CN104466177B - A kind of nickel coated perfluorocarbon positive electrode and preparation method thereof - Google Patents
A kind of nickel coated perfluorocarbon positive electrode and preparation method thereof Download PDFInfo
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- CN104466177B CN104466177B CN201410727090.4A CN201410727090A CN104466177B CN 104466177 B CN104466177 B CN 104466177B CN 201410727090 A CN201410727090 A CN 201410727090A CN 104466177 B CN104466177 B CN 104466177B
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- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
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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
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- H—ELECTRICITY
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
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Abstract
The invention discloses a kind of nickel coated perfluorocarbon positive electrode and preparation method thereof, this positive electrode is made up of perfluorocarbon particle surface one layer of nickel coating of cladding；Its preparation method be perfluorocarbon granule is sequentially passed through sensitization, activation, reduction treatment under the effect of dispersant after, nickel plating coating；Again the perfluorocarbon granule having plated nickel coating is carried out heat treatment, obtain nickel coated perfluorocarbon positive electrode；This preparation method is simple to operate, process conditions are gentle, low cost；The nickel coated perfluorocarbon positive electrode prepared, nickel coating is evenly coated, Stability Analysis of Structures, can be used for the lithium fluorocarbon battery preparing good conductivity, specific capacity is high, power density is big.
Description
Technical field
The present invention relates to a kind of nickel coated perfluorocarbon positive electrode and preparation method thereof, belong to cell positive material,
Particularly one-shot battery positive electrode field.
Background technology
Nearly ten years, China's mancarried electronic aid, aerostatics, Aero-Space and organism are implanted into the necks such as power supply
Territory development is swift and violent, therefore urgent to height ratio capacity, high power and light-weighted one-shot battery demand.
Lithium fluorocarbon battery is the one-shot battery that the most theoretical specific energy (2180Wh/kg) is maximum, and has
The advantages such as environment friendly and pollution-free, safety is high, temperature range width (-30～80 DEG C), stable operating voltage, have
Well application prospect.At present the most by the advanced country such as the U.S., Japan use in a large number military project, Aero-Space,
The advanced field such as accurate medical treatment.
At present, China's lithium fluorocarbon battery applications is less, and main cause has the following aspects: (1) perfluorocarbon
Costly, cause lithium fluorocarbon battery price high；(2) perfluorocarbon poorly conductive, causes lithium fluorocarbon electricity
Tank discharge efficiency is low；(3) perfluorocarbon surface can be low, causes perfluorocarbon positive electrode dispersion inequality, electrolyte parent
Poor with power, perfluorocarbon electrode produces serious polarization, and battery performance is greatly reduced (voltage is less than 3.0V).People
The method having attempted a lot of improvement perfluorocarbon battery performance.Fluorographite (CFx) is entered by A.Hamwi et al.
Go oxidation, be prepared for fluorine oxide graphite (GFO), to a certain degree improve the hydrophilic of fluorographite,
But it sacrifices the discharge voltage of lithium fluorocarbon battery.Q.Zhang et al. has carried out material with carbon-coated surface to CFx,
To improve its electrical conductivity, prepared lithium fluorocarbon cell voltage slightly improves, and battery multiplying power discharging property is
Improve.CFx is coated with by H.Groult et al. polypyrrole (PPy) that can conduct electricity, and to a certain degree carries
The high high rate performance of lithium fluorocarbon battery.Above-mentioned improved method has necessarily improving lithium fluorocarbon battery performance
Help, but owing to effect is obvious not, thus do not apply in lithium-perfluorocarbon production technology temporarily.
Summary of the invention
It is an object of the invention to be to provide a kind of nickel coating to be evenly coated, Stability Analysis of Structures, can be used for preparation conduction
The nickel coated perfluorocarbon positive electrode of the lithium fluorocarbon battery that property is good, specific capacity is high, power density is big.
Another object of the present invention there are provided a kind of simple to operate, process conditions are gentle, low cost
The method of the perfluorocarbon positive electrode of the nickel coated described in preparation.
