CN102983326B - Spherical lithium-nickel-cobalt composite oxide positive electrode material preparation method - Google Patents
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Abstract
The present invention belongs to the field of lithium ion battery positive electrode material preparation, and provides a spherical lithium-nickel-cobalt composite oxide positive electrode material preparation method, which comprises: carrying out wet material grinding on lithium, nickel, cobalt and doped elements, then carrying out spray drying to obtain a well-sphericized precursor, and sintering under an oxygen atmosphere to obtain the spherical lithium-nickel-cobalt composite oxide positive electrode material, wherein the chemical composition of the positive electrode material meets a general formula LixNi1-y-zCoyMzO2, M is at least one selected from Al, Mg and Mn, x is more than or equal to 1.0 and is less than or equal to 1.1, y is more than or equal to 0.1 and is less than or equal to 0.4, and z is more than or equal to 0 and is less than or equal to 0.3. With the method, corrosion on equipment by ammonia gas and environmental pollution are reduced, material circulation stability is improved through metal element doping, and practical applications of the material are improved.
Description
Technical field
The present invention relates to field of lithium ion secondary, be specifically related to a kind of preparation method of anode material for lithium-ion batteries, be to provide a kind of preparation method of spherical elements doped lithium nickel/cobalt composite oxide positive electrode in particular.
Background technology
Lithium ion battery from 1991 by LiCoO
2since doing the secondary cell commercialization of positive electrode, because of its have that output voltage is high, the advantage such as energy density is large, have extended cycle life, memory-less effect, be widely used in fields such as mobile communication, notebook computer, portable power tool, electric automobile, Aero-Space.
Novel anode material is one of key technology of restriction lithium rechargeable battery fast development, is the bottleneck of current lithium ion battery development, which determine the performance of lithium ion battery, price, application etc.The positive electrode being commonly used for lithium ion battery at present has the LiMn of spinel structure
2o
4, layer structure LiMnO
2, layer structure LiCoO
2, LiNiO
2with the LiFePO of olivine
4.Cobalt acid lithium is commercial lithium-ion batteries positive electrode conventional at present, and preparation technology is very ripe, but the shortcomings such as its natural resources shortage, price are high, poor stability limit the use in electrokinetic cell field and energy storage field.Lithium nickelate is identical with cobalt acid lithium structure, theoretical capacity height actual capacity reaches 190 ~ 210mAh/g, but lithium nickelate difficulty, the thermostable type of synthetic chemistry metering ratio are poor, lithium nickelate is when the discharge and recharge degree of depth reaches certain degree simultaneously, interlamellar spacing can tighten suddenly, structural breakdown, causes chemical property to be deteriorated rapidly, not overcharging resisting.Therefore want the performance improving lithium nickelate must carry out ion doping to lithium nickelate structure, the doping of lithium nickelate mainly contains the doping of the doping of metal ion Co, Mn, Ti, Mg, Al etc. and anion mainly F element.Due to LiNiO
2with LiCoO
2the structure had, is easy to form solid solution, so add part metals ion Co can stablize LiNiO in lithium nickelate
2structure, although capacity declines to some extent, obviously can improve polarization and the high rate performance of lithium nickelate material.And the doping of metal ions M n, Mg and Al can stabilizing material structure, improve heat endurance and the cyclical stability of material.
The method of current synthesis lithium nickel cobalt oxides as cathode materials mainly contains solid phase method, co-precipitation is sent out, sol-gel process.When preparing now lithium ion secondary battery anode material binary material (lithium nickel cobalt dioxide) and ternary material (nickle cobalt lithium manganate), general employing coprecipitation, namely first presoma is prepared by coprecipitation, then by this sediment and the evenly rear high-temperature calcination of lithium salts ground and mixed.But coprecipitation is in preparation process, control effect many factors, productive rate is not high, easily forms flocculent deposit and be difficult to filter during ion precipitation, and more difficult formation spheric granules precipitation affects tap density, and ammonia precipitation exists the drawbacks such as environmental pollution simultaneously.Such as, publication number is that the invention of CN1232438A proposes method lithium nickel cobalt aluminum composite oxide having been prepared by nickel, cobalt, aluminium salt coprecipitation, but due to Al when this nickel, cobalt, aluminium three kinds of elements carry out co-precipitation
3+introducing, easy formation flocculent deposit, spherical nickel cobalt aluminium hydroxide or the carbonate precursor of high-tap density cannot be formed, make to wash drying and wait production procedure to add difficulty, finally sinter the nickel cobalt-aluminum composite metal oxide material tap density prepared not high simultaneously.Preparation process is affected because Al easily forms flocculent deposit in alkaline environment, Toda Kogyo Corp. of Japan proposes application of nickel, cobalt element first co-precipitation in alkaline environment in the invention of CN101595581A, Al carries out the secondary coprecipitation method precipitated again, improve tap density, but add production complexity simultaneously, and there is the shortcomings such as ammonia contaminated environment, etching apparatus, increase the requirement to consersion unit, improve the difficulty that co-precipitation is produced.
