WO2024082290A1 - Carbure de titane et son utilisation, procédé de préparation, batterie secondaire et dispositif électrique - Google Patents

Carbure de titane et son utilisation, procédé de préparation, batterie secondaire et dispositif électrique Download PDF

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WO2024082290A1
WO2024082290A1 PCT/CN2022/126796 CN2022126796W WO2024082290A1 WO 2024082290 A1 WO2024082290 A1 WO 2024082290A1 CN 2022126796 W CN2022126796 W CN 2022126796W WO 2024082290 A1 WO2024082290 A1 WO 2024082290A1
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titanium carbide
secondary battery
negative electrode
battery
present application
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PCT/CN2022/126796
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English (en)
Chinese (zh)
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赵欣
王国宝
王文轩
严涵
曹娇
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宁德时代新能源科技股份有限公司
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Priority to PCT/CN2022/126796 priority Critical patent/WO2024082290A1/fr
Priority to CN202280089077.3A priority patent/CN118556304A/zh
Publication of WO2024082290A1 publication Critical patent/WO2024082290A1/fr

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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers

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  • the present application relates to the field of material technology, and in particular to titanium carbide and its use, preparation method, secondary battery and electrical device.
  • secondary batteries are widely used in energy storage power systems such as hydropower, thermal power, wind power and solar power stations, as well as power tools, electric bicycles, electric motorcycles, electric vehicles, military equipment, aerospace and other fields.
  • energy storage power systems such as hydropower, thermal power, wind power and solar power stations, as well as power tools, electric bicycles, electric motorcycles, electric vehicles, military equipment, aerospace and other fields.
  • secondary batteries have made great progress, higher requirements have been put forward for their energy density, cycle performance and safety performance.
  • the conductivity requirements for the conductive agent used in secondary batteries are getting higher and higher.
  • Titanium aluminum carbide (Ti 3 AlC 2 ) is a ternary layered compound of the MAX phase. It is a new type of metal ceramic functional material that has the excellent properties of both metals and ceramics.
  • hydrofluoric acid HF
  • HF hydrofluoric acid
  • Two-dimensional layered titanium carbide has superb electrochemical properties due to its unique morphology, large specific surface area and atomic-level layer thickness, and has been widely used in lithium-ion batteries, solar cells, etc. Therefore, obtaining a titanium carbide layer structure with a larger specific surface area and higher conductivity is the focus of current scientific researchers.
  • the present application is made in view of the above-mentioned problems, and its purpose is to provide a titanium carbide having an excellent two-dimensional graphene-like structure, a thinner sheet structure, a larger specific surface area and a higher conductivity; when used as a conductive agent for a secondary battery, it can improve the cycle performance of the corresponding battery.
  • the first aspect of the present application provides titanium carbide having a lamellar structure and an average thickness of a single layer of 1-8 nm.
  • the titanium carbide of the present application increases its specific surface area and thus its conductivity by limiting the sheet structure of a specific single layer average thickness. When it is used as a conductive agent for a secondary battery, it can improve the cycle performance of the corresponding battery.
  • the specific surface area of the titanium carbide is 75-90 m 2 /g.
  • the conductivity of the titanium carbide is further improved through the specific surface area, thereby improving the cycle performance of the corresponding battery.
  • the porosity of the titanium carbide is 75%-98.5%.
  • the specific surface area and conductivity of the titanium carbide are further improved, thereby improving the cycle performance of the corresponding battery.
  • the single layer resistivity of the titanium carbide is 80-115 S/cm.
  • the specific surface area and conductivity of the titanium carbide are further improved, thereby improving the cycle performance of the corresponding battery.
  • a second aspect of the present application provides a method for preparing titanium carbide, comprising:
  • step (2) mixing the titanium aluminum carbide obtained in step (1) with hydrofluoric acid, and then filtering to obtain a solid;
  • step (3) mixing the solid obtained in step (2) with a sulfoxide compound, and then drying to obtain the titanium carbide;
  • the method of the present application obtains titanium carbide with a lamellar structure by treating and drying with sulfoxide compounds.
  • the titanium carbide has a thinner thickness than conventional technologies, so that the titanium carbide has a larger specific surface area and higher conductivity, thereby improving the cycle performance of the corresponding battery.
  • step (3) the solid obtained in step (2) is stirred and mixed with the sulfoxide compound at a rotation speed of 100-150 rpm for 30-70 hours.
  • the specific surface area and conductivity of the obtained titanium carbide are further improved, thereby improving the cycle performance of the corresponding battery.
  • the weight ratio of the solid to the sulfoxide compound is 1:(6-15), optionally 1:(8-12).
  • the specific ratio of the solid to the sulfoxide compound further improves the specific surface area and conductivity of the obtained titanium carbide, thereby improving the cycle performance of the corresponding battery.
  • the drying comprises vacuum drying at a temperature of 80-120° C.
  • the specific surface area and conductivity of the obtained titanium carbide are further improved, thereby improving the cycle performance of the corresponding battery.
  • the sulfoxide compound is dimethyl sulfoxide.
  • the specific surface area and conductivity of the obtained titanium carbide are further improved, thereby improving the cycle performance of the corresponding battery.
  • the third aspect of the present application provides use of the titanium carbide described in the first aspect of the present application or the titanium carbide prepared according to the method described in the second aspect of the present application as a conductive agent for a secondary battery.
  • the conductive agent is used in a negative electrode film layer of a secondary battery.