The invention provides a kind of nickel coated perfluorocarbon positive electrode, this nickel coated perfluorocarbon positive electrode is by being fluorinated
One layer of nickel coating of carbon granule Surface coating is constituted.
The nickel coated perfluorocarbon positive electrode of the present invention also includes following preferred version:
Preferably in nickel coated perfluorocarbon positive electrode, nickel coating thickness is 0.1～1.0 μm.
Preferably in nickel coated perfluorocarbon positive electrode, nickel coating is the nickel phosphorus conjunction of phosphorus weight/mass percentage composition ＜ 8%
Gold.
Preferably in nickel coated perfluorocarbon positive electrode, perfluorocarbon granule is fluorination coke, fluorographite, fluorination stone
One or more in ink alkene, fluorinated carbon fiber, carbon fluoride nano-tube granular materials.
In preferred nickel coated perfluorocarbon positive electrode, perfluorocarbon particle size distribution is between 2～20 μm, fluorine carbon
Atom number ratio is 0.8～1.2.
Present invention also offers the preparation method of described nickel coated perfluorocarbon positive electrode, this preparation method be by
After perfluorocarbon granule uses the washing of alcohol water mixed solvent, carry out sensitization, activation and reduction pretreatment successively, locate in advance
Perfluorocarbon granule after reason is dispersed in sulfur acid nickel, sodium hypophosphite, sodium citrate and chlorine under dispersant effect
Change in the mixing plating solution of ammonium and carry out chemical nickel plating coating；Again the perfluorocarbon granule having plated nickel coating is carried out at heat
Reason, to obtain final product.
The preparation method of the nickel coated perfluorocarbon positive electrode of the present invention also includes following preferred version:
Preferably mixing plating solution pH in preparation method is 8～8.5, and in every liter of mixing plating solution, solute is by following components
Composition: nickel sulfate 20～60g, sodium hypophosphite 15～30g, sodium citrate 30～60g, ammonium chloride 30～70g,
Dispersant 0.2～2mL.
Preferably mixing plating solution solvent in preparation method is water.
Preferably in preparation method, dispersant is one or more in OP-10, sucrose ester, Polysorbate.
Preferably in preparation method, heat treatment is to be in temperature by the perfluorocarbon granule having plated nickel coating
100～200 DEG C are incubated 1～4 hour.
Preferably in preparation method, alcohol water mixed solvent is that the mixing that second alcohol and water 1:2～3:1 by volume forms is molten
Agent.
Preferably in preparation method perfluorocarbon particulate material to manage usage amount in step throughout (molten less than 30g/L
Liquid).
Preferably in preparation method, washing is to wash under the ultrasonic wave added that frequency is 20～40kHz, and the time is
1～30min.
Preferably in preparation method, sensitization is the hydrochloric acid solution stirring that perfluorocarbon granule is placed in chloride containing stannous；Its
In, in the hydrochloric acid solution of every liter of chloride containing stannous, solute is composed of the following components: stannous chloride 2～8g, dense salt
Acid HCl 2～6mL, dispersant 0.2～2mL；Solvent is water.
Perfluorocarbon granule after preferably activation is by sensitized treatment in preparation method is placed in the hydrochloric acid of chloride containing palladium
Solution is stirred；Wherein, in the hydrochloric acid solution of every liter of chloride containing palladium, solute is composed of the following components: chlorination
Palladium 0.1～1g, concentrated hydrochloric acid HCl 4～10mL, dispersant 0.2～2mL；Solvent is water.
Perfluorocarbon granule after preferably reduction is by activation processing in preparation method is placed in ortho phosphorous acid sodium solution
In be stirred；Described ortho phosphorous acid sodium solution is composed of the following components: sodium hypophosphite 1～5wt%, point
Powder 0.2～2mL/L, solvent is water.
