CN108493447A - Preparation method of high-quality high-nickel multi-element positive electrode material - Google Patents
Preparation method of high-quality high-nickel multi-element positive electrode material Download PDFInfo
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- CN108493447A CN108493447A CN201810203577.0A CN201810203577A CN108493447A CN 108493447 A CN108493447 A CN 108493447A CN 201810203577 A CN201810203577 A CN 201810203577A CN 108493447 A CN108493447 A CN 108493447A
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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
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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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Abstract
The invention relates to a preparation method of a high-quality high-nickel multi-element anode material, which comprises the following steps: and (2) uniformly mixing the high-nickel multi-element precursor with a lithium source, then loading the mixture into a sagger with vent holes on the side wall and the bottom and a high-temperature-resistant organic film inside, then sending the sagger into a sintering furnace, sintering at high temperature under the condition of introducing oxygen, and crushing, sieving and demagnetizing after sintering to obtain the high-quality high-nickel multi-element cathode material. The preparation method can reduce the performance difference of the upper layer material and the lower layer material after sintering, improve the overall performance of the materials, prepare high-quality products while ensuring the production efficiency, and prolong the service life of the sagger.
Description
Technical field
It is nickelic more more particularly to a kind of high-quality the present invention relates to technical field prepared by anode material for lithium-ion batteries
The preparation method of first positive electrode.
Background technology
Currently, the main preparation methods of nickelic polynary positive pole material are solid-phase sintering, it is by nickel cobalt manganese hydroxide forerunner
Body and lithium source (lithium carbonate or lithium hydroxide) uniformly mix, and are then charged into ceramic saggar, place into sintering furnace and carry out high-temperature calcination,
It is crushed, is classified, sieved after calcining, you can obtain multicomponent material.However, the method has following defect：
1, during multicomponent material calcined crystalline, stable layered crystal structure is formed, a large amount of oxygen is needed to join
With react, and need certain partial pressure of oxygen to inhibit deoxidation of material during crystalline transition, and when in saggar material it is thicker
When, oxygen be difficult by diffusing into saggar bottom, subsurface material anoxic being made to cause levels difference in material properties larger, from
And material overall performance is caused to be affected, the general solution of this problem is to reduce ulking thickness in material sintering process,
But the problem that production efficiency can be brought relatively low simultaneously；
2, in sintering process, material is in direct contact with saggar, lithium source in melting process easily by High temperature diffusion into
Enter inside saggar so that saggar material microstructure changes, phenomena such as scaling occurs, ruptures so as to cause saggar, therefore casket
Alms bowl service life is relatively low.
Invention content
Based on this, the object of the present invention is to provide a kind of preparation method of the nickelic polynary positive pole material of high-quality, energy
The performance difference for reducing layer material above and below after being sintered, improves material overall performance, and Gao Pin is made while ensureing production efficiency
Matter product, and extend the service life of saggar.
The technical solution adopted by the present invention is as follows：
A kind of preparation method of the nickelic polynary positive pole material of high-quality, includes the following steps：
After mixing by nickelic polynary presoma and lithium source, it is packed into side wall and bottom is provided with venthole and inside is lined with
In the saggar of high temperature resistant organic film, it is re-fed into sintering furnace and carries out high temperature sintering under conditions of being passed through oxygen, after the completion of sintering
It is crushed, is sieved, removing magnetic, obtaining the nickelic polynary positive pole material of high-quality.
The present invention is transformed nickelic polynary positive pole material sintering saggar, to improve existing nickelic polynary positive pole material
Defect existing for sintering technology.By padding one layer of high temperature resistant organic film between material inside saggar, it can stop sintering process
Material is leaked out from the venthole of saggar, before sintering the phase, and metal can be fully met by diffusing to internal oxygen from material upper layer
Element oxide demand will not generate larger adverse effect even if there is the presence of high temperature resistant organic film, and work as and reach certain burning
When junction temperature, organic film starts to decompose, material lost flowability due to high temperature, therefore will not be flowed out from venthole, in organic film
After decomposition, oxygen can enter from the venthole of saggar side wall and bottom, increase partial pressure of oxygen of the subsurface material in sintering process,
Crystal oxygen defect caused by preventing material from being decomposed due to the smaller caused product deoxidation of partial pressure of oxygen in high-temperature burning process, to
It preferably crystallizes, reduces levels difference in material properties, improve the overall performance of material.
