CN104795557A - Porous metallic cathode material doped with lithium manganate/carbon for composite lithium batteries, and preparation method of porous metallic cathode material - Google Patents

Porous metallic cathode material doped with lithium manganate/carbon for composite lithium batteries, and preparation method of porous metallic cathode material Download PDF

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CN104795557A
CN104795557A CN201510152217.9A CN201510152217A CN104795557A CN 104795557 A CN104795557 A CN 104795557A CN 201510152217 A CN201510152217 A CN 201510152217A CN 104795557 A CN104795557 A CN 104795557A
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preparation
lithium manganate
positive electrode
carbon composite
nitrate
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朱申敏
石一杉
朱呈岭
李尧
张荻
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Shanghai Jiaotong 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
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
    • H01M4/50—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese
    • H01M4/505—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese of mixed oxides or hydroxides containing manganese for inserting or intercalating light metals, e.g. LiMn2O4 or LiMn2OxFy
    • 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
    • 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
    • H01M4/139—Processes of manufacture
    • 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
    • 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
    • H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
    • H01M4/52—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
    • H01M4/525—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron of mixed oxides or hydroxides containing iron, cobalt or nickel for inserting or intercalating light metals, e.g. LiNiO2, LiCoO2 or LiCoOxFy
    • 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
    • H01M2004/021—Physical characteristics, e.g. porosity, surface area
    • 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

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Abstract

The invention relates to a porous metallic cathode material doped with lithium manganate/carbon for composite lithium batteries, and a preparation method of the porous metallic cathodmaterial. The preparation method comprises the following steps: dissolving a surfactant in absolute ethyl alcohol, and stirring the surfactant and the absolute ethyl alcohol so as to obtain gel; adding lithium nitrate, and nitrate mixed with metal nitrate and manganese in the obtained gel, and performing uniform stir; after uniformly mixing, drying the mixture in a blast drying box, and further calcining the dried mixture in a muffle furnace so as to obtain the porous material doped with lithium manganate LiM0.2Mn1.8O4; dissolving the LiM0.2Mn1.8O4 in glucose solution, enabling the LiM0.2Mn1.8O4 to uniformly disperse, and after performing air blast drying, calcining the dried product in nitrogen atmosphere so as to obtain the metallic composite material LiM0.2Mn1.8O4/C doped with lithium manganate/carbon, wherein M refers to the doped metal. Compared with the prior art, the porous metallic cathode material prepared through the preparation method disclosed by the invention has the advantages that the crystallizing property is good, the particle size is about 20nm, and the material has good specific discharge capacity, rate capability and cycling properties as the cathode material for lithium batteries. The preparation idea of the preparation method disclosed by the invention can be applied to the preparation of other cathode materials of composite materials of porous metallic oxides.

