CN106602086A - Self-supporting oxygen reduction/oxygen evolution double-effect oxygen electrode catalyst and preparation method therefor - Google Patents
Self-supporting oxygen reduction/oxygen evolution double-effect oxygen electrode catalyst and preparation method therefor Download PDFInfo
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- CN106602086A CN106602086A CN201611037954.5A CN201611037954A CN106602086A CN 106602086 A CN106602086 A CN 106602086A CN 201611037954 A CN201611037954 A CN 201611037954A CN 106602086 A CN106602086 A CN 106602086A
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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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- 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
- Y02E60/50—Fuel cells
Abstract
The invention discloses a self-supporting oxygen reduction/oxygen evolution double-effect oxygen electrode catalyst and a preparation method therefor, and belongs to the fields of catalysis and materials. A certain amount of nitrogen source, sulfur source and transitional metal salt are dissolved in a water solution; and meanwhile, carbon paper is added to further synthesize a nitrogen, sulfur and transitional metal co-doped self-supporting oxygen reduction/oxygen evolution double-effect oxygen electrode through a hydrothermal reaction in one step. The method is simple and convenient to operate; the reaction is completed in one step; the adopted raw materials are common reagents used in laboratories, so that low manufacturing cost, short reaction period and high repeatability are realized; and the electrode represents high oxygen reduction and oxygen evolution double-effect property in electro-catalysis, is long in cycling life, and can be applied to many fields of a metal air cell, an integrated regenerative fuel cell, a zinc air flow cell and the like.
Description
Technical field
The invention belongs to be catalyzed and Material Field, and in particular to a kind of self-supporting hydrogen reduction/precipitation double-effect oxygen electrode catalysis
Agent and preparation method thereof, it is empty that the electrode catalyst can be widely applied to metal-air battery, integral regeneratable fuel cell, zinc
The numerous areas such as gas-liquid galvanic battery.
Background technology
The energy is the basis and power that the mankind advance.At present, 78% energy is from the fossil energy such as coal, oil and natural gas
Source.But these fossil energy reserves are limited and non-renewable.The exploitation reproducible utilization energy, improves it in energy resource consumption
Proportion is very urgent.However, solar energy, tide energy and wind energy equal energy source are unstable and uncontrollable, make to abandon wind and abandon
Optical phenomenon is serious.Energy storage device is the key technology for solving the unstable and uncontrollable problem of regenerative resource, is to improve energy profit
With the important means of rate.
In the energy storage technologies such as metal-air battery, zinc air redox flow battery, the reaction that positive pole hydrogen reduction and oxygen are separated out is moved
Mechanics is slow, and hydrogen reduction/precipitation dual purpose catalyst plays important role wherein on positive pole.Noble metal catalyst is at present
That what is known separates out catalyst with efficient hydrogen reduction or oxygen.Such as Pt, Au, Pd etc. are with excellent oxygen reduction catalytic activity, and RuO2,
Then there is IrO2 etc. excellent oxygen to separate out catalysis activity, but noble metal catalyst is difficult while possessing efficient hydrogen reduction and oxygen analysis
Go out economic benefits and social benefits catalysis activity.Relative low price, the metal oxide of reserves relative abundance also show efficient hydrogen reduction/analysis
Go out catalysis activity.But easily there is redox reaction in them, so as to cause lattice variations, swelling, less stable occur, and make
Its cannot as hydrogen reduction/precipitation dual purpose catalyst large-scale application.
Material with carbon element is cheap, abundance, easy control of structure, can be widely applied to electro-catalysis field.Wherein nitrogen and excessively
Metal-doped Graphene, CNT etc. mostly shows excellent oxygen reduction catalytic activity and stability.Sulphur and excessively gold
Graphene, CNT of category doping etc. also mostly show excellent oxygen and separate out catalysis activity.The many doping carbon-based materials of research
Hydrogen reduction and oxygen separate out avtive spot, the content of control accurate foreign atom, species and distribution, and build abundant hydrogen reduction
It is the key for preparing carbon-based hydrogen reduction/precipitation economic benefits and social benefits catalysis material to separate out avtive spot with oxygen.
