CN109761288A - A kind of preparation method of spherical nickel cobalt manganese persursor material - Google Patents
A kind of preparation method of spherical nickel cobalt manganese persursor material Download PDFInfo
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- CN109761288A CN109761288A CN201910278197.8A CN201910278197A CN109761288A CN 109761288 A CN109761288 A CN 109761288A CN 201910278197 A CN201910278197 A CN 201910278197A CN 109761288 A CN109761288 A CN 109761288A
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Abstract
The invention discloses a kind of preparation method of spherical nickel cobalt manganese persursor material, the presoma is the hydroxide of nickel, cobalt, manganese, molecular formula NixCoyMn1‑x‑y(OH)2, wherein 1.0,0 y≤0.2 < 0.6≤x <, comprising the following steps: (1) under a shielding gas by nickel cobalt manganese mixing salt solution, lye, complexing agent, cocurrent, which is added in the reactor equipped with bottom liquid, carries out coprecipitation reaction 90-110h；(2) it is separated by solid-liquid separation when the Slurry Granularity D50 in reactor reaches 10-14 μm, and the material after separation is aged, is washed, is dehydrated, the spherical nickel cobalt manganese persursor material of drying to obtain.The persursor material tap density that preparation process of the present invention obtains is high, it is ensured that the height ratio capacity of material and excellent cycle performance.
Description
Technical field
The invention belongs to battery material field more particularly to a kind of preparation methods of nickel cobalt manganese persursor material.
Background technique
Lithium ion secondary battery becomes more and more important in people's lives, is widely used in portable power by people
Source.Increasingly pay attention in Environmental, it is more more and more urgent to industrial upgrading, the investment of new energy material is persistently added
In the case where big, the production and selling scale of power driven vehicle also will be in explosive growth.Power vehicle lithium ion secondary battery
Have a higher requirement to energy density, cycle performance, efficiency for charge-discharge and security performance etc., research and development preparation and power vehicle lithium from
The nickel cobalt manganese persursor material that sub- battery matches, has broad application prospects.
The manufacturing method of the precursor of lithium ionic cell positive material of comparative maturity is continuity method and two kinds of batch process at present
Industrialized production, wherein the product stability of continuity method production is good, and size particles are mutually filled so that tap density height can
Reach >=2.2g/cm3, and high production efficiency, obtained battery material specific capacity is high, but the size distribution of its product is wide, micro-
Powder content is more, first is that influencing the rate of recovery of presoma and positive electrode product, increases production cost production；Second is that due to micro-
The presence of powder will cause larger impact to the cycle performance of battery, so that the cycle performance decline of battery is obvious, to influence electricity
The service life in pond.And the Granularity Distribution of common step-wise process production is narrow, exists in product without micro mist, presoma and positive material
The rate of recovery is high when material production, while obtained battery material cycle performance is excellent, but its stability is poor, granular size ratio
More consistent, it is low that mutual fillibility official post obtains tap density, essentially≤2.15g/cm3, since tap density is low so as to cause electricity
The specific capacity of pond material is low, and the General reactions control time is shorter, and so as to cause low output, production efficiency is low.
Regardless of the presoma product primary particle appearance and size of continuity method or general step-wise process production is small, especially once
Grain thickness is relatively thin, at 100 μm hereinafter, its granule-morphology be essentially sheet, it is needle-shaped, spindle equidimension smaller
Grain, by the mutual straight cutting of this little particle, perhaps oblique cutting grows into secondary class ball particle due to being that straight cutting or angle-inserting type are grown,
It will will form more porous on second particle surface so that surface compact degree is low, cause tap density lower, especially
It is bigger for the tap density influence for filling the batch process product of difference before second particle.
