CN108183228A - A kind of nitrogen-doped carbon nano-array/cobalt ferrite material - Google Patents
A kind of nitrogen-doped carbon nano-array/cobalt ferrite material Download PDFInfo
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- CN108183228A CN108183228A CN201810010066.7A CN201810010066A CN108183228A CN 108183228 A CN108183228 A CN 108183228A CN 201810010066 A CN201810010066 A CN 201810010066A CN 108183228 A CN108183228 A CN 108183228A
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- nitrogen
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- ferrite material
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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
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/362—Composites
- H01M4/364—Composites as mixtures
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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
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/52—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
- H01M4/525—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron of mixed oxides or hydroxides containing iron, cobalt or nickel for inserting or intercalating light metals, e.g. LiNiO2, LiCoO2 or LiCoOxFy
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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
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
- H01M4/625—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
- Y02E60/10—Energy storage using batteries
Abstract
It the present invention provides a kind of nitrogen-doped carbon nano-array/cobalt ferrite material, is calcined and obtained by polyaniline iron cobalt metal organic framework, nano material is double oxide, large specific surface area, catalytic site are more, catalytic efficiency higher；By the excellent compatibility of metal organic framework and each metal ion species, it is readily synthesized uniform more metal spinelles to the present invention, bimetallic oxide and conducting polymer are combined with this, advantage be combined with each other between can making different type electrodes material, polyaniline can form the carbon of doping nitrogen by calcining simultaneously, it further improves electric conductivity, solves iron cobalt/cobalt oxide poorly conductive, the defects of stability is poor.
Description
Technical field
The invention belongs to electrode material preparation fields, are related to a kind of cobalt ferrite and are carried on nitrogen-doped carbon nano-array material.
Background technology
In new energy technology（Such as metal-air battery, fuel cell and decomposition water）, the electricity between oxygen and water urges
It is very crucial step to change conversion.At present, the composite material of platinum and platinum is considered as the best of oxygen reduction reaction (ORR)
Catalyst, and the oxide of ruthenium and iridium is the optimum catalyst of oxygen evolution reaction (OER).However, these material costs are high and resistance to
Long property is poor, it is difficult to extensive use.Therefore, research concentrates on catalyst of the transition metal oxide as OER at present.Ferrite
MFe2O4（M=Co, Ni, Cu etc.）Have many advantages, such as, such as：The advantages that low cost, high abundance, hypotoxicity, but in electrochemical process
Middle poorly conductive limits its catalytic activity and stability, therefore need to find the method for overcoming the problems, such as its poorly conductive.
Invention content
For current ferrite electric conductivity it is poor the problem of, the present invention provides a kind of nanometer based on iron cobalt polyaniline array
Material, catalytic efficiency higher, electric conductivity are more preferable.
The present invention also provides a kind of preparation methods of above-mentioned electrode material.
To achieve the above object, the present invention adopts the following technical scheme that.
A kind of nitrogen-doped carbon nano-array/cobalt ferrite（N-C@CoFe2O4）Material passes through polyaniline-organic bone of iron cobalt metal
Frame（PANI-Fe/Co MOF）Calcining obtains under a shielding gas.
The calcination temperature is 300-500 DEG C, preferably 400 DEG C；Calcination time is preferably 2-4h.
The protective gas is selected from nitrogen or inert gas, such as helium, argon gas.
The metal organic framework of the iron cobalt-polyaniline, is prepared using following methods：
（1）It rinses, dry after carbon paper pickling；
The acid is nitric acid.A concentration of 1mol/L of the acid.
Pickling temperature is 60-90 DEG C.
（2）In step（1）The carbon paper surface of acquisition prepares polyaniline nano battle array using perchloric acid and aniline as raw material electro-deposition
Row（N-CNAs）, then rinse, dry；
The molar ratio of the perchloric acid and aniline is 10:1.
Electric current is 0.15mA/cm in electro-deposition2, sedimentation time 5400s.
