CN103682326A - High-capacity lithium cobalt oxide-base lithium ion battery anode material and preparation method thereof - Google Patents
High-capacity lithium cobalt oxide-base lithium ion battery anode material and preparation method thereof Download PDFInfo
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- 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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Abstract
The invention discloses a high-capacity lithium cobalt oxide-base lithium ion battery anode material. The material is a lithium cobalt oxide finished product which is obtained by mixing modified lithium cobalt oxide in different granularities and coating the lithium cobalt oxide, the anode material contains a cobalt-source substance, a lithium-source substance, a doping agent and a coating material, wherein the molar ratio of Li to Co is 0.95 to 1.2, the doping quantity of the doping agent is 0.01 to 10 percent by weight, and the doping quantity of the coating material is 0.01 to 20 percent by weight. The capacity of the lithium cobalt oxide material is improved by mixing the lithium cobalt oxide in different granularities, the stability, safety and electrochemical property of the material under the high voltage condition of more than 4.2V are improved through doping and coating, and the high-temperature circulating property is improved.
Description
Technical field
The present invention relates to anode material for lithium-ion batteries and preparation thereof, relate in particular to a kind of high power capacity cobalt acid lithium base lithium ion cell positive material and preparation method thereof.
Background technology
Along with the high speed development of electronic technology, the continuous upgrading of electronic product, requires also more and more higher to the energy density of battery.The charging voltage of the conventional small-scale lithium ion cell of using is 4.2V at present, take the high-end electronic product of intelligence that American apple company and Korea S Samsung be representative, himself product battery used is updated, cell voltage is promoted to 4.3V, 4.35V or higher high voltage battery core.Improve the charging voltage of battery, the capacity that can be in not increasing battery significantly improves battery under the condition of active material, be one of effective way improving energy content of battery density, for the high-energy-density and the continuation of the journey that meet high-end portable equipment, require to be significant.Therefore, domestic battery material is just towards high voltage future development.
Due to cobalt acid lithium have higher operating voltage, high energy density, easily synthetic and can fast charging and discharging etc. advantage, be therefore widely used.But cobalt acid lithium itself exists fault of construction, when the charge cutoff voltage of lithium ion battery is during higher than 4.2V, a large amount of Co in cobalt acid lithium structure
3+can become Co
4+, Co
4+existence can cause the formation of oxygen defect in cobalt acid lithium crystal formation, thereby weaken the adhesion between transition metal Co and oxygen, make Co
4+be dissolved in electrolyte, destroy the crystal structure of positive pole material of lithium cobalt acid, the specific capacity of battery is reduced rapidly, cycle performance variation.Therefore, first need to solve the stability of cobalt acid lithium structure under high voltage.
The method that improves lithium rechargeable battery high capacity also has: (a) Chinese patent CN 1665052A mixes by the cobalt acid lithium of the particle diameter that varies in size the compacted density that improves material, thereby the capacity that increases unit volume is realized high capacity, because its small particle diameter is more, to battery, brought potential safety hazard; (b) Chinese patent CN 101436666A proposes first to prepare oarse-grained cobalt acid lithium material, again by cobalt carbonate and lithium carbonate in large cobalt acid lithium particle surface granulation, thereby adhere to short grained cobalt acid lithium particle at large particle surface, and then tap density and the volume and capacity ratio of raising positive electrode, but it is bad to pass through once sintered its crystallinity of cobalt acid lithium, can affect the cycle performance of battery; (c) Chinese patent CN 102779976A propose the to vary in size cobalt acid lithium of particle mixes, then comes pressure-raising real density and security performance etc. through PROCESS FOR TREATMENT such as overdoping, sintering, coated, sintering.But its complex process, has increased production cost.
Given this, a kind of high power capacity cobalt acid of necessary exploitation lithium material, make it not only possess higher operating voltage and energy density, and when the charge cutoff voltage of lithium ion battery is during higher than 4.2V, possess high stability, fail safe and superior chemical property, high temperature cyclic performance particularly, thus meet the current market demand.
