Hydrothermal Synthesis Research Articles

Poly-m-aminophenol/CoFe2O4 (p-n) heterojunction: Sustainable decontamination of BPA, ciprofloxacin pollutants from water and its study of antimicrobial performance

The remarkable ability of magnetic p-n heterojunction catalyst constructed with p-type poly-m-aminophenol (PmAP)/n-type Cobalt ferrite (CoFe2O4) catalyst to degrade BPA, ciprofloxacin drug (CIF) and its antibacterial activity in killing the microbes was explored on Gram-positive (S. aureus) and Gram-negative (E. coli). The p-n heterojunction photocatalyst was synthesized easily via hydrothermal reaction followed by chemical oxidative polymerization process. PXRD, FTIR, SEM, HRTEM, XPS, EDX, PL/TRPL, BET surface area, VSM and Uv-DRS techniques were used to confirm the synthesized catalyst's physicochemical characteristics and structural details. At ambient conditions, the synthesized catalyst showed rapid mineralisation of the organic pollutants by nearly 100 % at a concentration of 50 ppm in just one hour, with a catalyst loading of 0.1 g. The mineralisation pathways of the organics were illustrated through the GC–MS and TOC analysis. Furthermore, the disinfection capacity of the heterojunction had showed 5 fold quicker than the individual catalysts. This p-n heterojunction catalyst show excellent activity and quick magnetic separable quality which make it a catalyst for sustainable water purification process in future.

Directed Hydrothermal Synthesis of Aluminosilicates of Various Structural Types and Prospects for Their Use in Medicine

Directed Hydrothermal Synthesis of Aluminosilicates of Various Structural Types and Prospects for Their Use in Medicine

A broad-spectrum oxidation capability Ru-CeO2 catalyst for efficient synergistic selective oxidation of benzyl alcohol

Selective oxidation of alcohols to aldehydes by molecular oxygen is one of the most important transformations in multiphase catalysis. In this paper, a catalyst with selective oxidation ability was designed and synthesized for the selective catalytic oxidation of benzyl alcohol. N-doped carbon materials were prepared by high-temperature calcination using hydrothermal reaction products of citric acid and melamine as a carbon source, and a bimetallic catalyst supported by Ru-CeO2 was constructed using the mixture as the carrier for the selective oxidation of benzyl alcohol to benzaldehyde. The results showed that the introduction of CeO2 could effectively improve the oxidizing ability and catalytic activity of the catalyst. The Ru-Ce0.05/NC170–600 catalyst was able to convert 85.5 % benzyl alcohol into benzaldehyde at 140 °C, 6 h, and 2 MPa, and the selectivity for benzaldehyde was 100 %. It was demonstrated by DFT that it was theoretically feasible to generate benzaldehyde by extracting hydrogen atoms from benzyl alcohol molecules. Further, the selective oxidation experiments on other alcohols showed that the catalyst has high activity for the oxidation of various alcohols to generate the corresponding carbonyl products, and it is a catalyst with broad-spectrum selective oxidation ability. In this study, a green synthesis route of benzaldehyde was proposed to solve the problems in the traditional process. Meanwhile, it provides a new idea for the synthesis of carbonyl products by selective oxidation of alcohols.

A Layered Titanate Nanowire Helps Pt/TiO2 Photocatalyst for Solar Hydrogen Evolution from Water with High Quantum Efficiency

Abstract Research into TiO2 photocatalysts for solar H2 evolution from water is still growing for environmentally benign and economically valid H2 production. Herein, in contrast to many researches on the modification of TiO2 toward higher photocatalytic activities, we develop a photocatalytically inactive TiO2-based nanostructure and use it, like graphene, as a booster of a benchmark TiO2. A layered potassium titanate with two-dimensional plate-like particle morphology was converted to the corresponding one-dimensional nanowire form via a hydrothermal reaction, after which the layered potassium titanate nanowire was acid-treated to obtain a layered titanate nanowire. This nanowire was completely inactive toward H2 evolution from water containing methanol under solar simulator irradiation. However, when Pt nanoparticle-loaded P25 TiO2 (Pt/P25) was mixed with a considerably smaller amount of the layered titanate nanowire in water, a durable composite was obtained and the composite showed a good photocatalytic activity three times higher than Pt/P25. The apparent quantum efficiency of the reaction at wavelength of 350 nm was 56%, which was higher than or comparable to those of the state-of-the-art TiO2-based photocatalysts. The possible reason for the enhanced photocatalytic activity of the Pt/P25 and layered titanate nanowire composite involved the transfer of photogenerated holes from Pt/P25 to the nanowire to suppress charge recombination and/or disaggregation (improved dispersion) of Pt/P25 particles on the nanowire.

