Three-dimensional porous SnO2@NC framework for excellent energy conversion and storage

SnO₂-based materials are deemed to be attractive electrodes for lithium/sodium ion batteries (LIBs and SIBs) and electrocatalytic CO₂ reduction reaction (CRR) because of high energy density and large abundance. However, the practical application of the SnO₂-based materials is prevented by low electrical conductivity and large volume change. Herein, we construct a three-dimensional (3D) porous network with SnO₂ nanoparticles into N-doped carbon (namely P–SnO₂@NC) synthesized by freeze drying followed by a pyrolyzation process. In the composite, the 3D hierarchical framework can facilitate the ion penetration and gas diffusion. In addition, the NC network can optimize the conductivity of the material and suppress the electrode material to fall off from the electrode. Therefore, the electrode delivers excellent electrochemical properties with high capacities of 510 mA h g⁻¹ after 1000 cycles for LIBs and 497 mA h g⁻¹ after 500 cycles for SIBs. Furthermore, the electrode shows high selectivity for CRR with a large coulombic efficiency (CE) of 52.7% for HCOOH at 0.6 V.     

Uniform α-Fe2O3 nanoparticles with narrow gap immobilized on CNTs through N-doped carbon as high-performance lithium-ion batteries anode

Fe₂O₃ with high theoretical capacity, low cost, and environmental friendliness has been attracted great attention in lithium-ion batteries (LIBs), which however is limited by low rate capability and fast capacity fading owing to low electronic conductivity, self-aggregation, and sever volume expansion. CNTs with excellent conductivity and unique 3D interconnected network are ideal matrices for composite electrochemical materials, but it is difficult to meet the demand of high capacity. Here, uniform α-Fe₂O₃ nanoparticles with narrow gap (~1.4 nm) were immobilized on CNTs through N-doped carbon (α-Fe₂O₃/CNTs-NC) that can address these issues. As an advanced LIBs anode, the electrode displays unprecedented specific capacity (1173 mAh/g at 0.2 A/g) and outstanding rate behavior (716.4 mAh/g at 5.0 A/g after 1200 cycles), which are even superior to the theoretical capacity (1007 mAh/g) and the performance of most reported Fe₂O₃-based anodes. Homogeneous nano-sized α-Fe₂O₃ with a narrow gap highly shortens the diffusion path for Li⁺ transport, exposes quite sufficient active sites, and prevents the volume change. Moreover, the 3D backbone of CNTs with a more homogeneously distributed electric field can enhance conductivity, and tightly contact with α-Fe₂O₃ by NC, then obtain robust structural stability, which boosts LIBs in storage capacity, rate capability, and cycling stability.     

Electrochemical behavior of carbon-coated SnS2 for use as the anode in lithium-ion batteries

Carbon-coated SnS₂ nanoparticles were prepared by a simple solvothermal route at low temperature. A carbon coating with a thickness of about 5 nm was deposited on nano-sized SnS₂ particles to serve as the anode in lithium-ion batteries. Both the nanostructure and the morphology of the SnS₂ powders were characterized by X-ray diffraction (XRD), Raman spectroscopy, and transmission electron microscopy (TEM). The coated samples were used as active anode materials for lithium-ion batteries, and their electrochemical properties were examined by constant current charge-discharge cycling, cyclic voltammetry and electrochemical impedance spectroscopy. The reversible capacity of the carbon-coated SnS₂ after 50 cycles was 668 mAh/g, which was much higher than that of the uncoated SnS₂ (293 mAh/g). The carbon-coated SnS₂ also had a better rate capability than the uncoated SnS₂ in the range of 0.008-1 C. The capacity retention of the carbon-coated SnS₂ was improved due to its good conductivity and the effective buffer matrix that alleviated volume expansion during the charge-discharge process.     

Vertically aligned,polypyrrole encapsulated MoS2/graphene composites for high-rate LIBs anode

Ultrathin MoS₂ nanosheets were vertically anchored on the reduced graphene oxide (MoS₂/rGO) via hydrothermal method. To further engineering the surface conductivity, ultrathin polypyrrol (PPy) layer was coated on the MoS₂/rGO composite via in situ polymerization to form a bi-continuous conductive network with a sandwich-like structure. The graphene nanosheets and the PPy coating can facilitate the electrons transfer rate, while the ultrathin MoS₂ nanosheets can enhance the utilization efficiency of the active materials. The obtained MoS₂/rGO-10 composite exhibits high reversible specific capacity (970?mAh?g^?1 at 0.1?A?g^?1) and rate capability (capacity retention of 64% at 3.2?A?g^?1). Moreover, the PPy@MoS₂/rGO hybrids reveal lower specific capacity but better rate capability, and a “trade-off” effect between electrons and ions transfer resistance was observed. This easy-scalable PPy surface conductivity engineering strategy may be applied in the preparation of high-performance LIBs active materials.     