The content of the invention
The present invention relates to based on carbon paper doping in one step nitrogen, sulphur, transition metal method, controllable doping nitrogen, sulphur
Content and distribution with transition metal atoms, while building the hydrogen reduction enriched and oxygen precipitation avtive spot.The carbon paper of making can
To be directly used as the electrode of hydrogen reduction and oxygen evolution reaction, show good hydrogen reduction and oxygen separates out catalysis activity, match in excellence or beauty
Commercial dual purpose catalyst.
For achieving the above object, the present invention is adopted the following technical scheme that：
(1) carbon paper is soaked in nitration mixture 1-12h, then deionized water is rinsed；
(2) a certain amount of nitrogen source (one kind in the organic matter such as thiocarbamide, urea, hexamethylenetetramine, thioacetamide is weighed
Or it is two or more), sulphur source (in the organic matter such as thiocarbamide, thioacetamide one or two), transition metal salt (molysite, nickel salt,
Cobalt salt one or more), the mol ratio of three is 1-5：1-5:1；In being dissolved in deionized water, it is uniformly mixing to obtain molten
Liquid；
(3) carbon paper after step (1) process is put in hydrothermal reaction kettle, pours above-mentioned steps (2) solution into toward in reactor,
Compactedness control terminates rear natural cooling in 50-80%, 120-200 DEG C of reaction 6-24h, reaction；
(4) carbon paper is taken out, with distillation water washing for several times, 6-24h is soaked with sulfuric acid, then deionized water cleaning；
(5) carbon paper is put in baking oven 60-100 DEG C and is dried 1-12h, obtain final product nitrogen, sulphur, the carbon paper of transition metal codope.
Carbon paper preferred thickness used by step (1) is 0.1-0.3mm, can be with hydrophilic, it is also possible to hydrophobic.
In step (1), nitration mixture used can be 1 with red fuming nitric acid (RFNA) and concentrated hydrochloric acid mixture, volume ratio:1-5, more preferably 1:
3；Can also be the mixture of red fuming nitric acid (RFNA) and the concentrated sulfuric acid, volume ratio is 1:1-5, more preferably 1:3, the mass concentration of concentrated hydrochloric acid
36%～38%, the weight/mass percentage composition of red fuming nitric acid (RFNA) is not less than 69%, the weight/mass percentage composition 98.3% of the concentrated sulfuric acid.
In step (2), the nitrogen source can come from the organic matters such as thiocarbamide, urea, hexamethylenetetramine, thioacetamide
One or more, sulphur source can come from one or more in the organic matters such as thiocarbamide, thioacetamide.Nitrogen source can and sulphur source
For same organic matter, such as thiocarbamide, thioacetamide, when nitrogen source and sulphur source are same organic matter, both consumptions are one；Nitrogen
Source and sulphur source may also be two kinds of organic matters.
In step (2), transition metal salt can be molysite (iron chloride, ferric sulfate, ferric nitrate etc.), or nickel salt
One or more in (nickel chloride, nickel sulfate, nickel acetate etc.) or cobalt salt (cobalt chloride, cobaltous sulfate, cobalt nitrate etc.).
In step (2), nitrogen source, sulphur source, the mol ratio of transition metal salt are 1-5：1-5:1, more preferably 3-5:3-5:1,
The total mol concentration of transition metal salt is preferably 0.01mol/L-0.1mol/L, preferred 0.05mol/L.
In step (3), reactor can be 50ml, 100ml, 200ml, and compactedness is controlled in 50-80%, more preferably
60%；Reaction temperature 120-200 DEG C, more preferably 180 DEG C；Reaction time 6-24h, more preferably 12h.
Advantages of the present invention
(1) present invention mixes nitrogen, sulphur and transition metal in carbon paper using simple one step hydro thermal method, mixes method letter
Single, easy to operate, mild condition, safety non-toxic can in high volume make.
