Nanosheet Research Articles

Defect engineering of two-dimensional ultrathin Co3O4 nanosheets for wireless and high-performance monitoring of the sensing properties of volatile organic compounds

Volatile organic compounds (VOCs) as serious outdoor and indoor air pollutants have attracted great attention. Many detection technologies of VOCs have been investigated. However, it is challenging to develop an efficient and portable wireless sensor for monitoring VOCs. Here, we proposed a new strategy to obtain a high-performance VOC sensor based on two-dimensional Co3O4 nanosheets (NSs) with numerous oxygen vacancy defects. The Co3O4 NS-30 W sensor detected 200 ppm ethanol and exhibited a high response value (10.70) and fast response and recovery behavior (20 s and 17 s, respectively). The effect of oxygen vacancy defects on the sensitive properties was studied by theoretical calculations on the (110) plane of Co3O4. Furthermore, a unique VOC wireless sensor was fabricated in order to enable wireless early warning from multiple terminals and monitoring of alcohol in exhaled gas. The VOC sensor exhibited a promising potential for precisely monitoring the alcohol consumption of drivers.

Influence of α-Fe2O3, CuO and GO 2D nano-fillers on the structure, physical properties and antifungal activity of Na-CMC–PAAm blend

The present work aims to improve the uses of the carboxymethyl cellulose–polyacrylamide (Na-CMC–PAAm) blend for energy storage, optoelectronic applications, biological control, and plant disease management. Nano-sized materials (α-Fe2O3 nanoplates (NP), CuO NP, and GO nanosheets (NS), were synthesized and incorporated into the blend. The phase purity and morphologies of the used fillers were studied by XRD and HR-TEM. The interactions and complexation between the nano-fillers and the blend chains were investigated using XRD and FTIR spectra. The chemical composition and surface morphology of the nanocomposites were studied using EDS and FE-SEM analysis. UV-vis-NIR spectra revealed that the blend shows about 95% transmittance, reduced by 10–30% after doping. The absorption and refractive indices, as well as the optical gaps of the blend, were greatly affected by the doping. The dielectric constant and loss depend on the type of filler and the applied frequency. The maximum ac conductivity of the blend at 303 K and 4.0 MHz is 21.5 × 10–4 S/m and increased to 23.5 × 10–4 S/m after doping with CuO NP. The thermal stability, activation energy, stress–strain curves, and tensile strength are dependent on the filler type. All nanocomposite solutions except the blend exhibited a wide range of antifungal properties against pre- and post-harvest phytopathogenic fungi. Aspergillus niger among the examined fungi showed high sensitivity to the tested nanocomposite solutions. Furthermore, the CuO/blend nanocomposite had the highest antifungal activity against all tested fungi. Based on that, we suggest the use of CuO/blend and GO/blend nanocomposites to control and combat pre- and post-harvest fungal plant diseases.

Study of Finite Element Simulation on the Mechano-Bactericidal Mechanism of Hierarchical Nanostructure Arrays.

Biomimetic nanostructures with bactericidal performance have become the research focus in constructing sterilization surfaces, but the mechano-bactericidal mechanism is still not fully understood, especially for the hierarchical nanostructure arrays with different heights. Herein, the interaction between Escherichia coli cells and nanostructure arrays was simulated by finite element, and the initial rupture points, i.e., critical action sites, of bacterial cells and the effects of nanostructure geometries on the cell rupture speed were analyzed based on the mechano-response of Escherichia coli cells on flat (identical heights) and hierarchical nanostructure arrays. The critical action sites of bacterial cells on nanostructure arrays are all at the three-phase junction zone of cell-liquid-nanostructure, but they are slightly shifted by the height difference ΔH of nanostructures on hierarchical nanopillar (NP)/nanosheet (NS) arrays, where the NP is higher than the NS. When ΔH < 20 nm, the site nears the NS corners, and when ΔH ≥ 20 nm, the site is consistent with that of the NP/NP array, i.e., the site locates at the three-phase junction zone of cell-liquid-high NP. In addition, except for decreasing the NP diameter, the NS thickness/width, or properly increasing the nanostructure spacing, the cell rupture can be accelerated via increasing the ΔH of nanostructures. ΔH = 40 nm is distinguished as the boundary for the effect of nanostructure ΔH on the cell rupture speed. When ΔH < 40 nm, the cell rupture speed rapidly increases as the ΔH increases; when ΔH ≥ 40 nm, the cell rupture speed reaches the maximum value and remains stable. This study provides a new strategy on how to design high-efficiency bactericidal surfaces.

