CN109817945A - A kind of nickelic positive electrode and preparation method thereof - Google Patents
A kind of nickelic positive electrode and preparation method thereof Download PDFInfo
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Abstract
The present invention provides a kind of nickelic positive electrode and preparation method thereof, the preparation method comprises the following steps: (1) mixing hydroxide nickel cobalt manganese with lithium source and the first additive, the first sintering is carried out after drying under oxygen atmosphere, obtains the first sintered material；(2) after the first sintered material for obtaining step (1) is broken, the second sintering is carried out under oxygen atmosphere, obtains the second sintered material；(3) after the second sintered material screening obtained step (2), Second addition is added, third sintering is carried out under oxygen or air atmosphere, obtains the nickelic positive electrode.The preparation method can promote positive electrode each component to be uniformly mixed, and the pattern for controlling material is smooth mellow and full single crystal grain, improves electrical property and cycle performance, substantially improve high temperature storage and produce gas and high temperature circulation production gas problem.
Description
Technical field
The invention belongs to battery material field, be related to a kind of preparation method of positive electrode, more particularly to it is a kind of it is nickelic just
The preparation method of pole material.
Background technique
811 positive electrodes of mainstream are all synthesis secondary ball aggregates currently on the market, and there are Ni/Li mixing is tight for the structure
Weight, pole piece compaction density is not high, and residual alkali is high, and pH high, cycle performance is general, and high temperature circulation produces the problems such as gas is serious, leads to battery
Storage or circulation diving, bulging bring security risk.
Summary of the invention
To solve the technical problems existing in the prior art, the present invention provides a kind of preparation method of nickelic positive electrode,
The preparation method can promote positive electrode each component to be uniformly mixed, and the pattern for controlling material is smooth mellow and full single crystal grain,
Electrical property and cycle performance are improved, high temperature storage is substantially improved and produces gas and high temperature circulation production gas problem.
In order to achieve the above object, the invention adopts the following technical scheme:
The present invention provides a kind of nickelic positive electrode and preparation method thereof, and the preparation method comprises the following steps:
(1) hydroxide nickel cobalt manganese is mixed with lithium source and the first additive, carries out first under oxygen atmosphere after dry
Sintering, obtains the first sintered material；
(2) after the first sintered material for obtaining step (1) is broken, the second sintering is carried out under oxygen atmosphere, obtains the
Two sintered materials；
(3) after the second sintered material screening obtained step (2), Second addition is added, is carried out under oxygen atmosphere
Third sintering, obtains the nickelic positive electrode.
Lithium source used in the present invention can be the common lithium source such as lithium hydroxide, lithium carbonate, lithium acetate or lithium oxalate.
As currently preferred technical solution, step (1) first additive is Zr, B, La, Y, V, Ti, Mg or Al
Organic compound or inorganic compound in any one or at least two combination.
Preferably, the inorganic compound of described Zr, B, La, Y, V, Ti, Mg or Al are Zr, B, La, Y, V, Ti, Mg or Al
Oxide.
Preferably, the content of first additive be 50~5000ppm, as 50ppm, 100ppm, 200ppm,
500ppm, 1000ppm, 1500ppm, 2000ppm, 3000ppm, 4000ppm or 5000ppm etc., it is not limited to cited
Numerical value, other unlisted numerical value are equally applicable in the numberical range.
Preferably, step (1) the mixed method is that mixing is sanded in wet process.
As currently preferred technical solution, the temperature of step (1) first sintering is 850~880 DEG C, such as 850
DEG C, 855 DEG C, 860 DEG C, 865 DEG C, 870 DEG C, 875 DEG C or 880 DEG C etc., it is not limited to cited numerical value, the numberical range
Other interior unlisted numerical value are equally applicable.
Preferably, step (1) it is described first sintering time be 6~15h, as 5h, 6h, 7h, 8h, 9h, 10h, 11h,
12h, 13h, 14h or 15h etc., it is not limited to cited numerical value, other interior unlisted numerical value of the numberical range are same
It is applicable in.
