CN106128792A - A kind of preparation method of the grapheme composite positive electrode material containing alcohol radical lithium - Google Patents
A kind of preparation method of the grapheme composite positive electrode material containing alcohol radical lithium Download PDFInfo
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- CN106128792A CN106128792A CN201610619958.8A CN201610619958A CN106128792A CN 106128792 A CN106128792 A CN 106128792A CN 201610619958 A CN201610619958 A CN 201610619958A CN 106128792 A CN106128792 A CN 106128792A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
- H01G11/50—Electrodes characterised by their material specially adapted for lithium-ion capacitors, e.g. for lithium-doping or for intercalation
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
- H01G11/32—Carbon-based
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
- H01G11/46—Metal oxides
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/84—Processes for the manufacture of hybrid or EDL capacitors, or components thereof
- H01G11/86—Processes for the manufacture of hybrid or EDL capacitors, or components thereof specially adapted for 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
- Y02E60/13—Energy storage using capacitors
Abstract
The present invention provides the preparation method of a kind of grapheme composite positive electrode material containing alcohol radical lithium.Including following step: step (1) is by Li2CO3And MoO3Mixing, puts into Muffle reaction in furnace after mix homogeneously, reaction obtains Li after terminating2MoO4Material；Step (2) will obtain Li2MoO4Putting into the Muffle reaction in furnace of hydrogen nitrogen mixed gas atmosphere protection, reaction obtains Li after terminating2MoO3Material；Step (3) is by graphite oxide and Li2CO3Mixing, puts into the Muffle reaction in furnace of nitrogen protection, obtains the grapheme material containing alcohol radical lithium after mix homogeneously；Step (4) is by above-mentioned grapheme material and Li2MoO3The Graphene that material is obtained containing alcohol radical lithium in ball milling after the ratio mixing of in mass ratio 50 5:1 is combined Li2MoO3Material.There is advantages that the Graphene containing alcohol radical lithium is combined Li2MoO3Material makes negative pole need not add the pre-embedding lithium technique of lithium sheet or complexity as the positive pole of lithium ion super capacitor, simplifies preparation technology, reduces cost.
Description
Technical field
The invention belongs to lithium ion super capacitor technical field, relate to a kind of lithium ion super capacitor positive electrode
Preparation method.
Background technology
In recent years, lithium rechargeable battery has obtained the biggest development, and this battery cathode generally uses the charcoal elements such as graphite
Material, positive pole uses cobalt acid lithium, LiMn2O4 etc. containing lithium metal oxide.After this set of cells is filled with, during charging, negative pole is to positive pole
Lithium ion is provided, and the lithium ion of positive pole returns negative pole when electric discharge, is therefore referred to as " rocking chair type battery ".With use metal
The lithium battery of lithium is compared, and this battery has high security and the feature of high cycle life.
But, owing to positive electrode is susceptible to the deformation of structure, therefore, lithium ion secondary electricity during removal lithium embedded
The cycle life in pond is still restricted.The most in recent years, body lithium rechargeable battery and double layer capacitor combined
System's research becomes new focus.
The carbon materials such as lithium-ion capacitor general anode material selection graphite, hard carbon, positive electrode selects electric double layer special
The absorbent charcoal material of property, is carried out the pre-doping of lithium ion, makes negative pole current potential significantly decline, thus improve by anticathode material
Energy density.Disclosing a kind of lithium-ion capacitor in patent CN200580001498.2, this lithium-ion capacitor uses
Plus plate current-collecting body and negative current collector are respectively provided with the hole running through positive and negative, respectively by positive active material and negative electrode active material shape
Become electrode layer, carry out electrochemical contact by anticathode, in advance lithium ion is carried in negative pole.Patent
CN200780024069.6 discloses the preprocess method of a kind of electrochemical capacitor negative pole, by vapor phase method or liquid phase
Method forms lithium layer on substrate, and then this lithium layer is transferred to the electrode layer of negative pole.The work that the method for these pre-doping relates to
Skill is more complicated, and needs raw material to carry out special handling, brings certain difficulty to manufacture process.
Summary of the invention
The technical problem to be solved in the present invention is to provide the preparation method of a kind of lithium ion super capacitor positive electrode, should
Positive electrode prepared by method can provide lithium source in lithium-ion capacitor, carries out the pre-embedding of complexity from without anticathode again
Lithium processes or adds lithium sheet in lithium-ion capacitor, simplifies technical process prepared by lithium-ion capacitor, reduces it
Process costs.