Summary of the invention
The technical problem to be solved by the present invention is to overcome the shortcomings of to mention in background above technology and defect, one kind is provided
The preparation method of high, electrochemical performance the spherical nickel cobalt manganese persursor material of presoma tap density.It is above-mentioned to solve
Technical problem, technical solution proposed by the present invention are as follows:
A kind of preparation method of spherical nickel cobalt manganese persursor material, the presoma are the hydroxide of nickel, cobalt, manganese, molecule
Formula is NixCoyMn1-x-y(OH)2, wherein 1.0,0 y≤0.2 < 0.6≤x <, comprising the following steps:
(1) under a shielding gas by nickel cobalt manganese mixing salt solution, lye, complexing agent, cocurrent is added in the reactor equipped with bottom liquid
Carry out coprecipitation reaction 90-110h；The bottom liquid is the mixed solution of sodium hydroxide and ammonium hydroxide, and controls ammonia concn in the liquid of bottom
It is preferably 24-30g/L for 20-30g/L()；
(2) it is separated by solid-liquid separation when the Slurry Granularity D50 in reactor reaches 10-14 μm, and the material after separation is carried out
Ageing, washing, dehydration, the spherical nickel cobalt manganese persursor material of drying to obtain；
Wherein, when coprecipitation reaction, control reaction temperature is 60-70 DEG C, and pH value control is 12.0-13.0,2h in 2h before reacting
PH value control is 11.5-12.0, revolving speed 50-210r/min afterwards.It is furthermore preferred that when coprecipitation reaction, control reaction temperature is
61-63 DEG C, pH value control is 12.2-12.6 in 2h before reacting, and pH value control is 11.5-11.8, revolving speed 50-180r/ after 2h
min。
Studies have shown that pattern of the above-mentioned technological parameter to presoma primary particle, size, there is the performance of final presoma
Very big influence.Coprecipitation reaction temperature is lower, more unfavorable for the growth of primary particle size, and reaction temperature is lower than 60 DEG C
When, the size of primary particle, pattern are not able to satisfy demand of the invention；But when temperature is higher than 70 DEG C, it will lead to forerunner
Cobalt, manganese oxidation in body, cause granularity that can not grow up, while can cause persursor material that cannot uniformly be co-precipitated.Primary particle
With the increase in reaction time, gradually grow up, when reacted between be lower than 90h when, since growth time is shorter, will lead to primary particle
Pattern it is shorter, it is relatively thin, while the tap density for also resulting in persursor material is lower；When being greater than 110h between when reacted, meeting
Cause the side length of the pattern triangle of primary particle too long, blocked up, it is so dense so as to cause persursor material, it is unfavorable for material lithium
Diffusion, to influence electrical property.PH needs Discrete control during coprecipitation reaction, and first segment pH value is relatively high mainly to be controlled
The quality and quantity of core processed, if but pH be greater than and 13 will appear cotton-shaped particle, later period particle can not normal growth；If pH value is less than 12
The quantity that will lead to core is few, and core can influence tap density than more loose.When second segment pH value is lower than 11.5, it can cause primary
Particle attenuates, is thinning, while also resulting in that particle size growth is too fast, can not meet need of the invention so as to cause primary particle pattern
It asks, while tap density also can be lower；When pH value is higher than 12.0, it will lead to granule size and be unable to satisfy demand of the invention.When
When ammonia value is lower than 20 g/L, it will lead to primary particle and attenuate, is thinning, will lead to the reduction of the tap density of presoma；When ammonia value
When higher than 30 g/L, since complexing power of the ammonia to nickel is most strong, it will lead to nickel precipitating and do not complete, to influence properties of product.Turn
Speed is too fast or also will affect properties of product slowly very much, and when speed of agitator is greater than 210r/min, the energy consumption of production is higher and will lead to
The cracking of product sphere, to influence properties of product；When speed of agitator is less than 50r/min, fluid will lead in reaction kettle not
Uniformly, at the same also result in charging solution concentration it is locally excessive, influence be co-precipitated effect, in addition revolving speed is too low also results in
The tap density of product reduces, be not able to satisfy the present invention claims.In short, the process conditions of only control the application are in above-mentioned limit
In fixed, each process conditions influence each other, and can just obtain the primary particle of specific morphology, size, the presoma being had excellent performance
Material.
