CN101269849A - High-density spherical lithium nickel cobalt manganese oxygen and method for preparing the same - Google Patents
High-density spherical lithium nickel cobalt manganese oxygen and method for preparing the same Download PDFInfo
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Abstract
The invention relates to a high density spherical shape LiNixCoyMn(1-x-y)O2 and a preparation method thereof, and belongs to the products of chemical industry, in particular to the preparation of the high density spherical shape LiNixCoyMn(1-x-y)O2 which is mainly used for manufacturing a lithium ion battery. Firstly, a high density spherical shape nickel cobalt and manganese predecessor body is synthesized by controlling the synthetic technology, secondly, the high density spherical shape nickel cobalt and manganese predecessor body is mixed with a lithium source and then is calcined under the specified conditions, so the high density spherical shape LiNixCoyMn(1-x-y)O2 can be obtained. The LiNixCoyMn(1-x-y)O2 is a spherical shape crystal, the mean grain size is 3-20 micrometers, the loose packed density is more than or equal to 1.0g/cm<3>, and the tap density is more than or equal to 2.0g/cm<3>. The synthesized LiNixCoyMn(1-x-y)O2 is of a single spherical shape, has better tap density, and can improve the volume ration capacity of the battery. The LiNixCoyMn(1-x-y)O2 is formed by calcining the predecessor body which has a spherical shape particle, high density, and complete crystalline form structure, compared with the synthetic technology of the predecessor body, the preparation method is simple, the cost is low, and the particle size can be controlled, and the industrialization is easy.
Description
Technical field
The present invention relates to a kind of lithium-nickel-manganese-cobalt-oxygen, chemical formula LiNi
xCo
yMn
1-x-yO
2, belong to the preparation of Chemicals, particularly high-density spherical lithium nickel cobalt manganese oxygen, be mainly used in the making lithium ion battery.
Background technology
Lithium ion battery is a kind of emerging power supply, and it has, and voltage height, capacity are big, safety and environmental protection etc. are many a bit, therefore are subjected to widespread use in the secondary cell field.At present the positive electrode material of lithium ion battery is used most often cobalt acid lithium, but because of cobalt is a strategy metal, and cobalt valency rising all the way in recent years causes and do battery cost with cobalt acid lithium and raise, and each big producer seeks the positive electrode material that can substitute the sour lithium of cobalt one after another.
Anode material for lithium-ion batteries is a kind of compound with stratiform, host structure, can allow lithium ion reversibly to deviate from and embed in the larger context, positive electrode material is the important component part of lithium ion battery, at present, the maximum positive electrode material that similar structures is arranged of research is lithium manganate (LiMn
2O
4), lithium nickelate (LiNiO
2) and the formed lithium nickel cobalt dioxide (LiNi that mutually mixes between them
xCo
1-xO
2), nickle cobalt lithium manganate (LiNi
xCo
yMn
1-x-yO
2) and iron lithium phosphate (LiFePO
4) etc.The lithium manganate cost is low, and security is good, but cycle performance, especially high temperature cyclic performance is poor, and certain dissolubility is arranged in electrolytic solution, and memory property is poor.The capacity of lithium nickelate is higher, cost is lower than the sour lithium of cobalt, but synthetic difficulty, the consistence and the poor safety performance that cause material, the application of influence on lithium cell, lithium nickel cobalt dioxide have the advantage of lithium nickelate and cobalt acid lithium concurrently, are being the new shape positive electrode materials that most possibly replaces cobalt acid lithium by people's approval once, but still having shortcomings such as synthesis condition is comparatively harsh, safety performance is relatively poor, over-all properties haves much room for improvement.LiFePO 4 material because of its draw materials more cheap and easy to get, at present also in people's attention.
