CN109103466A - A kind of molybdenum dioxide -- oxygen reduction catalyst of carbon nanocoils and its preparation method and application - Google Patents
A kind of molybdenum dioxide -- oxygen reduction catalyst of carbon nanocoils and its preparation method and application Download PDFInfo
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- CN109103466A CN109103466A CN201810797224.8A CN201810797224A CN109103466A CN 109103466 A CN109103466 A CN 109103466A CN 201810797224 A CN201810797224 A CN 201810797224A CN 109103466 A CN109103466 A CN 109103466A
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- spinning
- oxygen reduction
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- carbon nanocoils
- reduction catalyst
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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
- H01M4/9016—Oxides, hydroxides or oxygenated metallic salts
- H01M4/9025—Oxides specially used in fuel cell operating at high temperature, e.g. SOFC
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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
-
- 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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- 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
Abstract
The invention belongs to fuel-cell catalyst preparation technical fields, specifically disclose a kind of molybdenum dioxide -- the preparation method of the oxygen reduction catalyst of carbon nanocoils.Specific steps include: that ammonium molybdate is dissolved in the in the mixed solvent that solubilizer and solvent configure in proportion, and the carbon nanocoils containing ammonium molybdate are prepared by way of electrostatic spinning, and above-mentioned catalyst then can be obtained using Muffle furnace and the heating of tube furnace process control.The catalyst morphology that the invention is prepared is excellent, and nanowire diameter is uniform, purity is high, has good catalytic action in hydrogen reduction chemical reaction, and poison ability with intermediates such as good anti-CO.
Description
Technical field
The present invention is in fuel-cell catalyst field, and specifically a kind of molybdenum dioxide -- the hydrogen reduction of carbon nanocoils is urged
Agent and its preparation method and application.
Background technique
The chemical energy of fuel can be converted into electric energy by fuel cell, and being described as by U.S.'s Time is " 21 century
Mostly important new energy technology ".Wherein, elctro-catalyst is the material of most critical in fuel cell module, to the performance of battery,
Stability and cost have great influence.Currently, fuel-cell catalyst is still but the earth based on platinum base nano material
The content of upper platinum is limited, and research and development non-precious metal catalyst has been the common recognition of current academia.
The research of current non-precious metal catalyst is concentrated mainly on Fe, Co, Ni, but even for the ORR performance study of Mo
Seldom, but have research surface its with certain catalytic activity, there is actual researching value.
Summary of the invention
Aiming at the problems existing in the prior art, the present invention is successfully prepared a kind of titanium dioxide by electrostatic spinning technique
The oxygen reduction catalyst of molybdenum -- carbon nanocoils.
A kind of preparation method of the oxygen reduction catalyst of molybdenum dioxide -- carbon nanocoils, comprising the following steps:
(1) solubilizer is dissolved in solvent A, is transferred in the container of sealing, be placed on magnetic stirring apparatus and stir, stirring speed
Rate is 400-600rpm, and whipping temp is 40-50 DEG C, to liquid agitation in container to colorless and transparent, obtains mixed solvent；
(2) ammonium molybdate is dissolved in the in the mixed solvent of step (1) preparation, is transferred in the container of sealing, is placed in magnetic force and stirs
It mixes and is stirred on device, stirring rate 480-540rpm, whipping temp is 45-55 DEG C, the Portugal being stirred until homogeneous to solution in container
Grape wine and women-sensual pursuits, obtains solution；
(3) solution obtained by step (2) is transferred in the dedicated spinning cylinder in electrospinning device, adjusts spinning and sets
Standby parameter, can start spinning；After spinning, gained spinning is placed in baking oven and is dried,.
(4) it pre-oxidizes: the spinning after step (3) drying is placed in Muffle furnace, process control is carried out to temperature, realizes and spins
The heating pre-oxidation of silk, the spinning after pre-oxidation are rendered as sepia bulk；
(5) it is sintered: the spinning after step (4) resulting pre-oxidation is placed in progress process control heating in tube furnace, with
Make its carbonization, final catalyst can be obtained.
In step (1), the solubilizer is PVP K30 or polyacrylonitrile；Solvent A is N, N- dimethyl methyl
Amide, ethyl alcohol or ultrapure water；Solubilizer and solvent A mass ratio are 1:20-13:100.
In step (2), ammonium molybdate and mixed solvent mass ratio are 1:100-2:25.
In step (3), spinning collection device is dedicated masking foil；It is No. 17-21 that used syringe needle, which is arranged, in electrostatic spinning
Syringe needle, pushing away speed is 0.015mm/min-0.032mm/min, and temperature is 28 DEG C -35 DEG C, humidity 30%-50%, collects distance and is
14cm -18cm。
In step (3), the condition of drying are as follows: temperature is 55 DEG C -65 DEG C, humidity 35%, and the time is 10-12 hours.
