CN110508314A - A kind of Co2N-Ni3N loads graphene oxide-carbon cloth and analyses its preparation method of oxygen material - Google Patents
A kind of Co2N-Ni3N loads graphene oxide-carbon cloth and analyses its preparation method of oxygen material Download PDFInfo
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- CN110508314A CN110508314A CN201910839931.3A CN201910839931A CN110508314A CN 110508314 A CN110508314 A CN 110508314A CN 201910839931 A CN201910839931 A CN 201910839931A CN 110508314 A CN110508314 A CN 110508314A
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 222
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 137
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 125
- 239000004744 fabric Substances 0.000 title claims abstract description 117
- 239000000463 material Substances 0.000 title claims abstract description 73
- 229910052760 oxygen Inorganic materials 0.000 title claims abstract description 59
- 239000001301 oxygen Substances 0.000 title claims abstract description 59
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 title claims abstract description 58
- 229910003218 Ni3N Inorganic materials 0.000 title claims abstract description 50
- 238000004458 analytical method Methods 0.000 title claims abstract description 50
- 238000002360 preparation method Methods 0.000 title claims abstract description 38
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 69
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 26
- 229910017052 cobalt Inorganic materials 0.000 claims abstract description 24
- 239000010941 cobalt Substances 0.000 claims abstract description 24
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims abstract description 24
- 235000011114 ammonium hydroxide Nutrition 0.000 claims abstract description 15
- 238000005516 engineering process Methods 0.000 claims abstract description 9
- 230000003647 oxidation Effects 0.000 claims abstract description 7
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 7
- -1 transition metal nitride Chemical class 0.000 claims abstract description 5
- 229910020630 Co Ni Inorganic materials 0.000 claims description 57
- 229910002440 Co–Ni Inorganic materials 0.000 claims description 57
- 238000006243 chemical reaction Methods 0.000 claims description 54
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 35
- 239000000835 fiber Substances 0.000 claims description 29
- 238000005406 washing Methods 0.000 claims description 28
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 28
- 150000001875 compounds Chemical class 0.000 claims description 27
- 239000006185 dispersion Substances 0.000 claims description 24
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 18
- 239000012298 atmosphere Substances 0.000 claims description 16
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 14
- 235000019441 ethanol Nutrition 0.000 claims description 14
- 239000000126 substance Substances 0.000 claims description 14
- 229960004756 ethanol Drugs 0.000 claims description 13
- 239000012153 distilled water Substances 0.000 claims description 12
- 229910052757 nitrogen Inorganic materials 0.000 claims description 9
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 8
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 8
- 238000004090 dissolution Methods 0.000 claims description 8
- 238000001704 evaporation Methods 0.000 claims description 8
- 230000008020 evaporation Effects 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 8
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 8
- 239000012535 impurity Substances 0.000 claims description 8
- 229910017604 nitric acid Inorganic materials 0.000 claims description 8
- 239000007787 solid Substances 0.000 claims description 8
- 239000008247 solid mixture Substances 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 8
- 208000011580 syndromic disease Diseases 0.000 claims description 8
- GFHNAMRJFCEERV-UHFFFAOYSA-L cobalt chloride hexahydrate Chemical compound O.O.O.O.O.O.[Cl-].[Cl-].[Co+2] GFHNAMRJFCEERV-UHFFFAOYSA-L 0.000 claims description 7
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical class Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 claims description 7
- 229910002651 NO3 Inorganic materials 0.000 claims description 6
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 claims description 6
- 239000000428 dust Substances 0.000 claims description 6
- 229910021580 Cobalt(II) chloride Inorganic materials 0.000 claims description 5
- MEYVLGVRTYSQHI-UHFFFAOYSA-L cobalt(2+) sulfate heptahydrate Chemical compound O.O.O.O.O.O.O.[Co+2].[O-]S([O-])(=O)=O MEYVLGVRTYSQHI-UHFFFAOYSA-L 0.000 claims description 5
- AOPCKOPZYFFEDA-UHFFFAOYSA-N nickel(2+);dinitrate;hexahydrate Chemical compound O.O.O.O.O.O.[Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O AOPCKOPZYFFEDA-UHFFFAOYSA-N 0.000 claims description 5
- OQUOOEBLAKQCOP-UHFFFAOYSA-N nitric acid;hexahydrate Chemical compound O.O.O.O.O.O.O[N+]([O-])=O OQUOOEBLAKQCOP-UHFFFAOYSA-N 0.000 claims description 5
- 229920000049 Carbon (fiber) Polymers 0.000 claims description 4
- 239000004917 carbon fiber Substances 0.000 claims description 4
- 230000036571 hydration Effects 0.000 claims description 4
- 238000006703 hydration reaction Methods 0.000 claims description 4
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims description 3
- KTVIXTQDYHMGHF-UHFFFAOYSA-L cobalt(2+) sulfate Chemical compound [Co+2].[O-]S([O-])(=O)=O KTVIXTQDYHMGHF-UHFFFAOYSA-L 0.000 claims description 3
- 229940000406 drug candidate Drugs 0.000 claims description 3
- 239000003777 experimental drug Substances 0.000 claims description 3
- LAIZPRYFQUWUBN-UHFFFAOYSA-L nickel chloride hexahydrate Chemical compound O.O.O.O.O.O.[Cl-].[Cl-].[Ni+2] LAIZPRYFQUWUBN-UHFFFAOYSA-L 0.000 claims description 3
- 229910052698 phosphorus Inorganic materials 0.000 claims description 3
- 239000011574 phosphorus Substances 0.000 claims description 3
- 229910002804 graphite Inorganic materials 0.000 claims description 2
- 239000010439 graphite Substances 0.000 claims description 2
- GVPFVAHMJGGAJG-UHFFFAOYSA-L cobalt dichloride Chemical compound [Cl-].[Cl-].[Co+2] GVPFVAHMJGGAJG-UHFFFAOYSA-L 0.000 claims 1
- 239000007789 gas Substances 0.000 claims 1
- 238000010025 steaming Methods 0.000 claims 1
- 239000003054 catalyst Substances 0.000 abstract description 17
- 238000005868 electrolysis reaction Methods 0.000 abstract description 9
- 239000007772 electrode material Substances 0.000 abstract description 7
- 230000003197 catalytic effect Effects 0.000 abstract description 6
- 230000000694 effects Effects 0.000 abstract description 6
