CN100353593C - Production of lithium-cobalt-nickel oxide-base anode material by coprecipitation - Google Patents
Production of lithium-cobalt-nickel oxide-base anode material by coprecipitation Download PDFInfo
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- CN100353593C CN100353593C CNB2004100946363A CN200410094636A CN100353593C CN 100353593 C CN100353593 C CN 100353593C CN B2004100946363 A CNB2004100946363 A CN B2004100946363A CN 200410094636 A CN200410094636 A CN 200410094636A CN 100353593 C CN100353593 C CN 100353593C
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Abstract
The present invention relates to a method for preparing Li<1+x>Ni<1-y>CoyO2 powder. X is equal to or more than -0.2 but is equal to or less than 0.2, and y is equal to or more than 0.05 but is equal to or less than 0.5. The method comprises the steps that an excessive first solution is added to a second solution to form a mixed solution, the first solution is a saturated lithium hydroxide water solution, the second solution is a water solution containing nickel salt and cobalt salt, the metal ion concentration in the second solution is between 0.5 M and 10 M, and the mole ratio of the nickel salt and the cobalt salt is 1-y: y; the mixed solution is stirred; the mixed solution is filtered, and a precursor together-sinking object is obtained, and the mole ratio of lithium, nickel and cobalt ions is 1+x: 1-y: y; the precursor together-sinking object is heated to more than 600 DEG C.
Description
Technical field
The invention relates to a kind of preparation method of positive electrode, refer to a kind of preparation method who is applicable to lithium-nickel-cobalt-oxygen thing positive electrode especially.
Background technology
Because Portable, wireless, consumer products market that weight is light and handy is flourish, as the positive rapid spread in secondary cell market of its power supply.No matter be that electronics, information, communication apparatus or living doctor's equipment all have urgent demand to secondary cell.Common small-sized secondary batteries has nickel-cadmium cell, Ni-MH battery, lithium ion battery or the like at present.Wherein, lithium rechargeable battery is owing to have high volumetric capacitance, pollution-free, advantage such as the cycle charge discharge characteristic is good, and meets the compact requirement of modern electronic product, significantly is applied to various small-sized portable type 3C Products.
The lithium-nickel-cobalt-oxygen thing is one of positive electrode of lithium rechargeable battery.Yet the preparation method of known lithium-nickel-cobalt-oxygen thing is quite complicated.At first, known lithium-nickel-cobalt-oxygen thing preparation method is first with nickel salt and cobalt salt and alkaline solution such as potassium hydroxide or NaOH reaction, obtains the nickel hydroxide of alkalescence and the coprecipitated thing of cobalt hydroxide.This coprecipitated thing need be through washing repeatedly, to remove remaining potassium or sodium ion.Then, again with the coprecipitated thing of nickel hydroxide, cobalt hydroxide that cleans up and lithium hydroxide in the solid-state reaction mode after fully mixing, just can carry out sintering, finish whole processing procedure.But, the mixed process of this solid state reaction need be through very long milling time, add because of the reaction between powder particle and need be undertaken, need long high-temperature heat treatment just can obtain the crystalline phase that needs, cause known processing procedure very consuming time by ions diffusion.In addition, known processing procedure except the processing procedure time is long, mix with lapping mode (solid-state reaction) also more inhomogeneous, and easily because mixed grinding causes by other element pollution, and the also more also control of the composition of each composition.
Summary of the invention
Order of the present invention is being to provide a kind of Li
1+xNi
1-yCo
yO
2The preparation method of powder.
With respect to known technology, method of the present invention not only can be simplified processing procedure, and the lithium-nickel-cobalt-oxygen thing predecessor that generates reaches the mixing of atom level, can be under short period and lower heat treatment temperature synthetic lithium-nickel-cobalt-oxygen thing powder, significantly shorten the processing procedure time.And because of exempting the mixed grinding process, can avoid the pollution of other element, be easy to control the composition of positive electrode powder.
