CN105355841A - High-capacity and high-rate lithium battery anode material and preparation method thereof - Google Patents
High-capacity and high-rate lithium battery anode material and preparation method thereof Download PDFInfo
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- CN105355841A CN105355841A CN201510772303.XA CN201510772303A CN105355841A CN 105355841 A CN105355841 A CN 105355841A CN 201510772303 A CN201510772303 A CN 201510772303A CN 105355841 A CN105355841 A CN 105355841A
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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
- H01M4/04—Processes of manufacture in general
- H01M4/043—Processes of manufacture in general involving compressing or compaction
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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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- 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
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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
Abstract
The invention discloses a preparation method of a high-capacity and high-rate lithium battery anode material, and is characterized in that the preparation method includes the following steps: stirring needle-coke and a binder in a high-speed stirrer evenly; pressing the mixture after stirring under an ultra-high pressure of an isostatic pressing machine, to obtain an initially-pressed block; heating and sintering the initially-pressed block under a nitrogen atmosphere protection, cooling, and then crushing and shaping the semi-finished block, to obtain a carbon powder; and carrying out high temperature graphitization on the carbon powder, cooling, and then carrying out iron removal screening, to obtain the graphite powder with high rate, high capacity and high compaction. The graphite anode material prepared by the preparation method has the characteristics of high capacity, high rate and good cycling performance.
Description
Technical field
The present invention relates to a kind of battery material and preparation method thereof, especially a kind of high power capacity high-rate lithium battery negative material and preparation method thereof.
Background technology
Storage battery is that current storage battery mainly contains nickel-cadmium cell, nickel metal hydride battery, nickel-zinc cell, lead-acid battery, lithium battery etc. in the world widely used a kind of chemical " power supply ".Wherein, lithium battery is a class is negative material, the battery using non-aqueous electrolytic solution by lithium metal or lithium alloy.It to be proposed by GilbertN.Lewis early than 1912 and studies.Along with development, the progress of society, the raising of human life quality, digital product obtains universal, and lithium battery is also progressively valued by the people extensively for the energy as electric energy important in digital product and high end instrument product.
Compared with other a few class storage batterys, the advantage of lithium battery is:
(1) high-energy-density, the weight of lithium battery is the NI-G of identical capacity or the half of Ni-MH battery, and volume is the 20-30% of the 40-50% of NI-G, ni-mh;
(2) high voltage, the operating voltage of a lithium battery monomer is 3.7V (mean value), is equivalent to NI-G or the Ni-MH battery of three series connection;
(3) pollution-free, no matter to produce, use and scrap, lithium battery not containing and do not produce harmful metal elements and the material of such as cadmium, lead, mercury and so on;
(4) cycle life is high, and under normal operation, the useful life of lithium battery can reach more than 6 years, and the charging-discharging cycle of lithium battery can more than 500 times;
(5) memory-less effect, memory effect refers to that nickel-cadmium cell is in charge and discharge cycles process, the phenomenon of the capacity minimizing of battery, and lithium battery does not exist this effect;
(6) quick charge, uses the constant-current constant-voltage charging device that rated voltage is 4.2V that lithium battery can be made completely to be filled within one or two hour.
The raising of lithium cell cathode material to lithium battery performance plays vital effect.At present, lithium cell cathode material is divided into following several substantially: the first is carbon negative pole material, as electrographite, native graphite, carbonaceous mesophase spherules, petroleum coke, carbon fiber, thermal decomposed resins carbon etc.; The second is tin base cathode material; The third is lithium-containing transition metal nitride negative material; 4th kind is alloy type negative material; 5th kind is nanoscale negative material; 6th kind is nanometer oxide material.Wherein, graphite is the earliest for the carbon negative pole material of lithium battery, its good conductivity, and degree of crystallinity is high, has complete layered crystal structure, and be well suited for the embedding of lithium ion and deviate from, therefore, graphite material adopts maximum lithium cell cathode materials in prior art.Graphite is applied to lithium cell cathode material, and after requiring that graphite cathode material makes pole piece, compacting is high, and absorbency is good, and the battery capacity be assembled into is high, and multiplying power is good.
