CN105185963A - High-performance nitrogen-rich carbon composite electrode material and preparation method thereof - Google Patents
High-performance nitrogen-rich carbon composite electrode material and preparation method thereof Download PDFInfo
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- CN105185963A CN105185963A CN201510563682.1A CN201510563682A CN105185963A CN 105185963 A CN105185963 A CN 105185963A CN 201510563682 A CN201510563682 A CN 201510563682A CN 105185963 A CN105185963 A CN 105185963A
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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
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/362—Composites
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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
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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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
- H01M4/133—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
- 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
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
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- 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 present invention belongs to the technical field of the preparation of lithium-ion battery electrode materials, and specifically discloses a nitrogen-rich carbon composite electrode material and a preparation method thereof. The preparation method comprises the following steps: firstly, uniformly dispersing asphalt and melamine in a heating reactor at a high speed to obtain a mixture, cooling and then crushing the mixture, then calcining the mixture in an inert atmosphere, and performing ball milling screening and magnet removal to obtain the high-performance nitrogen-rich carbon composite electrode material. According to the present invention, the preparation process is simple, low in price and suitable for industrial production; in the aspect of material design, the nitrogen doping is used for improving excellent electrochemical performance of carbon composite materials, and hard carbon generated by the carbonization of melamine and soft carbon generated by the carbonization of asphalt are organically combined to generate a pore-rich hierarchical structure composite material. The prepared material has good charge-discharge reaction reversibility, excellent cycle performance and many other advantages, and can meet the requirements of high-capacity and high-rate lithium-ion batteries for the electrode materials.
Description
Technical field
The present invention relates to the preparing technical field of lithium ion battery electrode material, be specifically related to a kind of high-performance rich nitrogen type carbon composite electrode material and preparation method thereof.
Background technology
Energy crisis and the environmental crisis in the whole world force people to develop new energy and material to replace fossil feedstock.Lithium ion battery in secondary cell has the feature such as high voltage, large specific capacity, has become a class novel energy-storing power supply of people's first-selection.High-energy-density, high cyclical stability, the lithium ion battery of long life are electric automobile and the ultimate pursuit of other electronic equipments.In current business-like lithium ion battery negative material, based on native graphite and hard carbon graphitized material, but the layer structure of native graphite graphite layers in battery charge and discharge process can be peeling and form new surface and increase irreversible capacity loss, causes that its theoretical specific capacity is low, irreversible capacity is high, multiplying power and cycle performance poor.Although also there is above-mentioned shortcoming in hard carbon material, but its high rate charge-discharge performance is better than native graphite, therefore on large-sized power plant and power vehicle, adopt hard carbon material more, but the shortcomings such as current hard carbon material still exists that capacity is low, capacity attenuation is fast, cyclical stability is poor, complicated process of preparation, energy consumption height poor with compatibility of electrolyte.
In order to overcome above-mentioned defect, will design there is special construction carbon composite to meet high power capacity, powerful lithium ion battery to the demand of electrode material.The such as combination of hard carbon material and soft material with carbon element, easy formation classification material with carbon element structure, and the pore passage structure of the carbon composite of hierarchy extremely will be conducive to the transmission of electrons/ions, also the deintercalation of lithium ion and the infiltration of electrolyte is conducive to, effectively coulombic efficiency be can improve, the site of deintercalate lithium ions and the concertedness of electrolyte effectively increased.For another example by the atom of electron deficient, as nitrogen, phosphorus, boron are introduced in carbon structure, effectively can improve the surface polarity of carbon, strengthen transmission performance and the chemical reactivity of electronics.
The present invention starts with from two aspects, and to construct the hierarchy that new hard soft carbon combines, and in carbon-coating structure, embed hetero-atom be core, for the purpose of the chemical property promoting composite material by cooperative effect.We wish that the improvement of technique can obtain that preparation temperature is low, discharge and recharge reaction good reversibility, cycle performance is excellent, product cost is high, the simple high-performance of preparation process condition rich nitrogen type carbon composite electrode material.
Summary of the invention
The object of the invention is to overcome in carbon negative pole material prepared by existing method that ubiquitous structural stability is poor, capacity is low, cyclical stability is poor, preparation temperature is high, high in cost of production defect, provide a kind of high-performance rich nitrogen type carbon composite electrode material and preparation method thereof, the method has the plurality of advantages such as process conditions are simple, preparation temperature is low, obtained rich nitrogen type carbon composite electrode material discharge and recharge reaction good reversibility, cycle performance is excellent, cost is low, applicable industrial production.
