CN108091890A - A kind of preparation method based on silver-cobalt-guanine nano lamellar material - Google Patents
A kind of preparation method based on silver-cobalt-guanine nano lamellar material Download PDFInfo
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- CN108091890A CN108091890A CN201711395196.9A CN201711395196A CN108091890A CN 108091890 A CN108091890 A CN 108091890A CN 201711395196 A CN201711395196 A CN 201711395196A CN 108091890 A CN108091890 A CN 108091890A
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- guanine
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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
- H01M4/9083—Catalytic material supported on carriers, e.g. powder carriers on carbon or graphite
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- H01M4/88—Processes of manufacture
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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
- H01M4/9041—Metals or alloys
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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Abstract
The present invention relates to a kind of preparation method based on silver-colored cobalt guanine nano lamellar material, including：Under the conditions of existing for potassium hydroxide, silver nitrate and cobalt nitrate mixed solution with guanine suspension are mixed, freezed, is freezed, carbonization, pickling filters, it is dry to get.Of the invention simple, reaction condition is mild, be prepared based on silver-colored cobalt guanine nano lamellar material, the nano lamellar material undoped with silver is better than to take-off potential, half wave potential and the stability in anodizing reduction catalysts in Proton Exchange Membrane Fuel Cells.
Description
Technical field
It is more particularly to a kind of fast based on silver-cobalt-bird the invention belongs to the preparation field of mixed with nano metal organic carbon material
The preparation method of purine nano lamellar material.
Background technology
Carbon-carried transition metal nano particle is a kind of interesting non noble metal oxygen reduction catalysts.Introduce different dimensions
Nano-carbon material come carrying transition metal nano particle preparation catalyst, than the non-noble metal nanoparticles of not carbon-containing carrier
With better redox reaction catalytic activity and stability.Carbon nanomaterial with high-ratio surface and rock-steady structure and
Strong synergistic effect between transition metal base nano particle is that such material has super good oxygen reduction catalytic activity and stabilization
The reason for property.
Cobalt nanometer particle and Nano silver grain are of interest by people always as catalyst, by the cobalt nanometer particle of synthesis and
It is a superior strategy that Nano silver grain, which is grown in carbon material surface design catalyst,.Document report carbon-carried transition metal at present
The synthetic method of nano particle is mostly then the nano-carbon material of pre-synthesis different dimensions mixes metal salt.Incorporation methods lack
Point is that grain size, property of nano-particle of incorporation etc. are to determine, substantially immutable.Carbon, which is formed, using one kettle way carries transition gold
Metal nano-particle material is very rare in document.The particle diameter distribution of nano-particle and the dosage of metal salt, temperature, mechanical ultrasonic etc. have
Certain relation, thus can be by changing solvent, metal ion the conditional regulatories nanoparticle such as amount or heating, ultrasound and illumination
Size, the performance of son.Therefore one pot process carbon-carried transition metal nano-particle material is a kind of very easily synthetic method.
Proton Exchange Membrane Fuel Cells (PEMFCs) is a kind of novel energy that chemical energy is converted into electric energy, but sun at present
Pole and cathod catalyst are required to use precious metals pt.Therefore, new inexpensive, efficient, stable base metal is developed
PEMFC electrode catalysts are significant.
From 1964, the N for there are Co metal centers was found for the first time4Macrocyclic compound has catalysis ORR activity.Hereafter, many tools
There is M-N4The macrocycle molecule compound of (M Co, Fe, Ni, Mn etc.) coordination becomes research hotspot.These materials include porphyrin, phthalein
Cyanines, adjacent nitrogen di (hetero) is luxuriant and rich with fragrance and substitutes some derivatives of functional group etc..The activity of these materials is considered and metal center electronics structure
Type is related.
The content of the invention
The technical problems to be solved by the invention are to provide a kind of preparation based on silver-cobalt-guanine nano lamellar material
Method, this method is simple, and reaction condition is mild, overcomes pre-synthesis in the synthetic method of carbon-carried transition metal nano particle
Then the nano-carbon material of different dimensions mixes metal salt so that grain size, property of the nano-particle of incorporation etc. were to determine, base
This immutable problem.
A kind of preparation method based on silver-cobalt-guanine nano lamellar material of the present invention, is as follows：
Under the conditions of existing for potassium hydroxide, silver nitrate and cobalt nitrate mixed solution are mixed with guanine suspension, it is cold
Freeze, freeze, obtain based on silver-cobalt-guanine nano lamellar material presoma, carbonization, pickling filters, dry, is based on
Silver-cobalt-guanine nano lamellar material, the wherein molar ratio of guanine and silver nitrate are 1:0.1~0.5, guanine and nitric acid
The molar ratio of cobalt is 1:0.5~0.9, the molar ratio of potassium hydroxide and guanine is 1:1~3.
