CN109378483A - A kind of novel magnesium air cell catalyst layer material, preparation process and application - Google Patents
A kind of novel magnesium air cell catalyst layer material, preparation process and application Download PDFInfo
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- CN109378483A CN109378483A CN201811171916.8A CN201811171916A CN109378483A CN 109378483 A CN109378483 A CN 109378483A CN 201811171916 A CN201811171916 A CN 201811171916A CN 109378483 A CN109378483 A CN 109378483A
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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
- H01M4/86—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
- H01M4/8657—Inert electrodes with catalytic activity, e.g. for fuel cells consisting of more than one material, e.g. consisting of composites layered
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M12/00—Hybrid cells; Manufacture thereof
- H01M12/04—Hybrid cells; Manufacture thereof composed of a half-cell of the fuel-cell type and of a half-cell of the primary-cell type
- H01M12/06—Hybrid cells; Manufacture thereof composed of a half-cell of the fuel-cell type and of a half-cell of the primary-cell type with one metallic and one gaseous electrode
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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- H01M4/90—Selection of catalytic material
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- 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
- H01M4/9083—Catalytic material supported on carriers, e.g. powder carriers on carbon or graphite
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Abstract
The invention belongs to electrochemical technology fields, provide a kind of novel magnesium air cell catalyst layer material, preparation process and application.Novel magnesium air cell catalyst layer material includes graphene, mangano-manganic oxide and metal nano silver particles, wherein graphene makes mangano-manganic oxide and metal nano silver particles be uniformly adhered to its surface as carrier, and the mass fraction that the metal nano silver particles account for composite material is 22%~66%.The present invention obtains redox graphene by one step hydro thermal method and chemical reduction method and loads mangano-manganic oxide and technology nano silver particles composite material, the composite material stable chemical performance of acquisition, catalytic performance is good, high, the prepared magnesium air battery stable electrical properties of the conductivity of composite material.
Description
Technical field
The invention belongs to electrochemical technology fields, and in particular to a kind of Mn3O4- Ag/rGO new catalytic layer material, preparation work
Skill and application.
Background technique
In recent years, energy consumption gradually increases, and the contradiction of energy demand and supply increasingly contradiction, energy shortage problem is invited
People widely pay close attention to, and in addition fossil energy bring problem of environmental pollution also starts to influence the normal life of people, because of this person
The concern of clean energy resource is also gradually increased.Metal-air battery is a kind of oxygen using in air as active matter
Matter, oxygen reduction reaction occurs under the effect of the catalyst, electronics transfer occurs in the electrolytic solution, converts electric energy for chemical energy
A kind of device.Its anode is main using the oxygen in air as main reactant, and cathode is using common metal as reactant
And its product is pollution-free, meets requirement of the people for modern clean energy resource.
Preparing one kind, which has excellent performance, is for metal-air battery key technology, the good catalysis layer material of stability,
Catalysis layer material most outstanding at present remains Pt/C or Pt alloyed precious metal catalyst material, but due to the storage of noble metal
Storage is rare, expensive, significantly limits the large-scale industrialized production of fuel cell, therefore, finds a kind of new
The efficient oxygen reduction electro-catalyst of type is of great significance for the development of fuel cell.
Good catalyst should have following characteristics: large specific surface area, catalytic performance is excellent, good conductivity, and stability is good.
The features such as graphene has large specific surface area as a kind of novel two-dimentional carbon material, and flexibility is good, and conductivity is high, can make
Catalyst material is uniformly adhered to its surface, can generate synergistic effect with catalyst additionally, due to carbon material itself and improve
Catalytic effect, therefore graphene is the ideal material as catalyst carrier.Manganese-based catalyst is most popular at present urges
Agent, catalytic performance is good, from a wealth of sources, environmental-friendly；The study found that nano silver particles are also that a kind of catalytic performance is excellent
Catalysis material, and be compared to other noble metals, it is from a wealth of sources, it is cheap, and urged in graphene/manganese base
Metal Nano silver grain is introduced on the basis of agent can significantly improve its catalytic performance.
