CN110034290A - A kind of preparation method of sodium-ion battery self-supporting hard carbon cathode material - Google Patents
A kind of preparation method of sodium-ion battery self-supporting hard carbon cathode material Download PDFInfo
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- CN110034290A CN110034290A CN201910333330.5A CN201910333330A CN110034290A CN 110034290 A CN110034290 A CN 110034290A CN 201910333330 A CN201910333330 A CN 201910333330A CN 110034290 A CN110034290 A CN 110034290A
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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
- H01M10/054—Accumulators with insertion or intercalation of metals other than lithium, e.g. with magnesium or aluminium
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/362—Composites
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- 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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- 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
- H01M4/626—Metals
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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
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/628—Inhibitors, e.g. gassing inhibitors, corrosion inhibitors
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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
- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
- H01M2004/027—Negative electrodes
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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
A kind of preparation method of sodium-ion battery self-supporting hard carbon cathode material, glucose is dissolved in deionized water and obtains precursor solution: nickel foam being added in precursor solution and carries out hydro-thermal reaction, after reaction, cooled to room temperature is washed product, is dried；Place the product in being heat-treated under inert atmosphere, sodium-ion battery self-supporting hard carbon cathode material is obtained.The present invention is using nickel foam as supporter, in its surface in situ growing three-dimensional porous carbon materials.In follow-up heat treatment process, the catalyzed graphitization of metallic nickel is acted on, and enables and is partially graphitized with metallic nickel connected component, improves electron conductivity.Macrocellular foam nickel can effectively between expansion electrode and electrolyte contact area, prevent electrode from collapsing after cycling.In addition, ensuring the high electron conduction in electrode assembly in the case where not adding any adhesive, it is ensured that the excellent whole chemical property of self-supporting hard carbon electrode.
Description
Technical field
The invention belongs to self-supporting electrode fabrication fields, and in particular to a kind of sodium-ion battery is negative with self-supporting hard carbon
The preparation method of pole material.
Background technique
The research of successful experience based on lithium ion battery technology, the high-performance positive and negative pole material for sodium-ion battery is opened
Hair has achieved breakthrough.Currently, numerous studies are concentrated mainly in sodium-ion battery positive material, and negative electrode material
Selection is more restricted.Carbon based negative electrodes material has the characteristics that abundant raw material, low in cost, synthesis is simple and operating potential is low, non-
The sodium-ion battery often being had excellent performance suitable for building.Have studied various carbon materials, including graphite, expanded graphite, nothing
Shape carbon and graphene.In all Carbon anode candidates, drawn due to high electrochemical activity with relatively low cost, hard carbon
Many concerns are played.Hard carbon contains a large amount of disordered structure, and defective and gap, this facilitates high reversible capacity.However, a large amount of
The presence of disordered structure hinders the transmission and conduction of electronics, causes high rate performance barely satisfactory.Therefore, improve hard carbon material
Electric conductivity becomes one of research direction.
In general, the graphitic carbon of highly crystalline carbonaceous structure has high conductivity and good chemical stability.Hard carbon is direct
Being heated to high temperature (2500-3000 DEG C) can be improved its degree of graphitization.However this method usually requires a large amount of energy.One
Use transition metal such as iron (Fe), cobalt (Co) and nickel (Ni) former as the solid carbonaceous material of catalytic promoter when the effective method of kind
Position Nano graphite structure is known as catalyzed graphitization.Part stone can be prepared under lower temperature (< 1000 DEG C) by this method
Inkization carbon material shows low cost and the advantages of easy processing.But must be driven off catalyst granules before assembled battery,
Which increase cumbersome processes.At this stage, most of institute and factory coated method prepares electrode, need to integrate and examine
Consider the number of plies, the thickness of wet coating, the rheological behavior of coating fluid, the coating accuracy of requirement, coating supporting body material and the painting of coating
Cloth speed etc., complex process, technical difficulty and higher cost [Zhao Baiyuan electrodes of lithium-ion batteries coating technique and equipment research
[J] battery, 2000,30 (2): 56-58.].The addition of bonding agent and conductive agent can directly reduce battery capacity, and the matter being coated with
Amount depends on the coating technique of operator, it is difficult to industrialized production.Self-supporting electrode is realizing the same of composite material synergistic effect
When eliminate coating process, have very big application potential.
