29 results about "Electrochemical intercalation" patented technology

The invention belongs to the technical field of graphene material preparation, and particularly relates to a universal electrochemical preparation method of covalent functionalized graphene (CFG), which comprises the following steps: (1) in an oil seal state of light sealing oil, performing electrochemical intercalation treatment on a graphite electrode by using concentrated sulfuric acid; (2) after intercalation is completed, light sealing oil is injected into the electrolytic bath while concentrated sulfuric acid is discharged; (3) in the electrolytic bath, constructing a micro-liquid membrane reaction zone by using density and intermiscibility differences of three working liquids, namely light sealing oil, aqueous electrolyte and heavy sealing oil, and enabling the micro-liquid membrane reaction zone to be in contact with the intercalated graphite electrode to generate electrochemical oxidation to generate CFG; (4) controlling the micro-liquid membrane reaction area to directionally move relative to the intercalated graphite electrode, so that the whole intercalated graphite electrode is gradually and completely converted into CFG; and (5) putting the CFG structure after the reaction into a solvent, carrying out mechanical stripping to prepare a dispersion liquid of CFG, and drying to obtain CFG powder.

The invention discloses a graphene oxide sheet long-afterglow material and a preparation method and application thereof.The preparation method of the graphene oxide sheet long-afterglow material comprises the steps that a graphite oxide electrode sheet serves as a working electrode, and the working electrode, a counter electrode and a reference electrode are immersed in electrolyte; direct current is applied through an electrochemical workstation, so that the voltage difference between the working electrode and the reference electrode is 1.8-2.0 V, an electrochemical reaction circuit is formed, electrochemical reaction is carried out until the current in a loop where the working electrode and the counter electrode are located is smaller than or equal to 1 mA, the electrochemical reaction is stopped, and the electrolyte is a saturated boric acid aqueous solution. According to the invention, through electrochemical intercalation and oxygen evolution reaction, the graphite oxide electrode plate is stripped from the graphene oxide sheet and is simultaneously compounded with the boric acid crystal in situ, so that the graphene oxide sheet long-afterglow material is directly obtained in one step, and the danger of a traditional method and the redundancy of multi-step preparation are eliminated.

The invention discloses a method for extracting lithium from gas field produced water based on an electrochemical intercalation method. The method comprises the following steps: (1) pretreatment; (2) the pretreated gas field produced water serves as electrolyte to enter an electrolytic bath for lithium adsorption; (3) replacing the electrolyte with an eluent, exchanging the positive electrode and the negative electrode of a power supply of the electrolytic cell, and desorbing lithium under the action of a reverse electric field; (4) collecting the desorbed lithium ion solution, concentrating, adding a sodium carbonate solution or directly adding sodium carbonate, stirring at 60-65 DEG C, filtering, washing with water, and drying to obtain lithium carbonate; and (5) taking the liquid obtained by filtering in the step (4) as electrolyte, and repeating the steps (2)-(4) for 0-4 times. By utilizing an electrochemical intercalation method, the lithium ions in the gas field produced water can be efficiently and selectively separated, the lithium ion recovery rate is high, and the cost is low.

The application belongs to the technical field of graphene material preparation, and particularly relates to a general covalent functionalized graphene (CFG) electrochemical preparation method, which comprises the following steps: (1) under the condition of a light sealing oil seal, graphite electrodes are subjected to electrochemical intercalation treatment by using concentrated sulfuric acid; (2) after the intercalation is completed, light sealing oil is injected into an electrolytic cell while the concentrated sulfuric acid is discharged; (3) in the electrolytic cell, a micro-liquid film reaction zone is constructed by using the density and phase solubility difference of the light sealing oil, the aqueous electrolyte and the heavy sealing oil, and the micro-liquid film reaction zone is contacted with the intercalated graphite electrode to make the intercalated graphite electrode electrochemically oxidized to generate CFG; (4) by controlling the relative intercalated graphite electrode of the micro-liquid film reaction zone to move directionally, the whole intercalated graphite electrode is gradually and completely converted into CFG; (5) the CFG structure after the reaction is placed into a solvent to be mechanically exfoliated to prepare a CFG dispersion liquid, and the CFG powder is obtained after drying treatment.

