CN110492114A - A kind of N doping porous carbon oxygen reduction catalyst and its preparation method and application - Google Patents
A kind of N doping porous carbon oxygen reduction catalyst and its preparation method and application Download PDFInfo
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- CN110492114A CN110492114A CN201910770490.6A CN201910770490A CN110492114A CN 110492114 A CN110492114 A CN 110492114A CN 201910770490 A CN201910770490 A CN 201910770490A CN 110492114 A CN110492114 A CN 110492114A
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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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- 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
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Abstract
The present invention relates to a kind of N doping porous carbon oxygen reduction catalysts and its preparation method and application, belong to fuel cell catalyst materials field.A kind of preparation method of N doping porous carbon oxygen reduction catalyst, intermediate product is obtained by hydro-thermal reaction after polyvinylpyrrolidone and polyethylene oxide-polypropylene oxide-polyethylene oxide triblock copolymer (F127) are mixed, transparent membrane substance will be obtained after intermediate product drying；Transparent membrane substance is carbonized under a nitrogen atmosphere again, products therefrom washing, dry, grinding, both.The present invention prepares the easy to operate of nitrogen-doped nanometer Capsules shape porous carbon materials, and process is less, and equipment investment is few, reproducible, convenient for solving the problems, such as that large-scale production is difficult.
Description
Technical field
The present invention relates to a kind of N doping porous carbon oxygen reduction catalysts and its preparation method and application, belong to fuel cell
Catalyst material field.
Background technique
In recent years, energy shortage and environmental pollution are the two large problems of facing mankind, find a kind of alternative new energy
Very urgent, fuel cell has energy conversion rate height, advantages of environment protection as a kind of energy conversion device.Fuel electricity
The oxygen reduction reaction of pool cathode plays key effect in a fuel cell, since its slow dynamics Controlling step limits combustion
Expect the reaction speed of battery.Although traditional Pt sill is most practical, most effective elctro-catalyst in oxygen reduction reaction,
In fuel cell industries, they are by high cost and are easy the obstruction being poisoned.Therefore, exploitation it is cheap, efficiently, height endurability and
Stable elctro-catalyst becomes imperative research.
Doping hetero atom can destroy the electroneutral of carbon material, increase absorption position and the hydrogen reduction site of oxygen molecule.Therefore,
Heteroatom doping carbon material has received widespread attention.The radius of N is greater than carbon, and electronegativity is slightly less than carbon, and than phosphorus, sulphur etc., other are miscellaneous
Atom is easier and carbon combines.There are 5 electronics to contribute nitrogen with better electronics in exoelectron, this nitrogen source derives from pyrrole
Nitrogen is coughed up, pyrroles's nitrogen promotes significantly catalytic performance, more more significant than the hetero atoms improving performance such as phosphorus, sulphur.When N doped carbon, nitrogen
Interaction between atom and surrounding C atom leads to the redistribution of charge density and spin density, then in carbon material table
Face generates some active sites for having abundant electronics or lacking electronics.Therefore, doping nitrogen can improve the electronics knot of carbon material
Performance is closed, catalytic activity is improved.But N doping porous carbon oxygen reduction catalyst is tested mainly based on MgO hard template at present,
Preparation process is cumbersome, and needs to remove hard template.
Summary of the invention
In order to find alternative catalyst, solve that existing catalyst preparation is at high cost, the cumbersome problem of preparation process, this
Invention provides that a kind of preparation process is simple, preparation method of nitrogen-doped nanometer Capsules shape porous carbon oxygen reduction catalyst.
For achieving the above object, the invention adopts the following technical scheme:
One aspect of the present invention provides a kind of preparation method of N doping porous carbon oxygen reduction catalyst, by polyvinyl pyrrole
It is obtained after alkanone (PVP) and polyethylene oxide-polypropylene oxide-polyethylene oxide triblock copolymer mixing through hydro-thermal self assembly
Intermediate product will be carbonized after intermediate product drying, products therefrom washing, dry, grinding, both.
The dosage of polyvinylpyrrolidone described in above-mentioned preparation method is polyethylene oxide-polypropylene oxide-polycyclic oxygen
The 10%~30% of ethane triblock copolymer amount of substance.
Preferably, the dosage of the polyvinylpyrrolidone is that polyethylene oxide-polypropylene oxide-polyethylene oxide three is embedding
The 10% of section copolymer quality.
Hydro-thermal self-assembling reaction condition described in above-mentioned preparation method are as follows: 25~100 DEG C, heat preservation 2~for 24 hours.
In above-mentioned preparation method, Zn (OH) is added before hydro-thermal self-assembling reaction2, Zn (OH)2With polyethylene oxide-polycyclic oxygen
Propane-polyethylene oxide triblock copolymer mass ratio is 1~2:4.
