CN107871854A - A kind of preparation method of graphite negative material of lithium ion battery second particle - Google Patents
A kind of preparation method of graphite negative material of lithium ion battery second particle Download PDFInfo
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- CN107871854A CN107871854A CN201610851983.9A CN201610851983A CN107871854A CN 107871854 A CN107871854 A CN 107871854A CN 201610851983 A CN201610851983 A CN 201610851983A CN 107871854 A CN107871854 A CN 107871854A
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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
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/139—Processes of manufacture
- H01M4/1393—Processes of manufacture of electrodes based on carbonaceous material, e.g. graphite-intercalation compounds or CFx
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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 present invention relates to technical field of lithium ion battery negative, specifically a kind of preparation method of graphite negative material of lithium ion battery second particle, it comprises the steps:A kind of Delanium raw material are heated up while stirring, then constant temperature obtains secondary coated particle;Graphitization processing obtains second particle cladding;Second particle cladding is subjected to fusion extrusion process;Second particle cladding after fusion is subjected to uniform premix processing;Screening process obtains second particle A;By another Delanium raw material, high temperature graphitization processing, then crushing and classification processing are carried out, obtains individual particle B;By second particle A and individual particle B mixtures, composite particles graphite cathode material is produced.Compared with prior art, the product of preparation has higher tap density to the present invention, has taken into account the excellent charging of second particle material and cycle performance, the characteristics of having taken into account high-tap density, the high power capacity of individual particle material again.
Description
Technical field
The present invention relates to technical field of lithium ion battery negative, specifically a kind of graphite negative electrode of lithium ion battery
The preparation method of material secondary particle.
Background technology
Lithium ion battery is by its high-energy-density, high working voltage, charge/discharge rates are fast, have extended cycle life, safe without dirt
The advantages that dye, successfully substitute other secondary cells, turn into the miniature electrics such as mobile phone, notebook computer and Video Camera
The main energy sources of product, and the industrialization process of electric automobile has greatly been promoted, many countries also start lithium comprehensively
For ion battery in military and aerospace field exploitation, this has just put forward higher requirement to lithium ion battery.
With development in science and technology, electronic product and energy automobile more are paid close attention to energy density and high power, especially
Energy automobile to high power can fast charging and discharging have very big requirement.Therefore in recent years for graphite modification into
For study hotspot.
The content of the invention
The purpose of the present invention is overcome the deficiencies in the prior art, and the Delanium raw material of two kinds of different sizes are entered respectively
After row processing, mixture processing is carried out according still further to certain proportion, has obtained that second particle material excellent charging and circulation can be taken into account
Performance, individual particle material high-tap density, the product of high power capacity performance have been taken into account again.
To achieve the above object, a kind of preparation method of graphite negative material of lithium ion battery second particle is designed, it is wrapped
Include following step:
(1), in inert gas, a kind of Delanium raw material that D50 is 8.5~10.5 μm is put into low-temperature surface and are modified
In reactor, using heating rate as 1.5 DEG C/min, for the speed of stirring in 28~38r/min, the heating-up time is 180~240min
Progress heats up while stir, then constant temperature 240min, obtains secondary coated particle;
(2) secondary coated particle, is obtained into second particle cladding with 2300~2800 DEG C of progress 52~70h of graphitization processing
Body;
(3) second particle cladding, is subjected to fusion extrusion process, fusion rotating speed is 700~800r/min, time of fusion
For 3min;At 14~17 μm, the material packing volume of fusion is 75~85% for fusion particle diameter D50 controls after fusion;
(4) the second particle cladding after fusion, is subjected to uniform premix processing;
(5) screening process, is carried out with the screen cloth of 60~150 mesh, extracting screen underflow obtains second particle A;
(6), by another Delanium raw material that D50 is 15.5~21 μm, high fire stons is carried out with 2400~2800 DEG C
Inkization handles 46~62h;
(7) another Delanium raw material after graphitization processing, are subjected to crushing and classification processing, obtaining D50 is
17.0~20.0 μm of individual particle B;
(8), by second particle A and individual particle B 100: 28~32 ratio mixtures by ratio of weight and the number of copies, composite particles stone is produced
Black negative material.
Described premix is handled handles 45~60min with 36r/min rotating speed.
The D50 of described secondary coated particle is 16~19 μm.
