CN100420077C - Positive pole material of lithium ion cell - Google Patents
Positive pole material of lithium ion cell Download PDFInfo
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- CN100420077C CN100420077C CNB2006100888085A CN200610088808A CN100420077C CN 100420077 C CN100420077 C CN 100420077C CN B2006100888085 A CNB2006100888085 A CN B2006100888085A CN 200610088808 A CN200610088808 A CN 200610088808A CN 100420077 C CN100420077 C CN 100420077C
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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
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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- Y02E60/10—Energy storage using batteries
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Abstract
This invention relates to a positive material of Li ionic batteries characterizing that it is a ball shape high tap density and high purity oxidized Ni Mn Co and Li in the molecular formula of Li(NiCoMn)1/3O2, the purity of 99.9-99.95% and a ball-shape secondary crystal composed of small grains, the mean diameter is 5-25mum, the tap density is greater than or equal to 2.5g/cu cm.
Description
Technical field
The present invention relates to a kind of positive electrode of lithium ion battery, the anode material for lithium-ion batteries of particularly spherical high-tap density high-purity mangesium oxide nickel manganese cobalt lithium belongs to chemical products.
The invention still further relates to the preparation method of this anode material spherical high-tap density oxidized Ni Mn Co and Li.
Background technology
Lithium ion battery is a kind of emerging power supply; it has the voltage height; capacity is big; plurality of advantages such as safety and environmental protection; therefore be subjected to accepting extensively of people; but the positive electrode of present lithium ion battery is used the most general cobalt acid lithium; its cost of material is higher; and fail safe is relatively poor; fettered the application of lithium ion battery; the also lithium compound of binary such as useful LiMn2O4 or ternary metal; but synthetic method complexity; the course of reaction gas that needs protection; the method that adopts complex-precipitation is with nickel; cobalt; the salting liquid of manganese closes the back with ammino and precipitates with NaOH; this method is because three's complexation constant difference is difficult to the material of the ratio that is fixed; and nickel; cobalt; if the salting liquid post precipitation of manganese forms hydroxide; be easy to be oxidized to the trivalent material, and trivalent material synthetic ternary material electrochemical properties after calcining can descend greatly.Therefore, the method that adopts in the document all is to need inert gas shielding, has increased production cost greatly.
Summary of the invention
Purpose of the present invention is the shortcoming and deficiency in order to overcome above-mentioned prior art just, and provide a kind of highly purified cobalt nickel oxide manganses lithium of anode material spherical high-tap density that is suitable for the lithium ion battery of suitability for industrialized production, thereby reduce the cost of lithium ion battery, promote it further to apply.
The present invention also provides the preparation method of this anode material spherical high-tap density oxidized Ni Mn Co and Li.
The objective of the invention is to realize by following technical proposal:
The positive electrode of lithium ion battery is characterized in that this positive electrode is spherical high-tap density high-purity mangesium oxide nickel manganese cobalt lithium, and molecular formula is Li (NiCoMn)
1/3O
2, purity is 99.9～99.95%, particle is the spherical secondary crystallization body that little crystal grain is formed, 5～25 microns of average diameters, tap density 〉=2.5g/cm
3
The preparation method of anode material for lithium-ion batteries is characterized in that it is undertaken by following step:
(a) at first with deionized water respectively with nickel, cobalt and the manganese aqueous solution of chlorate, sulfate or the nitrate preparation 0.5～2.0M of nickel, cobalt and the manganese of technical grade, wherein nickel, cobalt and manganese molecular proportion are 1: 1: 1, the bicarbonate of the alkali metal of technical grade or ammonium radical ion or carbonate are mixed with the aqueous solution of 0.5～2.0M, and two aqueous solution volume ratios are 1: 2.5～4;
