CN105293467A - Phenolic resin/coal tar pitch composite-base modified hard carbon negative electrode material and preparation method and application thereof - Google Patents
Phenolic resin/coal tar pitch composite-base modified hard carbon negative electrode material and preparation method and application thereof Download PDFInfo
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- CN105293467A CN105293467A CN201510685624.6A CN201510685624A CN105293467A CN 105293467 A CN105293467 A CN 105293467A CN 201510685624 A CN201510685624 A CN 201510685624A CN 105293467 A CN105293467 A CN 105293467A
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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 phenolic resin/coal tar pitch composite-base modified hard carbon negative electrode material and a preparation method and application thereof, and belongs to the field of electrochemistry. According to the phenolic resin/coal tar pitch composite-base modified hard carbon negative electrode material, phenolic resin and coal tar pitch serve as hard carbon precursors, and the mass ratio of the phenolic resin to the coal tar pitch is 2:1-4. The phenolic resin is modified through phosphoric acid, and the mass ratio of the phosphoric acid to the phenolic resin is 1-5:10. The particle size range of the hard carbon negative electrode material is 10-50 microns. The primary coulombic efficiency of the negative electrode material under the 0.5 C multiplying power is 80.55%, under the 2 C multiplying power, the volume is kept to be about 221 mAh/g after recycling is conducted 300 times, the volume does not greatly differ from the volume under the 0.5 C multiplying power and the 1 C multiplying power, and it shows that good volume maintaining performance and coulombic efficiency are achieved.
Description
Technical field
The present invention relates to electrochemical field, particularly a kind of resol/coal-tar pitch composite base modification hard carbon cathode material, its preparation method and application thereof.
Background technology
Graphite-like carbon negative pole material have electropotential low, have extended cycle life, the good and advantage such as cheap of security, become the main negative material of current commercial Li-ion battery.
But graphite negative electrodes material is due to its laminate structure, poor with the consistency of electrolytic solution, in the process of discharge and recharge, easily there is lyate ion embed altogether and cause structure deteriorate, thus affect cyclical stability and the coulombic efficiency of graphite cathode material, especially reduce the high rate performance of graphite cathode material, the lasting large current discharging capability etc. required by large-sized power battery can not be met.
With graphite-phase ratio, hard carbon (HC) has isotropic constitutional features, and interlamellar spacing is larger, lithium ion diffusion can be accelerated, meanwhile, hard carbon material cycle performance and the feature such as high rate performance is better, cost is low, make it in power-type lithium ion battery, again receive the concern of people.
Scientific research personnel is is researching and developing new lithium cell cathode material.The patent of invention that publication number is " CN102820455 " discloses a kind of lithium ion battery hard carbon cathode material and preparation method thereof.In this invention, be doped with silicon and phosphorus in described hard carbon cathode material, silicon precursor: phosphorus presoma: the mass ratio of hard carbon presoma is 1:0.1-5:5-30.This negative material significantly improves the loading capacity first (reaching 550.8mAh/g) of negative material, first charge-discharge efficiency (reaching 80.9%) and coulombic efficiency first, and has significantly laughed at irreversible capacity.
Development of new hard carbon cathode material is this area urgent problem to promote battery performance further.
Summary of the invention
In order to make up above deficiency, the invention provides a kind of resol/coal-tar pitch composite base modification hard carbon cathode material, its preparation method and application thereof.
Technical scheme of the present invention is:
A kind of resol/coal-tar pitch composite base modification hard carbon cathode material, hard carbon presoma is resol and coal-tar pitch, and the mass ratio of resol and coal-tar pitch is 2:1-4; The described phosphoric acid that is modified as carries out modification to resol, and the mass ratio of phosphoric acid and resol is 1-5:10; The particle size range of described hard carbon cathode material is 10-50 micron.
Preferably, the mass ratio of phosphoric acid and resol is 2-3:10.
