Two-dimensional MoS2 Nanosheets Research Articles

Discovery of Lipoxygenase-Like Materials for Inducing Ferroptosis.

Recent research has highlighted the pivotal role of lipoxygenases in modulating ferroptosis and immune responses by catalyzing the generation of lipid peroxides. However, the limitations associated with protein enzymes, such as poor stability, low bioavailability, and high production costs, have motivated researchers to explore biomimetic materials with lipoxygenase-like activity. Here, we report the discovery of lipoxygenase-like two-dimensional (2D) MoS2nanosheets capable of catalyzing lipid peroxidation and inducing ferroptosis. The resulting catalytic products were successfully identified using mass spectrometry and a luminescent substrate. Unlike native lipoxygenases, MoS2 nanosheets exhibited exceptional catalytic activity at extreme pH, high temperature, high ionic strength, and organic solvent conditions. Structure-activity relationship analysis indicates that sulfur atomic vacancy sites on MoS2 nanosheets are responsible for their catalytic activity. Furthermore, the lipoxygenase-like activity of MoS2 nanosheets was demonstrated within mammalian cells and animal tissues, inducing distinctive ferroptotic cell death. In summary, this research introduces an alternative to lipoxygenase to regulate lipid peroxidation in cells, offering a promising avenue for ferroptosis induction.

Multi-synergy enabling Ni-doped MoS2@N-doped carbon composite as versatile catalysts toward hydrogen production and photovoltaics

Construction of efficient non-precious catalyst with desired chemical composition and well-defined nanostructure is of great essential to enhance the kinetics of hydrogen evolution reaction (HER) and triiodide (I3−) reduction reaction (IRR), which is conducive to promote the development of green hydrogen production and obtain impressive photovoltaic performance of dye-sensitized solar cells (DSSCs). Herein, ZIF-8 derived N-doped carbon (NC) wrapped with two-dimensional Ni-doped MoS2 nanosheets (Ni–MoS2@NC) are elaborately designed. The catalytic activity of Ni–MoS2@NC for HER and IRR are significantly improved by modifying electronic structure through heteroatom doping. The optimized Ni–MoS2@NC has lower overpotential of 122 mV at 10 mA cm−2 in comparison with counterpart. Meanwhile, the power conversion efficiency (PCE) of DSSCs based on Ni–MoS2@NC CE catalyst is comparable to that of Pt. Density functional theory (DFT) calculation is used to unveil the mechanism of Ni–MoS2@NC for alkaline HER and IRR, namely, the multi-synergy of various sites endows Ni–MoS2@NC with appropriate Gibbs free energy for H∗ adsorption and water dissociation energy, while the top and interfacial S sites of Ni–MoS2@NC are responsible for the adsorption and activation of I3−. Our work provides a feasible route to design efficient catalysts in the field of energy conversion and understand mechanism.

Enhancing filler ratio and thermal conductivity of polyphenylene sulfide composites using molybdenum sulfide and carbon nanotubes: A layer-by-layer hot-pressing approach

In this study, we aimed to address challenges in thermal management and structural applications by developing composite materials with enhanced thermal conductivity and insulation properties. Our approach involved combining two-dimensional MoS2 nanosheets with carbon nanotubes (CNTs), leveraging their respective properties to create synergistic effects. MoS2, renowned for its remarkable electrical and mechanical attributes, was synthesized via a hydrothermal reaction and subsequently exfoliated using liquid-phase exfoliation techniques. Meanwhile, CNTs were surface-treated to prevent aggregation and ensure optimal dispersion within the composite matrix. These treated CNTs were then entangled with MoS2 nanosheets to form layered structures, facilitating the creation of efficient heat transfer pathways. The resulting MoS2-CNT composites were fabricated using a hot-pressing method, with polyphenylene sulfide (PPS) layers integrated for structural integrity. Through experimental investigation and characterization, our composites exhibited substantial improvements in thermal conductivity, achieving an impressive 5.77 W/mK. Additionally, the incorporation of PPS layers endowed the composites with insulation properties, further enhancing their suitability for diverse applications. Notably, the composite demonstrated a tensile strength of 67 MPa, indicating its potential for structural applications. This research underscores the promising potential of MoS2-CNT composites in addressing critical challenges in thermal management and structural engineering across various industries, including automotive and electronics. By offering a comprehensive solution that combines enhanced thermal conductivity, mechanical strength, and insulation properties, our composite material opens avenues for innovation in the development of advanced materials for next-generation technologies.