Summary of the invention
In industry preparation, there is coprecipitation technology complexity for prior art lithium ion anode material lithium/nickel/cobalt composite oxide, ammonia pollutes, sphericity is difficult to the problems such as control, the invention provides a kind of industrial production process of spherical elements doped lithium nickel/cobalt composite oxide positive electrode of free of contamination high discharge capacity.
For realizing object of the present invention, inventor provides following technical scheme:
A preparation method for spherical lithium-nickel-cobalcomposite composite oxide positive electrode material, comprises the steps:
(1) element Li:Ni:Co:M=x:(1-y-z is pressed in lithium source, nickel source, cobalt source, doped chemical M source): the mol ratio batch mixing of y:z, ball milling mixed processing is carried out after adding mill Jie solvent, the slurry obtained carries out mist projection granulating and obtains lithium nickel cobalt precursor powder
(2) the lithium nickel cobalt precursor powder obtained in step (1) (directly or after being pressed into block) is placed in calcining furnace to sinter, wherein: sintering atmosphere is oxygen atmosphere, sintering temperature controls at 700-900 DEG C, and insulation 5-30 hour, finally carries out crushing and classification and obtain chemical composition and meet general formula Li
xni
1-y-zco
ym
zo
2spherical lithium-nickel-cobalcomposite composite oxide positive electrode material, in formula: M is selected from least one in Al, Mg and Mn element, 1.0≤x≤1.1,0.1≤y≤0.4,0≤z≤0.3.
The present invention relates to a kind of preparation method of free of contamination spherical lithium nickel cobalt composite oxide, in the preparation of lithium nickel cobalt metal oxide, lithium, nickel, cobalt, doped chemical are carried out wet method abrasive material, ensure that the Homogeneous phase mixing of each element, then spray-driedly the good presoma of spheroidization is obtained, again under oxygen atmosphere sintering, obtain the high power capacity spherical lithium nickel cobalt composite oxide lithium ion cell positive material of metal ion mixing.Preparation method of the present invention avoids the complicated technology of co-precipitation, reduces SO4
2-the impact of foreign ion, avoids the environmental pollution using ammoniacal liquor to bring, also ensure that high-tap density simultaneously.The present invention adopts nickel, cobalt element to be formula system that is main, metallic element M doping, improves the cycle life of oxide while ensure that high charge-discharge capacity.The present invention adopts element doping, provides structural framing can to the crystal structure of lithium nickel cobalt oxides, effectively improves the structural collapse of material in charge and discharge process and cross charge and discharge performance.The present invention adopts oxidizing atmosphere, particularly the atmosphere of high oxygen concentration, can effectively by Ni
2+be oxidized to Ni
3+.The reason that sintering temperature controls between 700-900 DEG C is: sintering temperature is lower than 700 DEG C, react insufficient; When sintering temperature is higher than 900 DEG C, Ni
3+easily be reduced to Ni
2+, enter Li
+position, worsens material electrochemical performance.
As preferably, according to the preparation method of a kind of spherical lithium-nickel-cobalcomposite composite oxide positive electrode material of the present invention, wherein: in described step (1): the mol ratio of nickel, cobalt and doped chemical M is Ni:Co:M=(0.5-0.9): (0.1-0.4): (0-0.3).The present invention adopts nickel element to be main, and cobalt is molten altogether, and the formula system of M doping, both ensure that the high capacity characteristics of material, and also improved the cycle performance of material.
As preferably, according to the preparation method of a kind of spherical lithium-nickel-cobalcomposite composite oxide positive electrode material of the present invention, wherein: in described step (1): nickel source is its nitrate, acetate, oxide or hydroxide.