Natural overlaying behaviors push the limit of planar cyclic deformation performance in few‐layer MoS2 nanosheets

AbstractAs a typical two‐dimensional (2D) transition metal dichalcogenides (TMDCs) material with nonzero band gap, MoS2 has a wide range of potential applications as building blocks in the field of nanoelectronics. The stability and reliability of the corresponding nanoelectronic devices depend critically on the mechanical performance and cyclic reliability of 2D MoS2. Although an in situ technique has been used to analyze the mechanical properties of 2D materials, the cyclic mechanical behavior, that is, fatigue, remains a major challenge in the practical application of the devices. This study was aimed at analyzing the planar cyclic performance and deformation behavior of three‐layer MoS2 nanosheets (NSs) using an in situ transmission electron microscopy (TEM) variable‐amplitude uniaxial low‐frequency and cyclic loading–unloading tensile acceleration test. We also elucidated the strengthening effect of the natural overlaying affix fragments (other external NSs) or wrinkle folds (internal folds from the NS itself) on cycling performances and service life of MoS2 NSs by delaying the whole process of fatigue crack initiation, propagation, and fracture. The results have been confirmed by molecular dynamics (MDs) simulations. The overlaying enhancement effect effectively ensures the long‐term reliability and stability of nanoelectronic devices made of few‐layer 2D materials.image

Carbon dots and MnO2 nanosheet nanocomposites sensing platform for sensitive detection of oxalate in urine samples of urolithiasis patients

In the human body, oxalate tends to form calcium oxalate with calcium ions, which can trigger the formation of stones in the urinary system. Therefore, oxalate in urine is usually utilized as a crucial biomarker in clinical urolithiasis diagnoses. In this work, a turn-on fluorescent nanoprobe was developed based on nitrogen-doped carbon dots (N-CDs) and MnO2 nanosheets (NSs) nanocomposites for oxalate sensing in urolithiasis patients. MnO2 NSs is a good sensing platform with high extinction coefficients and rich redox chemistry. The fluorescent N-CDs can be quenched efficiently by MnO2 NSs through the inner filter effect (IFE) to form N-CDs-MnO2 nanocomposites. The reductive oxalate could operate the decomposition of MnO2 NSs to Mn2+ resulting in the dissociation of the N-CDs-MnO2 nanocomposites and fluorescence recovery of N-CDs. Under optimal conditions, the developed sensor revealed good specificity toward oxalate with a limit of detection (LOD) of 0.69 μM. The developed sensor was successfully applied to quantify oxalate content in 47 urine samples (41 urolithiasis patients and 6 healthy persons). The results showed great consistency with clinical diagnostic reports and computed tomography images. This novel method retains several unique advantages, including affordable, rapid, and validating potential clinical application.

Direct Observation of Photon Induced Giant Band Renormalization in 2D PdSe2 Dichalcogenide by Transient Absorption Spectroscopy.