In step (4), Muffle furnace heating rate is 0.5 DEG C/min-1.5 DEG C/min, and the temperature of pre-oxidation is 235 DEG C -285
DEG C, soaking time 60min-130min is pre-oxidized in air atmosphere.
In step (5), tube furnace heating rate is 4 DEG C/min-5.5 DEG C/min, and the temperature of carbonization is 750 DEG C -900 DEG C,
Soaking time is 60min-150min, is sintered in the case where nitrogen is protective gas, it is≤0.05L/min that nitrogen, which is passed through rate,.
By molybdenum dioxide prepared by the present invention -- the oxygen reduction catalyst of carbon nanocoils is used for Proton Exchange Membrane Fuel Cells
Cathodic oxygen reduction.
Catalyst morphology and crystal structure characterize products therefrom of the present invention using scanning electron microscope, it was demonstrated that institute
Catalyst is prepared with the distribution situation of uniform nanowire structure and nanoparticle in nano wire.
Electrocatalysis characteristic characterization: the electrocatalysis characteristic of electrochemical workstation evaluation prepared catalyst is utilized.
The invention has the benefit that
(1) elctro-catalyst prepared by the present invention has preferable electrocatalysis characteristic, and LSV take-off potential is 0.92V, half-wave
Current potential is 0.82V, limiting current density 5mA/cm2, and the ability that there are the intermediates such as certain anti-CO to poison.
(2) oxygen reduction catalyst prepared by the present invention has uniform nanowire structure, and nanowire diameter is about
200nm, wire length is about 10 μm, and molybdenum dioxide nano particle is evenly distributed on nano wire.
(3) the invention is simple and feasible, and the structure and product composition of nano wire can be controlled by adjusting Drugs proportion.
Detailed description of the invention
Fig. 1 is that embodiment 1 prepares molybdenum dioxide -- the SEM of the oxygen reduction catalyst of carbon nanocoils schemes；
Fig. 2 is molybdenum dioxide -- the oxygen reduction catalyst and business Pt/C catalyst of carbon nanocoils prepared by embodiment 1
The cyclic voltammetry curve in 0.1M KOH solution；
Fig. 3 is molybdenum dioxide -- the oxygen reduction catalyst and business Pt/C catalyst of carbon nanocoils prepared by embodiment 2
The cyclic voltammetry curve in 0.1M KOH solution.
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:
The oxygen reduction catalyst of molybdenum dioxide in present embodiment -- carbon nanocoils is to realize according to the following steps:
(1) configuration of polyacrylonitrile and N,N-dimethylformamide solvent: the polyacrylonitrile for weighing 1g is dissolved in the N of 10g, N-
In dimethyl formamide solution, then above-mentioned mixed solution is transferred in the beaker of sealing, is placed on magnetic stirring apparatus and stirs, stir
Mixing rate is 500rpm, and whipping temp is 50 DEG C, stirs to solution in beaker to colorless and transparent, obtains mixed solvent, spare.
(2) configuration of spinning solution: claiming the ammonium molybdate of 157mg to be dissolved in the solvent of step (1) preparation, and mixed solution is turned
It moves in the beaker of sealing, is placed on magnetic stirring apparatus and stirs, stirring rate 490rpm, whipping temp is 50 DEG C, to beaker
The vinicolor that interior solution is stirred until homogeneous obtains spinning solution, spare.
(3) spinning: solution obtained by step (2) is transferred in the syringe in electrospinning device, is adjusted spinning and is set
Standby parameter: selecting No. 18 syringe needles, and pushing away speed is 0.019mm/min, and temperature is 30 DEG C, and humidity 43%, collecting distance is 15cm, if
It can start spinning after the completion of setting；Gained spinning is placed in baking oven, temperature is 60 DEG C, humidity 35%, drying time 12
Hour.
(4) spinning of step (3) resulting drying is placed in Muffle furnace and carries out process control heating pre-oxidation, parameter is set
Be set to: heating rate is 1 DEG C/min, and Pre oxidation is 250 DEG C, and soaking time 80min carries out pre- oxygen in air atmosphere
Change.
(5) spinning after step (4) resulting pre-oxidation is placed in progress process control heating in tube furnace, tube furnace ginseng
Number setting are as follows: heating rate is 5 DEG C/min, and carburizing temperature is 800 DEG C, soaking time 110min, is protective gas in nitrogen
Lower sintering, it is 0.02L/min that nitrogen, which is passed through rate,.To get required catalyst after the completion of sintering.