(b) deionized water more than 1/2 of the aqueous solution volume of the chlorate of nickel, cobalt and the manganese of elder generation's adding (a) item, sulfate or nitrate preparation is stirred and heated to 30～90 ℃ in reactor, add in the aqueous solution of chlorate, sulfate or the nitrate of nickel, cobalt and manganese in (a) item with 2～5ml/min flow velocity then, and the pH value of the aqueous solution conditioned reaction system that is mixed with 0.5～2.0M with the bicarbonate or the carbonate of alkali metal or ammonium radical ion is 7.5～9.0 ± 0.1, stirred again 0.5～1 hour, and generated nickelous carbonate cobalt manganese precipitation;
(c) the nickelous carbonate cobalt manganese precipitation in centrifugation then (b) item, and with 1～5 times of deionized water wash 1～3 time of precipitation weight, up to washing lotion pH value＜7, filter the back filter cake and under 60～120 ℃ of temperature, dried 6～10 hours, obtain the highly purified nickelous carbonate cobalt of spherical high-tap density manganese;
(d) in another reactor, add 1～10% technical grade hydrogenperoxide steam generator, stir, be heated to 60～90 ℃, add the highly purified nickelous carbonate cobalt of the spherical high-tap density manganese in (c) item, its nickelous carbonate cobalt manganese and hydrogen peroxide consumption are by weight/volume 1: 4-40, stirred after 2 hours still aging 1 hour, nickelous carbonate cobalt manganese becomes black, centrifugation precipitates then, precipitate 1～3 time with the deionized water wash that adds 1～5 times of nickelous carbonate cobalt manganese weight again, filter cake was dried 6～10 hours under 60～120 ℃ of temperature, obtained the highly purified cobalt nickel oxide manganses of spherical high-tap density.
(e) mix with (d) cobalt nickel oxide manganses and lithium source and by mole 0.95～1.3: 1 of cobalt nickel oxide manganses and lithium at last after, calcined 3～20 hours 800～1100 ℃ temperature, obtain the highly purified oxidized Ni Mn Co and Li of spherical high-tap density.
Described lithium source is lithium carbonate, lithium nitrate, lithium oxalate or lithium hydroxide.
Cobalt nickel oxide manganses of the present invention is the cobalt that has replaced a part of costliness with more cheap nickel and manganese, greatly reduces the cost of material of product, and the lithium ion battery security of cobalt nickel oxide manganses during as the positive electrode of battery will obviously be better than cobalt acid lithium.
Compatibility according to nickel, cobalt, manganese three salting liquid mixes nickel, cobalt, manganese, and can form superstructure, occupies lattice position mutually, guarantees the electrochemical properties that it is excellent.Three's freely spreading in liquid also guaranteed the uniformity of mixing simultaneously, with precipitation reagent the three precipitated fully then, obtains the predecessor of ternary material, and then obtains final products with lithium source mixed calcining.
The ratio of nickel, cobalt, manganese is very big to the influence of its electrochemical properties, when three's molecular proportion at 1: 1: 1, just can form superstructure, obtain the anode material for lithium-ion batteries of electrochemical properties the best.
The raising meeting of cell positive material tap density obviously increases the volume of battery specific energy, and improves the specific area that tap density generally need reduce material, reduces the capacity performance of material.Because sphere material can improve tap density under bigger surface area, and its good fluidity, can reduce the internal resistance of battery, improves the performance of battery to a great extent.Therefore, the material of synthesizing spherical just becomes the key issue of present lithium ion battery performance improvement.Control suitable deposition condition and obtain the predecessor of spherical ternary material, the shape that guarantees its final material is remained sphere.
Mixed calcining heat of predecessor and lithium source and the time electrochemical properties to material also has great influence.Too high and low excessively temperature can reduce the specific capacity and the cycle life of material greatly, and if the inhomogeneous batch unsteadiness that also can cause performance of temperature, be difficult to guarantee the product quality of large-scale production.Guarantee the uniformity of temperature, also guaranteed the batch stable of product.
