CN109301199A - A kind of lithium battery cobalt phosphate lithium method for preparing anode material - Google Patents
A kind of lithium battery cobalt phosphate lithium method for preparing anode material Download PDFInfo
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- CN109301199A CN109301199A CN201811087675.9A CN201811087675A CN109301199A CN 109301199 A CN109301199 A CN 109301199A CN 201811087675 A CN201811087675 A CN 201811087675A CN 109301199 A CN109301199 A CN 109301199A
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- lithium
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- cobalt phosphate
- lithium battery
- anode material
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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
- H01M4/366—Composites as layered products
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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
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/5825—Oxygenated metallic salts or polyanionic structures, e.g. borates, phosphates, silicates, olivines
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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
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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 relates to cell positive material technical fields, especially a kind of lithium battery cobalt phosphate lithium method for preparing anode material, by phosphoric acid is mixed with urea, and after being dissolved in water, heat treatment, so that phosphoric acid and urea are under the premise of phosphoric acid is excessive, generate the material with chelation structure, and the powder such as frerrous chloride, calcium acetate are mixed in the case where completely cutting off air conditions, effectively avoid ferrous ion and air catalytic oxidation, and be added by acetic acid calcium powder, so that generating chlorination calcium component under subsequent effect；Be incorporated in vacuum environment physics it is dry-mixed enter lithium hydroxide, and after cobalt oxide is dissolved using solvent, mixing, so that generating the mixed material of phosphoric acid cobalt lithium and chlorination calcium component, and pass through calcination processing, it forms calcium chloride and coats cobalt phosphate lithium, improve the electrochemistry cycle performance of cobalt phosphate lithium positive electrode.
Description
Technical field
The present invention relates to cell positive material technical field, especially a kind of lithium battery is prepared with cobalt phosphate lithium positive electrode
Method.
Background technique
Phosphate of olivine type class intercalation materials of li ions LiMPO4Deng having the function of reversible removal lithium embedded and higher stable structure
Property.Especially LiFePO4It is cheap with abundant raw materials, it is environmental-friendly the features such as, when being used as positive electrode, heat
Stability is good, and cycle performance is excellent and highly-safe, comes into the industrialization stage.In recent years, lithium manganese phosphate, cobalt phosphate lithium
It gets the attention and furthers investigate.
Currently, common preparation method has solid phase method, sol-gal process, hydro-thermal method etc..Solid-phase synthesis is electrode material
It is most common in preparation, it is to be subsequently placed in high temperature furnace, than mixed grinding, tabletting in air or inertia by metering by reactant
It is sintered in gas.High temperature solid phase synthesis is easy to operate, easy to industrialized production, but that there are synthesis temperatures is high, sintering time is long,
The problems such as particle diameter distribution is uneven, consistency and reproducibility are poor.For this purpose, thering is researcher to disclose using metatitanic acid in the prior art
Lithium, cobalt oxide and diammonium hydrogen phosphate are raw material, uniformly mixed by certain stoichiometric ratio, in 350 DEG C of pre-burning 9h, then again 750
Roast 30h at DEG C, charge/discharge capacity is 86/70mAh/g for the first time under products obtained therefrom 0.1C charge-discharge magnification.Sol-gal process is
Organic or inorganic compound is cured by the processes such as dissolution, colloidal sol, gel, heat treatment preparation is then carried out and produces
Object has many advantages, such as that synthesis temperature is low, partial size is small, particle diameter distribution is narrow, large specific surface area, but its to synthesis condition require it is harsh,
Long preparation period has researcher to use lithium acetate, cobalt acetate and phosphoric acid for raw material in the method, at room temperature, in vinyl second two
Reaction stirring forms gel in alcohol, and aging two days, under protection of argon gas, 700 DEG C of roasting 12h obtained submicron order pink
LiCoPO4, under C/50 multiplying power discharging, initial capacity is only 65mAh/g；LiCoPO is produced using gel method4When, and have studied
Influence of the element doping to material property, but its effect is still generally, and specific discharge capacity is still undesirable.The alcohols precipitation method
It is that a certain amount of alcohols is added in the Aqueous extracts of concentration, the Precipitation from solution of the ingredient insoluble in alcohols, so that two kinds
Sediment generates synthesis mixing on one side one time in the liquid phase, more more uniform than ball mill mixing, at the same without the concern for temperature and
The factors such as pH are influenced caused by reaction, simple process.
But either the methods of high temperature process heat, collosol and gel or alcohols precipitating, for what is prepared
In LiCoPO4 presoma product, still remain more impurity and complex process, it is at high cost the defects of, cause preparation production
Product stability is not high, and the product of acquisition is for during lithium battery, the lithium battery performance of acquisition to be poor, cobalt phosphate lithium positive electrode
Specific capacity it is low, and the stable electrochemical property in use process is poor.