At this moment, having the nickle cobalt lithium manganate (also being lithium-nickel-manganese-cobalt-oxygen) that above advantage can overcome various material shortcomings simultaneously again concurrently attracted attention by the people.The method of at present synthetic nickle cobalt lithium manganate mainly is divided into two kinds: a kind of is high-temperature solid phase reaction method, and it is with lithium source, nickel source, cobalt source, manganese source ground and mixed together, and calcining is synthetic under about 1000 ℃ of high temperature again.Its shortcoming is that nickel, cobalt, three kinds of elements of manganese are failed full and uniform mixing, thereby can not be distributed in fully in the crystalline structure, causes the synthetic powder body material irregular, does not have fixed shape, and tap density is low, has hindered the practical application of this material.Another kind method is a coprecipitation method, the salt that is about to manganese source, nickel source, cobalt source be mixed with mixing solutions and alkali lye together successive add in the reactor co-precipitation presoma of output nickel, cobalt, manganese to.Coprecipitation method has realized providing advantageous conditions to three kinds of atoms of elements level uniform mixing and for industrialization, and, do not change the pattern of presoma in the sintering process after adding the lithium source, do not change the granularity of presoma substantially yet, so being a kind of comparatively ideal, coprecipitation method prepares approach, but the synthetic granular precursor all is irregularly shaped at present, even say sphere, also is the particle of secondary agglomeration.
Summary of the invention
Order of the present invention is solving problems of the prior art, a kind of preparation method with high-density spherical lithium nickel cobalt manganese oxygen of good fluidity is provided, by the control synthesis technique, at first synthetic a kind of high density spherical nickel-cobalt manganese presoma, again this nickel cobalt manganese presoma with after mix in the lithium source, calcine under given conditions, obtain high-density spherical lithium nickel cobalt manganese oxygen, this method technology is simple, realizes technology easily.The lithium-nickel-manganese-cobalt-oxygen that synthesizes is single sphere, has excellent accumulation density, can improve the volume of battery specific storage.
Technical scheme of the present invention is:
A kind of high-density spherical lithium nickel cobalt manganese oxygen, this lithium-nickel-manganese-cobalt-oxygen are spheroidal crystal, 3～20 microns of median sizes, loose density 〉=1.0g/cm
3, tap density 〉=2.0g/cm
3
A kind of preparation method of high-density spherical lithium nickel cobalt manganese oxygen, undertaken by following step:
1., at first respectively the nickel salt of technical grade, cobalt salt, manganese salt to be mixed with nickel cobalt manganese melting concn in the ratio of x: y: 1-x-y and additive with deionized water be that 0.5M～10M, additive concentration are the solution of 0.05M～5M, 0＜x＜1 wherein; 0＜y＜1; 0＜1-x-y＜1.
2., with deionized water alkaline precipitating agent, the complexing agent of technical grade being made into alkaline precipitating agent concentration is that 1M～15M, complexing agent concentration are the solution of 0.05M～5M.
3., the stirring of opening reaction vessel, drop into 3 liters deionized water earlier and do end water, and end water is heated to 30 ℃～70 ℃, by 1.: 2.=1.00: 0.5～4.0, will 1., 2. two kinds of solution join in the reaction vessel simultaneously, control pH value 8～13.Precipitation overflow ageing in another container that reaction generates got final product in 4～10 hours.
The precipitation of filtering 4., then 3., and with the deionized water wash of 3～10 times of weight of filter cake 1～5 time, up to PH less than 7.5, filtration then, filter cake dried by the fire in 70～120 ℃ baking oven 4～15 hours, can dry, and obtained nickel cobalt manganese presoma.
5., get the 4. oven dry powder of item, press nickel cobalt manganese presoma with lithium salts: the molar ratio ingredient of lithium salts=1: 0.9～1.2, the mixture for preparing add deionized water and stirring evenly after, pack in the crucible, 150 ℃ of insulations 4 hours, take out grinding, 700～900 ℃ of temperature lower calcinations 4～15 hours, obtain high-density spherical lithium nickel cobalt manganese oxygen again.
Above-mentioned used nickel salt is one or more in single nickel salt, nickelous chloride, the nickelous nitrate; Cobalt salt is one or more in cobalt chloride, rose vitriol, the Xiao Suangu; Manganese salt is one or more in Manganous chloride tetrahydrate, manganous sulfate, the manganous nitrate.
