CN110350191A - Sodium/lithium ion battery phosphate cathode material preparation method - Google Patents

Sodium/lithium ion battery phosphate cathode material preparation method Download PDF

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Publication number
CN110350191A
CN110350191A CN201910628119.6A CN201910628119A CN110350191A CN 110350191 A CN110350191 A CN 110350191A CN 201910628119 A CN201910628119 A CN 201910628119A CN 110350191 A CN110350191 A CN 110350191A
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ion battery
lithium ion
sodium
cathode material
phosphate cathode
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CN201910628119.6A
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CN110350191B (en
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李长明
吴超
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QINGDAO JIUHUAN XINYUE NEW ENERGY TECHNOLOGY Co.,Ltd.
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Southwest University
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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
    • H01M10/00—Secondary cells; Manufacture thereof
    • H01M10/05—Accumulators with non-aqueous electrolyte
    • H01M10/052—Li-accumulators
    • H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
    • 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
    • H01M4/36—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
    • H01M4/624—Electric conductive fillers
    • H01M4/625—Carbon or graphite
    • 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

Abstract

The invention discloses a kind of sodium/lithium ion battery phosphate cathode material preparation methods, comprising the following steps: (1) is thoroughly mixed phytic acid in a solvent with carbon material, Phosphateadsorption is made to form phosphate group on the carbon material；(2) metal salt containing metal ion is added into the system that step (1) obtains and is sufficiently mixed, make metal ion Electrostatic Absorption on the phosphate group, metal ion is crystallized according to the distribution of phosphate group arranged on the carbon material, forms the material with pore structure.The present invention forms phosphate group using phytic acid uniform adsorption on the carbon material, then metal ion is crystallized according to the distribution of phosphate group arranged on the carbon material, so as to form the specified pore structure for mass transfer of uniform, controllable, as sodium/anode material for lithium-ion batteries, rapid mass transfer can be achieved, reinforce electronics transfer, to have high capacity, high magnification and excellent cyclical stability.

