CN107221683A - The preparation method of PtVFe/WC/C nanometers of oxygen reduction catalysts - Google Patents
The preparation method of PtVFe/WC/C nanometers of oxygen reduction catalysts Download PDFInfo
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- CN107221683A CN107221683A CN201710583717.7A CN201710583717A CN107221683A CN 107221683 A CN107221683 A CN 107221683A CN 201710583717 A CN201710583717 A CN 201710583717A CN 107221683 A CN107221683 A CN 107221683A
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- oxygen reduction
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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
- H01M4/8825—Methods for deposition of the catalytic active composition
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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
- H01M4/92—Metals of platinum group
- H01M4/921—Alloys or mixtures with metallic elements
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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
- H01M4/92—Metals of platinum group
- H01M4/923—Compounds thereof with non-metallic elements
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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
- H01M4/92—Metals of platinum group
- H01M4/925—Metals of platinum group supported on carriers, e.g. powder carriers
- H01M4/926—Metals of platinum group 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 discloses a kind of preparation method of the nano combined oxygen reduction catalysts of PtVFe/WC/C, wherein, laboratory prepares gained before PtVFe solution is, comprises the following steps：1）140mg tungsten carbides and toner mixture are added in 200mL hexanes, then ultrasound 2 hours adds the ready PtVFe solution of 60mg（Platinum source, vanadium source, source of iron are acetylacetone,2,4-pentanedione platinum, vanadium acetylacetonate, iron pentacarbonyl）Prepare PtVFe/WC/C mixed solutions；2）Mixed solution is subjected to ultrasound 1 hour, then stirred 16 hours；3）In nitrogen（N2）The lower stirring of protection 48 hours, this suspension slowly evaporates；4）Product will be evaporated in N2Protection is lower to be collected and dries, and obtains PtVFe/WC/C powder；5）By PtVFe/WC/C powder in N2The lower heat treatment 60min of protection, temperature is 260 DEG C；6）PtVFe/WC/C powder is in 15%H after being heat-treated2+85%N2The lower calcining 120min of protection, temperature is 400 DEG C, obtains the nano combined oxygen reduction catalysts of PtVFe/WC/C.PtVFe/WC/C oxygen reduction catalysts prepared by the present invention have preferable electro-chemical activity and stability, can not only improve the efficiency of cathode reaction, and can be very good to extend its service life cycle.
Description
Technical field
The present invention relates to a kind of preparation method of PtVFe/WC/C nano-composite catalysts, more particularly to one kind is in hydrogen reduction
The preparation method of PtVFe/WC/C composite catalysts in reaction.
Background technology
It is maximally effective in terms of hydrogen utilization with fuel cell such as Proton Exchange Membrane Fuel Cells of the hydrogen as fuel
Mode because its high conversion efficiency, low stain, light, high power density, while as the energy in automobile, space shuttle, build
Build and be widely used in terms of industrial.Catalyst is one of part of fuel cell most critical, in manufacture fuel electricity
Catalyst account for close to 30% in the cost in pond.In a fuel cell by sintering and dissolving, the stability of platinum base catalysis is
Decline.It is activity, stability and low consumption to realize that application of the fuel cell in terms of hydrogen reduction is finally commercialized most critical challenge.
At low temperature（<100℃）, fuel cell is the limitation of catalyst cathode power most lasting in terms of hydrogen reduction the problem of.Recently, exist
The research of electrocatalyst for cathode has focussed on binary platinum base oxygen reduction catalyst, as Pt-Fe, Pt-Ni, and Pt-Co,
It was reported that platinum alloy enhances performance of the platinum-based electrocatalyst in terms of hydrogen reduction.This may be attributed to the key between platinum and platinum
Property away from the closest electron number of, platinum and platinum surface oxide layer.
Metal carbides, particularly tungsten carbide（WC）Be defined as fuel-cell catalyst carrier, due to it
High stability, low-resistivity and the strong synergy between metallic catalyst, Chhina etc. are also reported in sour environment
Under, WC is than C as more stable during carrier.Due to the strong interaction of metal and carrier, WC can also strengthen platinum based catalyst
Surface-active.The seminar in Shen is it has been reported that with WC Modified Platinums or platinum based catalyst, WC can strengthen fuel as carrier
Activity of the battery in terms of hydrogen reduction, this is attributable to the distribution evenly of metallic particles and carrier and forms cooperative effect.