  • the content of the conductive agent is 0.4%-1%, based on the total weight of the negative electrode film layer.
  • the fourth aspect of the present application also provides a secondary battery, characterized in that it comprises the titanium carbide described in the first aspect or the titanium carbide prepared according to the method described in the second aspect of the present application.
  • the obtained battery has good cycle performance.
  • a fifth aspect of the present application provides an electrical device, comprising the secondary battery of the fourth aspect of the present application.
  • the titanium carbide of the present application has a thinner average single-layer thickness, a larger specific surface area, and a higher conductivity; when used as a conductive agent for a secondary battery, it can improve the cycle performance of the battery.
  • FIG1 is a scanning electron microscope image of titanium carbide prepared in Example 1 of the present application; wherein FIG(b) is a partial enlarged view of FIG(a).
  • FIG. 2 is a schematic diagram of a secondary battery according to an embodiment of the present application.
  • FIG. 3 is an exploded view of the secondary battery according to the embodiment of the present application shown in FIG. 1 .
  • FIG. 4 is a schematic diagram of an electric device using a secondary battery as a power source according to an embodiment of the present application.
  • Secondary battery 51. Casing; 52. Electrode assembly; 53. Cover plate; 6. Electrical device.
  • “Scope” disclosed in the present application is limited in the form of lower limit and upper limit, and a given range is limited by selecting a lower limit and an upper limit, and the selected lower limit and upper limit define the boundary of a special range.
  • the scope limited in this way can include or exclude end values, and can be arbitrarily combined, that is, any lower limit can form a scope with any upper limit combination. For example, if the scope of 60-120 and 80-110 is listed for a specific parameter, it is understood that the scope of 60-110 and 80-120 is also expected.
  • the minimum range values 1 and 2 listed, and if the maximum range values 3,4 and 5 are listed, the following scope can be fully expected: 1-3, 1-4, 1-5, 2-3, 2-4 and 2-5.
  • the numerical range "a-b” represents the abbreviation of any real number combination between a and b, wherein a and b are real numbers.
  • the numerical range "0-5" represents that all real numbers between "0-5" have been fully listed herein, and "0-5" is just the abbreviation of these numerical combinations.
  • a parameter is expressed as an integer ⁇ 2, it is equivalent to disclosing that the parameter is, for example, an integer of 2, 3, 4, 5, 6, 7, 8, 9, 10, 11, 12, etc.
  • the method includes steps (a) and (b), which means that the method may include steps (a) and (b) performed sequentially, or may include steps (b) and (a) performed sequentially.
  • the method may further include step (c), which means that step (c) may be added to the method in any order.
  • the method may include steps (a), (b) and (c), or may include steps (a), (c) and (b), or may include steps (c), (a) and (b), etc.
  • the “include” and “comprising” mentioned in this application represent open-ended or closed-ended expressions.
  • the “include” and “comprising” may represent that other components not listed may also be included or only the listed components may be included or only the listed components may be included.
  • the term "or” is inclusive.
  • the phrase “A or B” means “A, B, or both A and B”. More specifically, any of the following conditions satisfies the condition "A or B”: A is true (or exists) and B is false (or does not exist); A is false (or does not exist) and B is true (or exists); or both A and B are true (or exist).
  • Titanium aluminum carbide (Ti 3 AlC 2 ) is a ternary layered compound of the MAX phase. It is a new type of metal ceramic functional material with excellent properties of both metals and ceramics.
  • hydrofluoric acid HF
  • HF hydrofluoric acid
  • Two-dimensional layered titanium carbide has superb electrochemical properties due to its unique morphology, large specific surface area and atomic-level layer thickness, and has been widely used in lithium-ion batteries, solar cells, etc. Therefore, obtaining a titanium carbide layer structure with a larger specific surface area and higher conductivity for application in secondary batteries is the focus of current scientific researchers.
  • the present application obtains titanium carbide with a thinner sheet structure through hydrofluoric acid corrosion and subsequent sulfoxide compound treatment.
  • the titanium carbide has an excellent two-dimensional graphene-like structure, a larger specific surface area and higher conductivity.
  • the titanium carbide can be used as a conductive agent in secondary batteries to improve the cycle performance of the corresponding batteries.
  • the first aspect of the present application provides titanium carbide having a lamellar structure, and an average thickness of a single layer is 1-8 nm, optionally 1-5 nm, and further optionally 1.5-2.5 nm.
  • the titanium carbide of the present application increases its specific surface area by limiting the sheet structure of a specific single-layer average thickness; and has abundant electronic groups, which increases its conductivity and reduces the occurrence of side reactions, thereby improving the cycle performance of the corresponding battery.
  • the thickness is measured using a scanning electron microscope, and the average thickness is the arithmetic mean of the thicknesses of 10 randomly selected single layers.
  • the maximum plane area of the titanium carbide layer is 300-800 nm 2 , preferably 400-600 nm 2 .
  • the specific surface area of the titanium carbide is further increased, thereby improving its conductivity and thus improving the cycle performance of the corresponding battery.
  • the specific surface area of the titanium carbide is 75-90 m 2 /g, preferably 85-90 m 2 /g, measured according to the gas adsorption BET method of GB/T 19587-2004.
  • the conductivity of the titanium carbide is further improved, thereby improving the cycle performance of the corresponding battery.
  • the porosity of the titanium carbide is 75%-98.5%.
  • the specific surface area and conductivity of the titanium carbide are further improved, thereby improving the cycle performance of the corresponding battery.