X-ray diffraction profile analysis of green synthesized ZnO and TiO2 nanoparticles

Abstract ZnO and TiO2 nanoparticles were prepared through a plant-extract mediated hydrothermal synthesis. X-ray diffraction (XRD) study confirmed the crystalline nature and the phase characteristic of the obtained nanoparticles. X-ray diffraction profile analysis models such as Williamson-Hall analysis, size-strain plot and Rietveld analysis were further used in evaluating the microstructural parameters of the obtained materials. The calculated particle size for all the models was in great agreement, with values in the range of 55.46-87.6 nm recorded for ZnO, while for TiO2, the crystallite size was in the range of 33.82-41.9 nm. The calculated crystal microstrain varied based on the model, while the stress in the ZnO and TiO2 nanoparticles was evaluated at 3.8 and 13.7 MPa, respectively. Furthermore, TiO2 nanoparticles had a higher energy density of 8.96 × 10-8 KJ/m3 compared to 7.12 × 10-8 KJ/m3 obtained for ZnO.

V-Based MXene/MAX Heterostructure Composites with Enhancing Dielectric Loss for Broadband Microwave Absorption.

Electromagnetic wave absorption performance is strictly dependent on attenuation and impedance matching, which are directly influenced by the ratio of MXene/MAX in the multilayer structured MXene/MAX composites. However, there is still a challenge to achieve collaborative optimization of dielectric loss and impedance matching by precisely regulating the proportional relationship of MXene/MAX. Herein, V-based MXene/MAX heterostructure composites with different V2C/V2AlC ratios were successfully synthesized by rationally controlling the temperature and time of the hydrothermal reaction. Experimental results indicated that V2C-100 °C-1 harvested the balance between reduced impedance matching and enhanced dielectric losses, which was attributed to the mildly enhanced conduction loss and polarization loss. The first principles indicated that abundant electrons migrate from the V atoms of the MXene to the C atoms of the MAX phase. The charge redistributed and accumulated at the interface, exciting the increase in the dielectric loss of V2C-100 °C-1. As a result, the V2C-100 °C-1 heterostructure composite had an excellent electromagnetic absorption effect with a minimum reflection loss of -50.06 dB and a wide effective absorption bandwidth of 4.0 GHz (12.72-16.72 GHz). This work provides a valuable experience for the development of efficient MXene-based microwave absorbing materials.

Kinetic Study and Catalytic Activity of Cr3+ Catalyst Supported on Calcium Silicate Hydrates for VOC Oxidation

Volatile organic compounds (VOCs) are pollutants that pose significant health and environmental risks, necessitating effective mitigation strategies. Catalytic oxidation emerges as a viable method for converting VOCs into non-toxic end products. This study focuses on synthesizing a catalyst based on calcium silicate hydrates with chromium ions in the CaO-SiO2-Cr(NO3)3-H2O system under hydrothermal conditions and evaluating its thermal stability and catalytic performance. A catalyst with varying concentrations of chromium ions (10, 25, 50, 100 mg/g Cr3+) was synthesized in unstirred suspensions under saturated steam pressure at a temperature of 220 °C. Isothermal curing durations were 8 h, 16 h, and 48 h. Results of X-ray diffraction and atomic absorption spectroscopy showed that hydrothermal synthesis is effective for incorporating up to 100 mg/g Cr3+ into calcium silicate hydrates. The catalyst with Cr3+ ions (50 mg/g) remained stable up to 550 °C, beyond which chromatite was formed. Catalytic oxidation experiments with propanol and propyl acetate revealed that the Cr3+ catalyst supported on calcium silicate hydrates enhances oxygen exchange during the heterogeneous oxidation process. Kinetic calculations indicated that the synthesized catalyst is active, with an activation energy lower than 65 kJ/mol. This study highlights the potential of Cr3+-intercalated calcium silicate hydrates as efficient catalysts for VOC oxidation.