A review study on titanium niobium oxide-based composite anodes for Li-ion batteries: Synthesis,structure, and performance

The growing demands for Li-ion batteries (LIBs) in the electrification revolution, require the development of advanced electrode materials. Recently, intercalating titanium niobium oxide (TNO) anode materials with the general formula of TiNb_xO_2+2.5x have received lots of attention as an alternative to graphite and Li₄Ti₅O₁₂ commercial anodes. The desirability of this family of compounds stems from their high theoretical capacities (377–402 mAh/g), high safety, high working voltage, excellent cycling stability, and significant pseudocapacitive behavior. However, the rate performance of TNO-based anodes is poor owing to their low electronic and ionic conductivities. TNO-based composites generally are prepared with two aims of enhancing the conductivity of TNO and achieving a synergic effect between the TNO and the other component of the composite. Compositing with carbon matrices, such as graphene and carbon nanotubes (CNTs) are the most studied strategy for improving the conductivity of TNO and optimizing its high-rate performance. Also, for obtaining anode materials with high capacity and high long-term stability, the composites of TNO with transition metal dichalcogenides (TMDs) materials were proposed in previous literature. In this work, a comprehensive review of the TNO-based composites as the anodes for LIBs is presented which summarizes in detail the main recent literature from their synthesis procedure, optimum synthesis parameters, and the obtained morphology/structure to their electrochemical performance as the LIBs anode. Finally, the research gaps and the future perspective are proposed.     

In-situ synthesis of reduced graphene oxide wrapped Mn3O4 nanocomposite as anode materials for high-performance lithium-ion batteries

We report a novel in-situ symbiosis method to prepare reduced graphene oxide wrapped Mn₃O₄ nanoparticles (rGO/Mn₃O₄) with uniform size about 50 nm as anodes for lithium-ion batteries (LIBs), which can simplify the preparation process and effectively reduce pollution. The rGO/Mn₃O₄ nanocomposite exhibited a reversible specific capacity of 795.5 mAh g^?1 at 100 mA g^?1 after 200 cycles (capacity retention: 87.4%), which benefits from the unique structural advantages and the synergistic effect of rGO and Mn₃O₄. The Mn₃O₄ nanoparticles encapsulated among the rGO nanosheets exhibited good electrochemical activity, and the multilayer wrinkled rGO sheets provided a stable 3D conduction channel for Li⁺/e^? transport. The rGO/Mn₃O₄ nanocomposite is a promising anode candidate for advanced LIBs with excellent cycling performance and rate performance. Furthermore, this new preparation method can be extended to green and economical synthesis of advanced graphene/manganese-based nanocomposites.     

Synthesis and Electrochemical Performance of Spheroid LiNi<Subscript>1/3</Subscript>Co<Subscript>1/3</Subscript>Mn<Subscript>1/3</Subscript>O<Subscript>2</Subscript> in the Electrolyte Modified by Ethylene Sulfate and Methylene Methanedisulfonate

In this study, spheroid LiNi_1/3Co_1/3Mn_1/3O₂ (NCM111) cathode material were synthesized using LiOH with Ni_0.5Co_0.2Mn_0.3(OH)₂ precursor by a simple solid-state reaction, and characterized by X-ray diffraction and scanning electron microscopy. Electrochemical behavior of NCM111 was investigated by electrochemical impedance spectroscopy (EIS) combining with cyclic voltammogram (CV) and charge/discharge test in the 1 M LiPF₆-EC:EMC electrolyte with ethylene sulfate (DTD) and methylene methanedisulfonate (MMDS) additives either singly or in combination with high cutoff voltage of 3.0–4.5 V at room temperature of 25 °C or elevated temperature of 55 °C. It was found that DTD additive can increase the initial coulombic efficiency of NCM111, and the spheroid NCM111 can obtain the maximum initial discharge capacity of 177.81 mAh/g with the 2 wt% DTD, and keep 92.29% capacity retention after 80 cycles. The MMDS additives would decrease the initial discharge capacity of the NCM111, and enhance significantly long cycle life of the NCM111 with the capacity retention of 99.23% over 80 cycles at high voltage of 4.5 V. The additive combination 2 wt% DTD?+?1 wt% MMDS was an optimal additive combination, demonstrating the 102.2% capacity retention over 80 cycles at room temperature and the 94.2% capacity retention over 70 cycles at elevated temperature of 55 °C. EIS results revealed that the additive blend of 2 wt% DTD?+?1 wt% MMDS can drastically lower the kinetics impedance and suppress the growth rate of R _ct for the NCM111 electrode.     

