CN110311124A - A kind of carbon silicon combination electrode material and preparation method thereof - Google Patents
A kind of carbon silicon combination electrode material and preparation method thereof Download PDFInfo
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- CN110311124A CN110311124A CN201910739680.1A CN201910739680A CN110311124A CN 110311124 A CN110311124 A CN 110311124A CN 201910739680 A CN201910739680 A CN 201910739680A CN 110311124 A CN110311124 A CN 110311124A
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- 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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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/362—Composites
- H01M4/366—Composites as layered products
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- 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
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Abstract
The invention discloses a kind of silicon-carbon composite electrode materials and preparation method thereof, are related to electrode material preparation technical field.The preparation method of the carbon silicon combination electrode material includes dispersing silicon in after carbon by high temperature solid state reaction carbon silicon combination electrode material is prepared.Wherein, high temperature solid state reaction is carried out using pitch cracking carbon and graphite as dispersible carrier carbon base body using silicon as activated centre.The synergistic effect between composite material each component is utilized by this method, achieve the purpose that mutual supplement with each other's advantages, carbon silicon combination electrode material is prepared, so that the composite material being prepared not only has relatively good mechanical stability, and in the electrolytic solution relative to the exposure of activated centre silicon, the unstability on its surface can also substantially reduce, so that its cycle performance and first charge-discharge efficiency are much better than pure silicon material, can then effectively improve the chemical property of battery.
Description
Technical field
The present invention relates to electrode material preparation technical field, in particular to a kind of carbon silicon combination electrode material and its
Preparation method.
Background technique
With the extensive use and development of various mancarried electronic aids and electric car, to the lithium ion of Novel high-specific capacity flexible
Battery material develops great urgency.
But lithium ion battery in the prior art, since there are serious during deintercalation for the silicon of its electrode material
Bulk effect makes activated centre lose electrical contact performance, so that its chemical cycle is influenced, so that there are electrochemistry energy-absorbings for its battery
Lower technical problem.
In consideration of it, the present invention is specifically proposed.
Summary of the invention
The purpose of the present invention includes providing a kind of preparation method of carbon silicon combination electrode material, can be anti-by high temperature solid-state
It silicon should be prepared is scattered in and form inserted high capacity Si-C composite material in carbon, to effectively improve the electrochemistry of electrode
Can, to effectively improve the chemical property of battery.
The present invention is implemented as follows:
In a first aspect, the embodiment of the present invention provides a kind of preparation method of carbon silicon combination electrode material, comprising:
Silicon-carbon composite electrode material is obtained after dispersing carbon for silicon by high temperature solid state reaction；
Wherein, high temperature solid state reaction is to crack carbon and graphite as dispersible carrier carbon base body using pitch using silicon as activated centre
It carries out.
In alternative embodiments, carbon silicon combination electrode material includes at least inserted Si/C composite material or Si-
Al/C composite material.
In alternative embodiments, Si/C composite material is prepared by high temperature solid state reaction to specifically include:
Pitch is dissolved in organic solution and forms the first mixed solution；
The first mixed solution is added in graphite, and carrying out oscillation makes graphite dispersion uniformly form the second mixed solution afterwards；
The second mixed solution is added in silicon powder, and is mixing uniformly to form slurry；
It is formed after slurry to be carried out to high-temperature heat treatment under hybrid protection atmosphere with pitch cracking carbon and graphite as dispersion load
The Si/C composite material of body carbon base body.
In alternative embodiments, carbon is dispersed for silicon by high temperature solid state reaction and prepares Si-Al/C composite material tool
Body includes:
Silicon powder and aluminium powder are mixed, and carries out heat treatment under hybrid protection atmosphere and composite material precursor is prepared；
Pitch is dissolved in organic solution, and is stirred after graphite is added and forms slurry after grinding uniformly；
Composite material precursor is added after slurry after carrying out high-temperature heat treatment and forms that crack carbon and graphite with pitch be point
Dissipate the Si-Al/C composite material of carrier carbon base body.
In alternative embodiments, the mass ratio of pitch, graphite and silicon powder is 2:1:0.4~1.
In alternative embodiments, organic solution is tetrahydrofuran, acetone or aqueous isopropanol.
