CN109273669A - A kind of super integrated flexible cathode of lithium ion battery and preparation method thereof - Google Patents
A kind of super integrated flexible cathode of lithium ion battery and preparation method thereof Download PDFInfo
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- CN109273669A CN109273669A CN201811176388.5A CN201811176388A CN109273669A CN 109273669 A CN109273669 A CN 109273669A CN 201811176388 A CN201811176388 A CN 201811176388A CN 109273669 A CN109273669 A CN 109273669A
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- carbon felt
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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
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/131—Electrodes based on mixed oxides or hydroxides, or on mixtures of oxides or hydroxides, e.g. LiCoOx
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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
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/133—Electrodes based on carbonaceous material, e.g. graphite-intercalation compounds or CFx
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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
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/139—Processes of manufacture
- H01M4/1391—Processes of manufacture of electrodes based on mixed oxides or hydroxides, or on mixtures of oxides or hydroxides, e.g. LiCoOx
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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
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/139—Processes of manufacture
- H01M4/1395—Processes of manufacture of electrodes based on metals, Si or alloys
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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
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Abstract
The present invention relates to a kind of lithium ion battery flexibility cathode and preparation method thereof, preparation includes the following steps: that (1) is chosen three-dimensional carbon-based material carbon felt and supported as flexible back bone, and carries out surface preparation to it；(2) by treated, carbon felt sufficiently infiltrates in metal salt solution, and under certain temperature, additive and pH value condition, solvent thermal reaction certain time is in a kettle to be prepared the super integrated flexible cathode of transition metal oxide/carbon felt.The advantages that method of the invention is simple and easy, and preparation parameter controllability is strong, selects flexible support material of the carbon felt as negative electrode of lithium ion battery, and conductive good, raw material is easy to get, is cheap.It is good that the super integrated flexible cathode of the transition metal oxide/carbon felt being prepared is used as lithium ion battery negative material flexibility, and has both higher charging and discharging capacity and cyclical stability.
Description
Technical field
The present invention relates to super integrated flexible cathode of a kind of lithium ion battery and preparation method thereof, belong to electrochemistry and new energy
Source material technical field.
Background technique
Lithium ion battery (LIBs) is a kind of green secondary energy sources environmental-friendly, charge-discharge performance is excellent, exploitation benefit
It is wide with atmosphere pollution caused by energy crisis existing for the world today and conventional fossil fuel burn can be effectively relieved
It is general to be applied to laptop, mobile phone and the electric powered motor energy.Electronic equipment becomes more diverse and more in recent years
Functionalization, along with flexible intelligent mobile phone, wearable computer, implantable medical electronic device and smartwatch/glasses etc. are new general
The it is proposed of thought proposes the new requirement such as flexibility, lighting and micromation to lithium ion battery.In order to adapt to next-generation flexibility
The development of electronic equipment, the flexibility and charge-discharge characteristic of lithium ion battery are to be improved.
Three key building blocks of flexible lithium ion battery be respectively as follows: flexible electrode (anode and cathode), electrolyte and
Encapsulating material.How to try to construct folding flexible electrode, and select the electrode active material with suitable construction, to change
The removal lithium embedded characteristic of kind lithium ion is the critical path for realizing high-performance flexible lithium ion battery.Transition metal oxide conduct
Theoretical capacity with higher, discharge voltage plateau be higher when lithium ion battery negative material, the simple multiplicity of preparation method, raw material
It is cheap, have good prospect and potentiality.But it is more common in powder body material at present, needs to use when preparing negative electrode of lithium ion battery
Copper foil is as collector, and there are also very big rooms for promotion for electrode plates flexibility.Carbon felt is a kind of three-dimensional carbon-based material, is had
Self-supporting porous structure and biggish specific surface area, are conducive to the load of active material.In addition, carbon felt also have it is a series of excellent
Good characteristic: ultra-thin, lightweight, flexibility be good, good conductivity, can be processed into various shape and size, as needed to adapt to not
Same requirement.There is carbon felt the carbon skeleton of self-supporting can replace traditional collector, its own porous knot having
Structure can guarantee the quick diffusion of electrolyte, in addition, lithium ion battery anode active material can be grown directly upon carbon skeleton
On, it realizes active material/collector integral structure, meets the needs of existing lithium ion battery flexibility.
Summary of the invention
The purpose of the invention is to adapt to nowadays lithium ion battery flexibility, lighting and the new demand of micromation, mention
For super integrated flexible cathode of a kind of lithium ion battery and preparation method thereof.
