CN113443623A - Method for reducing graphitization temperature through composite catalysis - Google Patents

Method for reducing graphitization temperature through composite catalysis Download PDF

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CN113443623A
CN113443623A CN202110810106.8A CN202110810106A CN113443623A CN 113443623 A CN113443623 A CN 113443623A CN 202110810106 A CN202110810106 A CN 202110810106A CN 113443623 A CN113443623 A CN 113443623A
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mass ratio
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sodium
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不公告发明人
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Shaanxi Zeming Future Technology Co ltd
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00—Carbon; Compounds thereof
    • C01B32/20—Graphite
    • C01B32/205—Preparation
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00—Carbon; Compounds thereof
    • C01B32/20—Graphite
    • C01B32/21—After-treatment
    • 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
    • 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
    • H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
    • H01M2004/027—Negative electrodes
    • 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 method for realizing graphitization of a carbon source at a low temperature by multi-step linkage and multi-metal concerted catalysis. The catalysis is a multi-step linkage multi-metal composite catalysis process, different properties of various intermediate products are generated in a carbon source phase change process, different catalytic actions of different metal composites are mutually linked, and a low-temperature catalytic graphitization process is jointly completed. The catalytic graphitization reaction process is mild, and the graphite prepared by using the catalytic system at a low temperature has good graphitization degree (crystallinity), and can be used as a lithium battery cathode. The graphite prepared by the method is used as the negative electrode material of the lithium battery, and has the characteristics of high specific capacity, excellent cycling stability and low cost.

Description

Method for reducing graphitization temperature through composite catalysis
Technical Field
The invention belongs to the technical field of graphite material preparation, and particularly relates to a method for reducing the synthesis temperature of a graphite material by adding a catalyst, wherein the obtained product is graphite and can be used as a lithium battery negative electrode material.
Background
The graphitization process belongs to a phase change process of a carbon material, and the specific change is as follows: the carbon atoms are converted into ordered structures from amorphous structures (the carbon atoms in the graphite layer form a two-dimensional layered structure through sp2 hybridization, and the layers form a three-dimensional structure through pi-pi bond mutual attraction). This phase transition process requires high temperatures, greater than 2600 ℃, to allow the reaction to proceed. It is now common in the industry to use acheson furnaces to provide high temperatures of greater than 2600 c to complete the graphitization process to produce graphite materials (i.e., synthetic graphite), such as CN101648808B and CN 202011434666. In 2020, the domestic lithium battery cathode needs about 30 million tons of artificial graphite, and a large amount of energy consumption is formed in the high-temperature calcination process at the temperature of more than 2600 ℃. Therefore, the graphitization temperature is reduced by using a catalytic mode, so that a large amount of electric energy can be saved.
The idea of lowering the graphitization temperature by introducing a catalytic means was proposed in 1966 by yokokawa et al, tokyo university, japan (Carbon, 1966, 4, 459). They tried to add various metals as catalysts individually, but the graphitization degree of the obtained product is poor (less than 50%) at low temperature, and the lithium-grade graphite material requirement cannot be met. CN108101043B proposes that the graphitization degree (crystallinity) of the graphite product is good by using magnesium-based metal as a catalyst and catalyzing at low temperature; however, the magnesium catalyzed process is a violent exothermic reaction process (the exothermic quantity is about 4190J/g); the method brings serious potential safety hazard to industrial mass production. Therefore, the search for mild low temperature catalytic graphitization methods is a technical bottleneck in the art. .
Disclosure of Invention
In order to solve the problems, the invention provides a method for realizing low-temperature graphitization of a carbon precursor by multi-step linkage and multi-metal compound concerted catalysis at low temperature. The catalytic graphitization reaction process is mild, and the graphite prepared by using the composite catalyst at a low temperature has good graphitization degree (crystallinity), so that the graphite requirement of a lithium battery can be met. The catalyst is a multi-metal composite catalyst, and utilizes the property of various intermediate products generated in the phase change process of a carbon precursor, different metals realize different catalytic actions on different intermediate products, and multiple steps are mutually connected, so that the low-temperature catalytic graphitization process is jointly completed. The graphite prepared by the method is used as the negative electrode material of the lithium battery, and has the characteristics of high specific capacity, excellent cycling stability and low cost.