As preferably, according to the preparation method of a kind of spherical lithium-nickel-cobalcomposite composite oxide positive electrode material of the present invention, wherein: in described step (1): cobalt source is its nitrate, acetate, oxide or hydroxide.
As preferably, according to the preparation method of a kind of spherical lithium-nickel-cobalcomposite composite oxide positive electrode material of the present invention, wherein: in described step (1): doped chemical M source is its nitrate, acetate, oxide or hydroxide.
As preferably, according to the preparation method of a kind of spherical lithium-nickel-cobalcomposite composite oxide positive electrode material of the present invention, wherein: in described step (1): mill Jie solvent is pure water, ethanol or acetone.
As preferably, according to the preparation method of a kind of spherical lithium-nickel-cobalcomposite composite oxide positive electrode material of the present invention, wherein: in described step (1): the mol ratio of lithium and Ni-Co-M presses LiOH:(Ni+Co+M)=(1.0-1.1): 1.The present invention adopts the excessive formula of lithium salts, effectively can make up the volatilization disappearance of lithium salts in sintering process.
As preferably, in described step (1): the size distribution D50 of the lithium nickel cobalt precursor powder that mist projection granulating obtains is 1-20 μm.When D50≤1 μm, material packed density is low; When D50 >=20 μm, material compacted density and processing characteristics undesirable.
Compared with prior art, the present invention has following advantage:
(1) pollution-free, non-corrosive raw material, avoids anticorrosion to erosion equipment of ammoniacal liquor, greatly reduces equipment requirement and reduce environmental pollution;
(2) utilize spraying dry to prepare spheric granules, improve the tap density of material;
(3) utilize metal ion mixing, improve the chemical property of lithium nickel cobalt dioxide, ensure that the high power capacity of material and high cycle life.
Accompanying drawing explanation
Fig. 1 is the X-ray diffractogram of the lithium/nickel/cobalt composite oxide positive electrode powder obtained in embodiment 1.
Fig. 2 is the charging and discharging curve figure of the lithium/nickel/cobalt composite oxide positive electrode powder obtained in embodiment 1.
Fig. 3 is the scanning electron microscope (SEM) photograph of the lithium/nickel/cobalt composite oxide positive electrode powder obtained in embodiment 3.
Detailed description of the invention
Below in conjunction with embodiment and accompanying drawing, further illustrate content of the present invention.Should be appreciated that enforcement of the present invention is not limited to the following examples, any pro forma accommodation make the present invention and/or change all will fall into scope.
In the present invention, if not refer in particular to, all parts, percentage are unit of weight, and all equipment and raw material etc. all can be buied from market or the industry is conventional.Method in following embodiment, if no special instructions, is the conventional method of this area.
embodiment 1:
By nickel nitrate, cobalt nitrate, aluminum nitrate and lithium carbonate in molar ratio Ni:Co:Al:Li=0.8:0.15:0.05:1.05 carry out weighing, add after mixing and stir in sand milling bucket, add pure water, solid content is made to control after 30%, carry out stirring sand milling 4h, open spray-drying installation, precursor pulp is beaten to centrifugal atomizer by peristaltic pump, controls atomizer rotating speed and start spraying dry, and collect the presoma powder obtained.
Above-mentioned presoma powder is placed in calcining furnace heat, under pure oxygen atmosphere, heating rate is 3 DEG C/min, and temperature controls at 750 DEG C, is incubated 15 hours, and after reaction, rate of temperature fall is at 5 DEG C/min, and obtaining chemical composition after pulverizing is Li
1.05ni
0.8co
0.15al
0.05o
2finished product aluminum-doped nickel lithium carbonate for lithium.As shown in Figure 1, as can be seen from Figure 1 sinter is α-NaFeO to its X-ray diffractogram
2layer structure, does not have dephasign.