This invention relates to the field of graphene preparation technology and provides a method for preparing low-defect graphene powder using a high-temperature molten salt intercalation and instantaneous expansion method. First, a graphite / molten salt composite electrode is prepared. Then, salt is intercalated into the graphite using an electrochemical intercalation method. Finally, the intercalated graphite is exfoliated into thin-layer graphene using a negative pressure high-power microwave exfoliation method or a normal pressure high-temperature quenching exfoliation method. The raw materials used in this invention are low-cost and environmentally friendly, and the production process is safe and efficient. Through the optimized combination of molten salt electro-assisted intercalation technology and the instantaneous expansion method, the prepared graphene not only has a layer count controlled at 3-5 layers and a flake size of 25-300 μm, but also exhibits few defects on the graphene flakes, providing strong technical support for promoting the high-quality development of related industries.

The invention belongs to the technical field of two-dimensional material preparation, and particularly relates to a preparation method of a Zr2N2X two-dimensional material. The preparation method comprises the following steps: firstly, by taking layered ZrNCl as a working electrode, applying constant current into an electrolyte containing organic ammonium salt, and carrying out electrochemical intercalation reaction to prepare an intercalated ZrNCl two-dimensional nanosheet; and mixing the ZrNCl subjected to electrochemical intercalation treatment with anhydrous Na2X (X = S, Se or Te), carrying out sealed reaction in a protective atmosphere, and carrying out solid-phase topological chemical conversion to generate the Zr2N2X two-dimensional material. Through the synergistic effect of electrochemical intercalation pretreatment and topological chemical conversion, the harsh degree of reaction conditions is reduced, meanwhile, the product quality and the process controllability are comprehensively improved, and a solid foundation is laid for industrial application of the two-dimensional semiconductor material.

The utility model relates to the technical field of graphene preparation, and discloses a device for preparing graphene by electrochemical intercalation, which comprises an electrolytic tank, an electrochemical intercalation layer, a first electrode, a second electrode, a third electrode and a fourth electrode, the electrolytic tank is of a square open structure, and the bottom of an inner cavity of the electrolytic tank is funnel-shaped; the top of the filter box is communicated with the electrolytic tank through a connecting pipe; the stirring assembly comprises a rotating shaft which is transversely and rotationally connected to the interior of the electrolytic tank, the rotating shaft is of a hollow structure, and stirring rods are arranged on the outer portion of the rotating shaft at equal intervals in the circumferential direction; the anti-blocking collecting assembly comprises a filter plate, the filter plate is horizontally arranged, and filter holes penetrating through the filter plate are uniformly formed in the surface of the filter plate; the rotating rod is transversely arranged and rotationally connected to the lower portion of the center of the filter plate, eccentric wheels are symmetrically and fixedly arranged on the outer portion of the rotating rod in a sleeving mode, the graphene electrolysis rate can be increased, graphene can be conveniently collected, and practicability is high.

The invention provides a large-size monoclinic phase VO2 nanosheet or film and a preparation method and application thereof.The preparation method comprises the steps that VCl3 and V2O3 serve as raw materials, and VOCl single crystals are prepared through a chemical vapor transport method; the method comprises the following steps: tabletting a VOCl single crystal to obtain a VOCl single crystal wafer, and performing electrochemical intercalation stripping in an organic salt electrolyte by taking the VOCl single crystal wafer as a cathode and platinum as a counter electrode to obtain a VOCl single-layer nanosheet; the preparation method comprises the following steps: dispersing VOCl single-layer nanosheets in a polar organic solvent, dripping the obtained solution on a substrate material, and drying; or dripping the obtained solution on an organic filter membrane, carrying out suction filtration to obtain a VOCl thin film, transferring the VOCl thin film to a substrate material, and drying; and carrying out annealing treatment on the VOCl single-layer nanosheet or the VOCl thin film. The thicknesses of the VO2 nanosheet and the thin film can be adjusted, the thinnest thickness can be within 1nm, and the transverse sizes of the VO2 nanosheet and the thin film can be more than tens of microns and 500 microns respectively.

The present invention discloses a graphene oxide composite material, a preparation method thereof and an application. The preparation method includes the following steps: using graphite as the anode and a platinum sheet as the cathode, preparing intercalated graphite by an electrochemical intercalation method; using the intercalated graphite as the anode and a platinum sheet as the cathode, and using Eaton's reagent as the electrolyte, preparing a graphene oxide dispersion by an electrochemical oxidation and exfoliation method; mixing the graphene oxide dispersion and a polymer monomer uniformly, and carrying out in-situ polymerization on the obtained reaction solution to prepare the graphene oxide composite material. The method of the present invention can fully exert the excellent properties of GO in the composite material, and significantly improve the mechanical properties and electrochemical properties of the composite material. This process omits a large number of cumbersome processes such as washing and drying of graphene oxide, enables graphene oxide to always maintain a few-layer or even single-layer morphology so as to achieve the best modification effect, and avoids the problem of agglomeration of graphene oxide caused by physical blending, which reduces the performance of the composite material.

