CN109841847A - The preparation method of bending-resistant flexible air cathode suitable for metal-air battery - Google Patents
The preparation method of bending-resistant flexible air cathode suitable for metal-air battery Download PDFInfo
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Abstract
The present invention relates to a kind of preparation methods of bending-resistant flexible air cathode suitable for metal-air battery, it is the following steps are included: 1) by catalyst material, zirconia ball, organic solvent are ground together, and filter out catalyst material and organic solvent through strainer, obtain solution A；2) polymer material is added in organic solvent, obtains solution B；3) solution A and solution B are mixed to form electrostatic spinning solution；4) electrostatic spinning is carried out with electrostatic spinning solution；5) it is statically placed in air after completing electrostatic spinning, hot-press solidifying is carried out after dry tack free；6) by after hot-press solidifying collector and its surface film taking-up be cooled to room temperature, carry out high temperature cabonization, then cooled to room temperature, obtain a kind of bending-resistant flexible air cathode suitable for metal-air battery, be resistant to repeatedly bend, and catalyst material and be distributed near carbon fiber, effectively improve catalytic efficiency, with good chemical property, flexible electronic field can be applied to.
Description
Technical field
The present invention relates to battery material technical field, in particular to a kind of bending-resistant flexible suitable for metal-air battery
Air yin and its pole preparation method.
Background technique
In recent years, flexible electronic and wearable electronic field are quickly grown, such as wearable sensors, flexible display
Deng.Traditional energy has been unable to satisfy the specific demand of flexible electronic, it would therefore be highly desirable to research and develop it is a kind of be suitable for flexible electronic, can
Dress the bending-resistant flexible energy of electronics.
The bending-resistant flexible energy suitable for flexible electronic, wearable electronic need to have three characteristics: first, it is small in size and
Energy density is high, has good chemical property；Second, since flexible electronic is commonly used for wearable sensors, such as rehabilitation
Muscle sensor in training needs continuously to bend in the course of work, therefore its energy should also have good mechanical flexibility, can
Adapt to the operating condition continuously bent.Metal air battery cathodes reaction raw materials are the oxygen in air, small in size, light-weight,
Specific energy is high, excellent electrochemical performance, and environmental-friendly, receives significant attention, especially all solid state metal-air battery.It is common
Metal-air battery such as lithium-air battery, zinc-air battery, aluminium-air cell etc..Metal-air battery is mainly by metal sun
Pole, electrolyte and air cathode composition.Wherein, metal anode is usually aluminium foil, zinc foil etc., can meet flexibility requirements；Use gel
Electrolyte replaces conventional liquid electrolyte that can solve electrolyte leakage problem, while meeting flexible demand.Currently, sky resistant to bending
Gas cathode is a problem to be solved.
Traditional air cathode is usually to mix material requested (conductive carbon material, catalyst, binder), using template
Method, column template, brushing, blade coating, spraying or rolling method, be deposited on collector (such as nickel foam) surface, by height warm
Pressure, is made air cathode.The air cathode specific surface area prepared by this method is low, and during bending or torsion easily
There is the case where surfacing fracture, does not have flexible characteristic.
Electrostatic spinning is a kind of novel non-thermoplastic forming technique, can prepare the electrode material based on three-dimensional microstructures
Material, apply this technology prepare electrode have article introduction, such as Sun Ke, land-sea latitude, Li Da, wait method of electrostatic spinning prepare
Manganese oxide nano wire electrode and its chemical property [J] Journal of Inorganic Materials, 2009,24 (2): 357-360.Using electrostatic
Spin processes prepare the three-diemsnional electrode of mesoporous material, can effectively shorten the diffusion length of ion, can mention under lesser size
For higher energy density and circulation volume, and it is not necessarily to binder.Electrostatic spinning prepares electrode, and spinning solution is generally used such as height
Molecule aggregation solution (such as polyacrylonitrile (PAN)), carbon-fiber film is made in spinning, urges using the addition of the method for grafting or chemically grown
Agent material, by hot setting, (such as Sun Ke, land-sea latitude, Li Da wait method of electrostatic spinning to prepare oxygen for carbonization preparation completion
Change manganese nano wire electrode and its chemical property [J] Journal of Inorganic Materials, 2009,24 (2): 357-360).This method
Air cathode obtained has flexible characteristic, but chemical property is poor, mainly due in preparation process, surface carbon material
It is unevenly distributed with catalyst material, Cluster Phenomenon easy to form, this inhomogenous distribution substantially reduces catalyst material
Catalytic efficiency.In addition, this carbon film electrodes are more fragile, though having ultra-slim features, few bending, continuous long-time are only limited
Bending will lead to carbon film rupture.