The D50 of described another Delanium raw material is 18~18.5 μm.
Compared with prior art, the product of preparation has higher tap density to the present invention, has taken into account second particle material
Excellent charging and cycle performance, the characteristics of having taken into account high-tap density, the high power capacity of individual particle material again;It is obtained in addition to produce
Product are by individual particle and the accumulation filling of secondary coated particle, and for increase particle respectively to going tropism to be distributed, pole piece bounce-back is small, while makes electrolysis
Liquid is more unimpeded in charcoal and graphite material is embedded into, and cycle performance is more excellent, and its chemical property is summarized as follows:(1) put first
Capacitance is in more than 350mAh/g;(2) discharge platform and platform conservation rate are higher;(3) good cycle (350 circulations, capacity
Keep > 94%);(4) Product processing performance is good, and pole piece bounce-back is small;(4) preparation for processing is fairly simple, is adapted to industrial metaplasia
Production.
Embodiment
The present invention is further described in conjunction with embodiment.
Embodiment 1
The preparation method of this example comprises the steps:
(1), in inert gas, by a kind of Delanium raw material that D50 is 8.5 μm, it is put into low-temperature surface and is modified instead
Answer in kettle, using heating rate as 1.5 DEG C/min, for the speed of stirring in 28r/min, the heating-up time is that 180min carries out one side heating
While stirring, then constant temperature 240min, obtain secondary coated particle;
(2) secondary coated particle, is obtained into second particle cladding with 2300 DEG C of progress graphitization processing 52h;
(3) second particle cladding, is subjected to fusion extrusion process, fusion rotating speed is 700r/min, and time of fusion is
3min;Fusion particle diameter D50 after fusion is 15 μm, and the material packing volume of fusion is 80%;;
(4), the second particle cladding after fusion is carried out at uniform premix with 36r/min rotating speed processing 45min
Reason;
(5) screening process, is carried out with the screen cloth of 60 mesh, extracting screen underflow obtains second particle A;
(6), by another Delanium raw material that D50 is 15.5 μm, high temperature graphitization processing are carried out with 2400 DEG C
46h;
(7) another Delanium raw material after graphitization processing, are subjected to crushing and classification processing, obtaining D50 is
17.0 μm individual particle B;
(8), by second particle A and individual particle B by ratio of weight and the number of copies 100:28 ratio mixture, produces composite particles graphite
Negative material.
Embodiment 2
The preparation method of this example comprises the steps:
(1), in inert gas, by a kind of Delanium raw material that D50 is 9.0 μm, it is put into low-temperature surface and is modified instead
Answer in kettle, using heating rate as 1.5 DEG C/min, for the speed of stirring in 35r/min, the heating-up time is that 200min carries out one side heating
While stirring, then constant temperature 240min, obtain secondary coated particle;
(2) secondary coated particle, is obtained into second particle cladding with 2500 DEG C of progress graphitization processing 60h;
(3) second particle cladding, is subjected to fusion extrusion process, fusion rotating speed is 750r/min, and time of fusion is
3min;Fusion particle diameter D50 after fusion is 16 μm, and the material packing volume of fusion is 77%;
(4), the second particle cladding after fusion is carried out at uniform premix with 36r/min rotating speed processing 50min
Reason;
(5) screening process, is carried out with the screen cloth of 100 mesh, extracting screen underflow obtains second particle A;
(6), by another Delanium raw material that D50 is 18 μm, high temperature graphitization processing 52h is carried out with 2600 DEG C;
(7) another Delanium raw material after graphitization processing, are subjected to crushing and classification processing, obtaining D50 is
18.0 μm of individual particle B;
(8), by second particle A and individual particle B by ratio of weight and the number of copies 100: 30 ratio mixture, composite particles graphite is produced
Negative material.