  • the average pore size of the titanium carbide is 2-8 nm, optionally 3-4 nm, measured using a scanning electron microscope.
  • the specific surface area and conductivity of the titanium carbide are further improved, thereby improving the cycle performance of the corresponding battery.
  • the resistivity of the single layer sheet of titanium carbide is 80-115 S/cm, optionally 100-110 S/cm, measured according to ASTM F76-08.
  • a second aspect of the present application provides a method for preparing titanium carbide, comprising:
  • step (2) mixing the titanium aluminum carbide obtained in step (1) with hydrofluoric acid, and then filtering to obtain a solid;
  • step (3) mixing the solid obtained in step (2) with a sulfoxide compound, and then drying to obtain the titanium carbide;
  • the average thickness of a single layer is 1-8 nm, optionally 1-5 nm, and further optionally 2-3 nm.
  • the method of the present application obtains titanium carbide with a lamellar structure by treating and drying with sulfoxide compounds.
  • the titanium carbide has a thinner thickness than conventional technologies, so that the titanium carbide has a larger specific surface area and higher conductivity, thereby improving the cycle performance of the corresponding battery.
  • MAX phase refers to a compound of formula Mn + 1AXn , which is composed of alternating stacks of n+1 MX sheets and 1 A-layer atomic plane.
  • the MXs are bonded to each other by strong covalent bonds, and the MX sheets are bonded to the A-layer atomic plane by weak covalent bonds, making it easier for the A atoms to break free from the constraints of the MX sheets.
  • the MAX phase Ti 3 AlC 2 in step (1) can be a commercially available product, or can be prepared by a corresponding preparation method, for example, including
  • step (1ii) heating the mixture in step (1i), for example, heating to 1000-1500°C, preferably 1300-1400°C, at a heating rate of 3-7°C/min under a continuous inert gas flow, such as Ar gas flow, and maintaining the temperature for 0.5-3 hours, cooling naturally to room temperature, and then sieving out powder particles with an average volume particle size of 20-38 ⁇ m, i.e., layered titanium aluminum carbide of the MAX phase.
  • a continuous inert gas flow such as Ar gas flow
  • step (2) comprises mixing the titanium aluminum carbide obtained in step (1) with hydrofluoric acid, and then filtering to obtain a solid.
  • step (2) comprises mixing the titanium aluminum carbide obtained in step (1) with hydrofluoric acid for 10-60 hours; then filtering to obtain a solid filtrate; then centrifuging and washing the solid filtrate with water until the pH value of the centrifugal supernatant is greater than 6; then filtering the obtained mixture with suction to obtain the solid.
  • step (2) comprises dissolving the obtained Ti 3 AlC 2 in a 30-50 wt % hydrofluoric acid aqueous solution, preferably a commercially available hydrofluoric acid solution (40 wt %, 22.5 mol/L), wherein the weight ratio of Ti 3 AlC 2 to hydrofluoric acid (calculated as HF) is 1:(8-25), preferably 1:(10-20), and more preferably 1:(13-15); maintaining the obtained mixed solution at 25-60° C., preferably 30-40° C., for 10-40 hours, preferably 20-30 hours, while stirring with a magnetic stirrer; then filtering with a suction filtration device at room temperature to obtain a solid filtrate; then washing the obtained solid filtrate with 500 ml of deionized water each time for 5-8 times, each time centrifuging the mixture of the filtrate and water at a speed of 2000-5000 rpm for 1-5 minutes until the pH value of the supernatant is above 6; and then filtering with
  • step (3) the solid obtained in step (2) is stirred and mixed with the sulfoxide compound at a rotation speed of 100-150 rpm for 30-70 hours.
  • the specific surface area and conductivity of the obtained titanium carbide are further improved, thereby improving the cycle performance of the corresponding battery.
  • the weight ratio of the solid to the sulfoxide compound is 1:(6-15), optionally 1:(8-12).
  • the specific ratio of the solid to the sulfoxide compound further improves the specific surface area and conductivity of the obtained titanium carbide, thereby improving the cycle performance of the corresponding battery.
  • the drying comprises vacuum drying at a temperature of 80-120° C., preferably at a pressure of 0.005-0.015 MPa.
  • the sulfoxide compound in step (3), is dimethyl sulfoxide.
  • the specific surface area and conductivity of the obtained titanium carbide are further improved, thereby improving the cycle performance of the corresponding battery.
  • the third aspect of the present application provides use of the titanium carbide described in the first aspect of the present application or the titanium carbide prepared according to the method described in the second aspect of the present application as a conductive agent for a secondary battery.
  • the conductive agent may be used in a negative electrode film layer or a positive electrode film layer of a secondary battery.
  • the conductive agent is used in the negative electrode film layer of a secondary battery.
  • the content of the conductive agent is 0.2%-1%, optionally 0.4%-1%, further optionally 0.4%-0.6%, based on the total weight of the negative electrode film layer.
  • the fourth aspect of the present application also provides a secondary battery, characterized in that it comprises the titanium carbide described in the first aspect or the titanium carbide prepared according to the method described in the second aspect of the present application.
  • the obtained battery has good cycle performance.
  • the titanium carbide is used as a conductive agent for a positive electrode film layer or a negative electrode film layer, preferably as a conductive agent for a negative electrode film layer.
  • the secondary battery is a metal ion battery, including but not limited to a lithium ion secondary battery, a sodium ion secondary battery, a potassium ion secondary battery, a magnesium ion secondary battery, an aluminum ion secondary battery, or a zinc ion secondary battery.
