CN104900878A - Production method of artificial graphite anode material for high-capacity lithium ion battery - Google Patents
Production method of artificial graphite anode material for high-capacity lithium ion battery Download PDFInfo
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- CN104900878A CN104900878A CN201510338421.XA CN201510338421A CN104900878A CN 104900878 A CN104900878 A CN 104900878A CN 201510338421 A CN201510338421 A CN 201510338421A CN 104900878 A CN104900878 A CN 104900878A
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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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- 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
- H01M4/139—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
- H01M2220/00—Batteries for particular applications
- H01M2220/10—Batteries in stationary systems, e.g. emergency power source in plant
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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
- H01M2220/00—Batteries for particular applications
- H01M2220/20—Batteries in motive systems, e.g. vehicle, ship, plane
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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
- H01M2220/00—Batteries for particular applications
- H01M2220/30—Batteries in portable systems, e.g. mobile phone, laptop
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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 provides a production method of an artificial graphite anode material for a high-capacity lithium ion battery. Petroleum coke coarse powder is taken as a raw material A, asphalt micro powder is taken as a raw material B, and single transition metal micro powder and multiple transition metal mixed micro powder are taken as a raw material C; the raw materials A and C are mixed in certain weight ratio, graphitized at the temperature of 2,800 DEG C-3,200 DEG C and then smashed; the smashed mixed materials and the raw material B are mixed in a certain weight ratio, modified at the temperature of 300 DEG C-600 DEG C and then carbonized at the temperature of 1,200 DEG C-1,500 DEG C after mixing or are directly carbonized at the temperature of 1,200 DEG C-1,500 DEG C after mixing, and the mixed materials are smashed, subjected to impurity removal and sieved after cooled to the room temperature. The method has the advantages as follows: the degree of graphitization of the material is improved due to adding of metal elements, and the material capacity is improved; the raw material A is graphitized in a coarse powder state, the surface oxidation area and the oxidation degree of particles can be reduced, and the capacity of the material can be improved, and the yield can be increased.
Description
Technical field
The present invention relates to a kind of high-capacity lithium ion cell artificial plumbago negative pole material production method, belong to technical field of lithium ion battery negative.
Background technology
Lithium ion battery is a kind of desirable green power supply, since nineteen ninety comes out, performance because of its brilliance obtains swift and violent development, lithium ion battery has captured rapidly many fields with the advantage that other battery is incomparable, as known mobile phone, notebook computer, camera, video camera and electric tool etc., and increasing country by lithium battery applications in power station, the dynamic purposes such as power vehicle, military affairs.Wherein, negative material is the key factor of lithium ion battery energy storage, and its performance decides the development level of lithium ion battery to a certain extent.Carbonaceous material is that people's early start is studied and is applied to the material of lithium ion battery negative, commercially still occupies an leading position so far.
Although the commercialization of the graphite cathode material of lithium ion battery, also exists the weakness that some are difficult to overcome, the negative material that exploitation performance is more excellent remains the important topic of Study on Li-ion batteries.The negative pole of lithium ion battery is mixed and made into pasty state binder is evenly coated on Copper Foil by negative electrode active material material with carbon element or non-carbon material, adhesive, additive, and drying, roll extrusion form.Make, can key be prepare the negative material of reversibly de-/embedding lithium ion lithium ion battery success.
In general, a kind of good negative material is selected should to follow following principle: specific energy is high, electrode potential is low, discharge and recharge reaction good reversibility, good with the compatibility of electrolyte and binding agent.The crystal structure of material is regular, and in charge and discharge process, irreversible change does not occur structure is that acquisition specific capacity is high, the key of the lithium ion battery had extended cycle life.But, this field link the weakest is at present still to the research of the Structure and Properties of intercalation materials of li ions.The reversibility that the present invention is directed to carbonaceous material carries out Improvement, reaches higher embedding lithium and cycle performance.
Summary of the invention
The object of this invention is to provide a kind of high-capacity lithium ion cell artificial plumbago negative pole material production method, too high to overcome Delanium raw material degree of oxidation in graphitizing process, cause the artificial defects such as loss capacity, Cycle Difference, yield are low.