Insight into fundamental light-matter interaction as well as underlying photo-physical processes is crucial for the development of novel optoelectronic devices. Palladium diselenide (PdSe2 ), an important representative of emerging 2D noble metal dichalcogenides, has gain considerable attention owing to its unique optical, physical, and chemical properties. In this study, 2D PdSe2 nanosheets (NSs) are prepared using the liquid-phase exfoliation method. A broadband carrier relaxation dynamics from visible to near-infrared bands are revealed using a time-resolved transient absorption spectrometer, giving results that indicate band filling and bandgap renormalization (BGR) effects in the 2D PdSe2 NSs. The observed blue-shift of the transient absorption spectra at the primary stage and the subsequent red-shift can be ascribed to this BGR effect. These findings reveal the many-body character of the 2D TMDs material and may hold keys for applications in the field of optoelectronics and ultrafast photonics.

Surfactant regulated Core-Double-Shell NF@NiO nanosheets matrix as integrated anodes for Lithium-Ion batteries

The direct oxidation of three-dimensional nickel foam (3D NF) to nickel oxide (NiO) as integrated anode material for lithium-ion batteries (LIBs) has attracted significant attention towards achieving high-areal-capacity and high-energy density LIBs. However, the rate capability of such monolithic NiO in LIBs usually falls off rapidly due to the poor electrical conductivity that hindered its ionic transport kinetics. Herein, to ease the ionic transport constrains, a surfactant-regulated strategy is developed for preparing in-situ core-double-shell architecture that consists of core nickel skeleton, dense nickel oxide shell and porous nickel oxide nanosheets (NS) shell as anode materials for LIBs. Among the three employed surfactants including cationic surfactant, anionic surfactant and nonionic surfactant, the anionic surfactant (sodium dodecyl sulfate, SDS) modulated anode denoted SDS-NF@NiONS exhibits ultrahigh reversible areal capacity of 8.64 mAh cm−2@ 0.4 mA cm−2, and excellent rate areal capacity of 5.20 mAh cm−2 @ 3.0 mA cm−2, which did not only show the best ever reported NiO-based high-areal-capacity based electrodes, but also demonstrate impressive performance in practical full cell LIBs. In addition, in-situ Raman and kinetic analyses confirm the mechanism of Li-ion storage and facile ionic transport kinetics in this proposed design.

Is there a limit when the access resistance impact on the extraction of key GAA NS FETs devices parameters can (not) be avoided?

DC measurements are performed on n-type Si-channel gate-all-around (GAA) vertically stacked lateral nanosheet (NS) FETs. In this work, the impact of varying external access resistance values on extracted device parameters is analysed. Even if the parameters extraction is made using more access resistance insensitive methodologies, such as Y function-based methods, this work shows that in some cases a higher access resistance can still have an impact on the estimated parameter values, in particular for low field mobility. Moreover, by adding an external resistance only on the source side, the impact of this constructed asymmetry is evidenced on the drain current and transconductance characteristics even at low applied drain bias. The impact of the asymmetry may be enhanced by increasing the applied drain bias. A novel and intuitive Y-function strategy is used to estimate the main device electrical parameters.

Ultralow Dark Current Room‐Temperature Infrared Photodetector Based on InSb Nanosheets/MoS2 Van der Waals Heterostructure

As a narrow‐bandgap semiconductor, InSb is widely used in infrared (IR) detection due to its excellent performance and other characteristics such as ultrahigh electron mobility, extremely high quantum efficiency, and robust chemical properties. Herein, an ultralow dark current room‐temperature IR photodetector based on InSb nanosheets (NSs)/MoS2 flakes van der Waals (vdW) heterostructure is presented. Benefiting from a large surface‐to‐volume ratio and phonon scattering suppressed on the nanostructure, InSb NSs devices have high photosensitivity and low dark current density (16.67 A cm−2). To further suppress the dark current, a vdW heterojunction composed of InSb NSs and MoS2 is fabricated. When the InSb NSs/MoS2 vdW heterostructures’ photodetector work on a photovoltaic model (zero‐bias operation), the device shows a dark current density as low as 0.12 A cm−2 at room temperature, exhibiting a high external quantum efficiency (EQE) of 3.6 × 102%, the responsivity of 3.8 A W−1, and detectivity of 1.2 × 109 cm Hz1/2 W−1 under 1310 nm laser illumination. These results demonstrate that InSb NSs vdW heterostructure is a feasible scheme to realize InSb room‐temperature IR detection.