  • the secondary battery is a lithium ion secondary battery or a sodium ion secondary battery.
  • the components, material types or contents of the batteries mentioned are applicable to both lithium-ion secondary batteries and sodium-ion secondary batteries.
  • a secondary battery is provided.
  • a secondary battery includes a positive electrode sheet, a negative electrode sheet, an electrolyte and a separator.
  • active ions are embedded and released back and forth between the positive electrode sheet and the negative electrode sheet.
  • the electrolyte plays the role of conducting ions between the positive electrode sheet and the negative electrode sheet.
  • the separator is set between the positive electrode sheet and the negative electrode sheet, mainly to prevent the positive and negative electrodes from short-circuiting, while allowing ions to pass through.
  • the positive electrode sheet includes a positive electrode current collector and a positive electrode film layer disposed on at least one surface of the positive electrode current collector, wherein the positive electrode film layer includes a positive electrode active material.
  • the positive electrode current collector has two surfaces opposite to each other in its thickness direction, and the positive electrode film layer is disposed on any one or both of the two opposite surfaces of the positive electrode current collector.
  • the positive electrode current collector may be a metal foil or a composite current collector.
  • aluminum foil may be used as the metal foil.
  • the composite current collector may include a polymer material base layer and a metal layer formed on at least one surface of the polymer material base layer.
  • the composite current collector may be formed by forming a metal material on a polymer material substrate.
  • the metal material includes but is not limited to aluminum, aluminum alloy, nickel, nickel alloy, titanium, titanium alloy, silver and silver alloy, etc.
  • Polymer material substrate such as substrates of polypropylene (PP), polyethylene terephthalate (PET), polybutylene terephthalate (PBT), polystyrene (PS), polyethylene (PE), etc.
  • the positive electrode active material may include a positive electrode active material for a battery known in the art.
  • the positive electrode active material of the lithium ion secondary battery may include at least one of the following materials: olivine-structured lithium-containing phosphate, lithium transition metal oxide and their respective modified compounds.
  • the present application is not limited to these materials, and other traditional materials that can be used as positive electrode active materials for batteries may also be used. These positive electrode active materials may be used alone or in combination of two or more.
  • lithium transition metal oxides may include, but are not limited to , lithium cobalt oxide (such as LiCoO2 ), lithium nickel oxide (such as LiNiO2 ), lithium manganese oxide (such as LiMnO2 , LiMn2O4 ), lithium nickel cobalt oxide, lithium manganese cobalt oxide, lithium nickel manganese oxide, lithium nickel cobalt manganese oxide (such as LiNi1 / 3Co1 / 3Mn1 / 3O2 (also referred to as NCM333 ), LiNi0.5Co0.2Mn0.3O2 (also referred to as NCM523 ) , LiNi0.5Co0.25Mn0.25O2 (also referred to as NCM211 ) , LiNi0.6Co0.2Mn0.2O2 (also referred to as NCM622 ), LiNi0.8Co0.1Mn0.1O2 (also referred to as NCM811 ), lithium nickel cobalt aluminum oxide (such as LiNi 0.85 Co 0.15 Al 0.05
  • lithium-containing phosphates with an olivine structure may include, but are not limited to, lithium iron phosphate (such as LiFePO 4 (also referred to as LFP)), a composite material of lithium iron phosphate and carbon, lithium manganese phosphate (such as LiMnPO 4 ), a composite material of lithium manganese phosphate and carbon, lithium iron manganese phosphate, and a composite material of lithium iron manganese phosphate and carbon.
  • the weight ratio of the positive electrode active material in the positive electrode film layer is 80-100% by weight, based on the total weight of the positive electrode film layer.
  • the positive electrode active material of the sodium ion secondary battery may include at least one of the following materials: at least one of a sodium transition metal oxide, a polyanionic compound, and a Prussian blue compound.
  • the present application is not limited to these materials, and other conventionally known materials that can be used as positive electrode active materials for sodium ion batteries may also be used.
  • the transition metal in the sodium transition metal oxide, may be at least one of Mn, Fe, Ni, Co, Cr, Cu, Ti, Zn, V, Zr and Ce.
  • the sodium transition metal oxide is, for example, Na x MO 2 , wherein M is one or more of Ti, V, Mn, Co, Ni, Fe, Cr and Cu, and 0 ⁇ x ⁇ 1.
  • the polyanionic compound can be a class of compounds having sodium ions, transition metal ions and tetrahedral (YO 4 ) n- anion units.
  • the transition metal can be at least one of Mn, Fe, Ni, Co, Cr, Cu, Ti, Zn, V, Zr and Ce;
  • Y can be at least one of P, S and Si;
  • n represents the valence state of (YO 4 ) n- .
  • the polyanionic compound may also be a compound having sodium ions, transition metal ions, tetrahedral (YO 4 ) n- anion units and halogen anions.
  • the transition metal may be at least one of Mn, Fe, Ni, Co, Cr, Cu, Ti, Zn, V, Zr and Ce;
  • Y may be at least one of P, S and Si, and n represents the valence state of (YO 4 ) n- ;
  • the halogen may be at least one of F, Cl and Br.
  • the polyanionic compound may also be a compound having sodium ions, tetrahedral (YO 4 ) n- anion units, polyhedral units (ZO y ) m+ and optional halogen anions.
