CN106532034A - Preparation method of lithium nickel cobalt manganese oxide material - Google Patents
Preparation method of lithium nickel cobalt manganese oxide material Download PDFInfo
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- CN106532034A CN106532034A CN201510570272.XA CN201510570272A CN106532034A CN 106532034 A CN106532034 A CN 106532034A CN 201510570272 A CN201510570272 A CN 201510570272A CN 106532034 A CN106532034 A CN 106532034A
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- nickel
- cobalt
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- manganese oxide
- lithium nickel
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/50—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese
- H01M4/505—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese of mixed oxides or hydroxides containing manganese for inserting or intercalating light metals, e.g. LiMn2O4 or LiMn2OxFy
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/52—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
- H01M4/525—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron of mixed oxides or hydroxides containing iron, cobalt or nickel for inserting or intercalating light metals, e.g. LiNiO2, LiCoO2 or LiCoOxFy
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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
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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- Manufacturing & Machinery (AREA)
- Battery Electrode And Active Subsutance (AREA)
Abstract
The invention relates to a preparation method of a lithium nickel cobalt manganese oxide material. The method comprises the following steps of (1) pre-sintering of a lithium nickel cobalt manganese oxide precursor; (2) mixing; (3) treatment before sintering; (4) sintering; and (5) high-speed dispersing, screening and packaging, thereby obtaining the lithium nickel cobalt manganese oxide material. According to the preparation method, a pretreatment technology is adopted and combined with a mixture pressing and linear cutting technology before sintering, so that the loading capacity of the lithium nickel cobalt manganese oxide material during sintering is increased, the volume shrinkage after sintering is reduced, the production capacity is improved and the labor cost is reduced; and meanwhile, the alkalinity of the lithium nickel cobalt manganese oxide material is reduced, the service life of a refractory material is prolonged by more than one time and the unit cost is reduced. Due to the pre-sintering effect, the agglomerate hardness when the lithium nickel cobalt manganese oxide material is sintered is relatively low, a sintered material block is easy to crush, and can be screened and packaged only by simple dispersion to obtain ideal material particle size distribution; risk of introducing a foreign matter is avoided; and the security, the reliability and the quality level of the lithium nickel cobalt manganese oxide material are improved.
Description
Technical field
The present invention relates to anode material for lithium-ion batteries technical field, especially a kind of preparation method of nickel-cobalt lithium manganate material.
Background technology
Nickel-cobalt lithium manganate material, claims in the industry ternary material, chemical general formula LiNixMnyCozO2(x+y+z=1), as lithium ion
The positive electrode of battery, is widely used in the fields such as communication, electric tool, electric bicycle and electric automobile power battery.
For the preparation method of nickel-cobalt lithium manganate material, in current industry, the preparation method of main flow is high temperature solid-state method, as shown in figure 1,
The solid compounds such as the oxide or carbonation of lithium are selected, are mixed homogeneously with the hydroxide (ternary precursor) of nickel cobalt manganese,
Its reaction is made to generate nickel-cobalt lithium manganate material by high temperature sintering.
Foreign body in positive electrode, particularly metallic foreign body are very harmful for battery system, caused interior due to metallic foreign body
Portion's short circuit is fatal for power battery pack.Therefore, it is highly important to reduce and prevent the foreign body in positive electrode.
But due to material prepared by conventional high temperature solid-state method, as shown in figure 3, its caking is serious, hardness is high, makes last handling process ratio
It is more complicated.Need broken, roll-in, machinery to grind the even operation such as airflow milling, classification to process, numerous and diverse process increased material
The chance contacted with machinery equipment in production process, it is easy to introduce debris, foreign body, is had undesirable effect to the quality of material.By
During calcination, volume contraction substantially, had both made that the actual production capacity of preparation process is relatively low, and relative thermal loss is more, also makes system
The cost of standby process remains high.Also, as ternary precursor and lithium carbonate are alkaline matter so that during sintering reaction,
Holding and refractory material used being burnt by alkaline corrosion, it is easy to damage, refractory material service life is universal shorter.