Enhanced colorimetric strategy: Aptamer-triggered assembly of Ni-Fe layered double oxide/DNA networks for ultrasensitive detection of chloramphenicol

In this study, a colorimetric assay was designed for ultrasensitive detection of chloramphenicol (CAP). In the presence of CAP, Ni-Fe layered double oxide/DNA networks (Ni-Fe LDO/DNA NWs) can be formed based on the combination of G-quadruplex (G4), DNA and magnetic Ni-Fe LDO nanosheets (NSs). Then, the as-formed Ni-Fe LDO/DNA NWs was applied to catalyze the oxidation of 3,3′,5,5′-tetramethylbenzidine (TMB) based on the enhanced peroxidase-like catalytic activity for the colorimetric analysis of CAP. To effectively enhanced the detection sensitivity, enzyme-free amplification methods including catalytic hairpin assembly (CHA) and hybridization chain reaction (HCR) were employed during this process. In addition, the background signal can be effectively reduced by means of the magnetic separation. Under optimal conditions, this strategy exhibited a wide linear range from 0.1 fM to 0.01 nM (r2 = 0.998), and the limit of detection (LOD) was obtained as 11.6 aM. Furthermore, the high specificity and stability of this strategy allowed its successful application to the quantitative analysis of residual CAP in genuine milk samples.

Injectable Hydrogel Containing TiO Nanosheets for Synergistic Photothermal/Thermodynamic Therapy.

Tumors have become the biggest obstacle to human health, and there are various treatment methods at present. Photothermal therapy (PTT) is usually ineffective and does not inhibit tumor progression due to the inability of the lasers to penetrate deeply. Therefore, most existing studies chose a 1064 nm laser with stronger penetrating power; meanwhile, studies have shown that the inclusion of harmful free radicals can significantly improve the antitumor efficacy. Herein, TiO nanosheets (NSs) were creatively prepared and encapsulated with an alkyl radical generator {2,2'-azobis[2-(2-imidazoline-2-yl)propane] dihydrochloride, [AIPH]} in sodium alginate (ALG) hydrogel for effective tumor killing by PTT and pairing with dangerous free radicals. TiO NSs were obtained by the liquid-phase exfoliation method, together with AIPH, which were in situ coencapsulated multifunctional hydrogels formed by the combination of Ca2+ and ALG. This ALG hydrogel could enrich TiO NSs and AIPH at the tumor site for a long time, and through the excellent photothermal properties of TiO NSs, AIPH could slowly and effectively generate alkyl radicals at the tumor site, which, in turn, gave it a better antitumor effect compared with that of TiO NSs in the deep hypoxic environment of the tumor. The AIPH + TiO + ALG hydrogel has distinctive anticancer capabilities based on the results of both in vivo and in vitro experiments. This material also has good biosafety. By combining PTT and free radical treatment, this work provides a novel therapeutic method to achieve oxygen-independent free radical production and enhance therapeutic efficacy.

Advanced heterostructure of Pd nanosheets@Pt nanoparticles boosts methanol electrooxidation