For achieving the above object, a kind of Li provided by the invention
1+xNi
1-yCo
yO
2The preparation method of powder, wherein-0.2≤x≤0.2,0.05≤y≤0.5, may further comprise the steps:
(A) the first excessive solution is added in second solution, to form a mixed solution, wherein this first solution is saturated lithium hydroxide aqueous solution, this second solution is the aqueous solution that contains nickel salt and cobalt salt, and this second GOLD FROM PLATING SOLUTION belongs to ion concentration between between the 0.5M to 10M, wherein this nickel salt: the mole ratio of this cobalt salt is 1-y: y;
(B) stir this mixed solution;
(C) filter this mixed solution, obtain the coprecipitated thing of a forerunner, lithium ion in the coprecipitated thing of this forerunner: nickel ion: the mole ratio of cobalt ions is 1+x: 1-y: y; And
(D) heat more than the coprecipitated thing to 600 of this forerunner ℃.
Wherein nickel salt can be any known nickel salt, and preferable is the higher nickel salt of solubility, for example nickel nitrate, nickel acetate, nickel chloride or nickelous sulfate etc. in water.
Wherein cobalt salt can be any known cobalt salt, and preferable is the higher cobalt salt of solubility, for example cobalt nitrate, cobalt acetate, cobalt chloride or cobaltous sulfate etc. in water.
Wherein the volume of first solution of step (A) is more than 1 times of volume of second solution, is preferably between 1.5 times to 5 times.
Wherein the heat treatment time of step (C) is more than 4 hours, is preferably between 8 hours to 12 hours.
In addition, step (A) also can add a spot of another metallic salt again, replaces cobalt salt with part, in order to be doped in Li
1+xNi
1-yCo
yO
2Powder, its content accounts for whole Li
1+xNi
1-yCo
yO
2The mole ratio of powder is between 0 to 0.1.This is doped in Li
1+xNi
1-yCo
yO
2The metallic salt of powder can be any known metallic salt, and preferable is aluminium salt, magnesium salts, zinc salt, manganese salt or titanium salt.Thus, preparation method of the present invention can be at preparation Li
1+xNi
1-yCo
yO
2During powder, the required metal ion that mixes simultaneously, and do not need extra step.Therefore, preparation method of the present invention is a very simple and effective processing procedure.
Description of drawings
Fig. 1 is the X-ray diffraction diagram of one embodiment of the invention.
Fig. 2 is the cycle charge discharge electrograph of one embodiment of the invention.
Fig. 3 is the X-ray diffraction diagram of another embodiment of the present invention.
Fig. 4 is the cycle charge discharge electrograph of another embodiment of the present invention.
Embodiment
Li of the present invention
1+xNi
1-yCo
yO
2In the powder preparation method, the mole ratio of nickel salt and cobalt salt is according to Li
1+xNi
1-yCo
yO
2The metering of nickel and cobalt is than adding in the powder, and the mole ratio of nickel salt and cobalt salt is 0.8: 0.2 in the present embodiment.Li of the present invention
1+xNi
1-yCo
yO
2Nickel salt that uses in the powder preparation method and cobalt salt are preferably nickel salt soluble in water and cobalt salt, and nickel salt that is adopted and cobalt salt are nickel nitrate and cobalt nitrate in the present embodiment.Li of the present invention
1+xNi
1-yCo
yO
2In the powder preparation method, it is excessive that saturated lithium hydroxide aqueous solution needs.In present embodiment, the volume of saturated lithium hydroxide aqueous solution is the two volumes that contains the aqueous solution of 1M cobalt, nickel metal ion.