For solving problems, Chinese patent 201410855276.8, discloses soft carbon negative pole material of a kind of lithium ion battery modification and preparation method thereof.The present invention is at soft carbon dust granule interior doped graphene powder particle, and meanwhile, graphene powder Granular composite is carried in the nanometer clad material coating on described soft carbon dust particle top layer and forms conductive nano carbon-coating.Its preparation method is: carry out pre-burning after soft carbon raw material and grapheme material being carried out mixed grinding to 0.3 μm-4 μm; by the material after pre-burning in a solvent conductive agent, binding agent carry out mixed at high speed, obtain the soft carbon negative pole material of modification by heat-treating under protective atmosphere after mixed soft material with carbon element vacuumize.Utilizing the method to prepare modification, soft carbon negative pole material reversible specific capacity is greater than 360mAh/g, efficiency is greater than 85%, and has excellent quick lithium storage performance, and high rate performance and cycle performance have larger improvement.But the content of binding agent is higher in the present invention, bonding process is complicated, limits the improvement that cycle performance is larger to a certain extent.
Summary of the invention
For solving above-mentioned Problems existing, the object of the present invention is to provide a kind of high power capacity high-rate lithium battery negative material, described graphite cathode material is suppressed through hyperpressure in equal pressing equipment, and required binder amount is low, has high multiplying power and capacity.
For achieving the above object, technical scheme of the present invention is:
A preparation method for high power capacity high-rate lithium battery negative material, comprises the steps:
(1) needle coke and binding agent are stirred in homogenizer, mixing speed is 500-1000r/min, and mixing time is 20-30min;
(2) mixture after stirring is suppressed under the pressure of isostatic pressing machine 100-200MPa, obtain just briquetting;
(3) first briquetting is heated 500-1000 DEG C under nitrogen atmosphere protection, fire 10-20 hour, after having fired, naturally cool to room temperature, then semi-finished product block is carried out fragmentation and shaping, obtain carbon dust;
(4) by carbon dust high temperature graphitization, graphitization temperature is 2500-3000 DEG C, naturally cools, then carries out deironing screening, obtain high magnification, high power capacity, the graphite powder of high-pressure solid.
Separately, the D50 of needle coke is selected to be 4-6 μm in described step (1).
Further, the binding agent in described step (1) is any one or any combination in pitch or tar or resin.
And, in described step (1) needle coke and binding agent mass percent be 7:3 ~ 4:1.
Meanwhile, described binding agent needs hot mastication before high-speed stirred.
Further, a kind of high power capacity high-rate lithium battery negative material, adopts above-mentioned method to prepare.
Separately have, the D50 of described lithium cell cathode material is 9.5-18 μm, and tap density is 1.0-1.2g/cm
3, specific area is 0.9-3m
2/ g, ash content is 0.05-0.1%, and moisture is 0.1-0.2%.
Beneficial effect of the present invention is:
(1) in preparation process step (1) of the present invention, the proportioning of needle coke and binding agent is: 70:30 ~ 80:20 (wt%), under the condition that the content of binding agent is low, carry out granulation, make the graphite cathode material finally obtained have excellent cycle performance of battery;
(2) content due to binding agent is low, the oarse-grained carbon dust be made up of many small particle diameter material with carbon elements can be obtained, this carbon dust is in carbonization and graphited process, the contraction about 75% of binding agent, the contraction about 45% of needle coke, effectively good contraction makes to form space between graphitic molecules, and this structure can have certain space elasticity, obtained pole piece high-pressure solid, absorbency is good simultaneously;
(3) in step (2), mixture is suppressed through the hyperpressure of isostatic pressing machine 100-200MPa, can obtain isotropic material with carbon element, substantially increase the high rate performance finally obtaining lithium cell cathode material;
(4) preparation method of high power capacity high-rate lithium battery negative material of the present invention overcome in prior art produce at ambient pressure graphite cathode material need equipment many, yield poorly, shortcoming that energy consumption is large, there is good prospects for commercial application.