Summary of the invention
In consideration of it, being provided simultaneously with flexibility the purpose of the present invention is to provide a kind of excellent electrochemical performance, it is resistant to permanent more
The air cathode and preparation method thereof of secondary bending.
The technical scheme is that a kind of preparation side of the bending-resistant flexible air cathode suitable for metal-air battery
Method comprising following steps:
1) by large granular catalyst material, bulky grain zirconia ball, organic solvent are added in grinding cup, and gross mass is no more than
150 g, wherein the quality of bulky grain zirconia ball is greater than the quality of large granular catalyst material, and carries out nanometer to it and grind
Mill filters out catalyst material and organic solvent through strainer, obtains solution A after grinding；
2) polymer material is added in organic solvent, obtains solution B；
3) solution A and solution B are mixed, as electrostatic spinning solution；
4) electrostatic spinning is carried out to electrostatic spinning solution；
5) collector and its surface film that electrostatic spinning is completed are statically placed in air, it is solid that hot pressing is carried out after dry tack free
Change；
6) by after hot-press solidifying collector and its surface film taking-up be cooled to room temperature, be placed in closed atmosphere furnace high temperature carbon
Change, be passed through inert gas, by room temperature to 750-1100 DEG C, retention time 30-300 min, heating rate is 3-5 per minute
DEG C, then cooled to room temperature to get arrive a kind of bending-resistant flexible air cathode suitable for metal-air battery.
The large granular catalyst material is in manganese dioxide, di-iron trioxide, ferroso-ferric oxide, copper oxide or cobalt oxide
Any one.
The partial size of the large granular catalyst material and bulky grain zirconia ball is greater than 300 nanometers.
Grinding cup is placed in nano grinder in step 1), is carried out by control grinding cup rotation and revolution nano-milled.
The grinding of the nano grinder requires as follows: 800 ~ 1500 revs/min of corase grinding carries out 3 ~ 5 times, and fine grinding 1700 ~
It 2000 revs/min, carries out 3 ~ 5 times.
The partial size of catalyst material is Nano grade in solution A, and partial size is less than 100 nanometers.
The strainer scale is less than or equal to 100 nanometers.
Polymer material is polyacrylonitrile (PAN) or polyvinylpyrrolidone PVP in the step 2.
Electrostatic spinning solution is fitted into syringe in step 4), by syringe pump feed flow, using flat mouth stainless steel syringe needle,
Needle sizes are 0.8-1.5 mm, and printing substrate is nickel foam, which is apart from collector spacing as collector, syringe needle
9-20 cm, printing substrate earthing pole, stainless steel syringe needle connect high-voltage DC power supply, and voltage is 10-25 kV, and printing substrate revolving speed is
250-500 revs/min.
In step 5, by after standing collector and its surface film as in hot press, 200-450 DEG C of temperature, pressure
100-350 MPa solidifies hot pressing 20-180 minutes.
Beneficial effects of the present invention:
Catalyst, mixed polymer solution electrostatic spinning combination wet process nano-milling process, system are prepared using wet process is nano-milled
Standby bending-resistant flexible air cathode.Nm-class catalyst mixed polymer solution, by electrospinning process Direct Spinning in afflux
On body, catalyst material can be made to be evenly distributed on around carbon fiber, catalytic activity be improved, so that chemical property is good.There is collection
Fluid is resistant to permanent repeatedly bending as substrate, significant for flexible electronic field.
Detailed description of the invention
Fig. 1 is air cathode preparation technology flow chart of the present invention.
Fig. 2 is the air cathode that preparation is completed.
Fig. 3 is the constant-current discharge curve of aluminium-air cell under continuous bending state.