The object of the invention is to be achieved by the following technical programs.
A kind of high-performance rich nitrogen type carbon composite electrode material and preparation method thereof, step is as follows:
(1) pitch and melamine are added in the reactor with dispersed with stirring device, be heated to more than asphalt softening point 20 ~ 30 DEG C, dispersed with stirring, and maintain this temperature 1 hour, pitch is fully mixed with melamine.Broken after cooling.
Described pitch is coal tar pitch or petroleum asphalt, and its softening point is all 40 ~ 120 DEG C of scopes;
The mass ratio of described pitch and melamine is 1:x(0 < x≤2);
The mixing speed stirring pitch and melamine in described heating process is 3000 revs/min.
(2) by the solid matter of fragmentation, put into graphite crucible, be heated to 900 ~ 1100 DEG C from room temperature under an inert atmosphere and maintain this temperature 6 ~ 10 hours, obtain rich nitrogen type carbon composite head product.
Described inert atmosphere conditions is nitrogen or argon gas atmosphere.
The speed of described intensification is 3 ~ 5 DEG C/min.
(3) in vibration at high speed ball mill, 4 hours are processed after rich nitrogen type carbon composite head product step (2) obtained mixes with the lithium salts of certain mass, the setting speed of vibration at high speed ball mill is 1500 revs/min, cross 200 mesh sieves and except after magnetic, namely obtain high-performance rich nitrogen type carbon composite electrode material.
Described lithium salts is lithium carbonate or lithium fluoride.
The mass ratio of described rich nitrogen type carbon composite head product and lithium salts is 100:y(0.5 < y≤3).
compared with prior art, the advantage of the inventive method and obtained rich nitrogen type carbon composite electrode material and beneficial effect are:
The present invention is a kind of preparation method of high activity lithium ion battery negative material, first pitch and melamine are uniformly dispersed in heating reactor high speed by the method, broken after cooling, then calcine in an inert atmosphere, high-performance rich nitrogen type carbon composite electrode material can be obtained after ball milling sieves and removes magnetic.Asphalt carbonization to form soft material with carbon element, and mainly forms hard carbon material after melamine carbonization, easily form graded structure material with carbon element after compound carbonizing.Due to adding of nitrogen content height melamine, so form rich nitrogen type carbon composite.Nitrogen-atoms is as electron rich element, and its electronegativity is higher than carbon, and nitrogen atom doping can keep lattice structure and the duct of carbon, and due to the lattice position of nitrogen-atoms Substitute For Partial carbon, the extra lone pair electrons of nitrogen-atoms can give SP
2the negative electrical charge of the carbon skeleton extended system of hydridization, thus effectively improve the surface polarity of carbon, strengthen transmission performance and the chemical reactivity of electronics.The pore passage structure of the carbon composite of hierarchy will extremely be conducive to the transmission of electrons/ions, also the deintercalation of lithium ion and the infiltration of electrolyte is conducive to, the lithium salts simultaneously added is the collaborative quick formation impelling SEI film also, effectively coulombic efficiency be can improve, the site of deintercalate lithium ions and the concertedness of electrolyte effectively increased.It is simple, cheap that the present invention shows technique in preparation technology, is applicable to industrial feature; Design of material not only utilizes N doping promote the chemical property of carbon composite excellence, the soft carbon that the hard carbon making again melamine carbonization produce and asphalt carbonization produce organically combines and produces the abundant hierarchy composite material in duct.The plurality of advantages such as the preparation process condition of material is simple, preparation temperature is low, discharge and recharge reaction good reversibility, cycle performance is excellent, cost is low, applicable industrial production, can meet high power capacity, powerful lithium ion battery to the demand of electrode material.
Accompanying drawing explanation
The scanning electron microscopic picture of the product of Fig. 1 obtained by embodiment 1.
The CV curve of the product of Fig. 2 obtained by embodiment 1.
The product cycle life under 0.2C condition of Fig. 3 obtained by embodiment 1 ~ 5.
The charge-discharge magnification curve of the product of Fig. 4 obtained by embodiment 1.
