CN109244490A - A kind of preparation method of cementite@nitrogen-doped carbon nanocatalyst - Google Patents
A kind of preparation method of cementite@nitrogen-doped carbon nanocatalyst Download PDFInfo
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- CN109244490A CN109244490A CN201811062331.2A CN201811062331A CN109244490A CN 109244490 A CN109244490 A CN 109244490A CN 201811062331 A CN201811062331 A CN 201811062331A CN 109244490 A CN109244490 A CN 109244490A
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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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
- D01F9/08—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
- D01F9/12—Carbon filaments; Apparatus specially adapted for the manufacture thereof
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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 cementite@nitrogen-doped carbon nano wire and preparation method thereof with excellent electrocatalytic oxidation reduction activation, belongs to new energy materials applied technical field.Its preparation process is as follows: utilizing electrostatic spinning technique, the precursor solution of preparation is spun into nano wire；Under certain conditions, manufactured nano wire is heat-treated, obtains cementite@nitrogen-doped carbon nano-wire catalyst.Cementite@nitrogen-doped carbon nano-wire catalyst prepared by the present invention not only has the high half-wave hydrogen reduction current potential of 0.845V, more than the limiting current density of business platinum carbon, but also has fabulous stability.Preparation process of the present invention is simple, and technological parameter is adjustable, at low cost, and yield is high, excellent product performance, is very suitable for commercialization and promotes and applies.
Description
Technical field
The present invention relates to hydrogen reduction electro-catalysis fuel cell fields, and in particular, to a kind of oxygen reduction electro-catalyst use
The method of electrostatic spinning technique preparation.
Background technique
Hydrogen fuel cell belongs to novel energy resource material technology, has a very wide application prospect, but currently commercially used
Noble metal catalyst has the shortcomings that at high cost, durability is poor.Now widely used Pt/C catalyst is deposited using carbon dust as carrier
In poorly conductive, easy to reunite, perishable problem.In view of the above problems, the present invention is prepared for comparing table using electrostatic spinning technique
The catalyst that area is big, porosity is high, the nano-sized carbon of good conductivity is carrier.Electrostatic spinning is using polymer solution fluid in height
The effect being atomized in pressure electrostatic field, solution form jet stream after being atomized, and are collected device collection, and be finally solidified into.It utilizes
Method of electrostatic spinning selects suitable polymer solution, catalyst material can be prepared into pattern, this method yield easily
It is high, it is very suitable to industrial production.This technology shows the advantage of some protrusions on the material of preparation combinate form looks, than strictly according to the facts
Test that cost is relatively low, the membrane material specific surface of preparation is big, porosity is high, good dispersion, pattern is uniform, mechanical property is strong and tests
Journey operating procedure is simple, and the yield height etc. of catalyst, is suitable for various types of materials and prepares, and is very suitable for commercialization and promotes
Using.
Summary of the invention
The problems such as existing base metal elctro-catalyst oxygen reduction activity and low stability, the present invention use electrostatic spinning
Technical method prepares a kind of cementite@nitrogen-doped carbon nano-wire catalyst.
To achieve the above object, the present invention specifically uses following technical scheme:
A kind of preparation method of cementite@nitrogen-doped carbon nano-wire catalyst.Characterized by comprising the following steps:
(1) preparation of cementite@nitrogen-doped carbon nanowire precursor solution: a certain amount of DMF of accurate measuring is placed in burning
Cup in and magnetic agitation, a certain amount of PAN is added in whipping process, after PAN is completely dissolved, a certain proportion of acetyl is added
Acetone iron and DIPA, and stir until being completely dissolved.