Embodiment one: LiNi
0.8Co
0.2O
2Material
Is 0.8: 0.2 ratio with nickel nitrate and cobalt nitrate according to mole ratio, is mixed with the aqueous solution that contains the 1M metal ion, and it is dissolved in the aqueous solution fully.Then, add the saturated lithium hydroxide aqueous solution of two volumes again in this aqueous solution.After fully stirring, filter this aqueous solution and can obtain LiNi
0.8Co
0.2O
2The predecessor of material.This predecessor is placed oxygen atmosphere heat treatment, be warming up to 600 ℃, 700 ℃, 750 ℃, 800 ℃ or 900 ℃ with the programming rate of 1 ℃/min, and hold warm processing after 8 hours, reduce to room temperature in the cold mode of stove again, can obtain LiNi
0.8Co
0.2O
2Powder.Observe with the sweep electron microscope photo, synthetic powder diameter is about about 1 to 2 μ m.
Test result
A) composition analysis
The powder of preparation is dissolved in the aqueous hydrochloric acid solution, be diluted to debita spissitudo after, analyze the concentration of metal ion in the obtain solution with Atomic Absorption Spectrometer.Calculate the mole ratio of metal ion again.
Present embodiment is with identical manufacturing method thereof, through the heat treatment of different temperatures, and resulting lithium-nickel-cobalt-oxygen thing powder, its results of elemental analyses is as shown in table 1.Find the result all with the composition (LiNi that is scheduled to
0.8Co
0.2O
2) very approaching.This is just expression also, and in the resulting lithium-nickel-cobalt-oxygen thing of preparation method of the present invention positive electrode, the metering of nickel and cobalt meets the mole ratio (0.8: 0.2) of nickel salt and cobalt salt than (0.8: 0.2).Therefore, among the preparation method of the present invention, in the nickel salt of preparing according to different nickel, cobalt mole ratio, cobalt saline solution, carry out coprecipitated reaction, can obtain Li really according to the metering ratio by adding excessive saturated lithium hydroxide aqueous solution
1+xNi
1-yCo
yO
2Product.
Table 1
B) X-ray diffraction analysis
Confirm in the synthetic lithium-nickel-cobalt-oxygen thing that the mole ratio of lithium, nickel, cobalt element is after the correct mole ratio, identifies the crystalline phase of lithium-nickel-cobalt-oxygen thing again with the X-ray diffraction diagram.Fig. 1 is the X-ray diffraction diagram of present embodiment, in order to analyze the crystalline phase of synthetic lithium-nickel-cobalt-oxygen thing positive electrode powder.As seen from Figure 1, under different heat treatment temperatures, with the synthetic LiNi of the processing procedure of present embodiment
0.8Co
0.2O
2The X-ray diffraction collection of illustrative plates of powder is all the same, is typical LiNi
0.8Co
0.2The crystallization of O2 structure, and do not have other secondary and generate mutually.Confirm that method of the present invention really can simpler mode fast, successfully prepare and form and the extremely close high-purity lithium-nickel-cobalt-oxygen thing of estimating of nickel, cobalt mole ratio.
C) cycle charge discharge electrical testing
According to 83: 10: 7 ratio of weight ratio, (NMP N-methylpyrollidone) is mixed into slurry, evenly coats on the aluminium foil again with solvent N-methyl nafoxidine ketone with the powder of present embodiment and acetylene carbon black and polyvinylidene fluoride (PVDF).After the drying, make suitable anodal test piece, and form 2032 button cells, to carry out the cycle charge discharge electrical testing with the lithium metal.
The cycle charge discharge electrical testing of present embodiment is to be under 4.3V and the 3.0V discharging and recharging cut-ff voltage, carries out charge-discharge test with the charge-discharge velocity of C/10, and its result as shown in Figure 2.In the present embodiment, (600 ℃～900 ℃) resulting lithium-nickel-cobalt-oxygen thing powder under the different heat treatment temperature, behind 13 circle cycle charge-discharges, the specific capacitance decline is all very little, the synthetic LiNi of expression present embodiment
0.8Co
0.2O
2The charge-discharge characteristic of positive electrode powder is good.Through the resulting LiNi of heat treatments at different
0.8Co
0.2O
2In the positive electrode powder, synthetic LiNi in heat is located down with 800 ℃
0.8Co
0.2O
2The cycle charge discharge electrical characteristics of positive electrode powder are best, are 178mAh/g than electric capacity just, and after discharging and recharging through 13 circles, specific capacitance is still up to 180mAh/g, the LiNi of visible present embodiment
0.8Co
0.2O
2Not only the cycle charge discharge electrical characteristics are good for the positive electrode powder, and have higher capacitance than existing mobile phone with anode material of lithium battery.