Embodiment
Applicant will be described in further detail the inventive method in conjunction with specific embodiments below, and object is to enable those skilled in the art be expressly understood the present invention.Following examples should not be understood to the restriction to claims of the present invention request protection range in any degree.Professional and technical personnel in the field prepare similar composite material also in the restriction of claims of the present invention request protection range by the amendment of this thinking.Coal tar pitch in the present invention, petroleum asphalt are changed to coal tar, emulsified asphalt or other modified pitch, all in the restriction of claims of the present invention request protection range.This electrode material is used as electrode material in sodium-ion battery or ultracapacitor, all in the restriction of claims of the present invention request protection range.
embodiment 1
A kind of high-performance rich nitrogen type carbon composite electrode material and preparation method thereof, described method step is as follows:
Be that the coal tar pitch of 120 DEG C and 600g analyze in the reactor that pure melamine adds with dispersed with stirring device by 1000g softening temperature, be heated to 150 DEG C, dispersed with stirring, mixing speed is 3000 revs/min, and maintain this temperature 1 hour, pitch is fully mixed with melamine.Broken after cooling.By the solid matter of fragmentation, put into graphite crucible, rise to 1100 DEG C from room temperature in a nitrogen atmosphere and keep this temperature 6 hours (speed of intensification is 5 DEG C/min).By the material and the lithium carbonate that obtain in mass ratio 100:0.5 in vibration at high speed ball mill, process 4 hours after mix, the setting speed of vibration at high speed ball mill is 1500 revs/min, crosses after 200 mesh sieves also remove magnetic, namely obtains high-performance richness nitrogen type carbon composite electrode material.
embodiment 2
A kind of high-performance rich nitrogen type carbon composite electrode material and preparation method thereof, described method step is as follows:
Be that the coal tar pitch of 45 DEG C and 1000g analyze in the reactor that pure melamine adds with dispersed with stirring device by 1000g softening temperature, be heated to 75 DEG C, dispersed with stirring, mixing speed is 3000 revs/min, and maintain this temperature 1 hour, pitch is fully mixed with melamine.Broken after cooling.By the solid matter of fragmentation, put into graphite crucible, rise to 900 DEG C from room temperature in a nitrogen atmosphere and keep this temperature 10 hours (speed of intensification is 5 DEG C/min).By the material and the lithium fluoride that obtain in mass ratio 100:0.5 in vibration at high speed ball mill, process 4 hours after mix, the setting speed of vibration at high speed ball mill is 1500 revs/min, crosses after 200 mesh sieves also remove magnetic, namely obtains high-performance richness nitrogen type carbon composite electrode material.
embodiment 3
A kind of high-performance rich nitrogen type carbon composite electrode material and preparation method thereof, described method step is as follows:
Be that the petroleum asphalt of 80 DEG C and 600g analyze in the reactor that pure melamine adds with dispersed with stirring device by 1000g softening temperature, be heated to 100 DEG C, dispersed with stirring, mixing speed is 3000 revs/min, and maintain this temperature 1 hour, pitch is fully mixed with melamine.Broken after cooling.By the solid matter of fragmentation, put into graphite crucible, rise to 1000 DEG C from room temperature in a nitrogen atmosphere and keep this temperature 6 hours (speed of intensification is 5 DEG C/min).By the material and the lithium carbonate that obtain in mass ratio 100:1 in vibration at high speed ball mill, process 4 hours after mix, the setting speed of vibration at high speed ball mill is 1500 revs/min, crosses after 200 mesh sieves also remove magnetic, namely obtains high-performance richness nitrogen type carbon composite electrode material.
embodiment 4
A kind of high-performance rich nitrogen type carbon composite electrode material and preparation method thereof, described method step is as follows:
Be that the petroleum asphalt of 95 DEG C and 2000g analyze in the reactor that pure melamine adds with dispersed with stirring device by 1000g softening temperature, be heated to 125 DEG C, dispersed with stirring, mixing speed is 3000 revs/min, and maintain this temperature 1 hour, pitch is fully mixed with melamine.Broken after cooling.By the solid matter of fragmentation, put into graphite crucible, keep this temperature 10 hours (speed of intensification is 5 DEG C/min) from room temperature to 1100 DEG C under an argon atmosphere.By the material and the lithium carbonate that obtain in mass ratio 100:3 in vibration at high speed ball mill, process 4 hours after mix, the setting speed of vibration at high speed ball mill is 1500 revs/min, crosses after 200 mesh sieves also remove magnetic, namely obtains high-performance richness nitrogen type carbon composite electrode material.