In order to achieve the above purpose, the method for reducing graphitization temperature by composite catalysis comprises the following steps:
grinding a carbon source into powder, mixing the carbon source with sodium salt and calcium salt according to a certain mass ratio, marking as A, adding copper sulfate with the mass fraction of 0.5-20 wt% of A, annealing for 2-10 hours at 300-600 ℃ in a nitrogen atmosphere, and marking as B as a solid product;
step two, mixing manganese salt and graphite powder according to the proportion of 1: 1-1: dispersing 10 in water with the mass ratio of 2 times of the total mass of the components, stirring for 2 hours, adding sodium hydroxide to adjust the pH value to 11, filtering and drying the product, and annealing for 2 hours at 300-600 ℃ in a nitrogen atmosphere, wherein the product is marked as C;
step three, mixing iron salt and citric acid according to the ratio of 5: 1-1: 1 is dispersed into water with the mass ratio of 5 times of the total mass of the gel, sodium thiosulfate with the mass ratio of ferric salt of 8 percent is added, the mixture is stirred for 1 hour, and the gel D is obtained after the mixture is dried at 130 ℃;
and step four, uniformly mixing the products B, C and D according to a certain mass ratio, annealing the mixture at 800-1700 ℃ for 2-10 hours in a nitrogen atmosphere, pickling the product with 1M hydrochloric acid, and washing the product with water to be neutral to obtain a low-temperature catalytic graphite product, wherein the purity and the graphitization degree of the low-temperature catalytic graphite product can meet the requirements of the lithium battery cathode material.
In the step 1, the carbon source is one or a mixture of any more of anthracite, asphalt, phenolic resin or coke.
In the step 1, the sodium salt is one or a mixture of any more of sodium chloride, sodium carbonate, sodium acetate and sodium sulfate; the calcium salt is one or a mixture of any more of calcium chloride, calcium carbonate, calcium acetate or calcium sulfate.
In the step 1, the mass ratio of the carbon source to the salt (the mass sum of the sodium salt and the calcium salt) is 100: 1 to 1:1, wherein the mass ratio of the sodium salt to the calcium salt is 10: 1-1: 10.
in the step 2, the manganese salt is one or a mixture of any more of manganese chloride, manganese carbonate, manganese sulfate or manganese nitrate.
In the step 3, the ferric salt is one or a mixture of any more of ferric chloride, ferric carbonate, ferric sulfate or ferric nitrate.
In the step 4, the mass ratio of the product B to (the sum of the masses of C and D) is 100: 1-1: 1, wherein the mass ratio of C to D is 10: 1 to 1: 10.
the invention provides a concept of multi-step linkage and low-temperature graphitization of a carbon precursor by a multi-metal compound in a synergistic catalysis manner. The graphitization degree of the obtained graphite product is higher than 90%, and when the graphite product is used as a lithium battery negative electrode material, good cycling stability and high specific capacity can be provided. The invention can realize graphitization at lower temperature (800-1700 ℃), and the catalytic process is mild and has no danger, and the invention has the characteristics of safe production, high repeatability and low cost.
