CN106654301A - Preparation method for carbon/metal oxide nanofiber composite catalyst - Google Patents
Preparation method for carbon/metal oxide nanofiber composite catalyst Download PDFInfo
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- CN106654301A CN106654301A CN201611185588.8A CN201611185588A CN106654301A CN 106654301 A CN106654301 A CN 106654301A CN 201611185588 A CN201611185588 A CN 201611185588A CN 106654301 A CN106654301 A CN 106654301A
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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
- H01M4/8647—Inert electrodes with catalytic activity, e.g. for fuel cells consisting of more than one material, e.g. consisting of composites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- H—ELECTRICITY
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M12/00—Hybrid cells; Manufacture thereof
- H01M12/08—Hybrid cells; Manufacture thereof composed of a half-cell of a fuel-cell type and a half-cell of the secondary-cell type
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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
- H01M4/88—Processes of manufacture
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- H—ELECTRICITY
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- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/90—Selection of catalytic material
- H01M4/9016—Oxides, hydroxides or oxygenated metallic salts
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- H—ELECTRICITY
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- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/96—Carbon-based electrodes
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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Abstract
The invention relates to a preparation method for a carbon/metal oxide nanofiber composite catalyst. The preparation method comprises the following steps of (a), dissolving a metal ion-containing salt solution and a high-molecular polymer into an organic solvent, and stirring to form a spinning precursor mixed solution, wherein the metal ion concentration is weighed based on a stoichiometric ratio; (b), performing electrostatic spinning on the spinning precursor mixed solution to form a composite non-woven material; and (c), putting the composite non-woven material into an inert atmosphere to be subjected to high-temperature calcining to obtain the carbon/metal oxide nanofiber composite catalyst. The carbon/metal oxide nanofiber composite catalyst has high electrical conductivity, reinforced oxygen reduction electro-catalytic property and excellent oxygen evolution performance, and is a dual-functional catalyst with efficient catalytic property.
Description
Technical field
The invention belongs to field of nanometer material technology, is related to a kind of preparation method of catalyst, and in particular to a kind of nanocarbon/metal oxygen
The preparation method of compound nanofiber composite catalyst.
Background technology
The Heavy environmental pollutions for being caused using traditional fuel due to energy crisis and in a large number, research and development cleaning, efficiently
And continuable novel energy causes people and more and more payes attention to and interest.Wherein metal-air battery, particularly has
The lithium-air battery of superelevation theoretical specific capacity has obtained in recent years quick development, but due to the negative electrode oxygen in course of reaction
Gas is reduced(ORR)And oxygen evolution reaction(OER)Dynamics is slow, causes metal-air battery to have discharge and recharge overpotential height, follow
The problems such as ring efficiency is low, high rate performance is poor, cycle life is short, so as to limit its extensive practical application.
At present, the cathod catalyst of metal-air battery mainly has following three kinds:Noble metal, carbon and metal oxide etc.,
Three respectively has pluses and minuses.Noble metal(Such as Pt)Catalytic performance is excellent, and catalysis activity is high, but its is expensive, high cost, limits
Its promotion and application;Material with carbon element catalyst, with low cost, wide material sources, but most material with carbon element is only to hydrogen reduction
(ORR)Effectively, oxygen is separated out(OER)It is invalid, in addition in long-term cyclic process, the less stable of material with carbon element;Metal oxygen
Compound catalyst, is a kind of bifunctional catalyst, effective to ORR, OER, and its low price, wide material sources, synthesis side
Method is simple, is especially suitable for practical application, but its electric conductivity is generally bad.
The content of the invention
The invention aims to overcome the deficiencies in the prior art and provide a kind of nanocarbon/metal oxide nanofiber and be combined
The preparation method of catalyst.