As good supporter and current-collector, nickel foam is had many advantages.For example, nickel foam is at low cost, show
Excellent electric conductivity, and huge surface area is provided for the growth of active material.Meanwhile self-supporting electrode saves electrode
Step process is applied, without in addition introducing the conductive agent and adhesive that may hinder electron motion.Therefore, urging by metal foam nickel
It is graphitized come improve hard carbon electric conductivity and optimization electrode structure be improve hard carbon material storage volume and reduce battery capacity damage
The available strategy of mistake.
Summary of the invention
It is from a wealth of sources it is an object of the invention to propose that a kind of material composition is stablized, the simple sodium ion electricity of technological operation
The preparation method of pond self-supporting hard carbon cathode material.Prepared negative electrode material is not necessarily to subsequent coating process, reduces capacity damage
It loses, benefit and industrialized production.
In order to achieve the above objectives, the technical solution adopted by the present invention is that:
1) 0.48-2.4g glucose is dissolved in 60ml deionized water, precursor solution is sufficiently stirred to obtain；
2) sealing, is subsequently placed in homogeneous reaction instrument in 160-200 after nickel foam and presoma being added in reaction kettle
DEG C carry out hydro-thermal reaction；
3) after reaction, cooled to room temperature, and product is washed, is dried；
4) product after drying is placed under 600~900 DEG C of inert atmospheres after being heat-treated and obtains sodium ion electricity after cleaning, drying
Pond self-supporting hard carbon cathode material.
The long 40mm of the nickel foam of the step 2), width 30mm, thickness 1.0mm.
The nickel foam of the step 2) is successively through deionized water, acetone, the hydrochloric acid and EtOH Sonicate that concentration is 1~5mol/L
30~60min, 30~60min, 5~10min and 30~60min are cleaned, then in 60~100 DEG C of 6~12h of vacuum drying.
The reaction kettle of the step 2) is polytetrafluoroethyllining lining.
Step 2) the hydro-thermal reaction time be 12~for 24 hours.
The washing of the step 3) uses one or both of deionized water and dehydrated alcohol, acetone to clean 3~6 respectively
It is secondary.
The drying of the step 3) is 80~120 DEG C of vacuum ovens dry 12~for 24 hours.
Product after drying is placed in ceramic crucible by the step 4), under protection of argon gas with the liter of 2~10 DEG C/min
Warm rate is from room temperature to 600~900 DEG C of 1~3h of heat treatment.
The cleaning of the step 4) is respectively washed 3~5 times using deionized water and dehydrated alcohol.
The drying of the step 4) is in a vacuum drying oven in 60~100 DEG C of dry 6~12h.
The present invention grows hard carbon material using metal foam nickel as self-supporter, on its surface.In follow-up heat treatment process,
The catalyzed graphitization of metallic nickel acts on, and enables and is partially graphitized with metallic nickel connected component, improves electron conductivity.Macropore
Nickel foam can effectively between expansion electrode and electrolyte contact area, prevent electrode from collapsing after cycling.In addition, not adding
Ensure the high electron conduction in electrode assembly in the case where adding any adhesive, it is ensured that the excellent entirety of self-supporting hard carbon electrode
Chemical property.
Compared with prior art, the present invention can obtain following the utility model has the advantages that
Carbon source of the present invention is glucose, is had many advantages, such as environmental-friendly, from a wealth of sources, cheap and easy to get.This hair
It is bright to synthesize final product using hydro-thermal method combination inert gas heat treatment method.Used preparation method is simple, is easy to grasp
Make, and does not need large scale equipment and harsh reaction condition, it is highly-safe, it is suitble to large-scale production.