Summary of the invention
Goal of the invention: the object of the invention is in order to make up the deficiencies in the prior art, high power capacity cobalt acid lithium base lithium ion cell positive material that a kind of security performance is good, chemical property is good and preparation method thereof is provided.
The technical solution used in the present invention:
A kind of high power capacity cobalt acid lithium base lithium ion cell positive material, described high power capacity cobalt acid lithium base lithium ion cell positive material mixes the cobalt acid lithium of the modification of large and small different-grain diameter, through being coated, obtain again cobalt acid lithium finished product, in described positive electrode, contain cobalt source material, lithium source substance, dopant M, dopant M ' and clad material N, wherein the mol ratio of Li:Co is 0.95～1.2, the volume of dopant M and dopant M ' is 0.01～10 wt%, and the volume of clad material N is 0.01～20 wt%.
The preparation method of a kind of high power capacity cobalt acid lithium base lithium ion cell positive material of the present invention, specifically comprises the steps:
(1) prepare large particle diameter cobalt acid lithium material A, D50 is 8～30 μ m, the preparation method who adopts is: cobalt source material, lithium source substance and dopant M are mixed according to a certain percentage, mixed method is that dry type is mixed or wet mixed, wherein the mol ratio of Li, Co is 0.95～1.2, the volume of dopant M is in 0.01～10 wt%(the present invention, to relate to the quality percentage composition of material addition, if without specified otherwise, is all for the quality of cobalt acid lithium base material); The material mixing is carried out to sintering, and sintering main temperature is controlled at 600 ℃～1350 ℃, and main warm area sintering time is 5～40 h, and whole sintering process is to carry out under air or oxygen atmosphere, and throughput control range is 2～30 m
3/ h, through fragmentation, pulverizing, classification, the PROCESS FOR TREATMENT such as sieve, obtains required cobalt acid lithium semi-finished product A by the material after sintering.
(2) prepare small particle diameter cobalt acid lithium material B, D50 is 1～8 μ m, the preparation method who adopts is: cobalt source material, lithium source substance and dopant M ' are mixed according to a certain percentage, mixed method is that dry type is mixed or wet mixed, wherein the mol ratio of Li, Co is 0.95～1.2, and the volume of dopant M ' is 0.01～10 wt%; The material mixing is carried out to sintering, and sintering main temperature is controlled at 300 ℃～1000 ℃, and main warm area sintering time is 4～35 h, and whole sintering process is to carry out under air or oxygen atmosphere, and throughput control range is 2～30 m
3/ h, through fragmentation, pulverizing, classification, the PROCESS FOR TREATMENT such as sieve, obtains required cobalt acid lithium semi-finished product B by the material after sintering.
(3) according to certain ratio, A, B bi-material are mixed, when take large particle diameter cobalt acid lithium A during as main body, the volume of small particle diameter cobalt acid lithium B is 0～50 wt%, its quality percentage composition is the mass percent with respect to large particle diameter cobalt acid lithium A, when small particle diameter volume is greater than 50%, the mass ratio of A:B is 1:2～2:1, after mixing, obtains material C, and D50 is 5～25 μ m.
(4) material C is coated, clad material is N, and the volume of N is 0.01～20 wt%, and method for coating used is that wet type is coated, dry type is coated or coprecipitation.
(5) material C after coated is carried out to sintering, sintering main temperature is controlled at 400～1250 ℃, and the sintering time of main temperature is 4～36 h, and whole sintering process is to carry out under air or oxygen atmosphere, and throughput control range is 2～30 m
3/ h, by the material after sintering through fragmentation, pulverizing, classification, sieve, the PROCESS FOR TREATMENT such as deironing, obtain required cobalt acid lithium finished product.
The cobalt source material relating in described step (1) and step (2) is selected from one or more the mixture into cobaltosic oxide, hydroxy cobalt oxide, cobalt hydroxide, cobalt carbonate, cobalt oxalate and cobalt oxide, and D50 is between 0.2～30 μ m.
The lithium source substance relating in described step (1) and step (2) is selected from as one or more the mixture in lithium hydroxide, lithium carbonate, lithium oxalate.