To reach above-mentioned purpose, the technical solution used in the present invention is:A kind of nanocarbon/metal oxide nanofiber is compound to urge
The preparation method of agent, it is comprised the following steps:
(a)Salting liquid containing metal ion and high molecular polymer are dissolved in organic solvent, stirring forms spinning presoma
Mixed liquor;
(b)The spinning presoma mixed liquor is carried out into electrostatic spinning and forms nonwoven composite;
(c)The nonwoven composite is placed in inert gas atmosphere to be carried out high-temperature calcination and obtains final product nanocarbon/metal oxidate nano
Fibre composite catalyst.
Optimally, 15 ~ 20V of voltage, inject speed for 0.5 ~ 1mm/min and receive distance for 15 ~ 20mm.
Optimally, the high-temperature calcination is to calcine 0.5 ~ 10 hour at 500 ~ 900 DEG C.
Optimally, in the nanocarbon/metal oxide nanofiber composite catalyst metal oxide load capacity be 10 ~
80wt%。
Because above-mentioned technical proposal is used, the present invention has compared with prior art following advantages:Nanocarbon/metal oxygen of the present invention
The preparation method of compound nanofiber composite catalyst, by by the mixed liquor of the salting liquid of metal ion and high molecular polymer
Carry out being calcined after electrostatic spinning, obtain with carbon fiber as core, metal oxide particle is embedded in the surface of carbon nano-fiber or interior
The nanofiber composite catalyst in portion so as to good electric conductivity, enhanced hydrogen reduction electrocatalysis characteristic and excellent oxygen
Performance is separated out, is a kind of bifunctional catalyst with efficient catalytic performance.
Description of the drawings
Accompanying drawing 1 is the electron microscope of obtained nanocarbon/metal oxide nanofiber composite catalyst in embodiment 1:(a)Scanning
Electron microscope, 10 μm;(b)Scanning electron microscope (SEM) photograph, 2 μm;(c)Transmission electron microscope picture, 0.5 μm;(d)5nm transmission electron microscope pictures(TEM), 5nm;
Accompanying drawing 2 is the obtained nanocarbon/metal oxide nanofiber composite catalyst of present invention N at different temperatures2Atmosphere is calcined
Performance afterwards:(a)Hydrogen reduction performance,(b)Oxygen separates out performance;
The performance of nanocarbon/metal oxide nanofiber composite catalyst in different loads amount obtained in the present invention of accompanying drawing 3:(a)
Hydrogen reduction performance,(b)Oxygen separates out performance;
Accompanying drawing 4 is the obtained nanocarbon/metal oxide nanofiber composite catalyst of the present invention and single C catalyst(N-C)、
Metal oxide catalyst(NCO)And commercialization Pt/C catalyst performance in the basic conditions:(a)Hydrogen reduction performance,(b)
Oxygen separates out performance;
Accompanying drawing 5 is obtained nanocarbon/metal oxide nanofiber composite catalyst property figure in embodiment 6:(a)ESEM
Figure, 10 μm, 500 DEG C;(b)ORR performances, 500 DEG C;(c)Scanning electron microscope (SEM) photograph, 500nm, 500 DEG C;(d)ORR performances, 700 DEG C.
Specific embodiment
The preparation method of nanocarbon/metal oxide nanofiber composite catalyst of the present invention, it is comprised the following steps:(a)Will
Salting liquid containing metal ion and high molecular polymer are dissolved in organic solvent, and stirring forms spinning presoma mixed liquor;Institute
Metal ion is stated for one or more in transition metal ions;As nickel ion and cobalt ions mix, the concentration of cobalt ions
For the twice of the nickel ion concentration;(b)The spinning presoma mixed liquor is carried out into electrostatic spinning and forms nonwoven composite;
(c)The nonwoven composite is placed in inert gas atmosphere to be carried out high-temperature calcination and obtains final product nanocarbon/metal oxide nanofiber
Composite catalyst.Composite catalyst be with carbon fiber as core, metal oxide particle be embedded in the surface of carbon nano-fiber or interior
The nanofiber composite catalyst in portion, separates out with good electric conductivity, enhanced hydrogen reduction electrocatalysis characteristic and excellent oxygen
Performance, is a kind of bifunctional catalyst with efficient catalytic performance.The concentration of nickel ion in salting liquid containing metal ion
For 0.05 ~ 1mol/L, high molecular polymer can be polyacrylonitrile, polyvinylpyrrolidone(PVP), the conventional high score such as polyaniline
Sub- material so that the salt containing metal ion is 60 ~ 90% with the mass ratio of high molecular polymer, so after high-temperature calcination most
Eventually the load capacity of metal oxide is about 10 ~ 80wt% in obtained nanocarbon/metal oxide nanofiber composite catalyst.It is organic
Solvent can usually dissolve those of polymer, such as dimethylformamide(DMF), absolute ethyl alcohol or DMSO etc..