The preparation method of the lithium ion super capacitor positive electrode that the present invention provides is:
Step (1) is by Li2CO3And MoO3The ratio mixing of 1-2:1, puts into Muffle furnace 500-700 after mix homogeneously in molar ratio
DEG C reaction 3-8 hour, reaction terminate after obtain Li2MoO4Material.
Step (2) will obtain Li2MoO4Put into the Muffle furnace 500-900 of hydrogen nitrogen mixed gas atmosphere protection containing 5% hydrogen
DEG C reaction 5-10 hour, reaction terminate after obtain Li2MoO3Material.
Step (3) is by graphite oxide and Li2CO3The ratio mixing of 50-10:1 in mass ratio, puts into nitrogen after mix homogeneously
In the Muffle furnace of protection, 200-600 DEG C of reaction 1-6h, obtains the grapheme material containing alcohol radical lithium.
Step (4) is by above-mentioned grapheme material and Li2MoO3After material is mixed in the ratio of 50-5:1 in mass ratio, ball milling obtains
It is combined Li to the Graphene containing alcohol radical lithium2MoO3Material.
The present invention provides the preparation technology flow process of a kind of lithium ion super capacitor as follows:
(1) Li will be combined containing the Graphene of alcohol radical lithium2MoO3Material, conductive agent, binding agent are according to the ratio of mass ratio 90:5:5
Example joins and is mixed into slurry in NMP, is then coated with on plus plate current-collecting body aluminium foil, obtains positive plate after drying；
(2) graphite or carbon cathode material, conductive agent, binding agent firmly are joined in NMP according to the ratio of mass ratio 90:5:5
It is mixed into slurry, is then coated with on negative current collector Copper Foil paper tinsel, after drying, obtains negative plate；
(3) according to the preparation technology of usual lithium ion battery, negative plate, barrier film and positive plate are formed electricity by the way of lamination
Core, then injects electrolyte in battery case, and the electrolyte of injection is 1mol/L LiPF6DOL-DME solution (DOL and DME
Volume ratio be 1:1), sealing, obtain lithium ion super capacitor.
The lithium ion battery that the technique using positive electrode of the present invention to prepare lithium ion super capacitor is general prepares work
Skill, enormously simplify the preparation technology of lithium ion super capacitor.
Graphene containing alcohol radical lithium prepared by the present invention is combined Li2MoO3Material is used as lithium ion super capacitor positive pole
During material, Li2MoO3Alcohol radical lithium on material and Graphene provides lithium source, the lithium ion abjection Li when initial charge2MoO3Material
It is inserted in graphite cathode with alcohol radical lithium, thus drags down and negative pole current potential therefore negative pole need not use metal lithium sheet or complexity
Pre-embedding lithium technique；Graphene is combined Li2MoO3Li in material2MoO3Support graphene film Rotating fields, effectively prevent graphite
Alkene material is reunited and is reduced specific surface area；Li simultaneously2MoO3Material forms Li after sloughing lithium ion2-xMoO3Material is that electrochemistry is lazy
Property material, do not affect the normal use of battery.
There is advantages that (1) Graphene containing alcohol radical lithium is combined Li2MoO3Material is as lithium ion
The positive pole of ultracapacitor makes negative pole need not add the pre-embedding lithium technique of lithium sheet or complexity, simplifies preparation technology, fall
Low cost；(2) Graphene is combined Li2MoO3Material has high connductivity, high-specific surface area can effectively substitute conventional activity
Charcoal positive electrode, it is achieved high-energy-density and high power density.
Accompanying drawing explanation
Fig. 1 is the cycle life figure of lithium ion super capacitor of the present invention.
Detailed description of the invention
Below in conjunction with the accompanying drawings, the preferably embodiment of the present invention is described in further detail:
Embodiment 1
(1) by Li2CO3And MoO3The ratio mixing of 1:1, puts into Muffle furnace 500 DEG C reaction 3 little after mix homogeneously in molar ratio
Time, reaction obtains Li after terminating2MoO4。
(2) Li will be obtained2MoO4Put into the Muffle furnace containing the hydrogen nitrogen mixed gas atmosphere protection that volumetric concentration is 5% hydrogen
500 DEG C are reacted 5 hours, and reaction obtains Li after terminating2MoO3Material.
(3) by graphite oxide and Li2CO3The ratio mixing of 50:1 in mass ratio, puts into the horse of nitrogen protection after mix homogeneously
Not 200 DEG C of reaction 6h in stove, obtain the grapheme material containing alcohol radical lithium.