(2) as a result the present invention shows that there is preferable hydrogen reduction and oxygen to separate out for it using carbon paper as analysis oxygen electro catalytic electrode
Performance and overpotential is relatively low.In 0.1mol/L KOH solutions, when it is 10mA/cm2 that it analyses oxygen current density, overpotential only has
0.4V, Tafel slope is 116mV/dec.In 0.1mol/L KOH solutions, its relative saturation calomel electrode starting point position for-
0.165V, half wave potential is -0.267V.
(3) this nitrogen, sulphur, transition metal codope carbon paper have excellent electric conductivity, good mechanical property, therefore can be with
Use as the self-supporting electrode of binding agent is not needed.
(4) there is excellent hydrogen reduction and oxygen to separate out performance for this nitrogen, sulphur, transition metal codope carbon paper, can substitute mesh
Front commercial noble metal ORR catalyst and OER catalyst.
(5) present invention can obtain granular substance by the way that carbon paper is soaked into 1-12h in nitration mixture in the outer surface of carbon paper fiber
Matter, Surface Creation nitrogen then again based on particulate material in carbon paper fiber, sulphur, transition metal codope film, from
And cause doping nitrogen, sulphur and transition metal atoms distribution controllable.
Description of the drawings
Fig. 1 is SEM (SEM) figure of original carbon paper in embodiment 1.
Fig. 2 is SEM (SEM) figure of carbon paper after chloroazotic acid process in embodiment 1.
Fig. 3 is gained nitrogen, sulphur, iron, SEM (SEM) figure of nickel co-doped carbon paper in embodiment 1.
Fig. 4 is that the analysis oxygen of gained nitrogen in embodiment 1, sulphur, iron, nickel co-doped carbon paper and original carbon paper and iridium dioxide is anti-
The polarization curve answered.
Fig. 5 is the hydrogen reduction of gained nitrogen in embodiment 1, sulphur, iron, nickel co-doped carbon paper and original carbon paper and 20%Pt/C
The polarization curve of reaction.
Fig. 6 is gained nitrogen, sulphur, iron, the polarization curve of the oxygen evolution reaction of the carbon paper of cobalt codope in embodiment 2.
Fig. 7 is gained nitrogen, sulphur, iron, the polarization curve of the oxygen reduction reaction of the carbon paper of cobalt codope in embodiment 2.
Fig. 8 is gained nitrogen, sulphur, the polarization curve of the oxygen evolution reaction of the carbon paper of iron codope in embodiment 3.
Fig. 9 is gained nitrogen, sulphur, the polarization curve of the oxygen reduction reaction of the carbon paper of iron codope in embodiment 3.
Specific embodiment
With reference to embodiment, the invention will be further described, but the present invention is not limited to following examples.
Embodiment 1
From on the thick hydrophilic carbon papers of 0.3mm, the long 12mm width 10mm fritter carbon papers (CP) of cutting one.Lower fritter carbon of room temperature
Paper is put in chloroazotic acid and soaks 6h, then takes out carbon paper and is cleaned with a large amount of distilled water.
Take 7.6g (100mmol) thiocarbamides and 0.25g ferric trichlorides and 0.284g tetra- hydration nickel acetate be dissolved in 60ml go from
In sub- water, solution is uniformly mixing to obtain.
Carbon paper after process is put in 100ml hydrothermal reaction kettles, above-mentioned solution is poured into toward in reactor, 200 DEG C in baking oven
Reaction 12h, reaction terminates rear natural cooling.
Carbon paper is taken out after cooling, is washed for several times with distilled water and ethanol, then 10h is soaked with 1mol/L sulfuric acid, then spent
Ionized water is cleaned.
Carbon paper is put in baking oven 60 DEG C and is dried 10h, obtain final product nitrogen, sulphur, iron, nickel co-doped carbon paper (Fe-Ni-NSCP).
