CN109686993A - A kind of N doping mesoporous carbon spheres Nonmetal oxygen reduction catalyst, preparation method and application - Google Patents
A kind of N doping mesoporous carbon spheres Nonmetal oxygen reduction catalyst, preparation method and application Download PDFInfo
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- CN109686993A CN109686993A CN201811597073.8A CN201811597073A CN109686993A CN 109686993 A CN109686993 A CN 109686993A CN 201811597073 A CN201811597073 A CN 201811597073A CN 109686993 A CN109686993 A CN 109686993A
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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
- H01M4/96—Carbon-based electrodes
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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
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Abstract
The invention discloses a kind of N doping mesoporous carbon spheres Nonmetal oxygen reduction catalysts, preparation method and application.The present invention is by polyacrylonitrile, polyvinylpyrrolidone and fumed silica are dissolved in dimethylformamide jointly, products therefrom is subjected to electrostatic spinning, spinning is received with aluminium foil, it first pre-oxidizes in air again, then it is carbonized in an inert atmosphere, finally up to N doping mesoporous carbon spheres Nonmetal oxygen reduction catalyst after removing template.Template used dose of the present invention cheap, and preparation method is simple, is easy to large-scale production.Prepared catalyst have apparent hydrogen reduction characteristic peak, compared to business Pt C catalyst, the catalyst is at low cost, has good stability.
Description
Technical field
The invention belongs to electrochemical technology fields, and in particular to a kind of nonmetallic hydrogen reduction catalysis of N doping mesoporous carbon spheres
Agent, preparation method and application.
Background technique
Fuel cell is a kind of device that the chemical energy of fuel can be directly translated into electric energy.It is different from common batteries
It is that fuel cell does not have the limitation of capacity, as long as theoretically constantly providing fuel for fuel cell, it can in a steady stream not
Disconnected ground externally exports electric energy.Since, without overheated machine process, fuel cell is not by Carnot cycle in entire energy conversion process
Limitation, therefore fuel cell generally all has relatively high energy transformation ratio.However so far, fuel cell does not obtain greatly
The commodity production and application of scale, one of important restriction factor are exactly its cathod catalyst.Current such catalyst master
Noble metal, especially platinum-base material, expensive, the limited source of such catalyst are used, and is had intolerant to carbon monoxide, first
The disadvantages of alcoholism [1,2].Therefore, finding more preferably cathod catalyst is that fuel cell obtains widespread commercial and needs to solve
One of important problem certainly.
Porous carbon materials are catalyzed due to being widely used in catalyst with good conductivity and higher specific surface area
Agent carrier, in supercapacitor and lithium ion battery.Hetero atom (such as nitrogen) doping can be by modified carbonaceous components.When nitrogen-atoms is mixed
Miscellaneous to after porous carbon materials, the charge density of porous carbon materials increases, and forms n-type semiconductor, and then make leading for porous carbon materials
Electrically increase [3].In addition introducing of the hetero atom in porous carbon materials structure also will increase the defective bit of porous carbon materials, improve
The catalytic activity of catalyst.The present invention provides a kind of relatively simple N doping mesoporous carbon spheres Nonmetal oxygen reduction catalyst systems
Preparation Method.
Bibliography
[1]C.H.S.Brian,H.Angellka,Materials for fuel-cell technologies.[J]
Nature,2001,414,345-352.
[2]V.R.Stamenkovic,B.Fowler,B.S.Mun,et al.,“Improved oxygen reduction
activity on Pt3Ni(111)via increased surface site availability.[J]Science,
2007,315(5811):493-497.
[3]T.Yang,J.Liu,R.Zhou,et al.,N-doped mesoporous carbon spheres as
the oxygen reduction reaction catalysts.[J]Journal of Materials Chemistry A,
2014,2(42):18139-18146.
Summary of the invention
For overcome the deficiencies in the prior art, the purpose of the present invention is to provide a kind of nonmetallic oxygen of N doping mesoporous carbon spheres
Reducing catalyst, preparation method and application.Preparation method of the present invention is simple, and cost of material is cheap, environmental-friendly；Catalyst has
Preferable hydrogen reduction performance.