（3）Hydro-thermal method is in step（2）The carbon paper surface of acquisition, with molysite, cobalt salt and DOBDC（2,5- dioxy -1,4- benzene two
Carboxylic acid）Prepare polyaniline-iron cobalt metal organic framework.
The molysite is preferably ferrous salt, selected from Iron dichloride tetrahydrate.
The cobalt salt is selected from cabaltous nitrate hexahydrate.
The molar ratio of the iron ion, cobalt ions and DOBDC is 56:29:25.
The hydrothermal temperature is 120 DEG C, and the reaction time is for 24 hours.
A kind of above-mentioned nitrogen-doped carbon nano-array/application of the cobalt ferrite material in oxygen evolution reaction electrode is prepared.
A kind of application of above-mentioned nitrogen-doped carbon nano-array/cobalt ferrite material in battery electrode and in decomposing water.
The present invention has the following advantages：
Nitrogen-doped carbon nano-array material is carried on based on cobalt ferrite the present invention provides one kind（N-C@CoFe2O4）, by poly-
Aniline-iron cobalt metal organic framework（PANI-Fe/Co MOF）Under a shielding gas calcining obtain, resulting materials for double oxide,
Large specific surface area, catalytic site are more, catalytic efficiency higher；The present invention is good by metal organic framework and each metal ion species
Compatibility causes it to be readily synthesized uniform more metal spinelles, is combined bimetallic oxide and conducting polymer with this,
Advantage be combined with each other between can making different type electrodes material, while polyaniline can form the carbon of doping nitrogen by calcining,
It further improves electric conductivity, solves iron cobalt/cobalt oxide poorly conductive, the defects of stability is poor.In addition, the system of the electrode material
Preparation Method is simple, and cost is relatively low, has good stability, it has excellent performance under alkaline condition.
Description of the drawings
Fig. 1 is N-CNAs and N-C@CoFe2O4Scanning electron microscope diagram piece；Wherein a is N-CNAs's, and b is N-C@
CoFe2O4's；
Fig. 2 is N-C@CoFe2O4The linear voltammetric scan curve tested in 1M KOH electrolyte solutions with N-CNAs；
Fig. 3 is N-C@CoFe2O4The cyclic voltammetry curve tested in 1M KOH electrolyte solutions；
Fig. 4 is N-C@CoFe2O4Sweep fast map of current；
Fig. 5 is N-C@CoFe2O4The i-t long-time stable linearity curves in 1M KOH electrolyte solutions；
Fig. 6 is N-C@CoFe2O4, N-CNAs and carbon paper impedance diagram.
Specific embodiment
With reference to embodiment and attached drawing, the present invention will be further described, but the present invention is not limited by following embodiments
System.
The preparation of 1 nitrogen-doped carbon nano-array of embodiment/cobalt ferrite material.
1.1 the preparation of carbon paper
Suitable quantity of water is taken to be added in large beaker, ready carbon paper is put into 50mL beakers, 20mL ultra-pure waters is taken to be added to this
In beaker, then take the HNO that the mass fraction of 1.345mL is 68%3It is slowly added into the beaker.Small beaker is put into burning
It in cup, then is put on magnetic stirring apparatus and carries out heating water bath, acid boils carbon paper 1 hour at 90 DEG C；Well-done carbon paper is taken out, in carbon
It is marked on paper, 50mL small beakers is taken to clean up, and add in suitable ultra-pure water wherein, the carbon paper marked is added in
Wherein, it carries out being cleaned by ultrasonic 5-10 minutes, then changes ultra-pure water into EtOH Sonicate and clean 5 minutes；It places into baking oven and dries.
