CN103490051A - Multi-element anode lithium battery material suitable for high voltage and preparation method for material - Google Patents
Multi-element anode lithium battery material suitable for high voltage and preparation method for material Download PDFInfo
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- CN103490051A CN103490051A CN201310428398.4A CN201310428398A CN103490051A CN 103490051 A CN103490051 A CN 103490051A CN 201310428398 A CN201310428398 A CN 201310428398A CN 103490051 A CN103490051 A CN 103490051A
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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
- H01M4/52—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
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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
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- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention provides a multi-element anode lithium battery material suitable for high voltage, and a preparation method for the material. The multi-element anode lithium battery material has the feature of a single-particle structure, and the particle size distribution is within the range of 0.5-15 mum; the chemical formula of the nickel-cobalt-manganese multi-element lithium battery anode material with composite doping elements is LiNiXCoyMnzMaNbO2, wherein the value range of x, y and z is that: x is not smaller than 0.2 and not larger than 0.9, y is not smaller than 0 and not larger than 0.4, z is not smaller than 0.1 and not larger than 0.5, 1-x-y-z equals to a+b, is larger than 0, and is not larger than 0.05, M is any one selected from titanium, aluminum, ferrum, vanadium, silicium, fluorine, lanthanide and actinide elements, and N is any one selected from calcium, magnesium, aluminum, zirconium, ferrum and titanium. Based on the preparation of the single-particle multi-element lithium battery anode material, the method of compositing specific doping elements is adopted, the structural stability under high voltage charge and discharge is improved and the cycle performance of the material is effectively improved without changing the electrochemical performance of the material.
Description
Technical field
The present invention relates to the anode material for lithium-ion batteries preparation field, be specially a kind of high-tension multielement cathode lithium electric material and preparation method thereof that is applicable to.
Background technology
At present, lithium ion battery, owing to having the characteristics such as voltage is high, energy density is high, have extended cycle life, is widely used in the portable electric appts such as mobile phone, notebook computer, digital camera.In recent years, various electronic products are gradually to miniaturization, intellectuality and functional diversities development, and this energy density to lithium ion battery is had higher requirement.
Improving the charging voltage of battery, can be in not increasing battery significantly improve the capacity of battery under the condition of active material, is one of effective way improved energy content of battery density.Yet, in the high voltage cyclic process, because the lithium ion of deviating from is too much, layer structure as the cobalt of main flow positive active material acid lithium is very unstable, especially in charging process, in cobalt acid lithium particle, have the lithium concentration gradient, particle surface layer lithium concentration is very low, very easy recurring structure subsides, and causes the cycle performance severe exacerbation of battery.Safer, more cheap LiNi now
0.5co
0.2mn
0.3o
2become gradually the focus of positive electrode development.
But the nickle cobalt lithium manganate polynary positive pole material still has self-defect, particularly under high voltage, interface is because there is the existence of free lithium, poor compatibility with electrolyte, cause cycle performance not good, and existing lithium ion polynary positive pole material mostly is polycrystalline structure, structure shakiness under high voltage, more aggravated the reaction with electrolyte, cycle performance is worsened.Therefore, the patent No. is that CN200810046300.8 discloses " a kind of nickel-cobalt-manganese multi-doped lithium ion battery cathode material and preparation method thereof ", prepared non-reunion individual particle material, improved the stability that particle discharges and recharges under high voltage, but still because the free lithium of layer structure and remained on surface, and cause the deterioration circulated.Therefore need to carry out material modification to this polynary lithium ion anode material, comprise coating and doping.Comparatively speaking, the doping means more easily prepare and do not introduce complicated preparation section.Doped chemical can play to layer structure the effect of bracing reinforcement, and to a certain degree can lightening material and the side reaction of electrolyte.
Summary of the invention
The present invention is just for the problem of above-mentioned existence, provide a kind of meet the requirement of making high-voltage lithium ion batteries be applicable to high-tension multielement cathode lithium electric material and preparation method thereof.