By research, it has been found that changing WC and C ratio, the activity and stability of catalyst are also changed.Therefore, based on oxygen
The basic research of elctro-catalyst is reduced, physical characterization and chemical property around PtVFe/WC/C elctro-catalysts are studied.
The content of the invention
In view of this, the invention provides a kind of preparation method of oxygen reduction electro-catalyst, the PtVFe/WC/C oxygen of preparation
Reducing catalyst can improve cathode reaction efficiency, extend service life cycle.
The preparation method of the PtVFe/WC/C oxygen reduction catalysts of the present invention, comprises the following steps：
1）140 mg tungsten carbides and toner mixture are added in 200 mL hexanes, ultrasound 2 hours, then add 60 mg preparations
Good PtVFe solution（Platinum source, vanadium source, source of iron are acetylacetone,2,4-pentanedione platinum, vanadium acetylacetonate, iron pentacarbonyl）PtVFe/WC/C is prepared to mix
Close solution；
2）Mixed solution is subjected to ultrasound 1 hour, then stirred 16 hours；
3）In nitrogen（N2）Protection lower stirring 4-8 hours, this suspension slowly evaporates；
4）Product will be evaporated in N2Protection is lower to be collected and dries, and obtains PtVFe/WC/C powder；
5）By PtVFe/WC/C powder in N2Protection 60 min of lower heat treatment, temperature is 260 DEG C；
6）PtVFe/WC/C powder is in 15% H after being heat-treated2 + 85% N2Protection 120 min of lower calcining, temperature is 400
DEG C, obtain the nano combined oxygen reduction catalysts of PtVFe/WC/C.
Further, the step 1）In, PtVFe solution（Platinum source, vanadium source, source of iron be acetylacetone,2,4-pentanedione platinum, vanadium acetylacetonate,
Iron pentacarbonyl）Source for laboratory prepare gained, hexane is solvent, at the same using ultrasound method, ultrasonic power is 80%,
Suspension particle size, the form of preparation can be controlled, and the dispersiveness of product is also preferable.
Further, the step 2）In, ultrasonic power is 80%, uses laboratory room small-sized magnetic stirrer..
Further, the step 3）In, stirring can exclude other gases in air under nitrogen atmosphere, it is to avoid oxidation.
Further, the step 4）In, drying temperature is 60 DEG C, and the time is 5 hours.
Further, the step 5）In, heat treatment can remove the organic shell remained in catalyst.
Further, the step 6）In, calcining is the significant process for preparing ternary alloy three-partalloy, can obtain more preferable by calcining
Performance.
The beneficial effects of the present invention are：The present invention utilizes thermal decomposition method and reducing process synthesis PtVFe/WC/C nanoparticles
Son.PtVFe, WC, C and hexane are mixed, PtVFe/WC/C nanometers are prepared by ultrasound, stirring, dry, heat treatment and calcining
Compound oxygen reduction catalyst.Using ultrasound and stirring, PtVFe/WC/C orderly pore structure can be effectively improved, so that it has
There are the specific physical properties of good transmission proton, while its particle size, dispersiveness and pattern can also be controlled.By
N2It is heat-treated under environment, can avoids aoxidizing and removing the organic shell in catalyst.Calcining is the weight for preparing alloy material
Process is wanted, the performance of material can be improved.PtVFe/WC/C is conductive composite, therefore as hydrogen reduction
Catalyst, can not only improve the hydrogen reduction efficiency of cathode reaction, and can greatly extend service life cycle；The present invention
The PtVFe/WC/C oxygen reduction catalysts of preparation have higher catalytic activity and stability, to ensure the anti-of oxygen reduction catalyst
Efficiency, stability and long circulation life are answered, be can be used in Cathodic oxygen reduction.