Therefore it is simple to prepare a kind of processing step, low in cost, the good Mn of catalytic performance3O4- Ag/rGO composite material at
For those skilled in the art's technical problem urgently to be resolved.
Summary of the invention
In view of the above-mentioned deficiencies in the prior art, it is an object of the present invention to provide a kind of graphene mutual load mangano-manganic oxide and
The composite material of metal nano silver particles, composite material catalytic performance of the invention is good, and stability is high.The present invention passes through simultaneously
One step hydro thermal method prepares graphene oxide-loaded Mn3O4- Ag further restores composite material by chemical method, preparation process
Simple at low cost, the composite material catalytic performance of acquisition is excellent, and stability is good.
Technical solution of the present invention:
A kind of novel magnesium air cell catalyst layer material, including graphene, mangano-manganic oxide and metal nano silver ion,
Mangano-manganic oxide and metal nano silver particles are uniformly adhered to graphene surface, wherein graphene accounts for magnesium air cell catalyst
The mass fraction of layer material is 10%-15%, and the mass fraction that metal nano silver particles account for magnesium air cell catalyst layer material is
22%~66%, rest part is mangano-manganic oxide.
A kind of preparation process of novel magnesium air cell catalyst layer material, steps are as follows:
Step 1 prepares the ethanol solution of the graphene oxide of 0.04mol/L-0.1mol/L；
Step 2 prepares graphene oxide-loaded mangano-manganic oxide and metal nano silver particles composite material: by manganese acetate
It is added in the ethanol solution for the graphene oxide that step 1 obtains, ultrasound and stirring are uniformly mixed to obtaining under room temperature
Solution a；Silver acetate is added into solution a again, room temperature ultrasound and 50 DEG C of -70 DEG C of stirrings are incited somebody to action to uniformly mixed solution b is obtained
To solution b be transferred in reaction kettle carry out 140 DEG C -160 DEG C of hydro-thermal process 7-9 hours；
Step 3 prepares magnesium air cell catalyst layer material: passing through the graphene oxide that hydro-thermal process obtains to step 2
It loads and adds NaBH aqueous solution (wherein NaBH mass and oxidation stone in mangano-manganic oxide and metal nano silver particles composite material
Black alkene mass ratio is 8:1), it is vigorously stirred, obtains mixed solution c；It is successively molten to mixing with deionized water and dehydrated alcohol
Liquid c carries out multiple eccentric cleaning, until mixed solution pH value is 7,50 DEG C of -70 DEG C of dryings, obtains graphene-supported four oxidation three
The composite material of manganese and nano silver particles, i.e. magnesium air cell catalyst layer material.
In step 1, it is ultrasonically formed the ethanol solution of graphene oxide, ultrasonic power 250W, ultrasonic time is
1h。
In step 2, prepare solution a stirring when it is 30 minutes, ultrasonic power 250W a length of, when it is 10 minutes a length of；Preparation
The constant temperature whipping temp of solution b be 60 DEG C, mixing time be 30 minutes, ultrasonic power 250W, when it is 30 minutes a length of；Hydro-thermal
Reaction temperature is 160 DEG C, and when reaction is 8 hours a length of.
In step 3, when stirring, is 2 hours a length of, and centrifuge speed 2500r-3000r, drying temperature is in drying box
It is 60 DEG C, 24 hours a length of when dry.
Graphene-supported mangano-manganic oxide and nanometer metallic silver corpuscle composite material are used for the catalyst material of magnesium air battery
Material.
Beneficial effects of the present invention:
1. the composite material that the present invention obtains a kind of novel graphene carried catalyst nano particle using one step hydro thermal method
Raw material acquisition is convenient, cheap, preparation process is simple, may be implemented to produce in batches, is that a kind of equipment investment is small, technique stream
The simple new catalyst preparation method of journey.
