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WO2025113137A1 - Matériau composite de pyrophosphate de phosphate ferrique de sodium, procédé de préparation, procédé d'évaluation et son procédé d'optimisation de processus et son utilisation - Google Patents

Matériau composite de pyrophosphate de phosphate ferrique de sodium, procédé de préparation, procédé d'évaluation et son procédé d'optimisation de processus et son utilisation Download PDF

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Publication number
WO2025113137A1
WO2025113137A1 PCT/CN2024/130592 CN2024130592W WO2025113137A1 WO 2025113137 A1 WO2025113137 A1 WO 2025113137A1 CN 2024130592 W CN2024130592 W CN 2024130592W WO 2025113137 A1 WO2025113137 A1 WO 2025113137A1
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Prior art keywords
sodium
composite material
iron pyrophosphate
sodium iron
pyrophosphate composite
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Chinese (zh)
Inventor
史利涛
刘佳斌
范伟贞
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JIUJIANG TINCI MATERIALS TECHNOLOGY Co Ltd
Guangzhou Tinci Materials Technology Co Ltd
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JIUJIANG TINCI MATERIALS TECHNOLOGY Co Ltd
Guangzhou Tinci Materials Technology Co Ltd
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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
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/362—Composites
    • H01M4/366—Composites as layered products
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B25/00—Phosphorus; Compounds thereof
    • C01B25/16—Oxyacids of phosphorus; Salts thereof
    • C01B25/26—Phosphates
    • C01B25/38—Condensed phosphates
    • C01B25/42—Pyrophosphates
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B25/00—Phosphorus; Compounds thereof
    • C01B25/16—Oxyacids of phosphorus; Salts thereof
    • C01B25/26—Phosphates
    • C01B25/45—Phosphates containing plural metal, or metal and ammonium
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
    • G01N23/20—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by using diffraction of the radiation by the materials, e.g. for investigating crystal structure; by using scattering of the radiation by the materials, e.g. for investigating non-crystalline materials; by using reflection of the radiation by the materials
    • G01N23/207—Diffractometry using detectors, e.g. using a probe in a central position and one or more displaceable detectors in circumferential positions
    • G—PHYSICS
    • G16—INFORMATION AND COMMUNICATION TECHNOLOGY [ICT] SPECIALLY ADAPTED FOR SPECIFIC APPLICATION FIELDS
    • G16C—COMPUTATIONAL CHEMISTRY; CHEMOINFORMATICS; COMPUTATIONAL MATERIALS SCIENCE
    • G16C20/00—Chemoinformatics, i.e. ICT specially adapted for the handling of physicochemical or structural data of chemical particles, elements, compounds or mixtures
    • G16C20/10—Analysis or design of chemical reactions, syntheses or processes
    • G—PHYSICS
    • G16—INFORMATION AND COMMUNICATION TECHNOLOGY [ICT] SPECIALLY ADAPTED FOR SPECIFIC APPLICATION FIELDS
    • G16C—COMPUTATIONAL CHEMISTRY; CHEMOINFORMATICS; COMPUTATIONAL MATERIALS SCIENCE
    • G16C60/00—Computational materials science, i.e. ICT specially adapted for investigating the physical or chemical properties of materials or phenomena associated with their design, synthesis, processing, characterisation or utilisation
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00—Secondary cells; Manufacture thereof
    • H01M10/05—Accumulators with non-aqueous electrolyte
    • H01M10/054—Accumulators with insertion or intercalation of metals other than lithium, e.g. with magnesium or aluminium
    • 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
    • H01M4/04—Processes of manufacture in general
    • 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
    • H01M4/04—Processes of manufacture in general
    • H01M4/0471—Processes of manufacture in general involving thermal treatment, e.g. firing, sintering, backing particulate active material, thermal decomposition, pyrolysis
    • 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
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • 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
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
    • 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
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
    • H01M4/5825—Oxygenated metallic salts or polyanionic structures, e.g. borates, phosphates, silicates, olivines
    • 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
    • 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
    • H01M4/624—Electric conductive fillers
    • H01M4/625—Carbon or graphite
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
    • C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/01—Particle morphology depicted by an image
    • C01P2004/03—Particle morphology depicted by an image obtained by SEM
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/60—Particles characterised by their size
    • C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/40—Electric properties
    • 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
    • H01M2004/021—Physical characteristics, e.g. porosity, surface area
    • 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
    • H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
    • H01M2004/028—Positive electrodes
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10—Energy storage using batteries