A kind of super integrated flexible cathode of lithium ion battery of the invention, is made of carbon felt and transition metal oxide,
It is calculated with the gross mass of the integrated electrode, the mass percentage of each section are as follows:
Carbon felt: 5%-95%；
Transition metal oxide: 95%-5%.
A kind of preparation method of the super integrated flexible cathode of lithium ion battery, specific preparation process is as follows:
Step 1: metal salt is added in alcoholic solution, stirring is made it completely dissolved, and obtains solution；
Step 2: carrying out surface preparation to three-dimensional carbon-based material carbon felt；
Step 3: pretreated carbon felt is added into the metal salt solution that step 1 obtains, and infiltrate it sufficiently, is added
A certain amount of sodium hydroxide；It is reacted under conditions of temperature is 50~250 DEG C, until the reaction is complete；
Step 4: after the reaction was completed to step 3, washing is filtered to filtrate pH and is in neutrality, product vacuum drying will be filtered, is obtained
The super integrated flexible cathode of transition metal oxide/carbon felt.
Alcohols described in step 1 include polyethylene glycol, polyethanol, ethyl alcohol and ethylene glycol and they in it is both any to appoint
The mixed liquor of meaning ratio mixing；
Metal salt solution described in step 1 includes copper, zinc, nickel, cobalt, manganese and iron salt solutions.
The concentration of metal salt solution is 0.001~1g mL in step 1-1。
The surface preparation process of three-dimensional carbon-based material carbon felt described in step 2 includes: that carbon felt EtOH Sonicate is clear
Wash 20min;Carbon felt after ultrasonic cleaning is added in potassium hydroxide solution, wherein carbon felt and potassium hydroxide quality ratio are
1:3 impregnates 12h;Carbon felt is put into baking oven, drying is moved back to tube furnace and risen under an argon atmosphere under conditions of 85 DEG C
Warm rate is 5 DEG C/min, 800 DEG C of heat preservation 1h.
The mass ratio of carbon felt and transition metal oxide is 1:0.05-10 in step 2.
The mass ratio of sodium hydroxide and metal salt is 1:0.01-10 in step 2.
Beneficial effect
1, a kind of super integrated flexible cathode of lithium ion battery of the invention has both preferable flexible frivolous property and charge and discharge cycles
Stability has certain promotional value and application prospect.
2, preparation is simple for a kind of super integrated flexible cathode of lithium ion battery of the invention, and preparation parameter can
Control property is strong, is a kind of cheap, environmentally friendly preparation method.
Detailed description of the invention
Fig. 1 is zinc oxide/carbon felt flexibility cathode XRD diagram in the embodiment of the present invention 1;
Fig. 2 is zinc oxide/carbon felt flexibility cathode SEM figure in the embodiment of the present invention 1；
Fig. 3 is zinc oxide/carbon felt flexibility cathode in the embodiment of the present invention 1 in 100mAg-1Charge and discharge cycles electric discharge in 100 weeks
Curve.
Fig. 4 is iron oxide/carbon felt flexibility cathode XRD diagram in the embodiment of the present invention 2;
Fig. 5 is iron oxide/carbon felt flexibility cathode SEM figure in the embodiment of the present invention 2；
Fig. 6 is iron oxide/carbon felt flexibility cathode in the embodiment of the present invention 2 in 200mAg-1Charge and discharge cycles electric discharge in 100 weeks
Curve.
Specific embodiment
It elaborates below with reference to embodiment and attached drawing to the present invention:
Embodiment 1: zinc oxide/carbon felt flexibility cathode
1) 2g Zn (CH is weighed3COO)2·2H2O is added in the mixed solution of 14mL polyethylene glycol and 76mL dehydrated alcohol, magnetic force
Stirring dissolves it sufficiently；
2) carbon felt is cleaned into 20min with EtOH Sonicate;Carbon felt after ultrasonic cleaning is added in potassium hydroxide solution,
Middle carbon felt and potassium hydroxide quality ratio are 1:3, impregnate 12h;Carbon felt is put into baking oven, after drying under conditions of 85 DEG C
Tube furnace is moved to, under an argon atmosphere, heating rate is 5 DEG C/min, 800 DEG C of heat preservation 1h.
3) carbon felt Jing Guo above-mentioned surface preparation process is sufficiently infiltrated in 1) mixed solution, is moved to equipped with 0.7g
In the polytetrafluoroethylene (PTFE) cup of NaOH, reacted for 24 hours at 140 DEG C；
4) it is cooled to room temperature after reaction, takes out product distillation and is washed to neutrality, dry to get zinc oxide/carbon felt is arrived
Flexible cathode.