  • Y may be at least one of P, S and Si, and n represents the valence state of (YO 4 ) n- ;
  • Z represents a transition metal, and may be at least one of Mn, Fe, Ni, Co, Cr, Cu, Ti, Zn, V, Zr and Ce, and m represents the valence state of (ZO y ) m+ ;
  • the halogen may be at least one of F, Cl and Br.
  • the polyanionic compound is, for example, at least one of NaFePO4, Na3V2(PO4)3 (sodium vanadium phosphate, abbreviated as NVP), Na4Fe3(PO4)2 ( P2O7 ) , NaM'PO4F ( M ' is one or more of V, Fe, Mn and Ni) and Na3 ( VOy ) 2 ( PO4 ) 2F3-2y ( 0 ⁇ y ⁇ 1 ).
  • the Prussian blue compound may be a compound having sodium ions, transition metal ions and cyanide ions (CN - ).
  • the transition metal may be at least one of Mn, Fe, Ni, Co, Cr, Cu, Ti, Zn, V, Zr and Ce.
  • the Prussian blue compound is, for example, Na a Me b Me' c (CN) 6 , wherein Me and Me' are each independently at least one of Ni, Cu, Fe, Mn, Co and Zn, 0 ⁇ a ⁇ 2, 0 ⁇ b ⁇ 1, 0 ⁇ c ⁇ 1.
  • the positive electrode film layer may also optionally include a binder.
  • the binder may include at least one of polyvinylidene fluoride (PVDF), polytetrafluoroethylene (PTFE), vinylidene fluoride-tetrafluoroethylene-propylene terpolymer, vinylidene fluoride-hexafluoropropylene-tetrafluoroethylene terpolymer, tetrafluoroethylene-hexafluoropropylene copolymer and fluorine-containing acrylate resin.
  • PVDF polyvinylidene fluoride
  • PTFE polytetrafluoroethylene
  • PTFE polytetrafluoroethylene
  • the weight ratio of the binder in the positive electrode film layer is 0-20% by weight, based on the total weight of the positive electrode film layer.
  • the positive electrode film layer may further include other conductive agents.
  • the other conductive agents may include at least one of superconducting carbon, acetylene black, carbon black, Ketjen black, carbon dots, carbon nanotubes, graphene and carbon nanofibers.
  • the weight ratio of the other conductive agents in the positive electrode film layer is 0-20% by weight, based on the total weight of the positive electrode film layer.
  • the positive electrode sheet can be prepared by the following method: the components for preparing the positive electrode sheet, such as the positive electrode active material, the conductive agent, the binder and any other components are dispersed in a solvent (such as N-methylpyrrolidone) to form a positive electrode slurry, wherein the positive electrode slurry has a solid content of 40-80wt%, and the viscosity at room temperature is adjusted to 5000-25000mPa ⁇ s, the positive electrode slurry is coated on the surface of the positive electrode collector, and after drying, it is cold-pressed by a cold rolling mill to form a positive electrode sheet; the positive electrode powder coating unit area density is 150-450mg/ m2 , and the positive electrode sheet compaction density is 2.0-3.6g/ cm3 , and can be optionally 2.3-3.5g/ cm3 .
  • the compaction density is calculated by the formula:
  • Compacted density coating surface density/(thickness of the electrode after extrusion - thickness of the current collector).
  • the negative electrode sheet includes a negative electrode current collector and a negative electrode film layer disposed on at least one surface of the negative electrode current collector, wherein the negative electrode film layer includes a negative electrode active material.
  • the negative electrode current collector has two surfaces opposite to each other in its thickness direction, and the negative electrode film layer is disposed on any one or both of the two opposite surfaces of the negative electrode current collector.
  • the negative electrode current collector may be a metal foil or a composite current collector.
  • the composite current collector may include a polymer material base layer and a metal layer formed on at least one surface of the polymer material substrate.
  • the composite current collector may be formed by forming a metal material on a polymer material substrate.
  • the metal material includes but is not limited to copper, copper alloy, nickel, nickel alloy, titanium, titanium alloy, silver and silver alloy, etc.
  • the polymer material substrate includes but is not limited to polypropylene (PP), polyethylene terephthalate (PET), polybutylene terephthalate (PBT), polystyrene (PS), polyethylene (PE) and other substrates.
  • the thickness of the negative electrode current collector is generally 3 ⁇ m to 15 ⁇ m.
  • the negative electrode active material of the lithium ion secondary battery may adopt the negative electrode active material for the battery known in the art.
  • the negative electrode active material may include at least one of the following materials: artificial graphite, natural graphite, soft carbon, hard carbon, silicon-based materials, tin-based materials, lithium titanate, etc.
  • the silicon-based material may be selected from at least one of elemental silicon, silicon oxide compounds, silicon-carbon composites, silicon-nitrogen composites, and silicon alloys.
  • the tin-based material may be selected from at least one of elemental tin, tin oxide compounds, and tin alloys.
  • the present application is not limited to these materials, and other traditional materials that can be used as negative electrode active materials for batteries may also be used. These negative electrode active materials may be used alone or in combination of two or more.
  • the negative electrode active material of the sodium ion secondary battery is usually a hard carbon material, a two-dimensional metal carbide or a nitride.
  • the negative electrode active material of the sodium ion secondary battery is usually a hard carbon material.
  • the weight ratio of the negative electrode active material in the negative electrode film layer is 70-100 weight %, based on the total weight of the negative electrode film layer.
  • the negative electrode film layer may further include a binder.