The preparation method of described resol/coal-tar pitch composite base modification hard carbon cathode material, comprises step:
1) resol is dissolved in dehydrated alcohol, adds phosphoric acid, be stirred to resol and dissolve completely;
2) get coal-tar pitch, and add washing oil in coal-tar pitch, at 150-180 DEG C, coal-tar pitch is dissolved completely, then add step 1) gained solution, be stirred to when becoming floss and pour in valve bag, put into the baking oven Procuring 5-15h of 60-80 DEG C;
3) Procuring gained sample is put into tube furnace, under an argon atmosphere with the temperature rise rate of 0.5-10 DEG C/min, charing 1-10h is carried out under 800-1500 °, sample after charing in ball mill with 300-800r/min ball milling 5-10h, then cross 200-600 mesh sieve, obtain resol/coal-tar pitch composite base modification hard carbon cathode material.
Preferably, the preparation method of described resol/coal-tar pitch composite base modification hard carbon cathode material, carbonization temperature is 900-1200 DEG C, and carbonization time is 3-5h.
Preferably, the preparation method of described resol/coal-tar pitch composite base modification hard carbon cathode material, the sample after charing in ball mill with 500-600r/min ball milling 6-7h.
Described resol/the application of coal-tar pitch composite base modification hard carbon cathode material in lithium cell cathode material.
Described resol/coal-tar pitch composite base modification hard carbon cathode material, as the application method of cathode of lithium battery, comprises step:
1) prepare some Copper Foils, Copper Foil is placed in dilute hydrochloric acid solution ultrasonic cleaning 3-5min, then Copper Foil is placed in acetone soln ultrasonic cleaning 3-5min; From acetone soln, take out Copper Foil, use deionized water and alcohol washes respectively, drying is weighed;
2) take N-Methyl pyrrolidone as the poly(vinylidene fluoride) solution that solvent configures 80-200mg/mL, be 90-95:1-3:2-8 mixing in mass ratio by resol/coal-tar pitch composite base modification hard carbon cathode material, carbon black, poly(vinylidene fluoride), grinding makes it mix, and prepares electrode slurry;
3) electrode slurry of preparation is uniformly coated on the Copper Foil processed, vacuum-drying at 100-120 DEG C, obtained electrode slice;
4) with the Copper Foil processed, the electrode slice prepared by step 3) is encased up and down, be put in smooth, rigidity, clean mould, make type at the pressure of 8-12Mpa, then in the glove box of applying argon gas, assemble button half-cell.
Preferably, resol described in 7/coal-tar pitch composite base modification hard carbon cathode material is as the application method of cathode of lithium battery, and in step 1), the diameter of Copper Foil is 8mm, and thickness is 10-20 micron.
Beneficial effect of the present invention is:
The preparation method of resol of the present invention/coal-tar pitch composite base modification hard carbon cathode material is simple, and mild condition is controlled.Resol/coal-tar pitch composite base modification the hard carbon cathode material of preparation, chemical property is good, and under 0.5C multiplying power, coulombic efficiency is 80.55% first, and under 2C multiplying power after 300 circulations, capacity remains on about 221mAh/g.
Resol/coal-tar pitch composite base modification the hard carbon cathode material of preparation is as ion cathode material lithium, and high rate performance significantly improves, and has Research Prospects widely in power cell practical application area.
Accompanying drawing explanation
In order to be illustrated more clearly in the embodiment of the present invention or technical scheme of the prior art, be briefly described to the accompanying drawing used required in embodiment or description of the prior art below, apparently, accompanying drawing in the following describes is only some embodiments of the present invention, for those of ordinary skill in the art, under the prerequisite not paying creative work, other accompanying drawing can also be obtained according to these accompanying drawings.
Fig. 1 is the SEM figure of the embodiment of the present invention 2 gained resol/coal-tar pitch composite base modification hard carbon cathode material;
Fig. 2 is the high rate performance curve of the embodiment of the present invention 2 gained resol/coal-tar pitch composite base modification hard carbon cathode material.