2. composite material surface of the present invention is uniformly distributed mangano-manganic oxide and metal silver nano-grain, two kinds of nano material phases
Mutually contact, uniformly mixes, is distributed in reduced graphene surface, can not only increase composite material specific surface area, can also be mutual
Effect improves the reducing power to oxygen.In addition, being led in the composite material obtained after hydro-thermal by secondary reduction
The reduced graphene carrier of excellent electrical property, also promotes the performance of composite material.Therefore composite material of the present invention has catalysis
It has excellent performance, the advantages of stable electrochemical property.
3. composite material used in the present invention is by combined factors such as control hydro-thermal time, reaction temperature, proportion of raw material
Consider gained, material oxygen catalytic performance will be greatly improved, thus chemical property, it is close that biggish electric current may finally be shown
Degree, stable electric current, voltage output.
Detailed description of the invention
Fig. 1 is the graphene-supported mangano-manganic oxide of the present invention and nano silver particles composite material X-ray diffractogram.
Fig. 2 is the graphene-supported mangano-manganic oxide of the present invention and nano silver particles composite material Raman spectrogram.
Fig. 3 is the transmission electron microscope microscopic appearance of the present invention graphene-supported mangano-manganic oxide and nano silver particles composite material
Figure.
Fig. 1 gives the X-ray diffractogram of graphene-supported mangano-manganic oxide Yu nano silver particles composite material, shows institute
Contain mangano-manganic oxide and nano silver particles in the composite material of preparation；Fig. 2 is graphene-supported mangano-manganic oxide and nano silver
Have in the Raman spectrogram of particle composite material, prepared graphene-supported mangano-manganic oxide and nano silver particles composite material
There are the peak D and the peak G of typical reduced graphene；Fig. 3 gives prepared graphene-supported mangano-manganic oxide and nanometer silver granuel
The electronic transmission Electronic Speculum microscopic appearance figure of sub- composite material, mangano-manganic oxide and nano silver particles are uniform in prepared composite material
Be distributed in reduced graphene surface.
Specific embodiment
Following non-limiting embodiments can with a person of ordinary skill in the art will more fully understand the present invention, but not with
Any mode limits the present invention.
Below in conjunction with attached drawing and technical solution, a specific embodiment of the invention is further illustrated.
Embodiment 1
The composite material of uniform load mangano-manganic oxide and nano silver particles on a kind of graphene, including reduced graphene,
Mangano-manganic oxide, nano silver particles, mangano-manganic oxide and nano silver particles are uniformly adhered to graphene surface, nano silver particles
Account for composite material mass fraction be 22%, preparation method the following steps are included:
Step 1 prepares graphene oxide water solution: the sheet graphene oxide of 40mg is distributed to the anhydrous second of 80mL
In alcohol, after ultrasonic machine ultrasonic vibration 1h, graphene oxide dispersion is obtained.
Step 2 prepares graphene oxide-loaded mangano-manganic oxide and metal nano silver particles composite material: by 240mg
Manganese acetate be added in the obtained graphene oxide water solution of step 1, by ultrasonic machine ultrasonic vibration 30min, and normal
It is stirred 30min under temperature, obtains uniformly mixed solution a, then 80mg silver acetate is added into solution a, it is super by ultrasonic machine
30min is swung in acoustic shock, and constant temperature waters is carried out at one 60 DEG C and stirs 30min, obtains uniformly mixed solution b, the solution b that will be obtained
It is transferred in reaction kettle and carries out hydro-thermal process, hydrothermal conditions are 160 DEG C, 8 hours.
Step 3 prepares redox graphene load mangano-manganic oxide and metal nano silver particles composite material: will walk
Carried out in rapid two hydro-thermal reaction material take out, remove supernatant liquor, bottom precipitation is got in beaker, be added on a small quantity go from
Sub- water is added 320mgNaBH particle, be vigorously stirred 2 hours, mixed solution c is obtained, with deionized water and dehydrated alcohol pair
Mixed solution c carries out multiple eccentric cleaning (revolving speed 3000r), until mixed solution pH value is 7, is transferred into drying box
It carries out 60 DEG C of freeze-day with constant temperature 24 hours, obtains graphene-supported mangano-manganic oxide in the composite material of nano silver particles.
