CN104966829A - Lithium battery carbon and nitrogen nanotube / lithium manganate electrode material preparation method - Google Patents
Lithium battery carbon and nitrogen nanotube / lithium manganate electrode material preparation method Download PDFInfo
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- CN104966829A CN104966829A CN201510248746.9A CN201510248746A CN104966829A CN 104966829 A CN104966829 A CN 104966829A CN 201510248746 A CN201510248746 A CN 201510248746A CN 104966829 A CN104966829 A CN 104966829A
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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
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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
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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
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
- H01M4/625—Carbon or graphite
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- 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 present invention discloses a lithium battery carbon and nitrogen nanotube / lithium manganate electrode material and a preparation method thereof, and the preparation method comprises the following steps: (1) carbon and nitrogen nanotubes are ultrasonically dispersed in a lower alcohol solution; (2) lithium manganate or a mixture of lithium and manganese salts is ultrasonically dispersed in a lower alcohol solution; (4) the dispersed material of the step (2) is added into the dispersed carbon and nitrogen nanotube alcohol solution, and the mixture is mixed, ultrasonically treated for a plurality of times, and is placed in an oven for drying; (5) the died mixture is thermally treated in inert atmosphere N2 or Ar to obtain an active material; (6) the thermally treated active material, conductive agent Super-p and binder polyvinylidene fluoride are mixed proportionally to obtain the carbon and nitrogen nanotube / lithium manganate electrode material. The carbon and nitrogen nanotube / lithium manganate electrode material is simple in process, low in cost, mild in conditions, and environment-friendly, large-scale production is easy to implement, and the prepared carbon and nitrogen nanotube / lithium manganate electrode material has high rate performance and long cycle life.
Description
Technical field
The present invention relates to a kind of preparation method of anode material for lithium-ion batteries, particularly a kind of preparation method of lithium battery carbon-nitrogen nano tube/manganic acid lithium electrode material.
Background technology
Along with the problems such as energy crisis, environmental pollution, climate warming become increasingly conspicuous, an urgent demand we develop green novel energy source, as solar energy, wind energy, geothermal energy, nuclear energy, tidal energy, long-life secondary cell etc.Lithium ion battery is a kind of novel secondary battery of alternative lead-acid battery, has high-energy-density, can discharge and recharge often, the advantages such as security performance is good, environmentally friendly.Lithium ion battery is primarily of positive electrode, and negative material, electrolyte and barrier film are formed, and wherein positive electrode constrains lithium ion battery overall performance to a great extent and promotes further, and therefore, developmental research positive electrode more and more comes into one's own.
LiMn2O4 (LMO), as a kind of novel anode material for lithium-ion batteries, has many advantages, and promoter manganese is abundant, it is cheap, and environmental pollution is less, and lithium manganate battery security performance is excellent.But due to the conductivity that it is lower, cause it when heavy-current discharge, its capacity and life-span can obviously reduce, so make rate charge-discharge characteristic and useful life limited.Be mainly used in electronics field now, and market scale larger electric vehicle field application scale still very little.Thus reduced costs into key, from LiMn2O4 angle, the fast and efficient production realizing LiMn2O4 is very important.Corrective measure mainly concentrates on aspects such as reducing production cost, raising product gram volume, high rate performance and cyclical stability.
Carbon nano-tube (CNTs) is a kind of one-dimensional material with special construction, can think seamless, the hollow " microtubule " that are reeled around central shaft by certain spiral angle by single or multiple lift graphite flake visually.The seamless pipe structure that the one-dimensional hollow graphite aspect that carbon nano-tube has uniqueness because of it is curled into, thus there is a series of outstanding character, if the chemical stability of height and thermal stability, high mechanical strength, special electric property are (according to the difference of caliber and helicity, can be the conductor not worse than copper, also can be semiconductor), it is the material that a class has applications well prospect.Carbon nano-tube, as conductive agent, is added in anode material for lithium-ion batteries and can be formed the very little conductive network of a specific insulation in positive electrode, can significantly improve the conductivity of positive electrode.