- 229920005596 polymer binder Polymers 0.000 abstract description 6
- 239000002491 polymer binding agent Substances 0.000 abstract description 6
- 150000004767 nitrides Chemical class 0.000 abstract description 5
- 229910052723 transition metal Inorganic materials 0.000 abstract description 4
- 238000006555 catalytic reaction Methods 0.000 abstract description 3
- 238000002207 thermal evaporation Methods 0.000 abstract description 3
- 239000002994 raw material Substances 0.000 abstract 1
- 238000000034 method Methods 0.000 description 8
- 239000000853 adhesive Substances 0.000 description 7
- 230000001070 adhesive effect Effects 0.000 description 7
- 239000006227 byproduct Substances 0.000 description 7
- 229920000642 polymer Polymers 0.000 description 7
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 6
- 239000003792 electrolyte Substances 0.000 description 6
- 229910052739 hydrogen Inorganic materials 0.000 description 6
- 239000001257 hydrogen Substances 0.000 description 6
- 238000004821 distillation Methods 0.000 description 5
- 230000036647 reaction Effects 0.000 description 4
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- UFMZWBIQTDUYBN-UHFFFAOYSA-N cobalt dinitrate Chemical compound [Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O UFMZWBIQTDUYBN-UHFFFAOYSA-N 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 238000002604 ultrasonography Methods 0.000 description 2
- KJTLSVCANCCWHF-UHFFFAOYSA-N Ruthenium Chemical compound [Ru] KJTLSVCANCCWHF-UHFFFAOYSA-N 0.000 description 1
- 150000001336 alkenes Chemical class 0.000 description 1
- 239000010405 anode material Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 229910001981 cobalt nitrate Inorganic materials 0.000 description 1
- BGORGFZEVHFAQU-UHFFFAOYSA-L cobalt(2+);sulfate;hydrate Chemical compound O.[Co+2].[O-]S([O-])(=O)=O BGORGFZEVHFAQU-UHFFFAOYSA-L 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000002848 electrochemical method Methods 0.000 description 1
- 230000005518 electrochemistry Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
- 238000011069 regeneration method Methods 0.000 description 1
- 229910052707 ruthenium Inorganic materials 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 229910000314 transition metal oxide Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/24—Nitrogen compounds
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/33—Electric or magnetic properties
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/50—Catalysts, in general, characterised by their form or physical properties characterised by their shape or configuration
- B01J35/58—Fabrics or filaments
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B1/00—Electrolytic production of inorganic compounds or non-metals
- C25B1/01—Products
- C25B1/02—Hydrogen or oxygen
- C25B1/04—Hydrogen or oxygen by electrolysis of water
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B11/00—Electrodes; Manufacture thereof not otherwise provided for
- C25B11/04—Electrodes; Manufacture thereof not otherwise provided for characterised by the material
- C25B11/051—Electrodes formed of electrocatalysts on a substrate or carrier
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B11/00—Electrodes; Manufacture thereof not otherwise provided for
- C25B11/04—Electrodes; Manufacture thereof not otherwise provided for characterised by the material
- C25B11/051—Electrodes formed of electrocatalysts on a substrate or carrier
- C25B11/073—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material
- C25B11/091—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material consisting of at least one catalytic element and at least one catalytic compound; consisting of two or more catalytic elements or catalytic compounds
-
- 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
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Electrochemistry (AREA)
- Metallurgy (AREA)
- Inorganic Chemistry (AREA)
- Catalysts (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
The present invention relates to nitride electrodes to analyse oxygen field of material technology, and discloses a kind of Co2N‑Ni3N loads graphene oxide-carbon cloth and analyses its preparation method of oxygen material, including formula as below raw material: cobalt source, nickel source, graphene oxide, carbon cloth, hexa, concentrated ammonia liquor.A kind of Co2N‑Ni3N loads graphene oxide-carbon cloth and analyses its preparation method of oxygen material, by using nitride Co2N and Ni3The main component of N catalyst, electrolysis strength are above traditional transition metal nitride, and the huge surface porosity factor of graphene oxide, and simultaneous oxidation graphene has amphipathic, make Co2N‑Ni3N uniform load improves electro catalytic activity and is electrolysed the efficiency of elutriation oxygen, make Co by ultrasonic disperse and hydro-thermal evaporation to electrode material effect electrochemical catalysis area between the surface and stratiform of graphene oxide, is increased2N‑Ni3N load graphene oxide is uniformly attached to the surface of carbon cloth, and not needing polymer binder makes catalyst is viscous to bond on electrode.
Description
Technical field
The present invention relates to nitride electrode analysis oxygen field of material technology, specially a kind of Co2N-Ni3N loads graphene oxide-
Carbon cloth analyses its preparation method of oxygen material.
Background technique
With becoming increasingly conspicuous for energy crisis and problem of environmental pollution, solar energy, wind energy, underground heat are continually developed in countries in the world
The various novel green renewable energy such as energy, Hydrogen Energy, Hydrogen Energy have many advantages, such as that environmentally protective, sustainable regeneration, energy density are high,
The extensive concern of people is received, water electrolysis hydrogen production is one of the effective technology for developing Hydrogen Energy, has technical level mature, automatic
The advantages that change degree is high, environment friendly and pollution-free, electrolysis water is made of two half-reactions, i.e. oxygen evolution reaction and evolving hydrogen reaction, they are logical
Need two kinds of catalyst often to reduce and generate H2And O2Required overpotential, therefore catalyst is water electrolysis hydrogen production process
One of the factor of middle most critical, wherein oxygen evolution reaction is related to the complex reactions such as proton couple electronic transfer, to limit electrolysis
The process of water.