(2) preparation of cementite@nitrogen-doped carbon nanowire precursor: a certain amount of above-mentioned (1) is drawn using syringe and is matched
The solution of the cementite@nitrogen-doped carbon nanowire precursor of system, using electrostatic spinning machine spinning, using roller reception device, and
Aluminium foil is pasted in cylinder surface, for receiving, by adjusting drum rotation speed, syringe needle is at a distance from roller, and electrostatic spinning machine is just
Negative voltage, the speed for promoting pump to push away, to realize the precursor preparation of cementite@nitrogen-doped carbon nano wire.By sample after the completion of preparation
Product are taken off, and drying is dried.
(3) the presoma pre-oxidation of cementite@nitrogen-doped carbon nano wire: by cementite@N doping obtained in above-mentioned (2)
The presoma of carbon nanocoils is put into crucible, is placed in Muffle furnace later, is pre-oxidized to obtain pre- oxygen under conditions set
The cementite@nitrogen-doped carbon nano wire of change.
(4) cementite@nitrogen-doped carbon nano wire is carbonized: by the cementite@nitrogen-doped carbon of above-mentioned (3) obtained pre-oxidation
Nano wire is put into tube furnace, and under the temperature and time of setting, nitrogen atmosphere is heat-treated to obtain cementite@nitrogen-doped carbon nano wire
Catalyst.
(5) it sample: takes out obtained sample in part above-mentioned (4) and is put into agate mortar, be fully ground into and urged
Agent sample.A certain amount of above-mentioned catalyst is taken, quantitative, special ratios Nafion, the mixed solution of dehydrated alcohol are put into
In, ultrasonic treatment after a certain period of time, obtains finely dispersed catalyst slurry.
(6) hydrogen reduction is tested: before electrode preparation, being polished glassy carbon electrode surface with the aluminium oxide of partial size 50nm, then
A certain amount of catalyst slurry is measured with liquid-transfering gun, uniformly drops on glass-carbon electrode, and make its natural air drying, is prepared
Test electrode.Test electrode is connected to electrochemical workstation, carries out electrochemical catalysis performance test under certain condition.
(7) it is characterized using the sample that scanning electron microscope (SEM) prepares step (4), it was demonstrated that its pattern is one
Wiener rice noodles.See attached drawing one.
(8) object phase and constituent analysis are carried out using sample of the XRD technical testing to preparation, sees attached drawing two.
Compared with prior art, the present invention has the following advantages that and excellent effect:
1 present invention can be directly realized by metal ion using electrostatic spinning technique and be uniformly dispersed in carbon surface or uniformly coat
In carbon, preparation method simple process is easily operated, and repeatability is high, can be used for large-scale commercial production.
2 present invention are directly loaded in base metal iron on carbon, have 320.6m2The high-specific surface area of/g, increases work
Property site, improves the oxygen reduction activity and stability of cementite@nitrogen-doped carbon nano-wire catalyst, hydrogen reduction half wave potential
Very close to business platinum carbon, Limited diffusion current density is greater than business platinum carbon, and performance is more excellent.
Catalyst prepared by 3 present invention has fabulous stability compared with business platinum carbon.After polarization in 10000 seconds,
The current density of the ORR of prepared catalyst is not lost, and under the same conditions, the loss of business Pt/C is up to 16%.
4 the present invention can match in excellence or beauty in oxygen reduction activity and platinum carbon, carrying current is bigger, stability more preferably in the case of, make
Standby cost base metal iron is far below widely used business platinum carbon, is very suitable for commercialization and promotes and applies.
Detailed description of the invention
Figure one is the SEM figure of cementite@nitrogen-doped carbon nano-wire catalyst prepared by embodiment 3.
Figure two is the XRD diagram of cementite@nitrogen-doped carbon nano-wire catalyst prepared by embodiment 3.
Figure three is the hydrogen reduction curve of cementite@nitrogen-doped carbon nano-wire catalyst prepared by embodiment 3.Embodiment 1,2
There is similar hydrogen reduction current potential with example 3.
Figure four is the LSV curve of cementite@nitrogen-doped carbon nano-wire catalyst prepared by embodiment 3.
Figure five is the K-L curve graph of cementite@nitrogen-doped carbon nano-wire catalyst prepared by embodiment 3.