It is filled after zinc oxide/carbon felt flexibility cathode of above method preparation is applied to lithium ion battery negative material
Specific discharge capacity and cycle performance test: zinc oxide/carbon felt is directly used as working electrode, and lithium metal is to electrode, 1mol/L
LiF6/ EC-DMC (volume ratio 1: 1) is electrolyte, is assembled into simulated battery in argon atmosphere glove box.To simulated battery
Charge-discharge test is carried out, voltage range is 0.01~3V (vs.Li+/ Li), current density 100mAg-1。
Test result: zinc oxide/carbon felt flexibility cathode XRD and SEM difference are as depicted in figs. 1 and 2.Zinc oxide/carbon
Felt flexibility cathode is in 100mAg-1100 weeks discharge curves of charge and discharge cycles are as shown in figure 3, be 100mAg in current density-1
When, reversible capacity is 520.2mAhg after recycling 100 weeks-1, compare capacity characteristic and stable circulation performance for pure zinc oxide electrode
It is greatly improved.
Embodiment 2: iron oxide/carbon felt flexibility cathode
1) 2.7g FeCl is weighed3·6H2O is put into 90mL equipped in the polytetrafluoroethylene (PTFE) cup of ethylene glycol solution, and magnetic agitation makes it
Sufficiently dissolution；
2) ammonium hydroxide is slowly added dropwise into above-mentioned solution, adjusts solution ph to 10,2g polyethylene glycol is then added and continues to stir
30min;
3) carbon felt is cleaned into 20min with EtOH Sonicate;Carbon felt after ultrasonic cleaning is added in potassium hydroxide solution,
Middle carbon felt and potassium hydroxide quality ratio are 1:3, impregnate 12h;Carbon felt is put into baking oven, after drying under conditions of 85 DEG C
Tube furnace is moved to, under an argon atmosphere, heating rate is 5 DEG C/min, 800 DEG C of heat preservation 1h.
4) carbon felt Jing Guo above-mentioned surface preparation process is moved in 2) mixed solution and is sufficiently infiltrated, at 200 DEG C
Reaction is for 24 hours；
4) it is cooled to room temperature after reaction, takes out product distillation and is washed to neutrality, dry to get iron oxide/carbon felt is arrived
Flexible cathode.
It is filled after iron oxide/carbon felt flexibility cathode of above method preparation is applied to lithium ion battery negative material
Specific discharge capacity and cycle performance test: iron oxide/carbon felt is directly used as working electrode, and lithium metal is to electrode, 1mol/L
LiF6/ EC-DMC (volume ratio 1: 1) is electrolyte, is assembled into simulated battery in argon atmosphere glove box.To simulated battery
Charge-discharge test is carried out, voltage range is 0.01~3V (vs.Li+/ Li), current density 200mAg-1。
Test result: iron oxide/carbon felt flexibility cathode XRD and SEM difference are as shown in Figure 4 and Figure 5.Zinc oxide/carbon
Felt flexibility cathode is in 200mAg-1100 weeks discharge curves of charge and discharge cycles are as shown in fig. 6, be 100mAg in current density-1
When, reversible capacity is 590mAhg after recycling 200 weeks-1, have both preferable flexibility and stable charge/discharge.
The basic principles, main features and advantages of the invention have been shown and described above.Those skilled in the art should
Understand, the present invention do not limited by above-mentioned specific embodiment, the description in above-mentioned specific embodiment and specification be intended merely into
One step illustrates the principle of the present invention, and under the premise of not departing from spirit of that invention range, the present invention also has various change and changes
Into these changes and improvements all fall within the protetion scope of the claimed invention.The scope of protection of present invention is by claim
Book and its equivalent thereof.
Claims (8)
1. a kind of super integrated flexible cathode of lithium ion battery, it is characterised in that: by three-dimensional carbon-based material carbon felt and transition gold
Belong to oxide composition；It is calculated with the gross mass of the composite material, mass percentage shared by transition metal oxide is 5%-
95%, remaining is carbon-based material.