Embodiment 2:
The oxygen reduction catalyst of molybdenum dioxide in present embodiment -- carbon nanocoils is to realize according to the following steps:
(1) configuration of PVP K30 and ultrapure aqueous solvent: the PVP K30 for weighing 0.49g is molten
In the ultrapure water of 9.8g, then above-mentioned mixed solution is transferred in the beaker of sealing, is placed on magnetic stirring apparatus and stirs, stirred
Rate is 400rpm, and whipping temp is 40 DEG C, stirs to solution in beaker to colorless and transparent, obtains mixed solvent, spare.
(2) configuration of spinning solution: the ammonium molybdate of 102.9mg is claimed to be dissolved in the solvent of step (1) preparation, by mixed solution
It is transferred in the beaker of sealing, is placed on magnetic stirring apparatus and stirs, stirring rate 480rpm, whipping temp is 45 DEG C, wait burn
The vinicolor that solution is stirred until homogeneous in cup, obtains spinning solution, spare.
(3) spinning: solution obtained by step (2) is transferred in the syringe in electrospinning device, is adjusted spinning and is set
Standby parameter: selecting No. 17 syringe needles, and pushing away speed is 0.015mm/min, and temperature is 28 DEG C, and humidity 30%, collecting distance is 14cm, if
It can start spinning after the completion of setting；Gained spinning is placed in baking oven, temperature is 55 DEG C, humidity 35%, drying time 10
Hour.
(4) spinning of step (3) resulting drying is placed in Muffle furnace and carries out process control heating pre-oxidation, parameter is set
Be set to: heating rate is 0.5 DEG C/min, and Pre oxidation is 235 DEG C, soaking time 60min, is carried out in air atmosphere pre-
Oxidation.
(5) spinning after step (4) resulting pre-oxidation is placed in progress process control heating in tube furnace, tube furnace ginseng
Number setting are as follows: heating rate is 4 DEG C/min, and carburizing temperature is 750 DEG C, soaking time 60min, in the case where nitrogen is protective gas
Sintering, it is 0.02L/min that nitrogen, which is passed through rate,.To get required catalyst after the completion of sintering.
Embodiment 3:
The oxygen reduction catalyst of molybdenum dioxide in present embodiment -- carbon nanocoils is to realize according to the following steps:
(1) it the configuration of PVP K30 and alcohol solvent: weighs 1.03g PVP K30 and is dissolved in
In 10ml ethanol solution, then above-mentioned mixed solution is transferred in the beaker of sealing, is placed on magnetic stirring apparatus and stirs, stirred
Rate is 600rpm, and whipping temp is 50 DEG C, stirs to solution in beaker to colorless and transparent, obtains mixed solvent, spare.
(2) configuration of spinning solution: the ammonium molybdate of 722.4mg is claimed to be dissolved in the solvent of step (1) preparation, by mixed solution
It is transferred in the beaker of sealing, is placed on magnetic stirring apparatus and stirs, stirring rate 540rpm, whipping temp is 55 DEG C, wait burn
The vinicolor that solution is stirred until homogeneous in cup, obtains spinning solution, spare.
(3) spinning: solution obtained by step (2) is transferred in the syringe in electrospinning device, is adjusted spinning and is set
Standby parameter: selecting No. 21 syringe needles, and pushing away speed is 0.032mm/min, and temperature is 35 DEG C, and humidity 50%, collecting distance is 18cm, if
It can start spinning after the completion of setting；Gained spinning is placed in baking oven, temperature is 65 DEG C, humidity 35%, drying time 12
Hour.
(4) it pre-oxidizes: the spinning of step (3) resulting drying being placed in Muffle furnace and carries out the pre- oxygen of process control heating
Change, parameter setting are as follows: heating rate is 1.5 DEG C/min, and Pre oxidation is 285 DEG C, soaking time 130min, in air gas
It is pre-oxidized under atmosphere.
(5) it is sintered: the spinning after step (4) resulting pre-oxidation is placed in progress process control heating in tube furnace, pipe
Formula furnace parameters setting are as follows: heating rate is 5.5 DEG C/min, and carburizing temperature is 900 DEG C, soaking time 150min, is in nitrogen
It is sintered under protective gas, it is 0.02L/min that nitrogen, which is passed through rate,.To get required catalyst after the completion of sintering.