Heterostructures have emerged as elaborate structures to improve catalytic activity owing to their combined surface and distinct inverse interface. However, fabricating advanced nanocatalysts with facet-dependent interface remains an unexploited and promising area. Herein, we render the controlled growth of Pt nanoparticles (NPs) on Pd nanosheets (NSs) by regulating the reduction kinetics of Pt2+ with solvents. Specifically, the fast reduction kinetic makes the Pt NPs uniformly deposited on the Pd NSs (U-Pd@Pt HS), while the slow reduction kinetic leads to the preferential growth of Pt NPs on the edge of the Pd NSs (E-Pd@Pt HS). Density functional theory calculations demonstrate that Pd (111)-Pt interface in U-Pd@Pt HS induces the electron-deficient status of Pd substrates, triggering the d-band center downshift and amplifying the Pd-Pt intermetallic interaction. The synergy between the electronic effect and interfacial effect facilitates the removal of poisonous intermediates on U-Pd@Pt HS. By virtue of the Pd NSs@Pt NPs interface, the heterostructure achieves exceptional methanol oxidation reaction activity as well as improved durability. This study innovatively proposes heterostructure engineering with facet-dependent interfacial modulation, offering instructive guidelines for the rational design of versatile heterocatalysts.

Electrochemical Fabrication of 2D CuO Nanosheets on Pt Foil as a Highly Sensitive Non‐Enzymatic Glucose Sensor

AbstractA simple and environmentally‐friendly approach was developed to synthesize 2D CuO nanosheets using electrochemical deposition. The formed 2D CuO nanosheets (NSs) exhibit numerous advantageous properties such as no toxicity, high electrical conductivity, large active surface area, and a p‐type semiconducting nature with a band gap of 1.2 eV. A sensitive electrochemical sensor was constructed for the amperometric detection of glucose to take advantage of these characteristics. The fabricated sensor displayed an excellent sensitivity of 2710 μA mM−1 cm−2 along with a wide linear range of 0.001–1.0 mM and a lower limit of detection of 0.8 μM (S/N=3). Additionally, the modified electrode possesses high selectivity and good stability. The outstanding electrocatalytic performance of the electrode is attributed to a large active surface area, unique structural morphology, and the high conductivity of the 2D CuO nanosheets.

First Demonstration of Vertical Sandwich GAA TFETs with Self-Aligned High-k Metal Gates and Abrupt Doping Tunneling Junctions

A new type of vertical sandwich gate-all around tunneling field-effect-transistors (TFETs), called VSATFETs, was demonstrated firstly with a CMOS-compatible process. The VSATFETs with self-aligned high-κ metal gates (HKMG) and abrupt doping tunneling junctions were fabricated with the epitaxial of p+−Si/i-SiGe/n+−Si sandwich structure and an isotropic quasi-atomic layer-etch (qALE) process. VSATFETs have the advantage of excellent control of channel size, because its gate-length is mainly determined by the thickness of SiGe film grown by epitaxy, and the diameter of the nanowires (NWs)/thickness of nanosheets (NSs) is determined by the qALE etching of SiGe selective to Si. A NW VSATFET with a diameter of 18 nm was fabricated and exhibits excellent characteristics: SSmin = 61.64 mV dec−1, Ion = 2.25 × 10−7 A u−1m−1 (@Vgs−Vt = 0.45 V, Vd = 0.65 V), Ion/Ioff = 1.81 × 106, DIBL = 7.58 mV. The effect of interface traps on the device performance was analyzed by the calibrated model. It is found that the device performance can be improved by decreasing the thickness/diameter of NS/NW TFET.

Compact Modeling of Process Variations in Nanosheet Complementary FET (CFET) and Circuit Performance Predictions