NiFe-NiFe2O4/rGO composites: Controlled preparation and superior lithium storage properties

Binary transition-metal oxides with spinel structure have great potential as advanced anode materials for lithium-ion batteries (LIBs). Herein, NiFe-NiFe₂O₄/ reduced graphene oxide (rGO) composites are obtained via a facile cyanometallic framework precursor strategy to improve the lithium storage performance of NiFe₂O₄. In the composites, NiFe-NiFe₂O₄ nanoparticles with adjustable mass ratios of NiFe₂O₄ to NiFe alloy are homogeneously deposited on rGO sheets. As anode material for LIBs, the optimized NiFe-NiFe₂O₄/rGO composite displays remarkably enhanced lithium storage performance with an initial specific capacity as high as 1362 mAh g⁻¹ at 0.1 A g⁻¹ and a decent capacity retention of ca. 80% after 130 cycles. Besides, the composite delivers a reversible capacity of 550 mAh g⁻¹ at 1 A g⁻¹ after 300 cycles. During the charge–discharge cycles, the aggregation of the NiFe-NiFe₂O₄ nanoparticles and the structural collapse of the electrode can be well alleviated by rGO sheets. Moreover, the conductivity of the electrode can be significantly improved by the well-conductive NiFe alloy and rGO sheets. All these contribute to the improved lithium storage performance of NiFe-NiFe₂O₄/rGO composites.     

Fullerene-like Re-Doped MoS2 Nanoparticles as an Intercalation Host with Fast Kinetics for Sodium Ion Batteries

Sodium ion batteries (SIBs) are considered as a promising alternative to threaten the reign of lithium ion batteries (LIBs) among various next-generation rechargeable energy storage systems, including magnesium ion, metal air, and metal sulfur batteries. Since both sodium and lithium are located in Group 1 of the periodic table, they share similar (electro)chemical properties with regard to ionization pattern, electronegativity, and electronic configuration; thus the vast number of compounds developed from LIBs can provide guidance to design electrode materials for SIBs. However, the larger ionic radius of the sodium cation and unique (de)sodiation processes may also lead to uncertainties in terms of thermodynamic or kinetic properties. Herein, we present the first construction of SIBs based on inorganic fullerene-like (IF) MoS₂ nanoparticles. Closed-shell-type structures, represented by C₆₀ fullerene, have largely been neglected for studies of alkali-metal hosting materials due to their inaccessibility for intercalating ions into the inner spaces. However, IF-MoS₂, with faceted surfaces, can diffuse sodium ions through the defective channels, thereby allowing reversible sodium ion intercalation/deintercalation. Interestingly, Re-doped MoS₂ showed good electrochemical performances with fast kinetics (ca. 74 mA h g⁻¹ at 20 C). N-type doping caused by Re substitution of Mo in IF-MoS₂ revealed enhanced electrical conductivity and an increased number of diffusion defect sites. Thus, chemical modification of fullerene-like structures through doping is proven to be a promising synthetic strategy to prepare improved electrodes.     

NiSe2 encapsulated in N-doped TiN/carbon nanoparticles intertwined with CNTs for enhanced Na-ion storage by pseudocapacitance

Transitional metal selenides are considered as potential anode candidates for sodium-ion batteries (SIBs) because of their relatively high theoretical capacity and environmental benign. However, the large volume change derived from the conversion reaction and the sluggish kinetics due to the inherent low electrochemical conductivity hinder their practical application. Herein, composite materials of NiSe₂ encapsulated in nitrogen-doped TiN/carbon nanoparticles with carbon nanotubes (CNTs) on the surface (NiSe₂@N-TCP/CNTs) are fabricated via pyrolysis and selenization processes. In this composite, TiN inside the carbon matrix can enhance the conductivity and structural stability. CNTs that are in-situ grown on the surface not only further enhance the conductivity of the composites, but also offer sufficient space to buffer the volume expansion and alleviate serious aggregation of NiSe₂ nanoparticles. Benefit from these merits, the NiSe₂@N-TCP/CNTs showed a lower charge transfer resistance and a faster Na⁺ diffusion rate than materials without growing CNTs. When used as the anode of SIBs, the NiSe₂@N-TCP/CNTs electrode delivered a reversible capacity of 344.0 mAh g^?1 after 1000 cycles at 0.2 A g^?1, and still maintained at 272.7 mAh g^?1 even at a high current density of 2 A g^?1. The remarkable electrochemical performance is mainly attributed to the special designed hierarchical structures and pseudocapacitance sodium storage behavior.     