Figure six is the I-T curve of cementite@nitrogen-doped carbon nano-wire catalyst prepared by embodiment 3, embodiment 1,2 and example
3 stability having the same.
Specific embodiment
Substantive content of the invention is further illustrated with example with reference to the accompanying drawing, but the contents of the present invention are not limited to
This.
Embodiment 1:
A kind of preparation method of cementite@nitrogen-doped carbon nano-wire catalyst is to realize according to the following steps in this embodiment
:
(1) preparation of cementite@nitrogen-doped carbon nanowire precursor solution: the DMF of accurate measuring 15mL is placed in beaker
In and magnetic agitation, the PAN being added in whipping process, after PAN is completely dissolved, be added 0.45g ferric acetyl acetonade and
The DIPA of 80mg, and stir until being completely dissolved.
(2) precursor preparation of cementite@nitrogen-doped carbon nano wire: above-mentioned (1) prepared carbon is drawn using syringe
Change iron@carbon matrix precursor, using electrostatic spinning machine, pastes aluminium foil using roller reception device, and in cylinder surface, for receiving,
By adjusting drum rotation speed 20rpm, syringe needle and roller distance 15cm, the positive voltage of electrostatic spinning machine is 7KV, negative voltage is-
5KV, the speed 0.02mm/min for promoting pump to push away, to realize the preparation of cementite@carbon nanometer presoma.By sample after the completion of preparation
It takes off, dries drying
(3) pre-oxidation of the presoma of cementite@nitrogen-doped carbon nano wire: cementite@nitrogen obtained in above-mentioned (2) is mixed
Miscellaneous carbon nanocoils are put into crucible, are put into Muffle furnace later, and temperature is 280 DEG C, and heating rate is 1 DEG C/min, soaking time
For 1h, the cementite@nitrogen-doped carbon nanowire precursor pre-oxidized.
(4) cementite@nitrogen-doped carbon nano wire is carbonized: above-mentioned (3) obtained sample is put into tube furnace, nitrogen atmosphere
Under, 900 DEG C, heating rate is 5 DEG C/min, soaking time 1h, obtains cementite@nitrogen-doped carbon nano-wire catalyst.
Embodiment 2:
A kind of preparation method of cementite@nitrogen-doped carbon nano-wire catalyst is to realize according to the following steps in this embodiment
:
(1) precursor solution of cementite@nitrogen-doped carbon nano wire is prepared: the DMF of accurate measuring 15mL is placed in beaker
In and magnetic agitation, the PAN being added in whipping process, after PAN is completely dissolved, be added 0.45g ferric acetyl acetonade and
The DIPA of 100mg, and stir until being completely dissolved.
(2) preparation of cementite@nitrogen-doped carbon nanowire precursor: above-mentioned (1) prepared carbon is drawn using syringe
Change iron@carbon matrix precursor, using electrostatic spinning machine, pastes aluminium foil using roller reception device, and in cylinder surface, for receiving,
By adjusting drum rotation speed 20rpm, syringe needle and roller distance 15cm, the positive voltage of electrostatic spinning machine is 7KV, negative voltage is-
5KV, the speed 0.02mm/min for promoting pump to push away, to realize the precursor preparation of cementite@carbon nanometer.By sample after the completion of preparation
Dry drying.
(3) the presoma pre-oxidation of cementite@nitrogen-doped carbon nano wire: by cementite@N doping obtained in above-mentioned (2)
The presoma of carbon nanocoils is put into crucible, is put into Muffle furnace later, and temperature is 280 DEG C, and heating rate is 1 DEG C/min, is protected
The warm time is 1h, the cementite@nitrogen-doped carbon nanowire precursor pre-oxidized.
(4) cementite@nitrogen-doped carbon nano wire is carbonized: above-mentioned (3) obtained sample is put into tube furnace, nitrogen atmosphere
Under, 900 DEG C, heating rate is 5 DEG C/min, soaking time 1h, obtains cementite@nitrogen-doped carbon nano-wire catalyst.