Mixing and lithium fully being embedded of lithium source and cobalt nickel oxide manganses guarantees the stability of lithium content in the product, and cobalt nickel oxide manganses is mixed with lithium salts.Then the sintering electric furnace is raised to fixed temperature, mixed material carries out dynamic sinter in the constant temperature cavity, and sieving after the discharging obtains final products.
Owing to adopt technique scheme, make the technology of the present invention compared with the prior art have following advantage and effect:
(a) the spherical cobalt nickel oxide manganses lithium tap density height that obtains of the present invention, the narrower building-up process of granulometric range does not need to feed Buchholz protection, reduces production costs.
(b) adopt strong oxidizer and spherical nickelous carbonate cobalt manganese, can obtain spherical cobalt nickel oxide manganses, can not destroy spheric granules, also reduced the impurity content of cobalt nickel oxide manganses simultaneously, reduced the three wastes disposal cost in the production process, guaranteed that also environment is not contaminated;
(c) preparation method's process automation degree height, technological parameter control is strict, guarantees the quality of product.
Embodiment:
Embodiment is raw materials used to be commercially available technical grade product
Embodiment 1
With deionized water respectively with 2 liters of the nickel of cobalt chloride 80.90g, the manganese sulfate 75.80g of technical grade, nickelous sulfate 95.43g preparation 0.5M, cobalt and the manganese aqueous solution, the sodium carbonate of technical grade is mixed with 5 liters of the aqueous solution of 0.5M, in reactor, add 1 liter of deionized water earlier and be stirred and heated to 30 ℃, 2 liters of the aqueous solution that add nickel, cobalt and manganese then with the 2ml/min flow velocity, and the pH value of aqueous solution conditioned reaction system that is mixed with 0.5M with sodium carbonate is 7.5 ± 0.1, stirred again 0.5 hour, and generated nickelous carbonate cobalt manganese precipitation; Centrifugation nickelous carbonate cobalt manganese precipitation 156.07g uses 156.07ml deionized water wash 3 times then, up to washing lotion pH value＜7, filters the back filter cake and dries 10 hours under 60 ℃ of temperature, obtains the highly purified nickelous carbonate cobalt of spherical high-tap density manganese; 4 liters of the technical grade hydrogenperoxide steam generators of adding 1% in another reactor, be stirred and heated to 60 ℃, add the highly purified nickelous carbonate cobalt of spherical high-tap density manganese 100g, stirred after 2 hours still aging 1 hour, nickelous carbonate cobalt manganese becomes black, centrifugation precipitates then, precipitate 3 times with the 100ml deionized water wash again, filter cake was dried 10 hours under 60 ℃ of temperature, after obtaining the highly purified cobalt nickel oxide manganses 71.17g of spherical high-tap density and lithium carbonate 46.43g mixing, 1000 ℃ temperature calcinings 8 hours, obtain the highly purified oxidized Ni Mn Co and Li of spherical high-tap density.The cobalt nickel oxide manganses lithium that obtains, purity are 99.9%, 25 microns of particle mean sizes, tap density 2.75g/cm
3
Embodiment 2