In alternative embodiments, hybrid protection atmosphere is Ar and H2Gaseous mixture, and H2Volume accounting is 4~6%.
In alternative embodiments, the temperature of high-temperature heat treatment is 900~1100 DEG C.
In alternative embodiments, heat treatment is carried out under hybrid protection atmosphere, and composite material precursor is prepared
In step:
The temperature of heat treatment is 600~700 DEG C.
In alternative embodiments, the mass ratio of silicon powder and aluminium powder is 5:1~2, so that Si-Al/C composite material is specific
Raw material including following components content: 8.7~10.5%wt of aluminium, 26.1~28.3%wt of silicon, 38.2~39.1%wt of graphite with
And pitch cracks 23~26.1%wt of carbon.
Second aspect, the embodiment of the present invention provide a kind of carbon silicon combination electrode material, by any in aforementioned embodiments
The preparation method of the carbon silicon combination electrode material of item is prepared.
The invention has the following advantages:
The embodiment provides a kind of preparation methods of carbon silicon combination electrode material, can be anti-by high temperature solid-state
Carbon silicon combination electrode material is prepared after silicon should being dispersed in carbon.Wherein, high temperature solid state reaction be using silicon as activated centre, with
Pitch cracks carbon and graphite is what dispersible carrier carbon base body carried out.It is imitated by this method using the collaboration between composite material each component
It answers, achievees the purpose that mutual supplement with each other's advantages, carbon silicon combination electrode material is prepared, so that the composite material being prepared is not
Only have relatively good mechanical stability, and relative to activated centre silicon exposure in the electrolytic solution, surface it is unstable
Property can also substantially reduce, so that its cycle performance and first charge-discharge efficiency are much better than pure silicon material, it then can be effective
The chemical property of ground improvement battery.
Detailed description of the invention
In order to illustrate the technical solution of the embodiments of the present invention more clearly, below will be to needed in the embodiment attached
Figure is briefly described, it should be understood that the following drawings illustrates only certain embodiments of the present invention, therefore is not construed as pair
The restriction of range for those of ordinary skill in the art without creative efforts, can also be according to this
A little attached drawings obtain other relevant attached drawings.
Fig. 1 is the preparation facilities for the silicon-carbon composite electrode material that the embodiment of the present invention provides；
Fig. 2 is the X ray picture for the silicon-carbon composite electrode material that the embodiment of the present invention is prepared；
The silicon-carbon composite electrode material that Fig. 3 is prepared for the embodiment of the present invention surrounds and watches shape appearance figure；
Fig. 4 is the first charge-discharge curve for the silicon-carbon composite electrode material that the embodiment of the present invention is prepared；
Fig. 5 is the first charge-discharge front and back X ray picture for the silicon-carbon composite electrode material that the embodiment of the present invention is prepared
Spectrum analysis figure；
Fig. 6 is the cycle performance figure for the silicon-carbon composite electrode material that the embodiment of the present invention is prepared.
Icon: 100- air inlet；The gas outlet 101-；103- quartz ampoule；105- reactant；107- furnace body.
Specific embodiment
It in order to make the object, technical scheme and advantages of the embodiment of the invention clearer, below will be in the embodiment of the present invention
Technical solution be clearly and completely described.The person that is not specified actual conditions in embodiment, according to normal conditions or manufacturer builds
The condition of view carries out.Reagents or instruments used without specified manufacturer is the conventional production that can be obtained by commercially available purchase
Product.
Feature and performance of the invention are described in further detail with reference to embodiments.
The embodiment provides a kind of preparation methods of silicon-carbon composite electrode material, mainly pass through high temperature solid-state
Reaction is so that silicon is scattered in carbon and silicon-carbon composite electrode material is prepared.Wherein, high temperature solid state reaction is with silicon for activity
Center is carried out using pitch cracking carbon and graphite as dispersible carrier carbon base body.
In detail, mutual supplement with each other's advantages is achieved the purpose that using the synergistic effect between composite material each component by this method, with
Carbon silicon combination electrode material is prepared so that the composite material being prepared not only have it is relatively good mechanically stable
Property, and in the electrolytic solution relative to the exposure of activated centre silicon, the unstability on surface can also substantially reduce, so that its
Cycle performance and first charge-discharge efficiency are much better than pure silicon material, can then effectively improve the chemical property of battery.