Research finds (ACS Catal. 2014,4,613), in CNTs, atom N (nitrogen-doped carbon nanometer pipe is introduced, NCNTs) significantly can increase the conductivity of material, surface wettability and mechanical strength, NCNTs is not needing surface preparation with active component compound tense simultaneously.At present, mostly existing patent is to adopt CNTs modification manganate cathode material for lithium, and the conductivity of its material is improved to some extent.But this material adopts traditional high temperature solid-state method synthesis, and energy consumption is high, preparation time is long, lot stability is poor, gram volume is on the low side, cycle life is short.In addition, carbon nano-tube needs surperficial acidifying or esterification treatment before using, and process is complicated and unfriendly to environment, in order to dispersed needs thing realize carbon nano-tube adds expensive dispersant (TNWDIS or SDS etc.).The volume energy density of lithium ion battery can be reduced like this and increase cost.
Summary of the invention
For making up the deficiencies in the prior art; the invention provides a kind of preparation technology simple; mild condition, environmental friendliness, with low cost, be easy to accomplish scale production and the preparation method of the lithium battery carbon-nitrogen nano tube/manganic acid lithium electrode material of rate charge-discharge performance and cycle life excellence.
The present invention is achieved through the following technical solutions:
A kind of lithium battery carbon-nitrogen nano tube/manganic acid lithium electrode material and preparation method thereof, its special character is: comprise the following steps:
(1) by carbon-nitrogen nano tube ultrasonic disperse in low-alcohol solution;
(2) by LiMn2O4 ultrasonic disperse in low-alcohol solution;
(3) be dissolved in low-alcohol solution after lithium salts and manganese salt being mixed according to mol ratio 0.1-5;
(4) material in step (2) or (3) is joined in scattered carbon-nitrogen nano tube alcoholic solution, then through stirring, ultrasonic several times, be placed in baking oven and dry;
(5) compound after drying is at inert atmosphere N
2or heat treatment obtains active material under Ar;
(6) active material after heat treatment and conductive agent Super-p, binding agent Kynoar are according to (90-95): (1-5): the ratio of (1-5) mixes and obtains carbon-nitrogen nano tube/manganic acid lithium electrode material.
Described in step (1), (2) and (3), low-alcohol solution is one or both the mixed liquor in methyl alcohol, ethanol, propyl alcohol, and in low-alcohol solution, the volume fraction of alcohol is 0-50%; Described in step (1), carbon-nitrogen nano tube is the carbon nano-tube of N doping.
Described in step (3), lithium salts can be one or more in the lithium salts such as lithium hydroxide, lithium acetate, lithium carbonate, and manganese salt can be manganese nitrate, manganese acetate, manganese carbonate, one or more in manganese dioxide or mangano-manganic oxide.
Ratio in step (4) in compound shared by carbon-nitrogen nano tube is 0-10 wt%.
In step (5), heat treated temperature is 100-800 DEG C, and heat treatment time is 0.1-3 h.
Described in step (6), the proportion of active material in carbon-nitrogen nano tube/manganic acid lithium electrode material is 90-97%, and conductive agent proportion is 0-5%.
Compared with prior art, the invention has the beneficial effects as follows:
1) this carbon-nitrogen nano tube/manganic acid lithium electrode material can be that carbon-nitrogen nano tube and LiMn2O4 reprocessing compound prepare, and also can be to prepare with carbon-nitrogen nano tube compound in LiMn2O4 building-up process.
2) use carbon-nitrogen nano tube not need to do surface preparation, technique is simple, mild condition, environmental friendliness, is easy to accomplish scale production.
3) do not need in process to add expensive Carbon nano-tube dispersant, with low cost.
4) use carbon-nitrogen nano tube can greatly reduce battery polarization internal resistance, realize big current multiplying power discharging, and keep high discharge capacity and long cycle life.
Accompanying drawing explanation
Accompanying drawing 1 is the SEM figure of fabricated in situ carbon-nitrogen nano tube/manganic acid lithium electrode material.
Accompanying drawing 2 is the XRD figure of fabricated in situ carbon-nitrogen nano tube/manganic acid lithium electrode material.
The XRD figure of carbon-nitrogen nano tube/manganic acid lithium electrode material that accompanying drawing 3 is prepared for reprocessing.