Hydrothermal synthesis of carbon dots incorporated in magnetite iron oxide nanoparticles for potential targeted brain cancer therapy: In-Vitro study

Surface modification of magnetite (Fe3O4) nanoparticles (NPs) using carbon dots (CDs) is a promising approach in biomedical applications due to excellent biocompatibility. Herein, the CDs were incorporated in the Fe3O4 NPs to observe the performance of CDs-Fe3O4 NPs for targeted brain cancer therapy. Scanning electron microscopy (SEM) images revealed the morphology of Fe3O4 NPs is rough and agglomerated. X-ray diffraction (XRD) diffraction pattern exhibits that the CDs are successfully incorporated in Fe3O4 NPs. Furthermore, magnetic properties evaluated using vibrating sample magnetometer (VSM) exhibited significant magnetization (51.362 emu/g) attributed to the greater occupancy of Fe+2 ions in the crystal lattice. XRD pattern confirmed the formation of NPs. Furthermore, functional groups of the NPs were validated through Fourier-transform infrared spectroscopy (FT-IR). The measurement of zeta potential affirmed the stability of the as-prepared Fe3O4 NPs, CDs, and CDs-Fe3O4 NPs, indicating a value of −7.64 mV, −0.5754 mV and −3.881 mV, respectively. Fe3O4 NPs exhibited a surface area of 58.6 m2/g as determined by Brunauer-Emmett-Teller (BET) analysis. The anticancer activity of the synthesized CDs-Fe3O4 NPs demonstrated inhibition against MG-U87 cells. Therefore, the synthesized CDs-Fe3O4 NPs hold potential for application in brain cancer therapy. In addition, CDs-Fe3O4 NPs exhibited exceptional biocompatibility and low cytotoxicity against osteoblast cells, establishing them as a safe biomaterial for biomedical applications.

A Multi‐Active Site Subnano Heterostructures Catalyst Grown In situ POM and Fe0.2Ni0.8Co2O4 onto Nickel Foam Toward Efficient Electrocatalytic Overall Water Splitting

AbstractDesigning efficient, durable, and cheap bifunctional electrocatalysts is a challenging goal in water splitting. Herein, trivanadium‐substituted Keggin‐type polyoxometalate H6PV3Mo9O40 (POM) and Fe0.2Ni0.8Co2O4 (FNCO) are in situ grown onto nickel foam (NF) yielding a self‐supporting nanoflower‐like heterojunction via convenient hydrothermal reaction. The POM‐Fe0.2Ni0.8Co2O4/NF as HER and OER electrocatalyst, displays low overpotential (89 and 259 mV) and high electrode stability at 10 mA cm−2. POM‐FNCO/NF as the cathode and anode requires a lower voltage (1.58 V) to provide 10 mA cm−2 for overall water splitting (OWS), which is better than that of commercial catalysts. The electronic sponge characteristics of POM provide more active sites and fast reaction kinetics for HER and OER. The synergy of POM and FNCO optimizes the electron distribution at the interface and enhances the intrinsic activity of HER/OER. Density Functional Theory (DFT) calculations show that water molecules preferentially bind to Co sites on POM‐FNCO. Additionally, POM has proton‐coupled electron transfer properties and its modified FNCO exhibits thermodynamic advantages. The synergistic effect of these two factors enables the efficient overall water splitting of POM‐FNCO. This study offers a novel pathway for the construction of self‐supporting efficient catalysts by in situ growth of POM nanoclusters and spinel oxide sub‐nanometer heterojunctions on NF.

Study on the synergistic hydrogen production performance and mechanism of NiO/WO3-biochar composite material in the photocatalytic 5-hydroxymethylfurfural conversion to 2,5-furandicarboxylic acid

In this work, a simple hydrothermal synthesis method is used to prepare photocatalytic NiO/WO3-biochar composite material, which is applied to catalyze the one-step conversion of 5-hydroxymethylfurfural to 2,5-furandicarboxylic acid with synergistic hydrogen production. The optoelectronic properties of NiO/WO3-biochar composite material are characterized. The results indicate that the p-n heterojunction-coupled biochar structure between NiO and WO3 in the NiO/WO3-biochar composite is an important prerequisite for ensuring the one-step oxidation reaction of 5-hydroxymethylfurfural. The experimental results reveal the possible reaction pathways. Under the optimal ratio of NiO/WO3-biochar composite material, the 5-hydroxymethylfurfural conversion rate reaches 100%, the 2,5-furandicarboxylic acid yield reaches 99.6%, and the Faraday efficiency of hydrogen evolution is 98%. This study provides a new approach for the one-step photocatalytic synthesis of 2,5-furandicarboxylic acid from 5-hydroxymethylfurfural, as well as a novel and efficient catalyst for photocatalytic oxidation technology.