Polyacrylonitrile, polyvinylpyrrolidone and fumed silica (template) are dissolved in dimethyl methyl by the present invention jointly
In amide, products therefrom is subjected to electrostatic spinning, spinning is received with aluminium foil, obtains carbon fiber, then carbon fiber is pre- in air
Oxidation, is then carbonized in an inert atmosphere, is catalyzed after finally removing template up to the nonmetallic hydrogen reduction of N doping mesoporous carbon spheres
Agent.Technical solution of the present invention is specifically described as follows.
A kind of preparation method of N doping mesoporous carbon spheres Nonmetal oxygen reduction catalyst, the specific steps are as follows:
1) polyacrylonitrile, polyvinylpyrrolidone and fumed silica are dissolved in jointly in dimethylformamide, in room
It is uniformly mixed under temperature；
2) electrostatic spinning apparatus is added in mixed system, using aluminium foil as screen is received, carries out electrostatic spinning；
3) first the obtained product of step 2) is put into tube furnace, under air atmosphere, after being warming up to 200~250 DEG C,
Pre-oxidation 1~4 hour, then in an inert atmosphere, is warming up at 700~950 DEG C and is carbonized 1~4 hour, sample after being finally carbonized
Product impregnate stirring in sodium hydroxide solution and remove silica, obtain N doping mesoporous carbon spheres Nonmetal oxygen reduction catalyst.
Above-mentioned steps 1) in, the mass ratio of polyacrylonitrile, polyvinylpyrrolidone and fumed silica is (2~5): (2
~5): (2~10).
Above-mentioned steps 1) in, the mass ratio of fumed silica and dimethylformamide is 1:10~1:20.
Above-mentioned steps 2) in, spinning condition is 12~18kV of voltage, receives 15~20cm of distance, 0.05~5mL/h of flow velocity.
Above-mentioned steps 3) in, the concentration of sodium hydroxide solution is 1~5mol.L-1, dipping mixing time is 4-8 hours.
The present invention also provides N doping mesoporous carbon spheres Nonmetal oxygen reduction catalysts made from a kind of above-mentioned preparation method.
The present invention further provides a kind of applications of above-mentioned N doping mesoporous carbon spheres Nonmetal oxygen reduction catalyst.
Compared to the prior art, the beneficial effects of the present invention are:
(1) preparation method is simple: obtaining tunica fibrosa by electrostatic spinning, roasting removal silica can be obtained mesoporous
Carbon ball.
(2) silica used in has been commercialized, cheap.
(2) used catalyst has an excellent oxygen reduction activity under alkaline condition, and than business Pt C catalyst have more
Excellent stability.
Detailed description of the invention
Fig. 1 is the scanning electron microscope (SEM) photograph that the embodiment of the present invention 1 prepares N doping mesoporous carbon spheres Nonmetal oxygen reduction catalyst
(10000 times).
Fig. 2 is the scanning electron microscope (SEM) photograph that the embodiment of the present invention 1 prepares N doping mesoporous carbon spheres Nonmetal oxygen reduction catalyst
(30000 times).
Fig. 3 is the N2 adsorption desorption figure that the embodiment of the present invention 1 prepares N doping mesoporous carbon spheres Nonmetal oxygen reduction catalyst.
Fig. 4 is the x-ray photoelectron energy that the embodiment of the present invention 1 prepares N doping mesoporous carbon spheres Nonmetal oxygen reduction catalyst
Spectrum analysis figure.
Fig. 5 is that the embodiment of the present invention 1 prepares N doping mesoporous carbon spheres Nonmetal oxygen reduction catalyst and commercial catalysts platinum
The chronoa mperometric plot figure of carbon, the figure are the catalyst and business after 9000s at constant voltage -0.35V, revolving speed 1600rpm
The current density percent loss of catalyst platinum carbon.
Fig. 6 is the cyclic voltammetric song that 1-5 of the embodiment of the present invention prepares N doping mesoporous carbon spheres Nonmetal oxygen reduction catalyst
Line.
Fig. 7 be in revolving speed 1600rpm, embodiment 1-5 prepare N doping mesoporous carbon spheres Nonmetal oxygen reduction catalyst with
Business platinum carbon linear scan curve comparison figure.
Specific embodiment
Technical solution of the present invention is described in detail with reference to the accompanying drawings and examples, but invention be not limited to it is following
Embodiment.
Each embodiment the method in the present invention is conventional method unless otherwise instructed.The raw material are such as without spy
It does not mentionlet alone bright, can be commercially available from public commercial source.