Simultaneously, it should be noted that in an embodiment of the present invention, carbon silicon combination electrode material includes at least inserted
Si/C composite material or Si-Al/C composite material.On the basis of fully taking into account silicon bulk effect and superficial phenomenon, using height
Warm solid phase reaction, which prepares silicon and is scattered in, forms inserted high capacity Si/C composite material in carbon.Si/C composite material not only has
Relatively good mechanical stability, and in the electrolytic solution relative to the exposure of activated centre silicon, the unstability on surface can also
It substantially reduces, therefore its cycle performance and first charge-discharge efficiency are much better than pure silicon material.With Al it is compound after, be prepared for Si-Al/
Reversible capacity reaches 700mah/g, first charge-discharge efficiency 92%, the first capacity retention ratio about 90% of 25 circulations to C composite for the first time
More than.
In detail, preparing Si/C composite material can be carried out by the preparation facilities of silicon-carbon composite electrode material shown in FIG. 1
Preparation, and this method specifically includes:
Pitch is dissolved in organic solution and forms the first mixed solution；
The first mixed solution is added in graphite, and carrying out oscillation makes graphite dispersion uniformly form the second mixed solution afterwards；
The second mixed solution is added in silicon powder, and is mixing uniformly to form slurry；
Reactant 105 can be formed after the solvent of slurry is volatilized, reactant 105 is put into quartz ampoule 103 shown in FIG. 1
Bottom, quartz ampoule 103 have air inlet 100 and gas outlet 101, after quartz ampoule 103 is placed in furnace body, can pass through air inlet
100 are passed through hybrid protection gas to quartz ampoule 103, so that reactant 105 can carry out high-temperature heat treatment under hybrid protection atmosphere,
And it is formed and carbon and graphite is cracked as the Si/C composite material of dispersible carrier carbon base body using pitch.Gas outlet can be passed through after the reaction was completed
101 hybrid protection gas is discharged.
In detail, preparing Si-Al/C composite material can also be by the preparation facilities of silicon-carbon composite electrode material shown in FIG. 1
It is prepared, and this method specifically includes:
Silicon powder and aluminium powder are mixed, and carries out heat treatment under hybrid protection atmosphere and composite material precursor is prepared,
Preferably, the temperature of heat treatment is 600~700 DEG C；
Pitch is dissolved in organic solution, and is stirred after graphite is added and forms slurry after grinding uniformly；
Reactant 105 can be formed after the slurry after solvent volatilizees is added in composite material precursor, reactant 105 is placed
In the bottom of quartz ampoule 103, after quartz ampoule 103 is placed in furnace body, can be passed through by air inlet 100 to quartz ampoule 103 mixed
Protective gas is closed, so that reactant 105 can carry out high-temperature heat treatment under hybrid protection atmosphere, and carries out shape after high-temperature heat treatment
Carbon and graphite are cracked as the Si-Al/C composite material of dispersible carrier carbon base body at using pitch.
It should be noted that due to the characteristic of pitch in above-mentioned steps, in thermal process reactor it is main in two steps into
Row occurs polymerization reaction in 300-400 DEG C of pitch first, generates long-chain molecule polymer, and when temperature continues to increase, this is poly-
It closes object and dehydrogenation reaction occurs, generate cracking carbon.Therefore, in an embodiment of the present invention, the temperature of heat treatment cracks carbon to pitch
Removal lithium embedded performance plays a decisive role.Heat treatment temperature is higher, and chemical property and the cycle performance for cracking carbon are better.But
After temperature is more than 1200 DEG C, silicon and carbon generate the SiC phase inert to lithium, therefore in an embodiment of the present invention using high warm
The temperature of processing is 900~1100 DEG C.Certainly, in other embodiments of the invention, the temperature of high-temperature heat treatment can be with root
It is adjusted according to demand, the embodiment of the present invention is without limitation.