Embodiment 3
The preparation method of this example comprises the steps:
(1), in inert gas, by a kind of Delanium raw material that D50 is 10.5 μm, it is put into low-temperature surface and is modified instead
Answer in kettle, using heating rate as 1.5 DEG C/min, for the speed of stirring in 38r/min, the heating-up time is that 240min carries out one side heating
While stirring, then constant temperature 240min, obtain secondary coated particle;
(2) secondary coated particle, is obtained into second particle cladding with 2500 DEG C of progress graphitization processing 60h;
(3) second particle cladding, is subjected to fusion extrusion process, fusion rotating speed is 800r/min, and time of fusion is
3min;Fusion particle diameter D50 after fusion is 17 μm, and the material packing volume of fusion is 80%;
(4), the second particle cladding after fusion is carried out at uniform premix with 36r/min rotating speed processing 60min
Reason;
(5) screening process, is carried out with the screen cloth of 150 mesh, extracting screen underflow obtains second particle A;
(6), by another Delanium raw material that D50 is 21 μm, high temperature graphitization processing 62h is carried out with 2800 DEG C;
(7) another Delanium raw material after graphitization processing, are subjected to crushing and classification processing, obtaining D50 is
20.0 μm of individual particle B;
(8), by second particle A and individual particle B by ratio of weight and the number of copies 100:32 ratio mixture, produces composite particles graphite
Negative material.
The chemical property comparative result of the embodiment of the present invention 1~3 is as shown in table 1.
Table 1
It is obvious to a person skilled in the art that the invention is not restricted to the details of above-mentioned one exemplary embodiment, Er Qie
In the case of without departing substantially from spirit or essential attributes of the invention, the present invention can be realized in other specific forms.Therefore, no matter
From the point of view of which point, embodiment all should be regarded as exemplary, and be nonrestrictive, the scope of the present invention is by appended power
Profit requires rather than described above limits, it is intended that all in the implication and scope of the equivalency of claim by falling
Change is included in the present invention.
Moreover, it will be appreciated that although the present specification is described in terms of embodiments, not each embodiment is only wrapped
Containing an independent technical scheme, this narrating mode of specification is only that those skilled in the art should for clarity
Using specification as an entirety, the technical solutions in the various embodiments may also be suitably combined, forms those skilled in the art
It is appreciated that other embodiment.
Claims (4)
1. a kind of preparation method of graphite negative material of lithium ion battery second particle, it comprises the steps:
(1), in inert gas, a kind of Delanium raw material that D50 is 8.5~10.5 μm are put into low-temperature surface modified-reaction
In kettle, using heating rate as 1.5 DEG C/min, the speed of stirring is carried out in 28~38r/min, heating-up time for 180~240min
Heat up while stir, then constant temperature 240min, obtain secondary coated particle;
(2) secondary coated particle, is obtained into second particle cladding with 2300~2800 DEG C of progress 52~70h of graphitization processing;
(3) second particle cladding, is subjected to fusion extrusion process, fusion rotating speed is 700~800r/min, and time of fusion is
3min;At 14~17 μm, the material packing volume of fusion is 75~85% for fusion particle diameter D50 controls after fusion;
(4) the second particle cladding after fusion, is subjected to uniform premix processing;
(5) screening process, is carried out with the screen cloth of 60~150 mesh, extracting screen underflow obtains second particle A;
(6), by another Delanium raw material that D50 is 15.5~21 μm, high temperature graphitizations are carried out with 2400~2800 DEG C
Handle 46~62h;
(7) another Delanium raw material after graphitization processing, are subjected to crushing and classification processing, obtain D50 as 17.0
~20.0 μm of individual particle B;
(8), by second particle A and individual particle B by ratio of weight and the number of copies 100:28~32 ratio mixtures, produce composite particles graphite and bear
Pole material.
2. the preparation method of graphite negative material of lithium ion battery second particle according to claim 1, it is characterised in that:
Described premix is handled handles 45~60min with 36r/min rotating speed.
3. the preparation method of graphite negative material of lithium ion battery second particle according to claim 1, it is characterised in that:
The D50 of described secondary coated particle is 16~19 μm.
4. the preparation method of graphite negative material of lithium ion battery second particle according to claim 1, it is characterised in that:
The D50 of described another Delanium raw material is 18~18.5 μm.