Furthermore due to all opening up venthole in the side wall of saggar and bottom, greatly improve gas diffusion effect, therefore energy
Largely increase saggar sintered material loadings, loads highly usable maximum and load highly without influencing product quality, it is real
Production efficiency is now improved, product production capacity is improved.
It is in direct contact with saggar in melting process in addition, high temperature resistant organic film has completely cut off lithium source, reduces saggar list
The damage of secondary sintering extends the service life of saggar.
Further,：The molecular formula of the nickelic polynary presoma is NixCoyMnzM(1-x-y-z)(OH)2, wherein 0.6≤x
Any one in ＜ 1,0 ＜ y≤0.2,0≤z≤0.2, M Al, Mg, Zr, Ti；The lithium source be lithium carbonate, lithium hydroxide,
Any one or more in lithium acetate, lithium oxalate.
Further, according to (Ni+Co+Mn+M):Li=1:The molar ratio of (1~1.05), by nickelic polynary presoma
It is uniformly mixed with lithium source.
Further, the decomposition temperature of the high temperature resistant organic film is higher than 400 DEG C, no sharp melting point, at 400~600 DEG C
Following temperature does not soften.Rule of thumb data, the material of sintering about in 400~600 DEG C or so lost flowabilities due to high temperature, because
This selection decomposition temperature is higher than 400 DEG C of organic film, can avoid material and is flowed out before consolidation from venthole.High temperature resistant organic film
The high temperature resistants organic materials such as polyimides can be selected in material.
Further, the thickness of the high temperature resistant organic film is 2-20 μm, and on the basis of preventing product material leakage, reduction has
The dosage of machine membrane material is increased with the oxygen consumption and impurity element that prevent excessive organic film material decomposition from bringing.
Further, the side wall of the saggar and bottom have multiple ventholes, and the aperture of each venthole is 2-
The surface density of 10mm, trepanning are 2500-10000/m2。
Further, the preparation method specifically includes following steps：
(1) nickelic polynary presoma is added with lithium source in batch mixer and is mixed；
(2) material after mixing is fitted into saggar, then stripping and slicing or jack processing is carried out to material, be conducive to follow-up
Gas diffusion in sintering process；
(3) saggar after charging is sent into sintering furnace, high temperature sintering, sintering temperature is carried out under conditions of being passed through oxygen
It is 200-1000 DEG C, is divided into 3-6 soaking zone, total duration is 10-42 hours；
(4) after sintering terminates cooling, sintering resulting material is crushed, be sieved, removes magnetic, it is high to obtain the high-quality
Nickel polynary positive pole material.
Further, the quantity of stripping and slicing is 4-36 blocks in step (2).
Further, in step (3), high temperature sintering is divided into following 3 soaking zones：It is small to be first warming up to 500-550 DEG C of heat preservation 4
When, then be warming up to 650-700 DEG C and keep the temperature 3 hours, it then heats to 810-870 DEG C and keeps the temperature 12 hours.
Early period, the burning of carbon and water that act as in lithium source, presoma of soaking zone was lost and preliminary solid solution；Mid-term is mainly protected
Temperature section act as the formation of product crystal under hot conditions and grows up；Later stage soaking zone act as annealing, and is protected by low temperature
Stress of the temperature by material in high-temperature calcination subsides, and product pattern is made to be improved, further promote granule strength.
Further, the aperture being sieved in step (4) is 400 mesh.
In order to better understand and implement, the invention will now be described in detail with reference to the accompanying drawings.
