CN101284684A - Preparing method for nickel-cobalt-lithium manganate precursor of lithium ionic cell positive material - Google Patents

Preparing method for nickel-cobalt-lithium manganate precursor of lithium ionic cell positive material Download PDF

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CN101284684A
CN101284684A CNA2008101107566A CN200810110756A CN101284684A CN 101284684 A CN101284684 A CN 101284684A CN A2008101107566 A CNA2008101107566 A CN A2008101107566A CN 200810110756 A CN200810110756 A CN 200810110756A CN 101284684 A CN101284684 A CN 101284684A
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cobalt
nickel
salt
lithium
preparation
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李永军
武浚
刘会基
刘进才
贺建军
朱英杰
刘晓刚
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Jinchuan Group Co Ltd
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Jinchuan Group Co Ltd
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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
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
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    • Y02E60/10—Energy storage using batteries

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Abstract

A method for preparing the nickel cobalt manganese acid lithium precursor of the anode material for a lithium battery relates to a method for preparing the material for the anode of the lithium battery. The chemical composition of the precursor is (NixCoyMn1-x-y)3O4, wherein X plus Y is less than 1. The method is characterized in that in the preparation process, an alkali solution containing ammonia is added in a solution containing soluble nickel salt, cobalt salt and manganese salt for co-precipitation reaction; the sediment product is calcined to obtain the oxide of (NixCoyMn1-x-y)3O4. The nickel cobalt manganese acid lithium precursor oxide of the anode material for the lithium battery prepared by the method is more favorable for the further even mixture with the compounds containing lithium during the subsequent process; the precipitator is sodium hydroxide or a sodium carbonate solution with a certain amount of ammonia added therein, so that the features of the product and the sizes of the grains can be effectively controlled at the same time of evenly precipitating metal ions, thus satisfying the requirements for the anode material for the lithium battery. The preparation cost is low, the sizes of the grains are even and the microcosmic features are globular or similar to the globular shape.

Description

A kind of preparation method of nickel-cobalt-lithium manganate precursor of lithium ionic cell positive material
Technical field
A kind of preparation method of nickel-cobalt-lithium manganate precursor of lithium ionic cell positive material relates to a kind of lithium ion cell positive material preparation method.
Background technology
Progress along with science and technology, electronic product is in development fast, people are also more and more higher to the lithium ion battery performance requriements, the market outlook of heavy body and high-power lithium ion battery are more and more wide, electrical appliances such as 3G written notes, notebook computer, digital camera, pick up camera, mobile DVD, electric bicycle are more and more higher to the requirement of lithium ion battery, demand is also increasing, and cell container is high more, and is also high more to the battery material performance demands.Simultaneously, raw-material price is also big more to the influence of battery price, and the prices of raw and semifnished materials such as cobalt, nickel are high at present, makes the lithium ion battery cost increase, and has strengthened the pressure of battery producer, simultaneously, and LiCoO 2Overcharge insecurity and limited its application in high capacity cell.The substitute products of electrode materials of seeking heavy body, low price and high security are very important.
At present, most commercialization lithium ion battery adopts LiCoO 2As positive electrode material, LiCoO 2Over-all properties better, but the lower (148mAh.g of actual reversible capacity -1), price is more expensive, security is relatively poor.LiNiO 2Have and LiCoO 2Quite similar laminate structure, its theoretical capacity and LiCoO 2Much at one, and actual reversible capacity compares LiCoO 2Height, and cost compares LiCoO 2Low, environmental pollution is little, and shortcoming is the synthetic difficulty of material, and cycle performance is relatively poor, does not possess using value.In recent years both at home and abroad to LiNi 1-xCo xO 2Study morely, prepared the high LiNi of a series of capacity 1-xCo xO 2, discover, replace LiNiO with Co 2In part Ni, the LiNi that synthesizes 1-xCo xO 2, also have and LiCoO 2And LiNiO 2Quite similar laminate structure has LiCoO simultaneously concurrently 2And LiNiO 2Advantage, promptly electrochemistry capacitance height, cyclicity are good, and be easily synthetic, and certain price advantage is arranged.And LiMnO 2As cell positive material, have specific storage height, the low advantage of cost and cause that battery industry pays close attention to widely, but it is because shortcomings such as high temperature decay, cycle performance difference make LiMnO 2Application be restricted.Therefore, in conjunction with LiMnO 2With the characteristics of lithium nickel cobalt dioxide, the mixed type nickel-cobalt lithium manganate material causes the very big concern of battery industry, and it is important composition with manganese, and price is with respect to LiCoO 2And LiNi 1-xCo xO 2Much lower, and capacity is with respect to pure LiMnO 2Want high, can prevent pure LiMnO 2Overcharge, and because LiNi 1-xCo xO 2With the H in the electrolytic solution +Ion exchange reaction can take place, and reduces LiMnO 2High temperature decay, the charge-discharge performance of mixed type nickle cobalt lithium manganate is than single LiMnO 2, LiNi 1-xCo xO 2Good.
