Layered Transition Metal Chalcogenides Research Articles

Sulfur vacancy riched pure 2H phase VS2 for efficient electrocatalytic hydrogen evolution

Vanadium disulfide (VS2), a typical metallic layered transition metal chalcogenide (TMC), has been widely concerned for its high electrical conductivity and reactivity in electrochemical energy storage and conversion applications. The 2H phase VS2 is expected to exhibit high electrocatalytic activity and be more stable for hydrogen evolution reaction (HER) than the 1T phase structure. But at present, there still lacks a facile method to prepare pure 2H phase VS2. Herein, we successfully prepared pure 2H–VS2 through a simple one-step low-temperature hydrothermal method. We have investigated the effect of the hydrothermal reaction conditions (including the proportion of raw materials and hydrothermal reaction temperatures) on the phase composition and microstructure. Under the optimal condition of 140°C-24 h with a vanadium sulfur ratio of 1:5, a nano-flower-like 2H–VS2 material with high crystallinity and rich sulfur vacancy defects was obtained. Leveraging these structural advantages, as a demonstration, the product exhibits excellent electrocatalytic HER activity (with η10 of 181 mV, Tafel slope of 52 mV dec−1, and J0 of 67.9 × 10−3 mA cm−2) and stability (it can continuously produce hydrogen for 20 h at a current density of 50 mA cm−2 with ultra-small increased potential of less than 5 mV). This work provides a new way for constructing atomic vacancy defects in layered TMCs for efficient electrocatalysis and is also expected to promote the research of the basic properties of high phase purity TMCs.

Mangenese Copper Selenide Nanosheet Arrays Derived from Metal-Organic Frameworks for Efficient Solid-State Asymmetric Supercapacitors

Metal chalcogenide nanostructures, particularly metal selenides, have unique properties, such as high electrical conductivity, large specific surface area, exclusive porous networks, and exceptional electrochemical properties compared to traditional nanostructures.1 2 A novel strategy is proposed to design and fabricate hierarchical Manganese copper selenide nanosheet (MnCuSe NS) arrays from metal-organic frameworks (MOFs). The hierarchical MnCuSe NS arrays can deliver enriched electroactive sites and shorten the ion/electron diffusion pathways. When evaluated as positive electrodes for supercapacitor (SC), the MnCuSe NS electrode displayed remarkable electrochemical properties with ultra-high specific capacity of ≈350.4 mA h g− 1 and an areal capacity of ≈0.94 mA h cm− 2 at a current density of 3 mA cm− 2, exceptional rate capability (≈79.5% of the capacity retention at a higher current density of 50 mA cm− 2), and outstanding cyclic stability (≈95.4 % of capacity retention after 10 000 cycles). Most importantly, the assembled MnCuSe NS//FeMnO/NG solid-state asymmetric SC exhibited a wide operating potential window of 1.6 V with an ultra-high volumetric capacity of ≈2.4 mA h cm− 3 at a current density of 3 mA cm− 2, an excellent energy density of ≈71.6 Wh Kg− 1 at a power density of ≈794 W Kg− 1, and ultra-long cycle life (≈93.4 % of capacity retention after 10 000 cycles). This proposed method provides a general protocol to design and fabricate metal selenide nanosheet arrays with superior electrochemical energy storage properties and exceptional cyclic stability, holding significant potential for future energy storage devices in commercial aspects. Keywords: Hierarchical, Metal-organic frameworks, Metal chalcogenide, Energy density, Asymmetric supercapacitorsReference:(1) Han, J. H.; Kwak, M.; Kim, Y.; Cheon, J. Recent Advances in the Solution-Based Preparation of Two-Dimensional Layered Transition Metal Chalcogenide Nanostructures. Chem. Rev. 2018, 118 (13), 6151–6188. https://doi.org/10.1021/acs.chemrev.8b00264.(2) Karuppasamy, K.; Vikraman, D.; Hussain, S.; Kumar Veerasubramani, G.; Santhoshkumar, P.; Lee, S.-H.; Bose, R.; Kathalingam, A.; Kim, H.-S. Unveiling a Binary Metal Selenide Composite of CuSe Polyhedrons/CoSe2 Nanorods Decorated Graphene Oxide as an Active Electrode Material for High-Performance Hybrid Supercapacitors. Chemical Engineering Journal 2022, 427, 131535. https://doi.org/10.1016/j.cej.2021.131535.