Construction of COFs@MoS2-Pd Hierarchical Tubular Heterostructures for Enhanced Catalytic Performance.

Here, we report ternary COFs@MoS2-Pd hybrids with an innovative self-sacrificial approach. MoO3@Covalent organic frameworks (COFs) microcables were first prepared and then two-dimensional MoS2 nanosheets (NSs) were integrated onto the surface of COFs, as COFs@MoS2, after treatment with hydrothermal reaction. The MoS2 NSs were used as an excellent support to introduce Pd nanoparticles (NPs) thanks to their reducing ability for the formation of the ternary COFs@MoS2-Pd hybrids. While COF microtubes improved the electrical conductivity of the hybrid materials, they also decreased the aggregation of MoS2 NSs, as a contribution to the enhanced catalytic performance. The mild reaction between MoS2 and Pd2+ ions realized the dense distribution of Pd NPs onto COFs@MoS2 for abundant active sites to further improve the catalytic performance. Thus, the hierarchical MoS2-based ternary hybrids were prepared with the enhanced catalytical performance as validated with the enzyme-like catalysis and the reduction of 4-nitrophenol.

Atomic vacancies of molybdenum disulfide nanoparticles stimulate mitochondrial biogenesis

Diminished mitochondrial function underlies many rare inborn errors of energy metabolism and contributes to more common age-associated metabolic and neurodegenerative disorders. Thus, boosting mitochondrial biogenesis has been proposed as a potential therapeutic approach for these diseases; however, currently we have a limited arsenal of compounds that can stimulate mitochondrial function. In this study, we designed molybdenum disulfide (MoS2) nanoflowers with predefined atomic vacancies that are fabricated by self-assembly of individual two-dimensional MoS2 nanosheets. Treatment of mammalian cells with MoS2 nanoflowers increased mitochondrial biogenesis by induction of PGC-1α and TFAM, which resulted in increased mitochondrial DNA copy number, enhanced expression of nuclear and mitochondrial-DNA encoded genes, and increased levels of mitochondrial respiratory chain proteins. Consistent with increased mitochondrial biogenesis, treatment with MoS2 nanoflowers enhanced mitochondrial respiratory capacity and adenosine triphosphate production in multiple mammalian cell types. Taken together, this study reveals that predefined atomic vacancies in MoS2 nanoflowers stimulate mitochondrial function by upregulating the expression of genes required for mitochondrial biogenesis.

Two-Dimensional MoS2 nanosheets as cocatalyst to augment the nanocatalytic tumor therapy

As an appealing modality of tumor nanocatalytic therapeutics, Fenton chemistry has been extensively employed to combat cancer through the generation of highly cytotoxic reactive oxygen species (ROS). For iron-triggered catalytic Fenton chemistry, the therapeutic consequence was largely dependent on the available catalytically active ferrous species. In this work, hydrothermally synthesized molybdenum disulfide (MoS2-PEG) nanosheets were served as Fenton cocatalyst to enhance the Fenton kinetics as contributed by ultrasmall gallic acid (GA)-coordinated Fe nanoparticles (GA-Fe NPs) in tumor destruction. The tetravalent Mo4+ species of MoS2-PEG cocatalysts could efficiently transfer Fe3+ species into Fe2+ species by the reduction process, regenerating the catalytically active Fe2+ species and restoring the catalytic activity of GA-Fe nanocatalysts during the Fenton-based tumor therapeutics. Based on systematic in vitro and in vivo investigations of cocatalyst-augmented Fenton nanotherapeutics against 4-T1 tumor cells/xenografts, we have demonstrated a proof-of-concept enhanced nanocatalytic tumor-therapeutic modality by MoS2-PEG/GA-Fe nanocatalyst/cocatalyst hybridized system, which offers an explicit cocatalytic strategy to improve the therapeutic efficacy during nanocatalytic tumor therapy.