Summary of the invention
The objective of the invention is to propose a kind of product pattern, granular size of making is effectively controlled, satisfy the anode material for lithium ion battery requirement, be beneficial in the subsequent processes preparation method with the further mixed uniformly nickel-cobalt-lithium manganate precursor of lithium ionic cell positive material of lithium-containing compound.
The objective of the invention is to be achieved through the following technical solutions.
A kind of preparation method of nickel-cobalt-lithium manganate precursor of lithium ionic cell positive material, its presoma chemical constitution be (Ni xCo yMn 1-x-y) 3O 4, wherein x+y＜1 is characterized in that its preparation process is to add the alkali lye that contains ammoniacal liquor to carry out coprecipitation reaction in the solution that contains soluble nickel salt, cobalt salt, manganese salt, precipitated product is calcined again, and obtains oxide compound (Ni xCo yMn 1-x-y) 3O 4
The preparation method of a kind of nickel-cobalt-lithium manganate precursor of lithium ionic cell positive material of the present invention, it is characterized in that described soluble nickel salt, cobalt salt, manganese salt are from nickelous chloride, cobalt chloride, Manganous chloride tetrahydrate, single nickel salt, rose vitriol, manganous sulfate, a kind of in nickelous nitrate, Xiao Suangu, the manganous nitrate or several.
The preparation method of a kind of nickel-cobalt-lithium manganate precursor of lithium ionic cell positive material of the present invention, it is 60～120g/L (volumetric concentration) that the GOLD FROM PLATING SOLUTION that it is characterized in that described soluble nickel salt, cobalt salt, manganese salt belongs to total ion concentration, and the ratio of the metal ion of its nickel salt, cobalt salt, manganese salt is oxide compound (Ni xCo yMn 1-x-y) 3O 4Stoichiometric ratio.
The preparation method of a kind of nickel-cobalt-lithium manganate precursor of lithium ionic cell positive material of the present invention is characterized in that described sodium hydroxide/ammonia water mixture or the yellow soda ash/ammoniacal liquor mixing solutions that contains ammoniacal liquor.
The preparation method of a kind of nickel-cobalt-lithium manganate precursor of lithium ionic cell positive material of the present invention, it is characterized in that the described concentration that contains the alkali lye sodium hydroxide/ammonia water mixture of ammoniacal liquor consists of: the concentration of sodium hydroxide solution is 80～200g/L, adding 100ml concentration in every liter of sodium hydroxide solution is 150～200g/L ammonia soln, with two kinds of solution uniform mixing.
The preparation method of a kind of nickel-cobalt-lithium manganate precursor of lithium ionic cell positive material of the present invention, it is characterized in that the concentration that the described concentration that contains the alkali lye yellow soda ash/ammonia water mixture of ammoniacal liquor consists of sodium carbonate solution is 80～200g/L, adding 100ml concentration in every liter of sodium carbonate solution is 150～200g/L ammonia soln, with two kinds of solution uniform mixing.
The preparation method of a kind of nickel-cobalt-lithium manganate precursor of lithium ionic cell positive material of the present invention, it is characterized in that the ratio that contains the solution of soluble nickel salt, cobalt salt, manganese salt in the described coprecipitation reaction and contain the alkali lye of ammoniacal liquor is 1: (1.1～1.3), pH value in reaction is 7～10, temperature is 40～70 ℃, and the reaction times is 8～40h.
