercapacitors, and lithium-ion batteries (LIBs) are emerging as promising solutions to these challenges [\u003cspan citationid=\"CR2\" class=\"CitationRef\"\u003e2\u003c/span\u003e, \u003cspan citationid=\"CR3\" class=\"CitationRef\"\u003e3\u003c/span\u003e].\u003c/p\u003e\u003cp\u003eAmong them, LIBs are promising energy storage technologies for a variety of applications, including mobile devices, portable electronics, hybrid electric vehicles, backup power systems, and military equipment. They are highly appealing because of their high power density, extended cycle life, and rapid charge-discharge capabilities[\u003cspan citationid=\"CR4\" class=\"CitationRef\"\u003e4\u003c/span\u003e, \u003cspan citationid=\"CR5\" class=\"CitationRef\"\u003e5\u003c/span\u003e]. Traditionally, noble-metal-based electrode materials have been widely used in both aqueous and non-aqueous LIBs due to their affordability, excellent energy performance, and remarkable cycling stability. Some other advanced materials explored for improvement in energy density and cyclic stability include metal oxides, hydroxides, binary transition metal oxides, conducting polymers, and metal chalcogenides. These materials, for instance, include metal oxides, such as V\u003csub\u003e2\u003c/sub\u003eO\u003csub\u003e5\u003c/sub\u003e[\u003cspan citationid=\"CR6\" class=\"CitationRef\"\u003e6\u003c/span\u003e], BiVO\u003csub\u003e4\u003c/sub\u003e, and SiO\u003csub\u003e2\u003c/sub\u003e[\u003cspan citationid=\"CR7\" class=\"CitationRef\"\u003e7\u003c/span\u003e], which are receiving attention in the application of LIB due to their interesting properties, which include affordability, a larger surface area, and good redox activity. Unfortunately, the limiting factors such as low rate capability and cyclic stability limit its practical application. Researchers have increasingly focused on binary semiconducting metal oxides due to their better electrical conductivity, thermal stability, and higher active surface area as compared to single-component oxides that can solve the above issues[\u003cspan citationid=\"CR8\" class=\"CitationRef\"\u003e8\u003c/span\u003e, \u003cspan citationid=\"CR9\" class=\"CitationRef\"\u003e9\u003c/span\u003e].\u003c/p\u003e\u003cp\u003eMulti objective utilization of materials, such as BiVO\u003csub\u003e4\u003c/sub\u003e and V\u003csub\u003e2\u003c/sub\u003eO\u003csub\u003e5\u003c/sub\u003e in terms of desirable attributes, such as a small bandgap, onset potential, high redox behavior, and long-time stability, also finds application for the treatment of wastewater, catalysis[\u003cspan citationid=\"CR10\" class=\"CitationRef\"\u003e10\u003c/span\u003e], and energy storage applications. For example, LIBs-based on V\u003csub\u003e2\u003c/sub\u003eO\u003csub\u003e5\u003c/sub\u003e exhibit improved electrochemical performance arising from its structure with layered lattice and variable oxidation states. Similarly, n-type semiconductor BiVO\u003csub\u003e4\u003c/sub\u003e boasts a low optical bandgap in the range 2.2\u0026ndash;2.5 eV, excellent reduction potential, superb light absorption ability, and a large capacitive capability. Crystalline forms of BiVO\u003csub\u003e4\u003c/sub\u003e include three forms: zircon-structured tetragonal, scheelite-structured tetragonal, and scheelite-structured monoclinic. Among these, the monoclinic crystal structure exhibits outstanding photocatalytic and electrochemical properties because of its unique lattice distortions, particularly between the BiO\u003csub\u003e6\u003c/sub\u003e octahedra and VO\u003csub\u003e4\u003c/sub\u003e tetrahedra, making it an ideal material for energy storage and conversion applications[\u003cspan citationid=\"CR11\" class=\"CitationRef\"\u003e11\u003c/span\u003e].