Technical scheme of the present invention: a kind of high-capacity lithium ion cell artificial plumbago negative pole material production method, concrete production technology is:
A () take petroleum coke as raw material A, raw material A is ground into the meal that particle diameter is 0.5 ~ 5.0mm, and described raw material A is petroleum coke or needle coke after retard petroleum coke, forging;
B () take pitch as raw material B, pulverized by raw material B airslide disintegrating mill, and be ground into the micro mist of particle diameter≤3 μm, described raw material B is petroleum asphalt or coal tar pitch;
C (), with single transition metal micro mist or multiple transition metal admixed finepowder for raw material C, median is≤50nm, and described transition metal chooses V, Ni, Co;
The raw material C micro mist that d raw material A meal that (a) step obtains by () and (c) step obtain is by weight A/C=100/(0.2 ~ 1) ratio be uniformly mixed, at 2800 ~ 3200 DEG C, graphitization is carried out after mixing, pulverize after cooling, being ground into median is 12 ~ 18 μm, then mechanical shaping process is carried out, make granule-morphology regular, close to circular;
The raw material B micro mist that e material that (d) step obtains by () and (b) step obtain, by weight (A+C)/B=100/(2 ~ 8) ratio mix, first at 300 ~ 600 DEG C, carries out modification after mixing, then carbonizes at 1200 ~ 1500 DEG C; Or mixing is direct afterwards to be carbonized at 1200 ~ 1500 DEG C;
F (), after the material that (e) step obtains is cooled to room temperature, is carried out breaing up, is sieved, removal of impurities, obtain product.
Described being uniformly mixed adopts twin-screw or two ribbon agitating mode.
Beneficial effect of the present invention:
1, be processed into meal because the present invention carries out mechanical crushing to petroleum coke, under meal state, carry out graphitization, the integrated oxidation area of material and the degree of oxidation of individual particles can be reduced, keep yield; After fine powder, material fine particle surface is not oxidized, can improve effective embedding lithium and ion transmission performance, and contributes to coated closely solid of pitch-coating layer, difficult drop-off;
2, petroleum coke carries out graphitization under meal state, not only can reduce material oxidation degree, and more can reduce the specific area of material after bonding after continuous Shape correction, improve drawing abillity, namely pole piece compacting bounce-back is little, pole piece compaction density is high;
3, adopt transient metal doped graphitization, the degree of graphitization of material can be improved, namely improve the capacity of Delanium; Adopt mechanical shaping, the uniformity of pitch-coating layer can be improved, thus improve all even compactness forming SEI film with electrolyte, reduce active site, and improve the tap density of material;
In sum, reversible capacity and the cycle life of the present invention by utilizing treatment technologies such as carrying out graphitization, transient metal doped graphitization, fine particle surface shaping under meal state can play material greatly, and its production technology is simple, production efficiency is high, cost is low, course of processing safety, can be used for suitability for industrialized production.
embodiment:
embodiment 1:
Take the rear petroleum coke raw material A 100kg of forging, be ground into the meal that particle diameter is about 2mm.
Take asphalt stock B 5kg, carry out air-flow crushing, powder particle diameter≤3 μm.
Take the raw material A meal 60kg crushed, add raw material C micro mist 600g, carry out being uniformly mixed 30 minutes under normal temperature state, then at 3000 DEG C, carry out graphitization.
Take the mixed material 50kg after graphitization, carry out that fine powder is broken, classification, classification median is 18 μm, then carries out mechanical shaping 30min.
Take the mixed material 20kg after shaping, add raw material B micro mist 600g, carry out mixing 30min at normal temperatures, then at 300 ~ 600 DEG C, carry out modification, and then carbonize at 1300 DEG C.
After material after carbonizing is cooled to room temperature, carry out breaing up, sieve, removal of impurities, obtain product.
Do experiment with LIR2430 type button cell, gained negative material discharge capacity is 358.2mAh/g, and discharging efficiency is 93.8%, as shown in table 1.
embodiment 2:
Take the rear petroleum coke raw material A 100kg of forging, be ground into the meal that particle diameter is about 4mm.
Take asphalt stock B 5kg, carry out air-flow crushing, powder particle diameter≤3 μm.
Take the raw material A 60kg crushed, add raw material C 480g, carry out being uniformly mixed 30 minutes under normal temperature state, then at 3000 DEG C, carry out graphitization.
Take the mixed material 50kg after graphitization, carry out that fine powder is broken, classification, classification median is 17 μm, then carries out mechanical shaping 30min.
Take the mixed material 20kg after shaping, add raw material B micro mist 800g, carry out mixing 30min at normal temperatures, then at 300 ~ 600 DEG C, carry out modification, and then carbonize at 1400 DEG C.
After material after carbonizing is cooled to room temperature, carry out breaing up, sieve, removal of impurities, obtain product.
