CN114142012A - Preparation method of lithium ion negative electrode material without graphitization - Google Patents
Preparation method of lithium ion negative electrode material without graphitization Download PDFInfo
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- 239000007773 negative electrode material Substances 0.000 title claims abstract description 38
- 238000005087 graphitization Methods 0.000 title claims abstract description 20
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 title claims abstract description 16
- 229910001416 lithium ion Inorganic materials 0.000 title claims abstract description 16
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 41
- 238000003763 carbonization Methods 0.000 claims abstract description 24
- 238000000034 method Methods 0.000 claims abstract description 18
- 238000005245 sintering Methods 0.000 claims abstract description 17
- 229910052744 lithium Inorganic materials 0.000 claims abstract description 16
- 238000005406 washing Methods 0.000 claims abstract description 15
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000000843 powder Substances 0.000 claims abstract description 14
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims abstract description 13
- 238000005554 pickling Methods 0.000 claims abstract description 13
- 238000002156 mixing Methods 0.000 claims abstract description 12
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 10
- 239000010439 graphite Substances 0.000 claims abstract description 10
- 239000003575 carbonaceous material Substances 0.000 claims abstract description 9
- 239000000126 substance Substances 0.000 claims abstract description 9
- 239000004115 Sodium Silicate Substances 0.000 claims abstract description 8
- 239000002253 acid Substances 0.000 claims abstract description 8
- 239000008367 deionised water Substances 0.000 claims abstract description 8
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 8
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229910052911 sodium silicate Inorganic materials 0.000 claims abstract description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000006258 conductive agent Substances 0.000 claims abstract description 7
- 239000000835 fiber Substances 0.000 claims abstract description 7
- 239000011230 binding agent Substances 0.000 claims abstract description 6
- 238000002791 soaking Methods 0.000 claims abstract description 5
- 239000000203 mixture Substances 0.000 claims abstract description 4
- 229910052751 metal Inorganic materials 0.000 claims description 8
- 239000002184 metal Substances 0.000 claims description 8
- 239000002245 particle Substances 0.000 claims description 8
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical group [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 6
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 6
- 230000000694 effects Effects 0.000 claims description 4
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 3
- 125000004432 carbon atom Chemical group C* 0.000 claims description 3
- XTEGARKTQYYJKE-UHFFFAOYSA-N chloric acid Chemical compound OCl(=O)=O XTEGARKTQYYJKE-UHFFFAOYSA-N 0.000 claims description 3
- 229940005991 chloric acid Drugs 0.000 claims description 3
- 229910017604 nitric acid Inorganic materials 0.000 claims description 3
- 238000011010 flushing procedure Methods 0.000 claims description 2
- 239000002952 polymeric resin Substances 0.000 claims description 2
- 229920003002 synthetic resin Polymers 0.000 claims description 2
- 239000000853 adhesive Substances 0.000 claims 1
- 230000001070 adhesive effect Effects 0.000 claims 1
- 229910021383 artificial graphite Inorganic materials 0.000 abstract description 9
- 238000005265 energy consumption Methods 0.000 abstract description 4
- 239000010405 anode material Substances 0.000 abstract description 3
- 238000000265 homogenisation Methods 0.000 abstract description 2
- 238000004140 cleaning Methods 0.000 abstract 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 14
- 239000000377 silicon dioxide Substances 0.000 description 7
- 235000012239 silicon dioxide Nutrition 0.000 description 7
- 241000196324 Embryophyta Species 0.000 description 5
- 229910052799 carbon Inorganic materials 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- 239000003245 coal Substances 0.000 description 3
- 229910021382 natural graphite Inorganic materials 0.000 description 3
- 239000011148 porous material Substances 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 239000010703 silicon Substances 0.000 description 3
- 229910052710 silicon Inorganic materials 0.000 description 3
- 239000004484 Briquette Substances 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000004146 energy storage Methods 0.000 description 2
- 238000005469 granulation Methods 0.000 description 2
- 230000003179 granulation Effects 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000007774 positive electrode material Substances 0.000 description 2
- 238000012216 screening Methods 0.000 description 2
- 235000017166 Bambusa arundinacea Nutrition 0.000 description 1
- 235000017491 Bambusa tulda Nutrition 0.000 description 1
- 241001330002 Bambuseae Species 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 229920000742 Cotton Polymers 0.000 description 1
- 229910000733 Li alloy Inorganic materials 0.000 description 1
- 235000015334 Phyllostachys viridis Nutrition 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 239000002194 amorphous carbon material Substances 0.000 description 1
- RHZUVFJBSILHOK-UHFFFAOYSA-N anthracen-1-ylmethanolate Chemical compound C1=CC=C2C=C3C(C[O-])=CC=CC3=CC2=C1 RHZUVFJBSILHOK-UHFFFAOYSA-N 0.000 description 1
