CN108063263A - A kind of Prussian blue type aluminium-air cell material and its preparation method and application - Google Patents
A kind of Prussian blue type aluminium-air cell material and its preparation method and application Download PDFInfo
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- CN108063263A CN108063263A CN201711121029.5A CN201711121029A CN108063263A CN 108063263 A CN108063263 A CN 108063263A CN 201711121029 A CN201711121029 A CN 201711121029A CN 108063263 A CN108063263 A CN 108063263A
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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
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/8647—Inert electrodes with catalytic activity, e.g. for fuel cells consisting of more than one material, e.g. consisting of composites
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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
- H01M12/00—Hybrid cells; Manufacture thereof
- H01M12/08—Hybrid cells; Manufacture thereof composed of a half-cell of a fuel-cell type and a half-cell of the secondary-cell type
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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
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/88—Processes of manufacture
- H01M4/8825—Methods for deposition of the catalytic active composition
- H01M4/8828—Coating with slurry or ink
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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
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/90—Selection of catalytic material
- H01M4/9075—Catalytic material supported on carriers, e.g. powder carriers
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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
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Abstract
The present invention provides a kind of flexible aluminium-air cell materials and its preparation method and application, and in particular to aluminium-air cell anode catalyst of the Prussian blue similar object nanometer frame of a kind of sulfur doping by surface modification and its preparation method and application.
Description
Technical field
The invention belongs to field of chemical power source, and in particular to a kind of flexibility aluminium-air cell material and preparation method thereof and should
With the material is a kind of aluminium-air cell anode catalytic of the Prussian blue similar object nanometer frame of sulfur doping by surface modification
Agent.
Background technology
The exhaustion of fossil energy and problem of environmental pollution promote people to go to explore novel renewable energy and energy storage device.Gold
Belong to fuel cell as a kind of emerging mechanism of new electrochemical power sources of recent decades, there is efficiently many advantages, such as with green, can make
For the substitute of the accumulators such as conventional lead acid.Very important one kind among these, aluminium-air cell, compared to other non-lithiums once
It is higher than energy and theoretical electromotive force for secondary cell, and negative material aluminium is cheap and easy to get, is that content is most abundant in the earth's crust
One of metal, global industry reserves are more than 25,000,000,000 tons, while the molecular weight very little of aluminium, light weight, and soft texture, can be with
Different shape is bent or is fabricated to easily for using.In addition the security of aluminium-air cell is significantly larger than lithium-air battery.
The anode of aluminium-air cell is oxygen reduction, and the oxidation of aluminium then occurs for cathode, ultimately generates aluminium hydroxide or the production of meta-aluminic acid root
Object, therefore a key technology of the battery is the anode catalyst of efficient stable.Early stage people are often with noble metals such as platinum, silver
Catalyst anode reacts, but these noble metal earth's crust reserves are low, expensive, can not large-scale use, therefore people
Cheap substitute is sought for, such as patent " aluminium-air cell air electrode and preparation method thereof " (publication number:
CN104505520B, publication date:2017.07.04) providing a kind of modified manganese dioxide material can obtain and precious metal catalyst
The comparable catalytic efficiency of agent.It is Prussian blue as a kind of material by extensive concern, in recent decades in energy storage and conversion
Field has shown excellent potentiality, such as a kind of patent " preparation method of prussian blue complex/carbon composite material and should
With " (publication number:CN103441241B, publication date:2016.08.10) provide a kind of Prussian blue analogues/carbon composite wood
The preparation method of material and its application as lithium ion and sodium-ion battery positive material.The iron cyaniding of the transition metal such as iron-cobalt-nickel
Object, ferrocyanide, cobalt cyanide etc. have constructed huge Prussian blue similar object family, additionally due to Prussian blue easy shape
Into cube shaped looks, substantial amounts of sulfide and oxide-based nanomaterial, the property of nano material have been derived in this, as template
It is largely influenced be subject to material size, pattern, size, so the controlledly synthesis of nano material is always what we studied
Emphasis.These materials have abundant ion aperture, the specific surface area of optimization, and unique pattern can fully optimize promotion aluminium
O for cathode of air battery catalytic activity and stability.In order to solve in the prior art, catalyst is with high costs, and catalytic efficiency is low etc. asks
Topic.The invention discloses a kind of aluminium based on Prussian blue similar object nanocube, high activity, high stability and morphology controllable
O for cathode of air battery catalyst with and its preparation method and application.