1.2 polyaniline nano arrays（N-CNAs）Preparation
50mL ultra-pure waters is taken to be added in beaker, beaker is placed on magnetic stirring apparatus and start to stir, are taken with liquid-transfering gun
4.310mL HClO4Be added in beaker, then take 0.460mL aniline solution be added to before beaker in, continue to stir
It mixes complete to solution mixing；Above-mentioned solution is poured into cleaned electrolytic cell, using the carbon paper that is ready for as working electrode,
Ag/AgCl reference electrodes are taken, graphite electrode is mounted on electrolytic cell, then carries out 0.15mA/cm with electrochemical workstation2,
The constant current electrochemical techniques deposition of 5400s；After the completion of deposition, the carbon paper removed, with ultrapure water, then in baking oven
Middle drying finally obtains the carbon paper of green.
1.3 polyanilines-iron cobalt metal organic framework（PANI-Fe/Co MOF）Preparation
10mL DMF solutions is taken to be added in beaker, liquid-transfering gun takes 2.000mL absolute ethyl alcohols and 1.000mL ultra-pure waters to be added to burning
In cup, beaker is placed on magnetic stirring apparatus, agitating solution is uniformly mixed；With electronic balance weighing 40mg DOBDC, 90mg
FeCl2·4H2O、68mg Co(NO3)2·6H2O is added in above-mentioned solution, and continues to stir, until solid is completely molten
Solution, solution becomes navy blue at this time；The carbon paper of gained in 1.2 is stood in water heating kettle vertically, above-mentioned dark blue solution is poured into
In reaction kettle, then reaction kettle is placed in 120 DEG C of baking oven and carries out hydro-thermal reaction 24 hours；After the completion of reaction, gained is taken out
Sample is washed repeatedly with ethyl alcohol, then vacuum drying 12 hours at 60 DEG C.
1.4 calcining
By 1.3 gained samples, 400 DEG C of argon atmosphere is calcined 2 hours in tube furnace, you can is obtained cobalt ferrite and is carried on N doping
Carbon nano-array material（N-C@CoFe2O4）.
2 nitrogen-doped carbon nano-array of embodiment/cobalt ferrite material（N-C@CoFe2O4）Physicochemical property.
Polyaniline nano array and Fig. 1 in embodiment 1 are a) polyaniline nano array material in the synthesis process（N-
CNAs）Scanning electron microscopic picture, b) be nitrogen-doped carbon nano-array/cobalt ferrite material（N-C@CoFe2O4）Scanning electron microscope figure
Piece, it is known that, successfully prepare N-CNAs and N-C@CoFe2O4。
3 nitrogen-doped carbon nano-array of embodiment/cobalt ferrite material（N-C@CoFe2O4）Catalytic activity.
3.1 linear sweep voltammetry
It is detected in 1M KOH electrolyte solutions（0V~0.8V vs.Ag/AgCl）N-CNAs and N-C@CoFe2O4It is corresponding linear
It is as shown in Figure 2 to scan voltammetry curve：N-C@CoFe2O4Starting overpotential for 1.42V, the starting overpotential of N-CNAs is
1.57V。N-C@CoFe2O4Overpotential is originated than relatively low, it is relatively low to carry out required potential during oxygen evolution reaction.It follows that N-C@
CoFe2O4OER catalytic activity than N-CNAs catalytic activity enhancing.
3.2 electrochemical surface active areas
N-C@CoFe2O4The cyclic voltammetry curve tested in 1M KOH electrolyte solutions（0V~0.8V vs.Ag/AgCl）Such as figure
Shown in 3, detected in 1M KOH electrolyte solutions（- 0.05V 0.05V vs.Ag/AgCl, sweep speed 20,40,60,
80、100mV/s）N-C@CoFe2O4Sweep fast electric current, with reference to Fig. 4, it is 8.3784 that can obtain its electrochemical surface active area, explanation
N-C@CoFe2O4There is the active site of more electrochemical reaction.
3.3 i-t long-time stabilities
It is detected in 1M KOH electrolyte solutions（0.6V vs. Ag/AgCl, time 36000s）N-C@CoFe2O4It long when
Between stability, as shown in Figure 5.As seen from the figure, curve is more straight, illustrates N-C@CoFe2O4It can keep in a long time
Stablize, i.e., stability is preferable.