A membrane-stacked electrolytic bath for lithium extraction from salt lakes by electrochemical intercalation / deintercalation includes a positioning supporting plate as well as a first compressing plate, a first rubber gasket, at least one electrochemical intercalation / deintercalation unit, a second rubber gasket, and a second compressing plate which are sequentially arranged in an overlapped manner; a compressing apparatus for abutting against the second compressing plate is arranged on one side of the second compressing plate to enable peripheral edges of the first compressing plate, the first rubber gasket, the electrochemical intercalation / deintercalation unit, the second rubber gasket, and the second compressing plate to be sealed; the first compressing plate is provided with water outlet pipes communicated with the electrochemical intercalation / deintercalation unit; and the second compressing plate is provided with water inlet pipes communicated with the electrochemical intercalation / deintercalation unit.

The present application discloses an electrode material for extracting lithium from salt lakes by an electrochemical insertion / extraction method, a preparation method thereof, and an application thereof. The electrode material includes a core and a shell layer coated on the surface of the core. The core includes lithium iron phosphate, and the shell layer includes vanadium dioxide. By coating vanadium dioxide on the surface of the lithium iron phosphate material in the present application, after performing the lithium extraction operation, the electrolyte is heated to 68 - 90 °C and then the de-lithiation step is carried out, which can improve the conductivity of the electrode, increase its current density, so that the embedded lithium ions are accelerated to escape into the electrolyte, and the lithium extraction efficiency is improved.

The invention discloses a method for preparing graphene by polyacid intercalation, wherein a graphite sheet is used as a working electrode and a platinum sheet is used as a counter electrode, a constant voltage is applied, and electrochemical intercalation is performed in a sulfuric acid solution, and sulfuric acid molecules are intercalated into the graphite interlayer under the driving of an electric field to obtain a graphite intercalation compound; the obtained graphite intercalation compound is ground, and the bottom product is collected by centrifugation after being fully mixed with a phosphoric acid solution; concentrated phosphoric acid is added to the bottom product and heated, and then a sodium tungstate solution is added to fully react and generate polyacids between graphite layers; the product after the reaction is washed with deionized water for several times, the washed product is redispersed in a dispersant, and the product is allowed to stand after ultrasound to obtain a graphene dispersion; the supernatant of the graphene dispersion after standing is taken, filtered, washed, and dried to obtain graphene. The method of the invention can synthesize high-quality graphene in a short time, and the obtained graphene has a large size, a small number of layers, and an extremely low oxygen content.

Methods for synthesizing layered lithium transition metal oxides from layered sodium transition metal oxides are provided. Also provided are electrodes for lithium-ion batteries that include the layered lithium transition metal oxides. Similarly, methods for the synthesis of layered sodium transition metal oxides from layered lithium transition metal oxides and electrodes for sodium-ion batteries that include the layered sodium transition metal oxides are provided. The methods couple electrochemical intercalation of alkali ions (Li+ or Na+) with ion-exchange to overcome the kinetic limitation of ion-exchange in the layered alkali transition metal oxides at low vacancy concentrations.

The application relates to the technical field of graphene preparation, and discloses a method for preparing high-conductivity graphene sheet layers through electrochemical intercalation. The steps include: preparing a composite intercalation electrolyte composed of soluble ferric salt and organic alcohol compound; constructing a reaction system by taking graphite as an anode and an inert electrode as a cathode; performing electrochemical intercalation and peeling through a staged voltage composed of a first direct current voltage and a second direct current voltage, wherein the first direct current voltage is determined according to a linear sweep voltammetry method; stirring is kept during the reaction process, and the product is collected to obtain a graphene sheet layer primary dispersion liquid; subsequently, the dispersion liquid is subjected to standing and centrifugal post-treatment, and the obtained graphene sheet layer can be optionally subjected to two-stage heat treatment to further strengthen the conductivity. The application realizes efficient and controllable peeling and synchronous in-situ repair of graphene, and the prepared graphene sheet layer has few defects and significantly improved conductivity.

The present disclosure provides methods of producing isolated graphene sheets from graphite. Isolated graphene sheets produced by said methods, as well as articles and devices containing said isolated graphene sheets, are also provided. Electrochemical intercalation reactors for performing said methods are also provided.