The present invention grows hard carbon material using metal foam nickel as self-supporter, in its surface in situ.One side nickel foam
The excellent electric conductivity of metal itself can effectively increase the transmission of electronics, and then reinforce electric conductivity；On the other hand subsequent
In heat treatment process, the catalyzed graphitization of nickel is acted on, and the hard carbon that is connected with metallic nickel is partially graphitized, electricity is accelerated
Conduction.The solid phase hard carbon of suitable thickness provides more sodium storage sites during charged/discharged recycles and shortens Na+Diffusion way
Diameter.Macrocellular foam nickel can effectively between expansion electrode and electrolyte contact area, prevent electrode from collapsing after cycling.This
Outside, the high electron conduction in electrode assembly is ensured in the case where not adding any adhesive, so that it is guaranteed that self-supporting hard carbon
The excellent whole chemical property of electrode.The raw materials used stable components of this method, from a wealth of sources, technological operation is simple, preparation
Electrode is not necessarily to subsequent coating process, reduces capacitance loss, benefit and industrialized production.
Detailed description of the invention
Fig. 1 is the X-ray diffraction analysis figure of self-supporting hard carbon cathode material prepared by the embodiment of the present invention 1；
Fig. 2 is scanning electron microscope (SEM) figure of self-supporting hard carbon cathode material prepared by the embodiment of the present invention 1；
Fig. 3 is scanning electron microscope (SEM) figure of self-supporting hard carbon cathode material prepared by the embodiment of the present invention 1；
Fig. 4 is transmission electron microscope (TEM) figure of self-supporting hard carbon cathode material prepared by the embodiment of the present invention 1；
Fig. 5 is the Raman figure of self-supporting hard carbon cathode material prepared by the embodiment of the present invention 1；
Fig. 6 is the cycle performance figure of self-supporting hard carbon cathode material prepared by the embodiment of the present invention 1.
Specific embodiment
The present invention is further elaborated with reference to the accompanying drawings and embodiments, but the present invention is not limited to following implementation
Example.
Embodiment 1:
1) 0.48g glucose is dissolved in 60ml deionized water, precursor solution is sufficiently stirred to obtain；
2) by long 40mm, width 30mm, thickness 1.0mm nickel foam successively through deionized water, acetone, the hydrochloric acid that concentration is 2mol/L
30min, 50min, 8min and 40min are cleaned with EtOH Sonicate, then in 60 DEG C of vacuum drying 12h, then by the bubble after drying
Sealing after foam nickel self-supporter and precursor solution B are added in the reaction kettle of polytetrafluoroethyllining lining, is subsequently placed in and is contrary
Ying Yizhong, in 180 DEG C of hydro-thermal reaction 18h；
3) cooled to room temperature after reaction, and deionized water and washes of absolute alcohol 6 time are used product respectively,
80 DEG C of vacuum ovens are dry for 24 hours；
4) product after drying is placed in ceramic crucible, under protection of argon gas with the heating rate of 5 DEG C/min from room temperature
It is respectively washed 3 times after being warming up to 800 DEG C of heat treatment 2h using deionized water and dehydrated alcohol, it is dry in 100 DEG C in a vacuum drying oven
Dry 6h obtains sodium-ion battery self-supporting hard carbon cathode material.
Show in X-ray diffraction (XRD) figure of prepared self-supporting three-dimensional hard carbon cathode material as seen from Figure 1
The sample of preparation shows two wide characteristic peaks at 23.0 ° and 44.0 ° respectively, corresponds respectively to (002) and (100) diffraction
Crystal face is the property of typical amorphous carbon.
As seen from Figure 2 in the SEM figure of prepared self-supporting three-dimensional hard carbon cathode material, by being wrapped in nickel foam
Carbon shell and finely dispersed carbon ball composition, be adhering completely to the surface of foam nickel skeleton.