embodiment 5
A kind of high-performance rich nitrogen type carbon composite electrode material and preparation method thereof, described method step is as follows:
Be that the petroleum asphalt of 80 DEG C and 200g analyze in the reactor that pure melamine adds with dispersed with stirring device by 1000g softening temperature, be heated to 110 DEG C, dispersed with stirring, mixing speed is 3000 revs/min, and maintain this temperature 1 hour, pitch is fully mixed with melamine.Broken after cooling.By the solid matter of fragmentation, put into graphite crucible, keep this temperature 6 hours (speed of intensification is 5 DEG C/min) from room temperature to 900 DEG C in a nitrogen atmosphere.By the material and the lithium carbonate that obtain in mass ratio 100:1 in vibration at high speed ball mill, process 4 hours after mix, the setting speed of vibration at high speed ball mill is 1500 revs/min, crosses after 200 mesh sieves also remove magnetic, namely obtains high-performance richness nitrogen type carbon composite electrode material.
Respectively sample obtained for embodiment 1 ~ 5 is made half-cell and carry out chemical property mensuration, half-cell method for providing is all as follows: be 80%:15%:5% mixing in mass ratio by testing sample, SuperPLi conductive black, sodium cellulosate, mix well with deionized water, stir into thick, be coated on Copper Foil, under vacuum (-0.1MPa) 60oC, drying 12 hours, is cut into the circular film that diameter is about 1cm after cooling.Half-cell adopts CR2016 type button cell to assemble in glove box, and barrier film is Celgard2400 polypropylene diaphragm, and electrolyte is 1MLiPF
6ethylene carbonate (EC) and diethyl carbonate (DEC) mixed electrolytic solution (illustrate: in mixed electrolytic solution, the volume ratio of EC, DEC is 1:1, LiPF in mixed electrolytic solution
6concentration is 1M), negative pole is circular lithium sheet (diameter 1.5cm) of commercialization, and electrochemical property test carries out on indigo plant electric CT2001A type battery test system (Wuhan Land Electronic Co., Ltd.'s production).
Fig. 1 is the scanning electron microscopic picture of embodiment 1, can find out prepared material feature in the form of sheets, and the product pattern obtained by other embodiments is consistent with embodiment 1, does not repeat.The cyclic voltammetry curve of Fig. 2 material prepared by embodiment 1, result shows that the redox peak of material with carbon element feature appears in the material with carbon element prepared at 0 ~ 0.2V, show that the removal lithium embedded reaction of embodiment 1 material all occurs in electronegative potential, different from the charge and discharge process of the 5th week because defining SEI film first.Fig. 3 result shows, combination electrode material prepared by embodiment 1 ~ 5 has good chemical property, good cycling stability, nitrogen element mainly because of electron rich is introduced, the electronic transmission performance of material and chemical reactivity strengthen, adding that the laminated structure of hard soft carbon formation contributes to the deintercalation process of lithium ion, materials exhibit is made to go out excellent chemical property.The material that embodiment 1 ~ 5 is prepared is under 0.2C condition, and initial discharge capacity is 615.1mAh/g, 678.3mAh/g, 648.3mAh/g, 543.4mAh/g, 425.9mAh/g respectively; After circulating 400 weeks, discharge capacity is respectively: 437.1mAh/g, 373.6mAh/g, 343.6mAh/g, 252.1mAh/g, 175.6mAh/g.Fig. 4 result shows that prepared material is under the density of big current 5A/g, and specific capacity still can remain on 210mAh/g, and high rate charge-discharge after-current density gets back to 0.1A/g, and specific capacity still can maintain 450mAh/g.
Claims (9)
1. a preparation method for high-performance rich nitrogen type carbon composite electrode material, comprises the steps:
(1) pitch and melamine are added in the reactor with dispersed with stirring device, be heated to more than asphalt softening point 20 ~ 30 DEG C, dispersed with stirring, and maintain this temperature 1 hour, pitch is fully mixed with melamine; Broken after cooling;
(2) by the solid matter of fragmentation, put into graphite crucible, be heated to 900 ~ 1100 DEG C from room temperature under an inert atmosphere and keep this temperature 6 ~ 10 hours, obtain rich nitrogen type carbon composite head product;
(3) in vibration at high speed ball mill, 4 hours are processed after rich nitrogen type carbon composite head product step (2) obtained mixes with lithium salts, the setting speed of vibration at high speed ball mill is 1500 revs/min, cross 200 mesh sieves and except after magnetic, namely obtain high-performance rich nitrogen type carbon composite electrode material.