The content of the invention
To achieve these goals, the present invention provides a kind of Prussian blue type aluminium-air cell materials and preparation method thereof
And application.The Prussian blue similar object nanometer frame of sulfur doping surface modification synthesized by the present invention has cube frame knot
Structure, and more amorphous nano particle is attached in cube face, it is big that this special nanotopography causes the material to exist
The active site of amount, and the material has larger opposite specific surface area so that aluminium-air cell performance is significantly promoted.
A kind of Prussian blue type aluminium-air cell material preparation method and application, its preparation method are as follows:
1) cobalt chloride hexahydrate, sodium citrate, water are mixed in beaker A, stirring and dissolving;
2) potassium ferricyanide, water are mixed in beaker B, stirring and dissolving;
3) solution in beaker B is poured into rapidly in beaker A, is then vigorously stirred solution in beaker A, is sufficiently mixed it,
Then the mouth of beaker A is sealed, beaker A is placed in freeze-day with constant temperature in baking oven;
4) beaker A is taken out, supernatant is carefully removed, adds water, solution is transferred in 2 centrifuge tubes, after centrifugation in removal
Clear liquid adds in water ultrasonic disperse solid.It centrifuges 7-10 times by same procedure, dries in an oven again;
5) by ferrous sulfate, hydrochloric acid solution is mixed in beaker C, stirring and dissolving, is added in drying product obtained by step 4), is surpassed
Sound;
6) solution after ultrasound is transferred in 2 centrifuge tubes, abandoning supernatant after centrifugation adds water, and ultrasonic disperse is solid
Body.It centrifuges 5-7 times by same procedure, dries in an oven again;
7) obtained solid, thioacetamide, absolute ethyl alcohol in step 6) are mixed in hydrothermal reaction kettle liner A, stirred
Dissolving, reaction kettle liner is sealed in stainless steel cauldron, is placed in baking oven and reacts, and is taken out reaction kettle and is cooled to room temperature;
8) solution after reaction is transferred in 2 centrifuge tubes, adds in absolute ethyl alcohol ultrasound point after centrifugation after abandoning supernatant
Dissipate solid.It is centrifuging 7-10 times by same procedure, is drying in an oven.
Further, 30 DEG C of baking oven constant temperature in the step 3), continue 24 it is small when.
Further, in the step 4), step 6), step 8), centrifugation rate is 10000rpm/min, the time 5
Minute.
Further, in the step 5), concentration of hydrochloric acid 2mol/L, when ultrasonic time is 1 small.
Further, in the step 6), oven temperature is 40 DEG C.
Further, in the step 7), oven temperature is 160 DEG C, reaction time 6h.
Further, in the step 8), oven temperature is 40 DEG C.
Further, it is electric in aluminium air such as Prussian blue type aluminium-air cell material prepared by any one the method
Application in pond as anode catalyst.
The Prussian blue similar object nanocube of sulfur doping of the surface modification has amorphous nanometer for surface growth
The cube frame structure of grain is as follows using step in flexible aluminium-air cell:
1) by 5g polyvinyl alcohol, 0.5g polyoxyethylene, 50mL water is mixed in the plastic beaker of 100mL, is put into oil bath pan
In, when 95 DEG C of stirrings 2 are small.
2) by 5g potassium hydroxide, 0.5g zinc oxide, 0.15g sodium stannates, 5mL water is mixed in the glass beaker of 25mL, stirs
Poured into after mixing dissolving in the solution that stirring is completed in step 1), 95 DEG C continue stirring 1 it is small when.
3) solution in step 2) is poured into while hot in tubular container, is put into -18 DEG C of freeze overnights of freezer compartment of refrigerator, Ran Houfang
Enter 4 DEG C of defrostings of cold compartment of refrigerator and store to obtain Signa Gel.
4) catalyst of preparation is weighed into 5mg, then the carbon dust of quality such as weighs, be put into 5ml petroleum ether ultrasound 3 it is small when bear
Carbon is carried, is finally putting into baking oven and dries petroleum ether.
5) product for obtaining step 4) weighs the N for adding in 0.98mL, N-dimethylformamide and 20 microlitres of nafion
(perfluorinated sulfonic acid-teflon-copolymers), ultrasound 1 are uniformly mixed that be prepared into solution electrode spare when small;
6) solution electrode for obtaining step 5), which applies, draws 100 microlitres in 1x2cm2It dries, is repeated 4 times on carbon cloth, as
Anode, with 1x2cm2Aluminium flake is cathode, and two electrode slices are crimped onto obtained by step 3) on Signa Gel, is wrapped up with sealed membrane solid
It is fixed.