As seen from Figure 3 in the SEM figure of prepared self-supporting three-dimensional hard carbon cathode material, what is grown in nickel foam divides
Dissipating uniform carbon ball diameter is~700nm, and relatively smooth carbon shell and carbon ball surface can reduce the loss of irreversible capacity.
There are the peak D and the peaks G in the Raman spectrum of prepared self-supporting three-dimensional hard carbon cathode material as seen from Figure 4
Two independent characteristic peaks are located at~1346cm-1 and~1591cm-1, it was confirmed that its amorphous structure.The peak D corresponds to
Sp3 hydridization carbon corresponds to the sp2 hydridization carbon with graphite-structure with disordered state and the peak G.The peak D has corresponding to sp3 hydridization carbon
There are disordered state and the peak G to correspond to the sp2 hydridization carbon with graphite-structure.The integrated intensity ratio (IG/ID) at the peak G and the peak D is available
In assessment degree of graphitization, higher IG/ID value indicates more graphite-structures, and high degree of graphitization indicates high electricity
Conductance.Raman fitting result shows prepared sample degree of graphitization with higher, during this is conducive to electrochemical reaction
Electric charge transfer.
The high resolution transmission electron microscope of prepared self-supporting three-dimensional hard carbon cathode material as seen from Figure 5
(HRTEM) in, fold stratiform graphitic carbon is generated after metallic nickel is catalyzed, thickness is about 30nm, about 84 layers of mono-layer graphite.Enhancing
The electric conductivity of hard carbon ensure that the fast transferring of electronics to improve high rate performance.
Prepared self-supporting three-dimensional hard carbon cathode material is under the current density of 0.1 Ag-1 as seen from Figure 6,
100 cycle performance figures.With the high reversible capacity of 307.5mAhg-1 after 100 charge-discharge cycles.
Embodiment 2:
1) 0.96g glucose is dissolved in 60ml deionized water, precursor solution is sufficiently stirred to obtain；
2) by long 40mm, width 30mm, thickness 1.0mm nickel foam successively through deionized water, acetone, the hydrochloric acid that concentration is 2mol/L
40min, 60min, 5min and 50min are cleaned with EtOH Sonicate, then in 80 DEG C of vacuum drying 10h, then by the bubble after drying
Sealing after foam nickel self-supporter and precursor solution B are added in the reaction kettle of polytetrafluoroethyllining lining, is subsequently placed in and is contrary
Ying Yizhong, 160 DEG C of hydro-thermal reactions for 24 hours；
3) cooled to room temperature after reaction, and product is cleaned 6 times with deionized water and acetone respectively, 100
The dry 18h of DEG C vacuum oven；
4) product after drying is placed in ceramic crucible, under protection of argon gas with the heating rate of 7 DEG C/min from room temperature
It is respectively washed 4 times after being warming up to 700 DEG C of heat treatment 2h using deionized water and dehydrated alcohol, in a vacuum drying oven in 60 DEG C of dryings
12h obtains sodium-ion battery self-supporting hard carbon cathode material.
Embodiment 3:
1) 1.44g glucose is dissolved in 60ml deionized water, precursor solution is sufficiently stirred to obtain；
2) by long 40mm, width 30mm, thickness 1.0mm nickel foam successively through deionized water, acetone, the hydrochloric acid that concentration is 3mol/L
50min, 30min, 10min and 60min are cleaned with EtOH Sonicate, then in 100 DEG C of vacuum drying 6h, then by the bubble after drying
Sealing after foam nickel self-supporter and precursor solution B are added in the reaction kettle of polytetrafluoroethyllining lining, is subsequently placed in and is contrary
Ying Yizhong, in 190 DEG C of hydro-thermal reaction 12h；
3) cooled to room temperature after reaction, and deionized water and washes of absolute alcohol 5 time are used product respectively,
The dry 21h of 90 DEG C of vacuum ovens；
4) product after drying is placed in ceramic crucible, under protection of argon gas with the heating rate of 10 DEG C/min from room temperature
It is respectively washed 5 times after being warming up to 900 DEG C of heat treatment 1h using deionized water and dehydrated alcohol, in a vacuum drying oven in 80 DEG C of dryings
9h obtains sodium-ion battery self-supporting hard carbon cathode material.
