CN102280619A - Preparation method of high-tap density spherical three-component anode material precursor - Google Patents
Preparation method of high-tap density spherical three-component anode material precursor Download PDFInfo
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Abstract
The invention discloses a preparation method of a high-tap density spherical three-component anode material precursor. The preparation method comprises the following steps of putting one or more nickel salts, one or more cobalt salts, one or more manganese salts, an alkaline aqueous solution and one or more complexing agents into a reactor to synthesize a spherical or spheroidic three-component anode material precursor through controlling stably synthetic process parameters according to a control crystallization method, wherein a chemical formula of the spherical or spheroidic three-component anode material precursor is NixCoyMnz(OH)2; x represents a number which is great than or equal to 0.5 and is less than or equal to 1; y represents a number which is great than or equal to 0 and is less than or equal to 0.5; z represents a number which is great than or equal to 0 and is less than or equal to 0.5; and the sum of the numbers represented respectively by x, y and z is equal to 1, adjusting the pH value of the spherical or spheroidic three-component anode material precursor through adding alkalis, carrying out surface treatment, washing and drying to obtain a three-component anode material precursor. The preparation method improves processing performances and tap density of the three-component anode material, overcomes the defects of material capacities and stability, through control of precursor morphology and particle sizes, controls physicochemical properties of the three-component anode material, and improves material stability.
Description
Technical field
The invention belongs to the new energy materials preparing technical field, the spherical tertiary cathode material presoma of particularly high jolt ramming preparation method.
Background technology
Lithium ion battery is the new generation of green high-energy battery, advantage such as have that voltage height, energy density are big, good cycle, self discharge are little, memory-less effect, operating temperature range are wide, be widely used in portable electric appts, as mobile phone, notebook computer, digital camera, MP3, MP4 etc., also have a good application prospect in electric automobile, lithium ion battery has good its development.
Positive electrode is the important component part of lithium ion battery.At present the industrialization anode material for lithium-ion batteries be LiCoO
2, the research comparative maturity, high comprehensive performance, but cost an arm and a leg, toxicity is bigger, there is defective in security performance, especially under the condition of overcharging, the material instability, easily and electrolyte react, application is a greater impact; LiCoO in addition
2Have only half lithium can reversiblely take off embedding, actual reversible capacity is about 145mAh/g, and the limiting lithium ion cell capacity improves, and can not satisfy the demand of electrical source of power batteries such as electric vehicle power sources, therefore needs to seek the new material of high-performance and low-cost.
In cobalt acid lithium substitution material, mainly contain LiFePO
4, LiMn
2O
4And LiNiO
2Deng, LiFePO wherein
4Have superior heat-stability and cyclicity, but actual capacitance low (<140mAh/g), operating voltage low (3.4V), electron conduction be poor, high rate during charging-discharging is poor, the limit battery energy density; LiMn
2O
4Cost is low, and fail safe is good, but the especially high-risk poor performance of cycle performance, structural instability causes significant capacity attenuation; LiNiO
2Cost is low, capacity height, but preparation difficulty, and there are serious safety problem in the consistency of material property and poor reproducibility, all are difficult to satisfy the requirement that the commercialization lithium ion battery improves specific capacity and reduces cost.
At present, tertiary cathode material nickel, cobalt and manganese oxide system has that cost is low, specific capacity is high, voltage platform is high, resisted advantages such as punching performance is good, good heat stability, and receives much concern.Studies show that this positive electrode concentrated LiCoO
2, LiMn
2O
4And LiNiO
2Advantage separately Deng material.
At present, synthesis of ternary positive electrode method is mainly high temperature solid-state method, exist three kinds of elements of nickel cobalt manganese to fail full and uniform mixing, fail to give full play to each self-applying, the synthetic material groups of grains becomes that bulk density is low, specific capacity is lower than the sour lithium of cobalt, hindered the practical application of this material, the bulk density and the volume and capacity ratio that therefore improve tertiary cathode material are significant to the practicability of tertiary cathode material.
Lithium ion anode material bulk density, pattern, particle size and distribution, impurity content and tertiary cathode material presoma are closely related.Mostly the tertiary cathode material of present domestic report is to be formed by random sheet or granular solid matter, and bulk density is low, influenced by the tertiary cathode material presoma, and the physical and chemical performance that improves presoma is particularly crucial to improving the tertiary cathode material performance.Main purpose of the present invention reaches the bulk density, processing characteristics, cycle performance and the thermal stability that improve tertiary cathode material by improving tertiary cathode material presoma physical and chemical performance.