In above-mentioned preparation method, it is preferred that the primary particle of the presoma is triangular in shape, the triangle of the primary particle
Each side length of shape is 400-2500 μm, and with a thickness of 200-400 μm, the D50 of primary particle is 12.5-13.5 μm, and specific surface area is
1.0-3.0m2/g.It is furthermore preferred that each side length of the triangle of the primary particle is 800-2000 μm, with a thickness of 300-400 μ
m.Being maintained above range can guarantee that the tap density of presoma is high, to guarantee the specific capacity of battery material, while again can be simultaneous
Care for the cycle performance of material.The side length of primary particle is too short, too low with thickness, causes the tap density of persursor material low, shadow
Ring the specific capacity of battery；Excessive, the too long surface that will lead to persursor material is excessively fine and close, is unfavorable for the expansion of lithium in sintering process
It dissipates, it is poor so as to cause the cyclicity of material.
In above-mentioned preparation method, it is preferred that Dmin >=4.5 μm of the presoma, D10 >=8 μm, D50=10-14 μm,
D90≤17 μm, and meet (D90-D10)/D50=0.6-0.7, tap density >=2.3g/cm3, specific surface area 0.5-4m2/g。
In above-mentioned preparation method, it is preferred that the nickel cobalt manganese mixing salt solution using soluble nickel salt, soluble cobalt with
Soluble manganese salt is prepared to obtain, and controls nickel, cobalt, three metal ion species overall control of manganese in the nickel cobalt manganese mixing salt solution and exist
1.5-2.20mol/L。
In above-mentioned preparation method, it is preferred that the lye is sodium hydroxide, and concentration control is 2.0-8.0mol/L, institute
Stating complexing agent is ammonium hydroxide, and concentration control is 5-13.5mol/L.
In above-mentioned preparation method, it is preferred that during coprecipitation reaction, the content for controlling solid matter in reaction system is
600-1000g/L(is more preferably 600-800g/L).In above range first is that can guarantee primary particle pattern, raising is shaken for control
Real density, second is that production efficiency can be improved.When less than 600 g/L, the pattern of primary particle is not required triangle, vibration
Real density is low, and production efficiency is low；When higher than 1000g/L, it will lead to particle and be saturated, fine particle occur, it cannot be guaranteed that
Size distribution is met the requirements, and extension at any time, and primary particle pattern will become needle-shaped.
In above-mentioned preparation method, it is preferred that when ripening, using 5-15wt.%, temperature is 60-75 DEG C of lye to material
Slurry carries out ripening 30-60min, and control drying temperature is 80-110 DEG C when dry.
It reduces the powder content in presoma product and need to guarantee the high-tap density of product simultaneously, lithium ion can be improved
The specific capacity and cycle life of battery.The size of primary particle pattern, growth pattern determine the tap density of presoma product,
How primary particle appearance and size to be done and changes simultaneously the direction of growth of primary particle greatly second particle surface compact is made to be to mention
The key of high-tap density.By controlling the shape and pattern size of primary particle, the side length and thickness for controlling primary particle can
The plentiful degree for improving primary particle, to improve the tap density of material.In the present invention, pass through the control of precursor preparation condition
System, the presoma tap density obtained using the triangle primary particle of specific dimensions size are high, it is ensured that the Fabrication of High Specific Capacitance of material
Amount and excellent cycle performance.
The present invention carries out coprecipitation reaction by the way of the intermittent feeding of reaction time length, can compared to continuous process
The size distribution for effectively improving product, greatly reduces the powder content of product, improves while reducing production cost
The cycle performance of material；Compared to traditional batch process, production efficiency and production capacity can be effectively improved, it is the most key
Be by this technique can very effective raising presoma product tap density, reach the level of continuity method product, can be
In the case where the cycle performance for guaranteeing material, the specific capacity of material is improved.
