CN103094536A - High-capacity lithium ion secondary battery cathode carbon material - Google Patents
High-capacity lithium ion secondary battery cathode carbon material Download PDFInfo
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- CN103094536A CN103094536A CN2013100455074A CN201310045507A CN103094536A CN 103094536 A CN103094536 A CN 103094536A CN 2013100455074 A CN2013100455074 A CN 2013100455074A CN 201310045507 A CN201310045507 A CN 201310045507A CN 103094536 A CN103094536 A CN 103094536A
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Abstract
The invention relates to a high-capacity lithium ion secondary battery cathode carbon material. The high-capacity lithium ion secondary battery cathode carbon material is prepared using through natural graphite and asphalt, wherein the weight ratio of the natural graphite to asphalt is 6:30-1; the particle sizes of the natural graphite are in a range of 8-27mum, and the specific surface area of the natural graphite is 5m<2>/g; and the asphalt is coal tar asphalt or petroleum asphalt. The carbon modified material can be widely applied to high-capacity lithium ion secondary cathode materials. The high-capacity lithium ion secondary battery cathode carbon material belongs to composite graphite, and has the advantages of good cycle performances, long battery life, high gram volume, high compacted density, small specific surface area and excellent processability.
Description
Technical field
The present invention relates to Carbon Materials of a kind of high-capacity lithium-ion secondary battery negative pole and preparation method thereof.
Background technology
At present, along with developing rapidly of international new forms of energy new material, being widely used and high speed development of various New-energy electric vehicles and portable electric appts, electric tool, requirement to chemical power source also improves in succession, lithium ion battery is the present more successful a kind of portable chemical power supply of exploitation, and it has, and voltage is high, specific energy large, discharging voltage balance, cryogenic property is good, security performance is excellent and easily store and the advantage such as long working life.Yet extensive use, electronics miniaturization and the microminiaturized degree of current electric automobile are more and more higher, and be also more deep with application to the research of lithium ion battery.
At present, in commercial lithium ion battery, negative material adopts graphite material mostly, its advantage be have higher specific capacity (＜372mAh/g), low electrode potential (＜1.0Vvs.Li
+/ Li), high efficient first, long cycle life.Graphite material again because of its kind, preparation method and heat treatment temperature not simultaneously, can cause the difference on the Nomenclature Composition and Structure of Complexes, and then cause the difference of embedding behavior and performance.
Graphite is divided into again Delanium and native graphite, and that Delanium has is good with compatibility of electrolyte, its embedding, to take off speed larger, and load character etc. is preferably arranged.The steady phase spherical carbon of Jie that PANASONIC has adopted graphited asphalt carbon microballoon namely to make take pitch as raw material is called for short MCMB.But the volume and capacity ratio that it is low and first efficient be still waiting to improve.Native graphite is current comparatively ideal negative material, has that cost is low, capacity is higher and the characteristics such as compaction capacity is good, and company has just adopted native graphite as SANYO GS.Shortcoming is that they are more responsive to some electrolyte, is subject to again the restriction of theoretical lithium storage content, is difficult to increase substantially very much by improving battery preparation technique merely.
Therefore, have higher capacity and Development of New Generation Novel anode material, become the hot subject in the Study on Li-ion batteries using field.Once, alloy material had been once the first-selection that people study, but the efficient first that it is low and high bulk effect cause relatively poor cyclical stability to fail to be well solved always, reach 600mAh/g as standby tin-oxide reversible capacities of employing CVD legal system such as Hironorid, but its irreversible capacity reaches 800mAh/g ［ J.Power So μ trces, 2001,97-98:229 ］ especially, efficient is obviously on the low side first, its drawbacks limit its application in lithium ion battery.The compound system of the silicon grain outer wrapping amorphous carbon layer of the subordinate's of Hitachi MAXwell company preparation, although improved structure and the electric conductivity of silicon materials, because its technical process is restive, uncertain factor is many, causes being difficult to realize producing in batches.Reported the negative material by the hard charcoal preparation of pyrolysis in Chinese invention patent CN01807830.3, because modifying on its surface, irreversible capacity is quite high, cause the high reason of irreversible capacity except electrode solution is decomposed to form passivating film, various active groups such as the hydroxyl of material surface, with and the moisture of absorption be also the main cause that forms irreversible capacity, although hydroxyl and moisture have been eliminated when pyrolysis; Due in the assembling and use procedure of battery, if electrode and various active gasess contact, as CO
2, O
2, also can strengthen irreversible reaction and lose reversible capacity, this is also that the commercialization pyrolyzed carbon materials is to the reason of air-sensitive.