Summary of the invention
The object of the invention provides the spherical tertiary cathode material presoma of a kind of high jolt ramming preparation method, improve tertiary cathode material processing characteristics, tap density, overcome material capacity and stable defective, by control presoma pattern and particle diameter, reach the physical and chemical performance of control tertiary cathode material, improve stability of material.
In order to reach above-mentioned purpose, solution of the present invention is:
The spherical tertiary cathode material presoma of high jolt ramming preparation method, nickel salt, cobalt salt, manganese salt and alkaline aqueous solution, complexing agent are placed in the reactor, adopt the crystallization control method, stable control synthesis technologic parameter, the spherical tertiary cathode material presoma of synthesizing spherical or class, chemical formula is Ni
xCo
yMn
z(OH)
2, 0.5≤X≤1,0≤Y≤0.5,0≤Z≤0.5, X+Y+Z=1 adds adjusting PH with base and carries out surface treatment, and the washing drying makes the tertiary cathode material presoma.
Described nickel salt, manganese salt, cobalt salt are one or more of S hydrochlorate, nitrate and chlorate, and nickel salt, manganese salt, cobalt salt solution concentration are 1.0~3.0mol/L.
Described complexing agent is one or more of ammoniacal liquor, ammonium hydrogencarbonate, ammonium carbonate, citric acid and ethylenediamine tetraacetic two acid disodiums, and concentration is 2~11mol/L.
Described alkaline aqueous solution is one or more of NaOH, KOH and LiOH, and alkaline aqueous solution concentration is 3~10mol/L.
Described crystallization control method is under argon gas, nitrogen or other inert gas shieldings, carries out the continuous precipitation mode and control the sediment crystal growth in reactor.
Described synthesis technologic parameter is that nickel salt, cobalt salt, manganese salt solution, alkaline aqueous solution, ammoniacal liquor are input in the eddy current type reactor continuously with measuring pump, and nickel content is 100~400mg/L in the control mother liquor; Precipitation temperature is 40~80 ℃; The reactor mixing speed is 100~400rpm, and the coprecipitation reaction time is 48~120 hours, and the pH value is controlled between 10.0~12.5, and the reactor feed liquid is discharged naturally.
Described synthesis technologic parameter is controlled at 300~1500g/l for the course of reaction solid content.
The described adjusting PH with base that adds carries out surface treatment and goes to ageing tank for synthesizing presoma, adds liquid caustic soda adjust pH to 12~13, stirs 1~2h, carries out Separation of Solid and Liquid, with deionized water wash Separation of Solid and Liquid gained solid product to washings pH value less than till 8; Drying obtains spherical tertiary cathode material presoma, product S(sulphur) content 800~1400ppm.
Described tertiary cathode material presoma is spherical in shape, and particle size distribution is narrow, and D50 is 5~30 μ m, tap density 〉=2.20g/cm
3
The invention has the advantages that: in reactor, adopt the crystallization control technology, the tertiary cathode material presoma of synthetic high densification, sphere, narrow particle size distribution, this technology can be controlled pattern, particle size distribution, the tap density of presoma, can strictly control Co, Ni, three kinds of element ratios of Mn, and guarantee that three kinds of elements mix fully, below the product S content may command 1200ppm, improve the high-temperature behavior of battery greatly.Adopt this presoma to prepare tertiary cathode material and guaranteed that material possesses good physics and chemical property.
Adopt tertiary cathode material presoma of the present invention to prepare tertiary cathode material and have excellent stability, improve the overcharge resistance performance and the specific capacity of tertiary cathode material.The pattern of may command material of the present invention, particle diameter, and this method has simply, controlled, is fit to suitability for industrialized production.
Description of drawings
Fig. 1 is the Ni that the embodiment of the invention 1 provides
0.5Co
0.2Mn
0.3(OH)
2The X diffracting spectrum of tertiary cathode material presoma;
Fig. 2 is that the embodiment of the invention 1 provides Ni
0.5Co
0.2Mn
0.3(OH)
2The particle size distribution figure of presoma;
Fig. 3 is the Ni that the embodiment of the invention 1 provides
0.5Co
0.2Mn
0.3(OH)
2The SEM(scanning electron microscope diagram of presoma).