Description

Sodium/lithium ion battery phosphate cathode material preparation method
Technical field
The present invention relates to sodium/technical field of lithium ion, and in particular to a kind of system of sodium/anode material for lithium-ion batteries Preparation Method.
Background technique
As various portable electronic products become increasingly popular, lithium ion battery is as a kind of power-supply device day easy to carry Benefit attracts attention.And the physicochemical property of sodium and lithium is approximate, battery charging and discharging principle is also similar, thus the research of sodium-ion battery It is paid more and more attention.In terms of practical application, the energy density of sodium-ion battery is usually less than lithium ion battery, therefore the two is suitable Close different fields.But research and develop the key that advanced positive and negative electrode material realizes practical application as sodium, lithium ion battery One.
Iron lithium phosphate (LiFePO4) as anode material for lithium-ion batteries of new generation, it is considered to be lithium ion battery is ideal Positive electrode.With LiFePO4It compares, FePO4, raw material sources simple with more synthesis technology extensively, the more low advantage of cost, However still need to overcome its low electron conduction at present, this directly affects the specific capacity of lithium ion battery.
Summary of the invention
The object of the present invention is to provide a kind of sodium/lithium ion battery phosphate cathode material preparation method, the phosphate Positive electrode can significantly improve sodium/lithium ion battery specific capacity and cyclical stability.
In order to achieve the goal above, the technical solution adopted by the present invention:
The invention discloses a kind of sodium/lithium ion battery phosphate cathode material preparation methods, comprising the following steps:
(1) phytic acid is thoroughly mixed in a solvent with carbon material, Phosphateadsorption is made to form phosphoric acid on the carbon material Group；
(2) metal salt containing metal ion is added into the system that step (1) obtains and is sufficiently mixed, makes metal ion On the phosphate group, metal ion crystallizes Electrostatic Absorption according to the distribution of phosphate group arranged on the carbon material, Form the material with pore structure, as described sodium/lithium ion battery phosphate cathode material.
As a preferred technical solution, in the step (1), carbon material includes but is not limited to carbon nanotube.
As a preferred technical solution, in the step (1), solvent includes but is not limited to water, dehydrated alcohol, N- methyl pyrrole The mixing of one or more of pyrrolidone and dimethylformamide.
As a preferred technical solution, in the step (2), metal ion includes but is not limited to Fe3+、Mn2+、Ni2+With Co2+One or more of mixing.
As a preferred technical solution, in the step (2), the metal salt containing metal ion includes but is not limited to Fe3+、 Mn2+、Ni2+And Co2+One or more of nitrate, sulfate and chlorate mixing.
As a preferred technical solution, in the step (2), into the system that step (1) obtains be added containing metal from The metal salt of son is simultaneously sufficiently mixed, and is regulated and controled the degree of supersaturation of metal salt and the temperature of solution, is made metal ion Electrostatic Absorption in institute It states on phosphate group, metal ion is crystallized according to the distribution of phosphate group arranged on the carbon material, and being formed has hole knot The material of structure, as described sodium/lithium ion battery phosphate cathode material.
As a preferred technical solution, in the step (2), the mass ratio of carbon material, phytic acid and metal salt be 1:1~ 10:10~30.
As a preferred technical solution, in the step (2), the temperature for regulating and controlling solution is -20~40 DEG C.
The product that step (2) is obtained as a preferred technical solution, filters, and obtained solid material is dried.
The solid material after drying is placed under 25~1000 DEG C of environment as a preferred technical solution, and is carried out at annealing Reason.
Beneficial effects of the present invention:
The present invention forms phosphate group using phytic acid uniform adsorption on the carbon material, and then metal ion is according to phosphate group Arrangement distribution crystallization on the carbon material, so as to form the specified pore structure for mass transfer of uniform, controllable, as Sodium/anode material for lithium-ion batteries can realize rapid mass transfer, reinforce electronics transfer, to have high capacity, high magnification and excellent Cyclical stability.
Detailed description of the invention
Fig. 1 is FePO made from embodiment 14The SEM photograph of (slurry)；
Fig. 2 is FePO made from embodiment 14The SEM photograph of (powder)；
Fig. 3 is FePO made from embodiment 14Property of the sodium-ion battery under 0.5C charge-discharge magnification as positive electrode It can figure；
Fig. 4 is FePO made from embodiment 14Property of the lithium ion battery under 0.5C charge-discharge magnification as positive electrode It can figure；
Fig. 5 is Mn made from embodiment 23(PO4)2The SEM photograph of (slurry)；
Fig. 6 is Mn made from embodiment 23(PO4)2Lithium ion battery as positive electrode is under 1 C charge-discharge magnification Performance map.
Specific embodiment
To make the objectives, technical solutions, and advantages of the present invention clearer, the present invention is made into one with reference to the accompanying drawing Step illustrates.
Embodiment 1
(1) phytic acid is thoroughly mixed in water with carbon nanotube, Phosphateadsorption is made to form phosphorus on the carbon nanotubes Acid groups；
(2) Fe (NO is added into the system that step (1) obtains3)3And it is sufficiently mixed, control carbon nanotube, phytic acid and Fe (NO3)3Mass ratio be 1:5:25, the temperature of solution is 0~5 DEG C, makes Fe3+Electrostatic Absorption is on the phosphate group, Fe3+It presses According to the distribution crystallization of phosphate group arranged on the carbon nanotubes；The SEM photograph of slurry obtained is as shown in Figure 1, from figure In visible uniform, controllable the pore structure that can be used for mass transfer；
(3) product for obtaining step (2) filters, and obtained solid material is dried, and is subsequently placed under 200 DEG C of environment It is made annealing treatment；The SEM photograph of powder obtained is as shown in Fig. 2, the hole that can be used for mass transfer of uniform, controllable as seen from the figure Structure.
Fig. 3 is FePO made from embodiment 14Property of the sodium-ion battery under 0.5C charge-discharge magnification as positive electrode It can scheme, it can be seen that recycling even across 300 times, battery still keeps higher specific capacity, shows fabulous stability.
Fig. 4 is FePO made from embodiment 14Property of the lithium ion battery under 0.5C charge-discharge magnification as positive electrode It can scheme, it can be seen that recycling even across 120 times, battery still keeps higher specific capacity, shows fabulous stability.
Embodiment 2
(1) phytic acid and carbon nanotube are thoroughly mixed in N-Methyl pyrrolidone, Phosphateadsorption is made to receive in carbon Phosphate group is formed on mitron；
(2) MnSO is added into the system that step (1) obtains4And it is sufficiently mixed, control carbon nanotube, phytic acid and MnSO4's Mass ratio is 1:8:20, and the temperature of solution is 20~25 DEG C, makes Mn2+Electrostatic Absorption is on the phosphate group, Mn2+According to phosphorus The distribution crystallization of the arrangement of acid groups on the carbon nanotubes；The SEM photograph of slurry obtained is as shown in figure 5, can from figure See the pore structure that can be used for mass transfer of uniform, controllable.
Fig. 6 is Mn made from embodiment 23(PO4)2Lithium ion battery as positive electrode is under 1 C charge-discharge magnification Performance map, it can be seen that recycling even across 100 times, battery still keeps higher specific capacity, shows fabulous stabilization Property.
Referring to the method for embodiment 1 and embodiment 2, using containing Fe3+、Mn2+、Ni2+、Co2+One or more of mixing Metal salt, can equally reach the purpose of the present invention.
The basic principles, main features and advantages of the present invention have been shown and described above.The technology of the industry Personnel are it should be appreciated that the present invention is not limited to the above embodiments, and the above embodiments and description only describe this The principle of invention, without departing from the spirit and scope of the present invention, various changes and improvements may be made to the invention, these changes Change and improvement all fall within the protetion scope of the claimed invention.The claimed scope of the invention by appended claims and its Equivalent thereof.

