CN103928672A - Anode active substance for lithium ion battery and preparation method thereof - Google Patents

Anode active substance for lithium ion battery and preparation method thereof Download PDF

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Publication number
CN103928672A
CN103928672A CN201410145083.3A CN201410145083A CN103928672A CN 103928672 A CN103928672 A CN 103928672A CN 201410145083 A CN201410145083 A CN 201410145083A CN 103928672 A CN103928672 A CN 103928672A
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lithium
ion battery
lithium ion
manganese
mno
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CN103928672B (en
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余志勇
吴莎
刘韩星
王壮
郑振宁
孙念
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Wuhan University of Technology WUT
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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
    • 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
    • H01M4/131—Electrodes based on mixed oxides or hydroxides, or on mixtures of oxides or hydroxides, e.g. LiCoOx
    • H01M4/1315—Electrodes based on mixed oxides or hydroxides, or on mixtures of oxides or hydroxides, e.g. LiCoOx containing halogen atoms, e.g. 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
    • H01M4/36—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
    • 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
    • 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
    • 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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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Composite Materials (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Battery Electrode And Active Subsutance (AREA)

Abstract

The invention provides an anode active substance for a lithium ion battery and a preparation method thereof. The anode active substance is fluorine-doped Li2MnO3; the composition formula is Li2MnO3-xFx and x is more than or equal to 0.03 and less than or equal to 0.12. The preparation method is simple; according to the battery produced by the preparation method, the first-time specific discharge capacity is 172.4-209.1mAh/g when the current density is 5mA/g, and keeps 112.7-139.9mAh/g after 20 times of cycles; the retention rate is 58.6-66.9%.

Description

A kind of positive active material and preparation method thereof for lithium ion battery
Technical field
The invention belongs to battery manufacture technical field, be specifically related to a kind of lithium ion battery positive active material and preparation method thereof.
Background technology
Along with the exhaustion day by day of fossil fuel, and the fast development of portable electric appts and electric vehicle, the research of the new forms of energy such as power-supply battery has become the focus of global concern, wherein lithium ion battery because its voltage is high, specific energy is high, discharge and recharge time length, memory-less effect, environmental pollution are little, quick charge, the excellent specific property such as have extended cycle life are used widely.On lithium ion battery structure, mainly comprise pole piece and nonaqueous electrolytic solution, described pole piece and nonaqueous electrolytic solution are sealed in battery container, described pole piece comprises positive pole, negative pole and the barrier film between positive pole and negative pole, described positive pole comprises collector body and loads on the positive electrode on collector body, and positive electrode comprises positive active material and adhesive.
Anode material for lithium-ion batteries, as the important component part of lithium ion battery, is all domestic and international scientific worker's study hotspot all the time.In recent years, along with the continuous expansion in development in science and technology and lithium ion battery applications field, people have higher requirement to the energy density of anode material for lithium-ion batteries, and therefore high theoretical capacity positive active material has caused researcher's extensive concern.At present commercialization or study more positive active material and comprise LiCoO 2, LiNiO 2, LiMn 2o 4and LiFePO 4deng, but be subject to materials theory capacity limit, be difficult to meet the demand of social development to lithium ion battery with high energy density.
Li 2mnO 3sill is the novel active substance of lithium ion battery anode of a class, because the advantages such as its theoretical capacity is high, with low cost, environmentally friendly become the focus that positive electrode is paid close attention to.It is generally acknowledged pure Li 2mnO 3electro-chemical activity is poor, and specific discharge capacity is very low.At present, main by forming Li 2mnO 3-LiMO 2(M=Ni, Co, Mn etc.) solid solution improves its performance, shows high specific discharge capacity.But the raw material Co that this class material adopts, Ni etc. are comparatively expensive, and synthesis temperature is high, and the stability of material in cyclic process is good not.