The particle size distribution figure of carbon-nitrogen nano tube/manganic acid lithium electrode material that accompanying drawing 4 is prepared for reprocessing.
Accompanying drawing 5 is the high rate performance figure of carbon-nitrogen nano tube/manganic acid lithium electrode material.
Accompanying drawing 6 is stable circulation performance figure under carbon-nitrogen nano tube/manganic acid lithium electrode material 5C multiplying power.
Embodiment
Below in conjunction with the drawings and specific embodiments, the present invention is further detailed explanation.
Embodiment 1
It is that 0.5 wt% carbon-nitrogen nano tube modifies lithium manganate material 0.5wt% NCNTs/LMO that content is prepared in reprocessing:
(1) carbon-nitrogen nano tube taking 0.5 gram is placed in absolute ethyl alcohol ultrasonic disperse 1 h that concentration is 50%.
(2) LiMn2O4 taking 99.5 grams is placed in 50% absolute ethyl alcohol ultrasonic disperse 1 h.
(3) added to by carbon-nitrogen nano tube in the manganate cathode material for lithium after ultrasonic disperse, compound through stirring, ultrasonic several times, is placed in baking oven and dries again.
(4) compound after drying is at N
2lower 300 DEG C of heat treatment 1 h of atmosphere.
(5) material after heat treatment and conductive agent Super-p, binding agent Kynoar mix according to the ratio of 94.5:3:2.5 and obtain carbon-nitrogen nano tube/manganic acid lithium electrode material 0.5wt% NCNTs/LMO.
Above-mentioned obtained carbon-nitrogen nano tube/manganic acid lithium electrode material 0.5 wt% NCNTs/LMO carries out performance test, and first discharge specific capacity is 114.3 mAh/g, first efficiency 90.5%; Under 5C multiplying power, specific discharge capacity is 89.9 mAh/g.
Embodiment 2
It is that 2 wt% carbon-nitrogen nano tubes modify lithium manganate material 2 wt% NCNTs/LMO that content is prepared in reprocessing:
(1) carbon-nitrogen nano tube taking 2 grams is placed in absolute ethyl alcohol ultrasonic disperse 1 h that concentration is 50%.
(2) LiMn2O4 taking 98 grams is placed in absolute ethyl alcohol ultrasonic disperse 1 h.
(3) added to by carbon-nitrogen nano tube in the manganate cathode material for lithium after ultrasonic disperse, compound through stirring, ultrasonic several times, is placed in baking oven and dries again.
(4) compound after drying is at N
2lower 300 DEG C of heat treatment 1 h of atmosphere.
(5) material after heat treatment and conductive agent Super-p, binding agent Kynoar mix according to the ratio of 94.5:3:2.5 and obtain carbon-nitrogen nano tube/manganic acid lithium electrode material 2wt% NCNTs/LMO.
Above-mentioned obtained carbon-nitrogen nano tube/manganic acid lithium electrode material 2wt% NCNTs/LMO carries out lithium battery performance test, and first discharge specific capacity is 115.8 mAh/g, first efficiency 91.2%; Under 5C multiplying power, specific discharge capacity is 95.2 mAh/g.
Embodiment 3
It is that 5 wt% carbon-nitrogen nano tubes modify lithium manganate material 5 wt% NCNTs/LMO that content is prepared in reprocessing:
(1) carbon-nitrogen nano tube taking 5 grams is placed in absolute ethyl alcohol ultrasonic disperse 1 h that concentration is 50%.
(2) LiMn2O4 taking 95 grams is placed in absolute ethyl alcohol ultrasonic disperse 1 h.
(3) added to by carbon-nitrogen nano tube in the manganate cathode material for lithium after ultrasonic disperse, compound through stirring, ultrasonic several times, is placed in baking oven and dries again.
(4) compound after drying is at N
2lower 300 DEG C of heat treatment 1 h of atmosphere.
(5) material after heat treatment and conductive agent Super-p, binding agent Kynoar mix according to the ratio of 94.5:3:2.5 and obtain carbon-nitrogen nano tube/manganic acid lithium electrode material 5wt% NCNTs/LMO.