Beneficial effects of the present invention are:Aluminium-air cell anode catalyst high activity provided by the present invention, high stability,
High efficiency and morphology controllable.
Description of the drawings
Fig. 1 is the X-ray diffractogram of sulfur doping Prussian blue similar object nanometer frame of the present invention Jing Guo surface modification
(XRD)。
Fig. 2 is the transmission electron microscope of sulfur doping Prussian blue similar object nanometer frame of the present invention Jing Guo surface modification
Scheme (TEM).
Fig. 3 is the scanning electron microscope of sulfur doping Prussian blue similar object nanometer frame of the present invention Jing Guo surface modification
Scheme (SEM).
Fig. 4 is the aluminium-air cell power of sulfur doping Prussian blue similar object nanometer frame of the present invention Jing Guo surface modification
Density map.
Fig. 5 is the aluminium-air cell capacity of sulfur doping Prussian blue similar object nanometer frame of the present invention Jing Guo surface modification
Figure.
Specific embodiment
To make the object, technical solutions and advantages of the present invention clearer, below in conjunction with attached drawing to embodiment party of the present invention
Formula is described in further detail, and following embodiment is only presently preferred embodiments of the present invention, is not intended to limit the invention, it is all
Within the spirit and principles in the present invention, any modifications, equivalent replacements and improvements are made should be included in the protection of the present invention
Within the scope of.
The water used in experimentation is the ultra-pure water that electrical conductivity is 18.25M Ω, and it is analysis to test reagent used
It is pure.
The instrument and reagent used:Indigo plant electricity CT2001A battery test systems are purchased from the limited public affairs of the blue electric electronics share in Wuhan City
Department tests for battery capacity;CHI660E electrochemical workstations are purchased from Shanghai Chen Hua instrument company, real for linear voltammetry
It tests;Excellent Pood laboratory Superpure water machine is purchased from Chengdu Ultra Pure Science & Technology Co., Ltd, is used to prepare ultra-pure water;Electronic balance is purchased from upper
Hai Bole mechanical & electronic equipment corporation, Ltds, for weighing drug;D/max-2400 is purchased from Rigaku company (Rigaku), carries out X
X ray diffraction characterizes;JSM-6701F cold field emission types scanning electron microscope is purchased from Jeol Ltd. and TECNAI
G2TF20 Flied emissions transmission electron microscope is purchased from FEI Co. of the U.S., for the morphology characterization of anode catalyst;Vacuum drying chamber
Purchased from Shanghai Yiheng Scientific Instruments Co., Ltd;KQ5200 ultrasonic cleaners are purchased from Kunshan Ultrasonic Instruments Co., Ltd.;Platform
Formula drying box is purchased from Chongqing testing equipment factory;Electronic thermostatic stainless steel water bath sieves cotton mill purchased from Shanghai Xuan Chang instruments;Cobalt chloride,
Sodium citrate, sodium stannate are purchased from Tianjin Kai Tong chemical reagent Co., Ltd;The potassium ferricyanide, ferrous sulfate, potassium hydroxide, oxygen
Change zinc and be purchased from Sinopharm Chemical Reagent Co., Ltd.;Polyvinyl alcohol, polyethylene glycol oxide are purchased from Shanghai Mike's woods biochemistry section
Skill Co., Ltd;Thioacetamide is purchased from Tianjin Kermel Chemical Reagent Co., Ltd..
A kind of preparation method of Prussian blue type aluminium-air cell material of embodiment 1
1) by 0.1428g cobalt chloride hexahydrates, 0.2647g sodium citrates, 20mL water is mixed in the beaker A of 50mL, stirs
Mix dissolving.
2) by the 0.1317g potassium ferricyanides, 20mL water is mixed in the beaker B of 50mL, stirring and dissolving.
3) solution in beaker B is poured into rapidly in beaker A, is then vigorously stirred solution 5 minutes in beaker A, make it fully
Mixing then seals the mouth of beaker A with preservative film, when beaker A is placed in constant temperature 24 is small in 30 degrees Celsius of baking ovens.