Binder-free multilayered SnO2/graphene on Ni foam as a high-performance lithium ion batteries anode

The reasonable structure construction of electrode materials with superior performance is desired for the new generation lithium ion batteries (LIBs). Herein, binder-free multilayered SnO₂/graphene (GN) on Ni foam was fabricated via a dip coating method. SnO₂ nanoparticles and GN were alternatively coated on Ni foam to form a sandwich-like structure. The wrapping of GN can raise the conductivity and keep the structural integrality of the binder-free material, preventing structure collapse arised from the volume expansion of SnO₂. Benefiting from the porous Ni foam framework and sandwich-like structure, the SnO₂/GN composite exhibited good rate performance and excellent cycle stability. High capacities of 708 and 609?mAh?g^?1 were achieved at rates of 1 and 2?A?g^?1. Besides, the SnO₂/GN electrode delivered a high capacity of 757?mAh?g^?1 after 500 cycles at 1?A?g^?1.     

Molybdenum carbide embedded in carbon nanofiber as a 3D flexible anode with superior stability and high-rate performance for Li-ion batteries

The fabrication process and material design of flexible lithium-ion batteries (LIBs) are essential in flexible portable devices. In particular, the carbon nanofiber (CNF)-based active anodes with flexibility synthesized using an electrospinning technique showed fairly stable cycling performance in the LIBs. In this study, we synthesized the molybdenum carbide (MoC) embedded in CNFs as an anode for LIBs (MoC/CNF) using an electrospinning technique with amorphous Mo precursor and polyacrylonitrile as the molybdenum and carbon sources, respectively, and using a heating process under an N₂ atmosphere. The as-prepared flexible MoC/CNF showed a 3D porous structure consisting of crystalline MoC and amorphous CNF. MoC/CNF, directly utilized as an active electrode without binder, conductor, or current collector, exhibited superior LIB performance, i.e. high capacity, cyclability, and high-rate properties. In particular, at a considerably high charge/discharge rate of 10?A?g^?1, the specific capacity of MoC/CNF (109?mAh?g^?1) was significantly higher than that of pure CNF electrode (3?mAh?g^?1).     

High-performance supercapacitor of manganese oxide/reduced graphene oxide nanocomposite coated on flexible carbon fiber paper

Although supercapacitors have higher power density than batteries, they are still limited by low energy density and low capacity retention. Here we report a high-performance supercapacitor electrode of manganese oxide/reduced graphene oxide nanocomposite coated on flexible carbon fiber paper (MnO₂–rGO/CFP). MnO₂–rGO nanocomposite was produced using a colloidal mixing of rGO nanosheets and 1.8 ± 0.2 nm MnO₂ nanoparticles. MnO₂–rGO nanocomposite was coated on CFP using a spray-coating technique. MnO₂–rGO/CFP exhibited ultrahigh specific capacitance and stability. The specific capacitance of MnO₂–rGO/CFP determined by a galvanostatic charge–discharge method at 0.1 A g⁻¹ is about 393 F g⁻¹, which is 1.6-, 2.2-, 2.5-, and 7.4-fold higher than those of MnO₂–GO/CFP, MnO₂/CFP, rGO/CFP, and GO/CFP, respectively. The capacity retention of MnO₂–rGO/CFP is over 98.5% of the original capacitance after 2000 cycles. This electrode has comparatively 6%, 11%, 13%, and 18% higher stability than MnO₂–GO/CFP, MnO₂/CFP, rGO/CFP, and GO/CFP, respectively. It is believed that the ultrahigh performance of MnO₂–rGO/CFP is possibly due to high conductivity of rGO, high active surface area of tiny MnO₂, and high porosity between each MnO₂–rGO nanosheet coated on porous CFP. An as-fabricated all-solid-state prototype MnO₂–rGO/CFP supercapacitor (2 × 14 cm) can spin up a 3 V motor for about 6 min.     