The catalyst that current oxygen evolution reaction uses is mostly the noble metals such as platinum, ruthenium, but its reserves is rare, price is high
Expensive, preparation difficulty, and the oxides such as transition metal oxide class catalyst such as nickel, cobalt, iron, need to be consolidated with polymer binder
Determine onto electrically-conductive backing plate to carry out electrochemical measurement, and the use of high molecular polymer adhesive will increase the series connection resistance of cell reaction
It is anti-, the active site of catalyst has been wrapped, catalytic activity is caused to reduce, oxygen evolution reaction can not be effectively reduced and generate O2Required
Overpotential, and high molecular polymer adhesive can be decomposed gradually in electrolytic process, cause catalyst that can not be fixed to conduction
Substrate and be lost in electrolyte, reduce analysis Oxygen Electrode Material practicability and durability.
Summary of the invention
(1) the technical issues of solving
In view of the deficiencies of the prior art, the present invention provides a kind of Co2N-Ni3N loads graphene oxide-carbon cloth analysis
Its preparation method of oxygen material, is attached to transition metal nitride on anode material without polymer binder, both solves macromolecule
The use of polymer binder can wrap the active site of catalyst, increase the series impedance of cell reaction, cause to urge
Change the problem of activity reduces, while solving high molecular polymer adhesive again can gradually decompose in electrolytic process, causes to urge
Agent can not be fixed to electrically-conductive backing plate and the problems in be lost to electrolyte.
(2) technical solution
To achieve the above object, the invention provides the following technical scheme: a kind of Co2N-Ni3N loads graphene oxide-carbon fiber
Wei Bu analyses its preparation method of oxygen material, the formula material including following parts by weight proportion: 10-12 parts of cobalt sources, 12-14 parts of nickel sources, 8-
12 parts of graphene oxides, 20-35 parts of carbon cloths, 15-17 parts of hexas, 20-25 parts of concentrated ammonia liquors, preparation method include and
Following experimental drug: dust technology, ethyl alcohol, distilled water, dilute hydrochloric acid.
Preferably, the cobalt source is any one of cobalt chloride hexahydrate, Cobalt monosulfate heptahydrate or cabaltous nitrate hexahydrate,
Middle cobalt chloride hexahydrate CoCl2·6H2CoCl in O2Mass fraction is 51.5-52.6%, Cobalt monosulfate heptahydrate CoSO4·7H2In O
CoSO4Mass fraction is 50.8-52.4%, cabaltous nitrate hexahydrate Co (NO3)2·6H2Co (NO in O3)2Mass fraction is 60.1-
61.3%, preferably cobalt chloride hexahydrate CoCl2·6H2O。
Preferably, the nickel source is six hydration Nickel Chlorides or Nickelous nitrate hexahydrate, Nickel dichloride hexahydrate NiCl2·6H2O
Middle NiCl2Mass fraction is 51.8-53.1%, Nickelous nitrate hexahydrate Ni (NO3)2·6H2Ni (NO in O3)2Mass fraction is
58.2-60.5%, preferably NiCl2·6H2O。
Preferably, the graphene oxide specification is 1-3 layers, diameter 0.5-2.5um, with a thickness of 0.5-1.5nm.
Preferably, the carbon cloth is graphitized carbon fibre cloth, phosphorus content >=95%.
Preferably, the hexa chemical formula is C6H12N4, mass fraction >=93.5.
Preferably, HNO in the dust technology3Mass fraction is 5-8%.
Preferably, ethyl alcohol mass fraction >=99.5%.
Preferably, the mass fraction of the concentrated ammonia liquor is 23.2-27.6%.
Preferably, the dilute hydrochloric acid substance withdrawl syndrome is 2.3-3.1mol/L, mass fraction 8-11%.
Preferably, the Co2N-Ni3N loads graphene oxide-carbon cloth and analyses oxygen material, and preparation method includes following step
It is rapid:
(1) preparation Co-Ni compound loads graphene oxide dispersion: 400mL distilled water being added into 1000mL beaker
With 250mL ethyl alcohol, 10-12 parts of cobalt sources, 12-14 parts of nickel sources and 15-17 parts of hexas, after dissolution is sufficiently stirred, then plus
Enter 8-12 parts of graphene oxides to stir evenly, material in beaker is transferred into high-pressure hydrothermal reaction kettle, heated at constant temperature is placed in
It is heated to 130-135 DEG C of reaction 7-10h in case, so that cobalt source and nickel source is uniformly attached to the surface of graphene oxide, reaction terminates
Reaction kettle is cooled to room temperature afterwards, obtains Co-Ni compound load graphene oxide dispersion.
(2) it prepares the graphene oxide-loaded carbon cloth of Co-Ni: graphitized carbon fibre is arranged in 200mL mass fraction
Impurity is removed for washing in 5-8% solution, dilute nitric acid solution is filtered, successively uses 500-800mL dehydrated alcohol and 3000-
4000mL distills water washing carbon cloth, and carbon cloth is placed in baking oven and is heated to 90-95 DEG C, dry moisture 5-8h, on
It states the load of Co-Ni compound made from step (1) graphene oxide dispersion to be put into 1000mL beaker, then adds into beaker
Enter 20-35 parts of processed graphitized carbon fibre cloth, then place the beaker in ultrasonic dispersers, is heated to 60-65 DEG C, ultrasound
Power is 800W, supersonic frequency 25KHz, is ultrasonically treated 12-18h, keeps Co-Ni graphene oxide and carbon cloth fully dispersed
Uniformly, it then places the beaker and is heated to 80-85 DEG C in baking oven, slow evaporation solution, dry 8-12h makes Co-Ni graphene oxide
It is uniformly attached to the surface of graphitized carbon fibre cloth, obtains the graphene oxide-loaded carbon cloth of Co-Ni.