2D Monolayer Catalysts: Towards Efficient Water Splitting and Green Hydrogen Production.

A viable alternative to non-renewable hydrocarbon fuels is hydrogen gas, created using a safe, environmentally friendly process like water splitting. An important role in water-splitting applications is played by the development of two-dimensional (2D) layered transition metal chalcogenides (TMDCs), transition metal carbides (MXenes), graphene-derived 2D layered nanomaterials, phosphorene, and hexagonal boron nitride. Advanced synthesis methods and characterization instruments enabled an effective application for improved electrocatalytic water splitting and sustainable hydrogen production. Enhancing active sites, modifying the phase and electronic structure, adding conductive elements like transition metals, forming heterostructures, altering the defect state, etc., can improve the catalytic activity of 2D stacked hybrid monolayer nanomaterials. The majority of global research and development is focused on finding safer substitutes for petrochemical fuels, and this review summarizes recent advancements in the field of 2D monolayer nanomaterials in water splitting for industrial-scale green hydrogen production and fuel cell applications.

Single Transition-Metal Atom Anchored on a Rhenium Disulfide Monolayer: An Efficient Bifunctional Electrocatalyst for the Oxygen Evolution and Oxygen Reduction Reactions.

Developing efficient oxygen evolution reaction (OER) and oxygen reduction reaction (ORR) bifunctional electrocatalysts is attractive for rechargeable metal-air batteries. Meanwhile, single metal atoms embedded in 2D layered transition metal chalcogenides (TMDs) have become a very promising catalyst. Recently, many attentions have been paid to the 2D ReS2 electrocatalyst due to its unique distorted octahedral 1T' crystal structure and thickness-independent electronic properties. Here, the catalytic activity of different transition metal (TM) atoms embedded in ReS2 using the density functional theory is investigated. The results indicate that TM@ReS2 exhibits outstanding thermal stability, good electrical conductivity, and electron transfer for electrochemical reactions. And the Ir@ReS2 and Pd@ReS2 can be used as OER/ORR bifunctional electrocatalysts with a lower overpotential for OER (ηOER) of 0.44 V and overpotentials for ORR (ηORR) of 0.26 V and 0.27 V, respectively. The excellent catalytic activity is attributed to the optimal adsorption strength for oxygen intermediates coming from the effective modulation of the electronic structure of ReS2 after Ir/Pd doping. The results can help to deeply understand the catalytic activity of TM@ReS2 and develop novel and highly efficient OER/ORR electrocatalysts.

Composites of Carbons/Indium Sulfide for Hydrogen Peroxide Production and Water Purification

Photocatalysis enables room temperature synthesis of hydrogen peroxide (H2O2) without any byproducts as well as offering advantages such as low cost, and no release of toxic chemicals [1]. Thus, photocatalysis is an appealing approach for the environmentally friendly synthesis of H2O2. Two-dimensional (2D) layered transition metal chalcogenide (TMC) photocatalysts are good at light harvesting due to their high specific surface area and exhibit excellent optoelectronic properties which make them suitable for environmental remediation and energy production [2]. Metal sulfides have a narrower band gap, which improves their light absorption ability in the visible spectrum. However, they often suffer from low quantum yield and high charge recombination rate. Carbonaceous materials have been proven as very effective co-catalysts with semiconductors at increasing their photoactivity and decreasing recombination rate [3]. The present study focusses on indium sulfide (In2S3) and its composites with carbon nano tubes (CNTs) and carbon quantum dots (CQDs) for H2O2 generation via two-electron oxygen reduction reaction. In2S3, In2S3-CNT and In2S3-CQD are synthesized via hydrothermal method. Structural and optical properties characterized using several techniques such as XRD, Raman, UV-Vis-DRS, PL spectra, SEM, TEM etc. show high crystallinity of In2S3 lattice, good dispersion of carbons on In2S3 lattice, improved light absorption and decrease in recombination rate in In2S3 carbon composites. Photoelectric properties are studied using chronoamperometry, EIS, cyclic voltammetry etc. The In2S3 carbon composites show good stability and lower charge transfer resistance and higher active surface area than pure In2S3. The carbon composite materials show a significantly higher performance than the pure In2S3. In2S3-CQD achieves H2O2 production rate of 634 µM h-1, which is ~ 17 times higher than that of pure In2S3. These composites also show good performance for water treatment with In2S3-CQD removing 93% chromium(VI) and 94% rhodamine B (RhB) from contaminated water upon 2h of irradiation. The mechanism of removal of the impurities is also discussed. In2S3-CQD has shown good results owing to their good light absorption, high specific surface area, and CQDs being able to act as electron reservoir. Keywords : Photocatalysis, Hydrogen peroxide photosynthesis, Advanced Oxidation processes, Wastewater Treatment.