In above-mentioned preparation method, the Carbonization Conditions are as follows: under nitrogen atmosphere, with 2 DEG C/min~5 DEG C/min heating rate
500~1000 DEG C are warming up to, cools to room temperature with the furnace after keeping the temperature 2~6h.
In above-mentioned preparation method, the washing are as follows: impregnated using 1~8mol/LHCl solution, 2500r/min~4000r/
It is centrifuged 5~10min with deionized water under min, then repeated centrifugation to neutrality uses dehydrated alcohol eccentric cleaning.
Preferably, HCl solution used is 2mol/LHCl solution.
Another aspect of the present invention provides a kind of N doping porous carbon oxygen reduction catalyst, and the catalyst is by above-mentioned preparation
Method is prepared, and the catalyst is the material with nano-hollow capsule-like structure, and specific surface area is 100~2000g/
m2。
Third aspect present invention provides above-mentioned N doping porous carbon oxygen reduction catalyst as fuel cell cathode catalyst
The application of agent material and catalyst carrier material.
The invention has the advantages that: the method for the present invention to select mature commercialization raw material from cost, and three block is total
C, H, O are contained only in polymer material, functional group only has hydroxyl, and the carbon source relatively friendly to environment, porous carbon shows nanometer sky
Heart-soothing capsule shape structure, due to its biggish specific surface area, it is easier to electrotransfer path be provided and oxygen absorbs site, introduce the miscellaneous original of N
After son, active site is increased, greatly promotes catalytic performance.
The use of catalyst material prepared by the method for the invention is three-dimensional porous shape high-specific surface area material, has good
Electrocatalysis characteristic, significantly reduce catalyst cost.
The present invention prepares that nitrogen-doped porous carbon material method is easy to operate, process is less, equipment investment is few, reproducible,
Convenient for solving mass production problem.
Detailed description of the invention
Fig. 1 is the phenogram of the embodiment of the present invention 1；It (a) is the catalysis of N doping porous carbon hydrogen reduction prepared by embodiment 1
The SEM image (scale 200nm) of agent material；Fig. 1 (b), (c) are that N doping porous carbon hydrogen reduction prepared by embodiment 1 is urged
The TEM image of agent material；Fig. 1 (d) is that the electronics of N doping porous carbon oxygen reduction catalyst material prepared by embodiment 1 spreads out
Penetrate figure；
Fig. 2 is N doping porous carbon oxygen reduction catalyst material prepared by comparative example and Examples 1 to 3 of the present invention
XRD spectra；
Fig. 3 is N doping porous carbon oxygen reduction catalyst material prepared by comparative example 1 and Examples 1 to 3 of the present invention
Raman spectrogram；
Fig. 4 is the full spectrum and C1s and N1s spectrogram of N doping porous carbon oxygen reduction catalyst material prepared by embodiment 1；Figure
The total spectrogram of 4 (a) XPS, Fig. 4 (b) C1s spectrogram, Fig. 4 (c) N1s spectrogram；
Fig. 5 is test result figure；Fig. 5 (a) is N doping porous carbon prepared by comparative example and the embodiment of the present invention 1~3
The polarization curve of the 1600rpm of oxygen reduction catalyst material, Fig. 5 (b) are the rotating disk test curves of embodiment 1, and Fig. 5 (c) is
The K-L curve of embodiment 1, Fig. 5 (d) are the cycle life curves of embodiment 2.
Specific embodiment
Following non-limiting embodiments can with a person of ordinary skill in the art will more fully understand the present invention, but not with
Any mode limits the present invention.
Test method described in following embodiments is unless otherwise specified conventional method；The reagent and material, such as
Without specified otherwise, commercially obtain.
Comparative example
1) polyethylene oxide-polypropylene oxide-polyethylene oxide triblock copolymer (referred to as: F127) for taking 4g, is added
The deionized water of 100ml, stirs evenly, and obtains clear transparent solutions.
2) 1.6g zinc hydroxide is added in solution, moves into reaction kettle, setting hydrothermal temperature is 80 DEG C, keeps the temperature 12h, then
It takes out, dries at 60 DEG C for 24 hours to transparent membrane substance.
3) transparent membrane substance is subjected to carbonization treatment, carbodiimide procedure are as follows: from room temperature with 2 in the tube furnace for being connected with nitrogen
DEG C/heating rate of min is warming up to 700 DEG C, keep the temperature 3h, after cool to room temperature with the furnace, take out；2mol/LHCl solution is used first
It impregnates, is centrifuged 5min with deionized water under 4000r/min, then repeated centrifugation to neutrality uses dehydrated alcohol eccentric cleaning, do
It is dry, grinding.