Brief description of the drawings
In order that the object, technical solutions and advantages of the present invention are clearer, below in conjunction with accompanying drawing the present invention is made into
The detailed description of one step, wherein：
Fig. 1 is the XRD for the catalyst that embodiment 1 is prepared；
Fig. 2 is the TEM-HRTEM figures for the catalyst that embodiment 1 is prepared；
The catalyst that Fig. 3 is embodiment 1, comparative example 1, comparative example 2 are prepared is in 0.5 M H2SO4CV figures in electrolyte；
The catalyst that Fig. 4 is embodiment 1, comparative example 1, comparative example 2 are prepared is in 0.5 M H2SO4LSV figures in electrolyte；
Fig. 5 is the catalyst for preparing of embodiment 1 in 0.5 M H2SO4Stability CV figures in electrolyte；
Fig. 6 is the catalyst for preparing of embodiment 1 in 0.5 M H2SO4Stability LSV figures in electrolyte.
Embodiment
Hereinafter with reference to accompanying drawing, the preferred embodiments of the present invention are described in detail.
Embodiment 1
The preparation method of the PtVFe/WC/C oxygen reduction catalysts of embodiment 1, comprises the following steps：
1）140 mg tungsten carbides and toner mixture are added in 200 mL hexanes, ultrasound 2 hours, then add 60 mg preparations
Good PtVFe solution (platinum source, vanadium source, source of iron are acetylacetone,2,4-pentanedione platinum, vanadium acetylacetonate, iron pentacarbonyl) prepares PtVFe/WC/C and mixed
Close solution；
2）Mixed solution is subjected to ultrasound 1 hour, then stirred 16 hours；
3）In nitrogen（N2）Protection lower stirring 4-8 hours, this suspension slowly evaporates；
4）Product will be evaporated in N2Protection is lower to be collected and dries, and obtains PtVFe/WC/C powder；
5）By PtVFe/WC/C powder in N2Protection 60 min of lower heat treatment, temperature is 260 DEG C；
6）PtVFe/WC/C powder is in 15% H after being heat-treated2 + 85% N2Protection 120 min of lower calcining, temperature is 400
DEG C, obtain the nano combined oxygen reduction catalysts of PtVFe/WC/C.
Comparative example 1
The oxygen reduction catalyst of comparative example 1 uses PtVFe/C catalyst, preparation method be the same as Example 1.
Comparative example 2
The oxygen reduction catalyst of comparative example 2 uses PtVFe/WC catalyst, preparation method be the same as Example 1.
Fig. 1 is the XRD for the catalyst that embodiment 1 is prepared, as shown in Figure 1.In XRD, the position institute of diffraction maximum
What is represented is PtVFe (111), and (200) and (220) crystal face shows the catalyst for face-centered cubic crystal.PtVFe spreads out
Penetrate the position at peak and monometallic Pt, V, Fe diffraction maximum peak position are equipped with deviation, show that the material that we prepare belongs to alloy.
Fig. 2 is the TEM-HRTEM figures for the PtVFe/WC/C composite catalyzing materials that embodiment 1 is prepared, as shown in Figure 2.
From the TEM figures in Fig. 2 it can be seen that prepared PtVFe/WC/C crystal is than more uniform, average grain diameter is less than 50 nm.From figure
HRTEM figures can obtain, PtVFe/WC/C spacing of lattice is 2.47.This trimetal nanoparticles does not only have high crystallization
Face, and Pt, V, Fe be uniformly distributed.
PtVFe/WC/C, the PtVFe for respectively preparing embodiment 1 and comparative example 1, comparative example 2/C, PtVFe/WC
Oxygen reduction catalyst is as working electrode, and platinum filament is as to electrode, and reversible hydrogen electrode is as reference electrode, and concentration is 0.5 M's
H2SO4Solution is prepared into three electrode oxygen reductions reaction electro-chemical test group as electrolyte.
Fig. 3 is embodiment 1, comparative example 1,2 three kinds of catalyst of comparative example in N20.5 M H during saturation2SO4In electrolyte
CV figures when the rotating speed of rotating disk electrode (r.d.e) is 1600 rpm, as shown in Figure 3.It can be seen that three kinds of catalyst are in hydrogen
Adsorption desorption area is characterized in different.