The preparation method of the nickel coated perfluorocarbon positive electrode of the present invention includes step in detail below:
Step 1: washing
Perfluorocarbon granule is placed in the mixed solvent of second alcohol and water 1:2～3:1 by volume composition, takes machinery
Stirring, mixing speed is 50～500 revs/min, and temperature is 15～40 DEG C, frequency be 20～40kHz super
The lower washing 1～30min of sound auxiliary, centrifugation, water washs for several times；
Step 2: sensitization
Step 1 gained perfluorocarbon granule is placed in the hydrochloric acid solution of the chloride containing stannous that temperature is 15～40 DEG C, adopts
Taking mechanical agitation, stir 1～10min with the speed of 50～500 revs/min, centrifugation, water washs for several times；
The hydrochloric acid solution of described chloride containing stannous is composed of the following components: stannous chloride 2～8g/L, concentrated hydrochloric acid HCl
2～6mL/L, dispersant 0.2～2mL/L, solvent is water；
Step 3: activation
The hydrochloric acid that perfluorocarbon granule after the sensitized treatment of step 2 is placed in the chloride containing palladium that temperature is 15～40 DEG C is molten
In liquid, take mechanical agitation, stir with the speed of 50～500 revs/min and carry out activation processing 1～10min, from
The heart separates, and water washs for several times；The hydrochloric acid solution of described chloride containing palladium is composed of the following components: Palladous chloride.
0.1～1g/L, concentrated hydrochloric acid HCl 4～10mL/L, dispersant 0.2～2mL/L, solvent is water；
Step 4: reduction
Perfluorocarbon granule after step 3 activation processing is placed in the ortho phosphorous acid sodium solution that temperature is 15～40 DEG C,
Take mechanical agitation, stir with the speed of 50～500 revs/min and carry out reduction treatment 0.5～5min, centrifugation；
Described ortho phosphorous acid sodium solution is composed of the following components: sodium hypophosphite 1～5wt%, dispersant 0.2～2
ML/L, solvent is water；
Step 5: chemical nickel plating
Perfluorocarbon granule after step 4 reduction treatment is placed in the plating solution that pH is 8～8.5,70～90 DEG C of temperature
Under the conditions of degree, take mechanical agitation, stir with the speed of 50～500 revs/min and carry out chemical nickel plating 0.5～10min,
Centrifugation, water washs for several times；Described plating solution is composed of the following components: nickel sulfate 20～60g/L, secondary Asia
Sodium phosphate 15～30g/L, sodium citrate 30～60g/L, ammonium chloride 30～70g/L, dispersant 0.2～2mL/L,
Solvent is water；
Step 6: heat treatment
Perfluorocarbon granule after step 5 chemical nickel plating is placed under the temperature environment of 100～200 DEG C, is incubated 1～4
Hour, obtain nickel coated perfluorocarbon positive electrode.
Beneficial effects of the present invention: the present invention uses nickel coated carbon fluoride powder granule to prepare a kind of electric conductivity first
Performance is good, constitutionally stable nickel coated perfluorocarbon positive electrode, can be used for preparing height ratio capacity and high power density
Lithium fluorocarbon battery.The advantage that technical solution of the present invention is prominent is: 1, the present invention is to carbon fluoride powder
Grain surface cladded with nickel, on the one hand can improve the electric conductivity of positive electrode, beneficially electron transmission, adds fast response speed
Degree, is effectively improved the discharge power of lithium fluorocarbon battery；On the other hand can with the amphipathic property of reinforcing material,
Be conducive to the exchange of material surface solution and ion transport, reduce electrode polarization, promote cell discharge voltage platform,
Improve cell power conversion efficiency.2, the nickel coated fluorination carbon dust prepared after the present invention uses nickel coated perfluorocarbon
End granular materials electric conductivity is greatly improved, when making perfluorocarbon electrode, it is possible to reduce uses or does not use carbon
Conductive agent.3, the preparation method of the present invention, all uses dispersant in whole preparation technology, can be by perfluorocarbon
Granule is effectively dispersed in solution, is more beneficial for sensitization, activates, reduces and nickel process, in order to obtains
Obtain coating to be evenly coated, constitutionally stable nickel coated perfluorocarbon positive electrode.4, the preparation technology behaviour of the present invention
Making simple, process conditions are gentle, and production cost is low, meets industrialized production.