In this work, a semi-analytical compact model of random process fluctuations in nanosheet (NS) gate-all-around (GAA) complementary FET (CFET) is proposed, including work-function variation (WFV), line edge roughness (LER), and gate edge roughness (GER). Different from the conventional NS GAA FET, GER has a significantly different impact on NS GAA CFET, due to the additional p-type work-function (p-WF) liner for p-FET threshold voltage tuning as well as the common metal gate, and a negative correlation with p-WF thickness is introduced into GER model. The proposed model is embedded into Berkeley short-channel insulated-gate field-effect transistor model-common multi-gate (BSIM-CMG) to predict the device performance variability by HSPICE Monte Carlo (MC) simulations. Excellent agreement between stochastic TCAD and HSPICE MC simulations is demonstrated. The effect of process variations on the power-performance-area (PPA) of standard cells (SDCs) and ring oscillator (RO) circuit is predicted by the proposed model. Most of the process variations make a more than <inline-formula xmlns:mml="http://www.w3.org/1998/Math/MathML" xmlns:xlink="http://www.w3.org/1999/xlink"> <tex-math notation="LaTeX">$-$</tex-math> </inline-formula> 10% to <inline-formula xmlns:mml="http://www.w3.org/1998/Math/MathML" xmlns:xlink="http://www.w3.org/1999/xlink"> <tex-math notation="LaTeX">$+$</tex-math> </inline-formula> 20% change in power consumption in NOR2. WFV has the greatest impact on RO PPA, making a <inline-formula xmlns:mml="http://www.w3.org/1998/Math/MathML" xmlns:xlink="http://www.w3.org/1999/xlink"> <tex-math notation="LaTeX">$-$</tex-math> </inline-formula> 10% to <inline-formula xmlns:mml="http://www.w3.org/1998/Math/MathML" xmlns:xlink="http://www.w3.org/1999/xlink"> <tex-math notation="LaTeX">$+$</tex-math> </inline-formula> 12.3% change in power consumption. The proposed model provides a helpful guideline for the random variation-aware CFET circuit design and related technology process development.

1D S-scheme heterojunction of urchin-like SiC-W18O49 for enhancing photocatalytic CO2 reduction

Constructing heterojunction is an important method to improve the performance of photocatalyst for CO2 reduction. In this work, W18O49 nanosheets (NSs) were grown on the surface of SiC nanocages (NCs) to form the sea urchin ball morphology by solvothermal method. The SiC-W18O49 composite photocatalyst processes 1D S-scheme heterojunction electron transport pathway. The special urchin morphology provides a large surface area for the contact between photocatalyst and CO2 reactants. Meantime, the S-scheme internal electric field at the heterogeneous interface of SiC-W18O49 composite photocatalyst can effectively promote the separation and migration of photogenerated carrier pairs owing to 1D heterojunction structure. The photocatalytic CO2 reduction products (CO + CH4 + CH3OH) can be produced up to 21.87 μmol g−1 h−1 by SiC-W18O49 composite photocatalyst, which was 3.38 and 3.71 times of the total reduction activity of the parent SiC and W18O49, respectively. This work will provide a new idea for the design of heterojunction morphology and structure for boosting photocatalytic CO2 reduction.

Facile Synthesis of MXene-Ti3C2/Co Nanosheet Hydrogel Sensor with the Assistance of a Smartphone for On-Site Monitoring of Glucose in Beverages

A one-step cobaltous chloride (CoCl2) molten salt method was employed to prepare multilayer MXene-Ti3C2/Co materials with further ultrasonic treatment to acquire single-layer MXene-Ti3C2/Co nanosheets (NSs). MXene-Ti3C2/Co NSs were characterized, and their enzyme-like activities were investigated. Under the catalysis of MXene-Ti3C2/Co NSs, 3,3′,5,5′-tetramethylbenzidine (TMB) could be oxidized by H2O2, with the color changing from colorless to blue. The affinity of MXene-Ti3C2/Co NSs to H2O2 and TMB was better than that of nanozymes reported in previous studies. The MXene-Ti3C2/Co NSs were used for the colorimetric determination of H2O2/glucose, with limits of detection (LODs) of 0.033 mM and 1.7 μM, respectively. MXene-Ti3C2/Co NSs embedded in sodium alginate (SA) hydrogel were used to construct a sensor platform. The digital pictures combined with a smartphone-installed app (color recognizer) could be used to analyze RGB values for colorimetric detection of glucose in beverages. This point-of-care testing platform has the advantages of cost-effectiveness and good transferability, with the potential to realize quick, intelligent and on-site detection.