As can be seen from Figure 1: catalyst is uniform nanowire structure, and nanowire diameter is about 200nm, and wire length is about
10 μm。
As can be seen from Figure 2: molybdenum dioxide-carbon nanocoils oxygen reduction catalyst LSV take-off potential is 0.92V, partly
Wave current potential is 0.82V, limiting current density 5mA/cm2；The LSV take-off potential of 20%Pt/C: 0.986V, half wave potential:
0.85 V, limiting current density: 5.3mA/cm2。
As can be seen from Figure 3: LSV take-off potential is 0.90V, half wave potential 0.81V, and limiting current density is
5.4mA/cm2；The LSV take-off potential of 20%Pt/C: 0.986V, half wave potential: 0.85V, limiting current density: 5.3mA/cm2。
Note: LSV take-off potential, half wave potential, limiting current density are to evaluate the important indicator of performance of oxygen-reducing catalyst,
The data of itself and 20%Pt/C can generally be compared.
Claims (9)
1. a kind of molybdenum dioxide -- the preparation method of the oxygen reduction catalyst of carbon nanocoils；Characterized by comprising the following steps:
(1) solubilizer is dissolved in solvent A, is transferred in the container of sealing, be placed on magnetic stirring apparatus and stir, stirring rate is
400-600rpm, whipping temp are 40-50 DEG C, to liquid agitation in container to colorless and transparent, obtain mixed solvent；
(2) ammonium molybdate is dissolved in the in the mixed solvent of step (1) preparation, is transferred in the container of sealing, is placed in magnetic stirring apparatus
Upper stirring, stirring rate 480-540rpm, whipping temp are 45-55 DEG C, the grape wine being stirred until homogeneous to solution in container
Color obtains solution；
(3) solution obtained by step (2) is transferred in the dedicated spinning cylinder in electrospinning device, adjusts spinning equipment ginseng
Number, can start spinning；After spinning, gained spinning is placed in baking oven and is dried；
(4) it pre-oxidizes: the spinning after step (3) drying is placed in Muffle furnace, process control is carried out to temperature, realizes spinning
Heating pre-oxidation, the spinning after pre-oxidation are rendered as sepia bulk；
(5) it is sintered: the spinning after step (4) resulting pre-oxidation is placed in progress process control heating in tube furnace, so that its
Carbonization, can be obtained final catalyst.
2. a kind of molybdenum dioxide -- the preparation method of the oxygen reduction catalyst of carbon nanocoils as described in claim 1；Its feature
It is, in step (1), the solubilizer is PVP K30 or polyacrylonitrile；Solvent A is N, N- dimethyl formyl
Amine, ethyl alcohol or ultrapure water；Solubilizer and solvent A mass ratio are 1:20-13:100.
3. a kind of molybdenum dioxide -- the preparation method of the oxygen reduction catalyst of carbon nanocoils as described in claim 1；Its feature
It is, in step (2), ammonium molybdate and mixed solvent mass ratio are 1:100-2:25.
4. a kind of molybdenum dioxide -- the preparation method of the oxygen reduction catalyst of carbon nanocoils as described in claim 1；Its feature
It is, in step (3), spinning collection device is dedicated masking foil；It is 17-21 needle that used syringe needle, which is arranged, in electrostatic spinning
Head, pushing away speed is 0.015mm/min-0.032mm/min, and temperature is 28 DEG C -35 DEG C, humidity 30%-50%, collects distance and is
14cm-18cm。
5. a kind of molybdenum dioxide -- the preparation method of the oxygen reduction catalyst of carbon nanocoils as described in claim 1；Its feature
It is, in step (3), the condition of drying are as follows: temperature is 55 DEG C -65 DEG C, humidity 35%, and the time is 10-12 hours.
6. a kind of molybdenum dioxide -- the preparation method of the oxygen reduction catalyst of carbon nanocoils as described in claim 1；Its feature
It is, in step (4), Muffle furnace heating rate is 0.5 DEG C/min-1.5 DEG C/min, and the temperature of pre-oxidation is 235 DEG C -285 DEG C,
Soaking time is 60min-130min, is pre-oxidized in air atmosphere.
7. a kind of molybdenum dioxide -- the preparation method of the oxygen reduction catalyst of carbon nanocoils as described in claim 1；Its feature
It is, in step (5), tube furnace heating rate is 4 DEG C/min-5.5 DEG C/min, and the temperature of carbonization is 750 DEG C -900 DEG C, heat preservation
Time is 60min-150min, is sintered in the case where nitrogen is protective gas, it is≤0.05L/min that nitrogen, which is passed through rate,.
8. a kind of molybdenum dioxide -- the oxygen reduction catalyst of carbon nanocoils, which is characterized in that be any by claim 1~7
Made from the item preparation method.
9. by a kind of molybdenum dioxide according to any one of claims 8 -- the oxygen reduction catalyst of carbon nanocoils is used for pem fuel
The cathodic oxygen reduction of battery.
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| CN111710876A (en) * | 2020-05-11 | 2020-09-25 | 江苏可兰素环保科技有限公司 | Non-noble metal cathode catalyst and preparation method thereof |
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Application publication date: 20181228 |