Embodiment 2
From on the thick hydrophilic carbon papers of 0.3mm, the long 12mm width 10mm fritter carbon papers of cutting one.Lower fritter carbon paper of room temperature is put
Enter and soak in chloroazotic acid 6h, then take out carbon paper and cleaned with a large amount of distilled water.
Take 7.6g (100mmol) thiocarbamides and 0.25g ferric trichlorides and 0.194g cobalt chlorides be dissolved in 60ml deionized waters,
It is uniformly mixing to obtain solution.
Carbon paper after process is put in 100ml hydrothermal reaction kettles, above-mentioned solution is poured into toward in reactor, 180 DEG C in baking oven
Reaction 18h, reaction terminates rear natural cooling.
Carbon paper is taken out after cooling, is washed for several times with distilled water and ethanol, then with 2mol/L salt acid soaks 6h, then spend from
Sub- water cleaning.
Carbon paper is put in baking oven 120 DEG C and is dried 6h, obtain final product the carbon paper (Fe-Co-NSCP) of nitrogen, sulphur, iron, cobalt codope.
Embodiment 3
From on the thick hydrophilic carbon papers of 0.3mm, the long 12mm width 10mm fritter carbon papers of cutting one.Lower fritter carbon paper of room temperature is put
Enter the nitration mixture (concentrated sulfuric acid：Red fuming nitric acid (RFNA)=3:1) immersion 1h, then takes out carbon paper and is cleaned with a large amount of distilled water in.
Take 7.6g (100mmol) thiocarbamides and 0.5g ferric trichlorides are dissolved in 60ml deionized waters, be uniformly mixing to obtain molten
Liquid.
Carbon paper after process is put in 100ml hydrothermal reaction kettles, above-mentioned solution is poured into toward in reactor, 180 DEG C in baking oven
Reaction 18h, reaction terminates rear natural cooling.
Carbon paper is taken out after cooling, is washed for several times with distilled water and ethanol, then with 2mol/L sulfuric acid soak 6h, then spend from
Sub- water cleaning.
Carbon paper is put in baking oven 100 DEG C and is dried 6h, obtain final product the carbon paper (Fe-NSCP) of nitrogen, sulphur, iron codope.
Claims (10)
1. a kind of preparation method of self-supporting hydrogen reduction/precipitation double effect oxygen electrode catalyst, it is characterised in that including following step
Suddenly：
(1) carbon paper is soaked in nitration mixture 1-12h, then deionized water is rinsed；
(2) a certain amount of nitrogen source, sulphur source, transition metal salt are weighed, the mol ratio of three is 1-5：1-5:1；It is dissolved in deionized water
In, it is uniformly mixing to obtain solution；
(3) carbon paper is put in hydrothermal reaction kettle after step (1) is processed, and pours above-mentioned steps (2) solution, compactedness into toward in reactor
Control terminates rear natural cooling in 50-80%, 120-200 DEG C of reaction 6-24h, reaction；
(4) carbon paper is taken out, with distillation water washing for several times, 6-24h is soaked with sulfuric acid, then deionized water cleaning；
(5) carbon paper is put in baking oven 60-100 DEG C and is dried 1-12h, obtain nitrogen, sulphur, the carbon paper of transition metal codope, i.e., from
Support hydrogen reduction/precipitation double effect oxygen electrode catalyst.
2., according to a kind of preparation method of the self-supporting hydrogen reduction/precipitation double effect oxygen electrode catalyst described in claim 1, it is special
Levy and be, the carbon paper thickness used by step (1) is 0.1-0.3mm, with hydrophilic or with hydrophobic.
3., according to a kind of preparation method of the self-supporting hydrogen reduction/precipitation double effect oxygen electrode catalyst described in claim 1, it is special
Levy and be, in step (1), nitration mixture used is red fuming nitric acid (RFNA) and concentrated hydrochloric acid mixture, and volume ratio is 1:1-5, preferably 1:3；Or
The mixture of red fuming nitric acid (RFNA) and the concentrated sulfuric acid, volume ratio is 1:1-5, preferably 1:3.