Phase-controlled synthesis of starch-derived Mo2C–MoC/C heterostructure catalyst for electrocatalytic hydrogen evolution reaction

The electronic structure of molybdenum carbide closely resembles that of Pt, making it a promising candidate material for replacing noble metal catalysts. However, the primary challenge is the controlled and eco-friendly synthesis of molybdenum carbide. Herein, we developed a sustainable and controlled method for synthesizing a heterostructure catalyst for the electrocatalytic hydrogen evolution reaction (HER) using starch as the raw material. Through a hydrothermal redox reaction and subsequent temperature-programmed treatment under an inert atmosphere, the hexagonal Mo2C-cubic MoC heterostructure nanoparticles were dispersed on a carbon matrix. Our investigation into the synthesis process extensively covered the growth of MoO2 nanocrystals and hydrochar during the hydrothermal redox reaction, as well as the phase evolution during the subsequent temperature-programmed treatment. Electrochemical assessments demonstrated the catalyst's remarkable efficiency for the hydrogen evolution reaction across both acidic and alkaline media, achieving a current density of 10 mA/cm2 with an overpotential of 139.4 mV in 1 M KOH solution and 160.7 mV in 0.5 M H2SO4 solution. Combining a series of electrochemical characterizations and applying the distribution of relaxation times (DRT) analysis to operando electrochemical impedance spectroscopy (EIS) data, the superior kinetic performance of the Mo2C–MoC/C was demonstrated, outperforming that of single-phase molybdenum carbide. Furthermore, the catalyst has demonstrated remarkable stability even at high current densities in both acidic and alkaline electrolytes, underscoring its potential as a cathode catalyst in both alkaline water electrolyzers and proton exchange membrane (PEM) electrolyzers.

Tailoring the crystalline and amorphous phase ratios of TiO2 through the use of organic additives during hydrothermal synthesis

The photocatalytic properties of TiO2 are primarily determined by its crystallinity and crystalline phase ratios. To improve the photocatalytic properties of TiO2, greater control over the formation of crystalline and amorphous phases during synthesis is therefore required. In this study, we demonstrate how the addition of minute amounts of three organic compounds (isopropanol, acetone and acetic acid) during hydrothermal treatment affects the amorphous and crystalline phase ratios: the addition of isopropanol or acetone accelerates the phase transition from anatase and brookite to rutile, whereas the addition of acetic acid inhibits the transformation of anatase to rutile, increasing the content of amorphous phase compared to samples where no organic compound was added. We show that the combination of the organic compound added, along with the duration of the hydrothermal treatment, can be used to tailor the phase composition of TiO2, so as to obtain either: i) TiO2 with a high content of both rutile and amorphous phase, ii) TiO2 with a high rutile content and iii) TiO2 with different ratios of all four phases, when the duration of synthesis is short (2–4 h). The materials synthesized exhibited high photocatalytic activity (in most cases higher than P25), which is attributed to the beneficial phase composition and high specific surface area.

Synthesis of Up-Conversion CaTiO3: Er3+ Films on Titanium by Anodization and Hydrothermal Method for Biomedical Applications

The present study investigates the effects of Er3+ doping content on the microstructure and up-conversion emission properties of CaTiO3: Er3+ phosphors as a potential material in biomedical applications. The CaTiO3: x%Er3+ (x = 0.5, 1.0, 1.5, 2.0, 2.5, and 3.0%) films were synthesized on Ti substrates by a hydrothermal reaction at 200 °C for 24 h. The SEM image showed the formation of cubic nanorod CaTiO3: Er3+ films with a mean edge size value of (1–5) μm. When excited with 980 nm light, the CaTiO3: Er3+ films emitted a strong green band and a weak red band of Er3+ ions located at 543, 661, and 740 nm. The CaTiO3: Er3+ film exhibited excellent surface hydrophilicity with a contact angle of ~zero and good biocompatibility against baby hamster kidney (BHK) cells. CaTiO3: Er3+ films emerge as promising materials for different applications in the biomedical field.