The silver nitrate and cobalt nitrate mixed solution, the solvent of guanine suspension are water.
The freezing is to use liquid nitrogen；Freeze-drying time is 2~3 days, and freeze temperature is -40 DEG C~-50 DEG C.
The carbonization carries out in argon atmosphere；Carburizing temperature be 700~800 DEG C, heating rate for 4~6 DEG C/
Min, carbonization time are 2~3h.
The pickling is with the dilute hydrochloric acid that concentration is 5%；Pickling time is 8~12h.
It is described that electrode catalyst redox is applied to based on silver-cobalt-guanine nano lamellar material.
The electrode catalyst redox refers in the potassium hydroxide solution of 0.1mol/L compared with silver chloride reference electricity
Redox (ORR) catalytic performance of pole.
The smaller nano material of grain size in order to obtain of the invention, before being based on silver-cobalt-guanine nano lamellar material
Body is driven to be freeze-dried to constant weight.
The present invention is tentatively freezed with liquid nitrogen, is subsequently freezed with freeze dryer.
The present invention is mixture prepared based on silver-cobalt-guanine nano-sheet material by silver nitrate and cabaltous nitrate hexahydrate
Material, wherein Nano silver piece lamellar spacing narrow distribution and homoepitaxial are in cobalt carbon material surface, similar sheet petal.Since silver is received
Rice piece is grown in cobalt carbon material surface, improves the electric conductivity of material, and is existed based on silver-cobalt-guanine nano lamellar material
The material undoped with silver nano-grain is better than to the catalytic effect of anodizing reduction in Proton Exchange Membrane Fuel Cells.
Advantageous effect
Of the invention simple, reaction condition is mild, be prepared based on silver-cobalt-guanine nano lamellar material, in proton
Take-off potential, half wave potential and the stability in anodizing reduction catalysts are better than undoped with silver in exchange film fuel battery
Nano lamellar material.
Description of the drawings
Fig. 1 is the SEM figures based on silver-cobalt-guanine nano lamellar material in embodiment 1；
Fig. 2 is the SEM figures based on cobalt-guanine nano lamellar material in comparative example 1；
Fig. 3 is the XRD diagram based on silver-cobalt-guanine nano lamellar material in embodiment 1；
Fig. 4 is the XRD diagram based on cobalt-guanine nano lamellar material in comparative example 1；
Fig. 5 is to be based on receiving based on cobalt-guanine in silver-cobalt-guanine nano lamellar material and comparative example 1 in embodiment 1
The LSV under 800rpm, 1600rpm schemes rice flaky material respectively in ORR test performances；
Fig. 6 is to be based on receiving based on cobalt-guanine in silver-cobalt-guanine nano lamellar material and comparative example 1 in embodiment 1
CV figure of the rice flaky material in ORR test performances.
Specific embodiment
With reference to specific embodiment, the present invention is further explained.It is to be understood that these embodiments are merely to illustrate the present invention
Rather than it limits the scope of the invention.In addition, it should also be understood that, after reading the content taught by the present invention, people in the art
Member can make various changes or modifications the present invention, and such equivalent forms equally fall within the application the appended claims and limited
Scope.
Embodiment 1
(1) 0.01mol guanines are dissolved in the potassium hydroxide aqueous solution of the 1mol/L of 10mL and obtain guanine suspension,
0.001mol silver nitrates and 0.009mol cabaltous nitrate hexahydrates are dissolved in 10mL water and obtain silver nitrate and cobalt nitrate mixed solution,
1mL silver nitrates and cobalt nitrate mixed solution with 1mL guanine suspensions are mixed, rocks uniformly, with liquid nitrogen frozen, and is transferred to
It is freezed 2~3 days in freeze dryer, freeze temperature is -40 DEG C~-50 DEG C, is obtained based on before silver-cobalt-guanine nano lamellar material
Drive body, under the conditions of argon gas 800 DEG C heat preservation 2h, heating rate be 4~6 DEG C/min, finally with 5% dilute hydrochloric acid pickling 8-12h,
It filters, it is dry in 60-80 DEG C of vacuum drying oven, it obtains based on silver-cobalt-guanine nano lamellar material (Ag:Co-1:9).
(2) silver-cobalt-guanine nano lamellar material, 350 μ L ethyl alcohol and 95 μ L Nafion will be based in 5mg steps (1)
It adds in plastic tube, and ultrasonic disperse 20min obtains mixed liquor, pipettes the 2.8 μ L mixed liquors twice with liquid-transfering gun, uniformly applies
In rotating disk electrode (r.d.e) black region, connection occasion China electrochemical workstation test ORR performances.