  • the binder may be selected from at least one of styrene-butadiene rubber (SBR), polyacrylic acid (PAA), sodium polyacrylate (PAAS), polyacrylamide (PAM), polyvinyl alcohol (PVA), sodium alginate (SA), polymethacrylic acid (PMAA) and carboxymethyl chitosan (CMCS).
  • SBR styrene-butadiene rubber
  • PAA polyacrylic acid
  • PAAS sodium polyacrylate
  • PAM polyacrylamide
  • PVA polyvinyl alcohol
  • SA sodium alginate
  • PMAA polymethacrylic acid
  • CMCS carboxymethyl chitosan
  • the negative electrode film layer may further optionally include other conductive agents.
  • the other conductive agents may be selected from at least one of superconducting carbon, acetylene black, carbon black, Ketjen black, carbon dots, carbon nanotubes, graphene and carbon nanofibers.
  • the weight ratio of the other conductive agents in the negative electrode film layer is 0-20 weight %, based on the total weight of the negative electrode film layer.
  • the negative electrode film layer may further include other additives, such as a thickener (such as sodium carboxymethyl cellulose (CMC-Na)), etc.
  • a thickener such as sodium carboxymethyl cellulose (CMC-Na)
  • the weight ratio of the other additives in the negative electrode film layer is 0-15% by weight, based on the total weight of the negative electrode film layer.
  • the negative electrode sheet can be prepared by the following method: the components for preparing the negative electrode sheet, such as the negative electrode active material, the conductive agent, the binder and any other components are dispersed in a solvent (such as deionized water) to form a negative electrode slurry, wherein the solid content of the negative electrode slurry is 30-70wt%, and the viscosity at room temperature is adjusted to 2000-10000mPa ⁇ s; the obtained negative electrode slurry is coated on the negative electrode collector, and after a drying process, cold pressing such as rolling, a negative electrode sheet is obtained.
  • the negative electrode powder coating unit area density is 75-220mg/ m2
  • the negative electrode sheet compaction density is 0.5-2.0g/ m3 .
  • the electrolyte plays the role of conducting ions between the positive electrode and the negative electrode.
  • the present application has no specific restrictions on the type of electrolyte, which can be selected according to needs.
  • the electrolyte can be liquid, gel or all-solid.
  • the electrolyte is an electrolyte solution, which includes an electrolyte salt and a solvent.
  • the electrolyte salt of the lithium ion secondary battery can be selected from one or more of lithium hexafluorophosphate (LiPF 6 ), lithium tetrafluoroborate (LiBF 4 ), lithium perchlorate (LiClO 4 ), lithium hexafluoroarsenate (LiAsF 6 ), lithium bis(fluorosulfonyl)imide (LiFSI), lithium bis(trifluoromethanesulfonyl)imide (LiTFSI), lithium trifluoromethanesulfonate (LiTFS), lithium difluorooxalatoborate (LiDFOB), lithium dioxalatoborate (LiBOB), lithium difluorophosphate (LiPO 2 F 2 ), lithium difluorobis(oxalatophosphate) (LiDFOP) and lithium tetrafluorooxalatophosphate (LiTFOP).
  • the electrolyte salt of the sodium ion secondary battery can be selected from one or more of sodium hexafluorophosphate, sodium bis(fluorosulfonyl)imide, sodium bis(trifluoromethanesulfonyl)imide, sodium trifluoromethanesulfonate, sodium tetrafluoroborate, sodium difluorophosphate, sodium perchlorate, and sodium chloride.
  • the solvent can be selected from one or more of fluoroethylene carbonate (FEC), ethylene carbonate (EC), propylene carbonate (PC), ethyl methyl carbonate (EMC), diethyl carbonate (DEC), dimethyl carbonate (DMC), dipropyl carbonate (DPC), methyl propyl carbonate (MPC), ethyl propyl carbonate (EPC), butylene carbonate (BC), methyl formate (MF), methyl acetate (MA), ethyl acetate (EA), propyl acetate (PA), methyl propionate (MP), ethyl propionate (EP), propyl propionate (PP), methyl butyrate (MB), ethyl butyrate (EB), 1,4-butyrolactone (GBL), sulfolane (SF), dimethyl sulfone (MSM), ethyl methyl sulfone (EMS) and diethyl sulfone (FEC),
  • the electrolyte may further include additives, such as negative electrode film-forming additives, positive electrode film-forming additives, and additives that can improve certain battery properties, such as additives that improve battery overcharge performance, additives that improve battery high or low temperature performance, etc.
  • additives such as negative electrode film-forming additives, positive electrode film-forming additives, and additives that can improve certain battery properties, such as additives that improve battery overcharge performance, additives that improve battery high or low temperature performance, etc.
  • the secondary battery further includes a separator.
  • the present application has no particular limitation on the type of separator, and any known porous separator with good chemical stability and mechanical stability can be selected.
  • the material of the isolation membrane can be selected from at least one of glass fiber, non-woven fabric, polyethylene, polypropylene and polyvinylidene fluoride.
  • the isolation membrane can be a single-layer film or a multi-layer composite film, without particular limitation.
  • the materials of each layer can be the same or different, without particular limitation.
  • the isolation film has a thickness of 6-40 ⁇ m, and optionally 12-20 ⁇ m.
  • the positive electrode sheet, the negative electrode sheet, and the separator may be formed into an electrode assembly by a winding process or a lamination process.
  • the secondary battery may include an outer package, which may be used to encapsulate the electrode assembly and the electrolyte.