The technical solution used in the present invention is such:
A kind ofly be applicable to high-tension multielement cathode lithium electric material, this multielement cathode lithium electric material is the individual particle pattern, and particle diameter is distributed as 0.5-15 μ m, adopts the nickel-cobalt-manganese multi anode material for lithium-ion batteries of composite mixed element, and chemical formula is LiNi
xco
ymn
zm
an
bo
2, in formula, the span of x, y, z is: 0.2≤x≤0.9,0≤y≤0.4,0.1≤z≤0.5,0<a+b=1-x-y-z≤0.05, in formula, M is any one in titanium, aluminium, iron, vanadium, silicon, fluorine, group of the lanthanides, actinides, N is any one in calcium, magnesium, aluminium, zirconium, iron, titanium.
The preparation method of multielement cathode lithium electric material comprises the following steps:
(1) join in proportion NaOH and NH by the mixing salt solution of nickel, cobalt, manganese and doped with the soluble-salt solution of M element
3mixed-alkali solution in, adjusting pH value be 7-10, forms suspension stir 1-5h at the temperature of 30-80 ℃ after, then by the suspension filtered washing that forms, oven dry acquisition the intermediate Ni doped with the polynary positive pole material of M element
xco
ymn
zm
a(OH)
2;
(2) by the intermediate of the obtained polynary positive pole material doped with the M element, be Li:(Ni+Co+Mn in molar ratio)=ratio of 1-1.12:1 and lithium salts mix, lithium salts is a kind of in lithium hydroxide, lithium carbonate or lithium nitrate, and add oxide or volatile salt doped with the N element to mix, grind 1-8h, at 350-550 ℃ of lower low temperature presintering 1-5h; Add the PVAC polyvinylalcohol solution that concentration is 1-10% in the material after presintering, the PVA solution usage by percentage to the quality, account for the 10-20% of quality of material after presintering, after mixing in the roasting temperature 10-25h of 800-1000 ℃, come out of the stove and be cooled to room temperature, obtain the individual particle structure nickel-cobalt-manganese multi anode material for lithium-ion batteries doped with M.
The mixed-alkali solution used in described step (1) is NaOH and NH
3mixed solution, the pH value of alkaline solution>8, wherein in mixed-alkali solution, the molar concentration of NaOH is 0.2-0.9mol/L, NH
3molar concentration be 0.1-0.9mol/L, the consumption of mixed-alkali solution is the intermediated chemistry formula Ni by doped with the polynary positive pole material of M element
xco
ymn
zm
a(OH)
2the 1-1.07 of the molal quantity calculated doubly.
The soluble-salt solution of the mixing salt solution of the nickel that uses, cobalt, manganese and the M element that adulterates is one or more the mixture in sulfate, nitrate, chlorate in described step (1), total metal molar concentration is 0.5-1.5mol/L, and in this metal salt solution, the mol ratio of nickel cobalt manganese and doping M element is by polynary anode material for lithium-ion batteries finished product chemical formula configuration.
Use is doped with the oxide of N element or volatile salt with doped with the intermediate Ni of the polynary positive pole material of M element in described step (2)
xco
ymn
zm
a(OH)
2mol ratio is by polynary anode material for lithium-ion batteries finished product chemical formula configuration.
The invention has the beneficial effects as follows:
(1), on the basis for preparing the polynary lithium ion anode material of individual particle, adopt the method for composite mixed element-specific.And be different from common doping way, composite mixed minute two kinds of forms of the present invention: a kind ofly will be acid element doping at intracell, and form distortional strain energy, and make structure more stable; A kind ofly will be alkaline element doping on the crystal top layer, the unsettled nickel element of Substitute For Partial, the side reaction of inhibition and electrolyte, under the prerequisite that does not change chemical property own, promote the structural stability of high voltage under discharging and recharging, effectively promote the cycle performance of material.
(2) this preparation method's doping is less, and does not substantially change original preparation technology, is easy to control, and production cost is low, easy to utilize.The product that adopts the inventive method to prepare can be widely used in the new energy devices such as conventional lithium ion battery, ultracapacitor, has a extensive future.