Embodiment
Embodiment 1
Take 100g resol stirring and dissolving in 150mL dehydrated alcohol, add 10g phosphoric acid, stir 3h, resol is dissolved completely.In the beaker of 500mL, add 50g coal-tar pitch, add washing oil, under 180 ° of C, make it dissolve completely, add the modified phenolic resins ethanol solution of above-mentioned preparation, continue to stir, become and pour in valve bag during floss, put into 60 ° of C baking oven Procuring 10h.
Sample after Procuring is put into tube furnace, under an argon atmosphere with the temperature rise rate of 3 DEG C/min, under 800 ° of C, carry out charing 3h, the sample after charing in ball mill with 400r/min ball milling 10h, then cross 400 mesh sieves, obtain resol/coal-tar pitch composite base modification hard carbon cathode material.
Embodiment 2
Take 100g resol stirring and dissolving in 150mL dehydrated alcohol, add 20g phosphoric acid, stir 3h, resol is dissolved completely.In the beaker of 500mL, add 100g coal-tar pitch, add washing oil, under 180 ° of C, make it dissolve completely, add the modified phenolic resins ethanol solution of above-mentioned preparation, continue to stir, become and pour in valve bag during floss, put into 60 ° of C baking oven Procuring 8h.
Sample after Procuring is put into tube furnace, under an argon atmosphere with the temperature rise rate of 5 DEG C/min, charing 3h is carried out under 1000 ° of C, sample after charing in ball mill with 400r/min ball milling 10h, then cross 400 mesh sieves, obtain resol/coal-tar pitch composite base modification hard carbon cathode material.
Embodiment 3
Take 100g resol stirring and dissolving in 150mL dehydrated alcohol, add 20g phosphoric acid, stir 3h, resol is dissolved completely.In the beaker of 500mL, add 150g coal-tar pitch, add washing oil, under 180 ° of C, make it dissolve completely, add the modified phenolic resins ethanol solution of above-mentioned preparation, continue to stir, become and pour in valve bag during floss, put into 60 ° of C baking oven Procuring 12h.
Sample after Procuring is put into tube furnace, under an argon atmosphere with the temperature rise rate of 5 DEG C/min, under 1200 ° of C, carry out charing 5h, the sample after charing in ball mill with 600r/min ball milling 6h, then cross 400 mesh sieves, obtain resol/coal-tar pitch composite base modification hard carbon cathode material.
Embodiment 4
Take 100g resol stirring and dissolving in 150mL dehydrated alcohol, add 40g phosphoric acid, stir 3h, resol is dissolved completely.In the beaker of 500mL, add 200g coal-tar pitch, add washing oil, under 180 ° of C, make it dissolve completely, add the modified phenolic resins ethanol solution of above-mentioned preparation, continue to stir, become and pour in valve bag during floss, put into 60 ° of C baking oven Procuring 10h.
Sample after Procuring is put into tube furnace, under an argon atmosphere with the temperature rise rate of 5 DEG C/min, under 1200 ° of C, carry out charing 3h, the sample after charing in ball mill with 500r/min ball milling 7h, then cross 400 mesh sieves, obtain resol/coal-tar pitch composite base modification hard carbon cathode material.
Embodiment 5
Take 100g resol stirring and dissolving in 150mL dehydrated alcohol, add 30g phosphoric acid, stir 3h, resol is dissolved completely.In the beaker of 500mL, add 100g coal-tar pitch, add washing oil, under 180 ° of C, make it dissolve completely, add the modified phenolic resins ethanol solution of above-mentioned preparation, continue to stir, become and pour in valve bag during floss, put into 60 ° of C baking oven Procuring 10h.
Sample after Procuring is put into tube furnace, under an argon atmosphere with the temperature rise rate of 5 DEG C/min, under 900 ° of C, carry out charing 5h, the sample after charing in ball mill with 500r/min ball milling 6h, then cross 2400 mesh sieves, obtain resol/coal-tar pitch composite base modification hard carbon cathode material.