  • the outer packaging of the secondary battery may be a hard shell, such as a hard plastic shell, an aluminum shell, a steel shell, etc.
  • the outer packaging of the secondary battery may also be a soft package, such as a bag-type soft package.
  • the material of the soft package may be plastic, and examples of the plastic include polypropylene, polybutylene terephthalate, and polybutylene succinate.
  • FIG2 is a secondary battery 5 of a square structure as an example.
  • the outer package may include a shell 51 and a cover plate 53.
  • the shell 51 may include a bottom plate and a side plate connected to the bottom plate, and the bottom plate and the side plate enclose a receiving cavity.
  • the shell 51 has an opening connected to the receiving cavity, and the cover plate 53 can be covered on the opening to close the receiving cavity.
  • the positive electrode sheet, the negative electrode sheet and the isolation film can form an electrode assembly 52 through a winding process or a lamination process.
  • the electrode assembly 52 is encapsulated in the receiving cavity.
  • the electrolyte is infiltrated in the electrode assembly 52.
  • the number of electrode assemblies 52 contained in the secondary battery 5 can be one or more, and those skilled in the art can select according to specific actual needs.
  • secondary batteries may be assembled into a battery module.
  • the number of secondary batteries contained in the battery module may be one or more, and the specific number may be selected by those skilled in the art according to the application and capacity of the battery module.
  • the plurality of secondary batteries 5 may be arranged in sequence along the length direction of the battery module. Of course, they may also be arranged in any other manner. Further, the plurality of secondary batteries 5 may be fixed by fasteners.
  • the battery module may further include a housing having a housing space, and the plurality of secondary batteries 5 are housed in the housing space.
  • the battery modules described above may also be assembled into a battery pack.
  • the battery pack may contain one or more battery modules, and the specific number may be selected by those skilled in the art according to the application and capacity of the battery pack.
  • the battery pack may include a battery box and a plurality of battery modules disposed in the battery box.
  • the battery box includes an upper box body and a lower box body, and the upper box body can be covered on the lower box body to form a closed space for accommodating the battery modules.
  • the plurality of battery modules can be arranged in the battery box in any manner.
  • the present application also provides an electrical device, which includes at least one of the secondary battery, battery module, or battery pack provided in the present application.
  • the secondary battery, battery module, or battery pack can be used as a power source for the electrical device, and can also be used as an energy storage unit for the electrical device.
  • the electrical device may include mobile devices (such as mobile phones, laptops, etc.), electric vehicles (such as pure electric vehicles, hybrid electric vehicles, plug-in hybrid electric vehicles, electric bicycles, electric scooters, electric golf carts, electric trucks, etc.), electric trains, ships and satellites, energy storage systems, etc., but are not limited to these.
  • a secondary battery, a battery module or a battery pack may be selected according to its usage requirements.
  • FIG4 is an example of an electric device.
  • the electric device is a pure electric vehicle, a hybrid electric vehicle, or a plug-in hybrid electric vehicle, etc.
  • a battery pack or a battery module may be used.
  • a device may be a mobile phone, a tablet computer, a notebook computer, etc. Such a device is usually required to be thin and light, and a secondary battery may be used as a power source.
  • titanium carbide aluminum powder and titanium carbide powder purchased from ThernFisher were mixed in a molar ratio of 1:1 and added to a ball mill for ball milling for 1 day; the ball-milled mixture was placed in an alumina boat, heated to 1350° C. at a rate of 5° C./min under a continuous Ar gas flow, and maintained at this temperature for 1 hour, and then sieved through a 400-mesh sieve to obtain MAX phase titanium carbide aluminum powder particles with an average volume particle size of 38 ⁇ m;
  • step (2) Dissolve 1 g of the powder particles obtained in step (1) in 30 mL of a 40 wt % hydrofluoric acid solution, and place the mixture at 35° C. for 24 hours while stirring with a magnetic stirrer; filter the mixture with a suction filtration device at room temperature at 0.01 MPa to obtain a solid filtrate, and then centrifuge and wash the filtrate with 500 ml of deionized water each time, remove the supernatant, and wash the mixture 7 times until the pH value of the centrifugal supernatant is greater than 6, and then filter the centrifugal precipitate with suction at room temperature to obtain a laminated titanium carbide filter cake;
  • step (3) mixing the laminated titanium carbide filter cake obtained in step (2) with 80 mL of dimethyl sulfoxide, stirring and mixing at a rotation speed of 150 rpm for 48 hours, and then placing in a vacuum drying oven at a temperature of 100° C. and a pressure of 0.01 MPa for 5 hours to obtain the lamellar titanium carbide;
  • FIG1 The scanning image of the titanium carbide is shown in FIG1 , wherein FIG(b) is a partial enlarged image of FIG(a); the average thickness of a single layer is 2 nm; and the specific surface area is 85 m 2 /g.
  • step (2) the mixture was placed at 35° C. for 12 hours while being stirred with a magnetic stirrer.
  • step (2) the mixture was placed at 35° C. for 36 hours while being stirred with a magnetic stirrer.
  • step (3) the filter cake obtained in step (2) was placed in a vacuum drying oven at a temperature of 100° C. and a pressure of 0.01 MPa for 5 hours to obtain the titanium carbide.
  • step (3) the filter cake obtained in step (2) was placed in 500 ml of anhydrous ethanol and ultrasonicated at 200 Hz for one hour, then centrifuged and the solid was dried at room temperature to obtain the titanium carbide.