Embodiment 2
A kind of composite material of uniform load mangano-manganic oxide and nano silver particles on graphene, including reduction graphite
Alkene, mangano-manganic oxide, nano silver particles, mangano-manganic oxide and nano silver particles are uniformly adhered to graphene surface, nano silver
Particle account for composite material mass fraction be 44%, preparation method the following steps are included:
Step 1 is walked, graphene oxide water solution is prepared: the sheet graphene oxide of 40mg is distributed to the anhydrous of 80mL
In ethyl alcohol, after ultrasonic machine ultrasonic vibration 1h, graphene oxide dispersion is obtained.
Step 2 prepares graphene oxide-loaded mangano-manganic oxide and metal nano silver particles composite material: by 160mg
Manganese acetate be added in the obtained graphene oxide water solution of step 1, by ultrasonic machine ultrasonic vibration 30min, and normal
It is stirred 30min under temperature, obtains uniformly mixed solution a, then 160mg silver acetate is added into solution a, it is super by ultrasonic machine
30min is swung in acoustic shock, and constant temperature waters is carried out at one 60 DEG C and stirs 30min, obtains uniformly mixed solution b, the solution b that will be obtained
It is transferred in reaction kettle and carries out hydro-thermal process, hydrothermal conditions are 160 DEG C, 8 hours.
Step 3 prepares redox graphene load mangano-manganic oxide and metal nano silver particles composite material: will walk
Carried out in rapid two hydro-thermal reaction material take out, remove supernatant liquor, bottom precipitation is got in beaker, be added on a small quantity go from
Sub- water is added 320mgNaBH particle, be vigorously stirred 2 hours, mixed solution c is obtained, with deionized water and dehydrated alcohol pair
Mixed solution c carries out multiple eccentric cleaning (revolving speed 3000r), until mixed solution pH value is 7, is transferred into drying box
It carries out 60 DEG C of freeze-day with constant temperature 24 hours, obtains the composite material of graphene-supported mangano-manganic oxide and nano silver particles.
Embodiment 3
A kind of composite material of uniform load mangano-manganic oxide and nano silver particles on graphene, including reduction graphite
Alkene, mangano-manganic oxide, nano silver particles, mangano-manganic oxide and nano silver particles are uniformly adhered to graphene surface, nano silver
Particle account for composite material mass fraction be 66%, preparation method the following steps are included:
Step 1 prepares graphene oxide water solution: the sheet graphene oxide of 40mg is distributed to the anhydrous second of 80mL
In alcohol, after ultrasonic machine ultrasonic vibration 1h, graphene oxide dispersion is obtained.
Step 2 prepares graphene oxide-loaded mangano-manganic oxide and metal nano silver particles composite material: by 80mg's
Manganese acetate is added in the obtained graphene oxide water solution of step 1, by ultrasonic machine ultrasonic vibration 30min, and in room temperature
Under be stirred 30min, obtain uniformly mixed solution a, then into solution a be added 240mg silver acetate, pass through ultrasonic machine ultrasound
30min is shaken, constant temperature waters is carried out at 60 DEG C and stirs 30min, obtains uniformly mixed solution b, obtained solution b is turned
It moves on to and carries out hydro-thermal process in reaction kettle, hydrothermal conditions are 160 DEG C, 8 hours.
Step 3 prepares redox graphene load mangano-manganic oxide and metal nano silver particles composite material: will walk
Carried out in rapid two hydro-thermal reaction material take out, remove supernatant liquor, bottom precipitation is got in beaker, be added on a small quantity go from
Sub- water is added 320mgNaBH particle, be vigorously stirred 2 hours, mixed solution c is obtained, with deionized water and dehydrated alcohol pair
Mixed solution c carries out multiple eccentric cleaning (revolving speed 3000r), until mixed solution pH value is 7, is transferred into drying box
It carries out 60 DEG C of freeze-day with constant temperature 24 hours, obtains the composite material of graphene-supported mangano-manganic oxide and nano silver particles.