Summary of the invention
The technical problem that invention solves is to provide Carbon Materials of a kind of high-capacity lithium-ion secondary battery negative pole and preparation method thereof.
A kind of high-capacity lithium-ion secondary battery negative pole Carbon Materials is made by native graphite and pitch that weight ratio is 6 ~ 30:1.
Described high-capacity lithium-ion secondary battery negative pole Carbon Materials, the particle diameter of its described native graphite is 8～27 μ m, specific area is less than or equal to 5m
2/ g; Described pitch is coal tar pitch or petroleum asphalt.
Described high-capacity lithium-ion secondary battery negative pole Carbon Materials, its described high-capacity lithium-ion secondary battery negative pole Carbon Materials is native graphite and pitch to be dissolved in carry out liquid-phase dehydration after organic solvent in pressure vessel again and process, then by coating modification, low-temperature setting, charing, finally by making after high-temperature heat treatment, cooling, screening.
Described high-capacity lithium-ion secondary battery negative pole Carbon Materials, its described carbon modified material of making is spherical or elliposoidal, and average grain diameter D50 is 2～28 μ m, and tap density is between 0.7～1.5g/cc, and the BET specific area is at 1.0～5.0m
2Between/g, real density 0.9～2.20g/cc, there is nano-pore its inside, aperture 0.2～0.6nm.
The preparation method of described high-capacity lithium-ion secondary battery negative pole Carbon Materials, step is as follows:
1. get the raw materials ready: with native graphite and the pitch ratio by weight 6～30:1, ready for use;
2. reinforced: as the raw material of getting ready to be dissolved in organic solvent, alternately to join while stirring in pressure vessel, continue to stir 1～3 hour, then added the reaction promoter of total weight 5%～20% in 8～25 minutes;
3. heat up: the heating that then heats up, in 6～7 hours, temperature is raised to 500～700 ℃; The negative pressure 1～4 hour time of wherein heating up is extracted the volatile matter in above-mentioned substance out;
4. keep constant temperature: keep constant temperature at 500～700 ℃, 5～8 hours time, extract simultaneously volatile matter out;
5. naturally cool to room temperature;
6. 2000～2800 ℃ of high temperature carry out graphitization processing;
Wherein, 6. 5. 4. 3. described step all carry out under anti-oxidation environment.
Described preparation method, its described anti-oxidation environment is to extract in non-negative pressure to pass into inert gas or hydrogen under state.
Described preparation method, its described inert gas is nitrogen, its flow is 0.5～2m
3/ h.
Described preparation method, its described reaction promoter is cycloalkane and/or aromatic solvent.
Described preparation method, its described aromatic solvent be selected from fear oil and washing oil in any.
Carbon modified material provided by the invention can be widely used in the high-capacity lithium-ion secondary battery cathode material.The carbon modified material that the present invention makes, be take native graphite as main material, take pitch as the modification medium, belong to composite graphite, this material has kept the advantage of native graphite height ratio capacity, efficient is low first to have overcome simultaneously the native graphite cycle performance, and the shortcoming that cycle performance is relatively poor possesses gram volume high, compacted density is high, specific area is little, and processing characteristics is good, the advantages such as good cycle.For the preparation of lithium ion battery, have very high electrical property, its first efficient and cycle performance all be significantly improved, can satisfy lithium ion battery to the demand of high power capacity and high cycle life, can stop to overcharge and cross and put, be well suited for for high-energy-density density lithium ion battery.The invention belongs to composite graphite, good cycle, battery life is long, and gram volume is high, and compacted density is high, and specific area is little, and processing characteristics is good.The characteristics of maximum of the present invention are that its preparation technology's flow process is simple simultaneously, process is easy to control, cost of manufacture is low, environmentally friendly etc., this material can not only satisfy the demand of high magnification capacity, can stop to overcharge and cross to put, reversible capacity and first efficient all be significantly improved, open up new way in lithium ion battery applications, be fit to commercial exploitation.
