CN103606702A - Easily-manufactured high-specific-capacity lithium ion battery - Google Patents
Easily-manufactured high-specific-capacity lithium ion battery Download PDFInfo
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- CN103606702A CN103606702A CN201310577372.6A CN201310577372A CN103606702A CN 103606702 A CN103606702 A CN 103606702A CN 201310577372 A CN201310577372 A CN 201310577372A CN 103606702 A CN103606702 A CN 103606702A
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- Prior art keywords
- ion battery
- lithium ion
- lithium
- porous
- graphite
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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
- 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
- H01M4/36—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
- H01M4/36—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
- H01M4/36—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
- H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
- H01M4/587—Carbonaceous material, e.g. graphite-intercalation compounds or CFx for inserting or intercalating light metals
-
- 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 an easily-manufactured high-specific-capacity lithium ion battery which comprises a positive plate, a negative plate, a diaphragm and electrolyte, wherein the diaphragm and the electrolyte are arranged between the positive plate and the negative plate, a positive pole is made of lithium NMC (nickel manganese cobalt) ternary-system materials, and a negative pole is made of porous graphite flake materials. According to the invention, a defect that Li<+> is not easy to be uniformly mixed with Co<2+>, Ni<2+> and Mn<2+> by using a solid-phase method is overcome, and a problem that existing porous carbon materials are high in production cost, complex in reaction required equipment, and low in discharge specific capacity is solved.
Description
Technical field
The present invention relates to battery, be specifically related to a kind of lithium ion battery that easy specific capacity is high of manufacturing.
Background technology
Lithium ion battery has advantages of that voltage is high, volume is little, quality is light, specific energy is high, memory-less effect, pollution-free, self discharge is little, the life-span is long, be widely used in walkie electronic apparatus power supply, as digital electrical apparatus battery, traditional application such as battery of mobile phone.LiCoO
2positive electrode as lithium ion battery has been commercially produced for many years, but due to Co scarcity of resources, its cost is far above negative pole, account for the more than 1/3rd of battery total cost, make lithium ion battery at high capacity cell, especially the application of electric automobiles is restricted, thereby the cost that how to reduce anode material for lithium-ion batteries becomes the key of Study on Li-ion batteries using.LiNiO
2and LiMn
2o
4once be considered to better substitute LiCoO
2material, but LiNiO
2preparation is difficult, and the transformation of crystal structure can occur in charge and discharge process, causes its capacity attenuation fast, and cycle performance and thermal stability are poor.LiMn
2o
4the discharge capacity of positive electrode is lower, at charge and discharge process, Jahn-Teller distortion effect can occur, and while causing temperature higher than 55 ℃, material structure deforms, and the Mn in crystal
3+can there is disproportionation, the Mn of generation
2+can be dissolved in electrolyte and make electrode active material loss, capacity attenuation is fast, has hindered LiMn
2o
4the application of positive electrode.And porous graphite sheet layer material has the advantages such as stable physicochemical properties, larger specific area, cheap raw material and simple preparation method; Therefore,, in order to explore the height of its specific capacity that is applied to lithium ion battery and the length of cycle life, be necessary to be applied to lithium ion battery negative material.
Summary of the invention
The object of the invention is the defect for above-mentioned prior art, a kind of lithium ion battery that easy specific capacity is high of manufacturing is provided, there is manufacture method relatively easy, the advantage that specific discharge capacity is high.
Object of the present invention can be achieved through the following technical solutions:
Manufacture the lithium ion battery that easy specific capacity is high, comprise positive plate, negative plate and be placed in barrier film and the electrolyte between positive and negative plate, the described anodal manganese lithium nickel cobaltate ternary system material that adopts, described negative pole adopts porous graphite sheet material.