Claims (10)

1. a kind of sodium/lithium ion battery phosphate cathode material preparation method, it is characterised in that: the following steps are included:
(1) phytic acid is thoroughly mixed in a solvent with carbon material, Phosphateadsorption is made to form phosphate group on the carbon material；
(2) metal salt containing metal ion is added into the system that step (1) obtains and is sufficiently mixed, makes metal ion electrostatic It is adsorbed on the phosphate group, metal ion is crystallized according to the distribution of phosphate group arranged on the carbon material, is formed Material with pore structure, as described sodium/lithium ion battery phosphate cathode material.
2. sodium according to claim 1/lithium ion battery phosphate cathode material preparation method, it is characterised in that: institute It states in step (1), carbon material includes but is not limited to carbon nanotube.
3. sodium according to claim 1/lithium ion battery phosphate cathode material preparation method, it is characterised in that: institute It states in step (1), solvent includes but is not limited to one of water, dehydrated alcohol, N-Methyl pyrrolidone and dimethylformamide Or several mixing.
4. sodium according to claim 1/lithium ion battery phosphate cathode material preparation method, it is characterised in that: institute It states in step (2), metal ion includes but is not limited to Fe3+、Mn2+、Ni2+And Co2+One or more of mixing.
5. sodium according to claim 4/lithium ion battery phosphate cathode material preparation method, it is characterised in that: institute It states in step (2), the metal salt containing metal ion includes but is not limited to Fe3+、Mn2+、Ni2+And Co2+Nitrate, sulfate And the mixing of one or more of chlorate.
6. according to claim 1 to sodium described in 5 any one/lithium ion battery phosphate cathode material preparation method, It is characterized in that: in the step (2), the metal salt containing metal ion being added into the system that step (1) obtains and sufficiently mixes Close, regulate and control the degree of supersaturation of metal salt and the temperature of solution, make metal ion Electrostatic Absorption on the phosphate group, metal from Son is crystallized according to the distribution of phosphate group arranged on the carbon material, material of the formation with pore structure, and the as described sodium/ Lithium ion battery phosphate cathode material.
7. sodium according to claim 6/lithium ion battery phosphate cathode material preparation method, it is characterised in that: institute It states in step (2), the mass ratio of carbon material, phytic acid and metal salt is 1:1~10:10~30.
8. sodium according to claim 6/lithium ion battery phosphate cathode material preparation method, it is characterised in that: institute It states in step (2), the temperature for regulating and controlling solution is -20~40 DEG C.
9. sodium according to claim 1/lithium ion battery phosphate cathode material preparation method, it is characterised in that: will The product filtering that step (2) obtains, obtained solid material are dried.
10. sodium according to claim 9/lithium ion battery phosphate cathode material preparation method, it is characterised in that: will Solid material after drying is placed under 25~1000 DEG C of environment and is made annealing treatment.
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CN113321198B (en) * 2021-05-28 2022-03-01 西南大学 Binary metal phosphate anode material and preparation method and application thereof

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