CN107293757A - The preparation method of PtCoFe/WC C oxygen reduction catalysts - Google Patents
The preparation method of PtCoFe/WC C oxygen reduction catalysts Download PDFInfo
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Abstract
The invention discloses a kind of preparation method of PtCoFe/WC C nanos compound oxygen reduction catalyst, comprise the following steps：1）The chloroplatinic acid of measured amounts（H2PtCl6）Solution, and weigh a certain amount of cobalt chloride（CoCl26H2O）, iron chloride (FeCl36H2O）And sodium borohydride（NaBH4）, then add excessive ethylene glycol（C2H6O2）Solution, is transferred in reactor after being well mixed and is reacted 12 hours at 200 DEG C, prepares PtCoFe mixed solutions；2）Mixed solution is subjected to ultrasound procedure；3）Mixed solution is inserted into centrifuge tube centrifugally operated；4）PtCoFe alloy powders are obtained after centrifugation product is placed in into oven drying processing；5）PtCoFe alloy powders and WC C powder mechanical mixtures are obtained into PtCoFe/WC C nano compound oxygen reduction catalyst.PtCoFe/WC C oxygen reduction catalysts prepared by the present invention have preferable electro-chemical activity and stability, can not only improve the efficiency of oxygen reduction cathode reaction, and can greatly extend service life cycle.
Description
Technical field
The present invention relates to a kind of preparation method of PtCoFe/WC-C nano-composite catalysts, more particularly to one kind in oxygen also
The preparation method of PtCoFe/WC-C composite catalysts in original reaction.
Background technology
According to the state of development of domestic economy and the fundamental realities of the country of China, coal accounts for main body in the energy resource structure of China
The situation of status needs to put into a large amount of manpowers slowly to be adjusted with material resources, and coal is as the main fuel of China, and its consumption has
One important feature --- raw coal directly burns, and oxysulfide, greenhouse gases, nitrogen oxides and the flue dust thus discharged is
The arch-criminal of the deterioration of the ecological environment, the common people have paid close attention to the yellow haze weather brought under rapid economic development and acid rain is existing
As.The today of oil after decades have been exploited, production technique is not good, continues to exploit difficult, the consumption of domestic petroleum
Demand increased continuously and healthily, causes the import volume of Jin20Nian Lai CNPCs to surge, by the end of dependence on foreign countries for oil in 2012
58.8% or so is up to, nearly 10 times have been turned over compared with 1993.Because China's energy prices are cheap, extensive economy is formed,
Domestic ecological environment is difficult to be further continued for bearing this Economic Development Mode, and various countries' pressure on the problem of tackling climate change is more next
It is bigger, it is necessary to accelerate Green Transformation develop process.Therefore, development clean energy technology to China's economy with ecology it is sustainable
Development construction is particularly critical.
Fuel cell（fuel cells）It is a kind of novel power generation device, possesses the combustion of the conventional fossils such as natural gas, coal, oil
Expect the matchless advantage of the energy, can be achieved that the chemical energy in fuel expeditiously is converted into electric energy, and energy conversion process
Zero-emission is basically reached, therefore its main energy sources for turning into 21 century is the desire of the people.Fuel cell power system is a kind of green
Color energy technology, to solve that global warming, traditional oil energy development difficulty that global village faces be big and ecological pollution etc. extremely
Close important, be considered as one of 21 century most important energy source and power, be always the research and development focus in clean energy resource field in the world.
Because Cathodic oxygen reduction (oxygen reduction reaction, be abbreviated as ORR) is that fuel cell electricity is urged
Change the committed step of reaction, had very important significance so exploring efficient, cheap cathodic oxygen reduction catalyst.According to the study
Show transition metal and its alloy, no matter price or performance are all to prepare the splendid selection of electrode material, belong to transition metal together
Platinum, cobalt, three kinds of elements of iron, the electronic configuration of its d track is special, and can make the chemical property of catalyst is improved.Greatly
Amount experiment shows that the influence of the carrier of catalyst to catalyst activity can not be ignored；Research finds that tungsten carbide has high stability
With the advantage such as low-resistivity, the platinum catalyst for making carrier with tungsten carbide has good hydrogen reduction electrocatalysis characteristic.But tungsten carbide is also
It is not employed as the carrier of PtCoFe ternary alloy catalysts in oxygen reduction reaction.Therefore, the basis based on oxygen reduction catalyst
Research, preliminary research has been carried out in terms of the chemical property and physical characterization of PtCoFe/WC-C composite catalysts.