Description

Porous metals adulterated lithium manganate/carbon composite lithium ion battery positive electrode and preparation method
Technical field
The present invention relates to a kind of preparation method of novel porous metal-doped LiMn2O4/carbon composite lithium ion battery positive electrode, specifically porous LiM 0.2mn 1.8o 4the preparation method of/C.
Background technology
LiMn 2o 4dissolving and the Jahn-Teller effect of Mn can be there is in charge and discharge process, make lattice produce distortion, lattice structure is unstable, causes electroactive some lost, specific capacity declines, and especially under high temperature (>55 DEG C), cycle performance is poor.Research finds, the transition metal substituted LiMn such as available Mg, Al, Zn, Ti, Cr, Fe, Co, Ni, Cu 2o 4middle part Mn, to strengthen the crystal field interaction of crystal Atom, suppresses the atomic migration and the structural phase transition that are unfavorable for de-lithium process in electrochemical reaction process, makes stable lattice, and improve material property, as energy density etc.Different according to the ratio replaced, material also embodies different performances.The LiM of quaternary xm ' 2-xo 4(0<x<1) and some other components more complicated, even five yuan, hexa-atomic, there is the material of same picket spinel structure, because introduce various metals atom in crystal structure, change the chemical property shown in embedding lithium/de-lithium reaction, lattice structure is stablized, the cycle performance of material can be improved, and often there is higher voltage (more than 4V, even reach 5V), there are more advantages as positive electrode.
According to pertinent literature report, suitable to LiMn 2o 4substitute manganese atom with transition metal moieties, the cycle performance of electrode can be improved, extend the life-span of electrode, thus be conducive to the raising of battery performance.But the replacement of too much transition metal, can cause the change of electrode material thing phase, generate cenotype even, changes the structure of lattice, hinder the diffusion of lithium ion in lattice, the capacity of electrode is significantly reduced, is unfavorable for the raising of electrode material performance.Therefore, this work, by the exploration to substitution amount, mainly stresses the performance of the material under less substitution amount.
The free diffusing of lithium ion between reactive species interface is the rate controlling step that its " deintercalation/embedding " reacts, and the therefore structure of active material, pattern is very large to the Electrochemical Performances of positive electrode.When the granularity of active material is excessive, then material specific surface is too small, less with the contact of electrolyte, is unfavorable for the diffusion of lithium ion, is unfavorable for making full use of of electrode material; And when crystal grain is less, the distance that Li ion is diffused into material surface from material center shortens, thus diffusion rate is comparatively large, and active material is fully used thus, and guiding discharge performance is also comparatively excellent.The nano-scale active material specific surface adopting soft chemical method to prepare is larger, and distribution of particles is relatively uniform, and the material formed has good structural stability, is conducive to " deintercalation/embedding " of Li ion, and has high specific capacity.But, when the particle size of material too small (as nanometer range), then material specific surface area can be made to increase, easily reunite when preparing electrode coating material; When preparing electrode slice, active material is difficult to be evenly distributed on electrode slice surface, also can have a negative impact to battery performance.In addition, particle size is too small, and System of Detecting Surface Defects For Material can increase, and electrode polarization rate improves.Consider in conjunction with many factors, porous powder material both can ensure the particle diameter of particle, can promote again dispersed at electrode surface of material.