Description of drawings
Fig. 1 is that carbon modified material in the embodiment of the present invention 1 is as the first charge-discharge curve of lithium ion battery negative material;
Fig. 2 is that carbon modified material in the embodiment of the present invention 2 is as the first charge-discharge curve of lithium ion battery negative material;
Fig. 3 is that carbon modified material in the embodiment of the present invention 3 is as the first charge-discharge curve of lithium ion battery negative material;
Fig. 4 is that carbon modified material in the embodiment of the present invention 4 is as the first charge-discharge curve of lithium ion battery negative material;
Fig. 5 is that carbon modified material in the embodiment of the present invention 5 is as the first charge-discharge curve of lithium ion battery negative material;
Fig. 6 is that carbon modified material in the embodiment of the present invention 6 is as the first charge-discharge curve of lithium ion battery negative material.
Embodiment
For further illustrating the present invention, illustrate with the following Examples:
Embodiment 1:
1. get the raw materials ready: take native graphite 150g and pitch 10g, ready for use;
2. reinforced: as the raw material of getting ready to be dissolved in organic solvent carbon disulfide, alternately to join while stirring in pressure vessel, continue to stir 3 hours, then added the oil of fearing of total weight 9% in 20 minutes;
3. heat up: the heating that then heats up, in 6 hours, temperature is raised to 500 ℃ and carries out surface modification treatment; The negative pressure 3 hours time of wherein heating up is extracted the volatile matter in above-mentioned substance out;
4. keep constant temperature: keep constant temperature at 500 ℃, 4 hours time, extract simultaneously volatile matter out;
5. naturally cool to room temperature;
6. high temperature is 2000 ℃, and is after carrying out graphitization processing in 24 hours, naturally cooling.The powder that obtains is crossed 200 mesh sieves, and the powder after sieve is modification powdered carbon sample;
Pass into nitrogen in above-mentioned heat treatment process or hydrogen is protected, also can pass into other inert gas such as argon gas or its mist.
Resulting carbon modified material is spherical or elliposoidal, and average grain diameter D50 is 20 μ m, and tap density is in the 1.0g/cc left and right, and the BET specific area is at 2.0m
2/ g left and right, about real density 1.25g/cc, there are a large amount of nano-pores its inside, aperture 0.1 ~ 0.6nm.
Take active material modification powdered carbon and binding agent Kynoar in the ratio (mass ratio) of 94: 6 again, it is dissolved in dimethyl pyrrolidone, repeatedly stir, be coated in equably active material on copper mesh again after binding agent and powdered carbon are mixed, vacuumize 12h, last compressing tablet, weighing require the electrode slice quality at 10～15mg.Electrochemical property test adopts the experimental cell of two electrode structures, and negative material is carbon powder material, lithium sheet just very, and the copper pool is collector; Electrolyte is 1mol/LLiClO
4The solution of/ethylene carbonate (EC)+diethyl carbonate (DEC); Barrier film is Celgard2400.Battery assembles in lower than 5% dry glove box in relative humidity and completes.When requirement discharged and recharged, still in drying box, measuring current density was 0.1mA/cm to battery model
2, charge cutoff voltage is 2.00V, discharge cut-off voltage is 0.001V.
The discharge capacity first of this material is 352.8mAh/g, and first charge-discharge efficiency is 95.7%.
Embodiment 2:
1. get the raw materials ready: take native graphite 100g and pitch 15g, ready for use;
2. reinforced: as the raw material of getting ready to be dissolved in organic solvent carbon disulfide, alternately to join while stirring in pressure vessel, continue to stir 2 hours, then added the oil of fearing of total weight 3% in 10 minutes;
3. heat up: the heating that then heats up, in 7 hours, temperature is raised to 600 ℃ and carries out surface modification treatment; The negative pressure 2 hours time of wherein heating up is extracted the volatile matter in above-mentioned substance out;
4. keep constant temperature: keep constant temperature at 600 ℃, 6 hours time, extract simultaneously volatile matter out;
5. naturally cool to room temperature;
6. high temperature is 2500 ℃, and is after carrying out graphitization processing in 48 hours, naturally cooling.The powder that obtains is crossed 200 mesh sieves, and the powder after sieve is modification powdered carbon sample;
Resulting carbon modified material is spherical or elliposoidal, and average grain diameter D50 is 30 μ m, and tap density is in the 1.5g/cc left and right, and the BET specific area is at 5.0m
2/ g left and right, about real density 2.25g/cc, there are a large amount of nano-pores its inside, aperture 0.1 ~ 0.6nm.
