• 专利标题:   Preparing graphene titanium carbide cross-linked thin film material used as a self-supporting electrode, involves chemical etching raw material MAX phase by lithium fluoride and hydrochloric acid, reacting under heating condition, washing, oscillation peeling and centrifugal separation.
  • 专利号:   CN115763087-A
  • 发明人:   YANG J, CHENG Q
  • 专利权人:   UNIV BEIHANG
  • 国际专利分类:   H01G011/22, H01G011/26, H01G011/36, H01G011/86
  • 专利详细信息:   CN115763087-A 07 Mar 2023 H01G-011/22 202326 Chinese
  • 申请详细信息:   CN115763087-A CN11519772 30 Nov 2022
  • 优先权号:   CN11519772

▎ 摘  要

NOVELTY - Preparing graphene titanium carbide crosslinked film material, comprises (1) chemically etching MAX phase of raw material by lithium fluoride and hydrochloric acid, reacting, preparing into single-layer MXene nanosheet aqueous dispersion by washing, vibration stripping and centrifuging, (2) reacting raw graphite powder with concentrated sulfuric acid and potassium permanganate and preparing into single-layer graphene oxide (GO) nanosheets, (3) stirring and reacting single-layer MXene nanosheet aqueous dispersion with single-layer graphene oxide nanosheet aqueous dispersion obtaining MXene nanosheet and graphene oxide nanosheet uniform dispersion, (4) concentrating MXene nanosheet and graphene oxide nanosheet homogeneous dispersion liquid, and (5) preapring graphene oxide titanium carbide MXene hydrogel film into graphene oxide titanium carbide with water by continuous vacuum filtration, washing with detergent, crosslinking and drying. USE - The method is useful for preparing graphene carbide cross-linked composite film used as a self-supporting electrode (claimed). ADVANTAGE - The method ensures that the composite film achieves interfacial synergy effects of graphene and titanium carbide MXene covalent bonds and ππ interactions, has a tensile strength of up to 1.63GPa and an electrical conductivity of 1423 S/cm, the volume specific capacity of the film is as high as 1382 F/cm3, the volumetric energy density of the asymmetric supercapacitor prepared with the thin film as a self-supporting cathode reaches 47.62 mWh/cm3. DETAILED DESCRIPTION - Preparing graphene titanium carbide crosslinked film material, comprises (1) chemically ethcing the MAX phase of raw material by lithium fluoride and hydrochloric acid, reacting under heating conditions, and preparing into a single-layer MXene nanosheet aqueous dispersion through the steps of washing, vibration stripping and gradient centrifugation, preferably, the MAX phase is titanium aluminum carbide, preferably, the MXene is Ti3C2Tx; preferably, the diameter of the single-layer MXene nanosheet is 5-30 microns, (2) reacting the raw graphite powder with concentrated sulfuric acid and potassium permanganate with a mass fraction of 98 wt.% at low temperature, and preparing into single-layer graphene oxide nanosheets after washing and gradient centrifugation water dispersion, preferably, the low temperature is -5℃ to 10℃; preferably, the diameter of the single-layer graphene oxide nanosheet is 5-30 microns, (3) stirring and reacting single-layer MXene nanosheet aqueous dispersion with single-layer graphene oxide nanosheet aqueous dispersion to obtain MXene nanosheet and graphene oxide nanosheet uniform dispersion, (4) concentrating MXene nanosheet and graphene oxide nanosheet homogeneous dispersion liquid to obtain graphene oxide titanium carbide MXene hydrogel, preferably, the concentration means is suction filtration and/or centrifugation, (5) preparing graphene oxide titanium carbide MXene hydrogel obtained into a hydrogel film with a thickness of 50-3000 microns on a flexible porous substrate, preferably, the film forming process includes suction filtration, cast film forming, doctor blade coating or centrifugal casting; preferably, the flexible porous substrate is a mixed cellulose ester filter membrane, (6) preparing the graphene oxide titanium carbide MXene hydrogel film into graphene oxide titanium carbide with limited water support by continuous vacuum filtration until the film presents a metallic luster MXene film, preferably, the Herman orientation factor i.e. parameter used to characterize the degree of film orientation of the graphene oxide titanium carbide MXene film is 0.830-0.901, preferably 0.87-0.901; preferably, the porosity of described graphene oxide titanium carbide MXene film is 5.36-18.71%, (7) reducing graphene oxide titanium carbide MXene thin film with reducing agent, obtaining graphene carbide titanium carbide MXene thin film, preferably, the reducing agent is hydroiodic acid, and (8) washing graphene titanium carbide MXene film with a detergent and replacing by a displacing agent, soaking in a crosslinking agent solution for crosslinking, drying, and making into a graphene titanium carbide crosslinked film, preferably thin film material, preferably, the detergent is absolute ethanol, and the displacing agent is N,N-dimethylformamide (DMF); the crosslinking agent is N,N-dimethylformamide solution of pyrene butyric acid N-carboxysuccinimide ester (PSE) and N,N-dimethylformamide solution.