Above-mentioned obtained carbon-nitrogen nano tube/manganic acid lithium electrode material 5wt% NCNTs/LMO carries out lithium battery performance test, and first discharge specific capacity is 116.3 mAh/g, first efficiency 94.2%; Under 5C multiplying power, specific discharge capacity is 100.5 mAh/g.
Embodiment 4
It is that 10 wt% carbon-nitrogen nano tubes modify lithium manganate material 10wt% NCNTs/LMO that content is prepared in reprocessing:
(1) carbon-nitrogen nano tube taking 10 grams is placed in absolute ethyl alcohol ultrasonic disperse 1 h that concentration is 50%.
(2) LiMn2O4 taking 90 grams is placed in absolute ethyl alcohol ultrasonic disperse 1 h.
(3) added to by carbon-nitrogen nano tube in the manganate cathode material for lithium after ultrasonic disperse, compound through stirring, ultrasonic several times, is placed in baking oven and dries again.
(4) compound after drying is at N
2lower 300 DEG C of heat treatment 1 h of atmosphere.
(5) material after heat treatment and conductive agent Super-p, binding agent Kynoar mix according to the ratio of 94.5:3:2.5 and obtain carbon-nitrogen nano tube/manganic acid lithium electrode material 10wt% NCNTs/LMO.
Above-mentioned obtained carbon-nitrogen nano tube/manganic acid lithium electrode material 10wt% NCNTs/LMO carries out lithium battery performance test, and first discharge specific capacity is 98.5 mAh/g, first efficiency 90.2%; Under 5C multiplying power, specific discharge capacity is 86.1 mAh/g.
Embodiment 5
Fabricated in situ content is that 0.5 wt% carbon-nitrogen nano tube modifies lithium manganate material 0.5wt% NCNTs/LMO:
(1) carbon-nitrogen nano tube taking 0.05 gram is placed in absolute ethyl alcohol ultrasonic disperse 1 h that concentration is 50%.
(2) lithium acetate of 5.6 grams is taken and the manganese acetate of 26.9 grams is dissolved in the absolute ethyl alcohol of 50%.
(3) carbon-nitrogen nano tube after dispersion is added in the mixed liquor of lithium salts and manganese salt again through stirring, ultrasonic several times, be placed in baking oven and dry.
(4) compound after drying is at N
2lower 700 DEG C of heat treatment 1 h of atmosphere.
(5) material after heat treatment and conductive agent Super-p, binding agent Kynoar mix according to the ratio of 94.5:3:2.5 and obtain carbon-nitrogen nano tube/manganic acid lithium electrode material 0.5 wt% NCNTs/LMO.
Above-mentioned obtained carbon-nitrogen nano tube/manganic acid lithium electrode material 0.5 wt% NCNTs/LMO carries out performance test, and first discharge specific capacity is 110.0 mAh/g, first efficiency 91.2%; Under 5C multiplying power, specific discharge capacity is 88.1 mAh/g.
Embodiment 6
Fabricated in situ content is that 2 wt% carbon-nitrogen nano tubes modify lithium manganate material 2wt% NCNTs/LMO:
(1) carbon-nitrogen nano tube taking 0.2 gram is placed in absolute ethyl alcohol ultrasonic disperse 1 h that concentration is 50%.
(2) lithium acetate of 5.5 grams is taken and the manganese acetate of 26.5 grams is dissolved in the absolute ethyl alcohol of 50%.
(3) carbon-nitrogen nano tube after dispersion is added in the mixed liquor of lithium salts and manganese salt again through stirring, ultrasonic several times, be placed in baking oven and dry.
(4) compound after drying is at N
2lower 700 DEG C of heat treatment 1 h of atmosphere.
(5) material after heat treatment and conductive agent Super-p, binding agent Kynoar mix according to the ratio of 94.5:3:2.5 and obtain carbon-nitrogen nano tube/manganic acid lithium electrode material 2wt% NCNTs/LMO.
Above-mentioned obtained carbon-nitrogen nano tube/manganic acid lithium electrode material 2wt% NCNTs/LMO carries out lithium battery performance test, and first discharge specific capacity is 114.0 mAh/g, first efficiency 92.2%; Under 5C multiplying power, specific discharge capacity is 95.1 mAh/g.
