CN104393261B - Preparation method of Cox/(CoO)y/Cz composite lithium ion battery electrode material - Google Patents
Preparation method of Cox/(CoO)y/Cz composite lithium ion battery electrode material Download PDFInfo
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- CN104393261B CN104393261B CN201410564123.8A CN201410564123A CN104393261B CN 104393261 B CN104393261 B CN 104393261B CN 201410564123 A CN201410564123 A CN 201410564123A CN 104393261 B CN104393261 B CN 104393261B
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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
- H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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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
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/362—Composites
- H01M4/364—Composites as mixtures
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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
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/52—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
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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
- H01M4/587—Carbonaceous material, e.g. graphite-intercalation compounds or CFx for inserting or intercalating light metals
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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 relates to the technical field of lithium ion battery electrode materials, in particular to a preparation method of Cox/(CoO)y/Cz composite lithium ion battery electrode material. The preparation method comprises the following steps: firstly, kapok fiber subjected to purification treatment is immersed in a Co (NO3)2 solution with a certain concentration, the kapok fiber is taken out and drained off after the kapok fiber turns into uniformly pink, the diffusion of ammonia gas is utilized to obtain a precursor of cobalt hydroxide/carbon hydroxide, the heat treatment time is controlled to obtain the Cox/(CoO)y/Cz composite material. According to the preparation method of the Cox/(CoO)y/Cz composite lithium ion battery electrode material, provided by the invention, the Cox/(CoO)y/Cz composite anode material has the advantages of being good in reversibility of charge-discharge reaction, excellent in cycle performance, high in chemical reactivity, and simple in preparation process conditions.
Description
Technical field
The present invention relates to the preparing technical field of lithium ion battery electrode material, and in particular to a kind of Cox/(CoO)y/CzIt is multiple
Close the preparation method of lithium ion battery electrode material.
Background technology
Lithium ion battery is because being widely used in mobile electricity with the incomparable excellent properties of other traditional secondary batteries
Sub- equipment and electric vehicle field.Negative material, as the essential part of lithium ion battery, is always section
The focus that scholars study.And traditional carbon based negative electrodes materials theory specific capacity is relatively low, it is impossible to meet the current society for developing rapidly
People are to Large Copacity, the demand of heavy-duty battery in meeting.Transition metal oxide theoretical specific capacity is high as CoO theoretical specific capacities reach
To being 716mAhg-1, it is considered to be the great negative material for wishing to replace carbon material of a class.But, transition metal oxide exists
Volumetric expansion present in charge and discharge process, causes the structure of electrode material to be destroyed, and powder of detached then have impact on battery
Cyclical stability.The method of enhancing transition metal oxide chemical property is broadly divided into nanosizing and Composite two at present
Kind.
Preparing the method for transition metal oxide electrode material mainly has hydro-thermal method, sol-gel processing, ammonia revulsion, quiet
Electrical spinning method etc., these methods can prepare the nanostructured of different-shape.But, there is synthesis in these synthetic methods
The shortcomings of complex process, hardly possible operation, hardly possible control, this increased cost and difficulty for the preparation of transition metal oxide electrode material
Topic.
In recent years, investigation of materials person starts to turn one's attention to nature, from the angle that biological framework and living resources are effectively utilized
Degree sets out, it is proposed that synthesizes " biological template " new ideas of new material using biomaterial and biological phenomenon, makes full use of nature
Boundary's biomaterial appearance structure diversity is unique with functional character.It is directly special using plant, animal and microorganism etc. itself
Natural structure as template, by hereditary its chemical composition or pattern, prepared a series of new materials.It is rich in nature
In rich colorful native template, vegetable material has that renewable, environment-friendly, phosphorus content is high, specific surface area is big, porous, moisture
The series of advantages such as storage and transport.Research finds that part natural plant material also has micro-tubular structure, when these micro-pipes and liquid
When body surface face contacts, more obvious " capillarity " can be produced, liquid enters micro-pipe because of capillarity.When micro-pipe and liquid
After body is disengaged, liquid can't be lost in micro-pipe, and liquid is full of whole micro-pipe.By " biological template " concept with " capillary is existing
As " inspiration, using bombax cotton as carbon source and template, using bombax cotton phosphorus content is high and capillarity, it is special to prepare
The Co of structurex/(CoO)y/CzComposite is expected to improve chemical property.