Description of the drawings
Fig. 1 is the structural schematic diagram of saggar used in the present invention.
Specific implementation mode
Embodiment 1
Positive electrode is prepared according to the following steps：
(1) (Ni+Co+Mn) is pressed:Li=1:1.03 molar ratio, by 622 ternary precursor (molecular formula：
Ni0.6Co0.2Mn0.2(OH)2) mixed 40 minutes with lithium carbonate addition high speed mixer.
(2) material after mixing is fitted into saggar, then stripping and slicing processing is carried out to material, be specifically uniformly cut into 36
Block.
As shown in Figure 1, the bottom of the saggar is square, its side length is 320mm, are highly 130mm, and material filling is high
Degree is 100mm, and the side wall of saggar and bottom have multiple ventholes, and the aperture of each venthole is 4mm, and the face of trepanning is close
Degree is 5000/m2。
Moreover, being lined with the high temperature resistant organic film that thickness is 10 μm inside the saggar, the high temperature resistant organic film covers casket
The bottom and side wall of alms bowl, between saggar and material, material is specially polyimides.
(3) saggar after charging is sent into sintering furnace, under conditions of being passed through purity more than 95% oxygen, carries out high temperature
Sintering, the temperature curve that sintering is arranged are：It is first warming up to 550 DEG C and keeps the temperature 4 hours, then be warming up to 700 DEG C and keep the temperature 3 hours, then rise
Temperature to 870 DEG C keep the temperature 12 hours.
(4) after sintering terminates simultaneously natural cooling, Mechanical Crushing is carried out to sintering resulting material, crosses 400 mesh sieve, except magnetic, is obtained
To finished product LiNi0.6Co0.2Mn0.2O2Positive electrode.
Embodiment 2
Positive electrode is prepared according to the following steps：
(1) (Ni+Co+Mn) is pressed:Li=1:1.05 molar ratio, by 811 ternary precursor (molecular formula：
Ni0.8Co0.1Mn0.1(OH)2) mixed 40 minutes with lithium carbonate addition high speed mixer.
(2) material after mixing is fitted into saggar, then stripping and slicing processing is carried out to material, be specifically uniformly cut into 36
Block.
As shown in Figure 1, the bottom of the saggar is square, its side length is 320mm, are highly 130mm, and material filling is high
Degree is 100mm, and the side wall of saggar and bottom have multiple ventholes, and the aperture of each venthole is 4mm, and the face of trepanning is close
Degree is 5000/m2。
Moreover, being lined with the high temperature resistant organic film that thickness is 10 μm inside the saggar, the high temperature resistant organic film covers casket
The bottom and side wall of alms bowl, between saggar and material, material is specially polyimides.
(3) saggar after charging is sent into sintering furnace, under conditions of being passed through purity more than 95% oxygen, carries out high temperature
Sintering, the temperature curve that sintering is arranged are：It is first warming up to 500 DEG C and keeps the temperature 4 hours, then be warming up to 650 DEG C and keep the temperature 3.5 hours, then
It is warming up to 820 DEG C and keeps the temperature 12 hours.
(4) after sintering terminates simultaneously natural cooling, Mechanical Crushing is carried out to sintering resulting material, crosses 400 mesh sieve, except magnetic, is obtained
To finished product LiNi0.8Co0.1Mn0.1O2Positive electrode.
Embodiment 3
Positive electrode is prepared according to the following steps：
(1) (Ni+Co+Al) is pressed:Li=1:1.05 molar ratio, by NCA presoma (molecular formula：Ni0.8Co0.15Al0.05
(OH)2) mixed 40 minutes with lithium carbonate addition high speed mixer.
(2) material after mixing is fitted into saggar, then stripping and slicing processing is carried out to material, be specifically uniformly cut into 36
Block.