Hollow engineering in CoNi@Air@C@MoS2 multicomponent composites derived from bimetallic CoNi Prussian blue analogs for ultra-wide bandwidth and strong electromagnetic wave absorption

In recent years, two-dimensional layered transition metal dichalcogenides-based multicomponent composites (MCCs) acting as electromagnetic wave (EMW) materials have received intensive investigations. However, the vulcanication of metal greatly hindered their enhancement of EMW absorption performances (EMWAPs). Herein, a combined metal-organic frameworks-derived and hydrothermal strategy was presented to produce yolk-shell structure (YSS) CoNi@Air@C@MoS2 MCCs. The results showed that the thermal and hydrothermal treatments resulted in the generation of YSS and two-dimensional MoS2 nanosheets, which maintained the original morphology of CoNi Prussian blue analogues. The protection of thick C layer well inhibited the vulcanization of inner CoNi alloy. The formed sheet-like MoS2 further optimized impedance matching characteristics, which led to the satisfactory EMWAPs of CoNi@Air@C@MoS2 MCCs. Furthermore, the EMWAPs could be further improved by optimizing the Ni:Co atom ratios CoNi@Air@C@MoS2 MCCs, which stemmed from their boosted impedance matching performances, EMW attention and polarization loss abilities. The absorption bandwidth and reflection loss values for YSS CoNi@Air@C@MoS2 MCCs are 8 GHz and −60.83 dB, which covered almost all C-Ku bands. In general, our research work provided a valid strategy to produce YSS magnetic CoNi@Air@C@MoS2 MCCs with high efficiency, which well avoided the vulcanization of metal nanoparticles, made best of hollow engineering and atomic ratio optimization strategy to boost the comprehensive EMWAPs.

Two-Dimensional MoS2 Nanosheets Derived from Cathodic Exfoliation for Lithium Storage Applications.

The preparation of 2H-phase MoS2 thin nanosheets by electrochemical delamination remains a challenge, despite numerous efforts in this direction. In this work, by choosing appropriate intercalating cations for cathodic delamination, the insertion process was facilitated, leading to a higher degree of exfoliation while maintaining the original 2H-phase of the starting bulk MoS2 material. Specifically, trimethylalkylammonium cations were tested as electrolytes, outperforming their bulkier tetraalkylammonium counterparts, which have been the focus of past studies. The performance of novel electrochemically derived 2H-phase MoS2 nanosheets as electrode material for electrochemical energy storage in lithium-ion batteries was investigated. The lower thickness and thus higher flexibility of cathodically exfoliated MoS2 promoted better electrochemical performance compared to liquid-phase and ultrasonically assisted exfoliated MoS2, both in terms of capacity (447 vs. 371 mA·h·g-1 at 0.2 A·g-1) and rate capability (30% vs. 8% capacity retained when the current density was increased from 0.2 A·g-1 to 5 A·g-1), as well as cycle life (44% vs. 17% capacity retention at 0.2 A·g-1 after 580 cycles). Overall, the present work provides a convenient route for obtaining MoS2 thin nanosheets for their advantageous use as anode material for lithium storage.

Morphological and Optical Characterization of Hydrothermally-Synthesized Two-Dimensional MoS2 Nanosheets

Transition metal dichalcogenides (TMDs) are extensively utilized in optoelectronics, sensors, and battery storage due to their versatile properties. Among the TMDs, Molybdenum disulfide (MoS2) nanosheets possess remarkable optical, electronic, and chemical properties. This study employed a cost-effective hydrothermal method to synthesize high-quality 2D MoS2 nanosheets. Different characterization techniques such as XRD, SEM, EDS, FTIR, Raman, UV–vis, and photoluminescence (PL) spectroscopy were utilized to evaluate the structural, morphological, chemical, and optical characteristics of the nanosheets. The XRD analysis revealed that the MoS2 nanosheets have a hexagonal crystal structure, with an average crystallite size of 27.76 nm. Furthermore, SEM images confirmed the formation of thin MoS2 nanosheets, with an estimated thickness ranging from 20–30 nm. The growth mechanism of the formation of MoS2 is discussed in detail. Different functional groups present in the material were analyzed using FTIR spectra. The difference in vibration modes analysed by Raman spectroscopy indicated the presence of layered nanosheets. The optical bandgap (2.20 eV) of the material was determined by analyzing its UV–vis spectroscopy data using the Tauc plot. PL analysis indicates a direct transition between the upper valence and lower conduction bands, suggesting that the nanosheets were synthesized with high quality. These findings have opened new possibilities for the use of MoS2 nanosheets in various applications such as optoelectronics and sensing devices.

Unveiling Xanthine Presence in Rohu Fish Using Ag+-Doped MoS2 Nanosheets Through Electrochemical Analysis.