Accompanying drawing explanation
Fig. 1 is the SEM figure of the high power capacity high-rate lithium battery negative material that the embodiment of the present invention 1 prepares.
Fig. 2 is the rebound curves figure of the high power capacity high-rate lithium battery negative material that the embodiment of the present invention 1 prepares.
Fig. 3 is the imbibition curve chart of the high power capacity high-rate lithium battery negative material that the embodiment of the present invention 1 prepares.
Fig. 4 is the compaction curve figure of the high power capacity high-rate lithium battery negative material that the embodiment of the present invention 1 prepares.
Fig. 5 is the first charge-discharge curve chart that the embodiment of the present invention 1 prepares the lithium battery that high power capacity high-rate lithium battery negative material makes.
Embodiment
In order to make object of the present invention, technical scheme and advantage clearly understand, further describe below in conjunction with drawings and Examples.
Embodiment 1
D50 is selected to be the needle coke of 5 μm, D50 adopts the American-European gram laser particle analyzer of LS-POP-6 to record, asphalt high-temperature softens, the mixing and stirring in homogenizer by 700g needle coke and 300g pitch, mixing speed is 800r/min, mixing time is 20min, mixture after stirring is suppressed under the pressure of isostatic pressing machine 200MPa, the first briquetting obtained under nitrogen atmosphere protection 800 DEG C fire 15 hours, room temperature is naturally cooled to after having fired, then semi-finished product block is carried out fragmentation and shaping, obtain the carbon dust that D50 is 16.51 μm, then by carbon dust high temperature graphitization at 3000 DEG C, naturally deironing screening is carried out after cooling, obtain high magnification, high power capacity, the graphite powder of high-pressure solid, gained graphite powder free from admixture, tap density is 1.149g/cm
3, specific area is 1.115m
2/ g, ash content is 0.05%, and moisture is 0.15%, compacted density is 1.69g/cm
2, secondary compaction density is 1.93g/cm
2.
Fig. 1 is the SEM figure of the lithium cell cathode material that embodiment 1 prepares; In order to check the rebound rate of the lithium cell cathode material utilizing embodiment 1 to prepare, carry out baking bounce-back test, to place thickness that 30min tests after roll-in for benchmark, test material is in the rebound rate of 95 DEG C of heating 6h, and Fig. 2 tests the rebound curves obtained; Fig. 3 is the imbibition curve of the lithium cell cathode material that embodiment 1 prepares, and can find out the increase along with compacted density, and the imbibition time of the lithium cell cathode material that embodiment 1 prepares also increases gradually, and this material has good absorbent; Have detected the compaction capacity of the lithium cell cathode material that embodiment 1 prepares further, Fig. 4 is the compaction curve of embodiment 1 material; Fig. 5 is the first charge-discharge curve chart of the lithium battery of the negative material making that embodiment 1 obtains, and concrete test data is in table 1.
Embodiment 2
D50 is selected to be the needle coke of 4 μm, D50 adopts the American-European gram laser particle analyzer of LS-POP-6 to record, tar hot mastication, the mixing and stirring in homogenizer by 750g needle coke and 250g tar, mixing speed is 500r/min, mixing time is 30min, mixture after stirring is suppressed under the pressure of isostatic pressing machine 200MPa, the first briquetting obtained under nitrogen atmosphere protection 1000 DEG C fire 10 hours, room temperature is naturally cooled to after having fired, then semi-finished product block is carried out fragmentation and shaping, obtain the carbon dust that D50 is 17.23 μm, then by carbon dust high temperature graphitization at 2500 DEG C, naturally deironing screening is carried out after cooling, obtain high magnification, high power capacity, the graphite powder of high-pressure solid, gained graphite powder free from admixture, tap density is 1.053g/cm
3, specific area is 1.162m
2/ g, ash content is 0.09%, and moisture is 0.19%, compacted density is 1.71g/cm
2, secondary compaction density is 1.99g/cm
2.