Do experiment with LIR2430 type button cell, gained negative material discharge capacity is 357.8mAh/g, and discharging efficiency is 94.3%, as shown in table 1.
embodiment 3:
Take acicular petroleum coke raw material A 100kg, be ground into the meal that particle diameter is about 4mm.
Take asphalt stock B 5kg, carry out air-flow crushing, powder particle diameter≤3 μm.
Take the raw material A 60kg crushed, add raw material C 540g, carry out being uniformly mixed 30 minutes under normal temperature state, then at 3200 DEG C, carry out graphitization.
Take the mixed material 50kg after graphitization, carry out that fine powder is broken, classification, classification median is 15 μm, then carries out mechanical shaping 30min.
Take the mixed material 20kg after shaping, add raw material B micro mist 600g, carry out mixing 30min at normal temperatures, then at 300 ~ 600 DEG C, carry out modification, and then carbonize at 1400 DEG C.
After material after carbonizing is cooled to room temperature, carry out breaing up, sieve, removal of impurities, obtain product.
Do experiment with LIR2430 type button cell, gained negative material discharge capacity is 352.2mAh/g, and discharging efficiency is 94.2%, as shown in table 1.
embodiment 4:
Take retard petroleum coke raw material A 100kg, be ground into the meal that particle diameter is about 5mm.
Take asphalt stock B 5kg, carry out air-flow crushing, powder particle diameter≤3 μm.
Take the raw material A 60kg crushed, add raw material C 300g, carry out being uniformly mixed 30 minutes under normal temperature state, then at 2800 DEG C, carry out graphitization.
Take the mixed material 50kg after graphitization, carry out that fine powder is broken, classification, classification median is 16 μm, then carries out mechanical shaping 30min.
Take the mixed material 20kg after shaping, add raw material B micro mist 800g, carry out mixing 30min at normal temperatures, then at 300 ~ 600 DEG C, carry out modification, and then carbonize at 1300 DEG C.
After material after carbonizing is cooled to room temperature, carry out breaing up, sieve, removal of impurities, obtain product.
Do experiment with LIR2430 type button cell, gained negative material discharge capacity is 348.6mAh/g, and discharging efficiency is 94.3%, as shown in table 1.
embodiment 5:
Take retard petroleum coke raw material A 100kg, be ground into the meal that particle diameter is about 3mm.
Take asphalt stock B 5kg, carry out air-flow crushing, powder particle diameter≤3 μm.
Take the raw material A 60kg crushed, add raw material C 180g, carry out being uniformly mixed 30 minutes under normal temperature state, then at 3200 DEG C, carry out graphitization.
Take the mixed material 50kg after graphitization, carry out that fine powder is broken, classification, classification median is 13 μm, then carries out mechanical shaping 30min.
Take the mixed material 20kg after shaping, add raw material B micro mist 1200g, carry out mixing 30min at normal temperatures, then at 300 ~ 600 DEG C, carry out modification, and then carbonize at 1400 DEG C.
After material after carbonizing is cooled to room temperature, carry out breaing up, sieve, removal of impurities, obtain product.
Do experiment with LIR2430 type button cell, gained negative material discharge capacity is 352.1mAh/g, and discharging efficiency is 93.6%, as shown in table 1.
embodiment 6:
Take acicular petroleum coke raw material A 100kg, be ground into the meal that particle diameter is about 2mm.
Take asphalt stock B 5kg, carry out air-flow crushing, powder particle diameter≤3 μm.
Take the raw material A 60kg crushed, add raw material C 120g, carry out being uniformly mixed 30 minutes under normal temperature state, then at 2900 DEG C, carry out graphitization.
Take the mixed material 50kg after graphitization, carry out that fine powder is broken, classification, classification median is 14 μm, then carries out mechanical shaping 30min.
Take the mixed material 20kg after shaping, add raw material B micro mist 400g, carry out mixing 30min at normal temperatures, then at 300 ~ 600 DEG C, carry out modification, and then carbonize at 1300 DEG C.
After material after carbonizing is cooled to room temperature, carry out breaing up, sieve, removal of impurities, obtain product.
Do experiment with LIR2430 type button cell, gained negative material discharge capacity is 343.2mAh/g, and discharging efficiency is 94.3%, as shown in table 1.
embodiment 7:
Take acicular petroleum coke raw material A 100kg, be ground into the meal that particle diameter is about 1mm.