(3) Co is prepared2N-Ni3N loads graphene oxide-carbon cloth and analyses oxygen material: by Co- made from above-mentioned steps (2)
The graphene oxide-loaded carbon cloth of Ni and 20-25 parts of concentrated ammonia liquors are sequentially placed into crucible and are placed in nitrogen protection furnace, then by case
Formula atmosphere furnace is passed through N2It is completely exhausted out air, is then 5 DEG C/min by box atmosphere furnace heating rate, rises to 380-400 DEG C instead
3-4h is answered, is after reaction cooled to room temperature material, and the solid mixture in crucible is passed sequentially through into 200-400mL substance
Amount concentration be 2.3-3.1mol/L dilute hydrochloric acid and 4000-5000mL distill water washing and remove the complete material of unreacted and anti-
By-product is answered, and the solids of washes clean is placed in baking oven and is heated to 80-85 DEG C of dry 6-9h, obtains Co2N-Ni3N load
Graphene oxide-carbon cloth analyses oxygen material.
(3) beneficial technical effect
Compared with prior art, the present invention has following beneficial technical effect:
1, a kind of Co2N-Ni3N loads graphene oxide-carbon cloth and analyses its preparation method of oxygen material, by using nitride
Co2N and Ni3The main component of N catalyst, in electrolytic process, the more a height of 5mA/cm of current density2When, Co2N-Ni3N compound
Very low overpotential, only 276-282mV are only needed, electrolysis output voltage is 363-368mV, is above traditional transition metal nitrogen
The electrolysis strength of compound, and the huge surface porosity factor of graphene oxide, simultaneous oxidation graphene have it is amphipathic, make
Co2N-Ni3N uniform load increases Co between the surface and stratiform of graphene oxide2N-Ni3The contact surface of N and electrolyte
Product, to increase electrode material effect electrochemical catalysis area, improve electro catalytic activity and be electrolysed the efficiency of elutriation oxygen.
2, a kind of Co2N-Ni3N loads graphene oxide-carbon cloth and analyses its preparation method of oxygen material, is graphitized by being added
Carbon cloth makes Co as electrode, by ultrasonic disperse and hydro-thermal evaporation2N-Ni3N load graphene oxide is uniformly attached to carbon
The surface of fiber cloth, not needing polymer binder makes catalyst is viscous to bond on electrode, solves most of analysis oxygen electrode at present
Material needs to have wrapped the active site of catalyst using high molecular polymer adhesive, increases the series connection of cell reaction
Impedance, the problem of causing catalytic activity to reduce, while solving high molecular polymer adhesive again can be gradually in electrolytic process
The problems in it decomposes, cause catalyst that can not be fixed to electrically-conductive backing plate and be lost to electrolyte, improve analysis Oxygen Electrode Material
Practicability and durability.
Specific embodiment
To achieve the above object, the invention provides the following technical scheme: a kind of Co2N-Ni3N loads graphene oxide-carbon fiber
Wei Bu analyses its preparation method of oxygen material, the formula material including following parts by weight proportion: 10-12 parts of cobalt sources, 12-14 parts of nickel sources, 8-
12 parts of graphene oxides, 20-35 parts of carbon cloths, 15-17 parts of hexas, 20-25 parts of concentrated ammonia liquors, preparation method include and
Following experimental drug: dust technology, ethyl alcohol, distilled water, dilute hydrochloric acid, cobalt source are cobalt chloride hexahydrate, Cobalt monosulfate heptahydrate or six water
Any one of cobalt nitrate is closed, wherein cobalt chloride hexahydrate CoCl2·6H2CoCl in O2Mass fraction is 51.5-52.6%, seven
Cobalt sulfate hydrate CoSO4·7H2CoSO in O4Mass fraction is 50.8-52.4%, cabaltous nitrate hexahydrate Co (NO3)2·6H2In O
Co(NO3)2Mass fraction is 60.1-61.3%, preferably cobalt chloride hexahydrate CoCl2·6H2O, nickel source are six hydration dichlorides
Nickel or Nickelous nitrate hexahydrate, Nickel dichloride hexahydrate NiCl2·6H2NiCl in O2Mass fraction is 51.8-53.1%, six hydration nitre
Sour nickel (NO3)2·6H2Ni (NO in O3)2Mass fraction is 58.2-60.5%, preferably NiCl2·6H2O, graphene oxide
Specification is 1-3 layer, diameter 0.5-2.5um, and with a thickness of 0.5-1.5nm, carbon cloth is graphitized carbon fibre cloth, phosphorus content >=
95%, hexa chemical formula is C6H12N4, mass fraction >=93.5, HNO in dust technology3Mass fraction is 5-8%, second
Alcohol mass fraction >=99.5%, the mass fraction of concentrated ammonia liquor are 23.2-27.6%, and dilute hydrochloric acid substance withdrawl syndrome is 2.3-
3.1mol/L, mass fraction 8-11%, Co2N-Ni3N loads graphene oxide-carbon cloth and analyses oxygen material, preparation method packet
Include following steps:
(1) preparation Co-Ni compound loads graphene oxide dispersion: 400mL distilled water being added into 1000mL beaker
With 250mL ethyl alcohol, 10-12 parts of cobalt sources, 12-14 parts of nickel sources and 15-17 parts of hexas, after dissolution is sufficiently stirred, then plus
Enter 8-12 parts of graphene oxides to stir evenly, material in beaker is transferred into high-pressure hydrothermal reaction kettle, heated at constant temperature is placed in
It is heated to 130-135 DEG C of reaction 7-10h in case, so that cobalt source and nickel source is uniformly attached to the surface of graphene oxide, reaction terminates
Reaction kettle is cooled to room temperature afterwards, obtains Co-Ni compound load graphene oxide dispersion.
(2) it prepares the graphene oxide-loaded carbon cloth of Co-Ni: graphitized carbon fibre is arranged in 200mL mass fraction
Impurity is removed for washing in 5-8% solution, dilute nitric acid solution is filtered, successively uses 500-800mL dehydrated alcohol and 3000-
4000mL distills water washing carbon cloth, and carbon cloth is placed in baking oven and is heated to 90-95 DEG C, dry moisture 5-8h, on
It states the load of Co-Ni compound made from step (1) graphene oxide dispersion to be put into 1000mL beaker, then adds into beaker
Enter 20-35 parts of processed graphitized carbon fibre cloth, then place the beaker in ultrasonic dispersers, is heated to 60-65 DEG C, ultrasound
Power is 800W, supersonic frequency 25KHz, is ultrasonically treated 12-18h, keeps Co-Ni graphene oxide and carbon cloth fully dispersed
Uniformly, it then places the beaker and is heated to 80-85 DEG C in baking oven, slow evaporation solution, dry 8-12h makes Co-Ni graphene oxide
It is uniformly attached to the surface of graphitized carbon fibre cloth, obtains the graphene oxide-loaded carbon cloth of Co-Ni.