The content of the invention
The technical problem to be solved in the present invention is to overcome existing defect, there is provided a kind of preparation method of nickel-cobalt lithium manganate material, is subtracted
Little nickel-cobalt lithium manganate material burn till after adhesion hardness, so as to simplify nickel-cobalt lithium manganate material burn till after handling process.
In order to solve above-mentioned technical problem, the invention provides following technical scheme：
A kind of preparation method of nickel-cobalt lithium manganate material of the present invention, comprises the following steps：
(1) precursor of nickel-cobalt-lithium-manganese-oxide pre-burning
By precursor of nickel-cobalt-lithium-manganese-oxide in temperature 400-500 DEG C, pre-burning 3-6 hours under the conditions of gravity-flow ventilation；
(2) mix
The precursor of nickel-cobalt-lithium-manganese-oxide of pre-burning in step (1) is mixed with mol ratio 1.04-1.06 with lithium carbonate, is obtained
Compound；
(3) burn pre-treatment
Compound in step (2) is loaded into pincers pot, vibration pincers pot is simultaneously gently pressed compound upper strata, makes compound keep tight in pincers pot
Real to fill, bulk density is more than 1.5g/cm3, then tangent line process is carried out in pincers pot；
(4) burn till
The compound that tangent line in step (3) is crossed is sintered in electrical kiln, sintering temperature is：0-500 DEG C 2 hours, 500-700
DEG C 3 hours, 700-900 DEG C 2 hours, 900-930 DEG C 1 hour, 930 DEG C 10 hours, then Temperature fall, compound shrink
Into small powder block；
(5) dispersion, screening are packed at a high speed
Compound after burning till in step (4) is positioned in homogenizer carries out decentralized processing, then sieves and nickel is obtained
Cobalt lithium manganate material.
Further, hydroxide of the precursor of nickel-cobalt-lithium-manganese-oxide for nickel cobalt manganese in step (1).
Further, it is that the compound filled in pincers pot is cut into uniform fritter that in step (3), tangent line is processed.
Further, the time that step (5) high speed blender carries out decentralized processing is 2 minutes.
Beneficial effects of the present invention：
1st, the present invention is adopted lithium nickel cobalt manganese oxide precursor leading pre-burning, then the pretreating process mixed with lithium carbonate, while
Compound is compressed before burning till the technique of tangent line for cooperation, and useful load when sintering nickel-cobalt lithium manganate material increases 10%-20%, burns
Volume shrinkage mass after knot is reduced, and production capacity improves 15%-25%, and cost of labor is reduced；Meanwhile, make nickel-cobalt lithium manganate material basicity
Reduce, the service life of refractory material is enhanced about more than once, reduce unit cost.
2nd, due to the effect of precursor of nickel-cobalt-lithium-manganese-oxide pre-burning, caking hardness when nickel-cobalt lithium manganate material burns till is relatively low for the present invention,
Material block after burning till is easily broken, it is only necessary to which simple dispersion can sieve packaging, it is possible to obtain preferable material particle size distribution,
Avoid the risk for introducing foreign body so that the overall security reliability of nickel-cobalt lithium manganate material and quality level are lifted.
3rd, compound consolidation is loaded crucible before burning till by the present invention, and carries out tangent line process in crucible, is to compound
Burn pre-treating technology to be protected.
Description of the drawings
Fig. 1 is traditional production technological process；
Fig. 2 is the production technological process of the present invention；
Fig. 3 is the schematic diagram of traditional filling pincers pot；
Fig. 4 be the present invention burn pre-treatment in filling pincers pot after tangent line schematic diagram；
Fig. 5 be the present invention burn till after-contraction into the schematic diagram of small powder block.
Specific embodiment
Embodiment cited by the present invention, is only intended to help and understands the present invention, should not be construed as the limit to the scope of the present invention
It is fixed, for those skilled in the art, without departing from the inventive concept of the premise, can also be to the present invention
Make improvements and modifications, these improve and modification is also fallen in the range of the claims in the present invention protection.