Dopant M ' in dopant M in described step (1) and step (2) is all selected from as First Transition element (Sc, Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Zn), the second transition elements (Y, Zr, Nb, Mo, Tc, Ru, Rh, Pd, Ag, Cd), alkaline earth element (Be, Mg, Ca, Sr, Ba) and rare earth element (La, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu) oxide, halide, hydroxide, metallorganic, nitrate, sulfate, carbonate, oxalates phosphate, silicate, citrate or with one or more mixture of the composite oxides of other metallic elements.
Clad material N in described step (4) is selected from as First Transition element (Sc, Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Zn), the second transition elements (Y, Zr, Nb, Mo, Tc, Ru, Rh, Pd, Ag, Cd), alkaline earth element (Be, Mg, Ca, Sr, Ba) and rare earth element (La, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu) oxide, halide, hydroxide, metallorganic, nitrate, sulfate, carbonate, oxalates phosphate, silicate, citrate or with one or more mixture of the composite oxides of other metallic elements.
Clad material N in described step (4) is one or more mixture of material mentioned in the metallic compound of element F or the metallic compound of element F and above-mentioned dopant M.
Beneficial effect: compared with prior art, the beneficial effect that the present invention brings is: high power capacity cobalt acid lithium base lithium ion cell positive material of the present invention and preparation method thereof carries out modification by adulterating or being coated to cobalt acid lithium, guarantees the stability of structure when cobalt acid lithium excessively takes off lithium under high voltage; By the cobalt acid lithium of large small particle diameter is mixed, improved the volume capacity of material, realize high capacity.By the method, obtain lithium cobaltate cathode material being greater than under the high voltage condition of 4.2V, there is Li
+de-embedding performance is good, capacity is high, security performance good, chemical property is good, the advantage such as high temperature cyclic performance excellence particularly, and this preparation method is simple to operate, can realize smoothly suitability for industrialized production.Through experiment test, learn, more than first discharge specific capacity all can reach 190 mAh/g, under 45 ℃ of conditions of high temperature, through 100 circulation volume conservation rates, reach more than 92%, 60 ℃ of capability retentions reach more than 88.5%, and 70 ℃ of capability retentions reach more than 83.6%.
Embodiment
Below in conjunction with specific embodiment, the invention will be further described:
Embodiment 1:
(1) prepare large particle diameter cobalt acid lithium material A, cobalt carbonate (D50 is 16 μ m), lithium carbonate, dopant oxidation magnesium and zirconia are mixed according to a certain percentage, wherein the mol ratio of Li, Co is 1.10, the volume of dopant oxidation magnesium is 1.5 wt%, and the volume of dopant oxidation zirconium is 2.5 wt%; Sintering main temperature is 1050 ℃, and main warm area sintering time is 22 h, and whole sintering process is to carry out under air atmosphere, and throughput control range is 15 m
3/ h, through fragmentation, pulverizing, classification, the PROCESS FOR TREATMENT such as sieve, obtains large particle diameter cobalt acid lithium A by the material after sintering, and D50 is 20 μ m.
(2) prepare small particle diameter cobalt acid lithium material B, cobalt carbonate (D50 is 2 μ m), lithium carbonate, dopant oxidation magnesium and zirconia are mixed according to a certain percentage, wherein the mol ratio of Li, Co is 1.10, and the volume of dopant oxidation magnesium is 1.8 wt%; Sintering main temperature is 400 ℃, and main warm area sintering time is 30 h, and whole sintering process is to carry out under air atmosphere, and throughput control range is 8 m
3/ h, through fragmentation, pulverizing, classification, the PROCESS FOR TREATMENT such as sieve, obtains small particle diameter cobalt acid lithium B by the material after sintering, and D50 is 3 μ m.
(3) ratio that is A:B=5:1 according to the weight ratio of A and B is mixed A, B bi-material, after mixing, obtains material C, and D50 is 17 μ m.
(4) material C is coated, clad material is cobalt oxide, and volume is 2 wt%, and method for coating used is that dry type is coated.