(3) Co is prepared2N-Ni3N loads graphene oxide-carbon cloth and analyses oxygen material: by Co- made from above-mentioned steps (2)
The graphene oxide-loaded carbon cloth of Ni and 20-25 parts of concentrated ammonia liquors are sequentially placed into crucible and are placed in nitrogen protection furnace, then by case
Formula atmosphere furnace is passed through N2It is completely exhausted out air, is then 5 DEG C/min by box atmosphere furnace heating rate, rises to 380-400 DEG C instead
3-4h is answered, is after reaction cooled to room temperature material, and the solid mixture in crucible is passed sequentially through into 200-400mL substance
Amount concentration be 2.3-3.1mol/L dilute hydrochloric acid and 4000-5000mL distill water washing and remove the complete material of unreacted and anti-
By-product is answered, and the solids of washes clean is placed in baking oven and is heated to 80-85 DEG C of dry 6-9h, obtains Co2N-Ni3N load
Graphene oxide-carbon cloth analyses oxygen material.
Embodiment 1:
(1) preparation Co-Ni compound loads graphene oxide dispersion: 400mL distilled water being added into 1000mL beaker
With 250mL ethyl alcohol, 10 parts of cobalt sources, 12 parts of nickel sources and 15 parts of hexas after dissolution is sufficiently stirred, add 8 parts of oxidations
Graphene stirs evenly, and material in beaker is transferred into high-pressure hydrothermal reaction kettle, is placed in heated at constant temperature case and is heated to 130
DEG C reaction 7h, so that cobalt source and nickel source is uniformly attached to the surface of graphene oxide, be after reaction cooled to room temperature reaction kettle,
Obtain Co-Ni compound load graphene oxide dispersion component 1.
(2) it prepares the graphene oxide-loaded carbon cloth of Co-Ni: graphitized carbon fibre is arranged in 200mL mass fraction
Impurity is removed for washing in 5% solution, filters dilute nitric acid solution, successively using 500mL dehydrated alcohol and 3000mL distillation washing
Carbon cloth is washed, and carbon cloth is placed in baking oven and is heated to 90 DEG C, dry moisture 5h, Co-Ni made from above-mentioned steps (1)
Compound load graphene oxide dispersion component 1 is put into 1000mL beaker, then 35 parts of addition is processed into beaker
Graphitized carbon fibre cloth, then places the beaker in ultrasonic dispersers, is heated to 60 DEG C, ultrasonic power 800W, supersonic frequency
For 25KHz, it is ultrasonically treated 12h, keeps Co-Ni graphene oxide and carbon cloth fully dispersed uniformly, then place the beaker baking oven
In be heated to 80 DEG C, slow evaporation solution, dry 8h makes Co-Ni graphene oxide uniformly be attached to the table of graphitized carbon fibre cloth
Face obtains the graphene oxide-loaded carbon cloth component 1 of Co-Ni.
(3) Co is prepared2N-Ni3N loads graphene oxide-carbon cloth and analyses oxygen material: by Co- made from above-mentioned steps (2)
The graphene oxide-loaded carbon cloth component 1 and 20 part concentrated ammonia liquor of Ni, which is sequentially placed into crucible, to be placed in nitrogen protection furnace, then will
Box atmosphere furnace is passed through N2It is completely exhausted out air, is then 5 DEG C/min by box atmosphere furnace heating rate, rises to 380 DEG C of reactions
Material is cooled to room temperature by 3h after reaction, and the solid mixture in crucible is passed sequentially through 200mL substance withdrawl syndrome
The complete material of water washing removing unreacted and byproduct of reaction are distilled for the dilute hydrochloric acid and 4000mL of 2.3mol/L, and will washing
Clean solids, which is placed in baking oven, is heated to 80 DEG C of dry 6h, obtains Co2N-Ni3N loads graphene oxide-carbon cloth analysis
Oxygen material 1.
Embodiment 2:
(1) preparation Co-Ni compound loads graphene oxide dispersion: 400mL distilled water being added into 1000mL beaker
With 250mL ethyl alcohol, 10.5 parts of cobalt sources, 12.5 parts of nickel sources and 15 parts of hexas after dissolution is sufficiently stirred, add 9 parts
Graphene oxide stirs evenly, and material in beaker is transferred into high-pressure hydrothermal reaction kettle, is placed in heated at constant temperature case and heats
To 130 DEG C of reaction 8h, so that cobalt source and nickel source is uniformly attached to the surface of graphene oxide, be after reaction cooled to reaction kettle
Room temperature obtains Co-Ni compound load graphene oxide dispersion component 2.
(2) it prepares the graphene oxide-loaded carbon cloth of Co-Ni: graphitized carbon fibre is arranged in 200mL mass fraction
Impurity is removed for washing in 6% solution, filters dilute nitric acid solution, successively using 600mL dehydrated alcohol and 3000mL distillation washing
Carbon cloth is washed, and carbon cloth is placed in baking oven and is heated to 90 DEG C, dry moisture 6h, Co-Ni made from above-mentioned steps (1)
Compound load graphene oxide dispersion component 2 is put into 1000mL beaker, then 32 parts of addition is processed into beaker
Graphitized carbon fibre cloth, then places the beaker in ultrasonic dispersers, is heated to 60 DEG C, ultrasonic power 800W, supersonic frequency
For 25KHz, it is ultrasonically treated 14h, keeps Co-Ni graphene oxide and carbon cloth fully dispersed uniformly, then place the beaker baking oven
In be heated to 80 DEG C, slow evaporation solution, dry 9h makes Co-Ni graphene oxide uniformly be attached to the table of graphitized carbon fibre cloth
Face obtains the graphene oxide-loaded carbon cloth component 2 of Co-Ni.