Porous powder material has higher specific area, shorter lithium ion diffusion length, and electrolyte easily enters positive electrode center by loose structure, electronics and lithium ion is spread conveniently by electrolyte, improves the conductivity of positive electrode.Porous powder material can optimize granular size and structure and morphology simultaneously, improves material electrochemical performance and conductance, becomes the emphasis of research gradually.In order to obtain loose structure, can adopt soft template method, die version method, solwution method etc., to improve the specific area of material, improve electrode performance further.When adopting template, constructor can be obtained and close the material required, but in order to prevent loose structure from caving in, sintering temperature can not be too high, thus make grain crystalline undesirable.
In addition, the conductivity of positive electrode generally has much room for improvement, as coated in carried out carbon to material, can not only improve conductivity, and the coating layer on surface can also play a supportive role to loose structure, and suppresses the dissolving of manganese, thus improves the chemical property of material.
Summary of the invention
Object of the present invention be exactly in order to overcome above-mentioned prior art exist defect and provide a kind of good specific discharge capacity that has, the porous metals adulterated lithium manganate/carbon composite lithium ion battery positive electrode of high rate performance and cycle performance and preparation method.
Object of the present invention can be achieved through the following technical solutions: the preparation method of a kind of porous metals adulterated lithium manganate/carbon composite lithium ion battery positive electrode, it is characterized in that, the method comprises the following steps: be dissolved in by surfactant in absolute ethyl alcohol, stirring obtains gel, then by lithium nitrate, the nitrate of doping metals nitrate and manganese adds wherein, abundant stirring, dry in air dry oven after mixing, calcine in Muffle furnace further, obtained porous adulterated lithium manganate material LiM 0.2mn 1.8o 4, by this LiM 0.2mn 1.8o 4dispersed in glucose solution, calcine in nitrogen atmosphere after forced air drying, obtain metal-doped mangaic acid lithium/carbon composite material LiM 0.2mn 1.8o 4/ C, wherein M refers to doping metals.
Described doping metals is transition metal, comprises iron, cobalt, nickel, manganese, zinc or copper.
Described surfactant comprises cationic surfactant, anion surfactant and non-ionic surface active agent; Surfactant is dissolved in absolute ethyl alcohol and refers to: by surfactant dissolves in absolute ethyl alcohol, make its concentration be 0.05-0.1g/mL.
Described surfactant comprises P123, F127 or cetyl amine bromide.
Described lithium nitrate, the consumption of the nitrate of doping metals nitrate and manganese is: solid Mn (NO 3) 24H 2o, LiNO 3, doping metals nitrate adds according to the ratio of mol ratio 9:5:1, LiNO 3content in described gel is 0.05-0.5mol/L.
Described abundant stirring refers to: by said mixture at room temperature magnetic agitation 12-24h;
In described air dry oven, drying refers to: by the colloidal sol 60-80 DEG C of forced air drying 24-48h in air dry oven mixed;
In described Muffle furnace, calcining refers to: under air atmosphere, Muffle furnace 2-5 DEG C/min is warming up to 500-700 DEG C, insulation 2-4h.
Described glucose solution refers to mixed solution DEXTROSE ANHYDROUS being dissolved in deionized water and absolute ethyl alcohol; The volume ratio of deionized water and absolute ethyl alcohol is 1:3, and the concentration of DEXTROSE ANHYDROUS in the mixed solution of deionized water and absolute ethyl alcohol is 0.06-0.08g/mL.
Described dispersedly refer to magnetic agitation 10-30min, then ultrasonic disperse 10-30min.
In described nitrogen atmosphere, calcining refers to: in nitrogen atmosphere, in tube furnace, 2-5 DEG C/min is warming up to 450-600 DEG C and keeps 2-5h.
A kind of porous metals adulterated lithium manganate/carbon composite lithium ion battery positive electrode adopting described method to prepare.
Compared with prior art, the present invention is template with surfactant first, take nitrate as predecessor, by sol-gal process and nitrates decompose method, completes novel porous LiMn2O4 dopant material LiM 0.2mn 1.8o 4synthesis, achieves and lithium manganate material is improved from composition and structure simultaneously, and it is coated to have carried out carbon to material.Prepared material has good crystallinity, even particle size, and size, at about 20nm, has good specific discharge capacity as anode material of lithium battery, high rate performance and cycle performance.It prepares the preparation that thought can be applied to other porous metal oxide composite material positive electrodes.
Accompanying drawing explanation