(4) by above-mentioned grapheme material and Li2MoO3After the ratio mixing of material 50:1 in mass ratio, ball milling obtains containing alcohol
The Graphene of base lithium is combined Li2MoO3Material.
(5) Li will be combined containing the Graphene of alcohol radical lithium2MoO3Material, conductive agent Ketjen black, binding agent PVDF are according to quality
Ratio than 90:5:5 joins and is mixed into slurry in NMP, is then coated with on plus plate current-collecting body aluminium foil, obtains positive pole after drying
Sheet.
(6) graphite cathode material, conductive agent Ketjen black, binding agent PVDF are joined according to the ratio of mass ratio 90:5:5
NMP is mixed into slurry, is then coated with on negative current collector Copper Foil paper tinsel, after drying, obtains negative plate.
(7) according to the preparation technology of usual lithium ion battery by negative plate, barrier film and positive plate group by the way of lamination
Becoming battery core, then inject electrolyte in battery case, the electrolyte of injection is 1mol/L LiPF6DOL-DME solution (DOL
It is 1:1 with the volume ratio of DME), sealing, obtain lithium ion super capacitor.
Embodiment 2
(1) by Li2CO3And MoO3The ratio mixing of 2:1, puts into Muffle furnace 700 DEG C reaction 8 little after mix homogeneously in molar ratio
Time, reaction obtains Li after terminating2MoO4。
(2) Li will be obtained2MoO4Put into the Muffle furnace containing the hydrogen nitrogen mixed gas atmosphere protection that volumetric concentration is 5% hydrogen
900 DEG C are reacted 10 hours, and reaction obtains Li after terminating2MoO3Material.
(3) by graphite oxide and Li2CO3The ratio mixing of 10:1 in mass ratio, puts into the horse of nitrogen protection after mix homogeneously
Not 600 DEG C of reaction 1h in stove, obtain the grapheme material containing alcohol radical lithium.
(4) by above-mentioned grapheme material and Li2MoO3After the ratio mixing of material 5:1 in mass ratio, ball milling obtains containing alcohol
The Graphene of base lithium is combined Li2MoO3Material.
(5) Li will be combined containing the Graphene of alcohol radical lithium2MoO3Material, conductive agent Ketjen black, binding agent PVDF are according to quality
Ratio than 90:5:5 joins and is mixed into slurry in NMP, is then coated with on plus plate current-collecting body aluminium foil, obtains positive pole after drying
Sheet.
(6) hard carbon cathode material, conductive agent Ketjen black, binding agent PVDF are joined according to the ratio of mass ratio 90:5:5
NMP is mixed into slurry, is then coated with on negative current collector Copper Foil paper tinsel, after drying, obtains negative plate.
(7) according to the preparation technology of usual lithium ion battery by negative plate, barrier film and positive plate group by the way of lamination
Becoming battery core, then inject electrolyte in battery case, the electrolyte of injection is 1mol/L LiPF6DOL-DME solution (DOL
It is 1:1 with the volume ratio of DME), sealing, obtain lithium ion super capacitor.
Embodiment 3
(1) by Li2CO3And MoO3The ratio mixing of 1.3:1, puts into Muffle furnace 600 DEG C reaction 7 after mix homogeneously in molar ratio
Hour, reaction obtains Li after terminating2MoO4。
(2) Li will be obtained2MoO4Put into the Muffle furnace containing the hydrogen nitrogen mixed gas atmosphere protection that volumetric concentration is 5% hydrogen
700 DEG C are reacted 8 hours, and reaction obtains Li after terminating2MoO3Material.
(3) by graphite oxide and Li2CO3The ratio mixing of 20:1 in mass ratio, puts into the horse of nitrogen protection after mix homogeneously
Not 300 DEG C of reaction 5h in stove, obtain the grapheme material containing alcohol radical lithium.
(4) by above-mentioned grapheme material and Li2MoO3After the ratio mixing of material 25:1 in mass ratio, ball milling obtains containing alcohol
The Graphene of base lithium is combined Li2MoO3Material.
(5) Li will be combined containing the Graphene of alcohol radical lithium2MoO3Material, conductive agent Ketjen black, binding agent PVDF are according to quality
Ratio than 90:5:5 joins and is mixed into slurry in NMP, is then coated with on plus plate current-collecting body aluminium foil, obtains positive pole after drying
Sheet.