Pass into nitrogen in above-mentioned heat treatment process or hydrogen is protected, also can pass into other inert gas such as argon gas or its mist.
The present embodiment other parts and embodiment 1 are identical.
The discharge capacity first of this material is 355.3mAh/g, and first charge-discharge efficiency is 94.5%.
Embodiment 3:
1. get the raw materials ready: take native graphite 120g and pitch 12g, ready for use;
2. reinforced: as the raw material of getting ready to be dissolved in organic solvent-benzene, alternately to join while stirring in pressure vessel, continue to stir 4 hours, then added the washing oil of total weight 10% in 30 minutes;
3. heat up: the heating that then heats up, in 6.5 hours, temperature is raised to 600 ℃ and carries out surface modification treatment; The negative pressure 3 hours time of wherein heating up is extracted the volatile matter in above-mentioned substance out;
4. keep constant temperature: keep constant temperature at 600 ℃, 5 hours time, extract simultaneously volatile matter out;
5. naturally cool to room temperature;
6. high temperature is 2600 ℃, and is after carrying out graphitization processing in 48 hours, naturally cooling.The powder that obtains is crossed 200 mesh sieves, and the powder after sieve is modification powdered carbon sample;
Resulting carbon modified material is spherical or elliposoidal, and average grain diameter D50 is 10 μ m, and tap density is in the 1.2g/cc left and right, and the BET specific area is at 3.0m
2/ g left and right, about real density 1.85g/cc, there are a large amount of nano-pores its inside, aperture 0.1 ~ 0.6nm.
Pass into nitrogen in above-mentioned heat treatment process or hydrogen is protected, also can pass into other inert gas such as argon gas or its mist.
The present embodiment other parts and embodiment 1 are identical.
Detection learns that the discharge capacity first of this material is 356.3mAh/g, and first charge-discharge efficiency is 94.9%.
Embodiment 4:
1. get the raw materials ready: take native graphite 130g and pitch 15g, ready for use;
2. reinforced: as the raw material of getting ready to be dissolved in organic solvent-benzene dimethylbenzene, alternately to join while stirring in pressure vessel, continue to stir 4 hours, then added the washing oil of total weight 9% in 30 minutes;
3. heat up: the heating that then heats up, in 6.5 hours, temperature is raised to 600 ℃ and carries out surface modification treatment; The negative pressure 3 hours time of wherein heating up is extracted the volatile matter in above-mentioned substance out;
4. keep constant temperature: keep constant temperature at 600 ℃, 5 hours time, extract simultaneously volatile matter out;
5. naturally cool to room temperature;
6. high temperature is 2800 ℃, and is after carrying out graphitization processing in 48 hours, naturally cooling.The powder that obtains is crossed 200 mesh sieves, and the powder after sieve is modification powdered carbon sample;
Resulting carbon modified material is spherical or elliposoidal, and average grain diameter D50 is 20 μ m, and tap density is in the 0.5g/cc left and right, and the BET specific area is at 0.5m
2/ g left and right, about real density 0.8g/cc, there are a large amount of nano-pores its inside, aperture 0.1 ~ 0.6nm.
Pass into nitrogen in above-mentioned heat treatment process or hydrogen is protected, also can pass into other inert gas such as argon gas or its mist.
The present embodiment other parts and embodiment 1 are identical.