Embodiment 4:
1) 1.92g glucose is dissolved in 60ml deionized water, precursor solution is sufficiently stirred to obtain；
2) by long 40mm, width 30mm, thickness 1.0mm nickel foam successively through deionized water, acetone, the hydrochloric acid that concentration is 1mol/L
60min, 45min, 6min and 30min are cleaned with EtOH Sonicate, then in 80 DEG C of vacuum drying 10h, then by the bubble after drying
Sealing after foam nickel self-supporter and precursor solution B are added in the reaction kettle of polytetrafluoroethyllining lining, is subsequently placed in and is contrary
Ying Yizhong, in 180 DEG C of hydro-thermal reaction 16h；
3) cooled to room temperature after reaction, and 6 are cleaned with deionized water, dehydrated alcohol and acetone respectively to product
It is secondary, in the dry 12h of 120 DEG C of vacuum ovens；
4) product after drying is placed in ceramic crucible, under protection of argon gas with the heating rate of 2 DEG C/min from room temperature
It is respectively washed 4 times after being warming up to 700 DEG C of heat treatment 2.5h using deionized water and dehydrated alcohol, it is dry in 90 DEG C in a vacuum drying oven
Dry 7h obtains sodium-ion battery self-supporting hard carbon cathode material.
Embodiment 5:
1) 2.4g glucose is dissolved in 60ml deionized water, precursor solution is sufficiently stirred to obtain；
2) by long 40mm, width 30mm, thickness 1.0mm nickel foam successively through deionized water, acetone, the hydrochloric acid that concentration is 5mol/L
45min, 55min, 7min and 35min are cleaned with EtOH Sonicate, then in 60 DEG C of vacuum drying 12h, then by the bubble after drying
Sealing after foam nickel self-supporter and precursor solution B are added in the reaction kettle of polytetrafluoroethyllining lining, is subsequently placed in and is contrary
Ying Yizhong, in 200 DEG C of hydro-thermal reaction 12h；
3) cooled to room temperature after reaction, and deionized water and washes of absolute alcohol 6 time are used product respectively,
The dry 15h of 110 DEG C of vacuum ovens；
4) product after drying is placed in ceramic crucible, under protection of argon gas with the heating rate of 7 DEG C/min from room temperature
It is respectively washed 3 times after being warming up to 600 DEG C of heat treatment 3h using deionized water and dehydrated alcohol, in a vacuum drying oven in 70 DEG C of dryings
10h obtains sodium-ion battery self-supporting hard carbon cathode material.
Embodiment 6:
1) 0.96g glucose is dissolved in 60ml deionized water, precursor solution is sufficiently stirred to obtain；
2) by long 40mm, width 30mm, thickness 1.0mm nickel foam successively through deionized water, acetone, the hydrochloric acid that concentration is 2mol/L
35min, 45min, 9min and 50min are cleaned with EtOH Sonicate, then in 80 DEG C of vacuum drying 6h, then by the foam after drying
Sealing after nickel self-supporter and precursor solution B are added in the reaction kettle of polytetrafluoroethyllining lining, is subsequently placed in homogeneous reaction
In instrument, 180 DEG C of hydro-thermal reactions for 24 hours；
3) cooled to room temperature after reaction, and deionized water and washes of absolute alcohol 3 time are used product respectively,
The dry 18h of 100 DEG C of vacuum ovens；
4) product after drying is placed in ceramic crucible, under protection of argon gas with the heating rate of 10 DEG C/min from room temperature
It is respectively washed 5 times after being warming up to 800 DEG C of heat treatment 1.5h using deionized water and dehydrated alcohol, in a vacuum drying oven in 100 DEG C
Dry 6h obtains sodium-ion battery self-supporting hard carbon cathode material.