Above-mentioned used additive is one or more in ammonium citrate, the ammonium oxalate.
Above-mentioned used alkaline precipitating agent is one or more in potassium hydroxide, the sodium hydroxide.
Above-mentioned used complexing agent is one or more among ammoniacal liquor, citric acid, the EDTA.
Above-mentioned used lithium salts is one or more in Quilonum Retard, the lithium hydroxide.
Lithium-nickel-manganese-cobalt-oxygen of the present invention is complete with a kind of density height, crystalline structure, particle shape forms for the calcining of spheric presoma, and is simpler than presoma synthesis technique, cost is low, particle diameter can be controlled, and industrialization easily.The present invention has following advantage:
1, adopts special depositing technology, the co-precipitation presoma for preparing a kind of nickel cobalt manganese, in the process of preparation, can effectively control the particle diameter and the size-grade distribution problem of product, make and be shaped as spheroidal particle, show as Fig. 1, make that also washing is easier, be easy to such an extent that prepare lithium-nickel-manganese-cobalt-oxygen of the present invention with this presoma.
2, lithium-nickel-manganese-cobalt-oxygen of the present invention can improve the volume of battery specific storage.It is fast that method of the present invention prepares speed, but continuous production is easy to realize industrialization.
Description of drawings
Fig. 1 is SEM figure of the present invention.
Concrete embodiment
Embodiment 1:
With deionized water rose vitriol is made into 1M, single nickel salt 0.6M, manganous sulfate 1M, ammonium citrate is made into the mixing solutions of 2M, with deionized water potassium hydroxide is made into 4M, ammoniacal liquor is made into the mixing solutions of 2M, open the stirring of reaction vessel, drop into 3 liters deionized water, and end water is heated to 40 ℃, nickel cobalt manganese solution joins in the reaction vessel with the flow velocity of 5ml/min, alkaline precipitating agent potassium hydroxide joins in the reaction vessel with the flow velocity of 5～15ml/min, by regulating the flow velocity of potassium hydroxide, the control pH value is 11.5 ± 0.3, the precipitation suspension that reaction generates overflows to ageing in another container, after the ageing 6 hours, washing of precipitate is clean, up to washing water PH less than 7.5, filter then, filter cake 90 ℃ of oven dry, take by weighing the product 90g after the oven dry, lithium hydroxide 38.8g is measured 50 ml deionized water, after mixing, put into corundum crucible, in retort furnace, establish 150 ℃ of temperature, after the oven dry, take out and grind, put into crucible again, 780 ℃ of calcinings 6 hours, obtain purity and be 〉=99.5% high-density spherical lithium nickel cobalt manganese oxygen, the lithium-nickel-manganese-cobalt-oxygen granularity that this condition makes is 10.52 μ m.
Embodiment 2:
With deionized water cobalt chloride is made into 2M, nickelous chloride is made into 0.5M, Manganous chloride tetrahydrate 0.5M, ammonium citrate is made into the mixing solutions of 1M, with deionized water potassium hydroxide is made into 4M, ammoniacal liquor is made into the mixing solutions of 2M, open the stirring of reaction vessel, drop into 3 liters deionized water, and end water is heated to 50 ℃, nickel cobalt manganese solution joins in the reaction vessel with the flow velocity of 4ml/min, alkaline precipitating agent potassium hydroxide joins in the reaction vessel with the flow velocity of 5～15ml/min, by regulating the flow velocity of potassium hydroxide, the control pH value is 10.5 ± 0.3, the precipitation suspension that reaction generates overflows to ageing in another container, after the ageing 6 hours, washing of precipitate is clean, up to washing water PH less than 7.5, filter then, filter cake 120 ℃ of oven dry, take by weighing the product 90g after the oven dry, Quilonum Retard 39.8g is measured 50 ml deionized water, after mixing, put into corundum crucible, in retort furnace, establish 150 ℃ of temperature, after the oven dry, take out and grind, put into crucible again, 800 ℃ of calcinings 10 hours, obtain purity and be 〉=99.5% high-density spherical lithium nickel cobalt manganese oxygen, the lithium-nickel-manganese-cobalt-oxygen granularity that this condition makes is 6.12 μ m.