  • the positive electrode active material lithium iron phosphate, conductive carbon black SP and binder PVDF were dispersed in a solvent NMP at a weight ratio of 98:1:1 and mixed evenly to obtain a positive electrode slurry; the positive electrode slurry was evenly coated on a positive electrode current collector aluminum foil, and after drying and cold pressing, a positive electrode sheet was obtained, and the coating amount per unit area was 0.27g/ 1540.25mm2 .
  • the negative electrode active material graphite, the thickener sodium carboxymethyl cellulose, the binder styrene-butadiene rubber, and the conductive agent of Preparation Example 1 were mixed in a mass ratio of 95.4:2:2:0.6, and deionized water was added to obtain a negative electrode slurry under the action of a vacuum mixer; the negative electrode slurry was evenly coated on a copper foil; the copper foil was dried at room temperature and then transferred to a 120°C oven for drying for 1 hour, and then supercooled pressed and cut to obtain a negative electrode sheet, and the coating amount per unit area was 0.17 g/1540.25 mm2 .
  • a 12 ⁇ m thick polypropylene separator with a porosity of 50% was selected.
  • the organic solvent is a mixed solution containing ethylene carbonate (EC), ethyl methyl carbonate (EMC) and diethyl carbonate (DEC), wherein the volume ratio of EC, EMC and DEC is 20:20:60.
  • EC ethylene carbonate
  • EMC ethyl methyl carbonate
  • DEC diethyl carbonate
  • the volume ratio of EC, EMC and DEC is 20:20:60.
  • argon atmosphere glove box with a water content of ⁇ 10ppm fully dried lithium salt LiPF6 is dissolved in the organic solvent and mixed evenly to obtain an electrolyte.
  • the concentration of the lithium salt is 1 mol/L.
  • the positive electrode sheet, isolation film, and negative electrode sheet are stacked in order, so that the isolation film is placed between the positive and negative electrode sheets to play an isolating role. Then, they are wound into a square bare battery cell, loaded with aluminum-plastic film, and then baked at 80°C to remove water, and 10g of the corresponding non-aqueous electrolyte is injected and sealed. After standing, hot and cold pressing, formation, clamping, capacity division and other processes, a finished battery with a capacity of 4000mAh is obtained.
  • the battery is prepared in a similar manner to the secondary battery of Example 1, but uses the conductive agent of the corresponding preparation example.
  • Example 10 Replace the positive electrode conductive agent with titanium carbide
  • the secondary battery is prepared in a similar manner to the secondary battery of Example 1, except that the conductive carbon black SP in the positive electrode plate is replaced by the conductive agent of Preparation Example 1.
  • Example 11 Changing the amount of conductive agent used
  • the secondary battery is similar to the secondary battery preparation method of Example 1, except that in the preparation of the negative electrode plate, the mass ratio of the negative electrode active material graphite, the thickener sodium carboxymethyl cellulose, the adhesive styrene-butadiene rubber, and the conductive agent of Preparation Example 1 is 95:2:2:1.
  • Example 12 Changing the amount of conductive agent used
  • the secondary battery is similar to the secondary battery preparation method of Example 1, except that in the preparation of the negative electrode plate, the mass ratio of the negative electrode active material graphite, the thickener sodium carboxymethyl cellulose, the adhesive styrene-butadiene rubber, and the conductive agent of Preparation Example 1 is 95.6:2:2:0.4.
  • Example 13 Changing the amount of conductive agent used
  • the secondary battery is similar to the secondary battery preparation method of Example 1, except that in the preparation of the negative electrode plate, the mass ratio of the negative electrode active material graphite, the thickener sodium carboxymethyl cellulose, the adhesive styrene-butadiene rubber, and the conductive agent of Preparation Example 1 is 94:2:2:2.
  • the secondary battery is prepared in a similar manner to the secondary battery of Example 1, but uses the conductive agent of the corresponding preparation comparative example.
  • Comparative Example 3 Neither the positive nor the negative electrode uses the titanium carbide of the present invention as a conductive agent
  • the secondary battery is prepared in a similar manner to the secondary battery of Example 1, but acetylene black is used as a conductive agent in the negative electrode plate.
  • the batteries of the embodiments and comparative examples were prepared according to the above method, and various performance parameters were measured. The results are shown in Table 2 below.
  • the titanium carbide of the present application has an excellent two-dimensional graphene-like structure, a thinner sheet structure, a larger specific surface area and a higher conductivity; when it is used as a conductive agent for a secondary battery, it can improve the cycle performance of the corresponding battery.
  • the number of cycles can be as high as 5,000 or more.

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Abstract

L'invention concernr du carbure de titane, qui a une structure lamellaire. L'épaisseur moyenne d'une couche unique est de 1 à 8 nm. Le carbure de titane a une excellente structure de graphène bidimensionnel, une structure lamellaire mince, une grande surface spécifique et une conductivité élevée. Lorsque le carbure de titane est utilisé en tant qu'agent conducteur d'une batterie secondaire, les performances de cycle de la batterie secondaire peuvent être augmentées.
PCT/CN2022/126796 2022-10-21 2022-10-21 Carbure de titane et son utilisation, procédé de préparation, batterie secondaire et dispositif électrique WO2024082290A1 (fr)

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CN202280089077.3A CN118556304A (zh) 2022-10-21 2022-10-21 碳化钛及其用途、制法、二次电池和用电装置

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