The content of the invention
For the deficiencies in the prior art, object of the present invention is to provide a kind of Cox/(CoO)y/CzComplex lithium
The preparation method of ion battery electrode materials, gained negative material have discharge and recharge reaction good reversibility, cycle performance it is excellent, change
Learn many advantages, such as reactivity is high, preparation process condition is simple.
The purpose of the present invention technical scheme is that.
A kind of Cox/(CoO)y/CzComposite lithium ion battery material preparation method, its step is as follows：
(1) bombax cotton is put into sonic oscillation 0.5~1 hour in deionized water, is taken out, length is cut into after drying
The about segment of 2~5mm, and be scattered in absolute ethyl alcohol, sonic oscillation 0.5~1 hour.
(2) configuration substance withdrawl syndrome is the Co (NO of 2~4mol/L3)2Solution.
(3) bombax cotton once purged in step (1) is pulled out from absolute ethyl alcohol, drains surface liquid, soaked completely
Enter the Co (NO for preparing3)2In solution.
Taken out after bombax cotton becomes uniform pink, drain surface liquid.
(4) bombax cotton after step (3) gained is drained is placed in concentrated ammonia liquor top, using the diffusion of ammonia, makes kapok
The cobalt nitrate contained in fiber reacts with ammonia, when the color of bombax cotton turns into blue-green, reaction is stopped immediately, obtains hydrogen
The presoma of cobalt oxide/bombax cotton.
(5) presoma that step (4) is obtained is put into graphite boat, is placed in tube furnace after good seal, protected in inert atmosphere
Under shield, 500~800 DEG C are warming up to certain heating rate, are then incubated 1~4 hour, preferably 3~4 hours.Cool to the furnace
Taken out after room temperature.
(6) it is to obtain final product Co by hand lapping Cheng Fenhou by the product of step (5)x/(CoO)y/CzComplex lithium
Ion battery electrode materials.
The inert atmosphere conditions are nitrogen or argon gas atmosphere.
Heating rate is 5 DEG C/min in the step (5).
The mass percent concentration of the concentrated ammonia liquor is 25%~28%.
Products therefrom is named as Cox/(CoO)y/CzBecause with the extension of soaking time, chemical composition can change
Become, the ultimate constituent may simultaneously contain CoO and Co if soaking time is short, be named as Co@CoO/C；Soaking time is lengthened, most
End-product chemical composition may comprise only Co, be Co/C without CoO.
Compared with prior art, the advantage of the inventive method is with beneficial effect：
The present invention is a kind of Cox/(CoO)y/CzThe preparation method of composite lithium ion battery material, by natural kapok
Fiber simultaneously as biological template and carbon source, using bombax cotton phosphorus content is high and capillarity, with reference to micro- test tube reaction method,
Nano particle is successfully loaded on hollow tubular fiber wall, the heating and thermal insulation time is controlled, so as to prepare Cox/(CoO)y/Cz
Composite nano materials.The bombax cotton for being used as biological template itself and do not have bioactivity, but its tube wall is still
The nano Co or CoO particles of generation can successfully be coated, this for other inactive biological template materials are provided it is theoretical according to
According to and experiment basis, expanded the range of application of biological template.In heat treatment process, bombax cotton is conduction through pyrolytic conversion
Property good amorphous " carbon skeleton ", and for the generation of nano particle provides reductive condition.By to Cox/(CoO)y/Cz
Electrode carries out electrochemical property test, draws the Co of the special construction pattern prepared by the present inventionx/(CoO)y/CzComposite Nano material
Material has good cycle performance and excellent high rate performance.
Brief description of the drawings
Fig. 1, Fig. 2 are the ESEM of the products C o@CoO/C composite lithium ion battery materials obtained by embodiment 1
Picture.
Fig. 3 is the transmission electron microscope picture of the products C o CoO/C composite lithium ion battery materials obtained by embodiment 1.
Fig. 4 is the X-ray diffractogram of the products C o@CoO/C composite lithium ion battery materials obtained by embodiment 1
Piece.
Fig. 5, Fig. 6 are the products C o/C composite lithium ion battery scanning of materials electron microscopic pictures obtained by embodiment 2.
Fig. 7 is the transmission electron microscope picture of the products C o/C composite lithium ion battery materials obtained by embodiment 2.
Fig. 8 is the X-ray diffraction picture of the products C o/C composite lithium ion battery materials obtained by embodiment 2.