With deionized water respectively with 2 liters of the nickel of cobaltous sulfate 224.74g, the manganese sulfate 178.35g of technical grade, nickelous sulfate 224.55g preparation 1.2M, cobalt and the manganese aqueous solution, the saleratus of technical grade is mixed with 6 liters of the aqueous solution of 1.2M, in reactor, add 1 liter of deionized water earlier and be stirred and heated to 55 ℃, 2 liters of the aqueous solution that add nickel, cobalt and manganese then with the 5ml/min flow velocity, and the pH value of aqueous solution conditioned reaction system that is mixed with 1.2M with sodium carbonate is 8.0 ± 0.1, stirred again 1.0 hours, and generated nickelous carbonate cobalt manganese precipitation; Centrifugation nickelous carbonate cobalt manganese precipitation 365.0g uses 1095ml deionized water wash 2 times then, up to washing lotion pH value＜7, filters the back filter cake and dries 8 hours under 80 ℃ of temperature, obtains the highly purified nickelous carbonate cobalt of spherical high-tap density manganese; 2 liters of the technical grade hydrogenperoxide steam generators of adding 5% in another reactor, be stirred and heated to 75 ℃, after adding the highly purified nickelous carbonate cobalt of spherical high-tap density manganese 200g and lithium nitrate 133.45g mixing, 800 ℃ temperature calcinings 20 hours, obtain the highly purified oxidized Ni Mn Co and Li of spherical high-tap density, purity is 99.93%, 20 microns of particle mean sizes, tap density 2.50g/cm
3
Embodiment 3
With deionized water respectively with 2 liters of the nickel of cobalt nitrate 389.85g, the manganese sulfate 298.74g of technical grade, nickelous sulfate 376.12g preparation 2.0M, cobalt and the manganese aqueous solution, the carbonic hydroammonium of technical grade is mixed with 9 liters of the aqueous solution of 2.0M, in reactor, add 1 liter of deionized water earlier and be stirred and heated to 90 ℃, 2 liters of the aqueous solution that add nickel, cobalt and manganese then with the 3.5ml/min flow velocity, and the pH value of aqueous solution conditioned reaction system that is mixed with 2.0M with carbonic hydroammonium is 8.5 ± 0.1, stirred again 1.0 hours, and generated nickelous carbonate cobalt manganese precipitation; Centrifugation nickelous carbonate cobalt manganese precipitation 605.20g uses 3026ml deionized water wash 1 time then, up to washing lotion pH value＜7, filters the back filter cake and dries 6 hours under 120 ℃ of temperature, obtains the highly purified nickelous carbonate cobalt of spherical high-tap density manganese; 0.4 liter of the technical grade hydrogenperoxide steam generator of adding 10% in another reactor, be stirred and heated to 90 ℃, add the highly purified nickelous carbonate cobalt of spherical high-tap density manganese 100g, stirred after 2 hours still aging 1 hour, nickelous carbonate cobalt manganese becomes black, centrifugation precipitates then, precipitate 1 time with the 500ml deionized water wash again, filter cake was dried 6 hours under 120 ℃ of temperature, after obtaining the highly purified cobalt nickel oxide manganses 71.98g of spherical high-tap density and lithium hydroxide 38.96g mixing, 1100 ℃ temperature calcinings 3 hours, obtain the highly purified oxidized Ni Mn Co and Li of spherical high-tap density, purity is 99.95%, 5 microns of particle mean sizes, tap density 2.62g/cm
3
Claims (2)
1. the preparation method of an anode material for lithium-ion batteries, this positive electrode is spherical high-tap density high-purity mangesium oxide nickel manganese cobalt lithium, molecular formula is Li (NiCoMn)
1/3O
2, purity is 99.9～99.95%, particle is the spherical secondary crystallization body that little crystal grain is formed, 5～25 microns of average diameters, tap density 〉=2.5g/cm
3, it is characterized in that it is undertaken by following step:
(a) at first with nickeliferous, cobalt and the manganese aqueous solution of deionized water with the chlorate of nickel, cobalt and the manganese of technical grade, sulfate or nitrate preparation 0.5～2.0M, wherein nickel, cobalt and manganese consumption atomic ratio are 1: 1: 1, with alkali metal or the bicarbonate of ammonium radical ion or the aqueous solution that carbonate be mixed with 0.5～2.0M of deionized water with technical grade, two kinds of aqueous solution volume ratios are 1: 2.5～4 again;