Summary of the invention
Technical problem to be solved by this invention is for above shortcomings in prior art, and a kind of lithium ion battery positive active material and preparation method thereof is provided, and cost of material is low, and technique is simple, and synthesis temperature is low, the Li of prepared fluorine doping 2mnO 3stable in properties, has improved anode material for lithium-ion batteries Li 2mnO 3chemical property, corresponding lithium ion battery specific capacity is large, good cycle.
The technical scheme that solution the technology of the present invention problem adopts is that this lithium ion battery positive active material is the Li of fluorine doping 2mnO 3, its composition formula is: Li 2mnO 3-xf x(0.03≤x≤0.12).
The present invention also provides the preparation method of above-mentioned lithium ion battery positive active material, it is characterized in that comprising the following steps:
(1) weigh lithium salts, manganese salt and lithium fluoride (0.03≤x≤0.12), be dissolved in and in deionized water, be mixed with salting liquid, described lithium salts is in lithium, manganese salt is in manganese, lithium salts, the mol ratio of manganese salt and lithium fluoride is 2-x:1:x, in salting liquid, manganese element molar concentration is 2～5mol/L, the aqueous citric acid solution that is 3～6mol/L by concentration adds in aforementioned salt solution and forms mixed solution, in citric acid and salting liquid, the mol ratio of metal cation is 0.5～1.5:1, regulate mixed solution pH value to 7～9 with ammoniacal liquor subsequently, again mixed solution is stirred 6～8 hours at 60～80 DEG C, make solution that sufficient complexing occur, form colloidal sol, obtain liquid precursor,
(2) step (1) gained liquid precursor is heated to 8～12h 60～80 DEG C of heating after 16～24 hours at 130～150 DEG C, obtain solid precursor;
(3) step (2) gained solid precursor is calcined at 450～500 DEG C after 3～7 minutes and ground, obtain Powdered presoma, again the pre-burning at 300～350 DEG C of Powdered presoma was heated to 600～700 DEG C with the programming rate of 2-4 DEG C/min after 1～2 hour, and be incubated 9～15h, obtain the Li of fluorine doping after cooling with stove 2mnO 3, obtain lithium ion battery positive active material.
The present invention program adopts the F ion part that bond energy is larger to replace O ion, makes positive electrode structure more stable, and has improved the chemical property of material.The method is by lithium salts, manganese salt, lithium fluoride and citric acid and deionized water are evenly mixed with to liquid precursor, and liquid towards presoma adds the dry rear solid precursor obtaining of thermal agitation and carries out pre-burning and calcination processing acquisition end product.
Press such scheme, the described lithium salts of step (1) comprises any one in lithium nitrate, lithium carbonate, lithium acetate; Described manganese salt comprises any one in manganese nitrate, manganese carbonate, manganese acetate.
The present invention also comprises according to above-mentioned and states lithium ion battery that lithium ion battery prepared by method prepares with positive active material with anodal, and uses this anodal lithium ion battery.
The invention has the beneficial effects as follows: use simple and easy method to prepare lithium ion battery positive active material, improved Li 2mnO 3chemical property.There is marked improvement improving aspect the specific capacity of lithium ion battery and cycle performance, by the battery of made of the present invention, in the time that current density is 5mA/g, first discharge specific capacity reaches 172.4～209.1mAh/g, after 20 circulations, remain on 112.7～139.9mAh/g, conservation rate is that 58.6～66.9%(adopts unadulterated Li 2mnO 3battery first discharge specific capacity be 154.2mAh/g; Circulate after 20 times and remain on 77.8mAh/g, capability retention is 50.4%).
Brief description of the drawings
Fig. 1 is the prepared Li of comparative example 1 of the present invention 2mnO 3xRD collection of illustrative plates;
Fig. 2 is the Li of the prepared fluorine doping of the embodiment of the present invention one 2mnO 3the figure of discharge capacity first under 5mA/g current density;
Fig. 3 is the Li of the prepared fluorine doping of the embodiment of the present invention one 2mnO 3cycle performance figure under 5mA/g current density.