(010) facets dominated LiFePO4 nano-flakes confined in 3D porous graphene network as a high-performance Li-ion battery cathode

Olivine-structured LiFePO₄ (LFP) has been widely considered as one of the most promising and safest high-power positive electrode materials for lithium-ion batteries (LIBs) as a power source in the electric transportation. However, the electrochemical behavior of LFP for lithium-storage is seriously restrained by its intrinsic feature of low electrical conductivity and poor lithium-ion diffusion ability. In this research, LFP nano-flakes with oriented (010) facets were prepared through the solvothermal method, and 3D porous composite of LFP nano-flakes confined on graphene (LFP@G) was synthesized by freeze-drying concentrated graphene-oxide-gel containing LFP nano-flakes followed by a heat-treatment process. As the cathode materials for LIBs, LFP@G composite can release a reversible specific capacity of 129 mAh g^?1 at a high current rate of 20?C. Meanwhile, a long cycling stability for LFP@G composite with a capacity of 139.8 mAh g^?1 over 600 cycles up to 10?C can be achieved. The superior electrochemical Li-storage properties of LFP@G composite can be ascribed to the fast lithium-ion transfer channels of LFP originated from the exposed (010) planes, shortened lithium-ion diffusion distance, and the excellent two-phase electric contact between LFP and graphene in the 3D porous graphene conductive network for fast electron and lithium-ion transport.     

Zn–Mn-ptcda derived two-dimensional leaf-like Zn0·697Mn0·303Se/C composites as anode materials for high-capacity Li-ion batteries

As the most widely used energy storage device today, lithium-ion batteries (LIBs) will determine the convenience and durability of people's future energy life to a certain extent. At present, there are many and mature researches on cathode materials for LIBs, so it is crucial to seek a high-performance anode material. In recent years, due to considerable theoretical capacity, abundant raw material reserves and unique physicochemical properties, Zn and Mn selenium compounds have become research hotspots for LIBs anode materials. In this work, a new MOF material Zn–Mn-ptcda was synthesized by a simple hydrothermal reaction. Using Zn–Mn-ptcda as the precursor, two-dimensional (2D) elliptical leaf-shaped Zn_0·697Mn_0·303Se/C composites were synthesized by direct selenization. Zn_0.697Mn_0.303Se/C has a large specific surface area of 213.9 m² g^?1, belongs to the mesoporous structure, and possesses excellent lithium storage performance, especially the rate performance. It has a reversible capacity of 1005.14 mAh g^?1 after 110 cycles at a current density of 100 mA g^?1. After 1000 cycles at a high current density of 1 A g^?1, it still maintains a good capacity of 653.79 mAh g^?1.     

Synthesis of Heterogeneous Li<Subscript>4</Subscript>Ti<Subscript>5</Subscript>O<Subscript>12</Subscript> Nanostructured Anodes with Long-Term Cycle Stability

The 0D-1D Lithium titanate (Li₄Ti₅O₁₂) heterogeneous nanostructures were synthesized through the solvothermal reaction using lithium hydroxide monohydrate (Li(OH)·H₂O) and protonated trititanate (H₂Ti₃O₇) nanowires as the templates in an ethanol/water mixed solvent with subsequent heat treatment. A scanning electron microscope (SEM) and a high resolution transmission electron microscope (HRTEM) were used to reveal that the Li₄Ti₅O₁₂ powders had 0D-1D heterogeneous nanostructures with nanoparticles (0D) on the surface of wires (1D). The composition of the mixed solvents and the volume ratio of ethanol modulated the primary particle size of the Li₄Ti₅O₁₂ nanoparticles. The Li₄Ti₅O₁₂ heterogeneous nanostructures exhibited good capacity retention of 125 mAh/g after 500 cycles at 1C and a superior high-rate performance of 114 mAh/g at 20C.     

Boosted sodium storage of GeS2/GeO2/ZnS composite via heterostructure engineering