Take asphalt stock B 5kg, carry out air-flow crushing, powder particle diameter≤3 μm.
Take the raw material A 60kg crushed, add raw material C 360g, carry out being uniformly mixed 30 minutes under normal temperature state, then at 3000 DEG C, carry out graphitization.
Take the mixed material 50kg after graphitization, carry out that fine powder is broken, classification, classification median is 13 μm, then carries out mechanical shaping 30min.
Take the mixed material 20kg after shaping, add raw material B micro mist 400g, carry out mixing 30min at normal temperatures, then at 300 ~ 600 DEG C, carry out modification, and then carbonize at 1200 DEG C.
After material after carbonizing is cooled to room temperature, carry out breaing up, sieve, removal of impurities, obtain product.
Do experiment with LIR2430 type button cell, gained negative material discharge capacity is 347.9mAh/g, and discharging efficiency is 94.1%, as shown in table 1.
embodiment 8:
Take the rear petroleum coke raw material A 100kg of forging, be ground into the meal that particle diameter is about 0.5mm.
Take asphalt stock B 5kg, carry out air-flow crushing, powder particle diameter≤3 μm.
Take the raw material A 60kg crushed, add raw material C 420g, carry out being uniformly mixed 30 minutes under normal temperature state, then at 2800 DEG C, carry out graphitization.
Take the mixed material 50kg after graphitization, carry out that fine powder is broken, classification, classification median is 12 μm, then carries out mechanical shaping 30min.
Take the mixed material 20kg after shaping, add raw material B micro mist 400g, carry out mixing 30min at normal temperatures, then at 300 ~ 600 DEG C, carry out modification, and then carbonize at 1300 DEG C.
After material after carbonizing is cooled to room temperature, carry out breaing up, sieve, removal of impurities, obtain product.
Do experiment with LIR2430 type button cell, gained negative material discharge capacity is 349.8mAh/g, and discharging efficiency is 94.2%, as shown in table 1.
embodiment 9:
Take retard petroleum coke raw material A 100kg, be ground into the meal that particle diameter is about 1mm.
Take asphalt stock B 5kg, carry out air-flow crushing, powder particle diameter≤3 μm.
Take the raw material A 60kg crushed, add raw material C 540g, carry out being uniformly mixed 30 minutes under normal temperature state, then at 2800 DEG C, carry out graphitization.
Take the mixed material 50kg after graphitization, carry out that fine powder is broken, classification, classification median is 15 μm, then carries out mechanical shaping 30min.
Take the mixed material 20kg after shaping, add raw material B micro mist 600g, carry out mixing 30min at normal temperatures, then at 300 ~ 600 DEG C, carry out modification, and then carbonize at 1400 DEG C.
After material after carbonizing is cooled to room temperature, carry out breaing up, sieve, removal of impurities, obtain product.
Do experiment with LIR2430 type button cell, gained negative material discharge capacity is 350.6mAh/g, and discharging efficiency is 94.5%, as shown in table 1.
embodiment 10:
Take the rear petroleum coke raw material A 100kg of forging, be ground into the meal that particle diameter is about 1mm.
Take asphalt stock B 5kg, carry out air-flow crushing, powder particle diameter≤3 μm.
Take the raw material A 60kg crushed, add raw material C 180g, carry out being uniformly mixed 30 minutes under normal temperature state, then at 3200 DEG C, carry out graphitization.
Take the mixed material 50kg after graphitization, carry out that fine powder is broken, classification, classification median is 13 μm, then carries out mechanical shaping 30min.
Take the mixed material 20kg after shaping, add raw material B micro mist 1000g, carry out mixing 30min at normal temperatures, then at 300 ~ 600 DEG C, carry out modification, and then carbonize at 1200 DEG C.
After material after carbonizing is cooled to room temperature, carry out breaing up, sieve, removal of impurities, obtain product.