The making of described negative pole porous graphite sheet material comprises the following steps:
A, under stirring condition, graphite is joined in the mixed acid solution of sulfuric acid and nitric acid, controlling temperature is 15 ℃～55 ℃, keeps 0.5h～2h, then centrifugation, be washed to acidity, dehydrate, then controlling microwave power is 3kW again, keeps 30s, obtain expanded graphite, allowance for expansion is 150mL/g～260mL/g, and wherein the mass ratio of graphite and mixed acid is 1: 2～6, and the mass ratio of sulfuric acid and nitric acid is 2～4: 1;
B, expanded graphite prepared by previous step join in solvent, solvent is one or more the mixing in water, ethanol and ethylene glycol, add again surfactant, adopt ultrasonic method or heating paddling process evenly to mix, obtain mixture, wherein, the mass ratio of expanded graphite and solvent is 2: 25～100;
C, pore creating material is dissolved in solvent, add again mixture obtained in the previous step, stirring at room 4h～8h, control mixing speed is 300r/min～400r/min, then in temperature, be dry under 60 ℃～80 ℃ conditions, obtain porous presoma, wherein the mass ratio of pore creating material and solvent is 1: 5～30, and in mixture, the mass ratio of expanded graphite and pore creating material is 1: 5～30;
D, porous presoma prepared by previous step are under inert gas atmosphere condition, inert gas atmosphere flow is 120mL/min～400mL/min, be warming up to 700 ℃～1100 ℃, control programming rate and be 2 ℃/min～20 ℃/min, porous presoma is heat-treated, and heat treatment time is 1h～5h, more extremely neutral with acid solution and distilled water washing, under the bake out temperature of 60 ℃～85 ℃, dry, obtain the porous stone ink sheet of the super electric negative pole of lithium electricity.
Described surfactant is one or more in softex kw, dodecyl sodium sulfate, lauryl sodium sulfate, cetyl benzene sulfonic acid sodium salt, sodium stearyl sulfate or polydiene propyl-dimethyl amine ammonium chloride.
Described pore creating material is one or more the mixing in zinc acetate, zinc chloride, potassium hydroxide, NaOH, calcium oxide, calcium carbonate, calcium hydroxide and potash.
The making of described anodal manganese lithium nickel cobaltate ternary system material comprises the following steps:
A, three kinds of sulfate of manganese cobalt nickel are pressed to Ni: Co: Mn=(1-x-y): x: y, 0.1≤y≤0.4,0.2≤x+y≤0.95, the mol ratio solution of making soluble in water;
B, under the condition stirring by solution evaporate to dryness, the powder that evaporate to dryness is obtained decomposes and obtains LiNi in 900～1000 ℃ of heating for 1-2.5 hour
1-x-yco
xmn
yo
2precursor composite oxides;
C, by precursor composite oxides and lithium carbonate or lithium hydroxide by 1: 1～1.05 mixed in molar ratio, be warming up to 650～750 ℃ of constant temperature 8～12 hours, cooling rear grinding in ball grinder 25～35 minutes, then be warming up to 800～900 ℃ of constant temperature 8～12 hours, obtain nickel cobalt lithium manganate ternary system anode material of lithium ion battery LiNi
1/3co
1/3mn
1/3o
2powder.
Beneficial effect of the present invention: the present invention has overcome solid phase method and has been difficult to make Li
+with Co
2+, Ni
2+, Mn
2+mixed uniformly deficiency, the conditions such as pH, concentration, temperature, mixing speed of simultaneously having avoided coprecipitation solution in preparing presoma process are controlled and are required harsh drawback, three kinds of sulfate are made to concentrated solution, then under the condition stirring by solution evaporate to dryness, guaranteed Co in presoma
2+, Ni
2+, Mn
2+even mixing, precursor preparation technology flow process is short, and solves that existing porous carbon materials production cost is high, reaction equipment needed thereby is complicated, the problem that specific discharge capacity is low.
Embodiment
Below by embodiment, the present invention is described in detail.