\u003c/p\u003e"},{"header":"2.0. Experimental","content":"\u003cdiv id=\"Sec3\" class=\"Section2\"\u003e\u003ch2\u003e2.1 Chemicals and electrode materials\u003c/h2\u003e\u003cp\u003eThe following chemicals are procured from Merck: bismuth nitrate pentahydrate [Bi(NO\u003csub\u003e3\u003c/sub\u003e)\u003csub\u003e3\u003c/sub\u003e\u0026middot;5H\u003csub\u003e2\u003c/sub\u003eO], ammonium metavanadate (NH\u003csub\u003e4\u003c/sub\u003eVO\u003csub\u003e3\u003c/sub\u003e), nitric acid (HNO\u003csub\u003e3\u003c/sub\u003e) All chemicals are analytical in grade and are used without purification.\u003c/p\u003e\u003c/div\u003e\u003cdiv id=\"Sec4\" class=\"Section2\"\u003e\u003ch2\u003e2.3 Synthesis of BiVO\u003csub\u003e4\u003c/sub\u003e NPs\u003c/h2\u003e\u003cp\u003eBismuth vanadate (BiVO\u003csub\u003e4\u003c/sub\u003e) NPs were synthesized using a hydrothermal method. First, 1 mmol of bismuth nitrate pentahydrate [Bi(NO\u003csub\u003e3\u003c/sub\u003e)\u003csub\u003e3\u003c/sub\u003e\u0026middot;5H\u003csub\u003e2\u003c/sub\u003eO] was dispersed in 35 mL of 0.5 M nitric acid (HNO\u003csub\u003e3\u003c/sub\u003e) solution and stirred for 30 minutes to ensure complete dissolution. In a separate step, 1 mmol of ammonium metavanadate (NH\u003csub\u003e4\u003c/sub\u003eVO\u003csub\u003e3\u003c/sub\u003e) was dissolved in 35 mL of distilled water and stirred under heat for 30 minutes until a clear solution was obtained. The clear solution was then added dropwise to the bismuth nitrate solution while stirring continuously. The resulting mixture, a brick-red suspension, was stirred for another 30 minutes. This suspension was then transferred to a 75 mL autoclave, sealed, and heated to 160\u0026deg;C for 42 hours. After the hydrothermal reaction, the brownish-yellow solid product was collected and washed three times with deionized water and ethanol. Finally, the product was dried at 80\u0026deg;C for 3 hours to obtain the BiVO\u003csub\u003e4\u003c/sub\u003e NPs.\u003c/p\u003e\u003c/div\u003e"},{"header":"3.0. Characterization","content":"\u003cp\u003eThe crystal structure and the size of BiVO\u003csub\u003e4\u003c/sub\u003e NPs were analysed using Rigaku martlab X- Ray diffractometer (XRD) with monochromatized CuKα radiation (1.5418\u0026Aring;) in 2θ range 10\u0026ndash;70. Functional group Bi-Oand V-O bond of BiVO\u003csub\u003e4\u003c/sub\u003e were analysed using FTIR (Bruker Alpha P-spectrophotometer) in the wavenumber range 350 to 4000 cm\u003csup\u003e\u0026minus;\u0026thinsp;1\u003c/sup\u003e. The optical properties of the NPs were evaluated using Agilent technology Cary-60 UV-Vis diffuse reflectance spectrophotometer (UV-Vis DRS) in the range of 200 to 800 nm. Morphological properties, elemental analysis, and size of the nano materials were identified using a scanning electron microscope, energy dispersive X-ray spectrometer (TESCAN Vega 3LMU. Horiba Xplora Plus Raman microscope was used to check Raman measurements. Biologics instrument was employed to study electrochemical properties.