The content of the invention
In view of this, the invention provides a kind of preparation method of oxygen reduction electro-catalyst, the PtCoFe/WC-C oxygen of preparation
Reducing catalyst can improve cathode reaction efficiency, and have extended cycle life.
The preparation method of the PtCoFe/WC-C oxygen reduction catalysts of the present invention, comprises the following steps：
1）The chloroplatinic acid of measured amounts（H2PtCl6）Solution, and weigh a certain amount of cobalt chloride（CoCl2•6H2O）, iron chloride
(FeCl3•6H2O）And sodium borohydride（NaBH4）, then add excessive ethylene glycol（C2H6O2）Solution, is transferred to after being well mixed
Reacted 12 hours at 200 DEG C in reactor, prepare PtCoFe mixed solutions；
2）Mixed solution is subjected to ultrasound procedure；
3）Mixed solution is inserted into centrifuge tube centrifugally operated；
4）PtCoFe alloy powders are obtained after centrifugation product is placed in into oven drying processing；
5）PtCoFe alloy powders and WC-C powder mechanical mixtures are obtained into the nano combined oxygen reduction catalysts of PtCoFe/WC-C.
Further, the step 1）In, platinum source is chloroplatinic acid, and cobalt source is cobalt chloride, and source of iron is iron chloride, by them and boron
The mixed solution of Sodium Borohydride powder is dissolved in preparation PtCoFe mixed solutions in ethylene glycol solution；PtCoFe/WC-C powder solvents
Hot method is prepared with mechanical mixing, makees the solvent-thermal method of reducing agent, the formation of product thing phase, the size of particle diameter, shape with ethylene glycol
State can be controlled, and the dispersiveness of product is also preferable.
Further, the step 2）In, ultrasonic power is 80%, and ultrasonic time is 1 hour.
Further, the step 3）In, centrifugal speed is 10000 rpm, and centrifugation time is 3 minutes.
Further, the step 4）In, heating-up temperature is 60 DEG C, and the heat time is 5 hours.
The beneficial effects of the present invention are：The present invention using solvent-thermal method mixing platinum acid chloride solution, cobalt chloride, iron chloride and
Sodium borohydride prepares PtCoFe alloy powders, recycles mechanical mixing to be mixed to get WC-C powder with PtCoFe alloy powders
The nano combined oxygen reduction catalysts of PtCoFe/WC-C, and the method that make use of ultrasonic wave added, effectively increase PtCoFe/WC-
C orderly pore structure degree is so as to make it have the specific physical properties of good transmission proton, then using centrifugally operated, removes
PtCoFe/WC-C degree of crystallization is improved while impurity molecule, PtCoFe/WC-C is conductive composite,
Therefore as oxygen reduction catalyst, the hydrogen reduction efficiency of cathode reaction can be not only improved, and can greatly extend
Service life cycle；PtCoFe/WC-C oxygen reduction catalysts prepared by the present invention have higher catalytic activity and stability, with
Ensure reaction efficiency, stability and the long circulation life of oxygen reduction catalyst, 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 PtCoFe/WC-C that embodiment 1 is prepared；
The SEM figures that Fig. 2 is the PtCoFe/WC-C that embodiment 1 is prepared；
The EDS figures that Fig. 3 is the PtCoFe/WC-C that embodiment 1 is prepared；
Fig. 4 is 1 two kinds of catalyst of embodiment 1 and comparative example in 0.5 M H2SO4Cathodic polarization curve figure in electrolyte；
Fig. 5 is 1 two kinds of catalyst of embodiment 1 and comparative example in 0.5 M H2SO4Tafel curve maps in electrolyte；
Fig. 6 is cathodic polarization curve figure of the embodiment 1 in different rotating speeds；
Fig. 7 is cathodic polarization curve figure of the comparative example 1 in different rotating speeds；
Fig. 8 is cathodic polarization curve figure of the embodiment 1 after the cyclic voltammetry scan of the different number of turns；
Fig. 9 is cathodic polarization curve figure of the comparative example 1 after the cyclic voltammetry scan of the different number of turns.