Drawings
FIG. 1 is an X-ray diffraction pattern of the graphite materials prepared in examples 1 and 5;
FIG. 2 is a transmission electron micrograph of the graphite material prepared in examples 1 and 5;
FIG. 3 is a scanning electron micrograph of the graphite material prepared in examples 1 and 5;
fig. 4 is a graph showing the charge/discharge specific capacity of the graphite material prepared in example 1 as a negative electrode material for a lithium battery.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
A composite catalytic graphitization temperature reduction method comprises the following steps:
grinding anthracite into powder, mixing the anthracite with sodium chloride and calcium carbonate, and marking as A, wherein the mass ratio of the anthracite to salt (sodium chloride and calcium carbonate) is 100: 1, the mass ratio of sodium chloride to calcium carbonate is 10: 1. then adding copper sulfate with the mass fraction of 0.5 wt% of A, annealing for 10 hours at 300 ℃ in a nitrogen atmosphere, and recording a solid product as B;
step two, mixing manganese chloride and graphite powder according to the proportion of 1: dispersing the mixture of 1 in water with the mass ratio of 2 times of the total mass of the mixture, stirring for 2 hours, adding sodium hydroxide to adjust the pH value to 11, filtering and drying a product, and annealing for 2 hours at 300 ℃ in a nitrogen atmosphere, wherein the product is marked as C;
step three, mixing ferric chloride and citric acid according to the ratio of 5: 1 into water with the mass ratio of 5 times of the total mass of the raw materials, adding sodium thiosulfate with the mass ratio of ferric chloride of 8 percent, stirring for 1 hour, and drying at 130 ℃ to obtain gel D;
step four, uniformly mixing products B, C and D, wherein the mass ratio of B to (the sum of the masses of C and D) is 100: 1, the mass ratio of C to D is 10: 1. annealing the mixture at 800 ℃ for 10 hours in nitrogen atmosphere, washing the product with 1M hydrochloric acid, and washing the product with water to be neutral to obtain the low-temperature catalytic graphite product, wherein the purity and the graphitization degree of the product can meet the requirements of the lithium battery cathode material.
Example 2
A composite catalytic graphitization temperature reduction method comprises the following steps:
grinding asphalt into powder, mixing the asphalt with sodium carbonate and calcium chloride, and recording as A, wherein the mass ratio of the asphalt to salt (sodium carbonate and calcium chloride) is 60: 1, the mass ratio of sodium carbonate to calcium chloride is 5: 1. adding copper sulfate with the mass fraction of 3wt% of A, annealing for 8 hours at 400 ℃ in a nitrogen atmosphere, and recording a solid product as B;
step two, mixing manganese carbonate and graphite powder according to the proportion of 1: 3, dispersing the mixture into water with the mass ratio of 2 times of the total mass of the mixture, stirring for 2 hours, adding sodium hydroxide to adjust the pH value to 11, filtering and drying a product, and annealing for 2 hours at 400 ℃ in a nitrogen atmosphere, wherein the product is marked as C;
step three, mixing iron carbonate and citric acid according to the ratio of 4: 1 is dispersed into water with the mass ratio of 5 times of the total mass of the materials, sodium thiosulfate with the mass ratio of iron carbonate of 8 percent is added, the mixture is stirred for 1 hour, and the gel D is obtained after the mixture is dried at 130 ℃;
step four, uniformly mixing products B, C and D, wherein the mass ratio of B to (the sum of the masses of C and D) is 70: 1, the mass ratio of C to D is 7: 1. annealing the mixture at 1000 ℃ for 8 hours in nitrogen atmosphere, washing the product with 1M hydrochloric acid, and washing the product with water to be neutral to obtain the low-temperature catalytic graphite product, wherein the purity and the graphitization degree of the product can meet the requirements of the lithium battery cathode material.