Embodiment 3:
With deionized water cobalt chloride is made into 1M, nickelous chloride is made into 0.8M, Manganous chloride tetrahydrate 0.8M, ammonium oxalate is made into the mixing solutions of 0.5M, with deionized water sodium hydroxide is made into 7M, ammoniacal liquor is made into the mixing solutions of 1M, open the stirring of reaction vessel, drop into 3 liters deionized water, and end water is heated to 40 ℃, nickel cobalt manganese solution joins in the reaction vessel with the flow velocity of 10ml/min, alkaline precipitating agent sodium hydroxide joins in the reaction vessel with the flow velocity of 5～15ml/min, by regulating the flow velocity of sodium hydroxide, the control pH value is 10 ± 0.3, the precipitation suspension that reaction generates overflows to ageing in another container, after the ageing 6 hours, washing of precipitate is clean, up to washing water PH less than 7.5, filter then, filter cake 95 ℃ of oven dry, take by weighing the product 105g after the oven dry, Quilonum Retard 40g is measured 55 ml deionized water, after mixing, put into corundum crucible, in retort furnace, establish 150 ℃ of temperature, after the oven dry, take out and grind, put into crucible again, 850 ℃ of calcinings 8 hours, obtain purity and be 〉=99.5% high-density spherical lithium nickel cobalt manganese oxygen, the lithium-nickel-manganese-cobalt-oxygen granularity that this condition makes is 14.36 μ m.
Embodiment 4:
With deionized water Xiao Suangu is made into 0.8M, nickelous nitrate is made into 0.5M, manganous nitrate 0.5M, ammonium citrate is made into the mixing solutions of 3M, with deionized water sodium hydroxide is made into 9M, ammoniacal liquor is made into the mixing solutions of 1M, open the stirring of reaction vessel, drop into 3 liters deionized water, and end water is heated to 50 ℃, nickel cobalt manganese solution joins in the reaction vessel with the flow velocity of 5ml/min, alkaline precipitating agent sodium hydroxide joins in the reaction vessel with the flow velocity of 5～15ml/min, by regulating the flow velocity of sodium hydroxide, the control pH value is 11 ± 0.3, the precipitation suspension that reaction generates overflows to ageing in another container, after the ageing 6 hours, washing of precipitate is clean, up to washing water PH less than 7.5, filter then, filter cake 100 ℃ of oven dry, take by weighing the product 90g after the oven dry, lithium hydroxide 38g is measured 50 ml deionized water, after mixing, put into corundum crucible, in retort furnace, establish 150 ℃ of temperature, after the oven dry, take out and grind, put into crucible again, 900 ℃ of calcinings 15 hours, obtain purity and be 〉=99.5% high-density spherical lithium nickel cobalt manganese oxygen, the lithium-nickel-manganese-cobalt-oxygen granularity that this condition makes is 8.75 μ m.
Embodiment 5:
With deionized water Xiao Suangu is made into 0.5M, nickelous nitrate is made into 1M, manganous nitrate 1M, ammonium oxalate is made into the mixing solutions of 3M, with deionized water sodium hydroxide is made into 7M, ammoniacal liquor is made into the mixing solutions of 1.2M, open the stirring of reaction vessel, drop into 3 liters deionized water, and end water is heated to 45 ℃, nickel cobalt manganese solution joins in the reaction vessel with the flow velocity of 6ml/min, alkaline precipitating agent sodium hydroxide joins in the reaction vessel with the flow velocity of 5～15ml/min, by regulating the flow velocity of sodium hydroxide, the control pH value is 12.5 ± 0.3, the precipitation suspension that reaction generates overflows to ageing in another container, after the ageing 6 hours, washing of precipitate is clean, up to washing water PH less than 7.5, filter then, filter cake 100 ℃ of oven dry, take by weighing the product 95g after the oven dry, Quilonum Retard 39.3g is measured 50 ml deionized water, after mixing, put into corundum crucible, in retort furnace, establish 150 ℃ of temperature, after the oven dry, take out and grind, put into crucible again, 780 ℃ of calcinings 15 hours, obtain purity and be 〉=99.5% high-density spherical lithium nickel cobalt manganese oxygen, the lithium-nickel-manganese-cobalt-oxygen granularity that this condition makes is 9.8 μ m.