As currently preferred technical solution, it is 3- that step (2) the broken granularity of the first sintered material, which is D50,
6 μm, 1.0 μm of D10 >, 18 μm of D90 <.
Wherein, D50 can be 3 μm, 3.5 μm, 4 μm, 4.5 μm, 5 μm, 5.5 μm or 6 μm etc., and D10 can be 1.5 μm, 2 μ
M, 5 μm, 8 μm, 10 μm, 12 μm or 15 μm etc., D90 can be 2 μm, 5 μm, 8 μm, 10 μm, 12 μm, 15 μm or 17 μm etc., but simultaneously
It is not limited only to cited numerical value, other unlisted numerical value are equally applicable in above-mentioned each numberical range.
As currently preferred technical solution, the temperature of step (2) second sintering is 800~880 DEG C, such as 800
DEG C, 810 DEG C, 820 DEG C, 830 DEG C, 840 DEG C, 850 DEG C, 860 DEG C, 870 DEG C or 880 DEG C etc., it is not limited to cited number
Value, other interior unlisted numerical value of the numberical range are equally applicable.
Preferably, the time of second sintering is 4~8h, such as 4h, 4.5h, 5h, 5.5h, 6h, 6.5h, 7h, 7.5h or
8h etc., it is not limited to cited numerical value, other interior unlisted numerical value of the numberical range are equally applicable.
As currently preferred technical solution, it is 3- that the granularity after step (3) the second sintered material screening, which is D50,
6 μm, 1.0 μm of D10 >, 18 μm of D90 <.
Wherein, D50 can be 3 μm, 3.5 μm, 4 μm, 4.5 μm, 5 μm, 5.5 μm or 6 μm etc., and D10 can be 1.5 μm, 2 μ
M, 5 μm, 8 μm, 10 μm, 12 μm or 15 μm etc., D90 can be 2 μm, 5 μm, 8 μm, 10 μm, 12 μm, 15 μm or 17 μm etc., but simultaneously
It is not limited only to cited numerical value, other unlisted numerical value are equally applicable in above-mentioned each numberical range.
As currently preferred technical solution, step (3) Second addition is Zr, B, La, Y, V, Ti, Mg or Al
Organic compound or inorganic compound in any one or at least two combination.
Preferably, the inorganic compound of described Zr, B, La, Y, V, Ti, Mg or Al are Zr, B, La, Y, V, Ti, Mg or Al
Oxide.
Preferably, the content of the Second addition be 50~5000ppm, as 50ppm, 100ppm, 200ppm,
500ppm, 1000ppm, 1500ppm, 2000ppm, 3000ppm, 4000ppm or 5000ppm etc., it is not limited to cited
Numerical value, other unlisted numerical value are equally applicable in the numberical range.
As currently preferred technical solution, the temperature of step (3) the third sintering is 300~700 DEG C, such as 300
DEG C, 350 DEG C, 400 DEG C, 450 DEG C, 500 DEG C, 550 DEG C, 600 DEG C, 650 DEG C or 700 DEG C etc., it is not limited to cited number
Value, other interior unlisted numerical value of the numberical range are equally applicable.
Preferably, the time of third sintering is 4~8h, such as 4h, 4.5h, 5h, 5.5h, 6h, 6.5h, 7h, 7.5h or
8h etc., it is not limited to cited numerical value, other interior unlisted numerical value of the numberical range are equally applicable.
As currently preferred technical solution, after step (3) third sintering to obtained material carry out screening and
Except magnetic.