The accompanying drawing explanation
The SEM figure that Fig. 1 is the nickel-cobalt-manganese multi anode material for lithium-ion batteries that contains doped chemical under this technique.
Fig. 2 is the nickel-cobalt-manganese multi anode material for lithium-ion batteries that contains doped chemical under this technique and the XRD comparison diagram of common individual particle multicomponent material.
Fig. 3 is nickel-cobalt-manganese multi anode material for lithium-ion batteries and the charging and discharging curve of common individual particle multicomponent material under 3-4.35V charging/discharging voltage and 0.2C charging and discharging currents that contains doped chemical.
Fig. 4 is nickel-cobalt-manganese multi anode material for lithium-ion batteries and the cyclic curve of common individual particle multicomponent material under 3-4.35V charging/discharging voltage and 1C charging and discharging currents that contains doped chemical.
Wherein a is common 523 type individual particle polynary positive pole materials, the individual particle polynary positive pole material that b is the common doped Ti element of 523 type, the 523 type individual particle polynary positive pole materials that c is doped Ti, Al element, the 523 type individual particle polynary positive pole materials that d is doped with Mg, Al.
Embodiment
In order to make purpose of the present invention, technical scheme and advantage clearer, below in conjunction with drawings and Examples, the present invention is further elaborated.Should be appreciated that specific embodiment described herein, only in order to explain the present invention, is not intended to limit the present invention.
Embodiment 1:
To contain the nickelous sulfate of Ni element 19.57g, containing the cobaltous sulfate of Co element 19.64g, containing the manganese sulfate of Mn element 18.18g, the Titanium Nitrate that contains the 0.53g of Ti element is dissolved in the 1L pure water, stirring and dissolving, be configured to the multi-element metal salting liquid of total metal molar concentration 1.0mol/L, in this solution, the mol ratio of nickel cobalt manganese is Ni:Co:Mn=5:2:3.
Above-mentioned solution is heated to 70 ℃, joins under stirring condition in the 1.7L alkaline solution, reacted.This alkaline solution NH
3content is 0.6mol/L, and NaOH content is 0.8mol/L.Adjusting pH value is 8.5, continues stirring 1h after reinforced the end, after standing 2h, filters, and obtains solid content, with the pure water washing material, then is placed in 110 ℃ of dry 5h of baking oven, must be doped with the intermediate of the polynary positive pole material of Ti.
By composite multi-component intermediate and 40.59gLiCO
3fully mix, in 550 ℃ of preliminary treatment 1h, again above-mentioned preliminary treatment material and 9.85gPVA solution (account for preliminary treatment quality of material percentage composition 11%) are mixed, then be placed in baking furnace, in 1000 ℃ of lower roasting 10h, come out of the stove, be cooled to normal temperature, cross 200 mesh sieve screenings after pulverizing, screenings is the micropore individual particle structure polynary positive pole material of doped Ti element.
The individual particle structure polynary positive pole material of doped Ti element prepared by the present embodiment, testing its particle size distribution by laser particle analyzer is 0.5-15 μ m.After this material is made to pole piece, by the test of battery performance test instrument, discharging and recharging under deboost of 3-4.35V, its chemical property 0.2C specific discharge capacity is 172.2mAh/g, the 1C specific discharge capacity is 169.5mAh/g, and 30 weeks circulation specific discharge capacities are 160.0mAh/g.
Embodiment 2:
To contain the nickel nitrate of Ni element 29.35g, containing the cobalt nitrate of Co element 11.74g, be dissolved in the 1.5L pure water containing the manganese nitrate of Mn element 16.48g with containing the Titanium Nitrate of Ti element 0.57g, stirring and dissolving, be configured to the multi-element metal salting liquid of total metal molar concentration 1.5mol/L, in this solution, the mol ratio of nickel cobalt manganese is Ni:Co:Mn=5:2:3.
Above-mentioned solution is heated to 50 ℃, joins under stirring condition in the 1.5L alkaline solution and reacted, this alkaline solution NH
3content is 0.4mol/L, and NaOH content is 0.9mol/L.Adjusting the pH value is 8.0, after reinforced the end, continues to stir 4h, after standing 2h, filters, and obtains solid content, with the pure water washing material, then is placed in 110 ℃ of dry 5h of baking oven, obtains the composite multi-component intermediate.