Claims (7)
1, a kind of high-density spherical lithium nickel cobalt manganese oxygen is characterized in that this lithium-nickel-manganese-cobalt-oxygen is a spheroidal crystal, 3～20 microns of median sizes, loose density 〉=1.0g/cm
3, tap density 〉=2.0g/cm
3
2, a kind of preparation method of high-density spherical lithium nickel cobalt manganese oxygen is characterized in that it is undertaken by following step:
1., at first respectively the nickel salt of technical grade, cobalt salt, manganese salt being mixed with nickel cobalt manganese melting concn in the ratio of x: y: 1-x-y and additive with deionized water is 0.5M～10M, additive concentration is the solution of 0.05M～5M, 0＜x＜1,0＜y＜1,0＜1-x-y＜1 wherein;
2., with deionized water alkaline precipitating agent, the complexing agent of technical grade being made into alkaline precipitating agent concentration is that 1M～15M, complexing agent concentration are the solution of 0.05M～5M;
3., open the stirring of reaction vessel, the deionized water that drops into 3 liters is done end water earlier, and end water is heated to 30 ℃～70 ℃, press 1.: 2.=1.00: 0.5～4.0, will be 1., 2. two kinds of solution join in the reaction vessel simultaneously, control pH value 8～13, precipitation overflow ageing in another container that reaction generates got final product in 4～10 hours;
The precipitation of filtering 4., then 3., and with the deionized water wash of 3～10 times of weight of filter cake 1～5 time, up to PH less than 7.5, filtration then, filter cake dried by the fire in 70～120 ℃ baking oven 4～15 hours, can dry, and obtained nickel cobalt manganese presoma;
5., get the 4. oven dry powder of item, press nickel cobalt manganese presoma with lithium salts: the molar ratio ingredient of lithium salts=1: 0.9～1.2, the mixture for preparing add deionized water and stirring evenly after, pack in the crucible, 150 ℃ of insulations 4 hours, take out grinding, 700～900 ℃ of temperature lower calcinations 4～15 hours, obtain high-density spherical lithium nickel cobalt manganese oxygen again.
3, the preparation method of lithium-nickel-manganese-cobalt-oxygen according to claim 2 is characterized in that used nickel salt is one or more in single nickel salt, nickelous chloride, the nickelous nitrate; Cobalt salt is one or more in cobalt chloride, rose vitriol, the Xiao Suangu; Manganese salt is one or more in Manganous chloride tetrahydrate, manganous sulfate, the manganous nitrate.
4, the preparation method of lithium-nickel-manganese-cobalt-oxygen according to claim 2 is characterized in that used additive is one or more in ammonium citrate, the ammonium oxalate.
5, the preparation method of lithium-nickel-manganese-cobalt-oxygen according to claim 2 is characterized in that used alkaline precipitating agent is one or more in potassium hydroxide, the sodium hydroxide.
6, the preparation method of lithium-nickel-manganese-cobalt-oxygen according to claim 2 is characterized in that used complexing agent is one or more among ammoniacal liquor, citric acid, the EDTA.
7, the preparation method of lithium-nickel-manganese-cobalt-oxygen according to claim 2 is characterized in that used lithium salts is one or more in Quilonum Retard, the lithium hydroxide.
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| 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 |
| CN102544506A (en) * | 2011-12-22 | 2012-07-04 | 中国矿业大学 | Method for preparing lithium battery anode material |
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