Accompanying drawing explanation
[Fig. 1] is the structural representation of nickel coated perfluorocarbon granule: 1 represents perfluorocarbon granule；2 represent nickel coating.
[Fig. 2] is the scanning electron microscope (SEM) photograph of the nickel coated perfluorocarbon granule that embodiment 1 prepares.
[Fig. 3] is the battery that the nickel coated perfluorocarbon positive electrode that embodiment 1 prepares is made with perfluorocarbon positive electrode
Specific discharge capacity comparison diagram.
Detailed description of the invention
Following example are intended to further illustrate present invention rather than limit the scope of the invention.
Embodiment 1
Taking the fluorographite granule 5g that fluorine carbon atomic ratio is 1.03, granular size is 5～10 μm, carries out chemical plating
Nickel processes, and the technique of chemical nickel plating is:
(1) clean
Above-mentioned perfluorocarbon is added ethanol with water volume ratio is 1:1, and cumulative volume is in the alcohol water blend of 1L.
Temperature is 25 DEG C, mixing speed 200 rpms, ultrasonic wave concussion, shakes frequency 30kHz, and the time is
5min。
By perfluorocarbon centrifugation, and with deionized water rinsing repeatedly.
(2) sensitization
It is stannous chloride (SnCl that perfluorocarbon after cleaning adds composition2·2H2O) 4g/L, 37%HCl 4mL/L,
OP-101mL/L, solvent is deionized water, and volume is in the solution of 1L.Temperature is 25 DEG C, mixing speed
200 rpms, the time is 2min.
By perfluorocarbon centrifugation, and it is 7 with deionized water rinsing to pH.
(3) activation
Perfluorocarbon after sensitization is added composition is Palladous chloride. (PdCl2) 0.4g/L, 37%HCl 8mL/L, OP-10
1mL/L, solvent is deionized water, and volume is in the solution of 1L.Temperature is 25 DEG C, mixing speed 200 turns
Per minute, the time is 2min.
By perfluorocarbon centrifugation, and it is 7 with deionized water rinsing to pH.
(4) reduction
Perfluorocarbon after activation is added composition is sodium hypophosphite (NaH2PO2·H2O) 3% mass fraction,
OP-101mL/L, solvent is deionized water, and volume is in the solution of 1L.Temperature is 25 DEG C, mixing speed
200 rpms, the time is 1min.
By perfluorocarbon centrifugation.
(5) chemical nickel plating
Perfluorocarbon after reduction is added composition is nickel sulfate (NiSO4 6H2O) 35g/L, sodium hypophosphite
(NaH2PO2·H2O) 20g/L, sodium citrate (C6H5Na3O7·2H2O) 45g/L, ammonium chloride (NH4Cl) 50g/L,
Surfactant 1mL/L, solvent is deionized water, and volume is in the solution of 1L.Adjust with ammonia or citric acid
Joint is pH 8～8.5, and temperature is 85 DEG C, mixing speed 200 rpms, and the time is 3min.
(6) heat treatment
Perfluorocarbon after chemical nickel plating is put in the baking oven of 150 DEG C, be incubated 2 hours.
Preparing the perfluorocarbon positive electrode of nickel coated, nickel coating thickness is about 0.5 μm, and nickel coating phosphorus content is about
3.5%.
Before and after thickness of coating uses laser particle analyzer comparative observation cladding, perfluorocarbon particle size draws.
By the perfluorocarbon after cladding and PVDF 8:1 in mass ratio, making stirring solvent with NMP uniform, warp exists
It is coated with on aluminium foil, dries, make electrode after cut-parts, then be assembled into 2032 types in the glove box of argon condition
Button lithium battery, negative pole is lithium sheet, and electrolyte solute is the LiPF6 of 1mol/L, and electrolyte solvent is 1:1's
PC (Allyl carbonate) and EC (ethylene carbonate), uses polyethylene diagrams.