The preparation method of a kind of nickel-cobalt-lithium manganate precursor of lithium ionic cell positive material of the present invention is characterized in that precipitated product being carried out the incinerating sintering temperature behind the described coprecipitation reaction is 500～800 ℃, and calcination time is 2～6h.
The preparation method of a kind of nickel-cobalt-lithium manganate precursor of lithium ionic cell positive material of the present invention, adopt coprecipitation method, adopt sodium hydroxide and yellow soda ash to make precipitation agent, prepare multicomponent nickel cobalt manganese oxyhydroxide or carbonate, again the nickel-cobalt-lithium manganate precursor of lithium ionic cell positive material oxide compound is made in the calcining of oxyhydroxide or carbonate, more helped in the subsequent processes further uniform mixing with lithium-containing compound; Precipitation agent is sodium hydroxide solution or the sodium carbonate solution that is added with certain ammoniacal liquor, can product pattern, granular size is effectively controlled, and satisfies the requirement of anode material for lithium ion battery.Preparation cost is low, the Ni of preparation xCo yMn 1-x-y(OH) 2, Ni xCo yMn 1-x-yCO 3Even particle size, microscopic appearance is sphere or class sphere.Oxide compound (Ni xCo yM 1-x-y) 3O 4To Ni xCo yMn 1-x-y(OH) 2, Ni xCo yMn 1-x-yCO 3Pattern and structure have very big inheritance.
Embodiment
A kind of preparation method of nickel-cobalt-lithium manganate precursor of lithium ionic cell positive material, its presoma chemical constitution be (Ni xCo yMn 1-x-y) 3O 4, x+y＜1 wherein, its preparation process is to add the alkali lye that contains ammoniacal liquor to carry out coprecipitation reaction in the solution that contains soluble nickel salt, cobalt salt, manganese salt, precipitated product is calcined again, and obtains oxide compound (Ni xCo yMn 1-x-y) 3O 4Comprise following each step:
1) takes by weighing nickel salt, cobalt salt, manganese salt according to the stoichiometric ratio of the product of desire preparation respectively, it is mixed with mixing solutions;
2) compound concentration is that sodium hydroxide (or yellow soda ash) solution and the concentration of 50～200g/L is 150～200g/L ammonia soln respectively, with the ratio uniform mixing of two kinds of solution in 10: 1, is mixed with precipitation agent.
3) with step 1) and 2) two kinds of solution of preparation add by constant flow pump and have in the reactor of stirring, control nickel, cobalt, manganese mixed salt solution flow (steady state value in 200～800ml/h) are 7～10 by the pH value in the flow control reactor of reconciling precipitation agent.Control reaction temperature is a steady state value in 40～70 ℃.
4) behind reaction 8～40h, the pure water of usefulness certain temperature is filtration washing gained throw out repeatedly.
5) mother liquor behind the filtration washing is recycled.The filter residue of gained carries out drying treatment at a certain temperature.Obtain Ni xCo yMn 1-x-y(OH) 2Or Ni xCo yMn 1-x-yCO 3
6) the product Ni that step 5) is obtained xCo yMn 1-x-y(OH) 2Or Ni xCo yMn 1-x-yCO 3Under air atmosphere, under 500～800 ℃ temperature, calcine.Behind calcining 2～6h, stop heating, obtain (Ni after the cooling xCo yMn 1-x-y) 3O 4
Method of the present invention can prepare and has molecular formula Ni xCo yMn 1-x-y(OH) 2, Ni xCo yMn 1-x-yCO 3Or (Ni xCo yMn 1-x-y) 3O 4, x+y＜1 anode material for lithium-ion batteries starting material wherein.Described nickel salt, cobalt salt, manganese salt is from nickelous chloride, cobalt chloride, Manganous chloride tetrahydrate, single nickel salt, rose vitriol, manganous sulfate, a kind of in nickelous nitrate, Xiao Suangu, the manganous nitrate or several.