It should also be noted that, in an embodiment of the present invention, the mass ratio of pitch, graphite and silicon powder is 2:1:0.4
~1.For example, the dosage of graphite may be selected to be 25g when the dosage of pitch is selected as 50g, the dosage of silicon powder may be selected to be 10g
~50g.Meanwhile in the preparation process of Si-Al/C composite material, the mass ratio of silicon powder and aluminium powder is 5:1~2, so that Si-
Al/C composite material specifically includes the raw material of following components content: 8.7~10.5%wt of aluminium, 26.1~28.3%wt of silicon, graphite
38.2~39.1%wt and pitch crack 23~26.1%wt of carbon.It may make and be prepared by the control of the dosage to each raw material
To the chemical property of silicon-carbon composite electrode material effectively ensured.
In detail, in an embodiment of the present invention, organic solution is tetrahydrofuran, acetone or aqueous isopropanol.Mixing is protected
Shield atmosphere is Ar and H2Gaseous mixture, and H2Volume accounting is 4~6%.By the setting of hybrid protection atmosphere, material may make
It is not easy to be oxidized in high-temperature atmosphere, to further guarantee the chemical property of Si-C composite material.
It is described in detail below by embodiment:
Embodiment 1
A kind of Si/C composite material is present embodiments provided, is prepared by the following method to obtain:
S1: the pitch of pre-reaction material is dissolved in the organic solutions such as tetrahydrofuran, acetone and forms the first mixed solution；
S2: it after the first mixed solution is added in the graphite that suitable average particle size is 1 micron, is vibrated in ultrasonator
15 minutes, the second mixed solution is formed after graphite dispersion is uniform；
S3: the silicon powder as activated centre being added thereto in the second mixed solution, and stirs and to form uniform slurry,
Uniform stirring at room temperature is transferred in quartz ampoule 103, while being passed through protective atmosphere to quartz ampoule 103 after volatilizing at room temperature,
Heat treatment, which is carried out, at 900 DEG C prepares composite material.
Embodiment 2
The present embodiment additionally provides a kind of Si-Al/C composite material, is prepared by the following method to obtain:
S1: granularity is mixed for 5 microns of silicon powder and atomized aluminium with the mass ratio of 5:1；
S2: after ball milling mixing is uniform in Ar milling atmosphere, in mixed gas (4%H2, 96%Ar) protection under, with
After 600 degree of heat treatments, it is prepared into composite material precursor；
S3: taking appropriate pitch to be dissolved in acetone, stir evenly, and 1-2 microns of graphite powder of granularity is slowly added to, is gently stirred
It mixes and suitably grinds；
S4: the silicon after heat treatment above-mentioned/aluminium powder is added in cold primer-oil, and is stirred evenly.At room temperature, to solvent
After volatilization, mixture is transferred in quartz ampoule 103, is placed in furnace body 107, heat treatment is carried out at 900 DEG C and prepares composite material.
The each component content for the Si-Al/C composite material that the above method is prepared is about aluminium 8.7%wt, silicon 26.1%
Wt, graphite 39.1%wt, pitch crack carbon 26.1%wt, and Si-Al/C composite material is placed in levigate in agate mortar, mistake 250
Finished product can be obtained in mesh.
Embodiment 3
A kind of Si/C composite material is present embodiments provided, is prepared by the following method to obtain:
S1: 50 grams of reactant pitches are dissolved in isopropanol and form the first mixed solution；
S2: after being sufficiently stirred 30 minutes, the graphite that 25 grams of D50 are 1 micron is added in the first mixed solution, and in ultrasound
The second mixed solution is formed after vibrating 15 minutes in device；
S3: it after graphite dispersion is uniform, is sufficiently stirred being added thereto as the 10 of activated centre grams of silicon powders.At room temperature
It is sufficiently stirred, is placed in ventilating kitchen, after volatilizing to solvent, go in quartz ampoule 103, be passed through protective gas (4%H2,
The temperature gradient for being heat-treated, and being heat-treated after 96%Ar) is to be warming up to 900 DEG C, and gradually cooling takes after reaction 3 as a child
Out.