Here, we envisage the development of the rapid, reliable, and facile electrochemical sensor for the primary detection of xanthine (Xn) which is significant for the food quality measurement, based on the silver-doped molybdenum disulfide (Ag@MoS2) nanosheets. The structural and compositional properties of the prepared samples were tested through X-ray diffraction (XRD), Fourier transform infrared (FT-IR) spectroscopy, and X-ray photon spectroscopy (XPS). The two-dimensional (2D) MoS2 nanosheets provide the large surface area for the sensing applications and the silver ions help in the enhanced electrochemical response. The fabricated enzymatic biosensor exhibits magnificent cyclic stability with a limit of detection of 27nM. Also, the sensor was tested for rapid, reproducible, specific, and regenerable up to 10 cycles and has a shelf life of 2weeks. The outcomes of this study suggest that the proposed matrix could be employed for the fabrication of devices for early detection of xanthine.

Synergetic enhancement effect of two-dimensional MoS2 nanosheets and metal organic framework-derived porous ZnO nanorods for photodegradation performance.

Two-dimensional transition metal dichalcogenides and semiconductor metal oxides have shown great potential in photocatalysis. However, their stability and efficiency need to be further improved. In this paper, porous ZnO nanorods with high specific surface area were prepared from metal-organic framework ZIF-8 by a simple hydrothermal method. A MoS2/ZnO composite was constructed by loading MoS2 onto the surface of porous ZnO nanorods. Compared with ZnO materials prepared by other methods, MoS2/ZnO prepared in this paper exhibits superior photocatalytic performance. The enhanced photocatalytic activity of the MoS2/ZnO composite can be attributed to the formation of heterojunctions and strong interaction between them, which greatly facilitate the separation of electrons and holes at the contact interface. In addition, due to the wide absorption region of the visible spectrum, MoS2 can greatly broaden the light absorption range of the material after the formation of the composite material, increase the utilization rate of visible light, and reduce the combination of electrons and holes. This study provides a new way to prepare cheap and efficient photocatalysts.

Phase engineering of two-dimensional MoS2 nanosheets

Phase engineering of two-dimensional MoS2 nanosheets

Enhanced Electrochemical Biosensing of the Sp17 Cancer Biomarker in Serum Samples via Engineered Two-Dimensional MoS2 Nanosheets on the Reduced Graphene Oxide Interface.

In the present investigation, we reported a label-free and highly effective immunosensor for the first time employing a nanostructured molybdenum disulfide nanosheets@reduced graphene oxide (nMoS2 NS@rGO) nanohybrid interface for the determination of sperm protein 17 (Sp17), an emerging cancer biomarker. We synthesized the nMoS2 NS@rGO nanohybrid using a one-step hydrothermal technique and then functionalized it with 3-aminopropyltriethoxysilane (APTES). Furthermore, the anti-Sp17 monoclonal antibodies were covalently attached to the APTES/nMoS2 NS@rGO/indium tin oxide (ITO) electrode utilizing 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide-N-hydroxy succinimide (EDC-NHS) coupling chemistry. Bovine serum albumin (BSA) was then used to block nonspecific binding regions on the anti-Sp17/APTES/nMoS2 NS@rGO/ITO bioelectrode. The morphological and structural features of the synthesized nanohybrid and the modified electrodes were studied using transmission electron microscopy, scanning electron microscopy with energy dispersive X-ray (EDX) composition studies, atomic force microscopy, Fourier transform infrared spectroscopy, and Raman spectroscopy. The immunoreaction between the Sp17 antigen and anti-Sp17 antibodies on the surface of the BSA/anti-Sp17/APTES/nMoS2 NS@rGO/ITO sensing bioelectrode was applied as the basis for the detection technique, which measured the electrocatalytic current and impedimetric response change. The designed BSA/anti-Sp17/APTES/nMoS2 NS@rGO/ITO bioelectrode showed improved amperometric and impedimetric biosensing performance in the response studies, including remarkable sensitivity (23.2 μA ng-1mL cm-2 and 0.48 kΩ mL ng-1 cm-2), wider linearity (0.05-8 and 1-8 ng mL-1), an excellent lower detection limit (0.13 and 0.23 ng mL-1), and a rapid response time of 20 min. The biosensor exhibited impressive storage durability lasting 7 weeks and showed remarkable precision in identifying Sp17 in serum samples from cancer patients, as confirmed using the enzyme-linked immunosorbent assay method.

Phase-dependent growth of Pt on MoS2 for highly efficient H2 evolution.