As currently preferred technical solution, the preparation method of the nickelic positive electrode of monocrystalline the following steps are included:
(1) hydroxide nickel cobalt manganese is mixed with lithium source and the first additive wet process sand milling, after drying under oxygen atmosphere
850~880 DEG C carry out first 6~15h of sintering, obtain the first sintered material；
(2) after the first sintered material for obtaining step (1) is broken, it is 3 that the broken granularity of the first sintered material, which is D50,
~6 μm, 18 μm of D90 <, second 4~8h of sintering is carried out for 800~880 DEG C under oxygen atmosphere, obtains the second burning by 1.0 μm of D10 >
Tie material；
(3) after the second sintered material screening obtained step (2), it is 3 that the granularity after the screening of the second sintered material, which is D50,
~6 μm, 1.0 μm of D10 >, 18 μm of D90 <, Second addition is added, carries out for 300~700 DEG C under oxygen or air atmosphere
Three 4~8h of sintering, are sieved and except magnetic obtains the nickelic pole material.
In the present invention, technique is sanded by wet process, it is ensured that in mixing process, lithium source and presoma reach nanoscale and mix
It closes, additive can be also evenly distributed in material structure, substantially reduce Li+Diffusion path during the sintering process, hence it is evident that promote
Crystal property into material sintering process cooperates the adjustment of sintering process, can obtain the good monocrystalline of crystallinity or class list
Brilliant 811 positive electrodes.The increase of material crushing stage is once sintered after once sintered simultaneously, for repairing crushing stage to material
It is damaged caused by surface, its crystallization can be promoted more perfect, particle surface is bright and clean mellow and full, and fine powder and clast are few, further improves
The cycle performance and storage performance of material.
Compared with prior art, the present invention at least has the advantages that
(1) present invention provides a kind of preparation method of nickelic positive electrode, the preparation method be prepared it is nickelic just
Pole material is monocrystalline or class monocrystalline pattern, and particle is uniform, and particle surface is bright and clean mellow and full；
(2) present invention provides a kind of nickelic positive electrode and preparation method thereof, and the preparation method is prepared nickelic
Positive electrode improves electrical property and cycle performance, substantially improves high temperature storage and produces gas and high temperature circulation production gas problem.
Detailed description of the invention
Fig. 1 is the flow diagram of nickelic method for preparing anode material provided by the invention；
Fig. 2 is the SEM figure for the nickelic positive electrode that the present invention is prepared；
Fig. 3 is the SEM figure for 811 positive electrodes being commercially available on the market；
Fig. 4 is the full battery normal temperature circulation test chart in the specific embodiment of the invention.
The present invention is described in more detail below.But following examples is only simple example of the invention, not generation
Table or limitation the scope of the present invention, protection scope of the present invention are subject to claims.
Specific embodiment
Of the invention for ease of understanding, it is as follows that the present invention enumerates embodiment.Those skilled in the art are it will be clearly understood that the implementation
Example is only to aid in the understanding present invention, should not be regarded as a specific limitation of the invention.
Embodiment 1
The present embodiment provides a kind of nickelic positive electrodes and preparation method thereof, and the preparation method comprises the following steps:
(1) hydroxide nickel cobalt manganese is mixed with lithium carbonate and butyl titanate wet process sand milling, in oxygen atmosphere after drying
Lower 850 DEG C carry out the first sintering 15h, obtain the first sintered material；
(2) after the first sintered material for obtaining step (1) is broken, it is 3 that the broken granularity of the first sintered material, which is D50,
~6 μm, 1.0 μm of D10 >, 18 μm of D90 <, 800 DEG C carry out the second sintering 8h, obtain the second sintered material；
(3) after the second sintered material screening obtained step (2), the granularity after the screening of the second sintered material is that D50 is
3-6 μm, 1.0 μm of D10 >, 18 μm of D90 <, ammonium metavanadate is added, 300 DEG C of progress thirds are sintered 8h, screening under oxygen atmosphere
The nickelic positive electrode is obtained with magnetic is removed.