Fig. 1 utilizes this surfactant to obtain the scanning electron microscopic picture of LiMn2O4 of carbon-clad metal doping in conjunction with nitrates decompose method for template.
Embodiment
Elaborate to embodiments of the invention below, the present embodiment is implemented under premised on technical solution of the present invention, give detailed execution mode and concrete operating process, but protection scope of the present invention is not limited to following embodiment.
Embodiment 1
Molal weight is that the high molecular polymer p123 of 5800 is dissolved in appropriate absolute ethyl alcohol by the first step, constantly stirs and obtain the P123 gel that the dispersed concentration of 20mL is 0.05g/mL under room temperature.
Second step, solid Mn (NO 3) 24H 2o, LiNO 3, Fe (NO 3) 39H 2o adds according to the ratio of mol ratio 9:5:1, LiNO 3amount be 0.05mol.
3rd step, by said mixture at room temperature middling speed magnetic agitation 12h.
4th step, by the colloidal sol 60 DEG C of forced air drying 24h in air dry oven mixed.
5th step, dried mixture in air atmosphere Muffle furnace 2 DEG C/min is warming up to 500 DEG C, insulation 2h.
6th step, dispersed in the mixed solution that obtained sample is dissolved in 5mL deionized water and 15mL absolute ethyl alcohol in 1.2g DEXTROSE ANHYDROUS, magnetic agitation 10min, then ultrasonic disperse 10min.
7th step, by the mixture 60 DEG C of forced air drying 24h in air dry oven obtained.
8th step, calcine in dried sample nitrogen atmosphere in tube furnace, 2 DEG C/min is warming up to 450 DEG C and keeps 2h.
By test analysis such as XRD, SEM, electro-chemical tests, the LiFe prepared 0.2mn 1.8o 4/ C, grain size is the lower specific discharge capacity of 5-15nm, 0.1C electric discharge is general LiMn 2o 41.3 times, circulation 50 circle after decay to 84.6% of initial capacity.Its scanning electron microscope (SEM) photograph as shown in Figure 1.
Embodiment 2
Molal weight is that the high molecular polymer p123 of 5800 is dissolved in appropriate absolute ethyl alcohol by the first step, constantly stirs and obtain the P123 gel that the dispersed concentration of 20mL is 0.08g/mL under room temperature.
Second step, solid Mn (NO 3) 24H 2o, LiNO 3, Fe (NO 3) 39H 2o adds according to the ratio of mol ratio 9:5:1, LiNO 3amount be 0.1mol.
3rd step, by said mixture at room temperature middling speed magnetic agitation 16h.
4th step, by the colloidal sol 70 DEG C of forced air drying 36h in air dry oven mixed.
5th step, dried mixture in air atmosphere Muffle furnace 3 DEG C/min is warming up to 600 DEG C, insulation 3h.
6th step, dispersed in the mixed solution that obtained sample is dissolved in 5mL deionized water and 15mL absolute ethyl alcohol in 1.4g DEXTROSE ANHYDROUS, magnetic agitation 20min, then ultrasonic disperse 20min.
7th step, by the mixture 60 DEG C of forced air drying 24h in air dry oven obtained.
8th step, calcine in dried sample nitrogen atmosphere in tube furnace, 3 DEG C/min is warming up to 550 DEG C and keeps 3h.
By test analysis such as XRD, SEM, electro-chemical tests, the LiFe prepared 0.2mn 1.8o 4/ C, grain size is the lower specific discharge capacity of 35-45nm, 0.1C electric discharge is general LiMn 2o 41.9 times, circulation 50 circle after decay to 93.3% of initial capacity.
Embodiment 3
Molal weight is that the high molecular polymer p123 of 5800 is dissolved in appropriate absolute ethyl alcohol by the first step, constantly stirs and obtain the P123 gel that the dispersed concentration of 20mL is 0.1g/mL under room temperature.
Second step, solid Mn (NO 3) 24H 2o, LiNO 3, Fe (NO 3) 39H 2o adds according to the ratio of mol ratio 9:5:1, LiNO 3amount be 0.5mol.
3rd step, by said mixture at room temperature middling speed magnetic agitation 24h.
4th step, by the colloidal sol 80 DEG C of forced air drying 48h in air dry oven mixed.
5th step, dried mixture in air atmosphere Muffle furnace 5 DEG C/min is warming up to 700 DEG C, insulation 4h.
6th step, dispersed in the mixed solution that obtained sample is dissolved in 5mL deionized water and 15mL absolute ethyl alcohol in 1.6g DEXTROSE ANHYDROUS, magnetic agitation 30min, then ultrasonic disperse 30min.
7th step, by the mixture 60 DEG C of forced air drying 24h in air dry oven obtained.
8th step, calcine in dried sample nitrogen atmosphere in tube furnace, 5 DEG C/min is warming up to 600 DEG C and keeps 5h.
By test analysis such as XRD, SEM, electro-chemical tests, the LiFe prepared 0.2mn 1.8o 4/ C, grain size is the lower specific discharge capacity of 20-30nm, 0.1C electric discharge is general LiMn 2o 41.5 times, circulation 50 circle after decay to 89.8% of initial capacity.