\u003c/p\u003e\u003cdiv id=\"Sec6\" class=\"Section2\"\u003e\u003ch2\u003e3.1. Electrochemical Measurements\u003c/h2\u003e\u003cp\u003eElectrochemical studies of BiVO\u003csub\u003e4\u003c/sub\u003e NPs were done for LIB anode applications. The electrochemical properties were studied in coin cell arrangement (CR2032) with lithium metal as both reference and counter electrode. The working electrode consisted of active material, acetylene black and polyvinylidene fluoride (PVDF) in the ratio 80:15:5. The materials were taken in the above ratio in an agate mortar and ground well. Further, a small quantity of N-methylpyrrolidine (NMP) was added to acquire slurry. The slurry was uniformly coated on pre-treated copper foil and subjected to drying at 110⁰C for 12 hours in a vacuum oven. The pretreatment of Cu foil was done by etching the foils in 5 N HNO\u003csub\u003e3\u003c/sub\u003e and then washings them abundantly with DD water, followed by acetone and finally air dried. Argon filled glove box assembled coin cells by dissolving 1 M LiPF\u003csub\u003e6\u003c/sub\u003e in ethylene carbonate, diethyl carbonate and dimethyl carbonate (2:1:2 v/v) as electrolyte and a porous polypropylene membrane as a separator. Charge/discharge tests are carried out on Biologic battery tester at room temperature at diverse current rates and respective voltage ranges [\u003cspan citationid=\"CR12\" class=\"CitationRef\"\u003e12\u003c/span\u003e].\u003c/p\u003e\u003c/div\u003e"},{"header":"4.0. Results and discussion","content":"\u003cdiv id=\"Sec8\" class=\"Section2\"\u003e\u003ch2\u003e4.1. XRD analysis\u003c/h2\u003e\u003cp\u003eX-ray diffraction (XRD) analysis was used to verify the hydrothermally produced BiVO\u003csub\u003e4\u003c/sub\u003e NPs phase purity and crystalline structure, as shown in Fig.\u0026nbsp;\u003cspan refid=\"Fig1\" class=\"InternalRef\"\u003e1\u003c/span\u003e(a). The XRD pattern's diffraction peaks are in good agreement with standard data (JCPDS card number. 14\u0026ndash;0688) and the monoclinic phase of BiVO\u003csub\u003e4\u003c/sub\u003e (space group: I2/a)[\u003cspan citationid=\"CR13\" class=\"CitationRef\"\u003e13\u003c/span\u003e]. It was discovered that the lattice parameters were a\u0026thinsp;=\u0026thinsp;5.195 nm, b\u0026thinsp;=\u0026thinsp;11.701 nm, and c\u0026thinsp;=\u0026thinsp;5.092 nm. The Scherrer equation was used to determine the BiVO\u003csub\u003e4\u003c/sub\u003e NPs average crystallite size:\u003c/p\u003e\u003cp\u003e\u003cb\u003eD\u0026thinsp;=\u0026thinsp;Kλ/βCos θ\u003c/b\u003e\u003c/p\u003e\u003cp\u003eWhere θ is the Bragg angle, β is the full width at half maximum (FWHM) of the diffraction peak, λ is the X-ray wavelength of the Cu Kα source (1.54 \u0026Aring;), and D is the crystallite size. The average crystallite size was calculated to be roughly 67 nm using this method.\u003c/p\u003e\u003c/div\u003e\u003cdiv id=\"Sec9\" class=\"Section2\"\u003e\u003ch2\u003e4.2. FTIR studies\u003c/h2\u003e\u003cp\u003eThe characteristic peaks in the FTIR spectrum of the synthesized BiVO\u003csub\u003e4\u003c/sub\u003e NPs (Fig.\u0026nbsp;\u003cspan refid=\"Fig2\" class=\"InternalRef\"\u003e2\u003c/span\u003e(b)) are in good agreement with those found in the literature. The stretching vibrations of the terminal V\u0026thinsp;=\u0026thinsp;O bonds are identified by a noticeable band at 1025 cm\u003csup\u003e\u0026minus;\u0026thinsp;1\u003c/sup\u003e[14\u003csup\u003e]\u003c/sup\u003e.The antisymmetric stretching of bridging oxygen atoms between two vanadium center (V\u0026ndash;O\u0026ndash;V connections) is linked to the peaks seen at 830 cm\u003csup\u003e\u0026minus;\u0026thinsp;1\u003c/sup\u003e and 720 cm\u003csup\u003e\u0026minus;\u0026thinsp;1\u003c/sup\u003e. Furthermore, the symmetric stretching vibrations of the V\u0026ndash;O\u0026ndash;V units are represented by a band that emerges at 412 cm\u003csup\u003e\u0026minus;\u0026thinsp;1\u003c/sup\u003e. The bending mode of adsorbed water molecules on the surface of the nanoparticle is responsible for a prominent peak at 1614 cm\u003csup\u003e\u0026minus;\u0026thinsp;1\u003c/sup\u003e[\u003cspan citationid=\"CR15\" class=\"CitationRef\"\u003e15\u003c/span\u003e, \u003cspan citationid=\"CR16\" class=\"CitationRef\"\u003e16\u003c/span\u003e].