The information of the model and manufacturer of instrument used in various embodiments of the present invention or equipment is as follows:
Air dry oven, model DHG-9920A, Shanghai Yiheng Scientific Instruments Co., Ltd, manufacturer；
Scanning electron microscope (SEM), model Phenom Pro X, the U.S., manufacturer；
Transmission electron microscope (TEM), model: JEM-2010HT, manufacturer: Jeol Ltd.；
X-ray photoelectron spectroscopy, model: AXIS UltraDLD, manufacturer: Japanese Shimadzu；
Electrochemical workstation, model: Autolab PGSTAT302N manufacturer: Switzerland ten thousand is logical.
In the embodiment of the present invention, the cyclic voltammetry curve of sample is in Autolab PGSTAT302N phone works station
It measures, specific test condition are as follows: under three-electrode system, using Ag/AgCl as reference electrode, platinum filament is to electrode, and load has catalysis
The glass-carbon electrode of agent is working electrode, scanning speed 10mV/s；The preparation process of working electrode are as follows: be dissolved in 5mg catalyst
In 1mL ethyl alcohol and 50 μ L Nafion (5% solution is bought in DuPont Corporation) mixed solution, 10 μ L drops are taken after ultrasonic disperse
It is added on glass-carbon electrode, after drying at room temperature, as working electrode.When carrying out cyclic voltammetry curve test, by nitrogen and oxygen
It each leads into 0.1M KOH electrolyte solution, to build nitrogen/oxygen atmosphere.Test before by electrode in electrolyte solution into
Then row 10 times circulations are tested with activated electrode.
In the embodiment of the present invention, the linear sweep voltammetry curve of sample is in Autolab PGSTAT302N phone works
It is measured in standing, test condition are as follows: under three-electrode system, using Ag/AgCl as reference electrode, platinized platinum is to electrode, and load has catalysis
The rotating disk electrode (r.d.e) of agent is working electrode, and 0.1M KOH is electrolyte solution, scanning speed 10mV/s；The system of working electrode
Standby process are as follows: 5mg catalyst is dissolved in 1mL ethyl alcohol and 50 μ LNafion (5% solution is bought in DuPont Corporation) mixing is molten
10 μ L are taken to be added drop-wise in rotating disk electrode (r.d.e) in liquid, after ultrasonic disperse, after drying at room temperature, as working electrode.It carries out linear
When scanning volt-ampere curve test, nitrogen and oxygen are each led into 0.1M KOH electrolyte solution, to build nitrogen/oxygen atmosphere
It encloses.Electrode is carried out to 10 circulations in electrolyte solution with activated electrode before test.When being tested under oxygen atmosphere, survey
Try linear sweep voltammetry curve of electrode under the conditions of different rotating speeds (400-2400rpm).
In the embodiment of the present invention, the chronoa mperometric plot of sample is in Autolab PGSTAT302N phone works station
It measures, test condition are as follows: under three-electrode system, using Ag/AgCl as reference electrode, platinized platinum is to electrode, and load has catalyst
Rotating disk electrode (r.d.e) is working electrode, and 0.1M KOH is electrolyte solution, scanning speed 10mV/s；The preparation of working electrode
Journey are as follows: 5mg catalyst is dissolved in 1mL ethyl alcohol and 50 μ LNafion (5% solution is bought in DuPont Corporation) mixed solution
In, take 10 μ L to be added drop-wise in rotating disk electrode (r.d.e) after ultrasonic disperse, after drying at room temperature, as working electrode.Chrono-amperometric is bent
The test condition of line are as follows: at constant potential -0.35V, revolving speed 1600rpm revolving speed, test electric current in 9000s and change with time
Situation.