Button cell CR2016 is used to carry out charge-discharge performance test to it.Sample thief respectively, positive plate is mixed and made into according to the ratio (mass percent) of 80:10:10 with acetylene black and bonding agent PVDF, negative pole is made by metal lithium sheet, electrolyte is for being dissolved in the LiPF6 of the 1.0mol/L in ethyl carbonate+diethyl carbonate (volume ratio 1:1) mixed solvent, barrier film is polypropylene microporous film, is assembled into button cell CR2016.Blue electricity (Wuhan) button cell test macro carries out electrochemical property test.At current density 0.1C, discharge and recharge blanking voltage carries out charge-discharge test under being respectively 4.2V and 3.0V, and charging and discharging curve as shown in Figure 2.
embodiment 2:
By nickel nitrate, cobalt nitrate, manganese nitrate and lithium carbonate in molar ratio Ni:Co:Mn:Li=0.8:0.1:0.1:1.05 carry out weighing, add after mixing and stir in sand milling bucket, add pure water, solid content is made to control after 30%, carry out stirring sand milling 4h, open spray-drying installation, precursor pulp is beaten to centrifugal atomizer by peristaltic pump, controls atomizer rotating speed and start spraying dry, and collect the presoma powder obtained.
Above-mentioned presoma powder is placed in calcining furnace heat, under pure oxygen atmosphere, heating rate is 3 DEG C/min, and temperature controls at 750 DEG C, is incubated 15 hours, and after reaction, rate of temperature fall is at 5 DEG C/min, and obtaining chemical composition after pulverizing is Li
1.05ni
0.8co
0.1mn
0.1o
2finished product mix manganese nickel cobalt acid lithium.Through particle size distribution test, material D10 is 4.06 μm, and D50 is 14.47 μm, and D90 is 24.72 μm.
embodiment 3:
By nickel nitrate, cobalt nitrate, magnesium acetate and lithium carbonate in molar ratio Ni:Co:Mg:Li=0.8:0.15:0.05:1.05 carry out weighing, add after mixing and stir in sand milling bucket, add pure water, solid content is made to control after 30%, carry out stirring sand milling 4h, open spray-drying installation, precursor pulp is beaten to centrifugal atomizer by peristaltic pump, controls atomizer rotating speed and start spraying dry, and collect the presoma powder obtained.
Above-mentioned presoma powder is placed in calcining furnace heat, under pure oxygen atmosphere, heating rate is 3 DEG C/min, and temperature controls at 750 DEG C, is incubated 15 hours, and after reaction, rate of temperature fall is at 5 DEG C/min, and obtaining chemical composition after pulverizing is Li
1.05ni
0.8co
0.15mg
0.05o
2finished product mix magnesium lithium nickel cobalt dioxide.As shown in Figure 3, the second particle of material is spherical to scanning electron microscope (SEM) photograph as can be seen from Figure 3, ensure that the tap density that material is higher.
embodiment 4:
By nickel oxide, cobalt oxide, manganese oxide and lithium carbonate in molar ratio Ni:Co:Mn:Li=0.8:0.1:0.1:1.10 carry out weighing, add after mixing and stir in sand milling bucket, add pure water, solid content is made to control after 25%, carry out stirring sand milling 6h, open spray-drying installation, precursor pulp is beaten to centrifugal atomizer by peristaltic pump, controls atomizer rotating speed and start spraying dry, and collect the presoma powder obtained.
Above-mentioned presoma powder is placed in calcining furnace heat, under pure oxygen atmosphere, heating rate is 3 DEG C/min, and temperature controls at 770 DEG C, is incubated 20 hours, and after reaction, rate of temperature fall is at 5 DEG C/min, and obtaining chemical composition after pulverizing is Li
1.10ni
0.8co
0.1mn
0.1o
2finished product mix manganese nickel cobalt acid lithium.Through inspection, this initial discharge capacity mixing manganese lithium nickel cobalt oxides is 165mAh/g.
comparative example 1:
Other operations are as embodiment 1, and difference is: by nickel nitrate, cobalt nitrate and lithium carbonate in molar ratio Ni:Co:Li=0.8:0.2:1.05 carry out weighing sand milling, after spraying, sinter that to obtain chemical composition is Li
1.05ni
0.8co
0.2o
2finished product lithium nickel cobalt dioxide.
。
comparative example 2:
By nickelous sulfate, cobaltous sulfate and aluminum sulfate in molar ratio 0.80:0.15:0.05 be hybridly prepared into the aqueous solution of 2mol/L, NaOH and ammoniacal liquor being mixed with concentration is respectively the mixed aqueous solution of 4mol/ ' L and 2mol/L.Then with peristaltic pump, nickel-cobalt-aluminium mixed aqueous solution and NaOH-ammoniacal liquor mixed ammonium/alkali solutions are added dropwise in reactor, all the time stir with agitator in process, control temperature of reaction kettle 50 DEG C, reactant liquor pH=11.0-11.5, after reaction carries out 20 hours, obtain the suspension of nickel cobalt aluminium hydroxide particle, use suction filtration machine to carry out washing suction filtration to this precipitate particles, after drying, obtain nickel cobalt aluminium hydroxide particle.