Synthesis and mechanism of MoS2 and graphene oxide insertion in porous multi metal ion modified MnO2 nanorods for dye degradation

Layered structure transition metal chalcogenide compound’s such as Molybdenum sulfide (MoS2) deposition in micro/meso porous architecture of MnO2 could provide hybrid interesting features. Multivalent MnO2 is an attractive low cost and toxic free catalytic material for oxidation reaction and electrochemical applications. Non-ionic surfactant implication in mesoporous metal ion modified MnO2 by deposition of metal chalcogenide is an effective composite for dye degradation applications. The low-cost pre-cursor makes it attractive for large-scale production at industrial scale. Hence, in the present study deals with exploit the mechanism of metal chalcogenide and graphene oxide insertion in porous manganese oxide matrix. The as prepared l surface properties of the Nickel and cobalt doped manganese oxide/MoS2 composite catalyst have shown effective congo red dye degradation activity. The complete color disappearance appeared after interaction with the composite catalyst.

Constructing a Functionalized Electrocatalyst of a Transition Metal Chalcogenide on Accordion-Like MXene to Boost the Hydrogen Evolution Reaction.

MXenes exhibit unique layered structures and excellent electrical conductivity, and their multiple surface termination groups are favorable for hosting impressive performance for electrochemical reactions. Therefore, a two-dimensional (2D) layered MXene-based catalyst may become a novel high-efficiency electrocatalyst to replace traditional noble metal electrocatalysts. In this work, a transition metal chalcogenide (MoS2/CuS) and MXene are combined to prepare a 2D electrocatalyst (MoS2/CuS/MXene) for the hydrogen evolution reaction (HER). MXene exhibited a large specific surface area in the shape of an accordion, which was very beneficial for the growth of nanomaterials. CuS/MXene promoted electron transfer and improved the exposed active site for HER. The exposed MoS2 edges exhibited a high chemical adsorption capacity, which is conducive to HER. Electrochemical tests reveal that the MoS2/CuS/MXene electrocatalyst can reduce the charge transfer resistance toward the HER and increase active sites for HER, leading to enhancing the catalytic performance. The MoS2/CuS/MXene electrocatalyst affords an efficient HER with a low overpotential (115 mV@10 mA cm-2). This work offers a new idea to create layered transition metal chalcogenide- and MXene-based electrocatalysts for HER.

Mn2+-Doped MoS2/MXene Heterostructure Composites as Cathodes for Aqueous Zinc-Ion Batteries.

Typical layered transition-metal chalcogenide materials, especially MoS2, are gradually attracting widespread attention as aqueous Zn-ion battery (AZIB) cathode materials by virtue of their two-dimensional structure, tunable band gap, and abundant edges. The metastable phase 1T-MoS2 exhibits better electrical conductivity, electrochemical activity, and zinc storage capacity compared to the thermodynamically stable 2H-MoS2. However, 1T-MoS2 is still limited by the phase stability and layered structure destruction for AZIB application. Thus, a three-dimensional interconnected network heterostructure (Mn-MoS2/MXene) consisting of Mn2+-doped MoS2 and MXene with a high percentage of 1T phase (82.9%) was synthesized by hydrothermal methods and investigated as the cathode for AZIBs. It was found that S-Mn-S covalent bonds between MoS2 interlayers and Ti-O-Mo bonds at heterogeneous interfaces can act as "electron bridges" to facilitate electron and charge transfer. And the doping of Mn2+ and the combination of MXene not only expanded the interlayer spacing of MoS2 but also maintained the metastable structure of 1T-MoS2 nanosheets, acting to reduce the activation energy for Zn2+ intercalation and enhance specific capacity. The obtained Mn-MoS2/MXene contains more 1T-MoS2 and provides an improved specific capacity of 191.7 mAh g-1 at 0.1 A g-1. Compared with Mn-MoS2 and pure MoS2, it also exhibits enhanced cycling stability with a capacity retention of 80.3% after 500 cycles at 1 A g-1. Besides, the conductivity of Mn-MoS2/MXene is significantly improved, which induces a lower activation energy of the zinc ions during intercalation/deintercalation.