Fig. 4 is embodiment 1 and comparative example 1,2 three kinds of catalyst of comparative example in 0.5 M H2SO4Rotating circular disk in electrolyte
LSV figures when the rotating speed of electrode is 1600 rpm, as shown in Figure 4.Test of the activity of catalyst in terms of the electroreduction of oxygen
Hydrodynamics rotating disk electrode (r.d.e) technology can be used.The pole measured in terms of hydrogen reduction with rotating disk electrode (r.d.e) is shown in figure
Change the position of curve, it can be seen that power of the PtVFe/WC/C nanometers of oxygen reduction catalysts in rotating disk electrode (r.d.e)
Area's current density is bigger, shows that the PtVFe/WC/C three-way catalysts prepared have more preferable electro-chemical activity.
Fig. 5 and Fig. 6 are respectively embodiment 1 in O2Saturation N20.5 M H during saturation2SO4In electrolyte in rotating disk electrode (r.d.e)
0th, the CV figures and LSV figures before and after 5000,10000 circle stability tests, as shown in the figure.It can clearly be seen that in CV figures, 5000,
Current density size and active area change very little after 10000 circles, illustrate that the stability of catalyst is fine.In figure 6,5000 circle
Current potential is constant afterwards, and anterioposterior curve is almost overlapped, and illustrates that stability is fine.But after 10000 circles, current potential becomes compared with before test
Negative, stability has declined.By CV, LSV stability diagram, we can obtain PtVFe/WC/C catalyst have it is very high steady
It is qualitative.In summary data analysis understands that ternary metal PtVFe receives by using different carrier modifications, wherein PtVFe/WC/C
Preferably, stability is preferably also the activity of rice oxygen reduction catalyst.
It can be proved by above-mentioned experiment, the PtVFe/WC/C that embodiment 1 is prepared by thermal decomposition method and reducing process
Oxygen reduction catalyst, with good crystallinity, and grain size is small, be evenly distributed, so the catalyst have it is more
Avtive spot, expression activitiy is good.PtVFe/WC/C active area is bigger, and current potential is shuffled, than other carrier electrochemistry oxygens also
Originality can have more superiority.CV curves active area, limiting current density before and after PtVFe/WC/C catalyst stability tests
Knots modification very little, is overlapped very well, take-off potential is essentially coincided before and after the test of LSV curve stabilities.So prepared by embodiment 1
PtVFe/WC/C nanometers of oxygen reduction catalysts are in 0.5 M H2SO4With good oxygen reduction catalytic activity and stably in electrolyte
Property.Therefore, in the present invention, PtVFe/WC/C oxygen reduction catalysts are prepared with thermal decomposition method and reducing process in oxygen reduction reaction
Middle performance is more preferable.
In the present invention, ultrasonically treated parameter can be conventional ultrasonically treated parameter, the equipment of certain other agitating solutions
The present invention is can also be used for, ultrasonic time can be with STOCHASTIC CONTROL with ultrasonic power；Platinum source, vanadium source, source of iron be only limitted to acetylacetone,2,4-pentanedione platinum,
Vanadium acetylacetonate, iron pentacarbonyl.Solvent is hexane, and different solvents can be used for the present invention, but the operation of ultrasonic agitation can
It is adjusted according to material therefor and feedstock property；PtVFe/WC/C powder is not limited to be prepared with thermal decomposition method and reducing process,
PtVFe/WC/C powder can be also prepared with other methods.
Finally illustrate, the above embodiments are merely illustrative of the technical solutions of the present invention and it is unrestricted, although pass through ginseng
According to the preferred embodiments of the present invention, invention has been described, it should be appreciated by those of ordinary skill in the art that can
So that various changes are made to it in the form and details, the present invention limited without departing from appended claims
Spirit and scope.
Claims (7)
1. a kind of preparation method of the nano combined oxygen reduction catalysts of PtVFe/WC/C, it is characterised in that：Comprise the following steps：
1）140 mg tungsten carbides and toner mixture are added in 200 mL hexanes, ultrasound 2 hours, then add 60 mg preparations
Good PtVFe solution（Platinum source, vanadium source, source of iron are acetylacetone,2,4-pentanedione platinum, vanadium acetylacetonate, iron pentacarbonyl）Prepare PtVFe/WC/C
Mixed solution；
2）Mixed solution is subjected to ultrasound 1 hour, then stirred 16 hours；
3）In nitrogen（N2）Protection lower stirring 4-8 hours, this suspension slowly evaporates；
4）Product will be evaporated in N2Protection is lower to be collected and dries, and obtains PtVFe/WC/C powder；
5）By PtVFe/WC/C powder in N2Protection 60 min of lower heat treatment, temperature is 260 DEG C；
6）PtVFe/WC/C powder is in 15% H after being heat-treated2 + 85% N2Protection 120 min of lower calcining, temperature is 400 DEG C,
Obtain the nano combined oxygen reduction catalysts of PtVFe/WC/C.