Embodiment
For making those skilled in the art understand better technical scheme of the present invention, below in conjunction with accompanying drawing, the present invention is described in further detail.
The embodiment of the present invention provides a kind of lithium ion battery positive active material with good chemical property.
Comparative example 1
Take 5.5160gLiNO 3, 7.1576gMn (NO 3) 2be dissolved in 10ml deionized water and form salting liquid, by 12.6718g citric acid with adding in aforementioned salt solution and form mixed solution after 10ml deionized water dissolving, with ammoniacal liquor adjustment mixed solution pH to 8, subsequently mixed solution is placed on to 60 DEG C of lasting stirrings 8 hours of constant temperature on magnetic force heating stirrer, obtains liquid precursor.By liquid precursor be placed in drying box in 80 DEG C after dry 16 hours at 150 DEG C the dry solid precursor that obtains for 12 hours, solid precursor is placed on and in Muffle furnace, at 500 DEG C, calcines the presoma that is ground into powder after 3 minutes, be heated to 600 DEG C of insulation 12h with the programming rate of 2 DEG C/min after Powdered presoma is incubated to one hour at 300 DEG C to obtain Li 2mnO 3.
The XRD collection of illustrative plates of this comparative example gained solid product as shown in Figure 1, its main diffraction maximum and Li 2mnO 3standard diagram (01-084-1634) coincide.
The positive active material Li that adopts this comparative example to prepare 2mnO 3mix by the mass ratio of 80:12:8 with conductive agent acetylene black and bonding agent polyvinylidene fluoride (PVDF1300), be dissolved in (Li in solvent 1-METHYLPYRROLIDONE (NMP) 2mnO 3-xf xwith NMP mass ratio be 1:3), stir into pasty state positive electrode coating, be evenly coated on the stainless steel substrate of diameter 14.8mm.The positive plate coating is placed in to vacuum drying chamber, and at 80 DEG C, vacuumize can be used for the assembling of battery for 12 hours later.
In the MBRAUN glove box that is full of high-purity argon gas, carry out anhydrous, the anaerobic assembling (wherein the content of moisture is less than 1ppm, and the content of oxygen is less than 1ppm) of lithium ion battery.Assembling sequence is followed successively by negative electrode casing, currect collecting net, metal lithium sheet negative pole, barrier film, electrolyte (EC:DMC=1:2), Li from top to bottom 2mnO 3-xf xpositive plate, currect collecting net, anode cover, finally use MSK-110 battery sealing machine packaged battery.After the CR2025 type button normal temperature battery standing 24h being assembled into, carry out electro-chemical test.Adopt Land CT2001A battery test system, the specific discharge capacity of characterizing battery, cyclical stability (voltage 2.0-4.8V).
Test result shows, under the current density of 5mA/g, and Li 2mnO 3first discharge specific capacity be 154.2mAh/g, the capacity after 20 times that circulates is 77.8mAh/g, the conservation rate of capacity is 50.4%.
Embodiment mono-
Take 2.9113gLi 2cO 3, 7.1576gMn (NO 3) 2and 0.0314gLiF is dissolved in 10ml deionization and forms salting liquid, after 12.6718g citric acid is dissolved with 10ml deionization, add in aforementioned salt solution and form mixed solution, with ammoniacal liquor adjustment mixed solution pH to 8, subsequently mixed solution is placed on to 60 DEG C of lasting stirrings 8 hours of constant temperature on magnetic force heating stirrer, obtains liquid precursor.By liquid precursor be placed in drying box in 80 DEG C after dry 16 hours at 150 DEG C the dry solid precursor that obtains for 12 hours, solid precursor is placed on and in Muffle furnace, at 500 DEG C, calcines the presoma that is ground into powder after 3 minutes, Powdered presoma is incubated at 300 DEG C after one hour to the Li that is heated to 600 DEG C of insulation 12h and obtains fluorine doping with the heating rate of 2 DEG C/min 2mnO 3(Li 2mnO 2.97f 0.03).