Crystal phase is a key factor determining the properties, and hence functions, of two-dimensional transition-metal dichalcogenides (TMDs)1,2. The TMDmaterials, explored for diverse applications3-8, commonly serve as templates for constructing nanomaterials3,9 and supported metal catalysts4,6-8. However, how the TMD crystal phase affects the growth of the secondary material is poorly understood, although relevant, particularly for catalyst development. In the case of Pt nanoparticles on two-dimensional MoS2 nanosheets used as electrocatalysts for the hydrogen evolution reaction7, only about two thirds of Pt nanoparticles were epitaxially grown on the MoS2 template composed of the metallic/semimetallic 1T/1T' phase but with thermodynamically stable and poorly conducting 2H phase mixed in. Here we report the production of MoS2 nanosheets with high phase purity and show that the 2H-phase templates facilitate the epitaxial growth of Pt nanoparticles, whereas the 1T'phase supports single-atomically dispersed Pt (s-Pt)atoms with Ptloading up to 10 wt%. We find that the Pt atoms in this s-Pt/1T'-MoS2 system occupy three distinct sites, with density functional theory calculations indicating for Pt atoms located atop of Mo atoms a hydrogen adsorption free energy of close to zero. This probably contributes to efficient electrocatalyticH2 evolution in acidic media, where we measure for s-Pt/1T'-MoS2 a mass activity of 85 ± 23 A [Formula: see text] at the overpotential of -50 mV and a mass-normalized exchange current density of 127 A [Formula: see text] and we see stable performance in an H-type cell and prototype proton exchange membrane electrolyser operated at room temperature. Although phase stability limitations prevent operation at high temperatures, we anticipate that 1T'-TMDs will also be effective supports for other catalysts targeting other important reactions.

Enhancing Lubrication Performance of Calcium Sulfonate Complex Grease Dispersed with Two-Dimensional MoS2 Nanosheets

Calcium sulfonate complex greases (CSCG) have proven to be a sustainable alternative to lithium complex greases, which still require appropriate additives to deliver lubrication performance benefits under extreme working conditions such as heavy load, high speed, and high temperature. The anti-wear and friction reducing properties of CSCG enhanced by two-dimensional MoS2 nanosheets (2D MoS2) with a narrow lateral size and thickness distributions were evaluated by a four-ball tribometer. The results showed that the CSCG with 0.6 wt.% 2D MoS2 performs best, with a 56.4% decrease in average friction coefficient (AFC), 16.5% reduction in wear scar diameter (WSD), 14.3% decrease in surface roughness, and a 59.4% reduction in average wear depth. Combining SEM-EDS images, Raman, and X-ray photoelectron spectra, it is illustrated that the physical transferred film and tribo-chemical film consisting of MoS2, Fe2O3, FeSO4, CaCO3, CaO, and MoO3 were generated on the worn surface, which improves the lubrication performance of CSCG considerably.

The Effect of Sonication Parameters on the Thickness of the Produced MoS2 Nano-Flakes

Liquid Phase Exfoliation (LPE) is a common route to produce two-dimensional MoS2 nanosheets. In this research, MoS2 powder is exfoliated by an ultrasonic probe (sonicator) in a water-ethanol solution. It is reported that MoS2 as a prototype 2D Transition Metal Dichalcogenide, has a band gap that increases with a decreasing number of layers. There are some factors that affect the average band gap energy value and the thickness of the exfoliated flakes. We varied different parameters of the ultrasonic probe like power, pulse percentage and time duration of sonication to investigate the effects on the number of MoS2 layers. Our findings from the UV-Visible spectra, SEM, FESEM and TEM images indicate that the minimum thickness for these samples was acquired at 50% of the input power of the sonicator we used (65 W) and the optimum pulse percentage is 50%. The current study also found that the average amount of band gap increased with an increase in sonication time, and then remained unchanged after 60 minutes.

In-situ-grown multidimensional Cu-doped Co1-xS2@MoS2 on N-doped carbon nanofibers as anode materials for high-performance alkali metal ion batteries