Embodiment one：
According to the nickel cobalt manganese hydroxide that component ratio is 5: 2: 3 shown in Fig. 2, is chosen, comprise the following steps that：
(1) take precursor of nickel-cobalt-lithium-manganese-oxide Ni0.5Co0.2Mn0.3(OH)2Portion, it is by which at 450 DEG C, pre- under the conditions of gravity-flow ventilation
Burn 5 hours；
(2) precursor of nickel-cobalt-lithium-manganese-oxide of pre-burning and lithium carbonate are according to mol ratio Li: (Ni+Co+Mn)=1.06, take correspondence
The lithium carbonate of weight is mixed with the precursor of nickel-cobalt-lithium-manganese-oxide of pre-burning, obtains compound；
(3) compound is loaded in crucible, is compressed in fact, loading density is more than 1.5g/cm3, then such as Fig. 4 institutes in crucible
Show mode tangent line；
(4) compound in crucible is sintered, through 0-500 DEG C 2 hours, 500-700 DEG C 3 hours, 700-900 DEG C is 2 little
When, 900-930 DEG C 1 hour, after 930 DEG C of sintering of 10 hours, Temperature fall burns till compound in rear crucible and is shrunk to small powder
Block, as shown in Figure 5.
(5) compound after burning till is stirred into 2 minutes as decentralized processing using homogenizer, then sieves and be obtained
Nickel-cobalt lithium manganate material.
Embodiment two：
According to the nickel cobalt manganese hydroxide that component ratio is 6: 2: 2 shown in Fig. 2, is chosen, comprise the following steps that：
(1) take precursor of nickel-cobalt-lithium-manganese-oxide Ni0.6Co0.2Mn0.2(OH)2Portion, it is by which at 450 DEG C, pre- under the conditions of gravity-flow ventilation
Burn 5 hours；
(2) precursor of nickel-cobalt-lithium-manganese-oxide of pre-burning and lithium carbonate are according to mol ratio Li: (Ni+Co+Mn)=1.06, take correspondence
The lithium carbonate of weight is mixed with the precursor of nickel-cobalt-lithium-manganese-oxide of pre-burning, obtains compound；
(3) compound is loaded in crucible, is compressed in fact, loading density is more than 1.5g/cm3, then such as Fig. 4 institutes in crucible
Show mode tangent line；
(4) compound in crucible is sintered, through 0-500 DEG C 2 hours, 500-700 DEG C 3 hours, 700-900 DEG C is 2 little
When, 900-930 DEG C 1 hour, after 930 DEG C of sintering of 10 hours, Temperature fall burns till compound in rear crucible and is shrunk to small powder
Block, as shown in Figure 5.
(5) compound after burning till is stirred into 2 minutes as decentralized processing using homogenizer, then sieves and be obtained
Nickel-cobalt lithium manganate material.
Claims (4)
1. a kind of preparation method of nickel-cobalt lithium manganate material, it is characterised in that comprise the following steps：
(1) precursor of nickel-cobalt-lithium-manganese-oxide pre-burning
By precursor of nickel-cobalt-lithium-manganese-oxide in temperature 400-500 DEG C, pre-burning 3-6 hours under the conditions of gravity-flow ventilation；
(2) mix
The precursor of nickel-cobalt-lithium-manganese-oxide of pre-burning in step (1) is mixed with mol ratio 1.04-1.06 with lithium carbonate, is obtained
Compound；
(3) burn pre-treatment
Compound in step (2) is loaded into pincers pot, vibration pincers pot is simultaneously gently pressed compound upper strata, makes compound keep tight in pincers pot
Real to fill, bulk density is more than 1.5g/cm3, then tangent line process is carried out in pincers pot；
(4) burn till
The compound that tangent line in step (3) is crossed is sintered in electrical kiln, sintering temperature is：0-500 DEG C 2 hours, 500-700
DEG C 3 hours, 700-900 DEG C 2 hours, 900-930 DEG C 1 hour, 930 DEG C 10 hours, then Temperature fall, compound shrink
Into small powder block；
(5) dispersion, screening are packed at a high speed
Compound after burning till in step (4) is positioned in homogenizer carries out decentralized processing, then sieves and nickel is obtained
Cobalt lithium manganate material.