The fluorographite of battery embodiment assembled nickel uncoated with the same terms is made the battery of positive pole and is carried out
Discharge test contrasts, and discharge current is 100mA/g.Result is illustrated in fig. 3 shown below.From test result, this
CFx after embodiment nickel coated increases on discharge platform than pure CFx, and specific discharge capacity improves 2
More than Bei.
Embodiment 2
Taking the fluorinated carbon fiber 20g that fluorine carbon atomic ratio is 0.85, granular size is 10～15 μm, carries out chemical plating
Nickel processes, and the technique of chemical nickel plating is:
(1) clean
Above-mentioned perfluorocarbon is added ethanol with water volume ratio is 1:2, and cumulative volume is in the alcohol water blend of 1L.
Temperature is 25 DEG C, mixing speed 200 rpms, ultrasonic wave concussion, shakes frequency 35kHz, and the time is
8min。
By perfluorocarbon centrifugation, and with deionized water rinsing repeatedly.
(2) sensitization
It is stannous chloride (SnCl that perfluorocarbon after cleaning adds composition2·2H2O) 7g/L, 37%HCl 5mL/L,
Sucrose ester and each 0.5mL/L of OP-10, solvent is deionized water, and volume is in the solution of 1L.Temperature is 25 DEG C,
Mixing speed 400 rpms, the time is 2min.
By perfluorocarbon centrifugation, and it is 7 with deionized water rinsing to pH.
(3) activation
Perfluorocarbon after sensitization is added composition is Palladous chloride. (PdCl2) 0.8g/L, 37%HCl 4mL/L, sucrose
Ester and each 0.5mL/L of OP-10, solvent is deionized water, and volume is in the solution of 1L.Temperature is 25 DEG C,
Mixing speed 200 rpms, the time is 2min.
By perfluorocarbon centrifugation, and it is 7 with deionized water rinsing to pH.
(4) reduction
Perfluorocarbon after activation is added composition is sodium hypophosphite (NaH2PO2·H2O) 4% mass fraction, sugarcane
Sugar ester and each 0.5mL/L of OP-10, solvent is deionized water, and volume is in the solution of 1L.Temperature is 25 DEG C,
Mixing speed 200 rpms, the time is 1min.
By perfluorocarbon centrifugation.
(5) chemical nickel plating
Perfluorocarbon after reduction is added composition is nickel sulfate (NiSO4·6H2O) 50g/L, sodium hypophosphite
(NaH2PO2·H2O) 25g/L, sodium citrate (C6H5Na3O7·2H2O) 30g/L, ammonium chloride (NH4Cl) 60g/L,
Sucrose ester and each 0.5mL/L of OP-10, solvent is deionized water, and volume is in the solution of 1L.With ammonia or
Citric acid is adjusted to pH 8～8.5, and temperature is 80 DEG C, mixing speed 200 rpms, and the time is 3min.
(6) heat treatment
Perfluorocarbon after chemical nickel plating is put in the baking oven of 200 DEG C, be incubated 1 hour.
Preparing the perfluorocarbon positive electrode of nickel coated, nickel coating thickness is about 0.6 μm, and nickel coating phosphorus content is about
3%.
Before and after thickness of coating uses laser particle analyzer comparative observation cladding, perfluorocarbon particle size draws.
By the perfluorocarbon after cladding and PVDF 8:1 in mass ratio, making stirring solvent with NMP uniform, warp exists
It is coated with on aluminium foil, dries, make electrode after cut-parts, then be assembled into 2032 types in the glove box of argon condition
Button lithium battery, negative pole is lithium sheet, and electrolyte solute is the LiPF6 of 1mol/L, and electrolyte solvent is 1:1's
PC (Allyl carbonate) and EC (ethylene carbonate), uses polyethylene diagrams.
The fluorographite of battery embodiment assembled nickel uncoated with the same terms is made the battery of positive pole and is carried out
Discharge test contrasts, and discharge current is 100mA/g.Show that the CFx after the present embodiment nickel coated is than pure CFx
Discharge platform increases, and specific discharge capacity improves more than 2 times.