\u003c/p\u003e\u003c/div\u003e\u003cdiv id=\"Sec10\" class=\"Section2\"\u003e\u003ch2\u003e4.3. UV-Vis analysis\u003c/h2\u003e\u003cp\u003eThe BiVO\u003csub\u003e4\u003c/sub\u003e NPs optical characteristics were examined through the technique of UV-Visible Diffuse Reflectance Spectroscopy (UV-DRS). The material's photocatalytic capacity under visible illumination was demonstrated by the recorded spectrum's significant absorption edge in the visible light band. Using the Kubelka\u0026ndash;Munk function on the reflectance data, the optical band gap was calculated and plotted as a Tauc plot, [(F(R)hv)\u003csup\u003e2\u003c/sup\u003e], versus photon energy (hν), assuming a direct allowed transition.\u003c/p\u003e\u003cp\u003eAn optical band gap of roughly 2.2 eV was obtained by extrapolating the linear part of the curve from the Tauc plot to the photon energy axis as shown in Fig.\u0026nbsp;\u003cspan refid=\"Fig1\" class=\"InternalRef\"\u003e1\u003c/span\u003e(c). This value validates the suitability of monoclinic BiVO\u003csub\u003e4\u003c/sub\u003e as a visible-light-responsive photocatalyst and is in good agreement with previously published data[\u003cspan citationid=\"CR17\" class=\"CitationRef\"\u003e17\u003c/span\u003e].\u003c/p\u003e\u003c/div\u003e\u003cdiv id=\"Sec11\" class=\"Section2\"\u003e\u003ch2\u003e4.4. Raman Studies\u003c/h2\u003e\u003cp\u003eThe symmetric stretching vibration mode of the vanadate group (VO\u003csub\u003e4\u003c/sub\u003e\u003csup\u003e3\u0026minus;\u003c/sup\u003e) is characterized by a clear and powerful peak centered about 827 cm\u003csup\u003e\u0026minus;\u0026thinsp;1\u003c/sup\u003e in the Raman spectra of BiVO\u003csub\u003e4\u003c/sub\u003e nanoparticles, as seen in the Fig.\u0026nbsp;\u003cspan refid=\"Fig1\" class=\"InternalRef\"\u003e1\u003c/span\u003e(d). Given that similar vibrational modes are commonly seen in this phase, this strong and sharp peak validates the creation of the monoclinic scheelite structure of BiVO\u003csub\u003e4\u003c/sub\u003e. Furthermore, the bending and asymmetric stretching modes of the VO\u003csub\u003e4\u003c/sub\u003e units are responsible for the smaller peaks seen in the lower wavenumber region. The produced BiVO\u003csub\u003e4\u003c/sub\u003e NPs phase purity and structural stability are further demonstrated by the lack of notable extra peaks or shifts. All things considered, the Raman study confirms that monoclinic BiVO\u003csub\u003e4\u003c/sub\u003e with distinct vibrational properties was successfully formed [\u003cspan citationid=\"CR18\" class=\"CitationRef\"\u003e18\u003c/span\u003e].\u003c/p\u003e\u003cp\u003e\u003c/p\u003e\u003c/div\u003e\u003cdiv id=\"Sec12\" class=\"Section2\"\u003e\u003ch2\u003e4.5. SEM Analysis\u003c/h2\u003e\u003cp\u003eSurface morphology and elemental analysis of the produced BiVO\u003csub\u003e4\u003c/sub\u003e NPs were carried out by scanning electron microscopy (SEM) and energy-dispersive X-ray spectroscopy (EDS), respectively, as presented in Fig.\u0026nbsp;\u003cspan refid=\"Fig2\" class=\"InternalRef\"\u003e2\u003c/span\u003e.The low-magnification SEM image (Figure. 2(a)) indicates that the BiVO\u003csub\u003e4\u003c/sub\u003e particles exhibit a spherical hierarchical structure, that are spherical aggregates with an average size in the micrometer range. At increased magnification (Fig.\u0026nbsp;\u003cspan refid=\"Fig2\" class=\"InternalRef\"\u003e2\u003c/span\u003e(b-c)), the morphology is resolved into ultrathin nanosheets emanating from a central core, indicating anisotropic growth and self-assembled architecture. Such a porous and layered morphology is beneficial in baterry applications. The EDS spectrum (Fig.