Claims (10)
1. a kind of sodium-ion battery preparation method of self-supporting hard carbon cathode material, which comprises the following steps:
1) 0.48-2.4g glucose is dissolved in 60ml deionized water, precursor solution is sufficiently stirred to obtain；
2) by nickel foam and presoma be added in reaction kettle after sealing, be subsequently placed in homogeneous reaction instrument 160-200 DEG C into
Row hydro-thermal reaction；
3) after reaction, cooled to room temperature, and product is washed, is dried；
4) product after drying is placed under 600~900 DEG C of inert atmospheres after being heat-treated and obtains sodium-ion battery use after cleaning, drying
Self-supporting hard carbon cathode material.
2. the sodium-ion battery according to claim 1 preparation method of self-supporting hard carbon cathode material, which is characterized in that
The long 40mm of the nickel foam of the step 2), width 30mm, thickness 1.0mm.
3. the sodium-ion battery according to claim 1 preparation method of self-supporting hard carbon cathode material, which is characterized in that
The nickel foam of the step 2) successively through deionized water, acetone, concentration be 1~5mol/L hydrochloric acid and EtOH Sonicate cleaning 30~
60min, 30~60min, 5~10min and 30~60min, then in 60~100 DEG C of 6~12h of vacuum drying.
4. the sodium-ion battery according to claim 1 preparation method of self-supporting hard carbon cathode material, which is characterized in that
The reaction kettle of the step 2) is polytetrafluoroethyllining lining.
5. the sodium-ion battery according to claim 1 preparation method of self-supporting hard carbon cathode material, which is characterized in that
Step 2) the hydro-thermal reaction time be 12~for 24 hours.
6. the sodium-ion battery according to claim 1 preparation method of self-supporting hard carbon cathode material, which is characterized in that
The washing of the step 3) uses one or both of deionized water and dehydrated alcohol, acetone to clean 3~6 times respectively.
7. the sodium-ion battery according to claim 1 preparation method of self-supporting hard carbon cathode material, which is characterized in that
The drying of the step 3) is 80~120 DEG C of vacuum ovens dry 12~for 24 hours.
8. the sodium-ion battery according to claim 1 preparation method of self-supporting hard carbon cathode material, which is characterized in that
Product after drying is placed in ceramic crucible by the step 4), under protection of argon gas certainly with the heating rate of 2~10 DEG C/min
Room temperature is to 600~900 DEG C of 1~3h of heat treatment.
9. the sodium-ion battery according to claim 1 preparation method of self-supporting hard carbon cathode material, which is characterized in that
The cleaning of the step 4) is respectively washed 3~5 times using deionized water and dehydrated alcohol.
10. the sodium-ion battery according to claim 1 preparation method of self-supporting hard carbon cathode material, feature exist
In the drying of the step 4) is in a vacuum drying oven in 60~100 DEG C of dry 6~12h.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113460983A (en) * | 2021-05-27 | 2021-10-01 | 常州工学院 | Self-supporting transition metal phosphide/carbon composite material film, preparation method and application thereof, and battery |
| CN115020668A (en) * | 2022-06-27 | 2022-09-06 | 广州鹏辉能源科技股份有限公司 | Carbon-based negative electrode for sodium/potassium ion battery and preparation method thereof |
-
2019
- 2019-04-24 CN CN201910333330.5A patent/CN110034290A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113460983A (en) * | 2021-05-27 | 2021-10-01 | 常州工学院 | Self-supporting transition metal phosphide/carbon composite material film, preparation method and application thereof, and battery |
| CN113460983B (en) * | 2021-05-27 | 2022-09-02 | 常州工学院 | Self-supporting transition metal phosphide/carbon composite material film, preparation method and application thereof, and battery |
| CN115020668A (en) * | 2022-06-27 | 2022-09-06 | 广州鹏辉能源科技股份有限公司 | Carbon-based negative electrode for sodium/potassium ion battery and preparation method thereof |
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Application publication date: 20190719 |