Summary of the invention
In order to solve the above technical problems existing in the prior art, the present invention is providing a kind of lithium battery cobalt phosphate lithium just
Pole material preparation method.
It is achieved particular by following technical scheme:
Lithium battery cobalt phosphate lithium method for preparing anode material, comprising the following steps:
It (1) is after 2:0.8-1.3 is mixed, to add water to after being completely dissolved, be warming up to 80- according to mass ratio by phosphoric acid and urea
90 DEG C, handle 20-30min；
(2) mass ratioes such as four water frerrous chloride powder and acetic acid calcium powder are uniformly mixed, mixed process is in isolation air item
It is carried out under part；
(3) by the material of step (1), the material and lithium hydroxide of step (2), in the case where vacuum degree is 0.02-0.08MPa, according to
Mass ratio is uniformly mixed for 1:1:3；
(4) cobalt oxide is uniformly mixed with solvent according to mass ratio for 1:3, and low whipping speed be 1000-3000r/min under,
The mixture that step (3) obtain is added thereto according to mass ratio for 1:1, is stirred evenly, heating concentration, and in inert gas
In the presence of be sintered, sintering temperature be 900-1200 DEG C, sintering time 8-12h, natural cooling to get.
It is preferred that the solvent is alcohol solution or alcohol and water according to mass ratio, to be that 1:0.1-0.7 is mixed mixed
Close liquid.
It is preferred that the ethanol water that the alcohol solution is dehydrated alcohol or mass concentration is 58.82-90.0%.
It is preferred that the alcohol solution is the ethanol water that mass concentration is 72.5%.
It is preferred that the inert gas is argon gas.
It is preferred that the step (4) also adds thereto during the mixture that step (3) obtain is added thereto
Enter the iron powder for having the mixture quality 1-5% for accounting for step (3) acquisition.
Compared with prior art, the technical effect of the invention is embodied in:
By phosphoric acid is mixed with urea, and after being dissolved in water, heat treatment, so that phosphoric acid and urea are before phosphoric acid is excessive
It puts, generates the material with chelation structure, and the powder such as frerrous chloride, calcium acetate are mixed in the case where completely cutting off air conditions, have
Effect avoids ferrous ion and air catalytic oxidation, and acetic acid calcium powder is added, so that generating chlorine under subsequent effect
Change calcium component；Be incorporated in vacuum environment physics it is dry-mixed enter lithium hydroxide, and by cobalt oxide using solvent dissolution after, mix
It closes, so that generating the mixed material of phosphoric acid cobalt lithium and chlorination calcium component, and passes through calcination processing, form calcium chloride and coat phosphorus
Sour cobalt lithium improves the electrochemistry cycle performance of cobalt phosphate lithium positive electrode.
The invention preparation process is simple, realizes in cobalt phosphate lithium positive electrode preparation process, generates through superchlorination
The cobalt phosphate lithium positive electrode of calcium cladding improves the chemical property of cobalt phosphate lithium positive electrode, and contract to a certain extent
Short process flow, reduces costs.Meanwhile in the invention, it is preferred to use FeF2·4H2O replaces FeCl2·4H2O,
The chemical property of positive electrode can effectively be enhanced, enhance coating function.
Specific embodiment
It is limited below with reference to specific embodiment technical solution of the present invention is further, but claimed
Range is not only limited to made description.
Embodiment 1
Lithium battery cobalt phosphate lithium method for preparing anode material, comprising the following steps:
(1) it is after 2:0.8 is mixed, to add water to after being completely dissolved according to mass ratio by phosphoric acid and urea, is warming up to 80 DEG C, place
Manage 20min；
(2) mass ratioes such as four water frerrous chloride powder and acetic acid calcium powder are uniformly mixed, mixed process is in isolation air item
It is carried out under part；
(3) by the material of step (1), the material and lithium hydroxide of step (2), in the case where vacuum degree is 0.02MPa, according to mass ratio
It is uniformly mixed for 1:1:3；
(4) cobalt oxide is uniformly mixed with anhydrous ethanol solvent according to mass ratio for 1:3, and low whipping speed is 1000r/min
Under, the mixture that step (3) obtain is added thereto according to mass ratio for 1:1, is stirred evenly, heating concentration, and in argon gas
Be sintered in the presence of equal inert gases, sintering temperature is 900 DEG C, sintering time 8h, natural cooling to get.