Fig. 9 is the circulation curve of the products C o@CoO/C composite lithium ion battery materials obtained by embodiment 1
Figure.
Products C o@CoO/C composite lithium ion battery materials of the Figure 10 obtained by embodiment 1 is under the conditions of 0.1A/g
Discharge curve.
Figure 11 is products C o/C composite lithium ion battery material the putting under the conditions of 0.1A/g obtained by embodiment 2
Electric curve.
Figure 12 is the scanning electron microscopic picture of the products C oO/C composite lithium ion battery materials obtained by embodiment 3.
Figure 13 is the scanning electron microscopic picture of the products C oO/C composite lithium ion battery materials obtained by embodiment 4.
Fig. 1 and Fig. 2 can be seen that tube wall inner homogeneous and be dispersed with flakey white particulate material, and size scope 2~
200nm.The high-resolution-ration transmission electric-lens picture of Fig. 3 can be seen that on amorphous carbon clearly lattice fringe occur, show particle knot
Brilliant degree is good.The X-ray diffraction picture of Fig. 4 can be seen that diffraction maximum of the material at 36.5 °, 42.4 ° and 61.5 ° is right respectively
Answer (111), (200) and (220) crystal face of CoO.(111) crystal face of diffraction maximum correspondence Co at 44.2 °.Fig. 5, Fig. 6 show
The scanning electron microscopic picture of embodiment 2, it can be seen that tablet is evenly distributed on and loose structure is formed on tube wall.The high score of Fig. 7
Transmission electron microscope picture is distinguished it can be seen that the crystal grain inlayed of amorphous carbon clearly lattice fringe, shows that grain crystalline degree is good
It is good.The X-ray diffraction picture of Fig. 8 can be seen that (111) crystal face of diffraction maximum correspondence Co of the material at 44.2 °.Fig. 9 is real
The circulation curve of example 1 is applied, in many circulation discharge processes, Co@CoO/C discharge capacities are with putting for Co@CoO/C electrodes
The increase of electric multiplying power and reduce, by after 50 ladder circulations, when current density comes back to 0.1Ag-1When, Co@
CoO/C discharge capacities substantially resume to original state, and capability retention is 96.94%.Figure 10 can be seen that in 0.1Ag-1Electricity
Under current density, Co@CoO/C keep good cyclical stability, and after 50 times, Co@CoO/C electrode reversible discharge capacities reach
308.1mAh/g, flushes with initial discharge capacity substantially.Figure 11 is the cyclic curve of embodiment 2, as seen from the figure Co/C tools
There is good cyclical stability, in 0.1Ag-1Under current density, after 50 circulations, Co/C electrode discharges capacity is 392mAh/
G, compared with secondary 429.1mAh/g, capability retention is 91.3%.
In transition processes of the Co@CoO/C to Co/C composites, the extension of soaking time causes that CoO is final by carbon reduction
It is completely converted into nano-scale cobalt granule.Co/C nano particles chemical property is more excellent than Co@CoO/C chemical properties,
One side Co is firmly embedded in kapok carbon tube wall, and in cyclic process, kapok has fabulous buffering as carbon source and masterplate
Effect；Another aspect Co/C is bigger compared with the load capacity of Co@CoO/C, with loose structure.
Specific embodiment
Applicant will be described in further detail to the inventive method in conjunction with specific embodiments below, it is therefore intended that make
Those skilled in the art are it can be clearly understood that the present invention.But following examples should not be understood to this hair in any degree
Bright claims are claimed the limitation of scope.
Medicine used is all purchased from Chemical Reagent Co., Ltd., Sinopharm Group in following examples.
The raw material bombax cotton of embodiment 1-4 derives from Hubei Province Xiaogan City surrounding area, is collected from natural silk cotton tree
.
It is that 28%, embodiment 2 is that 28%, embodiment 3 is that the mass percent concentration of concentrated ammonia liquor used is respectively embodiment 1
25%th, embodiment 4 is 26%.
Embodiment 1
A kind of Cox/(CoO)y/CzThe preparation method of composite lithium ion battery material, its step is as follows：
Bombax cotton is put into sonic oscillation 0.5 hour in deionized water first, is cleaned up, taken out, by it after drying
It is cut into length and is about the segment of 2~5mm, and is scattered in absolute ethyl alcohol, sonic oscillation 0.5 hour.Configuration concentration is
Co (the NO of 3.4mol/L3)2Solution, bombax cotton is pulled out from absolute ethyl alcohol, drains surface liquid, and bombax cotton is complete
Co (the NO that immersion is prepared3)2In solution.Taken out after bombax cotton becomes uniform pink, drain surface liquid.Then will
Bombax cotton after draining is placed in concentrated ammonia liquor top, using the diffusion of ammonia, makes the cobalt nitrate and ammonia that contain in bombax cotton
Reaction, when the color of bombax cotton turns into blue-green, stops reaction immediately, obtains the presoma of cobalt hydroxide/bombax cotton.