Compared with the prior art, the advantages of the present invention are as follows:
1, the persursor material tap density that preparation process of the present invention obtains is high, it is ensured that the height ratio capacity of material is followed with excellent
Ring performance.
2, it is high to be provided simultaneously with continuous process product specific capacity for presoma product produced by the invention, high production efficiency and
The respective advantage of step-wise process product good cycle, and the technological process of production is simple, product stability is good, can effectively solve mesh
Preceding market product fails to combine the problem of capacity and circulation.
Detailed description of the invention
In order to more clearly explain the embodiment of the invention or the technical proposal in the existing technology, to embodiment or will show below
There is attached drawing needed in technical description to be briefly described, it should be apparent that, the accompanying drawings in the following description is the present invention
Some embodiments for those of ordinary skill in the art without creative efforts, can also basis
These attached drawings obtain other attached drawings.
The SEM figure that Fig. 1 is product D in embodiment 1.
Fig. 2 is the SEM figure of product E in comparative example 1.
Fig. 3 is the SEM figure of product F in comparative example 2.
Fig. 4 is the SEM figure of product G in comparative example 3.
The SEM figure that Fig. 5 is product H in comparative example 4.
Fig. 6 is the SEM figure of product I in comparative example 5.
Fig. 7 is the SEM figure of product J in embodiment 2.
Specific embodiment
To facilitate the understanding of the present invention, the present invention is made below in conjunction with Figure of description and preferred embodiment more complete
Face meticulously describes, but the protection scope of the present invention is not limited to the following specific embodiments.
Unless otherwise defined, all technical terms used hereinafter and the normally understood meaning of those skilled in the art
It is identical.Technical term used herein is intended merely to the purpose of description specific embodiment, is not intended to the limitation present invention
Protection scope.
Unless otherwise specified, various raw material, reagent, the instrument and equipment etc. used in the present invention can pass through city
Field is commercially available or can be prepared by existing method.
Embodiment 1:
A kind of spherical nickel cobalt manganese persursor material, the chemical molecular formula of nickel cobalt manganese persursor material are Ni0.8Co0.1Mn0.1
(OH)2, primary particle is triangular in shape, and primary particle side length is 1500 μm, with a thickness of 300 μm, specific surface area 2.6m2/g。
The preparation method of above-mentioned persursor material the following steps are included:
(1) soluble metallic salt nickel sulfate, cobaltous sulfate, manganese sulfate are stoichiometrically configured to mixing salt solution A, salt-mixture
Total metal ion molality is 2mol/L in solution A；By sodium hydroxide solution by certain metering than being configured to deionized water
The precipitating reagent of 2.4mol/L；Complexing agent ammonia concn is controlled in 6.5mol/L；
(2) deionized water being added in reactor, for control speed of agitator in 180r/min, unlatching is heated to 63 DEG C, then
The ammonia concn that addition ammonium hydroxide is adjusted to reactor indsole liquid is 24g/L, and sodium hydroxide solution is added and adjusts pH value to 12.35,
Nitrogen is continually fed into reactor simultaneously；
(3) mixing salt solution A, precipitating reagent and complexing agent is added simultaneously into reaction kettle and carries out intermittent coprecipitation reaction, reaction
Temperature control pH value control pH value control after 12.35,2h in 63 DEG C, initial reaction stage 2h reacts 95h in 11.50-11.80,
Reaction process indsole liquefied ammonia concentration controls always as 24g/L, and when material D50 reaches 12.1 μm, stops reaction and obtaining reactant
Slurry, solid content 960g/L；
(4) reactant slurry is subjected to ageing reaction, ageing reaction with the lye that 60-75 DEG C of mass fraction is 10wt%-15wt%
Time is 30-60min, and the material after ageing reaction uses deionized water to be washed at normal temperature, washs the pH of terminal
Value is 7.5-8.5, and the reaction mass after washing obtains the product after being dehydrated, drying screening, and number is D(SEM figure as schemed
Shown in 1).