Embodiment 4
The present embodiment additionally provides a kind of Si-Al/C composite material, is prepared by the following method to obtain:
S1: granularity is uniformly mixed for 5 microns of silicon powder and atomized aluminium 5:1 in mass ratio, is ground in Ar atmosphere ball milling
Uniformly；
S2: in mixed gas (4%H2, 96%Ar) protection under, after being heat-treated at 700 DEG C, be prepared into composite wood
Material precursor；
S3: taking appropriate pitch to be dissolved in acetone, stir evenly, and 1-2 microns of graphite powder of granularity is slowly added to, is gently stirred
It mixes and suitably grinds；
S4: the silicon after heat treatment above-mentioned/aluminium powder is added in cold primer-oil, and is stirred evenly；
S5: at room temperature, after the solvent is volatilized, mixture is transferred in quartz ampoule, is placed in heating furnace body 107, sample
Heat treatment process it is the same manner as in Example 2, heat treatment reaction formed Si-Al/C composite material.
Wherein, the Si-Al/C composite material each component content that the above method is prepared is about aluminium 10.5%wt, silicon
28.3%wt, graphite 38.2%wt, pitch crack carbon 23%wt, and Si-Al/C composite material is placed in levigate in agate mortar, mistake
Finished product can be obtained in 250 meshes.
The Si-C composite material that embodiment 1 to embodiment 4 is prepared is tested for the property, as shown in Fig. 2, compound
In the X ray picture of material, correspond to graphite (111) direction at d for the strong diffraction maximum at 3.35.Due to pitch be cracked into it is unformed
Structure, therefore observe the disperse peak of carbon in X ray diffracting spectrum, do not find the diffraction maximum of SiC.Fig. 3 is silicon carbon material
Microscopic appearance, white particle be silicon particle, black be carbon matrix.As can be seen that silicon powder is dispersed in graphite and pitch is split
In the carbon parent for solving carbon composition, mosaic texture is formed.Since Carbon materials are for silicon, quality is softer, this to be embedded in
The stress of the volume expansion band of silicon can be alleviated to a certain extent.Pitch during heat treatment can recurring structure it is soft
Change, cracking generates a small amount of small molecule and constantly escapes from ontology at this time, forms loose porous structure.Silicon and graphite dispersion are dripping
In the presoma of blueness reaction, the porosity of pitch cracking carbon can be reduced to a certain extent, led to reduce porosity and exist
Cause the irreversible capacity of embedding de- lithium.Fig. 4 is the first charge-discharge curve of different materials, and wherein P is pitch cracking carbon, and SGP is to adopt
It is the Si-C composite material of precursor preparation with pitch, silicon powder and graphite.Fig. 5 is X-ray atlas analysis before and after first charge-discharge,
It can be seen from the figure that, due to the stability of graphite-structure, there is no variations for characteristic peak after recycling for the first time, but
It is that the characteristic peak of silicon does not have, illustrates after circulation terminates, silicon Jie becomes unformed state in composite material SGP.It can be seen in Fig. 6
Out, the coulombic efficiency of charge and discharge is gradually steady with the increase of the cycle-index of charge and discharge, and when recycling to 4th week, conservation rate exists
90% or more.
In conclusion the preparation method for the carbon silicon combination electrode material that the embodiment of the present invention provides, is fully taking into account
On the basis of silicon bulk effect and superficial phenomenon, silicon is prepared using high temperature solid state reaction it is scattered in and form inserted Gao Rong in carbon
Measure Si/C composite material.Si/C composite material not only has relatively good mechanical stability, but also relative to activated centre silicon
In the electrolytic solution, the unstability on surface can also substantially reduce, therefore its cycle performance and first charge-discharge efficiency are remote for exposure
Better than pure silicon material.With Al it is compound after, be prepared for Si-Al/C composite material for the first time reversible capacity reach 700mah/g, charge and discharge for the first time
Electrical efficiency 92%, the first capacity retention ratio about 90% or more of 25 circulations.
To sum up, the preparation method for the carbon silicon combination electrode material that the embodiment of the present invention provides, it is each using composite material
Synergistic effect between component, achievees the purpose that mutual supplement with each other's advantages, carbon silicon combination electrode material is prepared, so that being prepared into
To composite material not only there is relatively good mechanical stability, but also in the electrolytic solution relative to the exposure of activated centre silicon,
The unstability on its surface can also substantially reduce, so that its cycle performance and first charge-discharge efficiency are much better than pure silicon material
Material, can then effectively improve the chemical property of battery.