Specific embodiment
The embodiment of the present invention is described further below for attached drawing:
The present invention provides a kind of preparation method of bending-resistant flexible air cathode suitable for metal-air battery comprising following
Step:
1) by large granular catalyst material, bulky grain zirconia ball, organic solvent are added in grinding cup, and the bulky grain is urged
Agent material is any one in manganese dioxide, di-iron trioxide, ferroso-ferric oxide, copper oxide or cobalt oxide etc..It is described big
The partial size of particulate catalyst materials and bulky grain zirconia ball is greater than 300 nanometers.Gross mass is no more than 150 g, wherein greatly
The quality of particulate zirconium oxide bead is greater than the quality of large granular catalyst material, and carries out to it nano-milled, and grinding cup is set
In nano grinder, carried out by control grinding cup rotation and revolution nano-milled.The grinding of the nano grinder requires such as
Under: 800 ~ 1500 revs/min of corase grinding carries out 3 ~ 5 times, refines 1700 ~ 2000 revs/min, carries out 3 ~ 5 times.After grinding, through strainer
It filters out catalyst material and organic solvent, obtains solution A, the partial size of catalyst material is Nano grade in solution A, and partial size
Less than 100 nanometers, wherein the strainer scale is less than or equal to 100 nanometers；
2) polymer material is added in organic solvent, obtains solution B, polymer material is polyacrylonitrile (PAN) or polyethylene
Pyrrolidones PVP, wherein organic solvent can be DMF, ethyl alcohol, ethylene glycol etc.；
3) solution A and solution B are mixed, as electrostatic spinning solution；
4) electrostatic spinning is carried out to electrostatic spinning solution, electrostatic spinning solution is fitted into syringe, by syringe pump feed flow, is adopted
With flat mouth stainless steel syringe needle, needle sizes are 0.8-1.5 mm, and printing substrate is nickel foam, and the nickel foam is as collector, needle
Head is 9-20 cm apart from collector spacing, and printing substrate earthing pole, stainless steel syringe needle meets high-voltage DC power supply, voltage 10-25
KV, printing substrate revolving speed are 250-500 revs/min；
5) collector and its surface film that electrostatic spinning is completed are statically placed in air, it is solid that hot pressing is carried out after dry tack free
Change, by after standing collector and its surface film as in hot press, 200-450 DEG C of temperature, pressure 100-350 MPa, Gu
Change hot pressing 20-180 minutes；
6) by after hot-press solidifying collector and its surface film taking-up be cooled to room temperature, be placed in closed atmosphere furnace high temperature carbon
Change, be passed through inert gas, by room temperature to 750-1100 DEG C, retention time 30-300 min, heating rate is 3-5 per minute
DEG C, then cooled to room temperature to get arrive a kind of bending-resistant flexible air cathode suitable for metal-air battery.
Embodiment 1, using manganese dioxide as catalyst, polymer material is polyacrylonitrile (PAN), and organic solvent is diformazan
Base formamide DMF.
Nano-milled manganese dioxide-catalyst
By 4g manganese dioxide, 10.5g zirconium oxide, 10gDMF solvent is added in grinding cup, is placed in nano grinder.1000
Rev/min corase grinding 5 times, 2000 revs/min refine 3 times.It is filtered after ground with 100 nanometers of sieve, takes out filtrate 5.775g,
It wherein include 2.64g manganese dioxide, 4.125gDMF is solution A.
Electrostatic spinning prepares air cathode material
2.4g PAN is added in 24.825g DMF solution, 60 DEG C is heated and stirs 12 hours, is solution B.By solution A and molten
Liquid B mixing, is made into electrostatic spinning solution.Solution is moved into syringe, stainless steel syringe needle is 1.2 6mm, high-voltage DC power supply is connect,
Voltage is 19kV.Printing substrate is 0.2 mm thickness nickel foam, and revolving speed is 250 revs/min, and stainless steel syringe needle is 13 cm apart from substrate.
After electrostatic spinning film forming, nickel foam and its surface film are removed, is placed in air and stands 24 h.After preliminarily stabilised, set
In hot press, 250 DEG C, 250MPa hot pressing 2 hours.It after solidification, places it in tube furnace, is passed through argon gas, in argon atmospher
In, 850 DEG C are begun heat to from room temperature, 60 min is kept, increases 5 DEG C of temperature per minute.It is then down to room temperature naturally, from tubular type
Sample, as bending-resistant flexible air cathode are taken out in furnace, are the air cathode that preparation is completed shown in Fig. 2.To detect air
Electrode electro Chemical performance and bending performance prepare flexible solid gel electrolyte, electrolyte preparation side by taking aluminium-air cell as an example
Method is referring to a kind of flexible aluminium-air cell and preparation method thereof based on aeroge electrolyte of patent CN106169631A(), gold
Belong to anode and uses 0.2mm thick aluminum foil.By electrochemical workstation electric discharge performance, Fig. 3 show discharge current density and is
5mA/cm2, battery are continuously bent, and bending angle is 150 degree, and completing the primary bending time is 50 s, battery discharge in the case of this
Voltage change situation.