Transition metal dichalcogenides exhibit tremendous potential for sodium ion batteries (SIBs), owing to the outstanding specific capacity and aboundant reserves. However, the large ionic radius of sodium and poor conductivity often result in the fast decaying performance and inferior reaction kinetics. Herein, the GeS₂/GeO₂/ZnS@rGO (GGZ/C) ternary metal-based composite is fabricated as an anode material for SIBs. Notably, the GGZ/C composite is derived from the phase transformation of Zn₂GeO₄ precursor, which is beneficial for the heterostructure engineering. In this hierarchical structure, the metal phases ZnS and GeO₂ are used to form the heterogeneous framework, while graphene is applied to build a conductive network and anchor the host nanoparticles. Therefore, the great Na⁺ diffusion channels are achieved by the rational design of the huge exquisite interfaces among the heterogeneous mixed phases. Notably, it can almost completely relieve the volume expansion and restrain the internal stress of GGZ/C composite, providing the excellent structural tolerance. As expected, the GGZ/C composite exhibits excellent rate capability, with an impressive reversible capacity of 548 mAh g⁻¹ at a high rate of 5.0 A g⁻¹. Meanwhile, the GGZ/C also displays outstanding cycling performance with a specific capacity of 519 mAh g⁻¹ after 650 cycles at high rate of 5.0 A g⁻¹. This strategy offers the inspiration for rational heterostructure engineering for the energy storage materials with excellent reversible capacity and large volume variation.     

Synthesis of Si/Fe2O3-Anchored rGO Frameworks as High-Performance Anodes for Li-Ion Batteries

By virtue of the high theoretical capacity of Si, Si-related materials have been developed as promising anode candidates for high-energy-density batteries. During repeated charge/discharge cycling, however, severe volumetric variation induces the pulverization and peeling of active components, causing rapid capacity decay and even development stagnation in high-capacity batteries. In this study, the Si/Fe₂O₃-anchored rGO framework was prepared by introducing ball milling into a melt spinning and dealloying process. As the Li-ion battery (LIB) anode, it presents a high reversible capacity of 1744.5 mAh g⁻¹ at 200 mA g⁻¹ after 200 cycles and 889.4 mAh g⁻¹ at 5 A g⁻¹ after 500 cycles. The outstanding electrochemical performance is due to the three-dimensional cross-linked porous framework with a high specific surface area, which is helpful to the transmission of ions and electrons. Moreover, with the cooperation of rGO, the volume expansion of Si is effectively alleviated, thus improving cycling stability. The work provides insights for the design and preparation of Si-based materials for high-performance LIB applications.     

V2O3/rGO composite as a potential anode material for lithium ion batteries

V₂O₃ is a promising anode material and has attracted the interests of researchers because of its high theoretical capacity of 1070?mAh?g^?1, low discharge potential, inexpensiveness, abundant sources, and environmental friendliness. However, the development and application of V₂O₃ have been hindered by the low conductivity and drastic volume change of V₂O₃ composites. In this work, V₂O₃/reduced graphene oxide (rGO) nanocomposites are successfully prepared through a facile solvothermal method and annealing process. In this synthesis protocol, V₂O₃ nanoparticles (NPs) are encapsulated by rGO. This unique structure enables rGO to inhibit volume changes and improve the ion and electronic conductivity of V₂O₃. In addition, V₂O₃ NPs, which exhibit sizes of 5–40?nm, are uniformly dispersed on rGO sheets without aggregation. The Li⁺ storage behavior of V₂O₃/rGO is systematically investigated in the potential range 0.01–3.0?V. The V₂O₃/rGO nanocomposite can achieve a high reversible specific capacity of 823.4?mAh?g^?1 under the current density of 0.1?A?g^?1, and 407.3 mAh g^?1 under the high current density of 4.0?A?g^?1. The results of this study provide insight into the fabrication of rGO-based functional materials with extensive applications.     

Growth of titania and tin oxide from Ti2SnC via rapid thermal oxidation in air for lithium-ion battery application

Herein, we report the synthesis of TiO₂–SnO₂–C/carbide hybrid electrode materials for Li-ion batteries (LIBs) via two different methods of controlled oxidation of layered Ti₂SnC. The material was partially oxidized in an open-air furnace (OAF) or using a rapid thermal annealing (RTA) approach to obtain the desired TiO₂–SnO₂–C/carbide hybrid material; the carbide phase encompassed both residual Ti₂SnC and TiC as a reaction product. We tested the oxidized materials as an anode in a half cell to investigate their electrochemical performance in LIBs. Analysis of the various oxidation conditions indicated the highest initial lithiation capacity of 838 mAh/g at 100 mA/g for the sample oxidized in the OAF at 700°C for 1 h. Still, the delithiation capacity dropped to 427 mAh/g and faded over cycling. Long-term cycling demonstrated that the RTA sample treated at 800°C for 30 s was the most efficient, as it demonstrated a reversible capacity of around 270 mAh/g after 150 cycles, as well as a specific capacity of about 150 mAh/g under high cycling rate (2000 mA/g). Given the materials’ promising performance, this processing method could likely be applied to many other members of the MAX family, with a wide range of energy storage applications.