Adopt the method identical with comparative example 1 to prepare CR2025 type button normal temperature battery, its capacity, high rate performance, cyclical stability are tested to (voltage 2.0-4.8V).Test result shows, under the current density of 5mA/g, and Li 2mnO 2.97f 0.03discharge capacity be first 209.1mAh/g, the capacity after 20 times that circulates is 139.8mAh/g, the conservation rate of capacity is 66.9%.The specific capacity cycle graph of its first discharge specific capacity and 20 times is as Fig. 2, shown in Fig. 3.
Embodiment bis-
Take 5.3505gLiNO 3, 4.5980gMnCO 3and 0.0629gLiF is dissolved in 8ml deionized water and forms salting liquid, by 25.3435g citric acid with adding in aforementioned salt solution and form mixed solution after 30ml deionized water dissolving, with ammoniacal liquor adjustment mixed solution pH to 7, subsequently mixed solution is placed on to 80 DEG C of lasting stirrings 6 hours of constant temperature on magnetic force heating stirrer, obtains liquid precursor.By liquid precursor be placed in drying box in 80 DEG C after dry 24 hours at 130 DEG C the dry solid precursor that obtains for 8 hours, solid precursor is placed on and in Muffle furnace, at 500 DEG C, calcines the presoma that is ground into powder after 5 minutes, Powdered presoma is incubated at 300 DEG C after one hour to the Li that is heated to 700 DEG C of insulation 9h and obtains fluorine doping with the heating rate of 4 DEG C/min 2mnO 3(Li 2mnO 2.94f 0.06).
Adopt the method identical with comparative example 1 to prepare CR2025 type button normal temperature battery, its capacity, high rate performance, cyclical stability are tested to (voltage 2.0-4.8V).Test result shows, under the current density of 5mA/g, and Li 2mnO 2.94f 0.06discharge capacity be first 196.3mAh/g, the capacity after 20 times that circulates is 115mAh/g, the conservation rate of capacity is 58.6%.
Embodiment tri-
Take 5.2778gLiNO 3, 6.9211gMn (CH 3cOO) 2and 0.0943gLiF is dissolved in 20ml deionized water and forms salting liquid, by 38.0153g citric acid with adding in aforementioned salt solution and form mixed solution after 30ml deionized water dissolving, with ammoniacal liquor adjustment mixed solution pH to 9, subsequently mixed solution is placed on to 80 DEG C of lasting stirrings 6 hours of constant temperature on magnetic force heating stirrer, obtains liquid precursor.By liquid precursor be placed in drying box in 80 DEG C after dry 16 hours at 150 DEG C the dry solid precursor that obtains for 8 hours, solid precursor is placed on and in Muffle furnace, at 450 DEG C, calcines the presoma that is ground into powder after 7 minutes, Powdered presoma is incubated at 300 DEG C after 2 hours to the Li that is heated to 600 DEG C of insulation 15h and obtains fluorine doping with the heating rate of 3 DEG C/min 2mnO 3(Li 2mnO 2.91f 0.09).
Adopt the method identical with comparative example 1 to prepare CR2025 type button normal temperature battery, its capacity, high rate performance, cyclical stability are tested to (voltage 2.0-4.8V).Test result shows, under the current density of 5mA/g, and Li 2mnO 2.91f 0.09discharge capacity be first 188.4mAh/g, the capacity after 20 times that circulates is 116.4mAh/g, the conservation rate of capacity is 61.8%.
Embodiment tetra-
Take 4.9621gCH 3cOOLi, 7.1576gMn (NO 3) 2and 0.1258gLiF is dissolved in 10ml deionized water and forms salting liquid, by 12.6718g citric acid with adding in aforementioned salt solution and form mixed solution after 20ml deionized water dissolving, with ammoniacal liquor adjustment mixed solution pH to 8, subsequently mixed solution is placed on to 80 DEG C of lasting stirrings 6 hours of constant temperature on magnetic force heating stirrer, obtains liquid precursor.By liquid precursor be placed in drying box in 60 DEG C after dry 24 hours at 130 DEG C the dry solid precursor that obtains for 12 hours, solid precursor is placed on and in Muffle furnace, at 500 DEG C, calcines the presoma that is ground into powder after 7 minutes, Powdered presoma is incubated at 350 DEG C after one hour to the Li that is heated to 700 DEG C of insulation 9h and obtains fluorine doping with the heating rate of 2 DEG C/min 2mnO 3(Li 2mnO 2.88f 0.12).