Above-mentioned electrostatic spinning is directly spun using electrostatic spinning machine, and design parameter is:15 ~ 20V of voltage, inject speed
Be 0.5 ~ 1mm/min and receive distance be 15 ~ 20mm.Step(c)In, the high-temperature calcination is to calcine 0.5 at 500 ~ 900 DEG C
~ 10 hours;
The present invention is further described below in conjunction with accompanying drawing embodiment.
Embodiment 1
The present embodiment provides a kind of nanocarbon/metal oxide nanofiber composite catalyst(N-C@NCO)Preparation method, it includes
Following steps:
(a)By the salting liquid containing 1mmol nickel nitrates and 2mmol cobalt nitrates and 1.0g high molecular polymers(Polyacrylonitrile,
MACKLIN, mean molecule quantity 150000)It is dissolved in 10mL organic solvents(DMF)In, stir and form within 2 hours the mixing of spinning presoma
Liquid;
(b)By step(a)The spinning presoma mixed liquor for obtaining is placed in electrostatic spinning machine and carries out electrostatic spinning and form compound nothing
Woven material, the control parameter of electrostatic spinning machine is:Voltage 15V, inject speed for 0.5mm/min, receive distance for 15mm, obtaining
Diameter is about the filament of 1 ~ 2mm;
(c)Above-mentioned nonwoven composite is placed in nitrogen atmosphere, is calcined 5 hours at 800 DEG C.Obtained nanocarbon/metal oxygen
Compound nanofiber composite catalyst is as shown in Figure 1.Fig. 1(a)Composite catalyst obtained by showing is hollow Nano tubular construction,
Metal oxide particle is dispersed and is embedded in the surface and inside of carbon nano-fiber, such as Fig. 1(b)It is shown.Fig. 1(c)It is right
The transmission electron microscope picture answered(TEM), it can be seen that the nanofiber pipe is a loose structure, and metal oxide particle is with high
Density is dispersed in the surface and inside of carbon nano-fiber.Fig. 1(d)The lattice fringe of metal oxide particle is shown, its value
0.2427 nm just correspond to NiCo2O4's(311)Peak, while it can also be seen that the carbon-coating bag that is graphitized of metal oxide particle
Wrap up in, and the degree of graphitization of the carbon-coating is higher, this may promote raising of the composite catalyst to ORR and OER catalytic performances.
Embodiment 2
The present embodiment provides a kind of preparation method of nanocarbon/metal oxide nanofiber composite catalyst, its concrete steps and reality
Apply basically identical in example 1, except for the difference that:Step(c)In, it is to calcine 5 hours at 500 DEG C.
Embodiment 3
The present embodiment provides a kind of preparation method of nanocarbon/metal oxide nanofiber composite catalyst, its concrete steps and reality
Apply basically identical in example 1, except for the difference that:Step(c)In, it is to calcine 5 hours at 900 DEG C.
Composite catalyst in embodiment 1 to 3 is entered using rotating ring disk electrode (r.r.d.e) measuring technology in 0.1M KOH solutions
Row ORR and OER catalytic performance test:The rpm of electrode tip rotating speed 1600, potential scan rate:10 mV/s, electric potential scanning scope:-
0.9 ~ 0V, to electrode Pt silks, reference electrode Ag/AgCl electrodes(Note:Current potential is had been converted into relative to reversible hydrogen electrode in figure, with
It is easy to be compared with documentation);As a result it is as shown in Figure 2.Composite catalyst in embodiment 1 shows the catalytic of optimum
Energy.