(6) graphite cathode material, conductive agent Ketjen black, binding agent PVDF are joined according to the ratio of mass ratio 90:5:5
NMP is mixed into slurry, is then coated with on negative current collector Copper Foil paper tinsel, after drying, obtains negative plate.
(7) according to the preparation technology of usual lithium ion battery by negative plate, barrier film and positive plate group by the way of lamination
Becoming battery core, then inject electrolyte in battery case, the electrolyte of injection is 1mol/L LiPF6DOL-DME solution (DOL
It is 1:1 with the volume ratio of DME), sealing, obtain lithium ion super capacitor.
Embodiment 4
(1) by Li2CO3And MoO3The ratio mixing of 1.5:1, puts into Muffle furnace 650 DEG C reaction 5 after mix homogeneously in molar ratio
Hour, reaction obtains Li after terminating2MoO4。
(2) Li will be obtained2MoO4Put into the Muffle furnace containing the hydrogen nitrogen mixed gas atmosphere protection that volumetric concentration is 5% hydrogen
600 DEG C are reacted 8 hours, and reaction obtains Li after terminating2MoO3Material.
(3) by graphite oxide and Li2CO3The ratio mixing of 30:1 in mass ratio, puts into the horse of nitrogen protection after mix homogeneously
Not 400 DEG C of reaction 2h in stove, obtain the grapheme material containing alcohol radical lithium.
(4) by above-mentioned grapheme material and Li2MoO3After the ratio mixing of material 35:1 in mass ratio, ball milling obtains containing alcohol
The Graphene of base lithium is combined Li2MoO3Material.
(5) Li will be combined containing the Graphene of alcohol radical lithium2MoO3Material, conductive agent Ketjen black, binding agent PVDF are according to quality
Ratio than 90:5:5 joins and is mixed into slurry in NMP, is then coated with on plus plate current-collecting body aluminium foil, obtains positive pole after drying
Sheet.
(6) hard carbon cathode material, conductive agent Ketjen black, binding agent PVDF are joined according to the ratio of mass ratio 90:5:5
NMP is mixed into slurry, is then coated with on negative current collector Copper Foil paper tinsel, after drying, obtains negative plate.
(7) according to the preparation technology of usual lithium ion battery by negative plate, barrier film and positive plate group by the way of lamination
Becoming battery core, then inject electrolyte in battery case, the electrolyte of injection is 1mol/L LiPF6DOL-DME solution (DOL
It is 1:1 with the volume ratio of DME), sealing, obtain lithium ion super capacitor.
Embodiment 5
(1) by Li2CO3And MoO3The ratio mixing of 1.7:1, puts into Muffle furnace 600 DEG C reaction 6 after mix homogeneously in molar ratio
Hour, reaction obtains Li after terminating2MoO4。
(2) Li will be obtained2MoO4Put into the Muffle furnace containing the hydrogen nitrogen mixed gas atmosphere protection that volumetric concentration is 5% hydrogen
800 DEG C are reacted 6 hours, and reaction obtains Li after terminating2MoO3Material.
(3) by graphite oxide and Li2CO3The ratio mixing of 40:1 in mass ratio, puts into the horse of nitrogen protection after mix homogeneously
Not 500 DEG C of reaction 4h in stove, obtain the grapheme material containing alcohol radical lithium.
(4) by above-mentioned grapheme material and Li2MoO3After material is mixed in the ratio of 10:1 in mass ratio, ball milling is contained
The Graphene of alcohol radical lithium is combined Li2MoO3Material.
(5) Li will be combined containing the Graphene of alcohol radical lithium2MoO3Material, conductive agent Ketjen black, binding agent PVDF are according to quality
Ratio than 90:5:5 joins and is mixed into slurry in NMP, is then coated with on plus plate current-collecting body aluminium foil, obtains positive pole after drying
Sheet.
(6) graphite cathode material, conductive agent Ketjen black, binding agent PVDF are joined according to the ratio of mass ratio 90:5:5
NMP is mixed into slurry, is then coated with on negative current collector Copper Foil paper tinsel, after drying, obtains negative plate.
(7) according to the preparation technology of usual lithium ion battery by negative plate, barrier film and positive plate group by the way of lamination
Becoming battery core, then inject electrolyte in battery case, the electrolyte of injection is 1mol/L LiPF6DOL-DME solution (DOL
It is 1:1 with the volume ratio of DME), sealing, obtain lithium ion super capacitor.