Definitions

  • the present application belongs to the technical field of sodium ion battery materials, and specifically relates to a sodium iron pyrophosphate composite material and its preparation process, evaluation method, process optimization method and application.
  • Sodium-ion batteries are rocking-chair batteries, which are secondary batteries that rely on the insertion and extraction of ions between the positive and negative electrodes. Both the positive and negative electrode materials allow sodium ions to be reversibly inserted and extracted. Research on sodium-ion batteries has been going on since 1982, and has made great progress in recent years and has met the conditions for commercial application. At present, the positive electrode materials of sodium-ion batteries mainly include oxides, Prussian blue and polyanions.
  • sodium iron pyrophosphate composite material As a polyanion sodium ferric pyrophosphate cathode material, sodium iron pyrophosphate composite material has a structurally stable sodium ion diffusion channel and good cycle performance, as well as moderate operating voltage and specific capacity. It is a cheap and promising sodium ion battery cathode material.
  • the common synthesis method of this material is the liquid phase method, which has high requirements on reaction process conditions, complex production equipment, and great difficulty in mass production, and is not suitable for large-scale industrial applications.
  • the capacity performance of sodium iron pyrophosphate composite materials obtained by the existing synthesis process is limited, and there is still room for further improvement.
  • one of the objectives of the present application is to provide a sodium iron pyrophosphate composite material.
  • the second purpose of the present application is to provide a preparation process of sodium iron pyrophosphate composite material.
  • the third purpose of this application is to provide an evaluation method for sodium iron pyrophosphate composite materials.
  • the fourth purpose of this application is to provide an optimization method for the preparation process of sodium iron pyrophosphate composite material.
  • the fifth object of the present application is to provide a sodium iron pyrophosphate composite material for use as a positive electrode material for sodium ion batteries in sodium ion batteries.
  • the present application creatively discovers that when the sodium iron pyrophosphate composite material has a specific content of spinel NaFePO 4 phase, the capacity performance of the sodium iron pyrophosphate composite material can be effectively improved, but the NaFePO 4 phase in the sodium iron pyrophosphate composite material may also play a certain role as a structural phase.
  • the structural stability of the material will be destroyed, thereby reducing the overall electrochemical performance; and when its content is too high, the overall electrochemical performance will be reduced.
  • the sodium ferric pyrophosphate composite material comprises sodium ferric pyrophosphate and a carbon layer coated on the surface of the sodium ferric pyrophosphate, and has a chemical formula of Na 4 Fe 3(1-x) (PO 4 ) 2 P 2 O 7 @C, wherein 0 ⁇ x ⁇ 0.02.
  • the carbon content of the sodium iron pyrophosphate composite material is 2-5 wt %.
  • the size of the primary particles of the sodium iron pyrophosphate composite material is mainly distributed in the range of 100 to 200 nm, and the secondary particles are formed by agglomeration of the primary particles, and the size of the secondary particles is mainly distributed in the range of 300 to 800 nm.
  • NaFePO4 phase control is the most core difficulty in the synthesis of this material.
  • the present application also provides a preparation process of the sodium iron pyrophosphate composite material, comprising the following steps:
  • the raw materials for synthesizing Na 4 Fe 3(1-x) (PO 4 ) 2 P 2 O 7 include an iron source and a sodium source.
  • the iron source is ammonium ferrous phosphate
  • the sodium source includes sodium pyrophosphate and a P-free sodium source.
  • the P-free sodium source is selected from any one or more of sodium carbonate, ammonium bicarbonate, sodium acetate and sodium citrate.
  • the molar ratio of ammonium ferrous phosphate, the sodium source not containing P and sodium pyrophosphate is 3:(0.96-1):(0.5-0.54).
  • the carbon source is any one or more of glucose, sucrose, starch, and polyethylene glycol.
  • the amount of the carbon source is 5-20% of the mass of the raw material for synthesizing Na 4 Fe 3(1-x) (PO 4 ) 2 P 2 O 7 .
  • the wet grinding and mixing time is 4 to 6 hours;
  • the medium of the wet grinding is a solvent with a boiling point lower than 80° C., such as ethanol.
  • the grinding method is vibration milling or rolling milling, and more preferably continuous rolling ball milling.
  • the preset sintering parameters include the sintering heating rate, the sintering temperature and the sintering time, wherein at least one of the following conditions is satisfied:
  • the heating rate of the sintering is 10-15°C/min
  • the sintering temperature is 500-550°C
  • the sintering time is 8 to 12 hours.
  • the protective atmosphere is an inert gas or nitrogen; more preferably, it is one of high-purity nitrogen, argon, and argon-hydrogen mixed gas.
  • the present application discloses a method for evaluating a sodium iron pyrophosphate composite material, comprising the following steps:
  • the performance reference value in step S2 is Ir, and its interval range is 6.19 ⁇ Ir ⁇ 13; when Ir' is within the interval range of Ir, the performance evaluation result of the material is excellent.
  • reaction (1) has a greater entropy increase and a greater thermodynamic advantage, and the phase formation temperature range of NaFePO 4 is approximately 300-400°C, the electrochemically inert NaFePO 4 has a stronger tendency to form the target product than reaction (2).
  • the present application can reduce the phase formation time of NaFePO4 by increasing the heating rate, and combine the method of using lattice defects (controlling the iron-phosphorus ratio) to inhibit the formation of thermodynamically dominant impure phases to reduce the content of inert phases, thereby improving the material capacity performance.
  • the present application discloses a method for optimizing the preparation process of a sodium iron pyrophosphate composite material, using the above-mentioned sodium iron pyrophosphate composite material evaluation method to evaluate the sodium iron pyrophosphate composite material prepared by the above-mentioned preparation process of the composite sodium iron phosphate positive electrode material, and further comprising the following steps:
  • step (1) If the performance test value is not within the range of the performance reference value, repeat steps (1), (2), S1, and S2, and optimize and adjust the process parameters in step (1) or (2) according to the comparison results until the performance test value is within the range of the performance reference value, and then output the optimized process parameters.
  • step (1) or (2) are optimized and adjusted according to the comparison results, wherein the process parameters include the amount of iron source added to the preset feed in step (1) and/or the preset sintering parameters in step (2).
  • the amount of iron source added is correspondingly reduced, and/or the heating rate is increased; when Ir' is greater than the upper limit of the interval of Ir, the amount of iron source added is correspondingly increased, and/or the heating rate is reduced.
  • the present application also discloses the use of the sodium iron pyrophosphate composite material described above, or the sodium iron pyrophosphate composite material prepared by the above-mentioned preparation process, or the sodium iron pyrophosphate composite material evaluated as excellent by the above-mentioned evaluation method, or the sodium iron pyrophosphate composite material prepared by the sodium iron pyrophosphate composite material preparation process optimized by the above-mentioned optimization method as a positive electrode material for sodium ion batteries in sodium ion batteries.
  • the present application limits the content of the spinel NaFePO4 phase by the ratio of the characteristic peak and its peak intensity in the XRD spectrum obtained by XRD diffraction of the sodium iron pyrophosphate composite material under CuK ⁇ radiation, while ensuring the improvement of the capacity performance and avoiding the influence of its electrochemical inertness on other electrochemical properties of the material.
  • the present application proposes a solid phase synthesis method of composite sodium iron phosphate based on NH 4 FePO 4 ⁇ H 2 O as an iron source.
  • the raw material cost is low, the formula is easy to control, the synthesized product NaFePO 4 (Marticite) content is appropriate, the process is simple, the economic benefit is high, and the prepared material has excellent electrochemical properties.
  • the present application uses an evaluation method for sodium iron phosphate pyrophosphate composite materials to evaluate the performance of the prepared composite sodium iron phosphate.
  • the process is adjusted to control the iron-phosphorus ratio and sintering temperature, reduce the residence time in the NaFePO4 phase formation temperature range, control the phase formation of the NaFePO4 phase , and then control the content of the NaFePO4 phase in the product, thereby obtaining a process for preparing products with better performance.
  • FIG. 1 is an XRD diagram of the sodium iron pyrophosphate composite material prepared in Example 1.
  • FIG. 2 is a SEM image of the sodium iron pyrophosphate composite material prepared in Example 1.
  • FIG3-1 is a charge and discharge curve of a button cell assembled with the sodium iron pyrophosphate composite material prepared in Example 1. ...
  • Figure 3-2 is a cycle performance diagram of a button cell assembled with the sodium iron pyrophosphate composite material prepared in Example 1.
  • FIG. 4 is an XRD diagram of the sodium iron pyrophosphate composite material prepared in Example 2.
  • FIG. 5 is a SEM image of the sodium iron pyrophosphate composite material prepared in Example 2.
  • FIG. 7 is an XRD diagram of the sodium iron pyrophosphate composite material prepared in Example 3.
  • FIG8 is a SEM image of the sodium iron pyrophosphate composite material prepared in Example 3.
  • FIG9-1 is a charge and discharge curve of a button cell assembled with the sodium iron pyrophosphate composite material prepared in Example 3.
  • Figure 9-2 is a cycle performance diagram of a button cell assembled with the sodium iron pyrophosphate composite material prepared in Example 3.
  • FIG10 is an XRD diagram of the sodium iron pyrophosphate composite material prepared in Example 4.
  • FIG. 11 is a SEM image of the sodium iron pyrophosphate composite material prepared in Example 4.
  • FIG12-1 is a charge and discharge curve of a button cell assembled with the sodium iron pyrophosphate composite material prepared in Example 4.
  • FIG12-2 is a cycle performance diagram of a button cell assembled with the sodium iron pyrophosphate composite material prepared in Example 4.
  • FIG13 is an XRD diagram of the sodium iron pyrophosphate composite material prepared in Comparative Example 1.
  • FIG14 is a SEM image of the sodium iron pyrophosphate composite material prepared in Comparative Example 1.
  • Figure 15-1 is the charge and discharge curve of the button battery assembled with the sodium iron pyrophosphate composite material prepared in Comparative Example 1.
  • Figure 15-2 is a cycle performance diagram of the button battery assembled with the sodium iron pyrophosphate composite material prepared in Comparative Example 1.
  • Figure 16 is an XRD diagram of the sodium iron pyrophosphate composite material prepared in Comparative Example 2.
  • Figure 17 is a SEM image of the sodium iron pyrophosphate composite material prepared in Comparative Example 2.
  • Figure 18-1 is the charge and discharge curve of the button battery assembled with the sodium iron pyrophosphate composite material prepared in Comparative Example 2.
  • Figure 18-2 is a cycle performance diagram of the button battery assembled with the sodium iron pyrophosphate composite material prepared in Comparative Example 2.
  • the XRD pattern after deducting the baseline is shown in FIG1
  • the SEM pattern is shown in FIG2 .
  • the size of the primary particles of the sodium iron pyrophosphate composite material is mainly distributed in 100-200 nm, and the secondary particles are formed by agglomeration of the primary particles, and the size is mainly distributed in 300-800 nm.
  • the carbon content measured by the carbon-sulfur analyzer is 2.5wt%.
  • This peak intensity ratio IT / IO is defined as Ir, and the Ir of the material in this embodiment is 6.19.
  • the sodium iron pyrophosphate composite material Na 4 Fe 2.97 (PO 4 ) 2 P 2 O 7 @C prepared by the above method was assembled with a metal sodium sheet into a button cell for testing.
  • Comparative Example 2 shows that NaFePO4 phase is also one of the structural phases of composite sodium iron phosphate. Too low a content will also destroy the structural stability of NFPP itself and reduce the material performance. This Comparative Example 2 further reduces the Fe source ratio (reduced by 3%), and finally Ir is too high and the performance is poor. The decline in cycle performance indirectly indicates that the structural stability of the material itself is reduced in this case.