Interface engineering SnS2/MXene Nb2C self-powered photodetectors with high responsivity and detectivity

Research on two-dimensional (2D) materials and their van der Waals heterostructures (vdWHs) has generated a lot of interest in the fields of electronics and optoelectronics. However, the construction of 2D heterostructures remains a challenge because the most widely used deterministic placement method to perform 2D layer stacking often suffers from erratic control of lattice orientation over lattice orientations. Herein, a new 2D/2D SnS2/MXene Nb2C heterostructure for high-performance photodetectors (PDs) was designed and prepared by using a simple electrostatic assembly process. It was demonstrated that the combination of Nb2C MXene nanosheets (NSs) and SnS2 NSs significantly improved the performance of PDs by enhancing the charge transfer, carrier density, light adsorption, as well as by decreasing band bending edge and charge recombination. The SnS2/Nb2C PDs exhibited remarkable responsivity (102.44 μA/W) and ultrahigh specific detectivity (7.48 × 1012 Jones) at zero external bias under a 365 nm laser at level Ⅳ. Additionally, comprehensive investigations of energy level diagram derived from both experimental measurements and density functional theory calculations provided further insights of such photodetector system. This simple and reliable fabrication strategy opens a new avenue for the large-scale production of low-cost and high-quality MXenes-based heterogeneous bond for next-generation electronic and optoelectronic applications.

BiOBr/COF S-scheme photocatalyst for H2O2 production via concerted two-electron pathway

Constructing step-scheme (S-scheme) heterojunctions has become a popular strategy for efficient photocatalytic H2O2 generation. Herein, we in situ grew BiOBr nanosheets (NSs) on a Schiff-base covalent organic framework (COF) with large π-conjugated structures to prepare S-scheme BiOBr/COF photocatalysts for H2O2 synthesis. The highest photocatalytic H2O2 production performance of the composite sample constituting the S-scheme heterojunction is 3749 µmol g−1 h−1, which was 1.85 and 27 times the rates of COF and BiOBr, respectively. The construction of S-scheme heterojunction contributed to efficient carrier transfer and separation in space and enhanced redox power. Moreover, the lying-down O2-adsorption configuration on the COF surface favors the concerted two-electron O2 reduction process, which greatly reduced the reduction potential requirement for O2-to-H2O2 conversion. The synergy between the S-scheme heterojunction and the unique O2–COF interaction boosted photocatalytic H2O2 production activity.

MoSe2-NiSe dual co-catalysts modified g-C3N4 for enhanced photocatalytic H2 generation

Solar energy conversion into hydrogen (H2) energy has attracted much attention. However, the low light utilization rate and fast carrier recombination of photocatalysts extremely limit the practical application of photocatalytic H2 production. In this paper, MoSe2-NiSe with abundant active sites and interfacial electronic structures as dual co-catalysts were assembled on g-C3N4 nanosheets (NSs) vis a solvothermal reaction process. MoSe2-NiSe/g-C3N4 NSs composite exhibited improved light absorption and photoelectrochemical properties. The photocatalytic H2 production rate of MoSe2-NiSe/g-C3N4 composite achieved 2379.04 μmol·h−1·g−1, which is 99.25, 1.44, and 3.67 times those of pure g-C3N4 nanosheets (23.97 μmol·h−1·g−1), MoSe2/C3N4 (1654.57 μmol·h−1·g−1), and NiSe/C3N4 (649.08 μmol·h−1·g−1), respectively. The apparent quantum efficiency (AQE) value of MoSe2-NiSe/g-C3N4 achieved 4.07 % under light at λ = 370 nm. The corresponding characterization and experiments proved that 2D ultrathin g-C3N4 NSs with a large surface area and short charge-transfer distance could facilitate light scattering and the transport of photoexcited electrons. MoSe2-NiSe, as a dual co-catalyst, showed strong electronic synergistic interaction between the interfaces, thus improving the conductivity and promoting the electron transfer process.