Embodiment 1
1) F127 for taking 4g is added the deionized water of 100ml, stirs evenly, obtains clear transparent solutions.
2) 10% polyvinylpyrrolidone (PVP) of F127 mass is added, i.e. 0.4g PVP is stirred evenly, must be clarified
Clear solution.
3) 1.6g zinc hydroxide is added in solution, moves into reaction kettle, setting hydrothermal temperature is 80 DEG C, keeps the temperature 12h, then
It takes out, dries at 60 DEG C for 24 hours to transparent membrane substance.
4) transparent membrane substance is subjected to carbonization treatment, carbodiimide procedure are as follows: from room temperature with 2 in the tube furnace for being connected with nitrogen
DEG C/heating rate of min is warming up to 700 DEG C, keep the temperature 3h, after cool to room temperature with the furnace, take out；2mol/LHCl solution is used first
It impregnates, is centrifuged 5min with deionized water under 4000r/min, then repeated centrifugation to neutrality uses dehydrated alcohol eccentric cleaning, do
It is dry, grinding.
Embodiment 2
1) F127 for taking 4g is added the deionized water of 100ml, stirs evenly, obtains clear transparent solutions.
2) 20% polyvinylpyrrolidone (PVP) of F127 mass is added, i.e. 0.8g PVP is stirred evenly, must be clarified
Clear solution.
3) 1.6g zinc hydroxide is added in solution, moves into reaction kettle, setting hydrothermal temperature is 80 DEG C, keeps the temperature 12h, then
It takes out, dries at 60 DEG C for 24 hours to transparent membrane substance.
4) transparent membrane substance is subjected to carbonization treatment, carbodiimide procedure are as follows: from room temperature with 2 in the tube furnace for being connected with nitrogen
DEG C/heating rate of min is warming up to 700 DEG C, keep the temperature 3h, after cool to room temperature with the furnace, take out；2mol/LHCl solution is used first
It impregnates, is centrifuged 5min with deionized water under 4000r/min, then repeated centrifugation to neutrality uses dehydrated alcohol eccentric cleaning, do
It is dry, grinding.
Embodiment 3
1) F127 for taking 4g is added the deionized water of 100ml, stirs evenly, obtains clear transparent solutions.
2) 30% polyvinylpyrrolidone (PVP) of F127 mass is added, i.e. 1.2g PVP is stirred evenly, must be clarified
Clear solution.
3) 1.6g zinc hydroxide is added in solution, moves into reaction kettle, setting hydrothermal temperature is 80 DEG C, keeps the temperature 12h, then
It takes out, dries at 60 DEG C for 24 hours to transparent membrane substance.
4) transparent membrane substance is subjected to carbonization treatment, carbodiimide procedure are as follows: from room temperature with 2 in the tube furnace for being connected with nitrogen
DEG C/heating rate of min is warming up to 700 DEG C, keep the temperature 3h, after cool to room temperature with the furnace, take out；2mol/LHCl solution is used first
It impregnates, is centrifuged 5min with deionized water under 4000r/min, then repeated centrifugation to neutrality uses dehydrated alcohol eccentric cleaning, do
It is dry, grinding.
Example effects: in order to probe into the shape characteristic and chemical property that prepare nitrogen-doped carbon catalyst, using SEM,
The means such as XRD, XPS, Raman carry out physical characterization to the product of preparation and that product is prepared into electrode test is electrochemical accordingly
Learn performance.
Fig. 1 (a) is the SEM photograph (scale 200nm) of nitrogen-doped carbon catalyst prepared by embodiment 1, from Fig. 1 (a)
It can be seen that being nanometre glue cryptomere porous carbon under 50000 times of amplification factors in SEM photograph；It can from Fig. 1 (b) (c) TEM photo
Internal out is hollow structure, and wall thickness is about 5nm, and Fig. 1 (d) is its electronic diffraction ring, illustrates degree of graphitization height.
Fig. 2 (a) show the XRD spectra of nitrogen-doped carbon catalyst prepared by comparative example and Examples 1 to 3,2 θ=
29 ° of correspondence (002) crystal faces, are graphitized carbons, and polyvinylpyrrolidone doping is different, peak it is of different sizes, adding proportion is
When 10%, peak is maximum.Illustrate that C-N-10% degree of graphitization is high, there is preferable electric conductivity.Raman spectrogram is as shown in Figure 3.D
Peak is present in 1350cm-1, and the peak G is present in 1580cm-1.There are preferable degree of imperfection and stone it can be seen from the peak D and the peak G
Blackization degree.