Embodiment 7
Fabricated in situ content is that 5 wt% carbon-nitrogen nano tubes modify lithium manganate material 5wt% NCNTs/LMO:
(1) carbon-nitrogen nano tube taking 0.5 gram is placed in absolute ethyl alcohol ultrasonic disperse 1 h that concentration is 50%.
(2) lithium acetate of 5.4 grams is taken and the manganese acetate of 25.7 grams is dissolved in the absolute ethyl alcohol of 50%.
(3) then the carbon-nitrogen nano tube after dispersion is added in the mixed liquor of lithium salts and manganese salt again through stirring, ultrasonic several times, be placed in baking oven and dry.
(4) compound after drying is at N
2lower 700 DEG C of heat treatment 1 h of atmosphere.
(5) material after heat treatment and conductive agent Super-p, binding agent Kynoar mix according to the ratio of 94.5:3:2.5 and obtain carbon-nitrogen nano tube/manganic acid lithium electrode material 5wt% NCNTs/LMO.
Above-mentioned obtained carbon-nitrogen nano tube/manganic acid lithium electrode material 5wt% NCNTs/LMO carries out lithium battery performance test, and first discharge specific capacity is 115.8 mAh/g, first efficiency 93.2%; Under 5C multiplying power, specific discharge capacity is 98.1 mAh/g.
Claims (7)
1. lithium battery carbon-nitrogen nano tube/manganic acid lithium electrode material and preparation method thereof, is characterized in that: comprise the following steps:
(1) by carbon-nitrogen nano tube ultrasonic disperse in low-alcohol solution;
(2) by LiMn2O4 ultrasonic disperse in low-alcohol solution;
(3) be dissolved in low-alcohol solution after lithium salts and manganese salt being mixed according to mol ratio 0.1-5;
(4) material in step (2) or (3) is joined in scattered carbon-nitrogen nano tube alcoholic solution, then through stirring, ultrasonic several times, be placed in baking oven and dry;
(5) compound after drying is at inert atmosphere N
2or heat treatment obtains active material under Ar;
(6) active material after heat treatment and conductive agent Super-p, binding agent Kynoar are according to (90-95): (1-5): the ratio of (1-5) mixes and obtains carbon-nitrogen nano tube/manganic acid lithium electrode material.
2. a kind of lithium battery carbon-nitrogen nano tube/manganic acid lithium electrode material according to claim 1 and preparation method thereof, is characterized in that: low-alcohol solution described in step (1), (2) and (3) is one or both the mixed liquor in methyl alcohol, ethanol, propyl alcohol.
3. a kind of lithium battery carbon-nitrogen nano tube/manganic acid lithium electrode material according to claim 1 and 2 and preparation method thereof, is characterized in that: in low-alcohol solution described in step (1), (2) and (3), the volume fraction of alcohol is 0-50%.
4. a kind of lithium battery carbon-nitrogen nano tube/manganic acid lithium electrode material according to claim 1 and preparation method thereof, it is characterized in that: lithium salts described in step (3) can be one or more in the lithium salts such as lithium hydroxide, lithium acetate, lithium carbonate, manganese salt can be manganese nitrate, manganese acetate, manganese carbonate, one or more in manganese dioxide or mangano-manganic oxide.
5. a kind of lithium battery carbon-nitrogen nano tube/manganic acid lithium electrode material according to claim 1 and preparation method thereof, is characterized in that: the ratio in step (4) in compound shared by carbon-nitrogen nano tube is 0-10 wt%.
6. a kind of lithium battery carbon-nitrogen nano tube/manganic acid lithium electrode material according to claim 1 and preparation method thereof, it is characterized in that: in step (5), heat treated temperature is 100-800 DEG C, heat treatment time is 0.1-3 h.
7. a kind of lithium battery carbon-nitrogen nano tube/manganic acid lithium electrode material according to claim 1 and preparation method thereof, it is characterized in that: described in step (6), the proportion of active material in carbon-nitrogen nano tube/manganic acid lithium electrode material is 90-97%, conductive agent proportion is 0-5%.
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Application publication date: 20151007 |