4) beaker is taken out, carefully removes supernatant, suitable quantity of water is added in, solution is transferred in the centrifuge tube of 2 10mL,
10000rpm/min is centrifuged 5 minutes, removes supernatant, adds in water ultrasonic disperse solid.It is centrifuged again by same procedure
It is 7-10 times, dry in 40 DEG C of baking ovens.
5) by 0.50g ferrous sulfate, 20mL 2mol/L hydrochloric acid solutions are mixed in beaker C, stirring and dissolving, are added in
Drying product obtained by 0.050g steps 4), when ultrasound 1 is small.
6) solution after ultrasound is transferred in the centrifuge tube of 2 10mL, 10000rpm/min centrifugation 5min, abandoning supernatant
Water ultrasonic disperse solid is added in afterwards.It is centrifuged 5-7 times again by same procedure, it is dry in 40 DEG C of baking ovens.
7) by obtained solid in 0.040g steps 6), 0.100g thioacetamides, 40mL absolute ethyl alcohols are mixed in 50mL's
In hydrothermal reaction kettle liner A, reaction kettle liner is sealed in stainless steel cauldron by stirring and dissolving, be placed in baking oven 160 DEG C it is anti-
6h is answered, reaction kettle is taken out and is cooled to room temperature.
8) solution after reaction is transferred in the centrifuge tube of 2 10mL, 10000rpm/min centrifugation 5min, abandoning supernatant
Absolute ethyl alcohol ultrasonic disperse solid is added in afterwards.By same procedure in centrifugation 7-10 times, the drying in 40 DEG C of baking ovens.
A kind of application method of the Prussian blue type aluminium-air cell material of embodiment 2 as aluminium-air cell anode catalyst
1) by 5g polyvinyl alcohol, 0.5g polyoxyethylene, 50mL water is mixed in the plastic beaker of 100mL, is put into oil bath pan
In, when 95 DEG C of stirrings 2 are small.
2) by 5g potassium hydroxide, 0.5g zinc oxide, 0.15g sodium stannates, 5mL water is mixed in the glass beaker of 25mL, stirs
Poured into after mixing dissolving in the solution that stirring is completed in step 1), 95 DEG C continue stirring 1 it is small when.
3) solution in step 2) is poured into while hot in tubular container, is put into -18 DEG C of freeze overnights of freezer compartment of refrigerator, Ran Houfang
Enter 4 DEG C of defrostings of cold compartment of refrigerator and store to obtain Signa Gel.
4) catalyst of preparation is weighed into 5mg, then the carbon dust of quality such as weighs, be put into 5ml petroleum ether ultrasound 3 it is small when bear
Carbon is carried, is finally putting into baking oven and dries petroleum ether.
5) product for obtaining step 4) weighs the N for adding in 0.98mL, N-dimethylformamide and 20 microlitres of nafion
(perfluorinated sulfonic acid-teflon-copolymers), ultrasound 1 are uniformly mixed that be prepared into solution electrode spare when small;
6) solution electrode for obtaining step 5), which applies, draws 100 microlitres in 1x2cm2It dries, is repeated 4 times on carbon cloth, as
Anode, with 1x2cm2Aluminium flake is cathode, and two electrode slices are crimped onto obtained by step 3) on Signa Gel, is wrapped up with sealed membrane solid
It is fixed.
The member of the energy storage containing a kind of Prussian blue type aluminium-air cell anode catalyst in 3 embodiment 2 of embodiment
The performance test of part
Capacity is measured under 1mA/cm2 current densities to two electrode system of aluminium-air cell of gained, and in potential window
Linear voltammetry scanning is carried out in the range of 1.4V to 0.7V, sweep speed 5mV/s obtains linear volt-ampere curve.Using
Origin softwares are mapped, and draw the linear scan curve and battery capacity curve of the middle gained of step 6) in above-described embodiment 2.
The aluminium-air cell anode catalyst that invention prepares morphology controllable and efficient stable by high temperature hydro-thermal method passes through table
The Prussian blue similar object nanometer frame of sulfur doping of face modification, X-ray diffractogram (XRD) are as shown in Figure 1.Its special surface
Structure and amorphous FeCoSxConstruct greatly improved catalytic activity its with respect to specific surface area, as fig. 2 shows its transmission electricity
Sub- microscope figure (TEM) and scanning electron microscope diagram shown in Fig. 3.The aluminium of present invention synthesis morphology controllable and efficient stable is empty
This catalyst, is then put by the Prussian blue similar object nanometer frame of sulfur doping of the pneumoelectric pond anode catalyst Jing Guo surface modification
Power density is carried out in aluminium-air cell electrolyte and specific capacity measures, as a result respectively as shown in Figure 4 and Figure 5.Above-mentioned experiment is said
The Prussian blue similar object of sulfur doping of the aluminium-air cell anode catalyst of bright morphology controllable and efficient stable Jing Guo surface modification
Nanometer frame can be used as aluminium-air cell positive electrode, and with superperformance, maximum power density is up to 58.3 milliwatts
Every square centimeter, specific discharge capacity is up to 1259 every gram of milliampere hour under 1 milliampere of discharge current density every square centimeter.