Then, presoma is put into graphite boat, is placed in tube furnace after good seal, under flowing nitrogen atmosphere protection, with 5 DEG C of min-1
Speed be warming up to 500 DEG C, be incubated 2 hours.Cool to the furnace and take out after room temperature, then must after product is manually pulverized
To final product Co@CoO/C composite lithium ion battery materials.
Embodiment 2
A kind of Cox/(CoO)y/CzThe preparation method of composite lithium ion battery material, its step is as follows：
Bombax cotton is put into sonic oscillation 1 hour in deionized water first, is cleaned up, taken out, cut after drying
It is about the segment of 2~5mm into length, and is scattered in absolute ethyl alcohol, sonic oscillation 0.5 hour.Configuration concentration is
Co (the NO of 3.4mol/L3)2Solution, bombax cotton is pulled out from absolute ethyl alcohol, drains surface liquid, and bombax cotton is complete
Co (the NO that immersion is prepared3)2In solution.Taken out after bombax cotton becomes uniform pink, drain surface liquid.Then will
Bombax cotton after draining is placed in concentrated ammonia liquor top, using the diffusion of ammonia, makes the cobalt nitrate and ammonia that contain in bombax cotton
Reaction, when the color of bombax cotton turns into blue-green, stops reaction immediately, obtains the presoma of cobalt hydroxide/bombax cotton.
Then, presoma is put into graphite boat, is placed in tube furnace after good seal, under flowing argon gas atmosphere protection, with 5 DEG C of min-1
Speed be warming up to 500 DEG C, be incubated 4 hours.Cool to the furnace and take out after room temperature, then must after product is manually pulverized
To final product Co/C composite lithium ion battery materials.
Embodiment 3
A kind of Cox/(CoO)y/CzThe preparation method of composite lithium ion battery material, its step is as follows：
Bombax cotton is put into sonic oscillation 0.5 hour in deionized water first, is cleaned up, taken out, by it after drying
It is cut into length and is about the segment of 2~5mm, and is scattered in absolute ethyl alcohol, sonic oscillation 1 hour.Configuration concentration is
Co (the NO of 2.4mol/L3)2Solution, bombax cotton is pulled out from absolute ethyl alcohol, drains surface liquid, and bombax cotton is complete
Co (the NO that immersion is prepared3)2In solution.Taken out after bombax cotton becomes uniform pink, drain surface liquid.Then will
Bombax cotton after draining is placed in concentrated ammonia liquor top, using the diffusion of ammonia, makes the cobalt nitrate and ammonia that contain in bombax cotton
Reaction, when the color of bombax cotton turns into blue-green, stops reaction immediately, obtains the presoma of cobalt hydroxide/bombax cotton.
Then, presoma is put into graphite boat, is placed in tube furnace after good seal, under flowing nitrogen atmosphere protection, with 5 DEG C of min-1
Speed be warming up to 700 DEG C, be incubated 3 hours.Cool to the furnace and take out after room temperature, then must after product is manually pulverized
To final product Co/C composite lithium ion battery materials, product is detected through XRD and confirmed, as a result essentially identical with Fig. 8.
Embodiment 4
A kind of Cox/(CoO)y/CzThe preparation method of composite lithium ion battery material, its step is as follows：
Bombax cotton is put into sonic oscillation 0.5 hour in deionized water first, is cleaned up, taken out, by it after drying
It is cut into length and is about the segment of 2~5mm, and is scattered in absolute ethyl alcohol, sonic oscillation 0.5 hour.Configuration concentration is
Co (the NO of 3mol/L3)2Solution, bombax cotton is pulled out from absolute ethyl alcohol, drains surface liquid, and bombax cotton is soaked completely
Enter the Co (NO for preparing3)2In solution.Taken out after bombax cotton becomes uniform pink, drain surface liquid.Then will drip
Bombax cotton after dry is placed in concentrated ammonia liquor top, using the diffusion of ammonia, makes the cobalt nitrate contained in bombax cotton anti-with ammonia
Should, when the color of bombax cotton turns into blue-green, reaction is stopped immediately, obtain the presoma of cobalt hydroxide/bombax cotton.With
Afterwards, presoma is put into graphite boat, is placed in tube furnace after good seal, under flowing argon gas atmosphere protection, with 5 DEG C of min-1's
Speed is warming up to 800 DEG C, is incubated 4 hours.Cool to the furnace and take out after room temperature, then just obtain after product is manually pulverized
Final product Co/C composite lithium ion battery materials, product is detected through XRD and confirmed, as a result essentially identical with Fig. 8.