The above is only a preferred embodiment of the present invention, protection scope of the present invention is not limited merely to above-mentioned implementation
Example, all technical solutions belonged under thinking of the present invention all belong to the scope of protection of the present invention.It should be pointed out that for the art
Those of ordinary skill for, several improvements and modifications without departing from the principles of the present invention, these improvements and modifications
It should be regarded as protection scope of the present invention.
Claims (10)
1. a kind of preparation method of the bending-resistant flexible air cathode suitable for metal-air battery, it is characterised in that: it includes
Following steps:
1) by large granular catalyst material, bulky grain zirconia ball, organic solvent are added in grinding cup, and gross mass is no more than
150 g, wherein the quality of bulky grain zirconia ball is greater than the quality of large granular catalyst material, and carries out nanometer to it and grind
Mill filters out catalyst material and organic solvent through strainer, obtains solution A after grinding；
2) polymer material is added in organic solvent, obtains solution B；
3) solution A and solution B are mixed, as electrostatic spinning solution；
4) electrostatic spinning is carried out to electrostatic spinning solution；
5) collector and its surface film that electrostatic spinning is completed are statically placed in air, it is solid that hot pressing is carried out after dry tack free
Change；
6) by after hot-press solidifying collector and its surface film taking-up be cooled to room temperature, be placed in closed atmosphere furnace high temperature carbon
Change, be passed through inert gas, by room temperature to 750-1100 DEG C, retention time 30-300 min, heating rate is 3-5 per minute
DEG C, then cooled to room temperature to get arrive a kind of bending-resistant flexible air cathode suitable for metal-air battery.
2. the preparation method of the bending-resistant flexible air cathode according to claim 1 suitable for metal-air battery,
Be characterized in that: the large granular catalyst material is manganese dioxide, di-iron trioxide, ferroso-ferric oxide, copper oxide or cobalt oxide
In any one.
3. the preparation method of the bending-resistant flexible air cathode according to claim 1 suitable for metal-air battery,
Be characterized in that: the partial size of the large granular catalyst material and bulky grain zirconia ball is greater than 300 nanometers.
4. the preparation method of the bending-resistant flexible air cathode according to claim 1 suitable for metal-air battery,
It is characterized in that: grinding cup being placed in nano grinder in step 1), carried out by control grinding cup rotation and revolution nano-milled.
5. the preparation method of the bending-resistant flexible air cathode according to claim 4 suitable for metal-air battery,
Be characterized in that: the grinding of the nano grinder requires as follows: 800 ~ 1500 revs/min of corase grinding carries out 3 ~ 5 times, and fine grinding 1700 ~
It 2000 revs/min, carries out 3 ~ 5 times.
6. suitable for the bending-resistant flexible air cathode of metal-air battery described according to claim 1 or 2 or 3 or 4 or 5
Preparation method, it is characterised in that: the partial size of catalyst material is Nano grade in solution A, and partial size is less than 100 nanometers.
7. the preparation method of the bending-resistant flexible air cathode according to claim 1 suitable for metal-air battery,
Be characterized in that: the strainer scale is less than or equal to 100 nanometers.
8. the preparation method of the bending-resistant flexible air cathode according to claim 1 suitable for metal-air battery,
Be characterized in that: polymer material is polyacrylonitrile (PAN) or polyvinylpyrrolidone PVP in the step 2.
9. the preparation method of the bending-resistant flexible air cathode according to claim 1 suitable for metal-air battery,
It is characterized in that: electrostatic spinning solution being fitted into syringe in step 4), by syringe pump feed flow, using flat mouth stainless pin
Head, needle sizes are 0.8-1.5 mm, and printing substrate is nickel foam, and the nickel foam is as collector, and syringe needle is between collector
Away from for 9-20 cm, printing substrate earthing pole, stainless steel syringe needle connects high-voltage DC power supply, and voltage is 10-25 kV, and printing substrate turns
Speed is 250-500 revs/min.
10. the preparation method of the bending-resistant flexible air cathode according to claim 1 suitable for metal-air battery,
Be characterized in that: in step 5, by after standing collector and its surface film as in hot press, 200-450 DEG C of temperature, pressure
100-350 MPa solidifies hot pressing 20-180 minutes.
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| CN112615086A (en) * | 2020-12-08 | 2021-04-06 | 中国科学院深圳先进技术研究院 | Flexible pressure sensor and polymer hydrogel electrolyte |
| CN113871761A (en) * | 2021-09-23 | 2021-12-31 | 嘉兴南湖学院 | Air cathode catalyst layer ink suitable for aerosol printing and preparation method thereof |
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Application publication date: 20190604 |