2. the preparation method of nickel-cobalt lithium manganate material according to claim 1, it is characterised in that：Nickel in step (1)
Hydroxide of the cobalt manganic acid lithium presoma for nickel cobalt manganese.
3. the preparation method of nickel-cobalt lithium manganate material according to claim 1, it is characterised in that：Cut in step (3)
Line process is that the compound filled in pincers pot is cut into uniform fritter.
4. the preparation method of nickel-cobalt lithium manganate material according to claim 1, it is characterised in that：It is high in step (5)
Fast blender carry out decentralized processing time be 2 minutes.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201510570272.XA CN106532034A (en) | 2015-09-09 | 2015-09-09 | Preparation method of lithium nickel cobalt manganese oxide material |
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| CN201510570272.XA CN106532034A (en) | 2015-09-09 | 2015-09-09 | Preparation method of lithium nickel cobalt manganese oxide material |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107311242A (en) * | 2017-08-10 | 2017-11-03 | 济南大学 | A kind of lithium ion battery improved preparation method of large single crystal layered cathode material |
| CN108011144A (en) * | 2017-10-31 | 2018-05-08 | 合肥国轩高科动力能源有限公司 | Recovery treatment process of ternary cathode material of lithium ion battery |
| CN109686973A (en) * | 2018-12-12 | 2019-04-26 | 无锡晶石新型能源股份有限公司 | A kind of preparation method of the nickelic positive electrode of low-cost high-quality |
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| CN103066269A (en) * | 2012-12-25 | 2013-04-24 | 贵州省开阳安达磷化工有限公司 | Preparation method for ternary positive electrode active material and battery |
| CN103151512A (en) * | 2013-03-13 | 2013-06-12 | 山东海特电子新材料有限公司 | Wet-method preparation process of ternary positive material for lithium ion battery |
| CN103682306A (en) * | 2013-11-06 | 2014-03-26 | 杭州金马能源科技有限公司 | Preparation method of high-performance cobalt nickel lithium manganate ternary material |
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2015
- 2015-09-09 CN CN201510570272.XA patent/CN106532034A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103066269A (en) * | 2012-12-25 | 2013-04-24 | 贵州省开阳安达磷化工有限公司 | Preparation method for ternary positive electrode active material and battery |
| CN103151512A (en) * | 2013-03-13 | 2013-06-12 | 山东海特电子新材料有限公司 | Wet-method preparation process of ternary positive material for lithium ion battery |
| CN103682306A (en) * | 2013-11-06 | 2014-03-26 | 杭州金马能源科技有限公司 | Preparation method of high-performance cobalt nickel lithium manganate ternary material |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107311242A (en) * | 2017-08-10 | 2017-11-03 | 济南大学 | A kind of lithium ion battery improved preparation method of large single crystal layered cathode material |
| CN107311242B (en) * | 2017-08-10 | 2019-04-23 | 济南大学 | A kind of lithium ion battery improved preparation method of large single crystal layered cathode material |
| CN108011144A (en) * | 2017-10-31 | 2018-05-08 | 合肥国轩高科动力能源有限公司 | Recovery treatment process of ternary cathode material of lithium ion battery |
| CN108011144B (en) * | 2017-10-31 | 2019-09-13 | 合肥国轩高科动力能源有限公司 | Recovery treatment process of ternary cathode material of lithium ion battery |
| CN109686973A (en) * | 2018-12-12 | 2019-04-26 | 无锡晶石新型能源股份有限公司 | A kind of preparation method of the nickelic positive electrode of low-cost high-quality |
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