Shown in the full spectrum and C1s and N1s spectrogram such as Fig. 4 (a)~(c) of 1 resulting materials of embodiment.It can be defined from Fig. 4 (a)
It was found that there is C, N element exists, and can analyze sp3-C in the spectrogram of C1s, and sp2-C, C-N exist.In N1s spectrogram, Ke Yifen
It is precipitated with pyrroles's nitrogen, pyridine nitrogen, graphite nitrogen exists, and pyrroles's nitrogen accounting is larger, shows that N has been doped in carbon.
The catalyst of preparation is coated on glassy carbon electrode, cyclic voltammetric, polarization curve are carried out in 0.1M KOH solution
And stability test, test results are shown in figure 5.
It can be seen that from Fig. 5 (a), wherein F127 is molecular weight Mn=12600g/mol sample, is added without Zn (OH)2,
It is added without the carbon material that the pure material high temperature of PVP generates.In the polarization curve of the 1600rpm of the catalyst material of different proportion,
Embody optimal performance when the PVP ratio of addition is 10%: good take-off potential, good limiting current density are (real
Apply example 1), from Fig. 5 (b) as can be seen that embodiment 1 catalyst with rotating disk revolution increase, limiting current density also with
Increase, illustrate that diffusion layer is very thin, illustrate have many active sites.Fig. 5 (c) is to shift electron number under each current potential, then
Calculating transfer electron number according to K-L formula is 3.98, is conducive to four electronics transfers, is suitable for oxygen reduction catalyst.It can by Fig. 5 (d)
To find out, the polarization curve decaying tested after the circle of circulation 2000 and 5000 circles seldom, illustrates that stability is fine.
For any person skilled in the art, without departing from the scope of the technical proposal of the invention, all
Many possible changes and modifications are made to technical solution of the present invention using the technology contents of the disclosure above, or are revised as equivalent
The equivalent embodiment of variation.Therefore, anything that does not depart from the technical scheme of the invention, according to the technical essence of the invention to
Any simple modifications, equivalents, and modifications that upper embodiment is done should all still fall within the range of technical solution of the present invention protection
It is interior.
Claims (9)
1. a kind of preparation method of N doping porous carbon oxygen reduction catalyst, it is characterised in that: by polyvinylpyrrolidone and gather
Obtain intermediate product through hydro-thermal self assembly after the mixing of oxide-polypropylene oxide-polyethylene oxide triblock copolymer, will in
Between product it is dry after be carbonized, products therefrom washing, dry, grinding, both.
2. a kind of preparation method of N doping porous carbon oxygen reduction catalyst according to claim 1, it is characterised in that: institute
The dosage for stating polyvinylpyrrolidone is polyethylene oxide-polypropylene oxide-polyethylene oxide triblock copolymer amount of substance
10%~30%.
3. a kind of preparation method of N doping porous carbon oxygen reduction catalyst according to claim 2, it is characterised in that: institute
The dosage for stating polyvinylpyrrolidone is polyethylene oxide-polypropylene oxide-polyethylene oxide triblock copolymer amount of substance
10%.
4. a kind of preparation method of N doping porous carbon oxygen reduction catalyst according to claim 1, it is characterised in that: institute
State hydro-thermal self-assembling reaction condition are as follows: 25~100 DEG C, heat preservation 2~for 24 hours.
5. a kind of preparation method of N doping porous carbon oxygen reduction catalyst according to claim 1, which is characterized in that water
Zn (OH) is added before hot self-assembling reaction2, Zn (OH)2With polyethylene oxide-polypropylene oxide-polyethylene oxide triblock copolymer
The mass ratio of object is 1~2:4.
6. a kind of preparation method of N doping porous carbon oxygen reduction catalyst according to claim 1, which is characterized in that institute
State Carbonization Conditions are as follows: under nitrogen atmosphere, 500~1000 DEG C are warming up to 2 DEG C/min~5 DEG C/min heating rate, heat preservation 2~
Cool to room temperature after 6h with the furnace.
7. a kind of preparation method of N doping porous carbon oxygen reduction catalyst according to claim 1, which is characterized in that institute
State washing are as follows: impregnated using 1~8mol/LHCl solution, under 2500r/min~4000r/min with deionized water centrifugation 5~
Then 10min, repeated centrifugation to neutrality use dehydrated alcohol eccentric cleaning.
8. a kind of N doping porous carbon oxygen reduction catalyst, which is characterized in that the catalyst is by any one of claim 1~7
The method is prepared.
9. N doping porous carbon oxygen reduction catalyst is as fuel battery cathod catalyst material and catalyst described in claim 8
The application of carrier material.
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