\u0026nbsp;\u003cspan refid=\"Fig2\" class=\"InternalRef\"\u003e2\u003c/span\u003e(d)) identifies the presence of bismuth (Bi), vanadium (V), and oxygen (O), with typical peaks including Bi-M, Bi-L, V-K, and O-K, which confirm the successful formation of stoichiometric and phase-pure BiVO\u003csub\u003e4\u003c/sub\u003e free of detectable impurities [\u003cspan citationid=\"CR19\" class=\"CitationRef\"\u003e19\u003c/span\u003e].\u003c/p\u003e\u003cp\u003e\u003c/p\u003e\u003c/div\u003e\u003cdiv id=\"Sec13\" class=\"Section2\"\u003e\u003ch2\u003e4.6. TEM Studies\u003c/h2\u003e\u003cp\u003e\u003c/p\u003e\u003cp\u003eTEM and HRTEM images verify the nanoscale morphology and crystallinity of the resultant BiVO\u003csub\u003e4\u003c/sub\u003e NPs. Figure.4(a) exhibits aggregated, semi-spherical particles with dimensions of 20\u0026ndash;80 nm. Figure.4(b) depicts more distinct particles with smoother surfaces, with an average size of 15\u0026ndash;30 nm.Figure.4(c) is a closer image, with clear particle boundaries and verifying their nanocrystalline character. The HRTEM Figure.4(d) exhibits distinct lattice fringes, reflecting high crystallinity.The interplanar spacing observed is corresponding to the (001) plane, as depicted in the inset.This indicates a well-defined structure of scheelite-type for BiVO\u003csub\u003e4\u003c/sub\u003e. These characteristics render BiVO\u003csub\u003e4\u003c/sub\u003e appropriate for energy applications.\u003c/p\u003e\u003c/div\u003e\u003cdiv id=\"Sec14\" class=\"Section2\"\u003e\u003ch2\u003e4.6. Photoluminescence Studies\u003c/h2\u003e\u003cp\u003eIn electronic components, PL spectroscopy is frequently used to ascertain details such as the presence of surface defects, oxygen vacancies, and the effectiveness of charge-carrier trapping and transfer. This is explained by the fact that the recombination of photoexcited charges is the cause of the PL emission of BiVO\u003csub\u003e4\u003c/sub\u003e[\u003cspan citationid=\"CR20\" class=\"CitationRef\"\u003e20\u003c/span\u003e]. The recombination of the hole formed from the hybrid orbitals of Bi 6s and O 2p and the electron generated from the V 3d orbitals are responsible for the strong emission centred at 546 nm and the excitation at 340 nm, respectively, observed in the PL spectrum of BiVO\u003csub\u003e4\u003c/sub\u003e nanoparticles [\u003cspan citationid=\"CR21\" class=\"CitationRef\"\u003e21\u003c/span\u003e] (Fig.\u0026nbsp;4a-b).\u003c/p\u003e\u003cp\u003e\u003c/p\u003e\u003c/div\u003e"},{"header":"5.0. Electrochemical properties of BiVO nanoparticles","content":"\u003cp\u003e\u003c/p\u003e\u003cp\u003eThe electrochemical properties of the enhanced BiVO\u003csub\u003e4\u003c/sub\u003e electrode were thoroughly examined via galvanostatic charge\u0026ndash;discharge (GCD) experiments, prolonged cycling, and Coulombic efficiency testing, as illustrated in Fig.\u0026nbsp;4. As apparent from Fig.\u0026nbsp;\u003cspan refid=\"Fig4\" class=\"InternalRef\"\u003e5\u003c/span\u003e(a), the BiVO\u003csub\u003e4\u003c/sub\u003e electrode attained an initial discharge capacity of 198 mAh g\u003csup\u003e\u0026minus;\u0026thinsp;1\u003c/sup\u003e with a current density of C/10 (0.1C) in the voltage range 1.0\u0026ndash;2.5 V. The high initial capacity is because of the lithium intercalation/deintercalation reaction achieved by the porous nature and large surface area of the BiVO\u003csub\u003e4\u003c/sub\u003e nanomaterial. Yet, upon repeated cycling, the capacity decreased progressively, to 104 mAh g\u003csup\u003e\u0026minus;\u0026thinsp;1\u003c/sup\u003e after 54 cycles, showing a 48% capacity fade. This loss could be caused by active material degradation, structural instability, or SEI formation with time[\u003cspan citationid=\"CR22\" class=\"CitationRef\"\u003e22\u003c/span\u003e, \u003cspan citationid=\"CR23\" class=\"CitationRef\"\u003e23\u003c/span\u003e].