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Cited By (11)
Publication number | Priority date | Publication date | Assignee | Title |
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CN108615889A (en) * | 2018-05-11 | 2018-10-02 | 合肥国轩高科动力能源有限公司 | Single composite graphite particle slurry combining method for lithium ion battery |
CN109065887A (en) * | 2018-06-30 | 2018-12-21 | 合肥国轩高科动力能源有限公司 | Slurry mixing method for negative electrode of lithium ion power battery |
CN109935891A (en) * | 2019-04-08 | 2019-06-25 | 珠海冠宇电池有限公司 | A kind of cobalt acid lithium number lithium ion battery that high/low temperature is taken into account |
CN110642247A (en) * | 2019-09-30 | 2020-01-03 | 广东凯金新能源科技股份有限公司 | Artificial graphite negative electrode material, preparation method thereof and lithium ion battery |
CN110649256A (en) * | 2019-10-17 | 2020-01-03 | 石家庄尚太科技有限公司 | Single-particle and secondary-particle mixed high-energy-density graphite negative electrode material and preparation method thereof |
CN111370654A (en) * | 2018-12-26 | 2020-07-03 | 宁波杉杉新材料科技有限公司 | Composite graphite negative electrode material, lithium ion battery and preparation method and application thereof |
CN112645319A (en) * | 2020-12-23 | 2021-04-13 | 福建杉杉科技有限公司 | Composite graphite negative electrode material, lithium ion battery and preparation method |
CN112670466A (en) * | 2020-04-30 | 2021-04-16 | 宁波杉杉新材料科技有限公司 | Composite graphite negative electrode material, preparation method thereof and lithium ion battery |
CN113422024A (en) * | 2021-06-25 | 2021-09-21 | 洛阳月星新能源科技有限公司 | Preparation method of high-compaction-density composite negative electrode graphite material |
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CN108615889A (en) * | 2018-05-11 | 2018-10-02 | 合肥国轩高科动力能源有限公司 | Single composite graphite particle slurry combining method for lithium ion battery |
CN109065887A (en) * | 2018-06-30 | 2018-12-21 | 合肥国轩高科动力能源有限公司 | Slurry mixing method for negative electrode of lithium ion power battery |
CN111370654B (en) * | 2018-12-26 | 2022-02-22 | 宁波杉杉新材料科技有限公司 | Composite graphite negative electrode material, lithium ion battery and preparation method and application thereof |
CN111370654A (en) * | 2018-12-26 | 2020-07-03 | 宁波杉杉新材料科技有限公司 | Composite graphite negative electrode material, lithium ion battery and preparation method and application thereof |
CN109935891A (en) * | 2019-04-08 | 2019-06-25 | 珠海冠宇电池有限公司 | A kind of cobalt acid lithium number lithium ion battery that high/low temperature is taken into account |
CN109935891B (en) * | 2019-04-08 | 2021-10-29 | 珠海冠宇电池股份有限公司 | Lithium cobaltate digital lithium ion battery with high and low temperature consideration |
CN110642247A (en) * | 2019-09-30 | 2020-01-03 | 广东凯金新能源科技股份有限公司 | Artificial graphite negative electrode material, preparation method thereof and lithium ion battery |
CN110649256B (en) * | 2019-10-17 | 2021-04-27 | 石家庄尚太科技股份有限公司 | Single-particle and secondary-particle mixed high-energy-density graphite negative electrode material and preparation method thereof |
CN110649256A (en) * | 2019-10-17 | 2020-01-03 | 石家庄尚太科技有限公司 | Single-particle and secondary-particle mixed high-energy-density graphite negative electrode material and preparation method thereof |
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WO2021217587A1 (en) * | 2020-04-30 | 2021-11-04 | 宁德时代新能源科技股份有限公司 | Secondary battery and manufacturing method therefor, and apparatus comprising secondary battery |
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US12027695B2 (en) | 2020-04-30 | 2024-07-02 | Contemporary Amperex Technology Co., Limited | Secondary battery, process for preparing the same and apparatus containing the secondary battery |
CN112645319A (en) * | 2020-12-23 | 2021-04-13 | 福建杉杉科技有限公司 | Composite graphite negative electrode material, lithium ion battery and preparation method |
CN113422024A (en) * | 2021-06-25 | 2021-09-21 | 洛阳月星新能源科技有限公司 | Preparation method of high-compaction-density composite negative electrode graphite material |
CN113422024B (en) * | 2021-06-25 | 2023-03-10 | 洛阳月星新能源科技有限公司 | Preparation method of high-compaction-density composite negative electrode graphite material |
WO2023115509A1 (en) * | 2021-12-24 | 2023-06-29 | 宁德时代新能源科技股份有限公司 | Artificial graphite and preparation method therefor, and secondary battery and electrical device comprising artificial graphite |
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Application publication date: 20180403 |