Embodiment two: LiNi
0.8Co
0.17Al
0.03O
2Material
In order to improve LiNi
0.8Co
0.2O
2Thermostability, present embodiment is in LiNi
0.8Co
0.2O
2Middle doping Trace Aluminum ion.
At first, nitrate, cobalt nitrate and aluminum nitrate according to 0.8: 0.17: 0.03 ratio of mole ratio, are mixed with the aqueous solution that contains the 1M metal ion, and it is dissolved in the aqueous solution fully.Then, add the saturated lithium hydroxide aqueous solution of two volumes again in this aqueous solution.After fully stirring, filter this aqueous solution and can obtain LiNi
0.8Co
0.17Al
0.03O
2The predecessor of material.This predecessor is being passed under the oxygen atmosphere, holding warm processing with 800 ℃, can obtain LiNi
0.8Co
0.17Al
0.03O
2Powder.By this, other step need be do not increased, the anodal powder of lithium-nickel-cobalt-oxygen thing of other ion that mixes can be prepared easily.
Test result
A) X-ray diffraction analysis
Fig. 3 is LiNi
0.8Co
0.17Al
0.03O
2X-ray diffraction collection of illustrative plates.The LiNi of present embodiment
0.8Co
0.17Al
0.03O
2The same Fig. 1 of X-ray diffraction collection of illustrative plates, be the LiNi of a standard
0.8Co
0.2O
2The crystallization of structure, and do not have the generation of two second phases.
B) charge and discharge cycles test
According to 83: 10: 7 ratio of weight ratio, (NMP N-methylpyrollidone) is mixed into slurry, evenly coats on the aluminium foil again with solvent N-methyl nafoxidine ketone with the powder of present embodiment and acetylene carbon black and polyvinylidene fluoride (PVDF).After the drying, make suitable anodal test piece, and form 2032 button cells, to carry out the cycle charge discharge electrical testing with the lithium metal.Its result as shown in Figure 4, the scope that discharges and recharges between 3.0V～4.3V, the specific capacitance that goes out that records with the charge-discharge velocity of C/10 is 174mAh/g, the specific capacitances after discharging and recharging through 15 circles still have 161mAh/g, the specific capacitance decline is very little, the LiNi of expression present embodiment
0.8Co
0.17Al
0.03O
2The charge-discharge characteristic of positive electrode powder is good.In addition, can verify the LiNi of present embodiment by the performance curve of voltage among the figure and electric capacity
0.8Co
0.17Al
0.03O
2Positive electrode meets the performance of typical lithium cobalt nickel positive electrode at electric capacity that discharges and recharges and voltage.And, the LiNi of present embodiment
0.8Co
0.17Al
0.03O
2Positive electrode, when being put into 3.0V, after it discharged and recharged through 15 circles, specific capacitance still had 165 left and right sides mAh/g, that is behind doping Trace Aluminum ion, still has quite high capacitance.
The present invention can make nickel ion, cobalt ions, lithium ion directly generate the coprecipitated thing of lithium-nickel-cobalt-oxygen thing forerunner in solution by adding excessive saturated lithium hydroxide solution, just can heat-treat then, obtains product.In comparison, known lithium-nickel-cobalt-oxygen thing preparation method just seems very complicated.Therefore, the preparation method of lithium-nickel-cobalt-oxygen thing positive electrode of the present invention is not only with known complete different, and has tangible progressive on processing procedure is simplified.And method of the present invention is all carried out in liquid phase, does not need mixed grinding, can be by other element pollution, and composition is formed more easy to control, is good than known method really.