Claims (1)
1. a preparation method for nickel coated perfluorocarbon positive electrode, this positive electrode is coated with by perfluorocarbon particle surface
One layer of nickel coating is constituted, it is characterised in that preparation method comprises the following steps:
Step 1: washing
Perfluorocarbon granule is placed in the mixed solvent of second alcohol and water 1:1 by volume composition, takes mechanical agitation,
Mixing speed is 200 revs/min, and temperature is 25 DEG C, washs 5min under the ultrasonic wave added that frequency is 30kHz,
Centrifugation, water washs for several times；
Step 2: sensitization
Step 1 gained perfluorocarbon granule is placed in the hydrochloric acid solution of the chloride containing stannous that temperature is 25 DEG C, adopts
Taking mechanical agitation, stir 2min, centrifugation with the speed of 200 revs/min, water washs for several times；Described
The hydrochloric acid solution of chloride containing stannous is composed of the following components: stannous chloride 4g/L, concentrated hydrochloric acid HCl 4mL/L, point
Powder OP-10 is 1mL/L, and solvent is water；
Step 3: activation
Perfluorocarbon granule after step 2 sensitized treatment is placed in the hydrochloric acid solution of the chloride containing palladium that temperature is 25 DEG C
In, take mechanical agitation, stir with the speed of 200 revs/min and carry out activation processing 2min, centrifugation,
Water washs for several times；The hydrochloric acid solution of described chloride containing palladium is composed of the following components: Palladous chloride. 0.4g/L, dense salt
Acid HCl 8mL/L, dispersant OP-10 1mL/L, solvent is water；
Step 4: reduction
Perfluorocarbon granule after step 3 activation processing is placed in the ortho phosphorous acid sodium solution that temperature is 25 DEG C,
Take mechanical agitation, stir with the speed of 200 revs/min and carry out reduction treatment 1min, centrifugation；Described
Ortho phosphorous acid sodium solution composed of the following components: sodium hypophosphite 3wt%, dispersant OP-10 is 1mL/L,
Solvent is water；
Step 5: chemical nickel plating
Perfluorocarbon granule after step 4 reduction treatment is placed in the plating solution that pH is 8～8.5,85 DEG C of temperature
Under the conditions of, take mechanical agitation, stir with the speed of 200 revs/min and carry out chemical nickel plating 3min, centrifugal point
From, water washs for several times；Described plating solution is composed of the following components: nickel sulfate 35g/L, sodium hypophosphite 20g/L,
Sodium citrate 45g/L, ammonium chloride 50g/L, dispersant OP-10 are 1mL/L, and solvent is water；
Step 6: heat treatment
Perfluorocarbon granule after step 5 chemical nickel plating is placed under the temperature environment of 150 DEG C, is incubated 2 hours,
Obtain nickel coated perfluorocarbon positive electrode.
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| CN107369834B (en) * | 2017-07-12 | 2020-08-07 | 天津巴莫科技股份有限公司 | Composite carbon fluoride anode material and preparation method and application thereof |
| CN109888268B (en) * | 2017-12-06 | 2023-12-01 | 中国科学院大连化学物理研究所 | Oxide/fluorocarbon composite positive electrode material for lithium primary battery and preparation method thereof |
| CN109962240A (en) * | 2017-12-25 | 2019-07-02 | 中国电子科技集团公司第十八研究所 | Method for preparing anode slurry for lithium carbon fluoride battery with carbon nanotube as conductive agent |
| CN111029575B (en) * | 2019-11-06 | 2021-04-13 | 上海空间电源研究所 | Modified carbon fluoride positive electrode material, positive electrode plate containing modified carbon fluoride positive electrode material, battery and preparation method of modified carbon fluoride positive electrode material |
| CN111969188B (en) * | 2020-08-20 | 2022-06-17 | 贵州梅岭电源有限公司 | Low-temperature graphene/graphite fluoride cathode material |
| CN114400305A (en) * | 2021-12-14 | 2022-04-26 | 中国电子科技集团公司第十八研究所 | Thermal battery high-voltage spherical carbon fluoride anode material and preparation method thereof |
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