Test the first charge-discharge of the lithium battery of the negative material making that embodiment 2 obtains, concrete test data is in table 1.
Embodiment 3
D50 is selected to be the needle coke of 6 μm, D50 adopts the American-European gram laser particle analyzer of LS-POP-6 to record, resin hot mastication, the mixing and stirring in homogenizer by 800g needle coke and 200g resin, mixing speed is 1000r/min, mixing time is 20min, mixture after stirring is suppressed under the pressure of isostatic pressing machine 100MPa, the first briquetting obtained under nitrogen atmosphere protection 500 DEG C fire 20 hours, room temperature is naturally cooled to after having fired, then semi-finished product block is carried out fragmentation and shaping, obtain the carbon dust that D50 is 14.97 μm, then by carbon dust high temperature graphitization at 3000 DEG C, naturally deironing screening is carried out after cooling, obtain high magnification, high power capacity, the graphite powder of high-pressure solid, gained graphite powder free from admixture, tap density is 1.107g/cm
3, specific area is 1.585m
2/ g, ash content is 0.06%, and moisture is 0.13%, compacted density is 1.73g/cm
2, secondary compaction density is 2.01g/cm
2.
Test the first charge-discharge of the lithium battery of the negative material making that embodiment 3 obtains, concrete test data is in table 1.
The electric performance test result table of table 1 embodiment 1-3
From testing above, utilize lithium cell cathode material prepared by the inventive method, capacity, the more existing graphite cathode material of efficiency for charge-discharge have and improve significantly first, and this preparation method overcome in prior art produce at ambient pressure graphite cathode material need equipment many, yield poorly, shortcoming that energy consumption is large, market potential is huge.
It should be noted that, above embodiment is only in order to illustrate technical scheme of the present invention and unrestricted.Although with reference to preferred embodiment to invention has been detailed description, those of ordinary skill in the art is to be understood that, can modify to the technical scheme of invention or equivalent replacement, and not depart from the scope of technical solution of the present invention, it all should be encompassed in right of the present invention.
Claims (7)
1. a preparation method for high power capacity high-rate lithium battery negative material, is characterized in that, comprises the steps:
(1) needle coke and binding agent are stirred in homogenizer, mixing speed is 500-1000r/min, and mixing time is 20-30min;
(2) mixture after stirring is suppressed under the pressure of isostatic pressing machine 100-200MPa, obtain just briquetting;
(3) first briquetting is heated 500-1000 DEG C under nitrogen atmosphere protection, fire 10-20 hour, after having fired, naturally cool to room temperature, then semi-finished product block is carried out fragmentation and shaping, obtain carbon dust;
(4) by carbon dust high temperature graphitization, graphitization temperature is 2500-3000 DEG C, naturally cools, then carries out deironing screening, obtain high magnification, high power capacity, the graphite powder of high-pressure solid.
2. the preparation method of a kind of high power capacity high-rate lithium battery negative material according to claim 1, is characterized in that, selects the D50 of needle coke to be 4-6 μm in described step (1).
3. the preparation method of a kind of high power capacity high-rate lithium battery negative material according to claim 1, is characterized in that, the binding agent in described step (1) is any one or any combination in pitch or tar or resin.
4. the preparation method of a kind of high power capacity high-rate lithium battery negative material according to claim 1, is characterized in that, in described step (1), the mass percent of needle coke and binding agent is 7:3 ~ 4:1.
5. the preparation method of a kind of high power capacity high-rate lithium battery negative material according to claim 3, it is characterized in that, described binding agent needs hot mastication before high-speed stirred.
6. a high power capacity high-rate lithium battery negative material, is characterized in that, adopts the method described in claim 1-5 to prepare.