Embodiment 4
The present embodiment provides a kind of preparation method of nanocarbon/metal oxide nanofiber composite catalyst, its concrete steps and reality
Apply basically identical in example 1, except for the difference that:Step(a)In, containing 0.5mmol nickel nitrates and 1mmol cobalt nitrates in salting liquid
Salting liquid.
Embodiment 5
The present embodiment provides a kind of preparation method of nanocarbon/metal oxide nanofiber composite catalyst, its concrete steps and reality
Apply basically identical in example 1, except for the difference that:Step(a)In, containing 1.5mmol nickel nitrates and 3mmol cobalt nitrates in salting liquid
Salting liquid.
Composite catalyst in embodiment 1, embodiment 4 and 5 is carried out into ORR and OER catalytic performance tests, as a result such as Fig. 3
It is shown.Composite catalyst in embodiment 1 shows the catalytic performance of optimum.
Embodiment 6
The method can also be extended on different material with carbon elements and metal oxide, i.e., using the forerunner containing different metal ions
Liquid solution and suitable difference macromolecule polyalcohol, such that it is able to prepare various nanocarbon/metal oxide composite catalysts.This
Embodiment provides a kind of preparation method of nanocarbon/metal oxide nanofiber composite catalyst, its with embodiment 1 in basic one
Cause, except for the difference that:Using 1mmol nickel nitrates and the salting liquid of 1mmol lanthanum nitrates, and 1.0g polyvinylpyrrolidones;And point
It is not placed in 500 DEG C, 700 DEG C to be calcined(Carry out in nitrogen and air respectively, obtain composite catalyst and metal oxide
Catalyst).Metal oxide dispersion is uniform in obtained nanocarbon/metal oxide nanofiber composite catalyst, such as Fig. 5(a)With 5
(c)It is shown.Find that the ORR performances of composite catalyst will be aoxidized better than single metal by Rotation ring disk electrode Testing Technology Study
Thing catalyst, such as Fig. 5(b)With 5(d)It is shown.The nanocarbon/metal oxide catalyst that prepared by the method is simple, efficiently, cost
It is cheap, and excellent electrocatalysis characteristic is shown, and then metal-air battery is can apply to, and fuel cell and moisture
The fields such as solution, with wide potential application market.
Comparative example 1
This example provides a kind of single C catalyst(N-C)Preparation method, basic in its concrete steps and embodiment 1
Cause, except for the difference that:Step(a)In do not add nickeliferous, cobalt salting liquid.
Comparative example 2
This example provides a kind of only catalyst containing metal oxide, basically identical, the difference in its concrete steps and embodiment 1
Be:Step(c)In, calcined in air atmosphere, obtain the only catalyst containing metal oxide(NCO).
By oxygen of the catalyst and business-like Pt/C in embodiment 1, comparative example 1 and comparative example 2 under alkaline environment
Reduction electrocatalysis characteristic is compared, it can be found that composite catalyst shows the catalytic performance of optimum, when current density is 2.5
mA/cm2When, the current potential of N-C, NCO, N-C@NCO is respectively 0.65,0.69,0.76 V, and the catalytic performance of composite catalyst is most
Jie Jin business-like Pt/C catalyst, the limiting current density that essentially coincides with business-like Pt/C catalyst and closest is reached
Half wave potential, such as Fig. 4(a)It is shown.In addition to enhanced hydrogen reduction electrocatalysis characteristic, the catalyst after being combined also is showed
Go out excellent oxygen and separate out performance, as a result such as Fig. 4(b)It is shown, show in alkaline solution the composite catalyst carrying current,
Take-off potential aspect will be better than single carbon, metal oxide and business-like Pt/C catalyst.Thus explanation is by being somebody's turn to do
Carbon@metal oxide catalysts prepared by method are a kind of bifunctional catalysts with efficient catalytic performance.