Embodiment 1
1) take by weighing nickelous chloride 1018g respectively, cobalt chloride 127g, Manganous chloride tetrahydrate 67g, being mixed with nickel cobalt manganese element mol ratio and being 8: 1: 1, concentration is the mixed aqueous solution of 80g/L.
2) compound concentration is the aqueous sodium hydroxide solution of 100g/L respectively, and concentration is the ammonia soln of 180g/L, with 10: 1 by volume uniform mixing of two kinds of solution, is mixed with precipitation agent.
3) with step 1) and 2) two kinds of solution of preparation add by constant flow pump and have in the reactor of stirring, and control nickel, cobalt, manganese mixed salt solution flow are 300ml/h, are 9.0 by the pH value in the flow control reactor of reconciling precipitation agent.Control reaction temperature is 60 ℃.
4) behind the reaction times 40h, with 80 ℃ pure water filtration washing gained throw out repeatedly.
5) filtrate after will washing after filtration recycles.The filter residue of gained is placed on the baking oven that temperature is set at 80 ℃ and carries out drying treatment.Obtain Ni 0.8Co 0.1Mn 0.1(OH) 2
Embodiment 2
1) take by weighing nickelous chloride 521g respectively, cobalt chloride 276g, Manganous chloride tetrahydrate 261g, being mixed with nickel cobalt manganese element mol ratio is 4: 2: 4, concentration is the mixing solutions of 80g/L.
2)-3) with the step 2 of embodiment 1)-3).
4) behind the reaction times 20h, with 80 ℃ pure water filtration washing gained throw out repeatedly.
5) filtrate after will washing after filtration recycles.The filter residue of gained is placed on the baking oven that temperature is set at 80 ℃ and carries out drying treatment.Obtain Ni 0.4Co 0.2Mn 0.4(OH) 2
Embodiment 3
1) take by weighing single nickel salt 589g respectively, cobalt chloride 266g, manganous sulfate 358g, being mixed with nickel cobalt manganese element mol ratio is 4: 2: 4, concentration is the mixed aqueous solution of 80g/L.
2)-5) with the step 2 of embodiment 2)-5), obtain Ni equally 0.4Co 0.2Mn 0.4(OH) 2
Embodiment 4
1) take by weighing nickelous chloride 314g respectively, cobalt chloride 314g, Manganous chloride tetrahydrate 166g, being mixed with nickel cobalt manganese element mol ratio and being 1: 1: 1, concentration is the mixed aqueous solution of 1mol/L.
2) compound concentration is the aqueous sodium carbonate of 150g/L respectively, and concentration is the ammonia soln of 180g/L, with 10: 1 by volume uniform mixing of two kinds of solution, is mixed with precipitation agent.
3) with step 1) and 2) two kinds of solution of preparation add by constant flow pump and have in the reactor of stirring, and control nickel, cobalt, manganese mixed salt solution flow are 200ml/h, are 7.4 by the pH value in the flow control reactor of reconciling precipitation agent.Control reaction temperature is 60 ℃.
4) behind the reaction times 10h, with 80 ℃ pure water filtration washing gained throw out repeatedly.
5) filtrate after will washing after filtration recycles.The filter residue of gained carries out drying treatment in temperature is set at 80 ℃ baking oven.Obtain (Ni 1/3Co 1/3Mn 1/3) CO 3
Embodiment 5
Product (Ni with embodiment 4 1/3Co 1/3Mn 1/3) CO 3Put into constant temperature oven and calcine under air atmosphere, it is 650 ℃ that the interior temperature of stove is set.Behind the calcining 2h, stop to heat temperature control, take out after naturally cooling to room temperature with stove, obtain (Ni 1/3Co 1/3Mn 1/3) 3O4.
The product of above embodiment preparation, physical and chemical index is as follows: its size-grade distribution is at 5～20 mu m ranges, and pattern is sphere or class sphere, loose specific weight 〉=0.8g/cm 3, tap density 〉=1.60g/cm 3, through the X-ray diffraction analysis, thing is the pure phase of similar tricobalt tetroxide mutually.