\u003c/p\u003e\u003cp\u003eFigure \u003cspan refid=\"Fig4\" class=\"InternalRef\"\u003e5\u003c/span\u003e(b) shows the stable long-term cycling performance at increased current density of 50 mA g\u003csup\u003e\u0026minus;\u0026thinsp;1\u003c/sup\u003e, for which the BiVO\u003csub\u003e4\u003c/sub\u003e electrode still exhibits a fixed capacity of about 100 mAh g\u003csup\u003e\u0026minus;\u0026thinsp;1\u003c/sup\u003e even after 500 cycles, illustrating great cycling stability and rate ability. Such reliable long-term stability suggests great high-rate application prospect of BiVO\u003csub\u003e4\u003c/sub\u003e electrode material. In the Fig.\u0026nbsp;\u003cspan refid=\"Fig4\" class=\"InternalRef\"\u003e5\u003c/span\u003e(c) indicates the capacity and Coulombic efficiency trends after 54 cycles. While the discharge capacity continuously drops, the Coulombic efficiency is always high at about 98%, reflecting superior charge/discharge reversibility and small side reactions. This high efficiency implies that the electrode maintains structural integrity and stable electrochemical kinetics throughout cycling. In total, the findings confirm that the well-separated BiVO\u003csub\u003e4\u003c/sub\u003e electrode exhibits good electrochemical and structural stability, which is a promising anode material for high-rate lithium-ion battery applications. The high initial capacity, great Coulombic efficiency, and long-term cycling stability at various current densities confirm its appropriateness for energy storage technology[\u003cspan citationid=\"CR24\" class=\"CitationRef\"\u003e24\u003c/span\u003e, \u003cspan citationid=\"CR25\" class=\"CitationRef\"\u003e25\u003c/span\u003e].\u003c/p\u003e\u003cp\u003eThe cyclic voltammetry curve of BiVO\u003csub\u003e4\u003c/sub\u003e as a lithium-ion battery anode material was obtained in the potential window of 0.01\u0026ndash;3.0 V at 0.5 mV/s scan rate in the Fig.\u0026nbsp;\u003cspan refid=\"Fig4\" class=\"InternalRef\"\u003e5\u003c/span\u003ed. The CV profile shows well-defined redox peaks, validating the reversible lithiation and delithiation characteristics of BiVO\u003csub\u003e4\u003c/sub\u003e. During the first cathodic scan, a prominent reduction peak at 0.5 V is due to the conversion reaction of BiVO\u003csub\u003e4\u003c/sub\u003e with lithium ions to produce metallic Bi and Li\u003csub\u003e2\u003c/sub\u003eO, followed by dealloying of Bi with Li to produce Li\u003csub\u003ex\u003c/sub\u003eBi phases. The anodic peaks corresponding to these near 1.5-2.0 V are due to the dealloying of Li\u003csub\u003ex\u003c/sub\u003eBi and the partial re-formation of BiVO\u003csub\u003e4\u003c/sub\u003e, reflecting good electrochemical reversibility. The stable and almost overlapped curves in following cycles indicate superior cyclic stability and good electrode kinetics, which means that BiVO\u003csub\u003e4\u003c/sub\u003e retains structural integrity throughout repeated lithiation/delithiation cycles. In summary, the CV response validates the efficient redox activity and reversible Li\u003csup\u003e+\u003c/sup\u003e storage ability of BiVO\u003csub\u003e4\u003c/sub\u003e as a great anode material for lithium-ion batteries.