By composite multi-component intermediate and 43.08gLiOHH
2o and 0.18g nanometer Al
2o
3fully mix, in 350 ℃ of preliminary treatment 4h, again above-mentioned preliminary treatment material and 12.86gPVA solution (account for preliminary treatment quality of material percentage composition 15%) are mixed, then be placed in baking furnace, in 900 ℃ of lower roasting 18h, come out of the stove, be cooled to normal temperature, cross 200 mesh sieve screenings after pulverizing, screenings is the individual particle structure polynary positive pole material of doped Ti and Al element.
Individual particle structure polynary positive pole material prepared by the present embodiment, its particle size distribution is 0.7-20 μ m, and chemical property 0.2C specific discharge capacity is 180.8mAh/g, and the 1C specific discharge capacity is 173.5mAh/g, and 30 weeks circulation specific discharge capacities are 162.2mAh/g.
Embodiment 3:
To contain the nickel chloride of Ni element 29.47g, containing the cobalt chloride of Co element 11.72g, be dissolved in the 1.2L pure water containing the manganese chloride of Mn element 16.52g with containing the magnesium nitrate of Mg element 0.12g, stirring and dissolving, be configured to the multi-element metal salting liquid of total metal molar concentration 1.2mol/L, in this solution, the mol ratio of nickel cobalt manganese is Ni:Co:Mn=5:2:3.
Above-mentioned solution is heated to 60 ℃, joins under stirring condition in the 2L alkaline solution, reacted, this alkaline solution NH
3content is that 0.2mol/L, NaOH content are 0.5mol/L.Adjusting the pH value is 9.0, after reinforced the end, continues to stir 3h, after standing 2h, filters, and obtains solid content, with the pure water washing material, then is placed in 110 ℃ of dry 5h of baking oven, obtains the composite multi-component intermediate.
By composite multi-component intermediate and 41.94gLiOHH
2o and 0.21g nanometer Al
2o
3fully mix, in 400 ℃ of preliminary treatment 2h, again by above-mentioned preliminary treatment material and 16.68gPVA solution (account for the preliminary treatment material the quality percentage composition 18%) mix, then be placed in baking furnace, in 880 ℃ of lower roasting 20h, come out of the stove, be cooled to normal temperature, cross 200 mesh sieve screenings after pulverizing, screenings is the individual particle structure polynary positive pole material of doped with Mg and Al element.
The polynary positive pole material that this profile is the individual particle structure, its particle size distribution is 0.7-15 μ m, and chemical property 0.2C specific discharge capacity is 179.0mAh/g, and the 1C specific discharge capacity is 170.6mAh/g, and 30 weeks circulation specific discharge capacities are 165.3mAh/g.
The comparative example 1:
In embodiment 2, keep other parameter constants, changing sintering temperature in baking furnace is 720 ℃.The powder body material finally obtained is through X-ray diffraction (XRD) and ESEM (SEM) test, and what draw is not the individual particle structure polynary positive pole material that degree of crystallinity is intact.And the chemical property extreme difference, the 0.2C specific discharge capacity is only 75.3mAh/g, and the 1C specific discharge capacity is 42.6mAh/g, and discharge test can't be circulated because capacity is too low.
The comparative example 2:
In embodiment 3, keep other parameter constants, it is 2.31g that change adds the quality of magnesium nitrate.The individual particle structure polynary positive pole material that is doped Ti and Al element finally obtained, but test and can find out by XRD, this material XRD collection of illustrative plates has the dephasign peak of obvious MgO.By electrochemical property test, obtaining the 0.2C specific discharge capacity is 157.8mAh/g, and the 1C specific discharge capacity is 135.3mAh/g, and within 30 weeks, the circulation specific discharge capacity is 95.7mAh/g, and charge-discharge performance is poor.