Transition metal sulfides with the high theoretical capacity and low cost have been considered as advanced anode candidate for alkali metal ion batteries, but suffered from unsatisfactory electrical conductivity and huge volume expansion. Herein, a multidimensional structure Cu-doped Co1-xS2@MoS2 in-situ-grown on N-doped carbon nanofibers (denoted as Cu-Co1-xS2@MoS2 NCNFs) have been elaborately constructed for the first time. The bimetallic zeolitic imidazolate framework CuCo-ZIFs were encapsulated in the one-dimensional (1D) NCNFs through an electrospinning route and then on which the two-dimensional (2D) MoS2 nanosheets were in-situ grown via a hydrothermal process. The architecture of 1D NCNFs can effectively shorten ion diffusion path and enhance electrical conductivity. Besides, the formed heterointerface between MOF-derived binary metal sulfides and MoS2 can provide extra active centers and accelerate reaction kinetics, which guarantee a superior reversibility. As expected, the resulting Cu-Co1-xS2@MoS2 NCNFs electrode delivers excellent specific capacity of Na-ion batteries (845.6 mAh/g at 0.1 A/g), Li-ion batteries (1145.7 mAh/g at 0.1 A/g), and K-ion batteries (474.3 mAh/g at 0.1 A/g). Therefore, this innovative design strategy will bring a meaningful prospect for developing high-performance multi-component metal sulfides electrode for alkali metal ion batteries.

Photoluminescence of Two-Dimensional MoS2 Nanosheets Produced by Liquid Exfoliation

Extraordinary properties of two-dimensional materials make them attractive for applications in different fields. One of the prospective niches is optical applications, where such types of materials demonstrate extremely sensitive performance and can be used for labeling. However, the optical properties of liquid-exfoliated 2D materials need to be analyzed. The purpose of this work is to study the absorption and luminescent properties of MoS2 exfoliated in the presence of sodium cholate, which is the most often used surfactant. Ultrasound bath and mixer-assisted exfoliation in water and dimethyl sulfoxide were used. The best quality of MoS2 nanosheets was achieved using shear-assisted liquid-phase exfoliation as a production method and sodium cholate (SC) as a surfactant. The photoluminescent properties of MoS2 nanosheets varied slightly when changing the surfactant concentrations in the range C(SC) = 0.5–2.5 mg/mL. This work is of high practical importance for further enhancement of MoS2 photoluminescent properties via chemical functionalization.

Integrating thermal energy storage and microwave absorption in phase change material-encapsulated core-sheath MoS2@CNTs

Developing advanced nanocomposite integrating solar-driven thermal energy storage and thermal management functional microwave absorption can facilitate the cutting-edge application of phase change materials (PCMs). To conquer this goal, herein, two-dimensional MoS2 nanosheets are grown in situ on the surface of one-dimensional CNTs to prepare core-sheath MoS2@CNTs for the encapsulation of paraffin wax (PW). Benefiting from the synergistic enhancement photothermal effect of MoS2 and CNTs, MoS2@CNTs is capable of efficiently trapping photons and quickly transporting phonons, thus yielding a high solar-thermal energy conversion and storage efficiency of 94.97%. Meanwhile, PW/MoS2@CNTs composite PCMs exhibit a high phase change enthalpy of 101.60 J/g and excellent long-term thermal storage durability after undergoing multiple heating–cooling cycles. More attractively, PW/MoS2@CNTs composite PCMs realize thermal management functional microwave absorption in heat-related electronic application scenarios, which is superior to the single microwave absorption of traditional materials. The minimum reflection loss (RL) for PW/MoS2@CNTs is −28 dB at 12.91 GHz with a 2.0 mm thickness. This functional integration design provides some insightful references on developing advanced microwave absorbing composite PCMs, holding great potential towards high-efficiency solar energy utilization and thermally managed microwave absorption fields.

A MXene/MoS2 heterostructure based biosensor for accurate sweat ascorbic acid detection

Biosensors with high sensitivity to sweat composition analysis are essential for non-invasive, real-time physiological monitoring of individual health status. However, it is challenging to construct a well-conductive and stable interface for electrochemical sensors. Here, we construct a sensitive sweat biosensor for ascorbic acid (AA) quantification built on a heterostructure with three-dimensional (3D) linked network microstructures made from two-dimensional (2D) MoS2 nanosheets and 2D Ti3C2 MXene. The as obtained 2D/2D heterostructures presented numerous active sites and avoid the issue of reduced surface areas, which was generally brought on by the accumulation of 2D nanomaterials. The electrode modified with 2D/2D heterostructure could realize efficient electron transport by abundant accesses to absorb AA molecules. Based on the inherent conductivity, extremely porous structure, and active catalytic properties of 2D/2D heterostructures, the biosensor for detecting the AA in artificial sweat had a sensitivity of 54.6nA μM−1 and a detection limit of 4.2 μM. This study provided a new promising approach for the design of high-performance sensing interfaces and facilitated the widespread use of personalized diagnostic devices.