- 239000003830 anthracite Substances 0.000 description 1
- 239000010426 asphalt Substances 0.000 description 1
- 238000000498 ball milling Methods 0.000 description 1
- 239000011425 bamboo Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000010406 cathode material Substances 0.000 description 1
- 239000011280 coal tar Substances 0.000 description 1
- 239000000571 coke Substances 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 239000002737 fuel gas Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- PQTCMBYFWMFIGM-UHFFFAOYSA-N gold silver Chemical compound [Ag].[Au] PQTCMBYFWMFIGM-UHFFFAOYSA-N 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000004898 kneading Methods 0.000 description 1
- 239000001989 lithium alloy Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000011255 nonaqueous electrolyte Substances 0.000 description 1
- 239000002006 petroleum coke Substances 0.000 description 1
- 238000010248 power generation Methods 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- ABTOQLMXBSRXSM-UHFFFAOYSA-N silicon tetrafluoride Chemical compound F[Si](F)(F)F ABTOQLMXBSRXSM-UHFFFAOYSA-N 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000002344 surface layer Substances 0.000 description 1
Classifications
-
- 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
-
- 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
- C01B32/05—Preparation or purification of carbon not covered by groups C01B32/15, C01B32/20, C01B32/25, C01B32/30
-
- 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
-
- 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
- H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
- H01M4/386—Silicon or alloys based on silicon
-
- 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
-
- 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
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
- H01M4/625—Carbon or graphite
-
- 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 provides a preparation method of a lithium ion negative electrode material without graphitization, and relates to a negative electrode material domain. The preparation method of the lithium ion negative electrode material without graphitization comprises the following steps: putting the plant fiber into a carbonization furnace for carbonization treatment to obtain a carbon material; crushing and pickling: crushing a carbon material into powder, then carrying out acid washing, and then cleaning with deionized water to obtain pure carbon powder; mixing: mixing pure carbon powder into a sodium silicate solution, then carrying out homogenization treatment by using a homogenizer, and then placing the homogenized mixture into a graphite crucible; and (3) sintering: transferring the graphite crucible to a sintering furnace, and taking out a sintered body after sintering; and (3) crushing and pickling again: crushing the sintered body into powder, soaking and pickling with hydrofluoric acid, and washing with deionized water to obtain porous carbon powder; obtaining an anode material: and mixing the porous carbon powder with a conductive agent, a binder and a lithium simple substance to obtain a negative electrode material product. Compared with the high-temperature preparation of artificial graphite, the method can reduce energy consumption.
Description
Technical Field
The invention relates to the technical field of negative electrode materials, in particular to a preparation method of a lithium ion negative electrode material without graphitization.
Background
A lithium battery is a type of battery using a nonaqueous electrolyte solution, using lithium metal or a lithium alloy as a positive/negative electrode material. The great power development of new energy power generation can bring great consumption pressure, and an energy storage system is an effective way for solving the consumption problem. The lithium battery is the existing storage battery with outstanding capacity and safety. Therefore, the lithium battery is indispensable in the field of energy storage.
The material cost is large in proportion to the cost of the lithium battery, and is mainly composed of a positive electrode material, a negative electrode material, a diaphragm and electrolyte. The anode material of the existing lithium battery mostly adopts artificial graphite, the manufacturing process of the artificial graphite can be divided into four major steps and more than ten minor procedures, and granulation and graphitization are key. The production process of the artificial graphite cathode material can be divided into four steps: 1. pretreatment, 2, granulation, 3, graphitization and 4, ball milling and screening. In the graphitization production, anthracite, coke or petroleum coke is used as a raw material, the raw material is crushed, added with coal tar and asphalt for kneading, extruded or compression molded, and roasted at 800-1300 ℃ for about 200-250 h to obtain the amorphous carbon material. And roasting at 2400-2800 ℃ for 60-70 h to crystallize carbon (generally called graphitization treatment) so as to obtain the graphite. The artificial graphite has the defects of high energy consumption, environmental pollution and high cost in production.
Disclosure of Invention
Technical problem to be solved
Aiming at the defects of the prior art, the invention provides a preparation method of a lithium ion negative electrode material without graphitization, and solves the problem of high energy consumption when the artificial graphite is adopted to produce the negative electrode material.