(5) material C in step (4) is carried out to sintering, sintering main temperature is controlled at 660 ℃, and the sintering time of main temperature is 15 h, and whole sintering process is to carry out under air atmosphere, and throughput control range is 20 m
3/ h, by the material after sintering through fragmentation, pulverizing, classification, sieve, the PROCESS FOR TREATMENT such as deironing, obtain required cobalt acid lithium.
Embodiment 2:
(1) prepare large particle diameter cobalt acid lithium material A, cobalt carbonate (D50 is 20 μ m), lithium carbonate, dopant oxidation magnesium and zirconia are mixed according to a certain percentage, wherein the mol ratio of Li, Co is 1.10, the volume of dopant oxidation magnesium is 1.5 wt%, and the volume of dopant oxidation zirconium is 2.5 wt%; Sintering main temperature is 1050 ℃, and main warm area sintering time is 22 h, and whole sintering process is to carry out under air atmosphere, and throughput control range is 15 m
3/ h, through fragmentation, pulverizing, classification, the PROCESS FOR TREATMENT such as sieve, obtains large particle diameter cobalt acid lithium A by the material after sintering, and D50 is 22 μ m.
(2) prepare small particle diameter cobalt acid lithium material B, cobalt carbonate (D50 is 2 μ m), lithium carbonate, dopant oxidation magnesium and zirconia are mixed according to a certain percentage, wherein the mol ratio of Li, Co is 1.10, and the volume of dopant oxidation magnesium is 1.8 wt%; Sintering main temperature is 400 ℃, and main warm area sintering time is 30 h, and whole sintering process is to carry out under air atmosphere, and throughput control range is 8 m
3/ h, through fragmentation, pulverizing, classification, the PROCESS FOR TREATMENT such as sieve, obtains small particle diameter cobalt acid lithium B by the material after sintering, and D50 is 3 μ m.
(3) ratio that is A:B=6:1 according to the weight ratio of A and B is mixed A, B bi-material, after mixing, obtains material C, and D50 is 19 μ m.
(4) material C is coated, clad material is aluminum fluoride and zirconia, and the volume of aluminum fluoride is 2 wt%, and zirconic volume is 1.5%, and method for coating used is that dry type is coated.
(5) material C in step (4) is carried out to sintering, sintering main temperature is controlled at 660 ℃, and the sintering time of main temperature is 15 h, and whole sintering process is to carry out under air atmosphere, and throughput control range is 20 m
3/ h, by the material after sintering through fragmentation, pulverizing, classification, sieve, the PROCESS FOR TREATMENT such as deironing, obtain required cobalt acid lithium.
Embodiment 3:
(1) prepare large particle diameter cobalt acid lithium material A, cobalt carbonate (D50 is 7 μ m), lithium carbonate, dopant oxidation magnesium are mixed according to a certain percentage, wherein the mol ratio of Li, Co is 0.95, the volume of dopant oxidation magnesium is 0.01 wt%, sintering main temperature is controlled at 1350 ℃, main warm area sintering time is 5 h, and whole sintering process is to carry out under air atmosphere, and throughput control range is 30 m
3/ h, through fragmentation, pulverizing, classification, the PROCESS FOR TREATMENT such as sieve, obtains required cobalt acid lithium semi-finished product A by the material after sintering, and D50 is 10 μ m.
(2) materials A is coated, clad material is aluminium oxide, and volume is 0.01 wt%, and method for coating used is that wet type is coated.The coated solvent adopting of wet type is isopropyl alcohol.
(3) the cobalt acid lithium semi-finished product of gained in step (4) are carried out to sintering, sintering main temperature is controlled at 400 ℃, and the sintering time of main temperature is 36 h, and whole sintering process is to carry out under air atmosphere, and throughput control range is 30 m
3/ h, by the material after sintering through fragmentation, pulverizing, classification, sieve, the PROCESS FOR TREATMENT such as deironing, obtain required cobalt acid lithium finished product.