Embodiment 1
By 0.4g polyacrylonitrile, 0.4g polyvinylpyrrolidone and 0.4g fumed silica are dissolved in 9g dimethyl jointly
In formamide, spinning is carried out after being stirred at normal temperature to solid all dissolution, electrostatic spinning voltage is 14kV, receives distance
15cm, flow velocity 0.1mL/h.Spinning is received with aluminium foil, the spinning after reception is put into tube furnace, it is pre- at 220 DEG C in air
Oxidation is down to room temperature in 2 hours, then after being carbonized 2 hours at nitrogen atmosphere, 800 DEG C, by products therefrom 2mol/L hydrogen-oxygen
Template is removed after changing sodium solution dipping stirring 4 hours.It is non-up to N doping mesoporous carbon spheres after being dried in vacuo 6 hours at 60 DEG C
Metal oxygen reduction catalyst.Know that the carbon ball of embodiment preparation has preferable spherical structure by Fig. 1,2, partial size is 2-7 μm.Figure
The nitrogen-doped carbon ball that the mesoporous curve of typical IV type demonstrates synthesis in 3 has good meso-hole structure.As shown in Figure 4, nitrogen is mixed
Only there are three types of element and carbon, nitrogen in miscellaneous carbon ball, and the content of oxygen is respectively 89.56%, 7.92% and 2.52%.As shown in Figure 5
After 9000s, which is left 92%, and business platinum carbon catalyst is 60%, shows that the catalyst has and is better than
The durability of business platinum carbon catalyst.As shown in Figure 6 when voltage is -0.19V, nitrogen-doped carbon ball has apparent hydrogen reduction
Energy.Fig. 7 is the linear scan curve graph of the catalyst and business Pt/C catalyst.The take-off potential of the catalyst be-
0.0816V differs only by 0.036V with business Pt/C, and half wave potential is -0.218V, and business platinum carbon catalyst is -0.188V, only phase
Poor 0.03V.Show that the catalyst has preferable hydrogen reduction performance.
Embodiment 2
By 0.5g polyacrylonitrile, 0.5g polyvinylpyrrolidone and 0.8g fumed silica are dissolved in 12g diformazan jointly
In base formamide, spinning is carried out after being stirred at normal temperature to solid all dissolution, electrostatic spinning voltage is 12kV, receives distance
15cm, flow velocity 0.05mL/h.Spinning is received with aluminium foil, the spinning after reception is put into tube furnace, at 220 DEG C of air atmosphere
Pre-oxidation is down to room temperature in 3 hours, then after being carbonized 2 hours at nitrogen atmosphere, 800 DEG C, by products therefrom 1mol/L hydrogen
Sodium hydroxide solution dipping removes template after stirring 6 hours.Up to N doping mesoporous carbon spheres after being dried in vacuo 8 hours at 40 DEG C
Nonmetal oxygen reduction catalyst.As shown in Figure 6 when voltage is -0.234V, nitrogen-doped carbon ball has apparent hydrogen reduction performance.
The take-off potential of the catalyst is known by the linear scan curve graph of catalyst under the embodiment in Fig. 7 and half wave potential be respectively-
0.157V and -0.355V shows that the catalyst has certain hydrogen reduction performance.
Embodiment 3
By 0.5g polyacrylonitrile, 0.5g polyvinylpyrrolidone and 1.2g fumed silica are dissolved in 15g diformazan jointly
In base formamide, spinning is carried out after being stirred at normal temperature to solid all dissolution, electrostatic spinning voltage is 15kV, receives distance
15cm, flow velocity 0.08mL/h.Spinning is received with aluminium foil, the spinning after reception is put into tube furnace, in air atmosphere, 210 DEG C
Lower pre-oxidation is down to room temperature in 2 hours, then after being carbonized 1 hour at nitrogen atmosphere, 850 DEG C, is with concentration by products therefrom
1mol/L sodium hydroxide solution dipping removes template after stirring 8 hours.Up to N doping after being dried in vacuo 6 hours at 60 DEG C
Mesoporous carbon spheres Nonmetal oxygen reduction catalyst.As shown in Figure 6 when voltage is -0.225V, nitrogen-doped carbon ball has apparent oxygen
Reducing property.The take-off potential and half-wave electricity of the catalyst are known by the linear scan curve graph of catalyst under the embodiment in Fig. 7
Position is respectively -0.091V and -0.226V, shows that the catalyst has certain hydrogen reduction performance.