By lithium salts and the mixing of above-mentioned nickel cobalt aluminium hydroxide, by LiOH:(Ni+Co+Al) mol ratio of=1.05:1 is dry after carrying out wet-mixing, by this mixture under oxygen atmosphere, carry out the sintering of 15 hours under 750 DEG C of sintering temperatures, carrying out pulverizing, to obtain chemical composition be Li
1.05ni
0.8co
0.15al
0.05o
2lithium nickel cobalt lithium aluminate powder.
| Sulfur content % | Tap density g/mL | |
| Embodiment 1 | Do not detect | 2.23 |
| Comparative example 2 | 1.8 | 2.05 |
Embodiment 1-4 is compared can be found out with comparative example 1-2, and the sulphur impurity content that the spray-on process proposed by the present invention prepares spherical lithium nickel cobalt oxide material reduces greatly; And the chemical properties such as the cyclical stability of lithium nickel cobalt dioxide material are improved by doped with metal elements of the present invention.
Above preferred embodiment, just for instruction and explanation of content of the present invention, does not form the restriction to content of the present invention.Although inventor enumerates in more detail to invention has been, but, the content that those skilled in the art discloses according to summary of the invention part and embodiment, various amendment can be made or/and it is obvious for supplementing or adopting similar mode to substitute to described specific embodiment, and technique effect of the present invention can be realized, therefore, repeat no longer one by one herein.The term occurred in the present invention, for the elaboration of technical solution of the present invention and understanding, is not construed as limiting the invention.
Claims (4)
1. a preparation method for spherical lithium-nickel-cobalcomposite composite oxide positive electrode material, is characterized in that comprising the steps:
(1) element Li:Ni:Co:M=x:(1-y-z is pressed in lithium source, nickel source, cobalt source, doped chemical M source): the mol ratio batch mixing of y:z, ball milling mixed processing is carried out after adding mill Jie solvent, the slurry obtained carries out mist projection granulating and obtains lithium nickel cobalt precursor powder, the size distribution D50 of the lithium nickel cobalt precursor powder that mist projection granulating obtains is 1-20 μm
The mol ratio of nickel, cobalt and doped chemical M is Ni:Co:M=(0.5-0.9): (0.1-0.4): (0-0.3),
Lithium is excessive formula, and mol ratio is LiOH:(Ni+Co+M)=(1.0-1.1): 1,
Mill Jie solvent is pure water, ethanol or acetone,
(2) the lithium nickel cobalt precursor powder obtained in step (1) is placed in calcining furnace to sinter, wherein: sintering atmosphere is oxygen atmosphere, and sintering temperature controls at 700-900 DEG C, insulation 5-30 hour, finally carries out crushing and classification and obtains chemical composition and meet general formula Li
xni
1-y-zco
ym
zo
2spherical lithium-nickel-cobalcomposite composite oxide positive electrode material, in formula: M is selected from least one in Al, Mg and Mn element, 1.0≤x≤1.1,0.1≤y≤0.4,0≤z≤0.3.
2. the preparation method of a kind of spherical lithium-nickel-cobalcomposite composite oxide positive electrode material according to claim 1, is characterized in that, in described step (1): nickel source is its nitrate, acetate, oxide or hydroxide.
3. the preparation method of a kind of spherical lithium-nickel-cobalcomposite composite oxide positive electrode material according to claim 1, is characterized in that, in described step (1): cobalt source is its nitrate, acetate, oxide or hydroxide.
4. the preparation method of a kind of spherical lithium-nickel-cobalcomposite composite oxide positive electrode material according to claim 1, is characterized in that, in described step (1): doped chemical M source is its nitrate, acetate, oxide or hydroxide.
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| CN104779387B (en) * | 2015-04-14 | 2018-04-24 | 哈尔滨工程大学 | Lithium ion battery LiNi1-x-yCoxAlyO2The preparation method of material |
| CN106025179A (en) * | 2016-06-30 | 2016-10-12 | 湖南桑顿新能源有限公司 | Method for preparing cathode material lithium nickel cobalt aluminate for lithium ion battery by spray drying |
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