Sample obtained in embodiment 1~4 is made into half-cell respectively carries out chemical property measure, half-cell assembly method
It is as follows：By testing sample, Super P Li conductive blacks (Te Migao), PVDF (A Kema Kynoar binding agents
HSV900 types) in mass ratio it is 85%：10%：5% mixing, is mixed well with 1-METHYLPYRROLIDONE, stirs into thick, is applied
On Copper Foil, dried 6 hours at 60 DEG C of vacuum (- 0.1MPa), the circular film of diameter about 1cm is cut into after cooling.Half-cell exists
Assembled using CR2016 types button cell in glove box, barrier film is the polypropylene diaphragms of Celgard 2400, and electrolyte is containing 1M
LiPF6Ethylene carbonate (EC) (volume ratio of EC, DEC is in mixed electrolytic solution with diethyl carbonate (DEC) mixed electrolytic solution
1:1), negative pole is commercialization circle lithium piece (diameter 1.5cm), and electrochemical property test is in blue electricity CT2001A type battery testings system
Carried out on system (Wuhan Land Electronic Co., Ltd.'s production).
Claims (4)
1. a kind of Co/C composite lithium ion batteries material preparation method, its step is as follows：
（1）Bombax cotton is put into sonic oscillation 0.5 ~ 1 hour in deionized water, is taken out, be cut into after drying length for 2 ~
The segment of 5mm, and be scattered in absolute ethyl alcohol, sonic oscillation 0.5 ~ 1 hour；
(2) configuration amount of substance concentration is the Co (NO of 2 ~ 4mol/L3)2Solution；
(3) bombax cotton once purged in step (1) is pulled out from absolute ethyl alcohol, drains surface liquid, be completely immersed in the Co (NO that step (2) is prepared3)2In solution；
Taken out after bombax cotton becomes uniform pink, drain surface liquid；
（4）By step（3）Bombax cotton after gained is drained is placed in concentrated ammonia liquor top, and the diffusion using ammonia in micro-pipe makes
The cobalt nitrate solution contained in bombax cotton reacts with ammonia, when the color of bombax cotton turns into blue-green, stops immediately anti-
Should, obtain the presoma of cobalt hydroxide/bombax cotton；
（5）By step（4）The presoma for obtaining is put into graphite boat, is placed in tube furnace after good seal, under inert atmosphere protection,
500~800 DEG C are warming up to certain heating rate, then 3~4 hours is incubated, taken out after cooling to room temperature with the furnace；
（6）By step（5）Product be to obtain final product Co/C composite lithium ion batteries by hand lapping Cheng Fenhou
Material.
2. the preparation method according to right wants 1, it is characterised in that：The inert atmosphere conditions are nitrogen or argon gas gas
Atmosphere.
3. the preparation method according to right wants 1, it is characterised in that:The step(5) in heating rate be 5 DEG C/min.
4. the preparation method according to right wants 1, it is characterised in that: the mass percent concentration of the concentrated ammonia liquor is 25% ~ 28%.
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| CN106711424B (en) * | 2017-01-12 | 2019-10-18 | 青岛大学 | A kind of cobalt protoxide base nano-complex electrode material and preparation method thereof |
| CN106972177B (en) * | 2017-04-07 | 2019-06-28 | 武汉理工大学 | A kind of CoO/Co/C trielement composite material and its preparation method and application |
| CN110931798B (en) * | 2019-12-12 | 2020-10-09 | 哈尔滨理工大学 | Preparation method of 3DPC/Co/CoO lithium battery negative electrode material |
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| CN103331162B (en) * | 2013-06-17 | 2015-03-18 | 中国科学院上海硅酸盐研究所 | Mesoporous Co3O4/C composite material with high specific surface and crystallization hole wall and preparation method of material |
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