Efficiency and mechanism of modified carbon nitride for the co-adsorption of copper and tetracycline from water

The escalating contamination of heavy metal ions and antibiotics in the aqueous environment underscores the necessity of developing efficient treatment technologies for their concurrent removal. In this work, a phosphate-modified g-C3N4(PCN) by assembling phytic acid with graphitized carbon nitride was prepared through a hydrothermal reaction. The characterization results reveal that PCN exhibits increased porosity, an enhanced specific surface area, and larger pore volume in comparison to pristine CN. At pH 5.0 and 25 °C, PCN demonstrates remarkable adsorption capacities for Cu (II) (q = 172.3 mg g−1) and tetracycline (TC) (q = 63.1 mg g−1) in a single system, respectively, which correspondingly surpasses those of CN by 7 and 8 times. In systems where Cu (II) and TC coexist, Cu (II) enhances the TC removal rate by acting as a bridge. As Cu(II) concentration increases, TC adsorption efficiency significantly improves. Although common ions in solution influence PCN adsorption, it maintains high efficiency for TC and Cu(II) across various water matrices and in the presence of natural organic matter. Detailed characterization and computational chemical analysis reveal that the enhanced adsorption capacity of PCN is due to increased porosity and the presence of additional functional groups. Surface complexation and adsorption bridging are identified as the key mechanisms for effective Cu(II) and TC adsorption. Additionally, recycling experiments validate its reusability, thereby offering a novel avenue for the removal and recovery of TC and Cu(II) from wastewater.

Synthesis of Up-Conversion CaTiO3: Er3+ Films on Titanium by Anodization and Hydrothermal Method for Biomedical Applications.

The present study investigates the effects of Er3+ doping content on the microstructure and up-conversion emission properties of CaTiO3: Er3+ phosphors as a potential material in biomedical applications. The CaTiO3: x%Er3+ (x = 0.5, 1.0, 1.5, 2.0, 2.5, and 3.0%) films were synthesized on Ti substrates by a hydrothermal reaction at 200 °C for 24 h. The SEM image showed the formation of cubic nanorod CaTiO3: Er3+ films with a mean edge size value of (1-5) μm. When excited with 980 nm light, the CaTiO3: Er3+ films emitted a strong green band and a weak red band of Er3+ ions located at 543, 661, and 740 nm. The CaTiO3: Er3+ film exhibited excellent surface hydrophilicity with a contact angle of ~zero and good biocompatibility against baby hamster kidney (BHK) cells. CaTiO3: Er3+ films emerge as promising materials for different applications in the biomedical field.

Supercritical hydrothermal synthesis of ultra-fine Cu powders

ABSTRACT Ultra-fine Cu powders were synthesized using supercritical water as a reaction medium and formic acid as a reducing agent. The effects of reducing agent, reaction temperature, and complexing agent on the phase constituents, particle size distributions and morphology of the synthesized ultra-fine Cu powders were investigated. A complex mixture of Cu2O and Cu powders formed by pure supercritical water while high purity homogeneous ultra-fine Cu powders can be synthesized by supercritical water with formic acid as a reducing agent. Moreover, fine tuning of particle size and morphology can be realized by the addition of Ethylenediamine tetraacetic acid (EDTA). The modification mechanism of EDTA on the surfaces of ultra-fine Cu powders was investigated by X-ray photoelectron spectroscopy and Fourier transform infrared spectroscopy. EDTA adsorbed on the surfaces of nanoparticles by the dehydration reaction of carboxyl groups in the molecule of EDTA and hydroxyl groups on surfaces of copper nanoparticles (CuOH).

Synthesis, Structures, and Magnetic Investigations of Nickel Phosphates: Ni2(PO4)(OH), Ni7(PO4)3(HPO4)(OH)3, and NaNiPO4 Including Potential Haldane Behavior.

Three novel nickel-phosphate structures are reported, Ni2(PO4)(OH) (I), Ni7(PO4)3(HPO4)(OH)3 (II), and NaNiPO4 (III). Each new system was prepared via a high-temperature hydrothermal synthesis at 600-650 °C. All three compounds are built of quasi-one-dimensional (quasi-1-D) Ni2+ containing chains with varying phosphate bridging modes and were characterized by single crystal X-ray diffraction and magnetic susceptibility. All three compounds display very different magnetic behavior. Anisotropic magnetic data is reported for Ni2(PO4)(OH) (I) exhibiting slow antiferromagnetic ordering in the high-temperature regime with substructures that begin to form below 32 K at different field strengths. These characteristics affirm I as being one of the few Haldane-like material candidates. The Ni7(PO4)3(HPO4)(OH)3 (II) material is a member of the unusual ellenbergerite structural family and displays complex inter- and intrachain magnetic interactions while NaNiPO4 (III) shows antiferromagnetic ordering near 18 K. This magnetic behavior is correlated with their structures.