(3) Co is prepared2N-Ni3N loads graphene oxide-carbon cloth and analyses oxygen material: by Co- made from above-mentioned steps (2)
The graphene oxide-loaded carbon cloth component 2 and 21 part concentrated ammonia liquor of Ni, which is sequentially placed into crucible, to be placed in nitrogen protection furnace, then will
Box atmosphere furnace is passed through N2It is completely exhausted out air, is then 5 DEG C/min by box atmosphere furnace heating rate, rises to 380 DEG C of reactions
Material is cooled to room temperature by 3h after reaction, and the solid mixture in crucible is passed sequentially through 300mL substance withdrawl syndrome
The complete material of water washing removing unreacted and byproduct of reaction are distilled for the dilute hydrochloric acid and 4000mL of 2.6mol/L, and will washing
Clean solids, which is placed in baking oven, is heated to 80 DEG C of dry 7h, obtains Co2N-Ni3N loads graphene oxide-carbon cloth analysis
Oxygen material 2.
Embodiment 3:
(1) preparation Co-Ni compound loads graphene oxide dispersion: 400mL distilled water being added into 1000mL beaker
With 250mL ethyl alcohol, 11 parts of cobalt sources, 13 parts of nickel sources and 16 parts of hexas after dissolution is sufficiently stirred, add 10 parts of oxidations
Graphene stirs evenly, and material in beaker is transferred into high-pressure hydrothermal reaction kettle, is placed in heated at constant temperature case and is heated to 130
DEG C reaction 8h, so that cobalt source and nickel source is uniformly attached to the surface of graphene oxide, be after reaction cooled to room temperature reaction kettle,
Obtain Co-Ni compound load graphene oxide dispersion component 3.
(2) it prepares the graphene oxide-loaded carbon cloth of Co-Ni: graphitized carbon fibre is arranged in 200mL mass fraction
Impurity is removed for washing in 6% solution, filters dilute nitric acid solution, successively using 600mL dehydrated alcohol and 3500mL distillation washing
Carbon cloth is washed, and carbon cloth is placed in baking oven and is heated to 95 DEG C, dry moisture 7h, Co-Ni made from above-mentioned steps (1)
Compound load graphene oxide dispersion component 3 is put into 1000mL beaker, then 28 parts of addition is processed into beaker
Graphitized carbon fibre cloth, then places the beaker in ultrasonic dispersers, is heated to 65 DEG C, ultrasonic power 800W, supersonic frequency
For 25KHz, it is ultrasonically treated 16h, keeps Co-Ni graphene oxide and carbon cloth fully dispersed uniformly, then place the beaker baking oven
In be heated to 80 DEG C, slow evaporation solution, dry 10h makes Co-Ni graphene oxide uniformly be attached to graphitized carbon fibre cloth
Surface obtains the graphene oxide-loaded carbon cloth component 3 of Co-Ni.
(3) Co is prepared2N-Ni3N loads graphene oxide-carbon cloth and analyses oxygen material: by Co- made from above-mentioned steps (2)
The graphene oxide-loaded carbon cloth component 3 and 22 part concentrated ammonia liquor of Ni, which is sequentially placed into crucible, to be placed in nitrogen protection furnace, then will
Box atmosphere furnace is passed through N2It is completely exhausted out air, is then 5 DEG C/min by box atmosphere furnace heating rate, rises to 400 DEG C of reactions
Material is cooled to room temperature by 4h after reaction, and the solid mixture in crucible is passed sequentially through 400mL substance withdrawl syndrome
The complete material of water washing removing unreacted and byproduct of reaction are distilled for the dilute hydrochloric acid and 5000mL of 2.9mol/L, and will washing
Clean solids, which is placed in baking oven, is heated to 80 DEG C of dry 9h, obtains Co2N-Ni3N loads graphene oxide-carbon cloth analysis
Oxygen material 3.
Embodiment 4:
(1) preparation Co-Ni compound loads graphene oxide dispersion: 400mL distilled water being added into 1000mL beaker
With 250mL ethyl alcohol, 11.5 parts of cobalt sources, 13.5 nickel sources and 16 parts of hexas after dissolution is sufficiently stirred, add 11 parts of oxygen
Graphite alkene stirs evenly, and material in beaker is transferred into high-pressure hydrothermal reaction kettle, is placed in heated at constant temperature case and is heated to
135 DEG C of reaction 9h, make cobalt source and nickel source uniformly be attached to the surface of graphene oxide, reaction kettle are cooled to room after reaction
Temperature obtains Co-Ni compound load graphene oxide dispersion component 4.
(2) it prepares the graphene oxide-loaded carbon cloth of Co-Ni: graphitized carbon fibre is arranged in 200mL mass fraction
Impurity is removed for washing in 8% solution, filters dilute nitric acid solution, successively using 800mL dehydrated alcohol and 4000mL distillation washing
Carbon cloth is washed, and carbon cloth is placed in baking oven and is heated to 95 DEG C, dry moisture 8h, Co-Ni made from above-mentioned steps (1)
Compound load graphene oxide dispersion component 4 is put into 1000mL beaker, then 24 parts of addition is processed into beaker
Graphitized carbon fibre cloth, then places the beaker in ultrasonic dispersers, is heated to 65 DEG C, ultrasonic power 800W, supersonic frequency
For 25KHz, it is ultrasonically treated 16h, keeps Co-Ni graphene oxide and carbon cloth fully dispersed uniformly, then place the beaker baking oven
In be heated to 85 DEG C, slow evaporation solution, dry 10h makes Co-Ni graphene oxide uniformly be attached to graphitized carbon fibre cloth
Surface obtains the graphene oxide-loaded carbon cloth component 4 of Co-Ni.