As shown in Figure 1, the bottom of the saggar is square, its side length is 320mm, are highly 130mm, and material filling is high
Degree is 100mm, and the side wall of saggar and bottom have multiple ventholes, and the aperture of each venthole is 4mm, and the face of trepanning is close
Degree is 5000/m2。
Moreover, being lined with the high temperature resistant organic film that thickness is 10 μm inside the saggar, the high temperature resistant organic film covers casket
The bottom and side wall of alms bowl, between saggar and material, material is specially polyimides.
(3) saggar after charging is sent into sintering furnace, under conditions of being passed through purity more than 95% oxygen, carries out high temperature
Sintering, the temperature curve that sintering is arranged are：It is first warming up to 500 DEG C and keeps the temperature 4 hours, then be warming up to 650 DEG C and keep the temperature 3 hours, then rise
Temperature to 810 DEG C keep the temperature 12 hours.
(4) after sintering terminates simultaneously natural cooling, Mechanical Crushing is carried out to sintering resulting material, crosses 400 mesh sieve, except magnetic, is obtained
To finished product LiNi0.8Co0.15Al0.05O2Positive electrode.
Comparative example 1
Positive electrode is prepared according to the following steps：
(1) (Ni+Co+Mn) is pressed:Li=1:1.03 molar ratio, by 622 ternary precursor (molecular formula：
Ni0.6Co0.2Mn0.2(OH)2) mixed 40 minutes with lithium carbonate addition high speed mixer.
(2) material after mixing is fitted into common saggar, then stripping and slicing processing is carried out to material, be specifically uniformly cut into
36 pieces.The bottom of common saggar used is square, and its side length is 320mm, is highly 130mm, and material filling height is
100mm。
(3) saggar after charging is sent into sintering furnace, under conditions of being passed through purity more than 95% oxygen, carries out high temperature
Sintering, the temperature curve that sintering is arranged are：It is first warming up to 550 DEG C and keeps the temperature 4 hours, then be warming up to 700 DEG C and keep the temperature 3 hours, then rise
Temperature to 870 DEG C keep the temperature 12 hours.
(4) after sintering terminates simultaneously natural cooling, Mechanical Crushing is carried out to sintering resulting material, crosses 400 mesh sieve, except magnetic, is obtained
To finished product LiNi0.6Co0.2Mn0.2O2Positive electrode.
Comparative example 2
Positive electrode is prepared according to the following steps：
(1) (Ni+Co+Mn) is pressed:Li=1:1.05 molar ratio, by 811 ternary precursor (molecular formula：
Ni0.8Co0.1Mn0.1(OH)2) mixed 40 minutes with lithium carbonate addition high speed mixer.
(2) material after mixing is fitted into common saggar, then stripping and slicing processing is carried out to material, be specifically uniformly cut into
36 pieces.The bottom of common saggar used is square, and its side length is 320mm, is highly 130mm, and material filling height is
100mm。
(3) saggar after charging is sent into sintering furnace, under conditions of being passed through purity more than 95% oxygen, carries out high temperature
Sintering, the temperature curve that sintering is arranged are：It is first warming up to 500 DEG C and keeps the temperature 4 hours, then be warming up to 650 DEG C and keep the temperature 3 hours, then rise
Temperature to 855 DEG C keep the temperature 12 hours.
(4) after sintering terminates simultaneously natural cooling, Mechanical Crushing is carried out to sintering resulting material, crosses 400 mesh sieve, except magnetic, is obtained
To finished product LiNi0.8Co0.1Mn0.1O2Positive electrode.
Comparative example 3
Positive electrode is prepared according to the following steps：
(1) (Ni+Co+Al) is pressed:Li=1:1.05 molar ratio, by NCA presoma (molecular formula：Ni0.8Co0.15Al0.05
(OH)2) mixed 40 minutes with lithium carbonate addition high speed mixer.