Embodiment 3:
A kind of preparation method of cementite@nitrogen-doped carbon nano-wire catalyst is to realize according to the following steps in this embodiment
:
(1) precursor solution of cementite@nitrogen-doped carbon nano wire is prepared: the DMF of accurate measuring 15mL is placed in beaker
In and magnetic agitation, the ferric acetyl acetonade of 0.45g is added after PAN is completely dissolved in the PAN being slowly added in whipping process
It with the DIPA of 120mg, and stirs until be completely dissolved, obtains uniform solution.
(2) precursor preparation of cementite@nitrogen-doped carbon nano wire: above-mentioned (1) prepared carbon is drawn using syringe
Change iron@carbon matrix precursor solution, using electrostatic spinning machine, aluminium foil is pasted using roller reception device, and in cylinder surface, for connecing
It receives, by adjusting drum rotation speed 20rpm, syringe needle and roller distance 15cm, the positive voltage of electrostatic spinning machine are 7KV, negative voltage
For -5KV, the speed 0.02mm/min for promoting pump to push away, to realize the precursor preparation of cementite@carbon nanometer.It will after the completion of preparation
Sample is taken off, and drying is dried.
(3) the presoma pre-oxidation of cementite@nitrogen-doped carbon nano wire: by cementite@N doping obtained in above-mentioned (2)
The presoma of carbon nanocoils is put into crucible, is put into Muffle furnace later, and temperature is 280 DEG C, and heating rate is 1 DEG C/min, is protected
The warm time is 1h, the cementite@nitrogen-doped carbon nanowire precursor pre-oxidized.
(4) cementite@nitrogen-doped carbon nano wire is carbonized: above-mentioned (3) obtained sample is put into tube furnace, nitrogen atmosphere
Under, 900 DEG C, heating rate is 5 DEG C/min, soaking time 1h, obtains cementite@nitrogen-doped carbon nano-wire catalyst.
Claims (7)
1. a kind of cementite@nitrogen-doped carbon nano wire (Fe3C@NCF) catalyst preparation method.It is characterised in that it includes following
Step:
(1) preparation of cementite@nitrogen-doped carbon nanowire precursor solution: a certain amount of N-N dimethylformamide of accurate measuring
(DMF) it is placed in beaker simultaneously magnetic agitation, a certain amount of polyacrylonitrile (PAN) is added in whipping process, when PAN is completely molten
A certain proportion of ferric acetyl acetonade and diisopropyl azo-2-carboxylic acid (DIPA) is added in Xie Hou, and stirring is until be completely dissolved.
(2) precursor preparation of cementite@nitrogen-doped carbon nano wire: it is prepared that a certain amount of above-mentioned (1) is drawn using syringe
Cementite@carbon matrix precursor solution pastes aluminium foil using roller reception device, and in cylinder surface using electrostatic spinning machine spinning,
For receiving；By adjusting drum rotation speed, syringe needle is at a distance from roller, the positive and negative voltage of electrostatic spinning machine, and pump is promoted to promote
Speed realizes the preparation of cementite@nitrogen-doped carbon nano wire.Sample is taken off after the completion of preparation, dries drying.
(3) the presoma pre-oxidation of cementite@nitrogen-doped carbon nano wire: cementite@nitrogen-doped carbon obtained in above-mentioned (2) is received
Rice noodles presoma is put into crucible, is placed in Muffle furnace, under the temperature and time of setting, is carried out calcining pre-oxidation.
(4) cementite@nitrogen-doped carbon nano wire is carbonized: above-mentioned (3) obtained cementite@nitrogen-doped carbon nano wire is put into pipe
In formula furnace, under the temperature of setting, soaking time, heating rate and nitrogen atmosphere, carbonization obtains cementite@nitrogen-doped carbon nanometer
Line catalyst.