Comparative example 1:
This comparative example compared with Example 1, the difference is that reaction temperature control is 55 DEG C in step (3), reacts 85h, and
When material D50 reaches 13.2 μm, stop reaction.Final preparation product number is that E(SEM figure is as shown in Figure 2).
Comparative example 2:
This comparative example compared with Example 1, the difference is that in initial reaction stage 2h pH value control the pH value control after 11.8,2h
System reacts 45h in 11.0-11.50, and when material D50 reaches 13.95 μm, stops reaction.Finally preparing product number is F
(SEM figure is as shown in Figure 3).
Comparative example 3:
This comparative example compared with Example 1, the difference is that ammonia concn is adjusted to 18g/L in step (2), reacts 110h,
And material D50 stops reaction when reaching 12.5 μm.Final preparation product number is that G(SEM figure is as shown in Figure 4).
Comparative example 4:
The product of comparative maturity in the market is prepared using continuity method, principal component is NCM811(with sample D), and number is H(SEM figure
As shown in Figure 5).
Comparative example 5:
Product is prepared using market step-wise process, principal component is NCM811(with sample D), and number is that I(SEM figure is as shown in Figure 6).
Embodiment 2
A kind of spherical nickel cobalt manganese persursor material, the chemical molecular formula of nickel cobalt manganese persursor material are Ni0.6Co0.2Mn0.2
(OH)2, primary particle is triangular in shape, and primary particle side length is 1200 μm, with a thickness of 260 μm, specific surface area 2.9m2/g。
The preparation method of above-mentioned persursor material the following steps are included:
(1) soluble metallic salt nickel sulfate, cobaltous sulfate, manganese sulfate are stoichiometrically configured to mixing salt solution A, salt-mixture
Total metal ion molality is 1.8mol/L in solution A；By sodium hydroxide solution by certain metering than being prepared with deionized water
At the precipitating reagent of 2.2mol/L；Complexing agent ammonia concn is controlled in 6.0mol/L；
(2) deionized water being added in reactor, for control speed of agitator in 160r/min, unlatching is heated to 61 DEG C, then
The ammonia concn that addition ammonium hydroxide is adjusted to reactor indsole liquid is 25g/L, and sodium hydroxide solution is added and adjusts pH value to 12.25,
Nitrogen is continually fed into reactor simultaneously；
(3) mixing salt solution A, precipitating reagent and complexing agent is added simultaneously into reaction kettle and carries out intermittent coprecipitation reaction, reaction
Temperature control pH value control pH value control after 12.25,2h in 61 DEG C, initial reaction stage 2h reacts 98h in 11.60-11.80,
And material D50 stops reaction and obtaining reactant slurry, solid content 860g/L when reaching 12.2 μm；
(4) reactant slurry is subjected to ageing reaction, ageing reaction with the lye that 60-75 DEG C of mass fraction is 10wt%-15wt%
Time is 30-60min, and the material after ageing reaction uses deionized water to be washed at normal temperature, washs the pH of terminal
Value is 7.5-8.5, and the reaction mass after washing obtains the product after being dehydrated, drying screening, and number is J(SEM figure as schemed
Shown in 7).
The granular size for the product being prepared in embodiment 1-2 and comparative example 1-5 and chemical property such as the following table 1 institute
Show.
Table 1: the granular size and chemical property for the product being prepared in embodiment 1-2 and comparative example 1-5
Correlated performance result testing standard is as follows in upper table:
Particle size distribution test: Malvern laser particle analyzer MS2000；Test condition are as follows: a certain amount of sample (about 0.07g) is added
Not ultrasonic in pure water (800-850mL), 2500 turns of pump speed, obscurity reaches 10-15%, test result.
BET test: Bei Shide 3H-2000A；Test condition are as follows: a certain amount of sample is weighed, is desorbed, adsorption equilibrium,
Test result.
TD test: GB/T5162-2006, the measurement of metal powder tap density are referred to.