Optimizing scalable synthesis of high-quality FeSe quantum dot in organic and aqueous states

A typical layered transition metal chalcogenide nanostructure, FeSe quantum dots (QDs) have recently begun to attract for their unique optical properties, i.e., multicolored excitation dependent emission (MEDE) property that breaks conventional Kasha - Vavilov rule as well as their potential applications in biological, and optical/electronic sensing and imaging. In this article, we present robust and optimized protocols for the scalable synthesis of FeSe QDs either in aqueous or organic syntheses. The synthesis conditions were carefully compared to obtain insistent synthesis parameters, e.g., solvents, precursors, stabilizers, pH, temperature, concentration, and reaction time after reproduction experiments. Furthermore, post-treatment procedures, i.e., phase transition and PEGylation are also optimized for further potential environmental and biological applications. In the scale-up experiments, a 5-liter reactor was utilized to produce approximately 55 g of QDs per batch, showing a robust optical MEDE property. The most optimized experimental condition reached quantum yield (QY) up to 60 % at the typical synthesis conditions of pH 9.0, 95 °C for 4 h of reflux, and the production yield of ca. 20%. These high fluorescent QDs can be potentially applied for biological fluorophores as well as next-generation QD displays.

Metal-Organic Assembly Strategy for the Synthesis of Layered Metal Chalcogenide Anodes for Na+ /K+ -Ion Batteries.

Layered transition metal chalcogenides (MX, M=Mo, W, Sn, V; X=S, Se, Te) have large ion transport channels and high specific capacity, making them promising for large-sized Na+ /K+ energy-storage technologies. Nevertheless, slow reaction kinetics and huge volume expansion will induce an undesirable electrochemical performance. Numerous efforts have been devoted to designing MX anodes and enhancing their electrochemical performance. Based on the metal-organic assembly strategy, nanostructural engineering, combination with carbon materials, and component regulation can be easily realized, which effectively boost the performance of MX anodes. In this Review, we present a comprehensive overview on the synthesis of MX nanostructure using the metal-organic assembly strategy, which can realize the design of MX nanostructures, based on self-sacrificial templates, host@guest tailored templates, post-modified layer and derivative templates. The preparation routes and structure evolution are mainly discussed. Then, Mo-, W-, Sn-, V-based chalcogenides used for Na+ /K+ energy storage are reviewed, and the relationship between the structure and the electrochemical performance, as well as the energy storage mechanism are emphasized. In addition, existing challenges and future perspectives are also presented.

Improving intrinsic electrocatalytic activity of layered transition metal chalcogenides as electrocatalysts for water splitting

Electrochemical water splitting has been considered an important method for facilitating renewable and sustainable energy conversion. For the practical application of water electrocatalysis, it is important to develop a non-noble metal-based, earth-abundant, highly efficient, and stable electrocatalysts for water splitting. Among the various non-noble metal-based electrocatalysts, layered transition metal chalcogenides (TMCs) have emerged as fascinating materials for electrochemical water splitting. The unique structural and electronic properties of layered TMCs make them very attractive for understanding the fundamental principles of electrocatalysis, as well as for developing highly efficient and stable electrocatalysts for the practical application of water electrocatalysis. In this mini review, we present a comprehensive overview of recent developments to improve the intrinsic electrocatalytic activity of layered transition metal chalcogenide (TMC)-based electrocatalysts for practical applications in water splitting.

Core-Shell-Structured Carbon Nanotube@VS4 Nanonecklaces as a High-Performance Cathode Material for Magnesium-Ion Batteries.

As a typical layered transition metal chalcogenide, VS4 is considered as a promising cathode material for advanced magnesium-ion batteries. However, the poor electronic conductivity and severe polarization effect restrict its practical applications. Herein, we report a betaine-assisted solvothermal strategy to coat VS4 nanoblocks on the surface of carbon nanotubes (CNTs), obtaining unique core-shell-structured CNT@VS4 nanonecklaces. As a result of the morphology-controlling effect of betaine, VS4 exhibits an unusual nanoblock morphology, which renders abundant active sites and promotes the contact between the electrode and electrolyte. CNTs serve as a highly conductive skeleton, combining with the VS4 nanoblocks and ensuring their uniform distribution. As a benefit from the synergistic effect of abundant active sites and electron-conductive highways, the as-synthesized CNT@VS4 nanonecklaces manifest remarkable performance for magnesium storage, including a large reversible capacity of 170 mAh g-1 at 0.1 A g-1, outstanding cycle stability (76.3 mAh g-1 after 800 cycles at 0.5 A g-1), and superior rate performance (77.2 mAh g-1 at 2 A g-1).