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 PtCoFe/WC-C oxygen reduction catalysts of embodiment 1, comprises the following steps：
1）The chloroplatinic acid of measured amounts（H2PtCl6）Solution, and weigh a certain amount of cobalt chloride（CoCl2•6H2O）, iron chloride
(FeCl3•6H2O）And sodium borohydride（NaBH4）, then add excessive ethylene glycol（C2H6O2）Solution, is transferred to after being well mixed
Reacted 12 hours at 200 DEG C in reactor, prepare PtCoFe mixed solutions；
2）Mixed solution is subjected to ultrasound procedure；
3）Mixed solution is inserted into centrifuge tube centrifugally operated；
4）PtCoFe alloy powders are obtained after centrifugation product is placed in into oven drying processing；
5）PtCoFe alloy powders and WC-C powder mechanical mixtures are obtained into the nano combined oxygen reduction catalysts of PtCoFe/WC-C.
Comparative example 1
The oxygen reduction catalyst of comparative example 1 uses PtCoFe/C catalyst, PtCoFe/C method for preparing catalyst be the same as Example 1.
Fig. 1 is the XRD for the PtCoFe/WC-C composite catalyzing materials that embodiment 1 is prepared, as shown in Figure 1.Because figure
In there is sharp diffraction maximum, therefore obtained PtCoFe/WC-C composite catalyzings material is crystal structure.Peak 1 is WC in figure
（001）Diffraction maximum corresponding to crystal face.Peak 2 is WC in figure（100）Diffraction maximum corresponding to crystal face.Overlap peak 3 is Pt in figure
（111）Crystal face and PtCo（111）Overlapping diffraction maximum corresponding to crystal face.Overlap peak 4 is Co in figure（111）Crystal face and Fe（110）
Overlapping diffraction maximum corresponding to crystal face.Overlap peak 5 is WC in figure（101）Crystal face and CoFe（332）Overlapping corresponding to crystal face is spread out
Penetrate peak.Therefore Pt, Co, Fe, C and WC coexist in XRD, the composite catalyst of preparation.
Fig. 2 is the SEM figures for the PtCoFe/WC-C composite catalyzing materials that embodiment 1 is prepared, as shown in Figure 2.From Fig. 2
（a）In it can be seen that prepared PtCoFe/WC-C particles are evenly distributed on carrier, particle size is nanoscale, compares surface
Product is larger, there is more activated centre, therefore particle has higher activity.The Cluster Phenomenon of local area is due to single grain
The high surface energy of son can cause many crystal grain to be agglomerated into for offspring formation, it is also possible to which ultrasonic time is too short, and particle does not have
Have enough time scattering, again can be with dispersed after ultrasound.The SEM figure such as Fig. 2 of amplification（b）For the picture further amplified, by scheming
As understanding that the evengranular of nanometer particle size is dispersed on carrier.
Fig. 3 is the EDS figures for the PtCoFe/WC-C composite catalyzing materials that embodiment 1 is prepared, as shown in Figure 3.EDS energy
Spectrogram can intuitively reflect the essential element composition in prepared composite catalyst, as can be seen from Figure 3, main in embodiment 1
Member have platinum, cobalt, iron, tungsten and carbon, and this is consistent with the catalyst essential element reacted in XRD.
PtCoFe/WC-C, PtCoFe/ C oxygen reduction catalysts for respectively preparing embodiment 1 and comparative example 1 as
Working electrode, platinum filament is as to electrode, and saturated calomel electrode is as reference electrode, and concentration is 0.5 M H2SO4Solution is used as electricity
Liquid is solved, three electrode oxygen reductions reaction electro-chemical test group is prepared into.
Fig. 4 is 1 two kinds of catalyst of embodiment 1 and comparative example in 0.5 M H2SO4The moon in electrolyte in rotating disk electrode (r.d.e)
Pole polarization curve, as shown in Figure 4.It can be seen that the hydrogen reduction take-off potential of embodiment 1 substantially shuffles 26 mV or so, and have
Bigger limiting current density, therefore PtCoFe/WC-C catalyst prepared by embodiment 1 is than PtCoFe/C prepared by comparative example 1
Catalyst oxygen reduction superior performance.
Fig. 5 is 1 two kinds of catalyst of embodiment 1 and comparative example in 0.5 M H2SO4Tafel curve maps in electrolyte, such as scheme
Shown in 5.It can be seen that Tafel slope of two kinds of catalyst in areas of high potential is similar and is respectively provided with linear well close
System, comparative example 1 and the Tafel slopes of embodiment 1 are 61mV (°) respectively−1With 58mV (°)−1, Tafel curves are oblique
Rate is smaller, illustrates that reaction is more complete, catalytic performance is better, and the PtCoFe/WC-C catalyst that thus prepared by embodiment 1 is shown more
Good hydrogen reduction performance.