This invention discloses a method for the electrochemical preparation of amorphous hydroxyferric phosphate electrode materials. The method uses ferric phosphate as a raw material to prepare the working electrode. Then, in an aqueous three-electrode system, an electrochemical method is used to induce periodic intercalation and deintercalation of metal ions to drive the collapse and rearrangement of the ferric phosphate lattice. Simultaneously, the hydroxyl groups in the aqueous electrolyte replace the phosphate groups in the ferric phosphate under the drive of the electrochemical intercalation and deintercalation reaction, thereby achieving the preparation of the amorphous hydroxyferric phosphate electrode material. This invention uses an electrochemical method for in-situ conversion to prepare amorphous hydroxyferric phosphate, eliminating the need for high-temperature, high-pressure hydrothermal reactions. The process is simple, requires minimal equipment, and the controllable synthesis of amorphous hydroxyferric phosphate can be achieved by adjusting the electrochemical parameters.

The invention belongs to the field of new energy electrocatalytic materials, and particularly relates to a preparation method and application of an iron-loaded electron-rich black phosphorus nanosheet electrocatalyst, S1, tetrabutylammonium bromide and iron salt are dissolved in an acetonitrile solvent to obtain an electrolyte; s2, taking the black phosphorus block as a cathode and a platinum sheet as an anode, immersing the black phosphorus block and the platinum sheet in an electrolyte, and applying voltage by adopting a direct-current power supply to carry out electrochemical intercalation and stripping; and S3, carrying out ultrasonic treatment, washing and vacuum drying on the solution obtained in the step S2 to obtain the iron-loaded electron-rich black phosphorus nanosheet electrocatalyst. The invention also provides an application of the iron-loaded electron-rich black phosphorus nanosheet electrocatalyst prepared by the preparation method in electrocatalytic water desorption and oxygen desorption in an alkaline electrolyte. The catalytic material shows excellent electro-catalytic oxygen evolution activity and good catalytic stability in alkaline electrolyte.

The application relates to the technical field of graphene, in particular to a graphene material and a preparation method and a preparation device thereof, the preparation method comprises the following steps: preparing an electrolysis system, including an anode, a cathode and an electrolyte, a first extension direction of the anode intersects with a second extension direction of the cathode; graphite is used as the anode to perform an electrolysis reaction, and the graphite is driven to move along the first extension direction to adjust the distance between the anode and the cathode; as the distance between the anode and the cathode decreases, the current density on the surface of the graphite gradually increases; the graphite is first subjected to electrochemical intercalation and then subjected to electrolytic exfoliation to obtain a graphene dispersion liquid; the graphene dispersion liquid is subjected to purification treatment to obtain graphene. In the preparation method, the electrochemical intercalation and the electrolytic exfoliation reaction on the graphite are performed in sequence, the prepared graphene material has a high few-layer (carbon layer number is less than or equal to 5) rate, and the types and contents of oxygen-containing functional groups can be controlled.

The invention provides a preparation method and application of a metal-free high-temperature ferromagnetic material and a device, the high-temperature ferromagnetic material is obtained by inserting organic free radical molecules into two-dimensional material layers by using an electrochemical intercalation method, and the organic free radical molecules are pyraline, 7, 7, 8, 9-tetramethyl-3-piperidine, 7, 7, 8, 10-tetramethyl-3-piperidine, 7, 7, 8, 10-tetramethyl-3-piperidine, 7, 8, 10-tetramethyl-3 the two-dimensional material is any one or more of 1, 3, 4, 5, 6, 7, 8-tetracyano-p-benzoquinone dimethane (TCNQ), naphthoquinone (NTO) and hydroquinone, and the two-dimensional material is any one of graphene or molybdenum disulfide. By changing the molecular / two-dimensional material, a series of metal-free molecular intercalation material systems with high magnetism and high Curie temperature are realized; a material synthesis approach for controlling the magnetic difference by changing the carrier concentration of a molecular / two-dimensional material system is realized, and new development of organic / metal-free spin electronic devices and magnetoresistive devices is extended.