Embodiment 6
1) prepare diameter be 8mm, thickness be 15um Copper Foil several; Copper Foil is placed in dilute hydrochloric acid solution ultrasonic cleaning 3-5min, then Copper Foil is placed in acetone soln ultrasonic cleaning 3-5min; From acetone soln, take out Copper Foil, use deionized water and washes of absolute alcohol respectively, then dry, weigh;
2) take N-Methyl pyrrolidone as the poly(vinylidene fluoride) solution that solvent configures 100mg/mL, be 93:2:5 mixing in mass ratio by resol/coal-tar pitch composite base modification hard carbon cathode material, carbon black, poly(vinylidene fluoride), grinding makes it mix, and prepares electrode slurry;
3) electrode slurry of preparation is uniformly coated on the Copper Foil processed, vacuum-drying 24h at 120 DEG C, obtained electrode slice;
4) with the Copper Foil processed, the electrode slice prepared by step 3) is encased up and down, be put in smooth, rigidity, clean mould, make type at the pressure of 10Mpa, then in the glove box of applying argon gas, assemble button half-cell.
Utilize LAND battery test system, charge-discharge performance test (result as shown in Figure 2) is carried out with different multiplying, as can be seen from the figure resol/coal-tar pitch composite base modification hard carbon cathode material under 0.5C multiplying power first coulombic efficiency be 80.55%, under 2C multiplying power after 300 circulations, capacity remains on about 221mAh/g, be more or less the same with the capacity under 0.5C, 1C multiplying power, illustrate that there is good capacity retention energy and coulombic efficiency.There is excellent high rate charge-discharge performance compared with graphite type material, be applicable to being applied to power battery cathode material.
Claims (8)
1. resol/coal-tar pitch composite base modification hard carbon cathode material, is characterized in that: hard carbon presoma is resol and coal-tar pitch, the mass ratio of resol and coal-tar pitch is 2:1-4; The described phosphoric acid that is modified as carries out modification to resol, and the mass ratio of phosphoric acid and resol is 1-5:10; The particle size range of described hard carbon cathode material is 10-50 micron.
2. resol/coal-tar pitch composite base modification hard carbon cathode material as claimed in claim 1, is characterized in that: the mass ratio of phosphoric acid and resol is 2-3:10.
3. the preparation method of resol/coal-tar pitch composite base modification hard carbon cathode material as claimed in claim 1, is characterized in that, comprise step:
1) resol is dissolved in dehydrated alcohol, adds phosphoric acid, be stirred to resol and dissolve completely;
2) get coal-tar pitch, and add washing oil in coal-tar pitch, at 150-180 DEG C, coal-tar pitch is dissolved completely, then add step 1) gained solution, be stirred to when becoming floss and pour in valve bag, put into the baking oven Procuring 5-15h of 60-80 DEG C;
3) Procuring gained sample is put into tube furnace, under an argon atmosphere with the temperature rise rate of 0.5-10 DEG C/min, charing 1-10h is carried out under 800-1500 °, sample after charing in ball mill with 300-800r/min ball milling 5-10h, then cross 200-600 mesh sieve, obtain resol/coal-tar pitch composite base modification hard carbon cathode material.
4. the preparation method of resol/coal-tar pitch composite base modification hard carbon cathode material as claimed in claim 3, it is characterized in that: carbonization temperature is 900-1200 DEG C, carbonization time is 3-5h.
5. the preparation method of resol/coal-tar pitch composite base modification hard carbon cathode material as claimed in claim 3, is characterized in that: the sample after charing in ball mill with 500-600r/min ball milling 6-7h.
6. resol/the application of coal-tar pitch composite base modification hard carbon cathode material in lithium cell cathode material as claimed in claim 1.