Claims (10)
1. a kind of Prussian blue type aluminium-air cell material preparation method, it is characterised in that the preparation method is as follows:
1) cobalt chloride hexahydrate, sodium citrate, water are mixed in beaker A, stirring and dissolving;
2) potassium ferricyanide, water are mixed in beaker B, stirring and dissolving;
3) solution in beaker B is poured into rapidly in beaker A, is then vigorously stirred solution in beaker A, is sufficiently mixed it, then
The mouth of beaker A is sealed, beaker A is placed in freeze-day with constant temperature in baking oven;
4) beaker A is taken out, supernatant is carefully removed, adds water, solution is transferred in 2 centrifuge tubes, supernatant is removed after centrifugation,
Add in water ultrasonic disperse solid.It centrifuges 7-10 times by same procedure, dries in an oven again;
5) by ferrous sulfate, hydrochloric acid solution is mixed in beaker C, stirring and dissolving, adds in drying product obtained by step 4), ultrasound;
6) solution after ultrasound is transferred in 2 centrifuge tubes, abandoning supernatant after centrifugation, adds water, ultrasonic disperse solid.It presses
Same procedure centrifuges 5-7 times again, dries in an oven;
7) obtained solid, thioacetamide, absolute ethyl alcohol in step 6) are mixed in hydrothermal reaction kettle liner A, stirring and dissolving,
Reaction kettle liner is sealed in stainless steel cauldron, is placed in baking oven and reacts, reaction kettle is taken out and is cooled to room temperature;
8) solution after reaction is transferred in 2 centrifuge tubes, adding in absolute ethyl alcohol ultrasonic disperse after abandoning supernatant after centrifugation consolidates
Body.It is centrifuging 7-10 times by same procedure, is drying in an oven.
2. a kind of Prussian blue type aluminium-air cell material preparation method as described in claim 1, it is characterised in that described
30 DEG C of baking oven constant temperature in step 3), continue 24 it is small when.
3. a kind of Prussian blue type aluminium-air cell material preparation method as described in claim 1, it is characterised in that described
In step 4), step 6), step 8), centrifugation rate is 10000rpm/min, 5 minutes time.
4. a kind of Prussian blue type aluminium-air cell material preparation method as described in claim 1, it is characterised in that described
In step 5), concentration of hydrochloric acid 2mol/L, when ultrasonic time is 1 small.
5. a kind of Prussian blue type aluminium-air cell material preparation method as described in claim 1, it is characterised in that described
In step 6), oven temperature is 40 DEG C.
6. a kind of Prussian blue type aluminium-air cell material preparation method as described in claim 1, it is characterised in that described
In step 7), oven temperature is 160 DEG C, reaction time 6h.
7. a kind of Prussian blue type aluminium-air cell material preparation method as described in claim 1, it is characterised in that described
In step 8), oven temperature is 40 DEG C.
8. the Prussian blue type aluminium-air cell material that in claim 1-7 prepared by any one the method.
9. the answering as anode catalyst in aluminium-air cell of the Prussian blue type aluminium-air cell material described in claim 8
With.
10. a kind of energy storage components, it is characterised in that:The energy storage components contain the Prussia described in claim 7
Blue type aluminium-air cell material.
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CN108461765A (en) * | 2018-05-29 | 2018-08-28 | 武汉大学 | A kind of N-Fe/FeC3@AC microbial fuel cell air cathode electrocatalysis materials and preparation method thereof |
CN109461944A (en) * | 2018-10-10 | 2019-03-12 | 暨南大学 | The cube FeOOH or Fe being supported on nano-sized carbon band4(Fe(CN)6)3Preparation method and application |
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CN108461765B (en) * | 2018-05-29 | 2021-04-16 | 武汉大学 | N-Fe/FeC3Air cathode electro-catalytic material of @ AC microbial fuel cell and preparation method thereof |
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