Its effect is as shown in table 1, as shown in Table 1: the standby lithium ion super capacitor energy density of patent system of the present invention reaches
Arrive 57.5-62.4 wh/kg, reach the fluence level of conventional lithium ion super capacitor.
As shown in Figure 1: lithium ion super capacitor discharge and recharge prepared by the present invention 1000 times, energy has no substantially decay.
Table 1
| Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 | |
| Energy density (wh/kg) | 60.7 | 62.4 | 58.1 | 57.5 | 61.9 |
Above content is to combine concrete preferred implementation further description made for the present invention, it is impossible to assert this
Bright being embodied as is confined to these explanations.For general technical staff of the technical field of the invention, do not taking off
On the premise of present inventive concept, it is also possible to make some simple deduction or replace, all should be considered as belonging to the protection of the present invention
Scope.
Claims (10)
1. the preparation method of a lithium ion super capacitor positive electrode, it is characterised in that include following step:
Step (1) is by Li2CO3And MoO3Mixing, puts into Muffle reaction in furnace after mix homogeneously, reaction obtains Li after terminating2MoO4
Material；
Step (2) will obtain Li2MoO4The Muffle reaction in furnace of hydrogen nitrogen mixed gas atmosphere protection put into by material, and reaction obtains after terminating
To Li2MoO3Material；
Step (3) is by graphite oxide and Li2CO3Mixing, puts into the Muffle reaction in furnace of nitrogen protection, is contained after mix homogeneously
There is the grapheme material of alcohol radical lithium；
Step (4) is by above-mentioned grapheme material and Li2MoO3After material is mixed in the ratio of 50-5:1 in mass ratio, ball milling is contained
The Graphene having alcohol radical lithium is combined Li2MoO3Material.
2. the method for claim 1, it is characterised in that Li in described step (1)2CO3And MoO3Amount 1-in molar ratio
The ratio mixing of 2:1.
3. the method for claim 1, it is characterised in that the described step (1) reaction temperature in Muffle furnace is 500-
700 DEG C, the response time is 3-8 hour.
4. the method for claim 1, it is characterised in that in described step (2), the atmosphere in Muffle furnace is dense containing volume
Degree is the hydrogen nitrogen mixed gas of 5% hydrogen.
5. the method for claim 1, it is characterised in that the described step (2) reaction temperature in Muffle furnace is 500-
900 DEG C, the response time is 5-10 hour.
6. the method for claim 1, it is characterised in that graphite oxide and Li in described step (3)2CO3In mass ratio
The ratio mixing of 50-10:1.
7. the method for claim 1, it is characterised in that the described step (3) reaction temperature in Muffle furnace is 200-
600 DEG C, the response time is 1-6 hour.
8. the method for claim 1, it is characterised in that in described step (4) containing alcohol radical lithium Graphene with obtain
Li2MoO4The quality of material is mixed in the ratio of 50-5:1.
9. the preparation technology of a lithium ion super capacitor, it is characterised in that include following step:
Step A: the Graphene of the alcohol radical lithium obtained containing such as claim 1 is combined Li2MoO3Material, conductive agent, binding agent add
Enter in NMP, be mixed into slurry, be then coated with on plus plate current-collecting body aluminium foil, after drying, obtain positive plate；
Step B: graphite or carbon cathode material, conductive agent, binding agent firmly are joined and is mixed into slurry in NMP, is then coated with
On negative current collector Copper Foil paper tinsel, after drying, obtain negative plate；
Step C: negative plate, barrier film and positive plate are formed by the way of lamination according to the preparation technology of usual lithium ion battery
Battery core, then injects electrolyte, sealing in battery case, obtains lithium ion super capacitor.
10. preparation technology as claimed in claim 7, it is characterised in that in described step C, described electrolyte is 1mol/L
LiPF6DOL-DME solution, wherein, the volume ratio of DOL and DME is 1:1.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2018023325A1 (en) * | 2016-07-31 | 2018-02-08 | 肖丽芳 | Preparation method for graphene composite positive electrode material comprising alcohol-based lithium |
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| WO2018023325A1 (en) * | 2016-07-31 | 2018-02-08 | 肖丽芳 | Preparation method for graphene composite positive electrode material comprising alcohol-based lithium |
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Application publication date: 20161116 |
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