(2) material after mixing is fitted into common saggar, then stripping and slicing processing is carried out to material, be specifically uniformly cut into
36 pieces.The bottom of common saggar used is square, and its side length is 320mm, is highly 130mm, and material filling height is
100mm。
(3) saggar after charging is sent into sintering furnace, under conditions of being passed through purity more than 95% oxygen, carries out high temperature
Sintering, the temperature curve that sintering is arranged are：It is first warming up to 500 DEG C and keeps the temperature 4 hours, then be warming up to 650 DEG C and keep the temperature 3 hours, then rise
Temperature to 810 DEG C keep the temperature 12 hours.
(4) after sintering terminates simultaneously natural cooling, Mechanical Crushing is carried out to sintering resulting material, crosses 400 mesh sieve, except magnetic, is obtained
To finished product LiNi0.8Co0.15Al0.05O2Positive electrode.
Performance Evaluation
The upper and lower layer of material samples in saggar after step (3) sintering in embodiment 1-3, comparative example 1-3 respectively, then divides
Not carry out Mechanical Crushing, cross 400 mesh sieve, remove magnetic, 12 parts of positive electrode samples are obtained, carry out electrical performance evaluation respectively.
Appraisal procedure is as follows：According to mass ratio 90:5:5, positive electrode sample, conductive agent carbon black, binder PVDF are existed
It is assembled into 2016 type button cells in glove box, then carries out charge and discharge cycles test, selection voltage is 3.0-4.35V, and electric current is close
Degree is 1C/1C and 0.2C/0.2C, and assessment result see the table below.
As seen from the above table, by opening up venthole to saggar and pad sets high temperature resistant organic film, on embodiment 1-3 is obtained
The performance of subsurface material is almost the same, and comparative example 1-3 is using the performance difference of layer material is larger up and down made from common saggar.
Several embodiments of the invention above described embodiment only expresses, the description thereof is more specific and detailed, but simultaneously
It cannot therefore be construed as limiting the scope of the patent.It should be pointed out that coming for those of ordinary skill in the art
It says, without departing from the inventive concept of the premise, various modifications and improvements can be made, these belong to the protection of the present invention
Range.
Claims (10)
1. a kind of preparation method of the nickelic polynary positive pole material of high-quality, it is characterised in that：Include the following steps：
After mixing by nickelic polynary presoma and lithium source, it is packed into side wall and bottom is provided with venthole and inside is lined with resistance to height
It in the saggar of warm organic film, is re-fed into sintering furnace and carries out high temperature sintering under conditions of being passed through oxygen, carried out after the completion of sintering
Broken, sieving removes magnetic, obtains the nickelic polynary positive pole material of high-quality.
2. the preparation method of the nickelic polynary positive pole material of high-quality according to claim 1, it is characterised in that：It is described nickelic
The molecular formula of polynary presoma is NixCoyMnzM(1-x-y-z)(OH)2, wherein 0.6≤x ＜ 1,0 ＜ y≤0.2,0≤z≤0.2, M
For any one in Al, Mg, Zr, Ti；The lithium source is any one in lithium carbonate, lithium hydroxide, lithium acetate, lithium oxalate
Or it is a variety of.
3. the preparation method of the nickelic polynary positive pole material of high-quality according to claim 2, it is characterised in that：According to (Ni+
Co+Mn+M):Li=1:Nickelic polynary presoma is uniformly mixed by the molar ratio of (1~1.05) with lithium source.
4. the preparation method of the nickelic polynary positive pole material of high-quality according to claim 1, it is characterised in that：The resistance to height
The decomposition temperature of warm organic film is higher than 400 DEG C.
5. the preparation method of the nickelic polynary positive pole material of high-quality according to claim 1, it is characterised in that：The resistance to height
The thickness of warm organic film is 2-20 μm.