(3) Co is prepared2N-Ni3N loads graphene oxide-carbon cloth and analyses oxygen material: by Co- made from above-mentioned steps (2)
The graphene oxide-loaded carbon cloth component 4 and 24 part concentrated ammonia liquor of Ni, which is sequentially placed into crucible, to be placed in nitrogen protection furnace, then will
Box atmosphere furnace is passed through N2It is completely exhausted out air, is then 5 DEG C/min by box atmosphere furnace heating rate, rises to 400 DEG C of reactions
Material is cooled to room temperature by 4h after reaction, and the solid mixture in crucible is passed sequentially through 400mL substance withdrawl syndrome
The complete material of water washing removing unreacted and byproduct of reaction are distilled for the dilute hydrochloric acid and 5000mL of 2.9mol/L, and will washing
Clean solids, which is placed in baking oven, is heated to 85 DEG C of dry 9h, obtains Co2N-Ni3N loads graphene oxide-carbon cloth analysis
Oxygen material 4.
Embodiment 5:
(1) preparation Co-Ni compound loads graphene oxide dispersion: 400mL distilled water being added into 1000mL beaker
With 250mL ethyl alcohol, 12 parts of cobalt sources, 14 parts of nickel sources and 17 parts of hexas after dissolution is sufficiently stirred, add 12 parts of oxidations
Graphene stirs evenly, and material in beaker is transferred into high-pressure hydrothermal reaction kettle, is placed in heated at constant temperature case and is heated to 135
DEG C reaction 10h, so that cobalt source and nickel source is uniformly attached to the surface of graphene oxide, reaction kettle be cooled to room after reaction
Temperature obtains Co-Ni compound load graphene oxide dispersion component 1.
(2) it prepares the graphene oxide-loaded carbon cloth of Co-Ni: graphitized carbon fibre is arranged in 200mL mass fraction
Impurity is removed for washing in 8% solution, filters dilute nitric acid solution, successively using 800mL dehydrated alcohol and 4000mL distillation washing
Carbon cloth is washed, and carbon cloth is placed in baking oven and is heated to 95 DEG C, dry moisture 8h, Co-Ni made from above-mentioned steps (1)
Compound load graphene oxide dispersion component 5 is put into 1000mL beaker, then 20 parts of addition is processed into beaker
Graphitized carbon fibre cloth, then places the beaker in ultrasonic dispersers, is heated to 65 DEG C, ultrasonic power 800W, supersonic frequency
For 25KHz, it is ultrasonically treated 18h, keeps Co-Ni graphene oxide and carbon cloth fully dispersed uniformly, then place the beaker baking oven
In be heated to 85 DEG C, slow evaporation solution, dry 12h makes Co-Ni graphene oxide uniformly be attached to graphitized carbon fibre cloth
Surface obtains the graphene oxide-loaded carbon cloth component 5 of Co-Ni.
(3) Co is prepared2N-Ni3N loads graphene oxide-carbon cloth and analyses oxygen material: by Co- made from above-mentioned steps (2)
The graphene oxide-loaded carbon cloth component 5 and 25 part concentrated ammonia liquor of Ni, which is sequentially placed into crucible, to be placed in nitrogen protection furnace, then will
Box atmosphere furnace is passed through N2It is completely exhausted out air, is then 5 DEG C/min by box atmosphere furnace heating rate, rises to 400 DEG C of reactions
Material is cooled to room temperature by 4h after reaction, and the solid mixture in crucible is passed sequentially through 400mL substance withdrawl syndrome
The complete material of water washing removing unreacted and byproduct of reaction are distilled for the dilute hydrochloric acid and 5000mL of 3.1mol/L, and will washing
Clean solids, which is placed in baking oven, is heated to 85 DEG C of dry 9h, obtains Co2N-Ni3N loads graphene oxide-carbon cloth analysis
Oxygen material 5.
By the test of electrolytic catalysis analysis oxygen performance, electrochemical stability to embodiment 1-5, a kind of Co2N-Ni3N is negative
It carries graphene oxide-carbon cloth and analyses its preparation method of oxygen material, by using nitride Co2N and Ni3The main component of N catalyst,
In electrolytic process, the more a height of 5mA/cm of current density2When, Co2N-Ni3N compound only needs very low overpotential, only 276-
282mV, electrolysis output voltage are 363-368mV, are above the electrolysis strength of traditional transition metal nitride, and aoxidize stone
The black huge surface porosity factor of alkene, simultaneous oxidation graphene have it is amphipathic, make Co2N-Ni3N uniform load is to graphene oxide
Surface and stratiform between, increase Co2N-Ni3The contact area of N and electrolyte, to increase electrode material effect electrochemistry
It is catalyzed area, improve electro catalytic activity and is electrolysed the efficiency of elutriation oxygen.
A kind of Co2N-Ni3N loads graphene oxide-carbon cloth and analyses its preparation method of oxygen material, by the way that graphitized carbon is added
Fiber cloth makes Co as electrode, by ultrasonic disperse and hydro-thermal evaporation2N-Ni3N load graphene oxide is uniformly attached to carbon fiber
The surface for tieing up cloth, not needing polymer binder makes catalyst is viscous to bond on electrode, solves most of analysis oxygen electrode material at present
Material needs to have wrapped the active site of catalyst using high molecular polymer adhesive, increases the series connection resistance of cell reaction
It is anti-, the problem of causing catalytic activity to reduce, while solving high molecular polymer adhesive again and can gradually divide in electrolytic process
The problems in solution, cause catalyst that can not be fixed to electrically-conductive backing plate and be lost to electrolyte, improve the reality of analysis Oxygen Electrode Material
With property and durability.
Claims (11)
1. a kind of Co2N-Ni3N loads graphene oxide-carbon cloth and analyses its preparation method of oxygen material, including following parts by weight proportion
Formula material, it is characterised in that: 10-12 parts of cobalt sources, 12-14 parts of nickel sources, 8-12 parts of graphene oxides, 20-35 parts of carbon fibers
Cloth, 15-17 part hexa, 20-25 parts of concentrated ammonia liquors, preparation method include and following experimental drug: dust technology, ethyl alcohol, steaming
Distilled water, dilute hydrochloric acid.