The discharge capacity first of this material is 355.2mAh/g, and first charge-discharge efficiency is 95.1%
Embodiment 5:
1. get the raw materials ready: take native graphite 110g and pitch 8g, ready for use;
2. reinforced: as the raw material of getting ready to be dissolved in the organic solvent quinoline, alternately to join while stirring in pressure vessel, continue to stir 2 hours, then added the washing oil of total weight 5% in 10 minutes;
3. heat up: the heating that then heats up, in 7 hours, temperature is raised to 700 ℃ and carries out surface modification treatment; The negative pressure 3 hours time of wherein heating up is extracted the volatile matter in above-mentioned substance out;
4. keep constant temperature: keep constant temperature at 700 ℃, 4 hours time, extract simultaneously volatile matter out;
5. naturally cool to room temperature;
6. high temperature is 2600 ℃, and is after carrying out graphitization processing in 60 hours, naturally cooling.The powder that obtains is crossed 200 mesh sieves, and the powder after sieve is modification powdered carbon sample;
Resulting carbon modified material is spherical or elliposoidal, and average grain diameter D50 is 17 μ m, and tap density is in the 0.8g/cc left and right, and the BET specific area is at 1.5m
2/ g left and right, about real density 1.0g/cc, there are a large amount of nano-pores its inside, aperture 0.1 ~ 0.6nm.
Pass into nitrogen in above-mentioned heat treatment process or hydrogen is protected, also can pass into other inert gas such as argon gas or its mist.
The present embodiment other parts and embodiment 1 are identical.
The discharge capacity first of this material is 356.1mAh/g, and first charge-discharge efficiency is 95.2%
Embodiment 6:
1. get the raw materials ready: take native graphite 100g and pitch 15g, ready for use;
2. reinforced: as the raw material of getting ready to be dissolved in organic solvent carbon disulfide, alternately to join while stirring in pressure vessel, continue to stir 3 hours, then added the washing oil of total weight 4% in 20 minutes;
3. heat up: the heating that then heats up, in 6 hours, temperature is raised to 550 ℃ and carries out surface modification treatment; The negative pressure 3 hours time of wherein heating up is extracted the volatile matter in above-mentioned substance out;
4. keep constant temperature: keep constant temperature at 550 ℃, 4 hours time, extract simultaneously volatile matter out;
5. naturally cool to room temperature;
6. high temperature is 2700 ℃, and is after carrying out graphitization processing in 48 hours, naturally cooling.The powder that obtains is crossed 200 mesh sieves, and the powder after sieve is modification powdered carbon sample;
Resulting carbon modified material is spherical or elliposoidal, and average grain diameter D50 is 18 μ m, and tap density is in the 1.0g/cc left and right, and the BET specific area is at 2.5m
2/ g left and right, about real density 1.5g/cc, there are a large amount of nano-pores its inside, aperture 0.1 ~ 0.6nm.
Pass into nitrogen in above-mentioned heat treatment process or hydrogen is protected, also can pass into other inert gas such as argon gas or its mist.
The present embodiment other parts and embodiment 1 are identical.
The discharge capacity first of this material is 354.7mAh/g, and first charge-discharge efficiency is 95.3%
Table 1 is the electrical performance data of carbon modified material in various embodiments of the present invention.
Table 1
As can be seen from Table 1, the carbon modified material that the present invention makes is take native graphite as main material, take pitch as the modification medium, belong to composite graphite, this material has kept the advantage of native graphite height ratio capacity, and efficient is low first to have overcome simultaneously the native graphite cycle performance, the shortcoming that cycle performance is relatively poor, possess gram volume high, compacted density is high, and specific area is little, processing characteristics is good, the advantages such as good cycle.For the preparation of lithium ion battery, have very high electrical property, its first efficient and cycle performance all be significantly improved, can satisfy lithium ion battery to the demand of high power capacity and high cycle life, can stop to overcharge and cross and put, be well suited for for high-energy-density density lithium ion battery.
Above-described embodiment is described the preferred embodiment of the present invention; be not that scope of the present invention is limited; design under the prerequisite of spirit not breaking away from the present invention; various distortion and improvement that the common engineers and technicians in this area make technical scheme of the present invention all should fall in the definite protection range of claims of the present invention.
Claims (9)
1. high-capacity lithium-ion secondary battery negative pole Carbon Materials, is characterized in that: made by native graphite and pitch that weight ratio is 6 ~ 30:1.
2. high-capacity lithium-ion secondary battery negative pole Carbon Materials according to claim 1, it is characterized in that: the particle diameter of described native graphite is 8～27 μ m, and specific area is less than or equal to 5m
2/ g; Described pitch is coal tar pitch or petroleum asphalt.