Embodiment 2
The present embodiment provides a kind of preparation methods of nickelic positive electrode, and the preparation method comprises the following steps:
(1) hydroxide nickel cobalt manganese is mixed with lithium hydroxide and aluminium oxide wet process sand milling, after drying under oxygen atmosphere
880 DEG C carry out the first sintering 6h, obtain the first sintered material；
(2) after the first sintered material for obtaining step (1) is broken, it is 3 that the broken granularity of the first sintered material, which is D50,
~6 μm, 1.0 μm of D10 >, 18 μm of D90 <, 880 DEG C carry out the second sintering 4h, obtain the second sintered material；
(3) after the second sintered material screening obtained step (2), it is 3 that the granularity after the screening of the second sintered material, which is D50,
~6 μm, 1.0 μm of D10 >, 18 μm of D90 <, zirconium oxide is added, 700 DEG C of progresss thirds are sintered 4h under oxygen atmosphere, screening with
Except magnetic obtains the nickelic positive electrode.
Embodiment 3
The present embodiment provides a kind of preparation methods of nickelic positive electrode, and the preparation method comprises the following steps:
(1) hydroxide nickel cobalt manganese is mixed with lithium source and yttria wet process sand milling, after drying under oxygen atmosphere
820 DEG C carry out the first sintering 8h, obtain the first sintered material；
(2) after the first sintered material for obtaining step (1) is broken, it is 3 that the broken granularity of the first sintered material, which is D50,
~6 μm, 1.0 μm of D10 >, 18 μm of D90 <, 850 DEG C carry out the second sintering 6h, obtain the second sintered material；
(3) after the second sintered material screening obtained step (2), it is 3 that the granularity after the screening of the second sintered material, which is D50,
~6 μm, 1.0 μm of D10 >, 18 μm of D90 <, magnesium hydroxide is added, 500 DEG C of progress thirds are sintered 6h, screening under oxygen atmosphere
The nickelic positive electrode is obtained with magnetic is removed.
Embodiment 4
The present embodiment provides a kind of preparation methods of nickelic positive electrode, and the preparation method comprises the following steps:
(1) hydroxide nickel cobalt manganese is mixed with lithium oxalate and metaboric acid wet process sand milling, after drying 830 under oxygen atmosphere
DEG C carry out first sintering 10h, obtain the first sintered material；
(2) after the first sintered material for obtaining step (1) is broken, it is 3 that the broken granularity of the first sintered material, which is D50,
~6 μm, 1.0 μm of D10 >, 18 μm of D90 <, 820 DEG C carry out the second sintering 6h, obtain the second sintered material；
(3) after the second sintered material screening obtained step (2), it is 3 that the granularity after the screening of the second sintered material, which is D50,
~6 μm, 1.0 μm of D10 >, 18 μm of D90 <, lanthanum chloride is added, 600 DEG C of progresss thirds are sintered 5h under oxygen atmosphere, screening with
Except magnetic obtains the nickelic positive electrode.
Embodiment 5
The present embodiment provides a kind of preparation methods of nickelic positive electrode, and the preparation method comprises the following steps:
(1) hydroxide nickel cobalt manganese is mixed with lithium acetate and butyl titanate wet process sand milling, in oxygen atmosphere after drying
Lower 870 DEG C carry out the first sintering 8h, obtain the first sintered material；
(2) after the first sintered material for obtaining step (1) is broken, it is 3 that the broken granularity of the first sintered material, which is D50,
~6 μm, 18 μm of D90 <, the second sintering 5h is carried out for 860 DEG C under oxygen atmosphere, obtains the second sintered material by 1.0 μm of D10 >；
(3) after the second sintered material screening obtained step (2), it is 3 that the granularity after the screening of the second sintered material, which is D50,
~6 μm, 1.0 μm of D10 >, 18 μm of D90 <, ammonium metavanadate is added, 600 DEG C of progress thirds are sintered 5h, screening under oxygen atmosphere
The nickelic positive electrode is obtained with magnetic is removed.
Comparative example 1
For this comparative example other than the first sintering described without step (1), other conditions are same as Example 3.
Comparative example 2
For this comparative example other than the second sintering described without step (2), other conditions are same as Example 3.
Comparative example 3
For this comparative example other than without step (3) the third sintering, other conditions are same as Example 3.