Adopt the method identical with comparative example 1 to prepare CR2025 type button normal temperature battery, its capacity, high rate performance, cyclical stability are tested to (voltage 2.0-4.8V).Test result shows, under the current density of 5mA/g, and Li 2mnO 2.88f 0.12discharge capacity be first 172.4mAh/g, the capacity after 20 times that circulates is 112.7mAh/g, the conservation rate of capacity is 65.4%.
By the above detailed description to the embodiment of the present invention, can understand and the invention solves conventional Li 2mnO 3material electricity rate is led low, and electro-chemical activity is poor, all lower problems of cycle performance and discharge capacity, and the cost of material of employing is low, and synthesis temperature is low, prepared fluorine Li doped 2mnO 3electro-chemical activity is good, and under the current density of 5mA/g, first discharge specific capacity, at 172.4～209.1mAh/g, remains on 112.7～139.9mAh/g after 20 circulations, and conservation rate is 58.6～66.9%.
Be understandable that, above execution mode is only used to principle of the present invention is described and the illustrative embodiments that adopts, but the present invention is not limited thereto.For those skilled in the art, without departing from the spirit and substance in the present invention, can make various modification and improvement, these modification and improvement are also considered as protection scope of the present invention.

Claims (5)

1. a lithium ion battery positive active material, is characterized in that this positive active material is the Li of fluorine doping 2mnO 3, its composition formula is: Li 2mnO 3-xf x(0.03≤x≤0.12).
2. a preparation method for positive active material for lithium ion battery claimed in claim 1, is characterized in that comprising the following steps:
(1) weigh lithium salts, manganese salt and lithium fluoride (0.03≤x≤0.12), be dissolved in and in deionized water, be mixed with salting liquid, described lithium salts is in lithium, manganese salt is in manganese, lithium salts, the mol ratio of manganese salt and lithium fluoride is 2-x:1:x, in salting liquid, manganese element molar concentration is 2～5mol/L, the aqueous citric acid solution that is 3～6mol/L by concentration adds in aforementioned salt solution and forms mixed solution, in citric acid and salting liquid, the mol ratio of metal cation is 0.5～1.5:1, regulate mixed solution pH value to 7～9 with ammoniacal liquor subsequently, again mixed solution is stirred 6～8 hours at 60～80 DEG C, make solution that sufficient complexing occur, form colloidal sol, obtain liquid precursor,
(2) step (1) gained liquid precursor is heated to 8～12h 60～80 DEG C of heating after 16～24 hours at 130～150 DEG C, obtain solid precursor;
(3) step (2) gained solid precursor is calcined at 450～500 DEG C after 3～7 minutes and ground, obtain Powdered presoma, again the pre-burning at 300～350 DEG C of Powdered presoma was heated to 600～700 DEG C with the programming rate of 2-4 DEG C/min after 1～2 hour, and be incubated 9～15h, obtain the Li of fluorine doping after cooling with stove 2mnO 3, obtain lithium ion battery positive active material.
3. preparation method according to claim 2, is characterized in that the described lithium salts of step (1) comprises any one in lithium nitrate, lithium carbonate, lithium acetate; Described manganese salt comprises any one in manganese nitrate, manganese carbonate, manganese acetate.
4. a lithium ion battery, with anodal, is characterized in that comprising the lithium ion battery positive active material of preparing according to method described in claim 2-3.
5. a lithium ion battery, is characterized in that using lithium ion battery according to claim 4 with anodal.
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