3. high-capacity lithium-ion secondary battery negative pole Carbon Materials according to claim 1, it is characterized in that: described high-capacity lithium-ion secondary battery negative pole Carbon Materials is native graphite and pitch to be dissolved in carry out liquid-phase dehydration after organic solvent in pressure vessel again and process, then by coating modification, low-temperature setting, charing, finally by making after high-temperature heat treatment, cooling, screening.
4. high-capacity lithium-ion secondary battery negative pole Carbon Materials according to claim 3, it is characterized in that: the described carbon modified material of making is spherical or elliposoidal, average grain diameter D50 is 2～28 μ m, and tap density is between 0.7～1.5g/cc, and the BET specific area is at 1.0～5.0m
2Between/g, real density 0.9～2.20g/cc, there is nano-pore its inside, aperture 0.2～0.6nm.
5. the preparation method of the described high-capacity lithium-ion secondary battery negative pole of claim 1-4 any one Carbon Materials, it is characterized in that: step is as follows:
1. get the raw materials ready: with native graphite and the pitch ratio by weight 6～30:1, ready for use;
2. reinforced: as the raw material of getting ready to be dissolved in organic solvent, alternately to join while stirring in pressure vessel, continue to stir 1～3 hour, then added the reaction promoter of total weight 5%～20% in 8～25 minutes;
3. heat up: the heating that then heats up, in 6～7 hours, temperature is raised to 500～700 ℃; The negative pressure 1～4 hour time of wherein heating up is extracted the volatile matter in above-mentioned substance out;
4. keep constant temperature: keep constant temperature at 500～700 ℃, 5～8 hours time, extract simultaneously volatile matter out;
5. naturally cool to room temperature;
6. 2000～2800 ℃ of high temperature carry out graphitization processing;
Wherein, 6. 5. 4. 3. described step all carry out under anti-oxidation environment.
6. preparation method according to claim 5, it is characterized in that: described anti-oxidation environment is to extract in non-negative pressure to pass into inert gas or hydrogen under state.
7. preparation method according to claim 5, it is characterized in that: described inert gas is nitrogen, its flow is 0.5～2m
3/ h.
8. preparation method according to claim 5, it is characterized in that: described reaction promoter is cycloalkane and/or aromatic solvent.
9. preparation method according to claim 5 is characterized in that: described aromatic solvent is selected from fears any in oil and washing oil.
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| CN103346294A (en) * | 2013-06-24 | 2013-10-09 | 方大炭素新材料科技股份有限公司 | Preparation method of artificial graphite cathode material |
| CN103647082A (en) * | 2013-12-24 | 2014-03-19 | 中国船舶重工集团公司第七一二研究所 | Preparation method of lithium ion secondary battery hard-carbon microsphere negative electrode material |
| CN105047860A (en) * | 2014-12-19 | 2015-11-11 | 上海杉杉科技有限公司 | Battery cathode TiO2/intermediate-phase microsphere composite material and preparation method thereof |
| CN107871859A (en) * | 2016-09-27 | 2018-04-03 | 上海杉杉科技有限公司 | A kind of preparation method of Hyperhemodynamics lithium ion battery negative material |
| CN109599546A (en) * | 2018-12-05 | 2019-04-09 | 中南大学 | Asphalt carbon-coated natural mixed graphite material and method for preparing lithium ion battery cathode by using same |
| CN110880600A (en) * | 2019-11-21 | 2020-03-13 | 广东东岛新能源股份有限公司 | Negative electrode material with high temperature resistance, preparation method thereof and application thereof in lithium ion battery |
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| CN105047860A (en) * | 2014-12-19 | 2015-11-11 | 上海杉杉科技有限公司 | Battery cathode TiO2/intermediate-phase microsphere composite material and preparation method thereof |
| CN107871859A (en) * | 2016-09-27 | 2018-04-03 | 上海杉杉科技有限公司 | A kind of preparation method of Hyperhemodynamics lithium ion battery negative material |
| CN109599546A (en) * | 2018-12-05 | 2019-04-09 | 中南大学 | Asphalt carbon-coated natural mixed graphite material and method for preparing lithium ion battery cathode by using same |
| CN110880600A (en) * | 2019-11-21 | 2020-03-13 | 广东东岛新能源股份有限公司 | Negative electrode material with high temperature resistance, preparation method thereof and application thereof in lithium ion battery |
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Application publication date: 20130508 |