A method for preparing graphene by formic acid electrochemical intercalation and ultrasonic exfoliation belongs to the field of graphene preparation technology. The method includes the following steps: using graphite material as the working electrode, immersing it in a high-concentration formic acid aqueous solution as the electrolyte and intercalating agent, applying a constant voltage to carry out an electrochemical intercalation reaction, obtaining an expanded graphite intercalation precursor; washing and drying the precursor, dispersing it in a liquid medium, and performing ultrasonic exfoliation treatment to obtain a graphene dispersion; finally, obtaining the graphene material through solid-liquid separation and drying. This invention uses formic acid as the intercalation medium, avoiding the use of traditional strong acids and oxidants, significantly improving the cleanliness of the process. The combination of mild electrochemical intercalation conditions and subsequent ultrasonic treatment achieves efficient exfoliation of graphene and high fidelity of the lattice structure. The prepared graphene material has low defect density and excellent structural integrity and intrinsic properties. This invention has a simple process flow, mild operating conditions, and is environmentally friendly, suitable for the large-scale preparation of high-quality graphene.

This application relates to an electrode material, its preparation method, and its application in direct lithium extraction from salt lakes via electrochemical intercalation / deintercalation. The preparation method includes the following steps: (1) mixing mesoporous silica, a lithium source, an iron source, a phosphorus source, and a solvent, and performing a solvothermal reaction to obtain a mixture; (2) heating the obtained mixture to obtain a lithium iron phosphate composite; (3) mixing a coating material and the obtained lithium iron phosphate composite, and calcining to obtain the electrode material. The porous lithium iron phosphate ion sieve based on silica utilizes mesoporous silica as its core, which, compared to the difficult-to-form porous lithium iron phosphate core, possesses abundant pores, improving the porosity of the ion sieve and further enhancing mass transfer efficiency.

The invention belongs to the technical field of two-dimensional new materials, and particularly relates to a metal organic-MXenes material with controllable superconducting property and a preparation method thereof. The metal organic-MXenes material with the controllable superconducting property comprises sheet-shaped MXenes which are distributed in a layered mode and an organic metal compound which is perpendicular to the space between sheet layers of the sheet-shaped MXenes. The organic metal compound is a metallocene compound; the sheet-shaped MXenes are obtained by tabletting an MXene material; the MXene material is prepared by a wet chemical method or a Lewis acid molten salt method. An electrochemical intercalation strategy is utilized, effective intercalation of organic metal to the MXenes material is achieved, superconducting transformation of the MXenes is achieved through dimension reduction and electron injection, and the metal organic-MXenes material with the controllable superconducting property is obtained.

This invention discloses a long afterglow material of graphene oxide sheets, its preparation method, and its applications. The preparation method of the long afterglow material of graphene oxide sheets includes: using a graphene oxide electrode sheet as the working electrode, immersing the working electrode, counter electrode, and reference electrode in an electrolyte, applying direct current through an electrochemical workstation to make the voltage difference between the working electrode and the reference electrode 1.8~2.0V to form an electrochemical reaction circuit, and carrying out the electrochemical reaction until the current in the circuit containing the working electrode and counter electrode is ≤1mA, at which point the electrochemical reaction is stopped. The electrolyte is a saturated boric acid aqueous solution. This invention, through electrochemical intercalation and oxygen evolution reaction, allows the graphene oxide sheet to be exfoliated from the graphene oxide electrode sheet while simultaneously being in-situ composited with boric acid crystals, directly obtaining the long afterglow material of graphene oxide sheets in one step, thus avoiding the dangers and multi-step complexity of traditional methods.

Methods for synthesizing layered lithium transition metal oxides from layered sodium transition metal oxides are provided. Also provided are electrodes for lithium-ion batteries that include the layered lithium transition metal oxides. Similarly, methods for the synthesis of layered sodium transition metal oxides from layered lithium transition metal oxides and electrodes for sodium-ion batteries that include the layered sodium transition metal oxides are provided. The methods couple electrochemical intercalation of alkali ions (Li+ or Na+) with ion-exchange to overcome the kinetic limitation of ion-exchange in the layered alkali transition metal oxides at low vacancy concentrations.

The invention relates to an MXenes aluminum-based composite wire with a layered structure and a preparation method of the MXenes aluminum-based composite wire, and belongs to the technical field of high-strength, high-conductivity and heat-resistant aluminum wires. The MXenes aluminum-based composite wire with the layered structure comprises long-strip crystal grains which are formed by stretching a MXenes aluminum-based composite material with the layered structure along a conductive direction, the long-strip crystal grain comprises a crystal boundary, a two-dimensional MXenes sheet layer and nano Al2O3 nano particles. Through an electrochemical intercalation-heat treatment modification process, a nano-aluminum coating layer is constructed on the surface of MXenes in situ, the technical problem of weak interface bonding of MXenes and an aluminum matrix is solved, and the obtained Al2O3 nano-particle and MXenes synergistically enhanced composite material wire with a multi-scale layered heterostructure shows excellent comprehensive performance and has good application prospects. The technical effects of high strength, high conductivity and high heat resistance are achieved.