7. resol/coal-tar pitch composite base modification hard carbon cathode material, as the application method of cathode of lithium battery, is characterized in that, comprises step as claimed in claim 1:
1) prepare some Copper Foils, Copper Foil is placed in dilute hydrochloric acid solution ultrasonic cleaning 3-5min, then Copper Foil is placed in acetone soln ultrasonic cleaning 3-5min; From acetone soln, take out Copper Foil, use deionized water and alcohol washes respectively, drying is weighed;
2) take N-Methyl pyrrolidone as the poly(vinylidene fluoride) solution that solvent configures 80-200mg/mL, be 90-95:1-3:2-8 mixing in mass ratio by resol/coal-tar pitch composite base modification hard carbon cathode material, carbon black, poly(vinylidene fluoride), grinding makes it mix, and prepares electrode slurry;
3) electrode slurry of preparation is uniformly coated on the Copper Foil processed, vacuum-drying at 100-120 DEG C, obtained electrode slice;
4) with the Copper Foil processed, the electrode slice prepared by step 3) is encased up and down, be put in smooth, rigidity, clean mould, make type at the pressure of 8-12Mpa, then in the glove box of applying argon gas, assemble button half-cell.
8. resol/coal-tar pitch composite base modification hard carbon cathode material is as the application method of cathode of lithium battery as claimed in claim 7, and it is characterized in that: in step 1), the diameter of Copper Foil is 8mm, thickness is 10-20 micron.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201510685624.6A CN105293467A (en) | 2015-10-21 | 2015-10-21 | Phenolic resin/coal tar pitch composite-base modified hard carbon negative electrode material and preparation method and application thereof |
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| CN201510685624.6A CN105293467A (en) | 2015-10-21 | 2015-10-21 | Phenolic resin/coal tar pitch composite-base modified hard carbon negative electrode material and preparation method and application thereof |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107256948A (en) * | 2017-04-17 | 2017-10-17 | 方万里 | A kind of High Performance Phenolic Resins charcoal bag covers spherical graphite negative material preparation method |
| CN109911878A (en) * | 2017-12-13 | 2019-06-21 | 宁波杉杉新材料科技有限公司 | Modified hard carbon cathode material of high capacity pitch/epoxy resin-matrix and preparation method thereof |
| CN111342035A (en) * | 2020-03-11 | 2020-06-26 | 西安越遴新材料研究院有限公司 | Method for modifying silicon-carbon composite negative electrode by asphalt modification process derivative |
| CN113880068A (en) * | 2021-09-29 | 2022-01-04 | 蜂巢能源科技有限公司 | Hard carbon composite material and preparation method and application thereof |
| CN115558306A (en) * | 2021-07-02 | 2023-01-03 | 湖南中科星城石墨有限公司 | Isotropic asphalt material and preparation method and application thereof |
| CN116514094A (en) * | 2022-11-28 | 2023-08-01 | 昆明理工大学 | Preparation method and application of battery anode carbon material |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107256948A (en) * | 2017-04-17 | 2017-10-17 | 方万里 | A kind of High Performance Phenolic Resins charcoal bag covers spherical graphite negative material preparation method |
| CN109911878A (en) * | 2017-12-13 | 2019-06-21 | 宁波杉杉新材料科技有限公司 | Modified hard carbon cathode material of high capacity pitch/epoxy resin-matrix and preparation method thereof |
| CN111342035A (en) * | 2020-03-11 | 2020-06-26 | 西安越遴新材料研究院有限公司 | Method for modifying silicon-carbon composite negative electrode by asphalt modification process derivative |
| CN115558306A (en) * | 2021-07-02 | 2023-01-03 | 湖南中科星城石墨有限公司 | Isotropic asphalt material and preparation method and application thereof |
| CN115558306B (en) * | 2021-07-02 | 2023-10-17 | 湖南中科星城石墨有限公司 | Isotropic asphalt material and preparation method and application thereof |
| CN113880068A (en) * | 2021-09-29 | 2022-01-04 | 蜂巢能源科技有限公司 | Hard carbon composite material and preparation method and application thereof |
| CN116514094A (en) * | 2022-11-28 | 2023-08-01 | 昆明理工大学 | Preparation method and application of battery anode carbon material |
| CN116514094B (en) * | 2022-11-28 | 2023-10-03 | 昆明理工大学 | Preparation method and application of battery anode carbon material |
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