2. the preparation method of the nano combined oxygen reduction catalysts of PtVFe/WC/C according to claim 1, it is characterised in that：
The step 1）In, the source of PtVFe solution prepares gained for laboratory, and hexane is solvent, while using the method for ultrasound, surpassing
Acoustical power is 80%, and suspension particle size, the form of preparation can be controlled, and the dispersiveness of product is also preferable.
3. the preparation method of PtVFe/WC/C oxygen reduction catalysts according to claim 1, it is characterised in that：The step
2）In, ultrasonic power is 80%, uses laboratory room small-sized magnetic stirrer.
4. the preparation method of PtVFe/WC/C oxygen reduction catalysts according to claim 1, it is characterised in that：The step
3）In, N2Stirring can exclude other gases in air under atmosphere, it is to avoid oxidation.
5. the preparation method of PtVFe/WC/C oxygen reduction catalysts according to claim 1, it is characterised in that：The step
4）In, drying temperature is 60 DEG C, and the time is 5 hours.
6. the preparation method of PtVFe/WC/C oxygen reduction catalysts according to claim 1, it is characterised in that：The step
5）In, heat treatment can remove the organic shell remained in catalyst.
7. the preparation method of PtVFe/WC/C oxygen reduction catalysts according to claim 1, it is characterised in that：The step
6）In, calcining is the significant process for preparing ternary alloy three-partalloy, can obtain better performance by calcining.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107785564A (en) * | 2017-10-18 | 2018-03-09 | 武汉理工大学 | VTi2.6O7.7Nano particle, preparation and application |
| CN109546166A (en) * | 2019-01-25 | 2019-03-29 | 辽宁科技大学 | A kind of Pt/ metal carbides/carbon nanomaterial catalyst and preparation method thereof |
| CN110474047A (en) * | 2019-08-28 | 2019-11-19 | 湖南金富力新能源股份有限公司 | A kind of nickel-cobalt-manganese ternary presoma and the preparation method and application thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2004107482A1 (en) * | 2003-05-27 | 2004-12-09 | Symyx Technologies, Inc. | Platinum-vanadium-iron fuel cell electrocatalyst |
| US7053021B1 (en) * | 2004-04-22 | 2006-05-30 | The Research Foundation Of The State University Of New York | Core-shell synthesis of carbon-supported alloy nanoparticle catalysts |
| CN1810374A (en) * | 2005-11-07 | 2006-08-02 | 中山大学 | Carbon supported nanometer WC reinforced oxidation-reduction electrocatalyst and its prepn process |
-
2017
- 2017-07-18 CN CN201710583717.7A patent/CN107221683A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2004107482A1 (en) * | 2003-05-27 | 2004-12-09 | Symyx Technologies, Inc. | Platinum-vanadium-iron fuel cell electrocatalyst |
| US7053021B1 (en) * | 2004-04-22 | 2006-05-30 | The Research Foundation Of The State University Of New York | Core-shell synthesis of carbon-supported alloy nanoparticle catalysts |
| CN1810374A (en) * | 2005-11-07 | 2006-08-02 | 中山大学 | Carbon supported nanometer WC reinforced oxidation-reduction electrocatalyst and its prepn process |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107785564A (en) * | 2017-10-18 | 2018-03-09 | 武汉理工大学 | VTi2.6O7.7Nano particle, preparation and application |
| CN109546166A (en) * | 2019-01-25 | 2019-03-29 | 辽宁科技大学 | A kind of Pt/ metal carbides/carbon nanomaterial catalyst and preparation method thereof |
| CN110474047A (en) * | 2019-08-28 | 2019-11-19 | 湖南金富力新能源股份有限公司 | A kind of nickel-cobalt-manganese ternary presoma and the preparation method and application thereof |
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