The composite wood of graphene-supported mangano-manganic oxide and nano silver particles is prepared using one step hydro thermal method by the present invention
Material, and the good reduced graphene composite material of electric conductivity is obtained by secondary reduction, wherein the effect of hydro-thermal process is main
Be under conditions of high temperature and pressure, manganese acetate and silver acetate can be made to be converted into mangano-manganic oxide and metal nano silver particles, and
And graphene oxide one's duty can also be restored；After carrying out secondary reduction to composite material by chemical method, available conduction
The dilute carrier of reduction graphite of good performance, and avoid the graphene agglomeration occurred when dilatometry reduction.Finally obtain
The graphene-supported mangano-manganic oxide and its catalytic performance of the composite material of nano silver particles obtained is excellent, good conductivity, conduct
The battery stable electrical properties of positive electrode.
Claims (7)
1. a kind of novel magnesium air cell catalyst layer material, which is characterized in that the novel magnesium air cell catalyst layer
Material includes graphene, mangano-manganic oxide and metal nano silver ion, and mangano-manganic oxide and metal nano silver particles are uniformly attached
On the surface of graphene, wherein the mass fraction that graphene accounts for magnesium air cell catalyst layer material is 10%-15%, and metal receives
The mass fraction that rice silver particles account for magnesium air cell catalyst layer material is 22%~66%, and rest part is mangano-manganic oxide.
2. a kind of preparation process of novel magnesium air cell catalyst layer material, which is characterized in that steps are as follows:
Step 1 prepares the ethanol solution of the graphene oxide of 0.04mol/L-0.1mol/L；
Step 2 prepares graphene oxide-loaded mangano-manganic oxide and metal nano silver particles composite material: manganese acetate is added
In the ethanol solution of the graphene oxide obtained to step 1, ultrasound and stirring are to obtaining uniformly mixed solution under room temperature
a；Silver acetate is added into solution a again, room temperature ultrasound and 50 DEG C of -70 DEG C of stirrings are to uniformly mixed solution b is obtained, by what is obtained
Solution b, which is transferred in reaction kettle, carries out 140 DEG C -160 DEG C of hydro-thermal process 7-9 hours；Graphene, mangano-manganic oxide and metal nano
The mass ratio of silver ion according to claim 1 restriction；
Step 3, prepare magnesium air cell catalyst layer material: to step 2 by hydro-thermal process obtain it is graphene oxide-loaded
NaBH aqueous solution is added in mangano-manganic oxide and metal nano silver particles composite material, controls the quality of NaBH and graphene oxide
Than being vigorously stirred, obtaining mixed solution c for 8:1；Successively mixed solution c is carried out with deionized water and dehydrated alcohol more
Secondary eccentric cleaning, until mixed solution pH value be 7,50 DEG C of -70 DEG C of dryings, obtain graphene-supported mangano-manganic oxide and nano silver
The composite material of particle, i.e. magnesium air cell catalyst layer material.
3. preparation process according to claim 2, which is characterized in that
In step 1, it is ultrasonically formed the ethanol solution of graphene oxide, ultrasonic power 250W, ultrasonic time 1h.
4. preparation process according to claim 2 or 3, which is characterized in that
In step 2, prepare solution a stirring when it is 30 minutes, ultrasonic power 250W a length of, when it is 10 minutes a length of；Prepare solution b
Constant temperature whipping temp be 60 DEG C, mixing time be 30 minutes, ultrasonic power 250W, when it is 30 minutes a length of；When hydro-thermal reaction
A length of 8 hours.
5. preparation process according to claim 2 or 3, which is characterized in that
In step 3, when stirring, is 2 hours, centrifuge speed 2500r-3000r a length of, and drying temperature is 60 in drying box
DEG C, it is 24 hours a length of when dry.
6. preparation process according to claim 4, which is characterized in that
In step 3, when stirring, is 2 hours, centrifuge speed 2500r-3000r a length of, and drying temperature is 60 in drying box
DEG C, it is 24 hours a length of when dry.
7. the catalyst material that graphene-supported mangano-manganic oxide and nanometer metallic silver corpuscle composite material are used for magnesium air battery.
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