(II) technical scheme
In order to achieve the purpose, the invention is realized by the following technical scheme: a preparation method of a lithium ion negative electrode material without graphitization comprises the following steps:
step one, carbonization: putting the plant fiber into a carbonization furnace for carbonization treatment to obtain a carbon material;
step two, crushing and pickling: crushing a carbon material into powder, then carrying out acid washing for 2-3 times, and then washing and flushing for 2-3 times by using deionized water to obtain pure carbon powder;
step three, mixing: mixing pure carbon powder into a sodium silicate solution, wherein the molar mass ratio of carbon atoms to silicon atoms is 1: 0.85-1, then homogenizing by using a homogenizer, and then placing the homogenized mixture in a graphite crucible for later use;
step four, sintering: transferring the graphite crucible into a sintering furnace, wherein the sintering time is 8-12 h, the furnace is cooled for 2-3 h, and taking out a sintered body for later use;
step five, crushing and pickling again: crushing the sintered body into powder, soaking and pickling for 2-3 times by using hydrofluoric acid, and then washing for 2-3 times by using deionized water to obtain porous carbon powder;
step six, obtaining a negative electrode material: and mixing the porous carbon powder with a conductive agent, a binder and a lithium simple substance to obtain a negative electrode material product.
Preferably, the carbonization temperature in the first step is 500-650 ℃, and the carbonization time is 10-15 h.
Preferably, the average particle size of the carbon powder in the second step is 0.1-1 μm, and one or more of sulfuric acid, chloric acid and nitric acid is used in the acid washing.
Preferably, in the third step, the homogenization treatment is carried out for 2-4 hours under the reciprocating change of 0.8-1.2 MPa.
Preferably, the sintering temperature in the fourth step is 800-1000 ℃.
Preferably, the average particle size of the porous carbon powder in the fifth step is 10 +/-5 microns.
Preferably, in the sixth step, the conductive agent is a metal simple substance with a metal activity smaller than that of lithium, and the binder is polymer resin.
(III) advantageous effects
The invention provides a preparation method of a lithium ion negative electrode material without graphitization. The method has the following beneficial effects:
1. according to the invention, the plant fiber is adopted for carbonization treatment, and compared with coal blocks, the obtained carbon material is easy to crush.
2. According to the invention, carbon powder and sodium silicate solution are mixed, and hydrofluoric acid is used for dissolving silicon dioxide after sintering, so that the sintered body is a porous material.
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.
The first embodiment is as follows:
the embodiment of the invention provides a preparation method of a lithium ion negative electrode material without graphitization, which comprises the following steps:
step one, carbonization: the plant fiber is placed in a carbonization furnace for carbonization treatment, and the plant fiber is adopted for carbonization treatment, so that firstly, the plant fiber is easy to obtain, secondly, the coal briquette is relatively directly used, because the coal briquette is buried underground for a long time, the hardness is high, the crushing difficulty is high, cotton and bamboo can be preferentially selected as carbonization raw materials, the carbonization temperature is 500-650 ℃, the medium-temperature carbonization is adopted, the carbonization speed is ensured, the energy consumption can be reduced, meanwhile, the fuel gas produced in the carbonization treatment process can be used as fuel for carbonization heating, the time is 10-15 h, the full carbonization is ensured, and the carbon material is obtained;
step two, crushing and pickling: crushing a carbon material into powder, wherein the average particle size of carbon powder is 0.1-1 mu m, screening after crushing, removing large-particle materials, then carrying out acid washing for 2-3 times, removing other non-carbon elements as much as possible, using one or more of sulfuric acid, chloric acid and nitric acid in the acid washing, selecting multiple acids, improving the fault tolerance of non-carbon element removal, and then washing and washing for 2-3 times by using deionized water to obtain pure carbon powder;
step three, mixing: mixing pure carbon powder into a sodium silicate solution, wherein the molar mass ratio of carbon atoms to silicon atoms is 1: 0.85-1, then homogenizing by using a homogenizer to uniformly distribute the carbon powder and the sodium silicate, homogenizing for 2-4 h under the reciprocating change of 0.8-1.2 MPa, and then placing the homogenized mixture in a graphite crucible for later use;
step four, sintering: transferring the graphite crucible into a sintering furnace, wherein the sintering temperature is 800-1000 ℃, so that a system with uniformly distributed carbon powder and sodium silicate is solidified, simultaneously, the sodium silicate is dehydrated into silicon dioxide in the sintering process, the sintering time is 8-12 h, the furnace is cooled for 2-3 h, and a sintered body is taken out for standby;
step five, crushing and pickling again: crushing the sintered body into powder with the average particle size of 10 +/-5 microns, soaking and pickling for 2-3 times by using hydrofluoric acid, reacting the hydrofluoric acid with silicon dioxide to generate silicon fluoride gas, removing silicon dioxide to leave pores, enabling the powder to be a porous structure, soaking and pickling by using the hydrofluoric acid, wherein the silicon dioxide still exists in the powder, namely the surface layer of the powder is a porous structure of carbon, the inside of the powder is a homogeneous body of the silicon dioxide and the carbon, and the silicon dioxide exists, so that the overall structural strength of the powder can be improved, and then washing for 2-3 times by using deionized water to obtain porous carbon powder, namely the porous carbon powder has the average particle size of 10 +/-5 microns and is similar to graphite in function;
step six, obtaining a negative electrode material: the porous carbon powder is mixed with a conductive agent, a binding agent and a lithium simple substance, the conductive agent is a metal simple substance with metal activity smaller than that of lithium, the metal simple substance is preferably nanoscale powder of copper and silver gold, the metal simple substance and the lithium metal enter pores of carbon powder to be fixed in the mixing process, the lithium metal can be favorably embedded and separated in the sufficient electricity of the battery, and the binding agent is high molecular resin to obtain a negative electrode material product.