Embodiment 4
By 0.5g polyacrylonitrile, 0.8g polyvinylpyrrolidone and 0.8g fumed silica are dissolved in 12g diformazan jointly
In base formamide, spinning is carried out after being stirred at normal temperature to solid all dissolution, electrostatic spinning voltage is 16kV, receives distance
15cm, flow velocity 0.1mL/h.Spinning is received with aluminium foil, the spinning after reception is put into tube furnace, at 220 DEG C of air atmosphere
Pre-oxidation is down to room temperature in 2 hours, then after being carbonized 3 hours at nitrogen atmosphere, 900 DEG C, is with concentration by products therefrom
2mol/L sodium hydroxide solution dipping removes template after stirring 6 hours.Up to N doping after being dried in vacuo 4 hours at 80 DEG C
Mesoporous carbon spheres Nonmetal oxygen reduction catalyst.As shown in Figure 6 when voltage is -0.212V, nitrogen-doped carbon ball has apparent oxygen
Reducing property.The take-off potential and half-wave electricity of the catalyst are known by the linear scan curve graph of catalyst under the embodiment in Fig. 7
Position is respectively -0.157V and -0.355V, shows that the catalyst has certain hydrogen reduction performance.
Embodiment 5
By 0.5g polyacrylonitrile, 0.5g polyvinylpyrrolidone and 0.6g fumed silica are dissolved in 12g diformazan jointly
In base formamide, spinning is carried out after being stirred at normal temperature to solid all dissolution, electrostatic spinning voltage is 18kV, receives distance
15cm, flow velocity 0.2mL/h.Spinning is received with aluminium foil, the spinning after reception is put into tube furnace, it is pre- at 210 DEG C in air
Oxidation is down to room temperature in 4 hours, with concentration is 2mol/ by products therefrom then after being carbonized 4 hours at nitrogen atmosphere, 700 DEG C
L sodium hydroxide solution dipping removes template after stirring 6 hours.It is mesoporous up to N doping after being dried in vacuo 5 hours at 70 DEG C
Carbon ball Nonmetal oxygen reduction catalyst.Known to 6 when voltage is -0.208V, nitrogen-doped carbon ball has apparent hydrogen reduction
Energy.Know that the take-off potential of the catalyst and half wave potential are distinguished by the linear scan curve graph of catalyst under the embodiment in Fig. 7
For -0.111V and -0.254V, show that the catalyst has certain hydrogen reduction performance.
Claims (7)
1. a kind of preparation method of N doping mesoporous carbon spheres Nonmetal oxygen reduction catalyst, which is characterized in that specific step is as follows:
1) polyacrylonitrile, polyvinylpyrrolidone and fumed silica are dissolved in jointly in dimethylformamide, at room temperature
It is uniformly mixed；
2) electrostatic spinning apparatus is added in mixed system, using aluminium foil as screen is received, carries out electrostatic spinning；
3) first the obtained product of step 2) is put into tube furnace, under air atmosphere, after being warming up to 200~250 DEG C, pre- oxygen
Change 1~4 hour, then in an inert atmosphere, be warming up at 700~950 DEG C and be carbonized 1~4 hour, sample exists after being finally carbonized
Dipping stirring removes silica in sodium hydroxide solution, obtains N doping mesoporous carbon spheres Nonmetal oxygen reduction catalyst.
2. preparation method according to claim 1, which is characterized in that in step 1), polyacrylonitrile, polyvinylpyrrolidone
Mass ratio with fumed silica is (2~5): (2~5): (2~10).
3. preparation method according to claim 1, which is characterized in that in step 1), fumed silica and dimethyl methyl
The mass ratio of amide is 1:10~1:20.
4. preparation method according to claim 1, which is characterized in that in step 2), spinning condition is 12~18kV of voltage,
Receive 15~20cm of distance, 0.05~5mL/h of flow velocity.
5. preparation method according to claim 1, which is characterized in that in step 3), the concentration of sodium hydroxide solution is 1~
5mol.L-1, dipping mixing time is 4-8 hours.
6. N doping mesoporous carbon spheres Nonmetal oxygen reduction catalyst made from a kind of preparation method according to claim 1.
7. a kind of application of N doping mesoporous carbon spheres Nonmetal oxygen reduction catalyst according to claim 1.
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| CN111048795A (en) * | 2019-11-29 | 2020-04-21 | 上海应用技术大学 | Cobalt-nitrogen co-doped mesoporous carbon sphere electrocatalyst and preparation method and application thereof |
| CN111864219A (en) * | 2020-07-08 | 2020-10-30 | 上海大学 | Silicon-doped iron-nitrogen/carbon composite catalyst, and preparation method and application thereof |
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| CN111864219A (en) * | 2020-07-08 | 2020-10-30 | 上海大学 | Silicon-doped iron-nitrogen/carbon composite catalyst, and preparation method and application thereof |
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