2. preparation method according to claim 1, is characterized in that: described pitch is coal tar pitch or petroleum asphalt, and its softening point is all 40 ~ 120 DEG C of scopes.
3. preparation method according to claim 1, is characterized in that: the mass ratio of described pitch and melamine is 1:x; Wherein, 0 < x≤2.
4. preparation method according to claim 1, is characterized in that: in step (1), the mixing speed of dispersed with stirring is 3000 revs/min.
5. preparation method according to claim 1, is characterized in that: described inert atmosphere conditions is nitrogen or argon gas atmosphere.
6. preparation method according to claim 1, is characterized in that: the speed heated up in described step (2) is 3 ~ 5 DEG C/min.
7. preparation method according to claim 1, is characterized in that: the lithium salts in described step (3) is lithium carbonate or lithium fluoride.
8. preparation method according to claim 1, is characterized in that: the rich nitrogen type carbon composite head product in described step (3) and the mass ratio of lithium salts are 100:y; Wherein, 0.5 < y≤3.
9. the rich nitrogen type carbon composite electrode material obtained by the preparation method described in claim 1 or 2 or 3 or 4 or 5 or 6 or 7 or 8.
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| CN106058183A (en) * | 2016-07-11 | 2016-10-26 | 上海纳晶科技有限公司 | Preparation method of amorphous carbon-doped composite material for high-capacity energy storage device |
| CN107204467A (en) * | 2017-06-13 | 2017-09-26 | 中国电子新能源（武汉）研究院有限责任公司 | Sodium-ion battery cathode size, negative plate and battery |
| CN109609166A (en) * | 2019-01-21 | 2019-04-12 | 辽宁科技大学 | A kind of preparation method of the thin mosaic texture pitch coke of richness nitrogen |
| CN109628125A (en) * | 2019-01-21 | 2019-04-16 | 辽宁科技大学 | A kind of preparation method of the thin mosaic texture pitch coke of high micro strength richness nitrogen |
| CN112320797A (en) * | 2020-10-16 | 2021-02-05 | 中国科学院山西煤炭化学研究所 | Preparation method of activated carbon for desulfurization of tar hydrogenation product |
| CN114023573A (en) * | 2021-11-02 | 2022-02-08 | 南京信息工程大学 | Preparation method of triazinyl aza two-dimensional electrode material |
| CN114373908A (en) * | 2021-12-21 | 2022-04-19 | 中国科学院宁波材料技术与工程研究所 | Soft-hard carbon composite material and preparation method and application thereof |
| CN114715875A (en) * | 2022-03-31 | 2022-07-08 | 宁波大学 | Preparation method of thin-layer carbon-based material and application of thin-layer carbon-based material as battery material |
| CN115285989A (en) * | 2021-12-16 | 2022-11-04 | 榆林学院 | Coal tar pitch-based high-capacitance carbon and preparation method thereof |
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| CN109609166A (en) * | 2019-01-21 | 2019-04-12 | 辽宁科技大学 | A kind of preparation method of the thin mosaic texture pitch coke of richness nitrogen |
| CN109628125A (en) * | 2019-01-21 | 2019-04-16 | 辽宁科技大学 | A kind of preparation method of the thin mosaic texture pitch coke of high micro strength richness nitrogen |
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| CN114023573A (en) * | 2021-11-02 | 2022-02-08 | 南京信息工程大学 | Preparation method of triazinyl aza two-dimensional electrode material |
| CN114023573B (en) * | 2021-11-02 | 2023-11-10 | 南京信息工程大学 | Preparation method of triazinyl aza two-dimensional electrode material |
| CN115285989A (en) * | 2021-12-16 | 2022-11-04 | 榆林学院 | Coal tar pitch-based high-capacitance carbon and preparation method thereof |
| CN114373908A (en) * | 2021-12-21 | 2022-04-19 | 中国科学院宁波材料技术与工程研究所 | Soft-hard carbon composite material and preparation method and application thereof |
| CN114715875A (en) * | 2022-03-31 | 2022-07-08 | 宁波大学 | Preparation method of thin-layer carbon-based material and application of thin-layer carbon-based material as battery material |
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