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Abstract

La présente invention concerne un matériau de batterie au sodium-ion, et concerne spécifiquement un matériau composite de pyrophosphate de phosphate ferrique de sodium, et un procédé de préparation, un procédé d'évaluation et son procédé d'optimisation de processus et son utilisation. Le matériau composite pyrophosphate de phosphate ferrique de sodium présente une phase NaFePO4 de type spinelle ; et dans un diagramme de diffraction par rayons X obtenu en soumettant le matériau composite pyrophosphate de phosphate ferrique de sodium à une diffraction par rayons X à l'aide d'un rayonnement CuKα, il existe un pic de diffraction caractéristique T de pyrophosphate de phosphate ferrique de sodium et un pic de diffraction caractéristique O de NaFePO4 de type spinelle à 2θ de 33,6 ± 0,2° et 32,8 ± 0,2°, respectivement, leurs intensités de pic sont respectivement IT et IO, et le rapport d'intensité de pic de diffraction Ir est égal à IT/IO, où 6,19 ≤ Ir ≤ 13.
PCT/CN2024/130592 2023-11-23 2024-11-07 Matériau composite de pyrophosphate de phosphate ferrique de sodium, procédé de préparation, procédé d'évaluation et son procédé d'optimisation de processus et son utilisation Pending WO2025113137A1 (fr)

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CN202311574388 2023-11-23
CN202311612427.2A CN120033222A (zh) 2023-11-23 2023-11-29 焦磷酸磷酸铁钠复合材料及其制备工艺、评估方法、工艺优化方法和应用
CN202311612427.2 2023-11-29

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN120589713A (zh) * 2025-07-07 2025-09-05 上海懿烯电源科技有限公司 一种钠离子电池用磷酸焦磷酸铁钠正极材料及其制备方法

Citations (6)

* Cited by examiner, † Cited by third party
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