Example 3
A composite catalytic graphitization temperature reduction method comprises the following steps:
grinding oil-based needle coke into powder, mixing the oil-based needle coke with sodium acetate and calcium sulfate, and recording as A, wherein the mass ratio of the oil-based needle coke to the salt (sodium acetate and calcium sulfate) is 40: 1, the mass ratio of sodium chloride to calcium carbonate is 1: 1. then adding copper sulfate with the mass fraction of 10wt% of A, annealing for 5 hours at 500 ℃ in a nitrogen atmosphere, and recording a solid product as B;
step two, mixing manganese carbonate and graphite powder according to the proportion of 1: 5, dispersing the mixture into water with the mass ratio of 2 times of the total mass of the mixture, stirring for 2 hours, adding sodium hydroxide to adjust the pH value to 11, filtering and drying a product, and annealing for 2 hours at 500 ℃ in a nitrogen atmosphere, wherein the product is marked as C;
step three, mixing iron carbonate and citric acid according to the ratio of 3: 1 is dispersed into water with the mass ratio of 5 times of the total mass of the materials, sodium thiosulfate with the mass ratio of iron carbonate of 8 percent is added, the mixture is stirred for 1 hour, and the gel D is obtained after the mixture is dried at 130 ℃;
step four, uniformly mixing products B, C and D, wherein the mass ratio of B to (the sum of the mass of C and D) is 30: 1, the mass ratio of C to D is 4: 1. annealing the mixture at 1200 ℃ for 6 hours in nitrogen atmosphere, washing the product with 1M hydrochloric acid, and washing the product with water to be neutral to obtain the low-temperature catalytic graphite product, wherein the purity and the graphitization degree of the product can meet the requirements of the lithium battery cathode material.
Example 4
A composite catalytic graphitization temperature reduction method comprises the following steps:
grinding phenolic resin into powder, mixing coal-based needle coke with sodium sulfate and calcium acetate, and recording as A, wherein the mass ratio of the coal-based needle coke to salt (sodium sulfate and calcium acetate) is 10: 1, the mass ratio of sodium sulfate to calcium acetate is 1: 5. adding 15 wt% of copper sulfate of A, annealing at 600 ℃ for 2 hours in nitrogen atmosphere, and recording a solid product as B;
step two, mixing manganese nitrate and graphite powder according to the proportion of 1: 8, dispersing the mixture into water with the mass ratio of 2 times of the total mass of the mixture, stirring for 2 hours, adding sodium hydroxide to adjust the pH value to 11, filtering and drying a product, and annealing for 2 hours at 300 ℃ in a nitrogen atmosphere, wherein the product is marked as C;
step three, mixing ferric nitrate and citric acid according to the ratio of 2: dispersing the mixture of 1 in water of which the mass ratio is 5 times of the total mass of the mixture, adding sodium thiosulfate of which the mass ratio of the ferric nitrate is 8 percent, stirring for 1 hour, and drying at 130 ℃ to obtain gel D;
step four, uniformly mixing products B, C and D, wherein the mass ratio of B to (the sum of the masses of C and D) is 10: 1, the mass ratio of C to D is 2: 1. annealing the mixture at 1400 ℃ for 4 hours in a nitrogen atmosphere, washing the product with 1M hydrochloric acid, and washing the product with water to be neutral to obtain a low-temperature catalytic graphite product, wherein the purity and the graphitization degree of the product can meet the requirements of a lithium battery cathode material.
Example 5
A composite catalytic graphitization temperature reduction method comprises the following steps:
mixing anthracite and asphalt in a mass ratio of 1:1, grinding into powder, mixing a carbon source with sodium sulfate and calcium sulfate, and recording as A, wherein the mass ratio of the carbon source to salt (sodium sulfate and calcium sulfate) is 1:1, the mass ratio of sodium chloride to calcium carbonate is 1: 10. then adding copper sulfate with the mass fraction of 0.5 wt% of A, annealing for 10 hours at 300 ℃ in a nitrogen atmosphere, and recording a solid product as B;
step two, mixing manganese chloride and graphite powder according to the proportion of 1: 10, stirring for 2 hours, adding sodium hydroxide to adjust the pH value to 11, filtering and drying a product, and annealing for 2 hours at 500 ℃ in a nitrogen atmosphere, wherein the product is marked as C;
step three, mixing ferric nitrate and citric acid according to the proportion of 1: dispersing the mixture of 1 in water of which the mass ratio is 5 times of the total mass of the mixture, adding sodium thiosulfate of which the mass ratio of the ferric nitrate is 8 percent, stirring for 1 hour, and drying at 130 ℃ to obtain gel D;
step four, uniformly mixing products B, C and D, wherein the mass ratio of B to (the sum of the mass of C and D) is 1:1, the mass ratio of C to D is 1: 1. annealing the mixture at 1700 ℃ for 2 hours in nitrogen atmosphere, washing the product with 1M hydrochloric acid, and washing the product with water to neutrality to obtain the low-temperature catalytic graphite product, wherein the purity and the graphitization degree of the product can meet the requirements of the lithium battery cathode material.