2. a kind of preparation method of the super integrated flexible cathode of lithium ion battery, it is characterised in that: specific preparation process is as follows:
Step 1: metal salt is added in alcoholic solution, stirring is made it completely dissolved, and obtains solution；
Step 2: carrying out surface preparation to three-dimensional carbon-based material carbon felt；
Step 3: pretreated carbon felt is added into the metal salt solution that step 1 obtains, and infiltrate it sufficiently, is added
A certain amount of sodium hydroxide；It is reacted under conditions of temperature is 50~250 DEG C, until the reaction is complete；
Step 4: after the reaction was completed to step 3, washing is filtered to filtrate pH and is in neutrality, product vacuum drying will be filtered, is obtained
The super integrated flexible cathode of transition metal oxide/carbon felt.
3. the preparation method of the super integrated flexible cathode of lithium ion battery according to claim 2, it is characterised in that: described
Alcohols in step 1 includes polyethylene glycol, polyethanol, ethyl alcohol and ethylene glycol and any the two is mixed with arbitrary proportion in them
The mixed liquor of conjunction.
4. the preparation method of the super integrated flexible cathode of lithium ion battery according to claim 2, it is characterised in that: described
Metal salt solution in step 1 includes copper, zinc, nickel, cobalt, manganese and iron salt solutions.
5. the preparation method of the super integrated flexible cathode of lithium ion battery according to claim 2, it is characterised in that: described
The concentration of metal salt solution in step 1 is 0.001~1g mL-1。
6. the preparation method of the super integrated flexible cathode of lithium ion battery according to claim 2, it is characterised in that: described
The surface preparation process of three-dimensional carbon-based material carbon felt in step 2 includes: that carbon felt is cleaned 20min with EtOH Sonicate;
Carbon felt after ultrasonic cleaning is added in potassium hydroxide solution, wherein carbon felt and potassium hydroxide quality ratio are 1:3, are impregnated
12h;Carbon felt is put into baking oven, dries and is moved back to tube furnace, under an argon atmosphere, heating rate 5 under conditions of 85 DEG C
DEG C/min, 800 DEG C of heat preservation 1h.
7. the preparation method of the super integrated flexible cathode of lithium ion battery according to claim 2, it is characterised in that: described
The mass ratio of carbon felt and metal salt is 1:0.05-10 in step 3.
8. the preparation method of the super integrated flexible cathode of lithium ion battery according to claim 2, it is characterised in that: described
The mass ratio of sodium hydroxide and metal salt is 1:0.01-10 in step 3.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102544574A (en) * | 2011-12-30 | 2012-07-04 | 华中科技大学 | Flexible lithium ion battery and packaging method thereof |
| CN103606657A (en) * | 2013-12-10 | 2014-02-26 | 北京理工大学 | Lithium ion battery zinc oxide/porous carbon composite negative electrode material with high capacity and preparation method thereof |
| CN107221640A (en) * | 2017-06-09 | 2017-09-29 | 北京科技大学 | A kind of preparation method of the compound sodium negative pole of sodium-ion battery |
| CN108075134A (en) * | 2017-12-12 | 2018-05-25 | 江汉大学 | A kind of preparation method of lithium ion battery carbon cloth base cathode oxidation iron |
| CN108470895A (en) * | 2018-03-21 | 2018-08-31 | 同济大学 | A kind of kalium ion battery positive electrode and preparation method thereof, potassium iodine battery |
-
2018
- 2018-10-10 CN CN201811176388.5A patent/CN109273669A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102544574A (en) * | 2011-12-30 | 2012-07-04 | 华中科技大学 | Flexible lithium ion battery and packaging method thereof |
| CN103606657A (en) * | 2013-12-10 | 2014-02-26 | 北京理工大学 | Lithium ion battery zinc oxide/porous carbon composite negative electrode material with high capacity and preparation method thereof |
| CN107221640A (en) * | 2017-06-09 | 2017-09-29 | 北京科技大学 | A kind of preparation method of the compound sodium negative pole of sodium-ion battery |
| CN108075134A (en) * | 2017-12-12 | 2018-05-25 | 江汉大学 | A kind of preparation method of lithium ion battery carbon cloth base cathode oxidation iron |
| CN108470895A (en) * | 2018-03-21 | 2018-08-31 | 同济大学 | A kind of kalium ion battery positive electrode and preparation method thereof, potassium iodine battery |
Non-Patent Citations (1)
| Title |
|---|
| XUEYANG SHEN，ZIPING CAO，JINYA ZHANG等: "In-situ loading of ZnO nanoparticles on carbon felt as novel binder-free flexible anode for high performance lithium-ion batteries", 《MATERIALS LETTERS》 * |
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Application publication date: 20190125 |