Nonlocal correlation effects in fermionic many-body systems: Overcoming the noncausality problem

Motivated by the intriguing physics of quasi-two-dimensional fermionic systems, such as high-temperature superconducting oxides, layered transition metal chalcogenides, or surface or interface systems, the development of many-body computational methods geared at including both local and nonlocal electronic correlations has become a rapidly evolving field. It has been realized, however, that the success of such methods can be hampered by the emergence of noncausal features in the effective or observable quantities involved. Here, we present an approach wherein local many-body techniques such as dynamical mean-field theory (DMFT) are extended to nonlocal correlations and interactions, which preserves causality and has a physically intuitive interpretation. Our strategy has implications for the general class of DMFT-inspired many-body methods and can be adapted to cluster, dual boson, or dual fermion techniques with minimal effort.

Enhanced critical field and anomalous metallic state in two-dimensional centrosymmetric 1T′−WS2

Layered transition-metal chalcogenide material (TMD) offers a platform to investigate two-dimensional (2D) superconductivity. Here, we report an electrical transport study of 2D centrosymmetric superconductor $1{T}^{\ensuremath{'}}\text{\ensuremath{-}}\mathrm{W}{\mathrm{S}}_{2}$. For a typical five-layer sample, the 2D superconductivity is revealed in Berezinskii-Kosterlitz-Thouless (BKT) transition with the characteristic temperature ${T}_{BKT}\ensuremath{\sim}5\phantom{\rule{0.16em}{0ex}}\mathrm{K}$. The superconductivity is observed with a strong resist against the in-plane magnetic field. We find that the critical in-plane magnetic field is \ensuremath{\sim}3 times the Pauli paramagnetic limit ${B}_{p}$, with effective Zeeman-type spin-orbital coupling $\stackrel{\ifmmode \tilde{}\else \~{}\fi{}}{{\ensuremath{\beta}}_{\mathrm{SO}}}\ensuremath{\sim}2.8\phantom{\rule{0.16em}{0ex}}\mathrm{meV}$. In addition, we find the magnetoresistance trend to saturate at low temperature, suggesting anomalous quantum metallic states. These findings might stimulate further investigations on the correlation between superconductivity and symmetry of 2D superconductors, as well as the quantum metallic states at low temperature with finite magnetic field.

Excitation-dependent emissive FeSe nanoparticles induced by chiral interlayer expansion and their multi-color bio-imaging

Layered transition metal chalcogenide nanostructures reveal unprecedented electronic and optical properties due to the unusual arrangement of interlayers and electronic interactions between them. Here, we report layered FeSe nanoparticles (NPs) coupled by L- or D-cysteine as a chiral stabilizer to show multi-colored excitation dependent emission (MEDE) for both single- and two-photon photoluminescence breaking conventional Kasha and Vavilov rules of luminescence, which is the first report in inorganic nanostructure system. Structural analysis shows the chiral stabilizer-induced interlayer spacing expansion in a FeSe NP. The MEDE in FeSe NPs is revealed to originate from the impurity coupled to the Mott insulator character of FeSe and chiral interlayer expansion through the first-principles electronic structure calculations and the classical molecular dynamics. Taking advantage of biocompatibility and multiphoton excitation in FeSe NPs, MEDE was utilized for bio-imaging of neuron cells and tissues altering excitation wavelength from visible to near-infrared range expanding the capabilities of multi-color bio-labeling.

Experimental research progress of electronic band structure and low temperature transport based on molybdenum disulfide

Molybdenum disulfide is a layered transition metal chalcogenide semiconductor. It has many applications in the fields of two-dimensional spintronics, valleytronics and optoelectronics. In this review, molybdenum disulfide is taken as a representative to systematically introduce the energy band structures of single layer, bilayer and twisted bilayer molybdenum disulfide, as well as the latest experimental progress of its realization and low-temperature electrical transport, such as superconductivity and strong correlation phenomenon. Finally, two-dimensional transition metal chalcogenide moiré superlattice’s challenges in optimizing contact and sample quality are analyzed and the future development of this field is also presented.