Claims (10)

1. the preparation method of porous metals adulterated lithium manganate/carbon composite lithium ion battery positive electrode, it is characterized in that, the method comprises the following steps: be dissolved in by surfactant in absolute ethyl alcohol, stirring obtains gel, and then by lithium nitrate, the nitrate of doping metals nitrate and manganese adds wherein, abundant stirring, dry in air dry oven after mixing, calcine in Muffle furnace further, obtained porous adulterated lithium manganate material LiM 0.2mn 1.8o 4, by this LiM 0.2mn 1.8o 4dispersed in glucose solution, calcine in nitrogen atmosphere after forced air drying, obtain metal-doped mangaic acid lithium/carbon composite material LiM 0.2mn 1.8o 4/ C, wherein M refers to doping metals.
2. the preparation method of a kind of porous metals adulterated lithium manganate/carbon composite lithium ion battery positive electrode according to claim 1, it is characterized in that, described doping metals is transition metal, comprises iron, cobalt, nickel, manganese, zinc or copper.
3. the preparation method of a kind of porous metals adulterated lithium manganate/carbon composite lithium ion battery positive electrode according to claim 1, it is characterized in that, described surfactant comprises cationic surfactant, anion surfactant and non-ionic surface active agent; Surfactant is dissolved in absolute ethyl alcohol and refers to: by surfactant dissolves in absolute ethyl alcohol, make its concentration be 0.05-0.1g/mL.
4. the preparation method of a kind of porous metals adulterated lithium manganate/carbon composite lithium ion battery positive electrode according to claim 1 or 3, it is characterized in that, described surfactant comprises P123, F127 or cetyl amine bromide.
5. the preparation method of a kind of porous metals adulterated lithium manganate/carbon composite lithium ion battery positive electrode according to claim 1, it is characterized in that, described lithium nitrate, the consumption of the nitrate of doping metals nitrate and manganese is: solid Mn (NO 3) 24H 2o, LiNO 3, doping metals nitrate adds according to the ratio of mol ratio 9:5:1, LiNO 3content in described gel is 0.05-0.5mol/L.
6. the preparation method of a kind of porous metals adulterated lithium manganate/carbon composite lithium ion battery positive electrode according to claim 1, it is characterized in that, described abundant stirring refers to: by said mixture at room temperature magnetic agitation 12-24h;
In described air dry oven, drying refers to: by the colloidal sol 60-80 DEG C of forced air drying 24-48h in air dry oven mixed;
In described Muffle furnace, calcining refers to: under air atmosphere, Muffle furnace 2-5 DEG C/min is warming up to 500-700 DEG C, insulation 2-4h.
7. the preparation method of a kind of porous metals adulterated lithium manganate/carbon composite lithium ion battery positive electrode according to claim 1, it is characterized in that, described glucose solution refers to mixed solution DEXTROSE ANHYDROUS being dissolved in deionized water and absolute ethyl alcohol; The volume ratio of deionized water and absolute ethyl alcohol is 1:3, and the concentration of DEXTROSE ANHYDROUS in the mixed solution of deionized water and absolute ethyl alcohol is 0.06-0.08g/mL.
8. the preparation method of a kind of porous metals adulterated lithium manganate/carbon composite lithium ion battery positive electrode according to claim 1, is characterized in that, described dispersedly refers to magnetic agitation 10-30min, then ultrasonic disperse 10-30min.
9. the preparation method of a kind of porous metals adulterated lithium manganate/carbon composite lithium ion battery positive electrode according to claim 1, it is characterized in that, in described nitrogen atmosphere, calcining refers to: in nitrogen atmosphere, in tube furnace, 2-5 DEG C/min is warming up to 450-600 DEG C and keeps 2-5h.
10. the porous metals adulterated lithium manganate/carbon composite lithium ion battery positive electrode adopting the arbitrary described method of claim 1 ~ 9 to prepare.
CN201510152217.9A 2015-04-01 2015-04-01 Porous metallic cathode material doped with lithium manganate/carbon for composite lithium batteries, and preparation method of porous metallic cathode material Pending CN104795557A (en)

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CN107946589A (en) * 2017-11-28 2018-04-20 安徽零度新能源科技有限公司 A kind of positive electrode that can reduce electrode of lithium cell polarization phenomena

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CN105206799A (en) * 2015-08-19 2015-12-30 上海交通大学 Preparation method of porous metal doped lithium manganate/graphene lithium battery positive electrode material
CN106684369A (en) * 2017-02-16 2017-05-17 长沙理工大学 Sodium super ionic conductor-inlaid and coated positive electrode material for sodium-ion battery and synthesis method of positive electrode material
CN106684369B (en) * 2017-02-16 2019-10-15 长沙理工大学 A kind of Fast ion conductor inlays the sodium-ion battery positive material and its synthetic method of cladding
CN107946589A (en) * 2017-11-28 2018-04-20 安徽零度新能源科技有限公司 A kind of positive electrode that can reduce electrode of lithium cell polarization phenomena

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