Embodiment 4:
(1) prepare large particle diameter cobalt acid lithium material A, by cobalt carbonate (D50 is 29 μ m), lithium carbonate, dopant, be that titanium dioxide mixes according to a certain percentage, wherein the mol ratio of Li, Co is 1.2, the volume of dopant M is 10 wt%, sintering main temperature is controlled at 600 ℃, whole sintering process is to carry out under oxygen atmosphere, and throughput control range is 2 m
3/ h, through fragmentation, pulverizing, classification, the PROCESS FOR TREATMENT such as sieve, obtains required cobalt acid lithium semi-finished product A by the material after sintering, and D50 is 30 μ m.
(2) prepare small particle diameter cobalt acid lithium material B, by cobalt carbonate (D50 is 10 μ m), lithium carbonate, dopant, be that titanium dioxide mixes according to a certain percentage, wherein the mol ratio of Li, Co is 1.2, the volume of dopant M is 10 wt%, sintering main temperature is controlled at 300 ℃, main warm area sintering time is 35h, and whole sintering process is to carry out under oxygen atmosphere, and throughput control range is 2 m
3/ h, through fragmentation, pulverizing, classification, the PROCESS FOR TREATMENT such as sieve, obtains required cobalt acid lithium semi-finished product B by the material after sintering, and D50 is 10 μ m.
(3) ratio that is A:B=1:2 according to the weight ratio of A and B is mixed A, B bi-material, after mixing, obtains material C, and D50 is 25 μ m.
(4) material C is coated, clad material is manganese oxide, and volume is 20 wt%, and method for coating used is that dry type is coated.
(5) material C in step (4) is carried out to sintering, sintering main temperature is controlled at 1250 ℃, and the sintering time of main temperature is 4 h, and whole sintering process is to carry out under oxygen atmosphere, and throughput control range is 2 m
3/ h, by the material after sintering through fragmentation, pulverizing, classification, sieve, the PROCESS FOR TREATMENT such as deironing, obtain required cobalt acid lithium finished product.
Claims (7)
1. high power capacity cobalt acid lithium base lithium ion cell positive material, it is characterized in that: described high power capacity cobalt acid lithium base lithium ion cell positive material mixes the cobalt acid lithium of the modification of large and small different-grain diameter, through being coated, obtain again cobalt acid lithium finished product, in described positive electrode, contain cobalt source material, lithium source substance, dopant M, dopant M ' and clad material N, wherein the mol ratio of Li:Co is 0.95～1.2, the volume of dopant M and dopant M ' is 0.01～10 wt%, and the volume of clad material N is 0.01～20 wt%.
2. the preparation method of a kind of high power capacity cobalt acid lithium base lithium ion cell positive material according to claim 1, is characterized in that: described preparation method specifically comprises the steps:
(1) prepare large particle diameter cobalt acid lithium material A, D50 is 8～30 μ m, the preparation method who adopts is: cobalt source material, lithium source substance and dopant M are mixed according to a certain percentage, mixed method is that dry type is mixed or wet mixed, wherein the mol ratio of Li, Co is 0.95～1.2, and the volume of dopant M is 0.01～10 wt%; The material mixing is carried out to sintering, and sintering main temperature is controlled at 600～1350 ℃, and main warm area sintering time is 5～40 h, and whole sintering process is to carry out under air or oxygen atmosphere, and throughput control range is 2～30 m
3/ h, through fragmentation, pulverizing, classification, the PROCESS FOR TREATMENT such as sieve, obtains required cobalt acid lithium semi-finished product A by the material after sintering;
(2) prepare small particle diameter cobalt acid lithium material B, D50 is 1～8 μ m, the preparation method who adopts is: cobalt source material, lithium source substance and dopant M ' are mixed according to a certain percentage, mixed method is that dry type is mixed or wet mixed, wherein the mol ratio of Li, Co is 0.95～1.2, and the volume of dopant M ' is 0.01～10 wt%; The material mixing is carried out to sintering, and sintering main temperature is controlled at 300～1000 ℃, and main warm area sintering time is 4～35 h, and whole sintering process is to carry out under air or oxygen atmosphere, and throughput control range is 2～30 m
3/ h, through fragmentation, pulverizing, classification, the PROCESS FOR TREATMENT such as sieve, obtains required cobalt acid lithium semi-finished product B by the material after sintering;
(3) according to certain ratio, A, B bi-material are mixed, when take large particle diameter cobalt acid lithium A during as main body, the volume of small particle diameter cobalt acid lithium B is 0～50 wt%, its quality percentage composition is the mass percent with respect to large particle diameter cobalt acid lithium A, when small particle diameter volume is greater than 50%, the mass ratio of A:B is 1:2～2:1, after mixing, obtains material C, and D50 is 5～25 μ m;
(4) material C is coated, clad material is N, and the volume of N is 0.01～20 wt%, and method for coating used is that wet type is coated, dry type is coated or coprecipitation;
(5) material C after coated is carried out to sintering, sintering main temperature is controlled at 400～1250 ℃, and the sintering time of main temperature is 4～36 h, and whole sintering process is to carry out under air or oxygen atmosphere, and throughput control range is 2～30 m
3/ h, by the material after sintering through fragmentation, pulverizing, classification, sieve, the PROCESS FOR TREATMENT such as deironing, obtain required cobalt acid lithium finished product.