The graphite anode materials in examples 1 to 5 were subjected to charge and discharge tests by a half-cell test method. The testing method of the half cell comprises the following steps: preparing 6-7% polyvinylidene fluoride by taking N-methyl pyrrolidone as solventUniformly mixing a graphite negative electrode material, polyvinylidene fluoride and conductive carbon black according to the mass ratio of 91.6: 6.6: 1.8, coating the mixture on a copper foil, and putting the coated pole piece into a vacuum drying oven at the temperature of 110 ℃ for vacuum drying for 10 hours for later use. Then assembled into a 2032 type button cell in an argon-filled German Michelona glove box with 1mol/L LiPF6The three-component mixed solvent is characterized in that a mixed solution of EC, DMC and EMC 1:1:1 (volume ratio) is used as an electrolyte, a metal lithium sheet is used as a counter electrode, and electrochemical performance test is carried out on the assembled half cell on a LAND cell test system of Wuhanjinnuo electronic Co.
FIG. 1 is an X-ray diffraction pattern (XRD pattern) of the graphite materials prepared in examples 1 and 5, wherein the abscissa is an angle; the ordinate is the relative intensity. The graph can show that the graphite material is obtained, and the (002) diffraction peak of the graphite is at the position where the 2 theta is 26.8 degrees, and the graph 1 can show that the graphite material prepared by the method has high graphitization degree (namely high crystallinity) and good structural regularity;
FIG. 2 is a transmission electron micrograph of the graphite material prepared in examples 1 and 5;
FIG. 3 is a Scanning Electron Micrograph (SEM) of the graphite materials prepared in examples 1 and 5, and the SEM of the graphite materials prepared in examples 1 to 5 is the same, from which it can be seen that a graphite sheet structure is obtained by the present method;
fig. 4 is a charge and discharge curve diagram of the graphite material prepared in example 1 as a negative electrode material of a lithium ion battery. The graph shows that the first discharge specific capacity of the graphite carbon material is 365 mAh/g, and the coulombic efficiency is as high as 97%; its charge-discharge specific capacity and coulombic efficiency are higher.
The above-mentioned contents are only for illustrating the technical idea of the present invention, and the protection scope of the present invention is not limited thereby, and any modification made on the basis of the technical idea of the present invention falls within the protection scope of the claims of the present invention.

Claims (7)

1. A method for reducing graphitization temperature by composite catalysis is characterized by comprising the following steps:
grinding a carbon source into powder, mixing the carbon source with sodium salt and calcium salt according to a certain mass ratio, marking as A, adding copper sulfate with the mass fraction of 0.5-20 wt% of A, annealing for 2-10 hours at 300-600 ℃ in a nitrogen atmosphere, and marking as B as a solid product;
step two, mixing manganese salt and graphite powder according to the proportion of 1: 1-1: dispersing 10 in water with the mass ratio of 2 times of the total mass of the components, stirring for 2 hours, adding sodium hydroxide to adjust the pH value to 11, filtering and drying the product, and annealing for 2 hours at 300-600 ℃ in a nitrogen atmosphere, wherein the product is marked as C;
step three, mixing iron salt and citric acid according to the ratio of 5: 1-1: 1 is dispersed into water with the mass ratio of 5 times of the total mass of the gel, sodium thiosulfate with the mass ratio of ferric salt of 8 percent is added, the mixture is stirred for 1 hour, and the gel D is obtained after the mixture is dried at 130 ℃;
and step four, uniformly mixing the products B, C and D according to a certain mass ratio, annealing the mixture at 800-1700 ℃ for 2-10 hours in a nitrogen atmosphere, pickling the product with 1M hydrochloric acid, and washing the product with water to be neutral to obtain a low-temperature catalytic graphite product, wherein the purity and the graphitization degree of the low-temperature catalytic graphite product can meet the requirements of the lithium battery cathode material.