Example two:
three samples were randomly obtained from the anode material product produced according to example one and subjected to the experiment, and the results are shown in table 1:
TABLE 1 sample data
Table 2 shows the properties of the natural graphite negative electrode material, the artificial graphite negative electrode material, and the silicon-based negative electrode material.
| Type (B) | Natural graphite negative electrode material | Artificial graphite negative electrode material | Silicon-based negative electrode material |
| Theoretical capacity | 340～370mAh/g | 310～360mAh/g | 300～4000mAh/g |
| First time efficiency | ＞93％ | ＞93％ | ＞77％ |
As shown in tables 1 and 2, the produced negative electrode material for lithium batteries has a small difference in performance from the existing natural graphite negative electrode material, artificial graphite negative electrode material, and silicon-based negative electrode material.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (7)
1. A preparation method of a lithium ion negative electrode material without graphitization is characterized by comprising the following steps:
step one, carbonization: putting the plant fiber into a carbonization furnace for carbonization treatment to obtain a carbon material;
step two, crushing and pickling: crushing a carbon material into powder, then carrying out acid washing for 2-3 times, and then washing and flushing for 2-3 times by using deionized water to obtain pure carbon powder;
step three, mixing: mixing pure carbon powder into a sodium silicate solution, wherein the molar mass ratio of carbon atoms to silicon atoms is 1: 0.85-1, then homogenizing by using a homogenizer, and then placing the homogenized mixture in a graphite crucible for later use;
step four, sintering: transferring the graphite crucible into a sintering furnace, wherein the sintering time is 8-12 h, the furnace is cooled for 2-3 h, and taking out a sintered body for later use;
step five, crushing and pickling again: crushing the sintered body into powder, soaking and pickling for 2-3 times by using hydrofluoric acid, and then washing for 2-3 times by using deionized water to obtain porous carbon powder;
step six, obtaining a negative electrode material: and mixing the porous carbon powder with a conductive agent, a binder and a lithium simple substance to obtain a negative electrode material product.
2. The method for preparing a lithium ion negative electrode material without graphitization according to claim 1, wherein the method comprises the following steps: the carbonization temperature in the first step is 500-650 ℃, and the carbonization time is 10-15 h.
3. The method for preparing a lithium ion negative electrode material without graphitization according to claim 1, wherein the method comprises the following steps: and in the second step, the average particle size of the carbon powder is 0.1-1 mu m, and one or more of sulfuric acid, chloric acid and nitric acid is used in acid washing.
4. The method for preparing a lithium ion negative electrode material without graphitization according to claim 1, wherein the method comprises the following steps: and in the third step, homogenizing for 2-4 hours under the reciprocating change of 0.8-1.2 MPa.
5. The method for preparing a lithium ion negative electrode material without graphitization according to claim 1, wherein the method comprises the following steps: and the sintering temperature in the fourth step is 800-1000 ℃.
6. The method for preparing a lithium ion negative electrode material without graphitization according to claim 1, wherein the method comprises the following steps: the average particle size of the porous carbon powder in the step five is 10 +/-5 mu m.
7. The method for preparing a lithium ion negative electrode material without graphitization according to claim 1, wherein the method comprises the following steps: in the sixth step, the conductive agent is a metal simple substance with metal activity smaller than that of lithium, and the adhesive is polymer resin.
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| CN108996504A (en) * | 2018-08-31 | 2018-12-14 | 广东工业大学 | A kind of absorbent charcoal material and its preparation method and application of porous structure Heteroatom doping |
| CN110835107A (en) * | 2019-12-02 | 2020-02-25 | 吉林大学 | Biomass porous carbon material and preparation method thereof |
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