Do experiment with LIR2430 type button cell, gained negative material discharge capacity is 353.9mAh/g, and discharging efficiency is 94.2%, as shown in table 1.
subordinate list 1
button cell test data summary sheet
Claims (6)
1. a high-capacity lithium ion cell artificial plumbago negative pole material production method, concrete production technology is:
A () take petroleum coke as raw material A, raw material A is ground into the meal that particle diameter is 0.5 ~ 5.0mm;
B () take pitch as raw material B, pulverized by raw material B airslide disintegrating mill, is ground into the micro mist of particle diameter≤3 μm;
C (), with single transition metal micro mist or multiple transition metal admixed finepowder for raw material C, median is≤50nm;
The raw material C micro mist that d raw material A meal that (a) step obtains by () and (c) step obtain is by weight A/C=100/(0.2 ~ 1) ratio be uniformly mixed, at 2800 ~ 3200 DEG C, graphitization is carried out after mixing, pulverize after cooling, being ground into median is 12 ~ 18 μm;
The raw material B micro mist that e material that (d) step obtains by () and (b) step obtain, by weight (A+C)/B=100/(2 ~ 8) ratio mix, first at 300 ~ 600 DEG C, carries out modification after mixing, then carbonizes at 1200 ~ 1500 DEG C; Or mixing is direct afterwards to be carbonized at 1200 ~ 1500 DEG C;
F (), after the material that (e) step obtains is cooled to room temperature, is carried out breaing up, is sieved, removal of impurities, obtain product.
2. a kind of high-capacity lithium-ion artificial plumbago negative pole material production method as claimed in claim 1, is characterized in that: described raw material A is petroleum coke or needle coke after retard petroleum coke, forging.
3. a kind of high-capacity lithium-ion artificial plumbago negative pole material production method as claimed in claim 1, is characterized in that: described raw material B is petroleum asphalt or coal tar pitch.
4. a kind of high-capacity lithium-ion artificial plumbago negative pole material production method as claimed in claim 1, is characterized in that: described transition metal chooses V, Ni, Co.
5. a kind of high-capacity lithium-ion artificial plumbago negative pole material production method as claimed in claim 1, is characterized in that: the material that step (d) obtains, through graphitization and after pulverizing, carries out mechanical shaping process, makes granule-morphology regular, close to circular.
6. a kind of high-capacity lithium-ion artificial plumbago negative pole material production method as claimed in claim 1, is characterized in that: described in be uniformly mixed and adopt twin-screw or two ribbon agitating mode.
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| CN105272255A (en) * | 2015-10-23 | 2016-01-27 | 广西兴安县桂兴矿粉厂 | Manufacturing method of graphite electrode |
| CN109244392A (en) * | 2018-08-23 | 2019-01-18 | 武汉艾特米克超能新材料科技有限公司 | A kind of composite graphite negative electrode material and preparation method thereof and lithium ion battery |
| CN111048749A (en) * | 2019-10-30 | 2020-04-21 | 深圳市卓能新能源股份有限公司 | Negative pole piece, lithium ion battery and manufacturing method thereof |
| CN114725377A (en) * | 2022-04-20 | 2022-07-08 | 太原理工大学 | Transition metal regulated needle coke and preparation and application thereof |
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| CN102195036A (en) * | 2010-03-05 | 2011-09-21 | 宁波杉杉新材料科技有限公司 | Surface modified graphitized interphase carbon micro-powder and preparation method thereof |
| CN103066243A (en) * | 2012-12-06 | 2013-04-24 | 中南大学 | Coke powder-based cathode material of lithium ion power battery and preparation method thereof |
| KR20130056668A (en) * | 2011-11-22 | 2013-05-30 | 삼성전자주식회사 | Composite negative active material, method of preparing the same and lithium secondary battery comprising the same |
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| CN102195036A (en) * | 2010-03-05 | 2011-09-21 | 宁波杉杉新材料科技有限公司 | Surface modified graphitized interphase carbon micro-powder and preparation method thereof |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105272255A (en) * | 2015-10-23 | 2016-01-27 | 广西兴安县桂兴矿粉厂 | Manufacturing method of graphite electrode |
| CN109244392A (en) * | 2018-08-23 | 2019-01-18 | 武汉艾特米克超能新材料科技有限公司 | A kind of composite graphite negative electrode material and preparation method thereof and lithium ion battery |
| CN111048749A (en) * | 2019-10-30 | 2020-04-21 | 深圳市卓能新能源股份有限公司 | Negative pole piece, lithium ion battery and manufacturing method thereof |
| CN111048749B (en) * | 2019-10-30 | 2022-01-14 | 深圳市卓能新能源股份有限公司 | Negative pole piece, lithium ion battery and manufacturing method thereof |
| CN114725377A (en) * | 2022-04-20 | 2022-07-08 | 太原理工大学 | Transition metal regulated needle coke and preparation and application thereof |
| CN114725377B (en) * | 2022-04-20 | 2024-04-19 | 太原理工大学 | Needle coke regulated by transition metal and preparation and application thereof |
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| CN104900878B (en) | 2017-05-03 |
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