2. a kind of Co according to claim 12N-Ni3N loads graphene oxide-carbon cloth and analyses its preparation method of oxygen material,
Be characterized in that: the cobalt source is any one of cobalt chloride hexahydrate, Cobalt monosulfate heptahydrate or cabaltous nitrate hexahydrate, wherein six water
Close cobalt chloride CoCl2·6H2CoCl in O2Mass fraction is 51.5-52.6%, Cobalt monosulfate heptahydrate CoSO4·7H2CoSO in O4
Mass fraction is 50.8-52.4%, cabaltous nitrate hexahydrate Co (NO3)2·6H2Co (NO in O3)2Mass fraction is 60.1-
61.3%.
3. a kind of Co according to claim 12N-Ni3N loads graphene oxide-carbon cloth and analyses its preparation method of oxygen material,
Be characterized in that: the nickel source is six hydration Nickel Chlorides or Nickelous nitrate hexahydrate, Nickel dichloride hexahydrate NiCl2·6H2NiCl in O2
Mass fraction is 51.8-53.1%, Nickelous nitrate hexahydrate Ni (NO3)2·6H2Ni (NO in O3)2Mass fraction is 58.2-
60.5%.
4. a kind of Co according to claim 12N-Ni3N loads graphene oxide-carbon cloth and analyses its preparation method of oxygen material,
Be characterized in that: the graphene oxide specification is 1-3 layers, diameter 0.5-2.5um, with a thickness of 0.5-1.5nm.
5. a kind of Co according to claim 12N-Ni3N loads graphene oxide-carbon cloth and analyses its preparation method of oxygen material,
Be characterized in that: the carbon cloth is graphitized carbon fibre cloth, phosphorus content >=95%.
6. a kind of Co according to claim 12N-Ni3N loads graphene oxide-carbon cloth and analyses its preparation method of oxygen material,
Be characterized in that: the hexa chemical formula is C6H12N4, mass fraction >=93.5.
7. a kind of Co according to claim 12N-Ni3N loads graphene oxide-carbon cloth and analyses its preparation method of oxygen material,
It is characterized in that: HNO in the dust technology3Mass fraction is 5-8%.
8. a kind of Co according to claim 12N-Ni3N loads graphene oxide-carbon cloth and analyses its preparation method of oxygen material,
It is characterized in that: ethyl alcohol mass fraction >=99.5%.
9. a kind of Co according to claim 12N-Ni3N loads graphene oxide-carbon cloth and analyses its preparation method of oxygen material,
Be characterized in that: the mass fraction of the concentrated ammonia liquor is 23.2-27.6%.
10. a kind of Co according to claim 12N-Ni3N loads graphene oxide-carbon cloth and analyses its preparation method of oxygen material,
It is characterized by: the dilute hydrochloric acid substance withdrawl syndrome is 2.3-3.1mol/L, mass fraction 8-11%.
11. a kind of Co according to claim 12N-Ni3N loads graphene oxide-carbon cloth and analyses its preparation method of oxygen material,
It is characterized by: the Co2N-Ni3N loads graphene oxide-carbon cloth and analyses oxygen material, preparation method the following steps are included:
(1) preparation Co-Ni compound load graphene oxide dispersion: into 1000mL beaker be added 400mL distilled water and
250mL ethyl alcohol, 10-12 parts of cobalt sources, 12-14 parts of nickel sources and 15-17 parts of hexas, after dissolution is sufficiently stirred, adds
8-12 parts of graphene oxides stir evenly, and material in beaker is transferred into high-pressure hydrothermal reaction kettle, are placed in heated at constant temperature case
In be heated to 130-135 DEG C of reaction 7-10h, so that cobalt source and nickel source is uniformly attached to the surface of graphene oxide, after reaction
Reaction kettle is cooled to room temperature, Co-Ni compound load graphene oxide dispersion is obtained.
(2) prepare the graphene oxide-loaded carbon cloth of Co-Ni: it is 5- that graphitized carbon fibre, which is arranged in 200mL mass fraction,
Washing removes impurity in 8% solution, filters dilute nitric acid solution, is successively steamed using 500-800mL dehydrated alcohol and 3000-4000mL
Distilled water washs carbon cloth, and carbon cloth is placed in baking oven and is heated to 90-95 DEG C, dry moisture 5-8h, above-mentioned steps (1)
Co-Ni compound load graphene oxide dispersion obtained is put into 1000mL beaker, then 20-35 parts are added into beaker
Processed graphitized carbon fibre cloth, then places the beaker in ultrasonic dispersers, is heated to 60-65 DEG C, and ultrasonic power is
800W, supersonic frequency 25KHz are ultrasonically treated 12-18h, keep Co-Ni graphene oxide and carbon cloth fully dispersed uniformly,
It places the beaker again and is heated to 80-85 DEG C in baking oven, slow evaporation solution, dry 8-12h keeps Co-Ni graphene oxide uniformly attached
On the surface of graphitized carbon fibre cloth, obtain the graphene oxide-loaded carbon cloth of Co-Ni.
(3) Co is prepared2N-Ni3N loads graphene oxide-carbon cloth and analyses oxygen material: by Co-Ni oxygen made from above-mentioned steps (2)
Graphite alkene load carbon cloth and 20-25 parts of concentrated ammonia liquors are sequentially placed into crucible and are placed in nitrogen protection furnace, then by box gas
Atmosphere furnace is passed through N2It is completely exhausted out air, is then 5 DEG C/min by box atmosphere furnace heating rate, rises to 380-400 DEG C of reaction 3-
Material is cooled to room temperature by 4h after reaction, and the solid mixture in crucible is passed sequentially through to the amount of 200-400mL substance
The dilute hydrochloric acid and 4000-5000mL that concentration is 2.3-3.1mol/L distill water washing and remove the complete material of unreacted and react secondary
Product, and the solids of washes clean is placed in baking oven and is heated to 80-85 DEG C of dry 6-9h, obtain Co2N-Ni3N load oxidation
Graphene-carbon cloth analyses oxygen material.
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