(5) it sample: takes out obtained sample in above-mentioned (4) and is put into agate mortar, be fully ground into powder, obtain catalyst
Sample.A certain amount of above-mentioned catalyst is taken, is put into the Nafion of special ratios and a certain amount of solution of ethyl alcohol, it is sufficiently ultrasonic to obtain
To finely dispersed catalyst slurry.
(6) hydrogen reduction is tested: before electrode preparation, being polished glassy carbon electrode surface with the aluminium oxide of partial size 50nm, then with shifting
Liquid rifle measures a certain amount of above-mentioned (5) obtained catalyst slurry, uniformly drops on the glass-carbon electrode of diameter 4mm, its rear nature
It air-dries, the test electrode prepared.Test electrode is connected to electrochemical workstation, carries out electrochemistry under certain condition
Catalytic performance test.
2. a kind of preparation method of cementite@nitrogen-doped carbon nano-wire catalyst according to claim 1.Its feature exists
Polyvinyl alcohol (PVA) can be used in the polyacrylonitrile (PAN) used in the step (1), and polyvinylpyrrolidone (PVP) is replaced
Generation, the amount of used ferric acetyl acetonade are 0.2g~1g, can be replaced with iron chloride, the amount of used DIPA be 50mg~
The amount of 120mg, used DMF are that 10mL~20mL, used PAN or PVA and PVP are 0.5g~2g.
3. a kind of preparation method of cementite@nitrogen-doped carbon nano-wire catalyst according to claim 1.Its feature exists
It is 20rpm~40rpm in the step (2) electrostatic spinning drum rotation speed, syringe needle is 15cm~20cm, negative pressure at a distance from roller
For -4KV~-5KV, positive pressure is 8KV~12KV, promotes pump to push away speed within the scope of 0.015mm~0.025mm/min, temperature 25
DEG C, humidity is 20%~28%.
4. a kind of preparation method of cementite@nitrogen-doped carbon nano-wire catalyst according to claim 1.Its feature exists
It is 200 DEG C~300 DEG C in the step (3) Muffle furnace Pre oxidation, heating rate is 1 DEG C/min~5 DEG C/min, when heat preservation
Between be 1h~3h.
5. a kind of preparation method of cementite@nitrogen-doped carbon nano-wire catalyst according to claim 1.Its feature exists
It is 700 DEG C~1000 DEG C in the sintering carburizing temperature of the step (4) tube furnace, heating rate is 2 DEG C/min~5 DEG C/min.
6. a kind of preparation method of cementite@nitrogen-doped carbon nano-wire catalyst according to claim 1.Its feature exists
In the step (5) sample: it is fully ground gained sample, takes the catalyst of 5mg, the Nafion solution of the 5wt.% of 50 μ L, 600
The dehydrated alcohol of μ L, wiring solution-forming obtain finely dispersed catalyst slurry after sonicated 2 hours.
7. a kind of preparation method of cementite@nitrogen-doped carbon nano-wire catalyst according to claim 1.Its feature exists
It is 50mv/sec in the step (6) cyclic voltammetry (CV) sweep speed, linear sweep voltammetry (LSV) sweep speed is
5mv/sec, disk electrode revolving speed are 800rpm~2000rpm.
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Cited By (3)
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| CN110010916A (en) * | 2019-04-18 | 2019-07-12 | 江苏师范大学 | A kind of preparation method of efficient nitrogen-doped carbon nano wire fuel-cell catalyst |
| CN112652780A (en) * | 2020-12-15 | 2021-04-13 | 河南师范大学 | Fe/Fe3Preparation method of C nano-particle loaded porous nitrogen-doped carbon-based oxygen reduction catalyst |
| US11732370B2 (en) | 2020-07-23 | 2023-08-22 | Shaanxi University Of Science & Technology | Core-shell FE2P@c-FE3C electrocatalyst and preparation method and application thereof |
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