\u003c/p\u003e\u003cdiv id=\"Sec16\" class=\"Section2\"\u003e\u003ch2\u003e5.1. Impedance Spectra\u003c/h2\u003e\u003cp\u003e\u003c/p\u003e\u003cp\u003eThe impedance plots of BiVO\u003csub\u003e4\u003c/sub\u003e NPs, as evident from the Nyquist plot (Fig.\u0026nbsp;\u003cspan refid=\"Fig5\" class=\"InternalRef\"\u003e6\u003c/span\u003e), are rich in information regarding their electrical conductivity and charge transfer mechanism. The plot consists of a high-frequency semicircular arc followed by a low-frequency linear tail. Appearance of the semicircle signifies the charge transfer resistance (R\u003csub\u003ect\u003c/sub\u003e) at the electrode\u0026ndash;electrolyte interface, which is equivalent to the bulk resistance and interfacial phenomena of the material. The steep straight line at low frequencies indicates the Warburg impedance, which is generally related to ion diffusion inside the electrode material. The comparably small semicircle diameter suggests low charge transfer resistance, implying that the BiVO\u003csub\u003e4\u003c/sub\u003e nanoparticles are electrically conductive and support rapid charge transport. Such activity is favorable for electrochemical device applications, such as photocatalysis and energy storage, where rapid electron mobility and minimized recombination losses are essential.\u003c/p\u003e\u003c/div\u003e"},{"header":"6.0. Conclusion","content":"\u003cp\u003eIn summary, BiVO\u003csub\u003e4\u003c/sub\u003e NPs were effectively synthesized and methodically analyzed for their structural, optical, vibrational, and electrochemical characteristics. The monoclinic nature of the phase with a crystallite size of 67 nm was ensured through XRD analysis. The existence of distinctive vibrational modes relating to Bi\u0026ndash;O and V\u0026ndash;O bonds was ensured by FTIR and Raman spectroscopy, which confirmed the structural integrity of the material obtained. UV-Vis DRS was used to calculate the optical band gap of about 2.2 eV, and it was deemed appropriate for use in visible-light-driven applications. Electrochemical characterization showed that the optimized BiVO\u003csub\u003e4\u003c/sub\u003e electrode had a maximum initial discharge capacity of 198 mAh g\u003csup\u003e\u0026minus;\u0026thinsp;1\u003c/sup\u003e at C/10, with 104 mAh g\u003csup\u003e\u0026minus;\u0026thinsp;1\u003c/sup\u003e being retained after 54 cycles at a Coulombic efficiency of around 98%. Even at a high current density of 50 mA g⁻\u0026sup1;, the electrode retained 100 mAh g\u003csup\u003e\u0026minus;\u0026thinsp;1\u003c/sup\u003e capacity after 500 cycles, exhibiting good rate capability and cycling stability. These results indicate that BiVO\u003csub\u003e4\u003c/sub\u003e is a good candidate anode material for high-performance lithium-ion batteries due to its stable structure, efficient redox behavior, and long-term durability.\u003c/p\u003e"},{"header":"Declarations","content":"\u003cp\u003e\u003ch2\u003eDeclaration of Competing Interest\u003c/h2\u003e\u003cp\u003eThe authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper.\u003c/p\u003e\u003c/p\u003e\u003cp\u003e\u003ch2\u003eCredit Authorship\u003c/h2\u003e\u003cp\u003eR: Writing \u0026ndash; original draft, Method ology, Formal analysis, Data curation. K R: Writing \u0026ndash; review \u0026amp; editing, Conceptualization. T D: Data curation. J: Resources, Data curation. G : Supervision, writing and reviewing.\u003c/p\u003e\u003c/p\u003e\u003ch2\u003eAuthor Contribution\u003c/h2\u003e\u003cp\u003eR: Writing \u0026ndash; original draft, Method ology, Formal analysis, Data curation. K R: Writing \u0026ndash; review \u0026amp; editing, Conceptualization. T D: Data curation. J: Resources, Data curation. G : Supervision, writing and reviewing.