Negative pole porous graphite sheet material is prepared according to following steps:
A, under stirring condition, graphite is joined in the mixed acid solution of sulfuric acid and nitric acid, controlling temperature is 30 ℃, keep 1.5h, then centrifugation, is washed to acidity, dehydrate again, then controlling microwave power is 3kW, keeps 30s, wherein the mass ratio of graphite and mixed acid is 1: 4, and the mass ratio of sulfuric acid and nitric acid is 3: 1;
B, 0.1g expanded graphite prepared by previous step join in water 30ml, then add 0.5g dodecyl sodium sulfate, adopt ultrasonic method evenly to mix, and obtain mixture;
C, 0.5g zinc acetate and zinc chloride mixture are dissolved in 30ml water, add again mixture obtained in the previous step, stirring at room 5h, control mixing speed is 300r/min, then in temperature, be dry under 70 ℃ of conditions, obtain porous presoma, in mixture, the mass ratio of expanded graphite and zinc acetate and zinc chloride mixture is 1: 5;
D, porous presoma prepared by step 3 are under inert gas atmosphere condition, and inert gas atmosphere flow is 200mL/min, is warming up to 800 ℃, and controlling programming rate is 5 ℃/min, and porous presoma is heat-treated, and heat treatment time is 2h; Extremely neutral with acid solution and distilled water washing again, acid solution is that mass concentration is the hydrochloric acid solution of 5 ﹪, and bake out temperature is 70 ℃, obtains the porous stone ink sheet of the super electric negative pole of lithium electricity.
For positive pole, by 262.85 grams of nickelous sulfates, 169.02 grams of manganese sulfates and 281.10 grams of cobaltous sulfate dissolved waters, be mixed with solution, under the condition stirring, by solution evaporate to dryness, the pressed powder obtaining after evaporate to dryness is warmed up to 900 ℃ of heating 2 hours, obtain LiNi
1/3co
1/3mn
1/3o
2precursor composite oxides.
After the precursor composite oxides that obtain are fully mixed with 221.67 grams of lithium carbonates, be placed in muffle furnace and rise to 700 ℃ of constant temperature 10h with the programming rate of 2 ℃/min, cooling rear grinding in ball grinder 30 minutes, then be placed in muffle furnace and rise to 850 ℃ of constant temperature 10 hours with the programming rate of 2 ℃/min, obtain LiNi
1/3co
1/3mn
1/3o
2powder, the tap density of synthetic powder is 2.21g/cm
3, specific area is 0.44m2/g, middle grain diameter D50=8.5 μ m.Resulting materials is assembled into simulated battery, and barrier film is celgard2300, and negative pole is metal lithium sheet, and recording discharge capacity is 165mAh/g, and the special capacity fade after 30 circulations is 2.1%.
High-temperature calcination is prepared to LiNi
1/3co
1/3mn
1/3o
2the sulfur dioxide producing in precursor composite oxides process and sulfur trioxide mist are dry through the concentrated sulfuric acid, and pass into the mixed serum that manganese dioxide, manganese carbonate and water form mix compression with air after.The mixed ore pulp of manganese dioxide and manganese carbonate is prepared as follows: by 1mol manganese dioxide and 2mol manganese carbonate mixed grinding to 120 order, then adding distilled water to stir into solid-to-liquid ratio is the ore pulp of 1: 4, sulfur dioxide and sulfur trioxide mist are pressed into from agitator bottom, and becoming even minute bubbles to enter ore pulp through the Mass of stainless steel sieve plate, ore pulp is from tower top spray.Whole process constantly stirs, and extraction time is 7 hours, and extraction temperature is 85 ℃.To adding successively the leaching liquid from flow out on absorption tower Sodium Dimethyldithiocarbamate, ammonium sulfide and ammonium fluoride to till no longer producing precipitation, to filter and obtain clean manganese sulfate solution, filtrate obtains manganese sulfate monohydrate through crystallization.