Claims (5)
1. one kind is applicable to high-tension multielement cathode lithium electric material, it is characterized in that: this multielement cathode lithium electric material is the individual particle pattern, and particle diameter is distributed as 0.5-15 μ m, adopts the nickel-cobalt-manganese multi anode material for lithium-ion batteries of composite mixed element, and chemical formula is LiNi
xco
ymn
zm
an
bo
2, in formula, the span of x, y, z is: 0.2≤x≤0.9,0≤y≤0.4,0.1≤z≤0.5,0<a+b=1-x-y-z≤0.05, in formula, M is any one in titanium, aluminium, iron, vanadium, silicon, fluorine, group of the lanthanides, actinides, N is any one in calcium, magnesium, aluminium, zirconium, iron, titanium.
2. the preparation method of multielement cathode lithium electric material according to claim 1 is characterized in that comprising the following steps:
(1) join in proportion NaOH and NH by the mixing salt solution of nickel, cobalt, manganese and doped with the soluble-salt solution of M element
3mixed-alkali solution in, adjusting pH value be 7-10, forms suspension stir 1-5h at the temperature of 30-80 ℃ after, then by the suspension filtered washing that forms, oven dry acquisition the intermediate Ni doped with the polynary positive pole material of M element
xco
ymn
zm
a(OH)
2;
(2) by the intermediate of the obtained polynary positive pole material doped with the M element, be Li:(Ni+Co+Mn in molar ratio)=ratio of 1-1.12:1 and lithium salts mix, lithium salts is a kind of in lithium hydroxide, lithium carbonate or lithium nitrate, and add oxide or volatile salt doped with the N element to mix, grind 1-8h, at 350-550 ℃ of lower low temperature presintering 1-5h; Add the PVAC polyvinylalcohol solution that concentration is 1-10% in the material after presintering, the PVA solution usage by percentage to the quality, account for the 10-20% of quality of material after presintering, after mixing in the roasting temperature 10-25h of 800-1000 ℃, come out of the stove and be cooled to room temperature, obtain the individual particle structure nickel-cobalt-manganese multi anode material for lithium-ion batteries doped with M.
3. the preparation method of multielement cathode lithium electric material according to claim 2, it is characterized in that: the mixed-alkali solution used in described step (1) is NaOH and NH
3mixed solution, the pH value of alkaline solution>8, wherein in mixed-alkali solution, the molar concentration of NaOH is 0.2-0.9mol/L, NH
3molar concentration be 0.1-0.9mol/L, the consumption of mixed-alkali solution is the intermediated chemistry formula Ni by doped with the polynary positive pole material of M element
xco
ymn
zm
a(OH)
2the 1-1.07 of the molal quantity calculated doubly.
4. the preparation method of multielement cathode lithium electric material according to claim 2, it is characterized in that: the soluble-salt solution of the mixing salt solution of the nickel that uses, cobalt, manganese and the M element that adulterates is one or more the mixture in its sulfate, nitrate, chlorate in described step (1), total metal molar concentration is 0.5-1.5mol/L, and in this metal salt solution, the mol ratio of nickel cobalt manganese and doping M element is by polynary anode material for lithium-ion batteries finished product chemical formula configuration.
5. the preparation method of multielement cathode lithium electric material according to claim 2 is characterized in that: in described step (2), use is doped with the oxide of N element or volatile salt with doped with the intermediate Ni of the polynary positive pole material of M element
xco
ymn
zm
a(OH)
2mol ratio is by polynary anode material for lithium-ion batteries finished product chemical formula configuration.
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Cited By (20)
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| CN103730653A (en) * | 2014-01-08 | 2014-04-16 | 山东精工电子科技有限公司 | Method for preparing rare earth element-doped nickel cobalt lithium manganate positive electrode material |
| CN103855384A (en) * | 2014-03-25 | 2014-06-11 | 海宁美达瑞新材料科技有限公司 | Rare-earth doping modified lithium ion battery ternary positive electrode material and preparation method thereof |
| CN104134791A (en) * | 2014-07-10 | 2014-11-05 | 宁波金和新材料股份有限公司 | High-voltage mono-crystal lithium nickel cobalt manganese oxide anode material and preparation method thereof |
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