And method of the present invention also can be undertaken coprecipitatedly by directly add other metal ion in solution, reaches the effect of doping, does not need additionally to increase other step fully.This also be known method can't reach.
The foregoing description is only given an example for convenience of description, and the interest field that the present invention advocated should be as the criterion so that claim is described certainly, but not only limits to the foregoing description.
Claims (7)
1. Li
1+xNi
1-yCo
yO
2The preparation method of powder, wherein-0.2≤x≤0.2,0.05≤y≤0.5, may further comprise the steps:
(A) the first excessive solution is added in second solution, to form a mixed solution, wherein this first solution is saturated lithium hydroxide aqueous solution, this second solution is the aqueous solution that contains nickel salt and cobalt salt, and this second GOLD FROM PLATING SOLUTION belongs to ion concentration between between the 0.5M to 10M, this nickel salt: the mole ratio of this cobalt salt is 1-y: y;
(B) stir this mixed solution;
(C) filter this mixed solution, obtain the coprecipitated thing of a forerunner, lithium ion in the coprecipitated thing of this forerunner: nickel ion: the mole ratio of cobalt ions is 1+x: 1-y: y; And
(D) heat more than the coprecipitated thing to 600 of this forerunner ℃.
2. Li as claimed in claim 1
1+xNi
1-yCo
yO
2The preparation method of powder is characterized in that, wherein this nickel salt is nickel nitrate, nickel acetate, nickel chloride or nickelous sulfate.
3. Li as claimed in claim 1
1+xNi
1-yCo
yO
2The preparation method of powder is characterized in that, wherein this cobalt salt is cobalt nitrate, cobalt acetate, cobalt chloride or cobaltous sulfate.
4. Li as claimed in claim 1
1+xNi
1-yCo
yO
2The preparation method of powder is characterized in that, wherein the volume of this first solution is more than 1 times of volume of this second solution.
5. Li as claimed in claim 1
1+xNi
1-yCo
yO
2The preparation method of powder is characterized in that, wherein the heat treatment time of this step (D) is more than 4 hours.
6. Li as claimed in claim 1
1+xNi
1-yCo
yO
2The preparation method of powder is characterized in that, wherein this step (A) can add a metallic salt again, and wherein this metallic salt accounts for Li
1+xNi
1-yCo
yO
2The mole ratio of powder is between 0 to 0.1.
7. Li as claimed in claim 6
1+xNi
1-yCo
yO
2The preparation method of powder is characterized in that, wherein this metallic salt is aluminium salt, magnesium salts, zinc salt, manganese salt or titanium salt.
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|---|---|---|---|
| CNB2004100946363A CN100353593C (en) | 2004-11-11 | 2004-11-11 | Production of lithium-cobalt-nickel oxide-base anode material by coprecipitation |
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|---|---|
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| CN100353593C true CN100353593C (en) | 2007-12-05 |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4980080A (en) * | 1988-06-09 | 1990-12-25 | Societe Anonyme Dite: Saft | Process of making a cathode material for a secondary battery including a lithium anode and application of said material |
| CN1271185A (en) * | 2000-05-08 | 2000-10-25 | 许开华 | Preparation method and equipment of the anode material for lithium ion cell |
| CN1506312A (en) * | 2002-12-11 | 2004-06-23 | 中国科学院成都有机化学研究所 | Prepn process of submicron level positive pole material for lithium ion cell |
-
2004
- 2004-11-11 CN CNB2004100946363A patent/CN100353593C/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4980080A (en) * | 1988-06-09 | 1990-12-25 | Societe Anonyme Dite: Saft | Process of making a cathode material for a secondary battery including a lithium anode and application of said material |
| CN1271185A (en) * | 2000-05-08 | 2000-10-25 | 许开华 | Preparation method and equipment of the anode material for lithium ion cell |
| CN1506312A (en) * | 2002-12-11 | 2004-06-23 | 中国科学院成都有机化学研究所 | Prepn process of submicron level positive pole material for lithium ion cell |
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| CN1773750A (en) | 2006-05-17 |
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