3. the preparation method of a kind of high power capacity cobalt acid lithium base lithium ion cell positive material according to claim 2, it is characterized in that: the cobalt source material relating in described step (1) and step (2) is selected from one or more the mixture into cobaltosic oxide, hydroxy cobalt oxide, cobalt hydroxide, cobalt carbonate, cobalt oxalate and cobalt oxide, and D50 is between 0.2～30 μ m.
4. the preparation method of a kind of high power capacity cobalt acid lithium base lithium ion cell positive material according to claim 2, is characterized in that: the lithium source substance relating in described step (1) and step (2) is selected from as one or more the mixture in lithium hydroxide, lithium carbonate, lithium oxalate.
5. the preparation method of a kind of high power capacity cobalt acid lithium base lithium ion cell positive material according to claim 2, it is characterized in that: the dopant M ' in the dopant M in described step (1) and step (2) is all selected from as First Transition element (Sc, Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Zn), the second transition elements (Y, Zr, Nb, Mo, Tc, Ru, Rh, Pd, Ag, Cd), alkaline earth element (Be, Mg, Ca, Sr, Ba) and rare earth element (La, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu) oxide, halide, hydroxide, metallorganic, nitrate, sulfate, carbonate, oxalates, phosphate, silicate, citrate or with one or more mixture of the composite oxides of other metallic elements.
6. the preparation method of a kind of high power capacity cobalt acid lithium base lithium ion cell positive material according to claim 2, it is characterized in that: the clad material N in described step (4) is selected from as First Transition element (Sc, Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Zn), the second transition elements (Y, Zr, Nb, Mo, Tc, Ru, Rh, Pd, Ag, Cd), alkaline earth element (Be, Mg, Ca, Sr, Ba) and rare earth element (La, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu) oxide, halide, hydroxide, metallorganic, nitrate, sulfate, carbonate, oxalates phosphate, silicate, citrate or with one or more mixture of the composite oxides of other metallic elements.
7. the preparation method of a kind of high power capacity cobalt acid lithium base lithium ion cell positive material according to claim 2, is characterized in that: the clad material N in described step (4) is one or more mixture of material mentioned in the metallic compound of F element or the metallic compound of F element and above-mentioned dopant M.
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| CN104016421A (en) * | 2014-06-24 | 2014-09-03 | 南通瑞翔新材料有限公司 | Preparation method for lithium ion positive electrode material |
| CN104282880A (en) * | 2014-10-24 | 2015-01-14 | 湖南杉杉新材料有限公司 | Lithium-cobalt composite oxide lithium ion positive material and preparation method thereof |
| CN104362338A (en) * | 2014-09-17 | 2015-02-18 | 陈虹 | Fe-doped lithium ion cathode material and preparation method thereof |
| CN104538599A (en) * | 2015-01-09 | 2015-04-22 | 高淑萍 | Preparation method of lithium cobalt oxide positive electrode material coated with silicon-modified conducting polymer |
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