Fig. 1 shows：Nano silver piece lamellar spacing narrow distribution, about 100~200nm and homoepitaxial are in cobalt carbon material table
Face, similar sheet petal.
Fig. 3 shows：Nano silver piece is nano silver/silver chloride, and cobalt element peak is also shown in the figure, illustrate the material be silver-cobalt-
Guanine nano material.
Comparative example 1
(1) 0.01mol guanines are dissolved in the 1mol/L potassium hydroxide aqueous solutions of 10mL and obtain guanine suspension, it will
0.01mol cabaltous nitrate hexahydrates, which are dissolved in 10mL water, obtains cobalt nitrate solution, and 1mL cobalt nitrate solutions and 1mL guanines is suspended
Liquid mixes, and rocks uniformly, with liquid nitrogen frozen, and is transferred in freeze dryer and freezes 2~3 days, and freeze temperature is -40 DEG C~-50 DEG C,
Obtain based on cobalt-guanine nano lamellar material presoma, 800 DEG C of heat preservation 2h under the conditions of argon gas, heating rate for 4-6 DEG C/
Min, finally with 5% dilute hydrochloric acid pickling 8-12h, filter, it is dry in 60-80 DEG C of vacuum drying oven, obtain receiving based on cobalt-guanine
Rice flaky material (Ag:Co-0:10).
(2) cobalt-guanine nano lamellar material, 350 μ L ethyl alcohol and 95 μ L Nafion in 5mg steps (1) are added in into plastics
Guan Zhong, and ultrasonic disperse 20min, obtain mixed liquor, pipette the 2.8 μ L mixed liquors twice with liquid-transfering gun, are evenly coated in rotational circle
Disc electrode black region, connection occasion China electrochemical workstation test ORR performances.
Fig. 2 shows：Carbon cobalt bead is uniformly distributed, and for size in 100~300nm, bead surface is because carbon compared with smooth part
Package.
Fig. 4 shows：The position at peak corresponds to cobalt element, it was demonstrated that the material is simple cobalt carbon bead, i.e., fast based on cobalt-bird
Purine nano lamellar material.
Fig. 5 and Fig. 6 show：In embodiment 1 based on silver-cobalt-guanine nano lamellar material in ORR tests, starting electricity
Position, half wave potential and CV cyclical stabilities, which are better than in this comparative example of no silver-doped, is based on cobalt-guanine nano-sheet
Material.
Claims (6)
1. a kind of preparation method based on silver-cobalt-guanine nano lamellar material, is as follows：
Under the conditions of existing for potassium hydroxide, silver nitrate and cobalt nitrate mixed solution with guanine suspension are mixed, freezed, is frozen
It is dry, it obtains based on silver-cobalt-guanine nano lamellar material presoma, carbonization, pickling filters, dry, obtain based on silver-cobalt-
The molar ratio of guanine nano lamellar material, wherein guanine and silver nitrate is 1:0.1~0.5, guanine and cobalt nitrate rub
You are than being 1:0.5~0.9, the molar ratio of potassium hydroxide and guanine is 1:1~3.
2. a kind of preparation method based on silver-cobalt-guanine nano lamellar material described in accordance with the claim 1, feature exist
In the silver nitrate and cobalt nitrate mixed solution, the solvent of guanine suspension are water.
3. a kind of preparation method based on silver-cobalt-guanine nano lamellar material described in accordance with the claim 1, feature exist
In the freezing is to use liquid nitrogen；Freeze-drying time is 2~3 days, and freeze temperature is -40 DEG C~-50 DEG C.
4. a kind of preparation method based on silver-cobalt-guanine nano lamellar material described in accordance with the claim 1, feature exist
In the carbonization carries out in argon atmosphere；Carburizing temperature be 700~800 DEG C, heating rate be 4~6 DEG C/min, carbon
The change time is 2~3h.
5. a kind of preparation method based on silver-cobalt-guanine nano lamellar material described in accordance with the claim 1, feature exist
In the pickling is with the dilute hydrochloric acid that concentration is 5%；Pickling time is 8~12h.
6. a kind of preparation method based on silver-cobalt-guanine nano lamellar material described in accordance with the claim 1, feature exist
In described to be applied to electrode catalyst redox based on silver-cobalt-guanine nano lamellar material.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109449409A (en) * | 2018-10-30 | 2019-03-08 | 郭和俊 | A kind of novel processing step of ternary material |
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