(b) deionized water more than 1/2 of the aqueous solution volume of the chlorate of nickel, cobalt and the manganese of elder generation's adding (a) item, sulfate or nitrate preparation is stirred and heated to 30～90 ℃ in reactor, then with 2～5ml/min flow velocity add that (a) is nickeliferous, in the aqueous solution of chlorate, sulfate or the nitrate of cobalt and manganese, and the pH value of the aqueous solution conditioned reaction system that is mixed with 0.5～2.0M with the bicarbonate or the carbonate of alkali metal or ammonium radical ion is 7.5～9.0 ± 0.1, stirred again 0.5～1 hour, and generated nickelous carbonate cobalt manganese precipitation;
(c) the nickelous carbonate cobalt manganese precipitation in centrifugation then (b) item, and with 1～5 times of deionized water wash 1～3 time of precipitation weight, up to washing lotion pH value＜7, filter the back filter cake and under 60～120 ℃ of temperature, dried 6～10 hours, obtain sphere and have the nickelous carbonate cobalt manganese that certain tap density has certain purity;
(d) in another reactor, add 1～10% technical grade hydrogenperoxide steam generator, stir, be heated to 60～90 ℃, the sphere that adds in (c) item has the nickelous carbonate cobalt manganese that certain tap density has certain purity, its nickelous carbonate cobalt manganese and hydrogen peroxide consumption are by weight/volume 1: 4～40, weight is gram (g), volume is a milliliter (ml), stirred after 2 hours still aging 1 hour, nickelous carbonate cobalt manganese becomes black, centrifugation precipitates then, precipitate 1～3 time with the deionized water wash that adds 1～5 times of nickelous carbonate cobalt manganese weight again, filter cake was dried 6～10 hours under 60～120 ℃ of temperature, obtained sphere and had the cobalt nickel oxide manganses that certain tap density has certain purity;
(e) at last with (d) cobalt nickel oxide manganses and lithium source and by cobalt nickel oxide manganses with after the mol ratio 0.95～1.3: 1 of lithium is mixed, calcined 3～20 hours 800～1100 ℃ temperature, obtain spherical tap density 〉=2.5g/cm
3, the oxidized Ni Mn Co and Li of purity 99.9～99.95%.
2. the preparation method of positive electrode according to claim 1 is characterized in that described lithium source is lithium carbonate, lithium nitrate, lithium oxalate or lithium hydroxide.
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Cited By (1)
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| CN101229928B (en) * | 2007-01-25 | 2010-04-07 | 湖南科力远新能源股份有限公司 | Method for preparing spherical nickel-cobalt lithium manganate material |
| CN101355159B (en) * | 2008-09-17 | 2010-06-16 | 金瑞新材料科技股份有限公司 | Method for preparing lithium ion battery anode material nickle cobalt lithium manganate |
| CN101800308A (en) * | 2010-04-01 | 2010-08-11 | 无锡万达金属粉末有限公司 | Method for preparing fine grain polymerization multiaperture spherical lithium nickel cobalt manganese oxide |
| CN102956878B (en) * | 2012-11-22 | 2017-08-08 | 中国电子科技集团公司第十八研究所 | Spherical lamellar cathode material for lithium nickel manganese cobalt oxide lithium ion battery |
| CN106784784B (en) * | 2015-11-20 | 2019-12-06 | 中国科学院宁波材料技术与工程研究所 | nickel-cobalt-manganese precursor and preparation method thereof |
| CN107706364B (en) * | 2017-08-25 | 2020-10-13 | 宁波富理电池材料科技有限公司 | Positive electrode material precursor, preparation method thereof and positive electrode material |
| CN108011097A (en) * | 2017-11-28 | 2018-05-08 | 中国科学院大学 | A kind of preparation method for the anode material for lithium-ion batteries for improving chemical property |
| CN114646769B (en) * | 2022-03-18 | 2023-05-12 | 广东凯金新能源科技股份有限公司 | Automatic detection system for graphite compaction detection and application method thereof |
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| CN102790208B (en) * | 2012-08-17 | 2015-02-04 | 深圳市新昊青科技有限公司 | Preparation method of ternary precursor and ternary precursor |
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