7. a kind of high power capacity high-rate lithium battery negative material according to claim 6, is characterized in that, the D50 of described cell negative electrode material is 9.5-18 μm, and tap density is 1.0-1.2g/cm
3, specific area is 0.9-3m
2/ g, ash content is 0.05-0.1%, and moisture is 0.1-0.2%.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106082192A (en) * | 2016-06-13 | 2016-11-09 | 辽宁大化国瑞新材料有限公司 | Preparation method of artificial graphite powder for high-temperature gas cooled reactor nuclear fuel element and graphite powder |
| CN106252625A (en) * | 2016-08-26 | 2016-12-21 | 宁波杉杉新材料科技有限公司 | A kind of preparation method of EV graphite negative material of lithium ion battery |
| CN106410202A (en) * | 2016-08-17 | 2017-02-15 | 北京君研碳极科技有限公司 | Method for preparing electrode material from coal-to-oil residue |
| CN108110364A (en) * | 2017-12-27 | 2018-06-01 | 东莞鑫茂新能源技术有限公司 | A kind of lithium cell cathode material recoverying and utilizing method |
| CN109755569A (en) * | 2017-11-06 | 2019-05-14 | 上高县荣炭科技有限公司 | The granulation processing procedure of lithium cell cathode material |
| CN112072075A (en) * | 2020-09-02 | 2020-12-11 | 昆山宝创新能源科技有限公司 | Negative electrode film and preparation method and application thereof |
| CN114804093A (en) * | 2022-05-30 | 2022-07-29 | 乌海宝杰新能源材料有限公司 | Novel black phosphorus graphite composite negative electrode material and preparation method thereof |
| CN115196630A (en) * | 2022-06-07 | 2022-10-18 | 谢艳 | Preparation method for improving tap density of carbon electrode material for energy storage device |
| US11894548B2 (en) | 2018-08-17 | 2024-02-06 | Lg Energy Solution, Ltd. | Negative electrode active material, method of preparing the negative electrode active material, negative electrode, and secondary battery including the negative electrode |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106082192A (en) * | 2016-06-13 | 2016-11-09 | 辽宁大化国瑞新材料有限公司 | Preparation method of artificial graphite powder for high-temperature gas cooled reactor nuclear fuel element and graphite powder |
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| CN106410202A (en) * | 2016-08-17 | 2017-02-15 | 北京君研碳极科技有限公司 | Method for preparing electrode material from coal-to-oil residue |
| CN106252625A (en) * | 2016-08-26 | 2016-12-21 | 宁波杉杉新材料科技有限公司 | A kind of preparation method of EV graphite negative material of lithium ion battery |
| CN109755569A (en) * | 2017-11-06 | 2019-05-14 | 上高县荣炭科技有限公司 | The granulation processing procedure of lithium cell cathode material |
| CN113903916A (en) * | 2017-11-06 | 2022-01-07 | 上高县荣炭科技有限公司 | Application of coupling agent in granulation process of lithium battery negative electrode material and granulation process of lithium battery negative electrode material |
| CN108110364A (en) * | 2017-12-27 | 2018-06-01 | 东莞鑫茂新能源技术有限公司 | A kind of lithium cell cathode material recoverying and utilizing method |
| US11894548B2 (en) | 2018-08-17 | 2024-02-06 | Lg Energy Solution, Ltd. | Negative electrode active material, method of preparing the negative electrode active material, negative electrode, and secondary battery including the negative electrode |
| CN112072075A (en) * | 2020-09-02 | 2020-12-11 | 昆山宝创新能源科技有限公司 | Negative electrode film and preparation method and application thereof |
| CN114804093A (en) * | 2022-05-30 | 2022-07-29 | 乌海宝杰新能源材料有限公司 | Novel black phosphorus graphite composite negative electrode material and preparation method thereof |
| CN115196630A (en) * | 2022-06-07 | 2022-10-18 | 谢艳 | Preparation method for improving tap density of carbon electrode material for energy storage device |
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Application publication date: 20160224 |