Capacity and loop test:
GB/T2336 electrochemical property test, discharge platform capacity ratio and cycle life test method.
GB/23365 electrochemical property test, first discharge specific capacity and first charge-discharge efficiency test method.
Claims (10)
1. a kind of preparation method of spherical nickel cobalt manganese persursor material, the presoma is the hydroxide of nickel, cobalt, manganese, point
Minor is NixCoyMn1-x-y(OH)2, wherein 1.0,0 y≤0.2 < 0.6≤x <, which comprises the following steps:
(1) under a shielding gas by nickel cobalt manganese mixing salt solution, lye, complexing agent, cocurrent is added in the reactor equipped with bottom liquid
Carry out coprecipitation reaction 90-110h；The bottom liquid is the mixed solution of sodium hydroxide and ammonium hydroxide, and controls ammonia concn in the liquid of bottom
For 20-30g/L；
(2) it is separated by solid-liquid separation when the Slurry Granularity D50 in reactor reaches 10-14 μm, and the material after separation is carried out
Ageing, washing, dehydration, the spherical nickel cobalt manganese persursor material of drying to obtain；
Wherein, when coprecipitation reaction, control reaction temperature is 60-70 DEG C, and pH value control is 12.0-13.0,2h in 2h before reacting
PH value control is 11.5-12.0, revolving speed 50-210r/min afterwards.
2. preparation method according to claim 1, which is characterized in that the primary particle of the presoma is triangular in shape, institute
Each side length for stating the triangle of primary particle is 400-2500 μm, and with a thickness of 200-400 μm, the D50 of primary particle is 12.5-
13.5 μm, specific surface area 1.0-3.0m2/g。
3. preparation method according to claim 2, which is characterized in that each side length of the triangle of the primary particle is
800-2000 μm, with a thickness of 300-400 μm.
4. preparation method according to claim 1, which is characterized in that Dmin >=4.5 μm of the presoma, the μ of D10 >=8
M, D50=10-14 μm, D90≤17 μm, and meet (D90-D10)/D50=0.6-0.7, tap density >=2.3g/cm3, specific surface
Product is 0.5-4m2/g。
5. preparation method described in any one of -4 according to claim 1, which is characterized in that when coprecipitation reaction, control reaction
Temperature is 61-63 DEG C, and pH value control is 12.2-12.6 in 2h before reacting, and pH value control is 11.5-11.8, revolving speed 50- after 2h
180r/min。
6. preparation method described in any one of -4 according to claim 1, which is characterized in that the nickel cobalt manganese mixing salt solution benefit
Prepare to obtain with soluble nickel salt, soluble cobalt and soluble manganese salt, and control nickel in the nickel cobalt manganese mixing salt solution,
Cobalt, three metal ion species overall control of manganese are in 1.5-2.20mol/L.
7. preparation method described in any one of -4 according to claim 1, which is characterized in that the lye is sodium hydroxide,
Concentration control is 2.0-8.0mol/L.
8. preparation method described in any one of -4 according to claim 1, which is characterized in that the complexing agent is ammonium hydroxide, dense
Degree control is 5-13.5mol/L.
9. preparation method described in any one of -4 according to claim 1, which is characterized in that during coprecipitation reaction, control
The content of solid matter is 600-1000g/L in reaction system.
10. preparation method described in any one of -4 according to claim 1, which is characterized in that when ripening, using 5-
15wt.%, the lye that temperature is 60-75 DEG C carry out ripening 30-60min to slurry, and control drying temperature is 80- when dry
110℃。
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| CN114477311A (en) * | 2021-12-27 | 2022-05-13 | 中伟新材料股份有限公司 | Cobalt composite hydroxide, preparation method thereof, lithium ion battery positive electrode material and lithium ion battery |
| CN114751467A (en) * | 2022-04-29 | 2022-07-15 | 福安青美能源材料有限公司 | Aging method for directionally improving specific surface area of nickel-cobalt-manganese ternary precursor |
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