Embodiment
With NiSO
4, MnSO
4, CoSO
4The nickel of Ni:Mn:Co=5:3:2 ratio preparation in molar ratio manganese cobalt mixed aqueous solution, total concentration is 3.0 mol, be mixed with the sodium hydroxide solution of 10.0 mol, compound concentration is the ammonia spirit of 6.0 mol, respectively nickel cobalt-manganese salt solution, sodium hydroxide solution, ammonia spirit is input to measuring pump and fills with 6m in advance
3Carry out reactor in the reactor of volume.Under the argon shield condition, the control temperature of reaction kettle is 50 ℃, pH value 11.5, speed of agitator is 180r/min, control ammoniacal liquor flow, and nickel content is 200mg/L in the control mother liquor, the feed liquid solid content is 400g/L in the control reactor, and the reactor feed liquid is discharged naturally, continuous feed 60h, stop charging, material in the reactor is gone to ageing tank, add adjusting PH with base to 12.5, stir 1.0h, carry out Separation of Solid and Liquid, with deionized water wash Separation of Solid and Liquid gained solid product to washings pH value less than till 8; Drying obtains spherical tertiary cathode material presoma, product S content 1050ppm.Pattern is spherical in shape, and particle size distribution is narrow, and D50 is 11.5 μ m, and tap density is 2.35g/cm
3, as shown in Figure 1 to Figure 3.
With Ni (NO
3)
2, Mn (NO
3)
2, Co (NO
3)
2The nickel of Ni:Mn:Co=8:1:1 ratio preparation in molar ratio manganese cobalt mixed aqueous solution, total concentration is 2.0 mol, be mixed with the potassium hydroxide solution of 5 mol, compound concentration is the ammoniacal liquor and the 2 mol ammonium hydrogencarbonate mixed solutions of 4 mol, respectively nickel cobalt-manganese salt solution, sodium hydroxide solution, ammoniacal liquor and ammonium hydrogencarbonate mixed solution is input to measuring pump and fills with 6m in advance
3Carry out reactor in the reactor of volume.Under the nitrogen protection condition, the control temperature of reaction kettle is 55 ℃, pH value 11.0, speed of agitator is 240r/min, control ammoniacal liquor and carbonic hydroammonium mixed liquor flow, make that mother liquor content is 100mg/L in the reactor, the feed liquid solid content is 300g/L in the control reactor, and the reactor feed liquid is discharged naturally, continuous feed 50h, stop charging, material in the reactor is gone to ageing tank, add adjusting PH with base to 13.0, stir 2.0h, carry out Separation of Solid and Liquid, with deionized water wash Separation of Solid and Liquid gained solid product to washings pH value less than till 7.5; Drying obtains spherical tertiary cathode material presoma, product S content 850ppm.Pattern is spherical in shape, and particle size distribution is narrow, and D50 is 10.5 μ m, and tap density is 2.38g/cm
3
Embodiment 3
With NiCl
2, MnCl
2, CoCl
2The nickel of Ni:Mn:Co=7:2:1 ratio preparation in molar ratio manganese cobalt mixed aqueous solution, total concentration is 2.5 mol, be mixed with the sodium hydroxide solution of 4 mol, compound concentration is the ammoniacal liquor and 0.5 mol ethylenediamine tetraacetic, the two acid disodium mixed twine mixture solution of 4 mol, respectively nickel cobalt-manganese salt solution, sodium hydroxide solution, ammoniacal liquor and ethylenediamine tetraacetic two acid disodium mixed solutions is input to measuring pump and fills with 6m in advance
3Carry out reactor in the reactor of volume.Under nitrogen or other protective conditions of other inertia, the control temperature of reaction kettle is 45 ℃, pH value 10.5, speed of agitator is 150r/min, control mixed twine mixture flow, make that mother liquor content is 100mg/L in the reactor, the feed liquid solid content is 500g/L in the control reactor, and the reactor feed liquid is discharged naturally, continuous feed 80h, stop charging, material in the reactor is gone to ageing tank, add adjusting PH with base to 12.0, stir 4.0h, carry out Separation of Solid and Liquid, with deionized water wash Separation of Solid and Liquid gained solid product to washings pH value less than till 7.0; Drying obtains spherical tertiary cathode material presoma, product S content 950ppm.Pattern is spherical in shape, and particle size distribution is narrow, and D50 is 12.5 μ m, and tap density is 2.32g/cm
3
Embodiment 4
With NiSO
4,, MnCl
2, CoSO
4The nickel of Ni:Mn:Co=6:2:2 ratio preparation in molar ratio manganese cobalt mixed aqueous solution, total concentration is 2.5 mol, be mixed with the sodium hydroxide solution of 10 mol, compound concentration is the ammoniacal liquor and 0.2 mol ethylenediamine tetraacetic, the two acid disodium mixed twine mixture solution of 5.0 mol, respectively nickel cobalt-manganese salt solution, sodium hydroxide solution, ammoniacal liquor and ethylenediamine tetraacetic two acid disodium mixed solutions is input to measuring pump and fills with 6m in advance
3Carry out reactor in the reactor of volume.Under nitrogen or other protective conditions of other inertia, the control temperature of reaction kettle is 52 ℃, pH value 11.0, speed of agitator is 210r/min, control mixed twine mixture flow, make that mother liquor content is 300mg/L in the reactor, the feed liquid solid content is 600g/L in the control reactor, and the reactor feed liquid is discharged naturally, continuous feed 90h, stop charging, material in the reactor is gone to ageing tank, add adjusting PH with base to 13.0, stir 1.0h, carry out Separation of Solid and Liquid, with deionized water wash Separation of Solid and Liquid gained solid product to washings pH value less than till 7.5; Drying obtains spherical tertiary cathode material presoma, product S content 1020ppm.Pattern is spherical in shape, and particle size distribution is narrow, and D50 is 11.8 μ m, and tap density is 2.28g/cm
3
Measure D50, tap density, the product S content of tertiary cathode material presoma prepared in the foregoing description 1~4 respectively, and list in the table 1 respectively.