3.4 impedance
N-C@CoFe are detected in 1M KOH solutions2O4, N-CNAs and carbon paper impedance, impedance nyquist diagram is obtained, such as Fig. 6 institutes
Show：As can be seen from the figure the slope of curve of simple carbon paper is maximum, i.e. impedance is minimum, N-C@CoFe2O4Impedance is maximum, but three
It compares, gap is simultaneously little.The impedance of this three is smaller compared with the material that other have been reported simultaneously, this is because polyaniline is formed
Nano array structure can effectively prevent aggregation and stacking, reduce internal resistance.
Claims (9)
1. a kind of nitrogen-doped carbon nano-array/cobalt ferrite material, which is characterized in that pass through polyaniline-iron cobalt metal organic framework
Calcining obtains under a shielding gas.
2. nitrogen-doped carbon nano-array/cobalt ferrite material according to claim 1, which is characterized in that calcination temperature is
300-500℃。
3. nitrogen-doped carbon nano-array/cobalt ferrite material according to claim 1, which is characterized in that protective gas is selected from
Nitrogen or inert gas.
4. nitrogen-doped carbon nano-array/cobalt ferrite material according to claim 1, which is characterized in that the iron cobalt-polyphenyl
The metal organic framework of amine, is prepared using following methods：
（1）It rinses, dry after carbon paper pickling；
（2）In step（1）The carbon paper surface of acquisition prepares polyaniline nano array using perchloric acid and aniline as raw material electro-deposition,
Then it rinses, dry；
（3）Hydro-thermal method is in step（2）The carbon paper surface of acquisition, preparing polyaniline-iron cobalt metal with molysite, cobalt salt and DOBDC has
Machine skeleton.
5. nitrogen-doped carbon nano-array/cobalt ferrite material according to claim 4, which is characterized in that step（1）Middle pickling
Temperature is 60-90 DEG C.
6. nitrogen-doped carbon nano-array/cobalt ferrite material according to claim 4, which is characterized in that the perchloric acid with
The molar ratio of aniline is 10:1；The electric current of electro-deposition is 0.15mA/cm2, sedimentation time 5400s.
7. nitrogen-doped carbon nano-array/cobalt ferrite material according to claim 4, which is characterized in that the iron ion, cobalt
The molar ratio of ion and DOBDC are 56:29:25；Hydrothermal temperature is 120 DEG C, and the reaction time is for 24 hours.
8. a kind of nitrogen-doped carbon nano-array/cobalt ferrite material as described in claim 1-8 is any is preparing oxygen evolution reaction electricity
Application in extremely.
9. a kind of nitrogen-doped carbon nano-array/cobalt ferrite material as described in claim 1-8 is any is in battery electrode and decomposition
Application in water.
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109433240A (en) * | 2018-10-26 | 2019-03-08 | 济南大学 | A kind of nitrogen-doped carbon nano-array load iron phosphide/phosphatization cobalt preparation method |
| CN109585861A (en) * | 2018-11-07 | 2019-04-05 | 三峡大学 | A kind of preparation method of difunctional cobalt black and nitrogen-doped carbon In-situ reaction electrode |
| CN109585856A (en) * | 2018-11-07 | 2019-04-05 | 三峡大学 | A kind of preparation method of difunctional cobalt sulfide and sulphur, nitrogen-doped carbon In-situ reaction electrode |
| CN109599565A (en) * | 2018-11-07 | 2019-04-09 | 三峡大学 | A kind of preparation method of difunctional cobalt and nitrogen-doped carbon composite in-situ electrode |
| CN110112427A (en) * | 2019-04-11 | 2019-08-09 | 北京化工大学 | A kind of preparation method of the nitrogen of electrochemistry auxiliary, the carbon-based air electrode of phosphorus codope |