\u003c/p\u003e\u003ch2\u003eAcknowledgement\u003c/h2\u003e\u003cp\u003ePooja K. R. gratefully acknowledges the Department of Science and Technology KSTePS Fellowship (Award No: CHE-02/2024-25) for the financial support. One of the author G. Nagaraju acknowledges VGST-K-FIST 9GRD 950/2020\u0026ndash;2021), Govt. of Karnataka for financial support.\u003c/p\u003e\u003ch2\u003eData availability\u003c/h2\u003e\u003cp\u003eData will be made available on request.\u003c/p\u003e"},{"header":"References","content":"\u003col\u003e\n\u003cli\u003eC. 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Zhang, Innovative BVO@ CuO design: A high-performance vanadium-based anode material for Li-ion batteries, Journal of Alloys and Compounds 958 (2023) 170485.\u003c/li\u003e\n\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":"BiVO4 NPs, Anode, Li ion battery, Photoluminescence","lastPublishedDoi":"10.21203/rs.3.rs-7931892/v1","lastPublishedDoiUrl":"https://doi.org/10.21203/rs.3.rs-7931892/v1","license":{"name":"CC BY 4.0","url":"https://creativecommons.org/licenses/by/4.0/"},"manuscriptAbstract":"\u003cp\u003eIn this work, bismuth vanadate (BiVO\u003csub\u003e4\u003c/sub\u003e) NPs were prepared by a low temperature hydrothermal route and were well characterized to assess their electrochemical performances as an anode material for lithium-ion battery (LIB). X-ray diffraction (XRD) established the development of single monoclinic phase with a mean crystallite size of 67 nm. Fourier-transform infrared (FTIR) and Raman spectroscopy studies confirmed the occurrence of Bi-O and V-O vibrational modes, confirming the structural composition of the material synthesized. UV-Vis diffuse reflectance spectroscopy (DRS) confirmed an optical band gap of around 2.2 eV. Electrochemical performance investigations indicated that the BiVO\u003csub\u003e4\u003c/sub\u003e electrode provided an initial discharge capacity of 198 mAh g\u003csup\u003e\u0026minus;\u0026thinsp;1\u003c/sup\u003e at 0.1C (C/10), which decreased gradually to 104 mAh g\u003csup\u003e\u0026minus;\u0026thinsp;1\u003c/sup\u003e at 54 cycles while retaining a Coulombic efficiency of about 98%. In addition, at a current density of 50 mA g\u003csup\u003e\u0026minus;\u0026thinsp;1\u003c/sup\u003e, the electrode retained a stable capacity of 100 mAh g\u003csup\u003e\u0026minus;\u0026thinsp;1\u003c/sup\u003eeven at 500 cycles. The synergized structural stability, high lithium storage capacity, and superior cycling life highlight the promise of BiVO\u003csub\u003e4\u003c/sub\u003e as a good anode material for future lithium-ion batteries.\u003c/p\u003e","manuscriptTitle":"Synthesis of BiVO 4 nanostructures via Hydrothermal Synthesis: Evaluation of its Electrochemical Lithium ion battery performance","msid":"","msnumber":"","nonDraftVersions":[{"code":1,"date":"2025-12-04 17:16:07","doi":"10.21203/rs.3.rs-7931892/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":"8105c8c0-5a3b-4e14-b75a-fc036d429c07","owner":[],"postedDate":"December 4th, 2025","published":true,"recentEditorialEvents":[],"rejectedJournal":[],"revision":"","amendment":"","status":"posted","subjectAreas":[],"tags":[],"updatedAt":"2026-01-11T15:23:56+00:00","versionOfRecord":[],"versionCreatedAt":"2025-12-04 17:16:07","video":"","vorDoi":"","vorDoiUrl":"","workflowStages":[]},"version":"v1","identity":"rs-7931892","journalConfig":"researchsquare"},"__N_SSP":true},"page":"/article/[identity]/[[...version]]","query":{"redirect":"/article/rs-7931892","identity":"rs-7931892","version":["v1"]},"buildId":"8U1c8b4HqxoKbykW_rLl7","isFallback":false,"isExperimentalCompile":false,"dynamicIds":[84888],"gssp":true,"scriptLoader":[]}