The nickelic positive electrode of monocrystalline that embodiment 1-5 and comparative example 1-3 are provided is used to prepare anode pole piece, using people
It makes graphite cathode and prepares cathode pole piece, using high nickel electrolyte, the 2Ah soft-package battery of lamination is assembled into, to the electricity of battery
The cycle performance of performance and battery is tested, and the results are shown in Table 1.
Table 1
| Experiment case study | 1C gram volume mAh/g | 1C first charge discharge efficiency % | Multiplying power discharging 3C/1C |
| Embodiment 1 | 189.5 | 84.3 | 89.2% |
| Embodiment 2 | 188.7 | 84.5 | 87.9% |
| Embodiment 3 | 189.4 | 84.3 | 88.6% |
| Embodiment 4 | 188.6 | 85.2 | 89.1% |
| Embodiment 5 | 190.2 | 84.7 | 88.4% |
| Comparative example 1 | 184.3 | 82.6 | 85.2% |
| Comparative example 2 | 185.7 | 82.8 | 85.3% |
| Comparative example 3 | 183.2 | 81.6 | 83.7% |
The test work step of full battery normal temperature circulation test in the specific embodiment of the invention is as follows:
Step 1: shelving 10min；
Step 2:CCCV charging, electric current 0.2C, blanking voltage 4.2V end charging current 0.05C；
Step 3: shelving 10min；
Step 4:CC electric discharge, blanking voltage 2.7V, electric current 0.2C；
Step 5: shelving 10min；
Step 6:CCCV charging, electric current 1C, blanking voltage 4.2V end charging current 0.05C；
Step 7: shelving 10min；
Step 8:CC electric discharge, blanking voltage 2.7V, electric current 1C；
Step 9: circulation, originate work step Step 5, cycle-index 200 times；
Step 10: circulation, originate work step Step 1, cycle-index 15 times.
The Applicant declares that the present invention is explained by the above embodiments detailed construction feature of the invention, but the present invention is simultaneously
It is not limited to above-mentioned detailed construction feature, that is, does not mean that the present invention must rely on above-mentioned detailed construction feature and could implement.Institute
Belong to those skilled in the art it will be clearly understood that any improvement in the present invention, to the equivalence replacement of component selected by the present invention
And increase, selection of concrete mode of accessory etc., all of which fall within the scope of protection and disclosure of the present invention.
The preferred embodiment of the present invention has been described above in detail, still, during present invention is not limited to the embodiments described above
Detail within the scope of the technical concept of the present invention can be with various simple variants of the technical solution of the present invention are made, this
A little simple variants all belong to the scope of protection of the present invention.
It is further to note that specific technical features described in the above specific embodiments, in not lance
In the case where shield, can be combined in any appropriate way, in order to avoid unnecessary repetition, the present invention to it is various can
No further explanation will be given for the combination of energy.
In addition, various embodiments of the present invention can be combined randomly, as long as it is without prejudice to originally
The thought of invention, it should also be regarded as the disclosure of the present invention.
Claims (10)
1. a kind of preparation method of nickelic positive electrode, which is characterized in that the preparation method comprises the following steps:
(1) hydroxide nickel cobalt manganese is mixed with lithium source and the first additive, carries out the first sintering under oxygen atmosphere after dry,
Obtain the first sintered material；
(2) after the first sintered material for obtaining step (1) is broken, the second sintering is carried out under oxygen atmosphere, obtains the second burning
Tie material；
(3) after the second sintered material screening obtained step (2), Second addition is added, under oxygen or air atmosphere into
The sintering of row third, obtains the nickelic positive electrode.
2. preparation method according to claim 1, which is characterized in that step (1) first additive be Zr, B, La,
Y, the organic compound of V, Ti, Mg or Al or in inorganic compound any one or at least two combination；
Preferably, the inorganic compound of described Zr, B, La, Y, V, Ti, Mg or Al are the oxidation of Zr, B, La, Y, V, Ti, Mg or Al
Object；
Preferably, the content of first additive is 50~5000ppm；
Preferably, step (1) the mixed method is that mixing is sanded in wet process.