Topotactic Syntopogenous Sodium Vanadium Fluoride for High-Performance Sodium-Ion Batteries: Electron and Sodium-Ion Reservoirs in Perovskite/Diperovskite Superlattice.

In order to simultaneously accelerate ion and electron transfer in sodium-ion battery (SIB) cathodes, a topotactic superlattice was utilized, in which the atomically intrinsic lattice-matching effect from inner to external surface can boost the charge transfer due to the disappearance of the heterojunction interface. Herein, a topotactic syntopogenous Na3VF6/NaVF3 superlattice formulated as Na2.9V1.1F6 (NVF) was synthesized by a facile one-step low-temperature hydrothermal reaction. NVF nanoparticles show an excellent Na+ storage capacity (∼205 mAh g-1) in a high voltage window up to 4.2 V with ultralong cycling stability. That is associated with the mixed occupancy of V and Na in NVF. The multivalent V centers serve as electron reservoirs to inhibit phase transformation, and the Na-enriched Na3VF6 with better electron conductivity acts as a Na+ reservoir for effective electron transfer. Highly reversible (de)intercalation of Na+ is achieved in the channel of perovskite-type NaVF3 with structural integrity.

High-performance photocatalytic hydrogen evolution in a Zn0.5Cd0.5S/MoS2 p–n heterojunction

With respect to solid-solution photocatalysts for water splitting, researchers have focused on improving the loading and stability of catalysts, which have been major concerns and research interests. Herein, the fabrication of Zn0.5Cd0.5S/MoS2 nanocomposites involved a two-step method that encompassed hydrothermal synthesis and physical mixing. Experimental results confirmed that the Zn0.5Cd0.5S/MoS2 nanocomposites exhibited outstanding photocatalytic performance. In particular, they exhibited a notable hydrogen precipitation rate of 19.41 mmol/(g*h). The hydrogen production performance of Zn0.5Cd0.5S/MoS2 was approximately nine times greater than that of pure Zn0.5Cd0.5S, indicating a considerable increase. The observed enhancement in photocatalytic efficiency can be attributed to the formation of a p–n heterojunction between Zn0.5Cd0.5S and MoS2. This particular junction helped in separating and migrating photoinduced charge carriers, ultimately improving the photocatalytic performance. Furthermore, the addition of excess thiourea in MoS2 preparation produced Mo–O defects and increased the layer spacing of the involved material, improving the electron transfer and visible-light utilization of the material. The inhibition of carrier recombination was beneficial for synthesizing efficient and long-lasting photocatalysts.

Hydrothermal and electrochemical synthesis of Fe2O3 and ZnFe2O4/Fe2O3 photoanodes for photoelectrochemical applications: An experimental and theoretical study

Hematite (Fe2O3) is commonly utilized in the fabrication of photoelectrochemical cells for water-splitting reaction. However, its relatively low efficiency has highlighted the necessity for enhancements in Fe2O3-based photoanodes. In addressing this issue, this study implemented the addition of ZnFe2O4. The pure Fe2O3 was synthesized onto a Fluorine-doped Tin Oxide coated glass by the hydrothermal process, followed by the synthesis of various ZnFe2O4/Fe2O3 heterostructures using electrochemical deposition techniques. The thin film’s composition, surface morphology, and chemical species of the products were analyzed using X-ray Diffraction, Scanning Electron Microscopy, Transmission Electron Microscopy, and X-ray Photoelectron Spectroscopy, respectively. The performance of the Fe2O3-based photoanode was compared to that of various ZnFe2O4/Fe2O3 photoanodes through photoelectrochemical studies. Results indicated that a 50 s electrochemical deposition of ZnFe2O4 on Fe2O3 yielded the highest photoconversion efficiency. Additionally, Density Functional Theory was employed to investigate the electron energy level of ZnFe2O4, revealing alignment with the properties of Fe2O3. Theoretical analysis showed that the Fermi energy of ZnFe2O4 exceeded that of Fe2O3, suggesting a preferable direction for electron transfer from ZnFe2O4 to Fe2O3 which was in consistent to the Mott-Schottky analysis. The performance of the overall ZnFe2O4/Fe2O3 heterostructure photoanodes demonstrated greater efficiency compared to pristine Fe2O3.