The foregoing is only a preferred embodiment of the present invention, is not intended to restrict the invention, for the skill of this field
For art personnel, the invention may be variously modified and varied.All within the spirits and principles of the present invention, made any to repair
Change, equivalent replacement, improvement etc., should all be included in the protection scope of the present invention.
Claims (11)
1. a kind of preparation method of carbon silicon combination electrode material characterized by comprising
Silicon-carbon composite electrode material is obtained after dispersing carbon for silicon by high temperature solid state reaction；
Wherein, the high temperature solid state reaction is to crack carbon and graphite as dispersible carrier carbon using pitch using the silicon as activated centre
What matrix carried out.
2. the preparation method of carbon silicon combination electrode material according to claim 1, it is characterised in that:
The carbon silicon combination electrode material includes at least inserted Si/C composite material or Si-Al/C composite material.
3. the preparation method of carbon silicon combination electrode material according to claim 2, which is characterized in that anti-by high temperature solid-state
The Si/C composite material should be prepared to specifically include:
Pitch is dissolved in organic solution and forms the first mixed solution；
First mixed solution is added in the graphite, and carrying out oscillation makes the graphite dispersion uniformly form the second mixing afterwards
Solution；
Second mixed solution is added in silicon powder, and is mixing uniformly to form slurry；
It is formed after the slurry to be carried out to high-temperature heat treatment under hybrid protection atmosphere with pitch cracking carbon and the graphite
For the Si/C composite material of dispersible carrier carbon base body.
4. the preparation method of carbon silicon combination electrode material according to claim 2, which is characterized in that anti-by high temperature solid-state
Silicon should be dispersed in carbon and prepare the Si-Al/C composite material and specifically included:
Silicon powder and aluminium powder are mixed, and carries out heat treatment under hybrid protection atmosphere and composite material precursor is prepared；
The pitch is dissolved in organic solution, and is stirred after the graphite is added and forms slurry after grinding uniformly；
The composite material precursor is added after the slurry after carrying out high-temperature heat treatment formed with pitch cracking carbon and
The graphite is the Si-Al/C composite material of dispersible carrier carbon base body.
5. the preparation method of carbon silicon combination electrode material according to claim 3 or 4, it is characterised in that:
The mass ratio of the pitch, the graphite and the silicon powder is 2:1:0.4~1.
6. the preparation method of carbon silicon combination electrode material according to claim 3 or 4, it is characterised in that:
The organic solution is tetrahydrofuran, acetone or aqueous isopropanol.
7. the preparation method of carbon silicon combination electrode material according to claim 3 or 4, it is characterised in that:
The hybrid protection atmosphere is Ar and H2Gaseous mixture, and the H2Volume accounting be 4~6%.
8. the preparation method of carbon silicon combination electrode material according to claim 3 or 4, it is characterised in that:
The temperature of the high-temperature heat treatment is 900~1100 DEG C.
9. the preparation method of carbon silicon combination electrode material according to claim 4, which is characterized in that in the hybrid protection
It is carried out under atmosphere in the step of composite material precursor is prepared in heat treatment:
The temperature of the heat treatment is 600~700 DEG C.
10. the preparation method of carbon silicon combination electrode material according to claim 4, it is characterised in that:
The mass ratio of the silicon powder and the aluminium powder is 5:1~2, so that the Si-Al/C composite material is specifically included with the following group
Divide the raw material of content: 8.7~10.5%wt of aluminium, 26.1~28.3%wt of silicon, 38.2~39.1%wt of graphite and pitch cracking
23~26.1%wt of carbon.
11. a kind of carbon silicon combination electrode material, which is characterized in that multiple by carbon silicon described in any one of claims 1 to 10
The preparation method of composite electrode material is prepared.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115472809A (en) * | 2022-10-26 | 2022-12-13 | 晖阳(贵州)新能源材料有限公司 | Preparation method of graphite composite material with high first-time efficiency |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115472809A (en) * | 2022-10-26 | 2022-12-13 | 晖阳(贵州)新能源材料有限公司 | Preparation method of graphite composite material with high first-time efficiency |
| CN115472809B (en) * | 2022-10-26 | 2023-09-01 | 晖阳(贵州)新能源材料有限公司 | Preparation method of graphite composite material with high first efficiency |
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