2. The composite catalytic graphitization temperature reduction method of claim 1, wherein in step 1, the carbon source is one or a mixture of any of anthracite, pitch, phenolic resin, and coke.
3. The composite catalytic graphitization temperature reduction method according to claim 1, wherein in the step 1, the sodium salt is one or a mixture of any of sodium chloride, sodium carbonate, sodium acetate and sodium sulfate; the calcium salt is one or a mixture of any more of calcium chloride, calcium carbonate, calcium acetate or calcium sulfate.
4. The composite catalytic graphitization temperature reduction method according to claim 1, wherein in the step 1, the mass ratio of the carbon source to the salt (mass sum of sodium salt and calcium salt) is 100: 1-1: 1, wherein the mass ratio of the sodium salt to the calcium salt is 10: 1-1: 10.
5. the composite catalytic graphitization temperature reduction method of claim 1, wherein in step 2, the manganese salt is one or a mixture of any of manganese chloride, manganese carbonate, manganese sulfate and manganese nitrate.
6. The method for reducing the graphitization temperature through composite catalysis as claimed in claim 1, wherein in the step 3, the iron salt is one or a mixture of any of ferric chloride, ferric carbonate, ferric sulfate or ferric nitrate.
7. The composite catalytic graphitization temperature reduction method according to claim 1, wherein in the step 4, the mass ratio of the product B to the mass sum of (C and D) is 100: 1-1: 1, wherein the mass ratio of C to D is 10: 1-1: 10.
CN202110810106.8A 2021-07-18 2021-07-18 Method for reducing graphitization temperature through composite catalysis Pending CN113443623A (en)

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WO2018115177A1 (en) * 2016-12-23 2018-06-28 Sgl Carbon Se Graphite material
CN108557816A (en) * 2018-06-26 2018-09-21 武汉大学 A kind of preparation method of high specific surface area porous graphitized charcoal
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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20020012845A1 (en) * 2000-06-16 2002-01-31 Wan-Uk Choi Negative active material for rechargeable lithium battery and method of preparing the same
CN101445234A (en) * 2009-01-06 2009-06-03 黑龙江大学 A preparation method of graphitized carbon nano material
CN102394294A (en) * 2011-11-29 2012-03-28 上海交通大学 Preparation method of highly graphitized activated carbon-transition metal oxide nanocomposite material
CN102745677A (en) * 2012-07-06 2012-10-24 同济大学 Collaborative graphitization method for amorphous carbon material
JP2014229517A (en) * 2013-05-23 2014-12-08 日立化成株式会社 Negative electrode material for lithium ion secondary battery, negative electrode for lithium ion secondary battery, and lithium ion secondary battery
CN103318880A (en) * 2013-07-09 2013-09-25 中钢集团洛阳耐火材料研究院有限公司 Method for low-temperature graphitization of phenolic resin
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WO2018115177A1 (en) * 2016-12-23 2018-06-28 Sgl Carbon Se Graphite material
CN108557816A (en) * 2018-06-26 2018-09-21 武汉大学 A kind of preparation method of high specific surface area porous graphitized charcoal
CN110407204A (en) * 2019-09-04 2019-11-05 内蒙古奥原新材料有限公司 A kind of Preparation method and use of coke low temperature graphitization

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