Embodiment 2
Lithium battery cobalt phosphate lithium method for preparing anode material, comprising the following steps:
(1) it is after 2:1.3 is mixed, to add water to after being completely dissolved according to mass ratio by phosphoric acid and urea, is warming up to 90 DEG C, place
Manage 30min；
(2) mass ratioes such as four water frerrous chloride powder and acetic acid calcium powder are uniformly mixed, mixed process is in isolation air item
It is carried out under part；
(3) by the material of step (1), the material and lithium hydroxide of step (2), in the case where vacuum degree is 0.08MPa, according to mass ratio
It is uniformly mixed for 1:1:3；
(4) cobalt oxide is uniformly mixed with anhydrous ethanol solvent according to mass ratio for 1:3, and low whipping speed is 3000r/min
Under, the mixture that step (3) obtain is added thereto according to mass ratio for 1:1, is stirred evenly, heating concentration, and in argon gas
It is sintered in the presence of equal inert gases, sintering temperature is 900-1200 DEG C, sintering time 8-12h, natural cooling, i.e.,
?.
Embodiment 3
Lithium battery cobalt phosphate lithium method for preparing anode material, comprising the following steps:
(1) it is after 2:1 is mixed, to add water to after being completely dissolved according to mass ratio by phosphoric acid and urea, is warming up to 85 DEG C, processing
25min；
(2) mass ratioes such as four water frerrous chloride powder and acetic acid calcium powder are uniformly mixed, mixed process is in isolation air item
It is carried out under part；
(3) by the material of step (1), the material and lithium hydroxide of step (2), in the case where vacuum degree is 0.06MPa, according to mass ratio
It is uniformly mixed for 1:1:3；
(4) cobalt oxide is uniformly mixed with anhydrous ethanol solvent according to mass ratio for 1:3, and low whipping speed is 2000r/min
Under, the mixture that step (3) obtain is added thereto according to mass ratio for 1:1, is stirred evenly, heating concentration, and in argon gas
Be sintered in the presence of equal inert gases, sintering temperature is 1100 DEG C, sintering time 9h, natural cooling to get.
Embodiment 4
Unlike the first embodiment: the ethanol water that mass concentration is 58.82%.
Embodiment 5
Unlike the first embodiment: the ethanol water that mass concentration is 90.9%.
Embodiment 6
Unlike the first embodiment: the ethanol water that mass concentration is 72.5%.
Embodiment 7
Unlike the first embodiment: the ethanol water that mass concentration is 90.0%.
Embodiment 8
Unlike the first embodiment: the ethanol water that mass concentration is 91.1%.
Embodiment 9
Unlike the first embodiment: the ethanol water that mass concentration is 58%.
Embodiment 10
Unlike the first embodiment: the ethanol water that mass concentration is 95.2%.
Embodiment 11
Unlike the first embodiment: the step (4), being also added thereto has the mixture quality 1% for accounting for step (3) acquisition
Iron powder.
Embodiment 12
Unlike the first embodiment: the step (4), being also added thereto has the mixture quality 5% for accounting for step (3) acquisition
Iron powder.
Embodiment 13
Unlike the first embodiment: the step (4), being also added thereto has the mixture quality 3% for accounting for step (3) acquisition
Iron powder.
Embodiment 14
Unlike the first embodiment: the step (4), being also added thereto has the mixture quality 2% for accounting for step (3) acquisition
Iron powder.
The material of embodiment 1-14 preparation is handled using air-flow crushing, crushes pressure control at 0.6MPa, and will obtain
The powder obtained carries out specific surface area detection, as a result as shown in table 1 below.Meanwhile it also to the material of preparation, conductive agent acetylene black and gluing
Knot agent PVDF is that positive plate is made by mixing into 70:12:9 according to mass ratio, using coin shape simulated battery to the electrode slice of preparation
Battery assembly is carried out, metal lithium sheet is used to electrode, diaphragm is Celgard2325 composite membrane, and the battery being made into is in 3.5-5V electricity
0.1C(1C=170mAh/g is in pressure range) constant current charge-discharge test, result is as shown in table 1 below.And record 50 circulations
Discharge capacity and discharge capacity attenuation rate after electric discharge.
Table 1
| Dusty material specific surface area (m2/ g) | Discharge capacity (mAh/g) for the first time | 50 discharge capacities (mAh/g) | Capacity attenuation rate (%) | |
| Embodiment 1 | 208.3 | 157.8 | 145.3 | 7.92 |
| Embodiment 2 | 206.7 | 162.5 | 148.9 | 8.37 |
| Embodiment 3 | 207.9 | 155.9 | 146.7 | 5.90 |
| Embodiment 4 | 208.1 | 159.4 | 147.9 | 7.21 |
| Embodiment 5 | 207.8 | 163.3 | 147.3 | 9.80 |
| Embodiment 6 | 206.9 | 162.7 | 149.5 | 8.11 |
| Embodiment 7 | 208.2 | 162.9 | 150.7 | 7.49 |
| Embodiment 8 | 158.6 | 118.7 | 68.9 | 41.95 |
| Embodiment 9 | 146.9 | 121.4 | 67.8 | 44.15 |
| Embodiment 10 | 151.4 | 119.8 | 69.1 | 42.32 |
| Embodiment 11 | 205.4 | 171.2 | 163.8 | 4.32 |
| Embodiment 12 | 207.8 | 168.9 | 161.5 | 4.38 |
| Embodiment 13 | 206.9 | 164.7 | 159.7 | 3.04 |
| Embodiment 14 | 207.4 | 166.9 | 158.8 | 4.85 |
By 1 data of table show it can be seen from the invention preparation cell positive material, have it is preferably electrochemically stable
Property, specific surface area is higher, and discharge capacity is higher for the first time, and capacity attenuation rate is lower.