The invention provides a 1T / 2H MoS2 homojunction nanosheet, a preparation method and application thereof, and a self-powered photoelectric detector, and belongs to the technical field of self-powered photoelectric detection. The invention provides a preparation method of a 1T / 2H MoS2 homojunction nanosheet, which comprises the following steps: carrying out electrochemical intercalation on block MoS2 to obtain an intercalation product; and sequentially carrying out ultrasonic stripping and cleaning on the intercalation product to obtain the 1T / 2H MoS2 homojunction nanosheet. According to the preparation method, the 1T / 2H MoS2 homojunction nanosheet is obtained by adopting electrochemical intercalation, ultrasonic stripping and cleaning, the stable 1T / 2H mixed-phase MoS2 nanosheet is obtained by a method of regulating and controlling voltage and retaining a small amount of organic matters and ions, and the prepared self-powered photoelectric detector can stably operate for a long time.

The invention relates to the field of preparation of expandable graphite, in particular to a low-energy-consumption green expandable graphite processing method which comprises the following steps: firstly, carrying out microwave irradiation treatment on natural flake graphite to generate thermal stress cracks; and then the treated graphite serves as an anode and is placed in a composite electrolyte for constant-voltage electrochemical intercalation treatment. The electrifying duration and the initial voltage are adjusted in real time by detecting the settling velocity and the interlayer spacing of the intercalated graphite. Then, the intercalated graphite reaching the standard is placed in an organic solvent to be subjected to solvent replacement and auxiliary ultrasonic treatment, wormlike precursor graphite is obtained, and the preheating power of microwave expansion equipment is adjusted according to the turbidity of the replaced solution; and finally, determining the expansion duration by detecting the specific surface area of the precursor graphite. According to the method, the problem that in the prior art, the product quality is unstable due to the fact that the low-energy-consumption green expandable graphite electrolyte is prone to being excessively oxidized is solved through the process parameter adjusting procedure for detecting the expandable graphite.

The invention discloses a method for electrochemically regulating and controlling a MoS2 structure through potassium and application. According to the method, an integrated MoS2-based flexible self-supporting hydrogen evolution catalytic electrode is constructed by adopting an electrostatic spinning combined hydrothermal synthesis technology. The potassium ion battery is assembled by using the self-supporting electrode as a negative electrode, and the MoS2 is subjected to electrochemical intercalation structure regulation and control by using the operation environment of the potassium ion battery. The MoS2-based flexible electrode disclosed by the invention shows ideal super-hydrophilic property and super-hydrophobic property. Meanwhile, the electrode has excellent HER performance, the overpotential of the electrode in 0.5 M H2SO4 electrolyte under the current density of 10 mA cm < 2 > is only 51 mV, and the corresponding Tafel value is 77 mV dec1. And meanwhile, the amorphous MoS2 electrochemically regulated and controlled by potassium ions has more active sites, and can provide more excellent HER electro-catalytic performance. In addition, a parallel carbon layer on the outer surface of MoSx not only provides a faster electron transfer approach, but also constructs H adsorption and HER micro limited areas. The electrode obtained by electrochemically regulating and controlling the MoS2 structure through potassium has an extremely high electrochemical application prospect.

The invention discloses a graphene composite lubricating additive and a preparation method thereof.The preparation method comprises the steps that a graphite rod serves as an anode, molybdenum disulfide serves as a cathode, and electrochemical intercalation is conducted in a fluorine-containing electrolyte solution; the mixture obtained through electrolysis is subjected to high-pressure homogenization treatment, and stripping and superfine grinding are achieved; and after washing and freeze-drying, calcining in an inert atmosphere to finally obtain the product. The preparation of nano graphene and molybdenum disulfide, fluorine functional group surface modification and composite assembly are realized in one step through a synergistic process of electrochemical intercalation, high-pressure homogenization and calcination; the method is simple in process, green, environment-friendly and pollution-free; in the prepared composite lubricating additive, the molybdenum disulfide nanosheets are loaded on the surface of the fluorine-functionalized graphene, the molybdenum disulfide nanosheets and the fluorine-functionalized graphene have a synergistic effect, and the obtained additive has excellent friction performance and high temperature resistance and is suitable for lubrication under severe working conditions such as high speed, heavy load and high temperature.