1) physical index:
A) laser particle size (D 50): 12.030 μ m
B) loose specific weight: 0.98g/cm 3
C) tap density: 1.62g/cm 3
D) specific surface area: 8.39m 2/ g
2) chemical index (%): chemical ingredients sees Table 1.
Table 1 element oxide chemistry composition

Claims (8)

1. the preparation method of a nickel-cobalt-lithium manganate precursor of lithium ionic cell positive material, its presoma chemical constitution be (Ni xCo yMn 1-x-y) 3O 4, wherein x+y＜1 is characterized in that its preparation process is to add the alkali lye that contains ammoniacal liquor to carry out coprecipitation reaction in the solution that contains soluble nickel salt, cobalt salt, manganese salt, precipitated product is calcined again, and obtains oxide compound (Ni xCo yMn 1-x-y) 3O 4
2. the preparation method of a kind of nickel-cobalt-lithium manganate precursor of lithium ionic cell positive material according to claim 1, it is characterized in that described soluble nickel salt, cobalt salt, manganese salt are from nickelous chloride, cobalt chloride, Manganous chloride tetrahydrate, single nickel salt, rose vitriol, manganous sulfate, a kind of in nickelous nitrate, Xiao Suangu, the manganous nitrate or several.
3. the preparation method of a kind of nickel-cobalt-lithium manganate precursor of lithium ionic cell positive material according to claim 1, it is 60～120g/L (volumetric concentration) that the GOLD FROM PLATING SOLUTION that it is characterized in that described soluble nickel salt, cobalt salt, manganese salt belongs to total ion concentration, and the ratio of the metal ion of its nickel salt, cobalt salt, manganese salt is oxide compound (Ni xCo yMn 1-x-y) 3O 4Stoichiometric ratio.
4. the preparation method of a kind of nickel-cobalt-lithium manganate precursor of lithium ionic cell positive material according to claim 1 is characterized in that the described alkali lye that contains ammoniacal liquor is sodium hydroxide/ammonia water mixture or yellow soda ash/ammonia water mixture.
5. the preparation method of a kind of nickel-cobalt-lithium manganate precursor of lithium ionic cell positive material according to claim 1, it is characterized in that the concentration that the described concentration that contains the alkali lye sodium hydroxide/ammonia water mixture of ammoniacal liquor consists of sodium hydroxide solution is 80～200g/L, adding 100ml concentration in every liter of sodium hydroxide solution is 150～200g/L ammonia soln, with two kinds of solution uniform mixing.
6. the preparation method of a kind of nickel-cobalt-lithium manganate precursor of lithium ionic cell positive material according to claim 1, it is characterized in that the concentration that the described concentration that contains the alkali lye yellow soda ash/ammonia water mixture of ammoniacal liquor consists of sodium carbonate solution is 80～200g/L, adding 100ml concentration in every liter of sodium carbonate solution is 150～200g/L ammonia soln, with two kinds of solution uniform mixing.
7. the preparation method of a kind of nickel-cobalt-lithium manganate precursor of lithium ionic cell positive material according to claim 1, it is characterized in that the ratio that contains the solution of soluble nickel salt, cobalt salt, manganese salt in the described coprecipitation reaction and contain the alkali lye of ammoniacal liquor is 1: (1.1～1.3), pH value in reaction is 7～10, temperature is 40～70 ℃, and the reaction times is 8～40h.
8. the preparation method of a kind of nickel-cobalt-lithium manganate precursor of lithium ionic cell positive material according to claim 1 is characterized in that precipitated product being carried out the incinerating sintering temperature behind the described coprecipitation reaction is 500～800 ℃, and calcination time is 2～6h.
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CN102070179A (en) * 2010-11-24 2011-05-25 安徽亚兰德新能源材料有限公司 Method for preparing spherical carbonate ternary precursor
CN102092798A (en) * 2010-12-01 2011-06-15 兰州金川新材料科技股份有限公司 Method for continuously synthesizing precursor of lithium ion battery positive material
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CN114920304A (en) * 2016-04-29 2022-08-19 株式会社Lg 化学 Composite transition metal oxide precursor, positive electrode active material, and method for producing same
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