It is raw material that present embodiment adopts cheap graphite powder, recycling low-cost reagent modifies it, by chemical means, carry out pore-creating, and then to have made specific area be 400～1000 times of large porous stone ink sheets of graphite, by controlling activating reagent and the mass ratio of expanded graphite and the size that activation temperature is carried out control hole, and then determine the size of lithium ion battery specific discharge capacity under the condition of the two different quality ratio.Porous graphite sheet material prepared by the present invention has the features such as good conductivity, thickness is controlled, hole dimension is even, specific area is larger, and its specific area is 300～700m
2/ g, is applied to its specific discharge capacity of lithium ion battery by this porous carbon and reaches 400～1000mAh/g, is its 4～5 times with take that battery that graphite is negative material compares.
More than show and described basic principle of the present invention and principal character and advantage of the present invention.The technology people of the industry should understand; the present invention is not restricted to the described embodiments; that in above-described embodiment and specification, describes just illustrates principle of the present invention; without departing from the spirit and scope of the present invention; the present invention also has various changes and modifications, and these changes and improvements all fall in the claimed scope of the invention.The claimed scope of the present invention is defined by appending claims and equivalent thereof.
Claims (5)
1. manufacture the high lithium ion battery of easy specific capacity for one kind, comprise positive plate, negative plate and be placed in barrier film and the electrolyte between positive and negative plate, it is characterized in that: the described anodal manganese lithium nickel cobaltate ternary system material that adopts, described negative pole adopts porous graphite sheet material.
2. a kind of lithium ion battery that easy specific capacity is high of manufacturing according to claim 1, is characterized in that, the making of described negative pole porous graphite sheet material comprises the following steps:
A, under stirring condition, graphite is joined in the mixed acid solution of sulfuric acid and nitric acid, controlling temperature is 15 ℃～55 ℃, keeps 0.5h～2h, then centrifugation, be washed to acidity, dehydrate, then controlling microwave power is 3kW again, keeps 30s, obtain expanded graphite, allowance for expansion is 150mL/g～260mL/g, and wherein the mass ratio of graphite and mixed acid is 1: 2～6, and the mass ratio of sulfuric acid and nitric acid is 2～4: 1;
B, expanded graphite prepared by previous step join in solvent, solvent is one or more the mixing in water, ethanol and ethylene glycol, add again surfactant, adopt ultrasonic method or heating paddling process evenly to mix, obtain mixture, wherein, the mass ratio of expanded graphite and solvent is 2: 25～100;
C, pore creating material is dissolved in solvent, add again mixture obtained in the previous step, stirring at room 4h～8h, control mixing speed is 300r/min～400r/min, then in temperature, be dry under 60 ℃～80 ℃ conditions, obtain porous presoma, wherein the mass ratio of pore creating material and solvent is 1: 5～30, and in mixture, the mass ratio of expanded graphite and pore creating material is 1: 5～30;
D, porous presoma prepared by previous step are under inert gas atmosphere condition, inert gas atmosphere flow is 120mL/min～400mL/min, be warming up to 700 ℃～1100 ℃, control programming rate and be 2 ℃/min～20 ℃/min, porous presoma is heat-treated, and heat treatment time is 1h～5h, more extremely neutral with acid solution and distilled water washing, under the bake out temperature of 60 ℃～85 ℃, dry, obtain the porous stone ink sheet of the super electric negative pole of lithium electricity.
3. a kind of lithium ion battery that easy specific capacity is high of manufacturing according to claim 2, is characterized in that: described surfactant is one or more in softex kw, dodecyl sodium sulfate, lauryl sodium sulfate, cetyl benzene sulfonic acid sodium salt, sodium stearyl sulfate or polydiene propyl-dimethyl amine ammonium chloride.
4. a kind of lithium ion battery that easy specific capacity is high of manufacturing according to claim 3, is characterized in that: described pore creating material is one or more the mixing in zinc acetate, zinc chloride, potassium hydroxide, NaOH, calcium oxide, calcium carbonate, calcium hydroxide and potash.