Experimental Observation of Pressure-Induced Superconductivity in Layered Transition-Metal Chalcogenides (Zr,Hf)GeTe4 Explored by a Data-Driven Approach

Layered transition-metal chalcogenides (Zr,Hf)GeTe$_{4}$ were screened out from database of Atomwork as a candidate for pressure-induced superconductivity due to their narrow band gap and high density of state near the Fermi level. The (Zr,Hf)GeTe$_{4}$ samples were synthesized in single crystal and then the compositional ratio, crystal structures, and valence states were investigated via energy dispersive spectrometry, single crystal X-ray diffraction, and X-ray photoelectron spectroscopy, respectively. The pressure-induced superconductivity in both crystals were first time reported by using a diamond anvil cell with a boron-doped diamond electrode and an undoped diamond insulating layer. The maximum superconducting transition temperatures of ZrGeTe$_{4}$ and HfGeTe$_{4}$ were 6.5 K under 57 GPa and 6.6 K under 60 GPa, respectively.

Facile and scalable ambient pressure chemical vapor deposition-assisted synthesis of layered silver selenide (β-Ag2Se) on Ag foil as a possible oxygen reduction catalyst in alkaline medium

Here, we report a facile upscaled ambient pressure CVD-assisted synthesis of low-temperature phase silver selenide (β-Ag2Se) on Ag foil and its first-reported application (in its pristine form) as an ORR catalyst. The exfoliated β-Ag2Se via XRD, EDS, HRTEM, AFM, and HRSEM determines its stoichiometry and its hollow layered fern-like morphology. Differential scanning calorimetry (DSC) further confirms that the final product is the low-temperature phase β-Ag2Se. Electrochemical oxygen reduction reaction (ORR) of exfoliated β-Ag2Se exhibits a strong oxygen reduction current with an onset potential of 0.88 V/RHE under alkaline conditions, indicating the oxygen reduction property of β-Ag2Se. The significant value of limiting current (3 mA cm−2) as well as small Tafel slope (68.5 mV dec−1) substantiates β-Ag2Se as a superior layered transition metal chalcogenide suitable for various energy-related applications (typically fuel cells and metal-air batteries).

Layered Transition Metal Electride Hf2Se with Coexisting Two-Dimensional Anionic d-Electrons and Hf–Hf Metallic Bonds* *Supported by the National Natural Science Foundation of China (Grant No. 11774424), the Fundamental Research Funds for the Central Universities (Grant No. 2017RC20), the Research Funds of Renmin University of China (Grant No. 20XNH064), the CAS Interdisciplinary Innovation Team, the Beijing Natural Science Foundation (Grant No.

Electrides are unique materials, whose anionic electrons are confined to interstitial voids, and they have broad potential applications in various areas. In contrast to the majority of inorganic electrides, in which the anionic electrons primarily consist of s-electrons of metals, electrides with anionic d-electrons are very rare. Based on first-principles electronic structure calculations, we predict that the layered transition metal chalcogenide Hf2Se is a novel electride candidate with anionic d-electrons. Our results indicate that the anionic electrons confined in the Hf6 octahedra vacancy between [Hf2Se] layers mainly come from the Hf-5d orbitals. In addition, the anionic electrons coexist with the Hf–Hf multiple-center metallic bonds located in the center of neighboring Hf4 tetrahedra. The calculated work function (3.33 eV) for the (110) surface of Hf2Se is slightly smaller than that of Hf2S, which has recently been reported to exhibit good electrocatalytic performance. Our study of Hf2Se will enrich the electride family, and promote further research into the physical properties and applications of electrides.

Structural Manipulation of Layered TiS2 to TiS3 Nanobelts through Niobium Doping for High‐Performance Supercapacitors

AbstractUnraveling the influence of incorporating transition metal elements on layered transition metal chalcogenides for energy storage application remains a challenge. Herein, niobium (Nb)‐doped layered titanium disulfide (TiS2) is applied to generate novel compounds Ti1−xNbxS2 (x=0.05, 0.1 and 0.20). Interestingly, TiS3 nanobelts are formed in the resulting materials, which is proven by systematic morphological and structural characterization. It has been found that Nb‐doped TiS2 compounds demonstrate superior electrochemical capacitive activity, reaching up to a 63.2 % increase in gravimetric capacitance in 1 M Na2SO4 electrolyte compared with that of the Nb‐free TiS2. This remarkably enhanced capacity behavior is attributed to Nb doping resulting a structural transition of Layered TiS2 to TiS3 nanobelts.