Table 1 is an example physical and chemical performance tables of data of the present invention
As seen from the above table, the tertiary cathode material presoma even particle size distribution that the present invention improves is improved and is optimized tertiary cathode material pattern and composition by the present invention, improves tap density, reduce product S content, be used for tertiary cathode material and can improve its physical and chemical performance and electrical property.
Claims (9)
1. the spherical tertiary cathode material presoma of high jolt ramming preparation method, it is characterized in that: nickel salt, cobalt salt, manganese salt and alkaline aqueous solution, complexing agent are placed in the reactor, adopt the crystallization control method, stable control synthesis technologic parameter, the spherical tertiary cathode material presoma of synthesizing spherical or class, chemical formula is Ni
xCo
yMn
z(OH)
2, 0.5≤X≤1,0≤Y≤0.5,0≤Z≤0.5, X+Y+Z=1 adds adjusting PH with base and carries out surface treatment, and the washing drying makes the tertiary cathode material presoma.
2. the spherical tertiary cathode material presoma of high jolt ramming as claimed in claim 1 preparation method, it is characterized in that: described nickel salt, manganese salt, cobalt salt are one or more of S hydrochlorate, nitrate and chlorate, and nickel salt, manganese salt, cobalt salt solution concentration are 1.0~3.0mol/L.
3. the spherical tertiary cathode material presoma of high jolt ramming as claimed in claim 1 preparation method, it is characterized in that: described complexing agent is one or more of ammoniacal liquor, ammonium hydrogencarbonate, ammonium carbonate, citric acid and ethylenediamine tetraacetic two acid disodiums, and concentration is 2~11mol/L.
4. the spherical tertiary cathode material presoma of high jolt ramming as claimed in claim 1 preparation method, it is characterized in that: described alkaline aqueous solution is one or more of NaOH, KOH and LiOH, alkaline aqueous solution concentration is 3~10mol/L.
5. the spherical tertiary cathode material presoma of high jolt ramming as claimed in claim 1 preparation method; it is characterized in that: described crystallization control method is carried out the continuous precipitation mode and is controlled the sediment crystal growth under argon gas, nitrogen or other inert gas shieldings in reactor.
6. the spherical tertiary cathode material presoma of high jolt ramming as claimed in claim 1 preparation method, it is characterized in that: described synthesis technologic parameter is that nickel salt, cobalt salt, manganese salt solution, alkaline aqueous solution, ammoniacal liquor are input in the eddy current type reactor continuously with measuring pump, and nickel content is 100~400mg/L in the control mother liquor; Precipitation temperature is 40~80 ℃; The reactor mixing speed is 100~400rpm, and the coprecipitation reaction time is 48~120 hours, and the pH value is controlled between 10.0~12.5, and the reactor feed liquid is discharged naturally.
7. the spherical tertiary cathode material presoma of high jolt ramming as claimed in claim 1 preparation method, it is characterized in that: described synthesis technologic parameter is controlled at 300~1500g/l for the course of reaction solid content.
8. the spherical tertiary cathode material presoma of high jolt ramming as claimed in claim 1 preparation method, it is characterized in that: the described adjusting PH with base that adds carries out surface treatment and goes to ageing tank for synthesizing presoma, add liquid caustic soda adjust pH to 12~13, stir 1~2h, carry out Separation of Solid and Liquid, with deionized water wash Separation of Solid and Liquid gained solid product to washings pH value less than till 8; Drying obtains spherical tertiary cathode material presoma, product
SContent 800~1400ppm.
9. the spherical tertiary cathode material presoma of high jolt ramming as claimed in claim 1 preparation method, it is characterized in that: described tertiary cathode material presoma is spherical in shape, and particle size distribution is narrow, and D50 is 5~30 μ m, tap density 〉=2.20g/cm
3
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