5. a kind of lithium ion battery that easy specific capacity is high of manufacturing according to claim 1, is characterized in that, the making of described anodal manganese lithium nickel cobaltate ternary system material comprises the following steps:
A, three kinds of sulfate of manganese cobalt nickel are pressed to Ni: Co: Mn=(1-x-y): x: y, 0.1≤y≤0.4,0.2≤x+y≤0.95, the mol ratio solution of making soluble in water;
B, under the condition stirring by solution evaporate to dryness, the powder that evaporate to dryness is obtained decomposes and obtains LiNi in 900～1000 ℃ of heating for 1～2.5 hour
1-x-yco
xmn
yo
2precursor composite oxides;
C, by precursor composite oxides and lithium carbonate or lithium hydroxide by 1: 1～1.05 mixed in molar ratio, be warming up to 650～750 ℃ of constant temperature 8～12 hours, cooling rear grinding in ball grinder 25～35 minutes, then be warming up to 800～900 ℃ of constant temperature 8～12 hours, obtain nickel cobalt lithium manganate ternary system anode material of lithium ion battery LiNi
1/3co
1/3mn
1/3o
2powder.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104617261A (en) * | 2015-01-23 | 2015-05-13 | 东莞市翔丰华电池材料有限公司 | Method for preparing composite cathode material of silicon-carbon nanotube of lithium ion battery |
| CN114068885A (en) * | 2020-07-30 | 2022-02-18 | 湖南中科星城石墨有限公司 | Graphite material with porous carbon layer and preparation method and application thereof |
| CN115084500A (en) * | 2022-04-29 | 2022-09-20 | 远景动力技术(江苏)有限公司 | Polycrystalline ternary material and application thereof |
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| CN101425605A (en) * | 2007-11-01 | 2009-05-06 | 深圳市慧通天下科技股份有限公司 | Nickel-cobalt lithium manganate high power lithium ionic cell |
| CN102044664A (en) * | 2010-11-10 | 2011-05-04 | 湘西自治州兴湘科技开发有限责任公司 | Method for preparing nickel cobalt lithium manganate ternary system anode material of lithium ion battery |
| CN103259018A (en) * | 2013-04-27 | 2013-08-21 | 黑龙江大学 | Preparation method of porous graphite flake applied to super-electric negative pole of lithium battery |
| US20130216894A1 (en) * | 2012-02-16 | 2013-08-22 | Yanbo Wang | Inorganic nano sheet-enabled lithium-exchanging surface-mediated cells |
-
2013
- 2013-11-15 CN CN201310577372.6A patent/CN103606702A/en active Pending
Patent Citations (4)
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| CN101425605A (en) * | 2007-11-01 | 2009-05-06 | 深圳市慧通天下科技股份有限公司 | Nickel-cobalt lithium manganate high power lithium ionic cell |
| CN102044664A (en) * | 2010-11-10 | 2011-05-04 | 湘西自治州兴湘科技开发有限责任公司 | Method for preparing nickel cobalt lithium manganate ternary system anode material of lithium ion battery |
| US20130216894A1 (en) * | 2012-02-16 | 2013-08-22 | Yanbo Wang | Inorganic nano sheet-enabled lithium-exchanging surface-mediated cells |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104617261A (en) * | 2015-01-23 | 2015-05-13 | 东莞市翔丰华电池材料有限公司 | Method for preparing composite cathode material of silicon-carbon nanotube of lithium ion battery |
| CN114068885A (en) * | 2020-07-30 | 2022-02-18 | 湖南中科星城石墨有限公司 | Graphite material with porous carbon layer and preparation method and application thereof |
| CN115084500A (en) * | 2022-04-29 | 2022-09-20 | 远景动力技术(江苏)有限公司 | Polycrystalline ternary material and application thereof |
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Application publication date: 20140226 |