3. preparation method according to claim 1 or 2, which is characterized in that step (1) it is described first sintering temperature be
850~880 DEG C；
Preferably, the time of step (1) first sintering is 6~15h.
4. preparation method according to claim 1-3, which is characterized in that step (2) first sintered material
It is 3-6um that broken granularity, which is D50,1.0 μm of D10 >, D90 < 18um.
5. preparation method according to claim 1-4, which is characterized in that the temperature of step (2) second sintering
Degree is 800~880 DEG C；
Preferably, the time of second sintering is 4~8h.
6. preparation method according to claim 1-5, which is characterized in that step (3) second sintered material
Granularity after screening is that D50 is 3-6um, D10 > 1.0um, D90 < 18um.
7. preparation method according to claim 1-6, which is characterized in that step (3) second addition
Agent be Zr, B, La, Y, V, Ti, Mg or Al organic compound or in inorganic compound any one or at least two group
It closes；
Preferably, the inorganic compound of described Zr, B, La, Y, V, Ti, Mg or Al are the oxidation of Zr, B, La, Y, V, Ti, Mg or Al
Object；
Preferably, the content of the Second addition is 50~5000ppm.
8. preparation method according to claim 1-7, which is characterized in that the temperature of step (3) the third sintering
Degree is 300~700 DEG C；
Preferably, the time of the third sintering is 4~8h.
9. preparation method according to claim 1-8, which is characterized in that right after step (3) the third sintering
Obtained material sieve and except magnetic.
10. -9 described in any item preparation methods according to claim 1, which is characterized in that the preparation method includes following step
It is rapid:
(1) hydroxide nickel cobalt manganese and lithium source and the first additive wet process sand milling mixs, after drying 850 under oxygen atmosphere~
880 DEG C carry out first 6~15h of sintering, obtain the first sintered material；
(2) after the first sintered material for obtaining step (1) is broken, it is 3- that the broken granularity of the first sintered material, which is D50,
1.0 μm of 6um, D10 >, D90 < 18um, second 4~8h of sintering is carried out for 800~880 DEG C under oxygen atmosphere, obtains the second sintering
Material；
(3) after the second sintered material screening obtained step (2), it is 3- that the granularity after the screening of the second sintered material, which is D50,
Second addition, 300~700 DEG C of progress thirds under oxygen or air atmosphere is added in 6um, D10 > 1.0um, D90 < 18um
It is sintered 4~8h, obtains the nickelic positive electrode.
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Cited By (5)
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| CN110589901A (en) * | 2019-06-26 | 2019-12-20 | 浙江美都海创锂电科技有限公司 | Preparation method of nickel cobalt lithium manganate positive electrode material (Ni is more than or equal to 0.8) |
| CN112079400A (en) * | 2020-09-09 | 2020-12-15 | 合肥国轩高科动力能源有限公司 | Low-pH-value lithium ion battery high-nickel ternary material and preparation method and application thereof |
| CN112479270A (en) * | 2020-12-02 | 2021-03-12 | 山东丰元化学股份有限公司 | Preparation method of ternary positive electrode material of lithium ion power battery |
| CN112599763A (en) * | 2020-12-15 | 2021-04-02 | 惠州亿纬锂能股份有限公司 | Ternary single crystal positive electrode material and preparation method and application thereof |
| WO2022207008A1 (en) | 2021-12-24 | 2022-10-06 | 北京当升材料科技股份有限公司 | Single-crystal-type multi-element positive electrode material, and preparation method therefor and application thereof |
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| CN112599763A (en) * | 2020-12-15 | 2021-04-02 | 惠州亿纬锂能股份有限公司 | Ternary single crystal positive electrode material and preparation method and application thereof |
| WO2022207008A1 (en) | 2021-12-24 | 2022-10-06 | 北京当升材料科技股份有限公司 | Single-crystal-type multi-element positive electrode material, and preparation method therefor and application thereof |
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