4., according to a kind of preparation method of the self-supporting hydrogen reduction/precipitation double effect oxygen electrode catalyst described in claim 1, it is special
Levy and be, in step (2), the nitrogen source is selected from the organic matters such as thiocarbamide, urea, hexamethylenetetramine, thioacetamide
Plant or several, one or more of sulphur source in the organic matters such as thiocarbamide, thioacetamide.
5., according to a kind of preparation method of the self-supporting hydrogen reduction/precipitation double effect oxygen electrode catalyst described in claim 4, it is special
Levy and be, if nitrogen source and sulphur source are same organic matter；The consumption of nitrogen source and sulphur source is one.
6., according to a kind of preparation method of the self-supporting hydrogen reduction/precipitation double effect oxygen electrode catalyst described in claim 1, it is special
Levy and be, in step (2), transition metal salt is one or more in molysite, nickel salt or cobalt salt.
7., according to a kind of preparation method of the self-supporting hydrogen reduction/precipitation double effect oxygen electrode catalyst described in claim 1, it is special
Levy and be, in step (2), nitrogen source, sulphur source, the mol ratio of transition metal salt are 1-5：1-5:1, more preferably 3-5:3-5:1.
8., according to a kind of preparation method of the self-supporting hydrogen reduction/precipitation double effect oxygen electrode catalyst described in claim 1, it is special
Levy and be, in step (2), the total mol concentration of slaine is 0.01mol/L-0.1mol/L.
9., according to a kind of preparation method of the self-supporting hydrogen reduction/precipitation double effect oxygen electrode catalyst described in claim 1, it is special
Levy and be, in step (3), reactor compactedness is controlled 60%；Reaction temperature is 180 DEG C；Reaction time is 12h.
10. the self-supporting hydrogen reduction/precipitation double effect oxygen electrode catalyst for preparing according to claim 1-9 any one method.
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Cited By (6)
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| CN108963275A (en) * | 2018-06-01 | 2018-12-07 | 北京化工大学 | A kind of nonmetallic self-supporting air electrode and preparation method thereof |
| CN109473684A (en) * | 2018-09-29 | 2019-03-15 | 中国科学院山西煤炭化学研究所 | The elctro-catalyst and preparation method of a kind of sulphur-nitrogen-carbon-based oxygen reduction of transition metal codope and application |
| CN109518219A (en) * | 2018-12-24 | 2019-03-26 | 江苏大学 | A kind of preparation method and applications of graphene-based nickel cobalt bimetallic oxygen-separating catalyst |
| CN109768289A (en) * | 2018-12-27 | 2019-05-17 | 浙江工业大学 | A kind of flexible-paper-base biomorph Ni-V electrode and preparation method thereof |
| CN111883781A (en) * | 2020-06-05 | 2020-11-03 | 辽宁科技大学 | Activation method for nickel salt etched graphite felt electrode |
| CN112002912A (en) * | 2020-09-03 | 2020-11-27 | 四川轻化工大学 | Preparation method of nitrogen-doped carbon paper oxygen reduction reaction catalyst |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109518219A (en) * | 2018-12-24 | 2019-03-26 | 江苏大学 | A kind of preparation method and applications of graphene-based nickel cobalt bimetallic oxygen-separating catalyst |
| CN109768289A (en) * | 2018-12-27 | 2019-05-17 | 浙江工业大学 | A kind of flexible-paper-base biomorph Ni-V electrode and preparation method thereof |
| CN111883781A (en) * | 2020-06-05 | 2020-11-03 | 辽宁科技大学 | Activation method for nickel salt etched graphite felt electrode |
| CN112002912A (en) * | 2020-09-03 | 2020-11-27 | 四川轻化工大学 | Preparation method of nitrogen-doped carbon paper oxygen reduction reaction catalyst |
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Application publication date: 20170426 |