6. the preparation method of the nickelic polynary positive pole material of high-quality according to claim 1, it is characterised in that：The saggar
Side wall and bottom have multiple ventholes, the aperture of each venthole is 2-10mm, and the surface density of trepanning is 2500-
10000/m2。
7. according to the preparation method of the nickelic polynary positive pole material of claim 1-6 any one of them high-quality, it is characterised in that：
Specifically include following steps：
(1) nickelic polynary presoma is added with lithium source in batch mixer and is mixed；
(2) material after mixing is fitted into saggar, then stripping and slicing or jack processing is carried out to material；
(3) saggar after charging is sent into sintering furnace, high temperature sintering is carried out under conditions of being passed through oxygen, sintering temperature is
200-1000 DEG C, it is divided into 3-6 soaking zone, total duration is 10-42 hours；
(4) after sintering terminates cooling, sintering resulting material is crushed, be sieved, removes magnetic, it is nickelic more to obtain the high-quality
First positive electrode.
8. the preparation method of the nickelic polynary positive pole material of high-quality according to claim 7, it is characterised in that：Step (2)
The quantity of middle stripping and slicing is 4-36 blocks.
9. the preparation method of the nickelic polynary positive pole material of high-quality according to claim 7, it is characterised in that：Step (3)
In, high temperature sintering is divided into following 3 soaking zones：It is first warming up to 500-550 DEG C and keeps the temperature 4 hours, then be warming up to 650-700 DEG C of heat preservation
It 3 hours, then heats to 810-870 DEG C and keeps the temperature 12 hours.
10. the preparation method of the nickelic polynary positive pole material of high-quality according to claim 7, it is characterised in that：Step (4)
The aperture of middle sieving is 400 mesh.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| 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 |
| CN114249358A (en) * | 2022-03-01 | 2022-03-29 | 宜宾锂宝新材料有限公司 | Positive electrode material and preparation method thereof |
| CN114560511A (en) * | 2022-01-26 | 2022-05-31 | 泾河新城陕煤技术研究院新能源材料有限公司 | High-nickel cathode material with high cycle stability and preparation method thereof |
| CN115247958A (en) * | 2022-07-28 | 2022-10-28 | 广西立劲新材料有限公司 | Preparation method and device of long-life power type lithium manganate |
| CN115504511A (en) * | 2022-09-28 | 2022-12-23 | 安徽博石高科新材料股份有限公司 | Collinear production method of anode material |
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| CN103094545A (en) * | 2013-01-24 | 2013-05-08 | 湖南桑顿新能源有限公司 | Preparation method for cathode material of high-nickel lithium ion battery |
| CN103884190A (en) * | 2012-12-19 | 2014-06-25 | 日本精细陶瓷有限公司 | Ceramic coating sagger for manufacturing lithium ion anode active material and manufacturing method thereof |
| CN206192127U (en) * | 2016-08-20 | 2017-05-24 | 汕头市瑞升电子有限公司 | Sagger |
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| CN103884190A (en) * | 2012-12-19 | 2014-06-25 | 日本精细陶瓷有限公司 | Ceramic coating sagger for manufacturing lithium ion anode active material and manufacturing method thereof |
| CN103094545A (en) * | 2013-01-24 | 2013-05-08 | 湖南桑顿新能源有限公司 | Preparation method for cathode material of high-nickel lithium ion battery |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN114560511A (en) * | 2022-01-26 | 2022-05-31 | 泾河新城陕煤技术研究院新能源材料有限公司 | High-nickel cathode material with high cycle stability and preparation method thereof |
| CN114560511B (en) * | 2022-01-26 | 2023-07-18 | 泾河新城陕煤技术研究院新能源材料有限公司 | High-nickel positive electrode material with high cycle stability and preparation method thereof |
| CN114249358A (en) * | 2022-03-01 | 2022-03-29 | 宜宾锂宝新材料有限公司 | Positive electrode material and preparation method thereof |
| CN115247958A (en) * | 2022-07-28 | 2022-10-28 | 广西立劲新材料有限公司 | Preparation method and device of long-life power type lithium manganate |
| CN115504511A (en) * | 2022-09-28 | 2022-12-23 | 安徽博石高科新材料股份有限公司 | Collinear production method of anode material |
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| CN108493447B (en) | 2019-12-13 |
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