Above-described embodiment technology design only to illustrate the invention and feature, its object is to allow person skilled in the art
Scholar will appreciate that present disclosure and implement according to this, can not be limited the scope of the invention with this, all according to the present invention
Equivalence changes or modification that Spirit Essence is made, all should be included within the scope of the present invention.
Claims (4)
1. a kind of preparation method of nanocarbon/metal oxide nanofiber composite catalyst, it is characterised in that it includes following step
Suddenly:
(a)Salting liquid containing metal ion and high molecular polymer are dissolved in organic solvent, stirring forms spinning presoma
Mixed liquor;
(b)The spinning presoma mixed liquor is carried out into electrostatic spinning and forms nonwoven composite;
(c)The nonwoven composite is placed in inert gas atmosphere to be carried out high-temperature calcination and obtains final product nanocarbon/metal oxidate nano
Fibre composite catalyst.
2. the preparation method of nanocarbon/metal oxide nanofiber composite catalyst according to claim 1, its feature exists
In the parameter of the electrostatic spinning is:15 ~ 20V of voltage, inject speed for 0.5 ~ 1mm/min and receive distance for 15 ~
20mm。
3. the preparation method of nanocarbon/metal oxide nanofiber composite catalyst according to claim 1, its feature exists
In:The high-temperature calcination is to calcine 0.5 ~ 10 hour at 500 ~ 900 DEG C.
4. the preparation method of nanocarbon/metal oxide nanofiber composite catalyst according to claim 1, its feature exists
In:The load capacity of metal oxide is 10 ~ 80wt% in the nanocarbon/metal oxide nanofiber composite catalyst.
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Cited By (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN110508311A (en) * | 2019-08-30 | 2019-11-29 | 浙江工业大学 | A kind of porous boron doped carbon supported platinum nano beaded catalyst and its preparation method and application based on electrostatic spinning technique |
WO2020134740A1 (en) * | 2018-12-24 | 2020-07-02 | 江南大学 | Electrolysed water catalytic material of platinum-doped carbide and preparation method thereof |
CN111653789A (en) * | 2020-06-17 | 2020-09-11 | 泰州市海创新能源研究院有限公司 | Zinc-air battery catalyst and preparation method thereof |
CN112086652A (en) * | 2020-09-15 | 2020-12-15 | 香港科技大学深圳研究院 | Hollow carbon sphere/graphene bifunctional catalyst and preparation method and application thereof |
CN112553641A (en) * | 2020-11-24 | 2021-03-26 | 华南理工大学 | MXene and transition metal sulfide composite nano catalyst based on fiber framework and preparation method thereof |
CN113394411A (en) * | 2021-06-11 | 2021-09-14 | 内蒙古工业大学 | Preparation and application of perovskite nanofiber electrocatalyst for rechargeable zinc-air battery |
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Cited By (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2020134740A1 (en) * | 2018-12-24 | 2020-07-02 | 江南大学 | Electrolysed water catalytic material of platinum-doped carbide and preparation method thereof |
CN110508311A (en) * | 2019-08-30 | 2019-11-29 | 浙江工业大学 | A kind of porous boron doped carbon supported platinum nano beaded catalyst and its preparation method and application based on electrostatic spinning technique |
CN111653789A (en) * | 2020-06-17 | 2020-09-11 | 泰州市海创新能源研究院有限公司 | Zinc-air battery catalyst and preparation method thereof |
CN112086652A (en) * | 2020-09-15 | 2020-12-15 | 香港科技大学深圳研究院 | Hollow carbon sphere/graphene bifunctional catalyst and preparation method and application thereof |
CN112553641A (en) * | 2020-11-24 | 2021-03-26 | 华南理工大学 | MXene and transition metal sulfide composite nano catalyst based on fiber framework and preparation method thereof |
CN112553641B (en) * | 2020-11-24 | 2022-02-15 | 华南理工大学 | MXene and transition metal sulfide composite nano catalyst based on fiber framework and preparation method thereof |
CN113394411A (en) * | 2021-06-11 | 2021-09-14 | 内蒙古工业大学 | Preparation and application of perovskite nanofiber electrocatalyst for rechargeable zinc-air battery |
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