The foregoing is only a preferred embodiment of the present invention, but scope of protection of the present invention is not limited thereto,
Anyone skilled in the art in the technical scope disclosed by the present invention, according to the technique and scheme of the present invention and its
Inventive concept is subject to equivalent substitution or change, should be covered by the protection scope of the present invention.
Claims (7)
1. a kind of lithium battery cobalt phosphate lithium method for preparing anode material, which comprises the following steps:
It (1) is after 2:0.8-1.3 is mixed, to add water to after being completely dissolved, be warming up to 80- according to mass ratio by phosphoric acid and urea
90 DEG C, handle 20-30min；
(2) mass ratioes such as four water frerrous chloride powder and acetic acid calcium powder are uniformly mixed, mixed process is in isolation air item
It is carried out under part；
(3) by the material of step (1), the material and lithium hydroxide of step (2), in the case where vacuum degree is 0.02-0.08MPa, according to
Mass ratio is uniformly mixed for 1:1:3；
(4) cobalt oxide is uniformly mixed with solvent according to mass ratio for 1:3, and low whipping speed be 1000-3000r/min under,
The mixture that step (3) obtain is added thereto according to mass ratio for 1:1, is stirred evenly, heating concentration, and in inert gas
In the presence of be sintered, sintering temperature be 900-1200 DEG C, sintering time 8-12h, natural cooling to get.
2. lithium battery as described in claim 1 cobalt phosphate lithium method for preparing anode material, which is characterized in that the solvent
It is alcohol solution or alcohol and water according to the mixed liquor that mass ratio is that 1:0.1-0.7 is mixed.
3. lithium battery as claimed in claim 2 cobalt phosphate lithium method for preparing anode material, which is characterized in that the alcohols
The ethanol water that solution is dehydrated alcohol or mass concentration is 58.82-90.0%.
4. lithium battery as claimed in claim 3 cobalt phosphate lithium method for preparing anode material, which is characterized in that the alcohols
Solution is the ethanol water that mass concentration is 72.5%.
5. lithium battery as described in claim 1 cobalt phosphate lithium method for preparing anode material, which is characterized in that the inertia
Gas is argon gas.
6. lithium battery as described in claim 1 cobalt phosphate lithium method for preparing anode material, which is characterized in that the step
(4), during the mixture that step (3) obtain is added thereto, being also added thereto has the mixing for accounting for step (3) acquisition
The iron powder of amount of substance 1-5%.
7. the lithium battery cobalt phosphate lithium positive electrode of as the method according to claim 1 to 6 preparation.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0718388A2 (en) * | 1994-12-12 | 1996-06-26 | Erika Balle | Fire-protective substance and method for producing and depositing of a fire-protective substance |
| CN101318914A (en) * | 2008-07-23 | 2008-12-10 | 瓮福（集团）有限责任公司 | Method for preparing urea phosphoric acid with wet-process phosphoric acid |
| CN104694284A (en) * | 2013-12-04 | 2015-06-10 | 青岛浩泰水务有限公司 | Cleaning agent for sewage filter sieve |
-
2018
- 2018-09-18 CN CN201811087675.9A patent/CN109301199B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0718388A2 (en) * | 1994-12-12 | 1996-06-26 | Erika Balle | Fire-protective substance and method for producing and depositing of a fire-protective substance |
| CN101318914A (en) * | 2008-07-23 | 2008-12-10 | 瓮福（集团）有限责任公司 | Method for preparing urea phosphoric acid with wet-process phosphoric acid |
| CN104694284A (en) * | 2013-12-04 | 2015-06-10 | 青岛浩泰水务有限公司 | Cleaning agent for sewage filter sieve |
Non-Patent Citations (2)
| Title |
|---|
| JIANGFENG NI 等: "Carbon coated lithium cobalt phosphate for Li-ion batteries: Comparison of three coating techniques", 《JOURNAL OF POWER SOURCES》 * |
| 严鹏: "锂离子电池正极材料橄榄石结构LiCoPO_4的制备及改性进展", 《化工新型材料》 * |
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