| CN110265667A (en) * | 2019-06-12 | 2019-09-20 | 青岛科技大学 | A kind of novel nano composite catalyst and preparation method thereof applied to hydrogen reduction |
| CN110280290A (en) * | 2019-07-08 | 2019-09-27 | 华南理工大学 | One kind having flower-shaped type nitrogen-doped carbon-spinel-type microspherical catalyst of high-specific surface area and the preparation method and application thereof |
| CN111613802A (en) * | 2020-06-10 | 2020-09-01 | 中国船舶重工集团公司第七二五研究所 | Modified carbon brush electrode and preparation method thereof |
| CN111668499A (en) * | 2020-04-20 | 2020-09-15 | 中山大学 | Polyaniline-derived nitrogen-doped carbon-supported multi-element alloy catalyst and preparation method and application thereof |
| CN115487844A (en) * | 2022-08-09 | 2022-12-20 | 广州大学 | High-activity ORR catalytic material N-doped carbon dot/CoFe 2 O 4 And method for synthesizing the same |
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Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109433240A (en) * | 2018-10-26 | 2019-03-08 | 济南大学 | A kind of nitrogen-doped carbon nano-array load iron phosphide/phosphatization cobalt preparation method |
| CN109599565B (en) * | 2018-11-07 | 2022-03-04 | 三峡大学 | Preparation method of difunctional cobalt and nitrogen-doped carbon composite in-situ electrode |
| CN109585861A (en) * | 2018-11-07 | 2019-04-05 | 三峡大学 | A kind of preparation method of difunctional cobalt black and nitrogen-doped carbon In-situ reaction electrode |
| CN109585856A (en) * | 2018-11-07 | 2019-04-05 | 三峡大学 | A kind of preparation method of difunctional cobalt sulfide and sulphur, nitrogen-doped carbon In-situ reaction electrode |
| CN109599565A (en) * | 2018-11-07 | 2019-04-09 | 三峡大学 | A kind of preparation method of difunctional cobalt and nitrogen-doped carbon composite in-situ electrode |
| CN109585861B (en) * | 2018-11-07 | 2022-03-04 | 三峡大学 | Preparation method of dual-functional cobalt monoxide and nitrogen-doped carbon in-situ composite electrode |
| CN109585856B (en) * | 2018-11-07 | 2022-03-04 | 三峡大学 | Preparation method of dual-functional cobalt sulfide and sulfur and nitrogen doped carbon in-situ composite electrode |
| CN110112427A (en) * | 2019-04-11 | 2019-08-09 | 北京化工大学 | A kind of preparation method of the nitrogen of electrochemistry auxiliary, the carbon-based air electrode of phosphorus codope |
| CN110265667A (en) * | 2019-06-12 | 2019-09-20 | 青岛科技大学 | A kind of novel nano composite catalyst and preparation method thereof applied to hydrogen reduction |
| CN110280290A (en) * | 2019-07-08 | 2019-09-27 | 华南理工大学 | One kind having flower-shaped type nitrogen-doped carbon-spinel-type microspherical catalyst of high-specific surface area and the preparation method and application thereof |
| CN110280290B (en) * | 2019-07-08 | 2021-10-26 | 华南理工大学 | Flower-shaped nitrogen-doped carbon-spinel microsphere catalyst with high specific surface area and preparation method and application thereof |
| CN111668499A (en) * | 2020-04-20 | 2020-09-15 | 中山大学 | Polyaniline-derived nitrogen-doped carbon-supported multi-element alloy catalyst and preparation method and application thereof |
| CN111613802A (en) * | 2020-06-10 | 2020-09-01 | 中国船舶重工集团公司第七二五研究所 | Modified carbon brush electrode and preparation method thereof |
| CN115487844A (en) * | 2022-08-09 | 2022-12-20 | 广州大学 | High-activity ORR catalytic material N-doped carbon dot/CoFe 2 O 4 And method for synthesizing the same |
| CN115487844B (en) * | 2022-08-09 | 2023-11-14 | 广州大学 | Catalytic material N-doped carbon dot/CoFe of high-activity ORR 2 O 4 And method for synthesizing the same |
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