Fig. 6 and Fig. 7 are respectively embodiment 1 and comparative example 1 in 0.5 M H2SO4Each rotating speed of rotating disk electrode (r.d.e) in electrolyte
Under cathodic polarization curve figure, as shown in the figure.Under each rotating speed, hydrogen reduction electric current density gradually increases with the increase of overpotential
Greatly, a limiting current density is may eventually reach, and this limiting current density increases with being incremented by for rotating speed；In same rotational speed
Under, the limiting current density of embodiment 1 is all higher than the limiting current density of comparative example 1, and Koutecky-Levich formula are calculated
The electron transfer number of embodiment 1 and comparative example 1 is all close to four, and the electron transfer number of embodiment 1 is bigger, and thus embodiment 1 is made
Standby PtCoFe/WC-C catalyst shows more excellent hydrogen reduction performance.
Fig. 8 and Fig. 9 are respectively embodiment 1 and comparative example 1 in 0.5 M H2SO4In electrolyte before 1000 circle stability tests
Cathodic polarization curve afterwards, as shown in the figure.It can clearly be seen that the take-off potential of comparative example 1 is negative to move 8 mV or so, the 1st circle and the
The limiting current density of corresponding cathodic polarization curve reduces 20% after 1000 circle cyclic voltammetry scans；The stability of embodiment 1
Cathodic polarization curve shows good repeatability before and after test, and take-off potential is essentially coincided, limiting current density knots modification pole
It is small, compared with the take-off potential of comparative example 1, it is still the take-off potential corrigendum of embodiment 1.In summary data analysis is understood
The addition of tungsten carbide, improves stability of the PtCoFe/WC-C catalyst of the preparation of embodiment 1 in oxygen reduction reaction, also increases
The strong catalytic performance of catalyst.
It can be proved by above-mentioned experiment, the PtCoFe/ that embodiment 1 is prepared by solvent-thermal method and mechanical mixing
WC-C oxygen reduction catalysts, each element can coexist, and due to the reason that grain size is small, be evenly distributed, catalyst tool
There is more activated centre, therefore activity is preferably.The hydrogen reduction take-off potential of PtCoFe/WC-C catalyst substantially shuffles 26 mV
Left and right and PtCoFe/WC-C catalyst limiting current density is PtCoFe/C catalyst limiting current densities in oxygen reduction reaction
1.5 times, therefore PtCoFe/WC-C catalyst has more excellent hydrogen reduction performance.PtCoFe/C catalyst the 1st is enclosed and the 1000th circle
The limiting current density of corresponding cathodic polarization curve reduces 20% after cyclic voltammetry scan；PtCoFe/WC-C catalyst stabilizations
Property test before and after cathodic polarization curve show good repeatability, take-off potential is essentially coincided, limiting current density knots modification
It is minimum.So PtCoFe/WC-C nano-composite catalysts prepared by embodiment 1 are in 0.5 M H2SO4Have well in electrolyte
Oxygen reduction catalytic activity and stability.Therefore, in the present invention, PtCoFe/WC- is prepared with solvent-thermal method and mechanical mixing
C oxygen reduction catalysts performance in oxygen reduction reaction 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；Source of iron, cobalt source, platinum source are only limitted to iron chloride, chlorination
Cobalt, chloroplatinic acid.Different reducing agents can be used for the present invention, but the operation of ultrasound centrifugation can be according to material therefor and feed stock
Matter is adjusted；PtCoFe/WC-C powder is not limited to be prepared with mechanical mixing with solvent-thermal method, can also be made with other methods
Standby PtCoFe/WC-C powder.
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 (5)
1. a kind of preparation method of the nano combined oxygen reduction catalysts of PtCoFe/WC-C, it is characterised in that：Comprise the following steps：
1）The chloroplatinic acid of measured amounts（H2PtCl6）Solution, and weigh a certain amount of cobalt chloride（CoCl26H2O）, iron chloride
(FeCl36H2O）And sodium borohydride（NaBH4）, then add excessive ethylene glycol（C2H6O2）Solution, is transferred to after being well mixed
Reacted 12 hours at 200 DEG C in reactor, prepare PtCoFe mixed solutions；
2）Mixed solution is subjected to ultrasound procedure；
3）Mixed solution is inserted into centrifuge tube centrifugally operated；
4）PtCoFe alloy powders are obtained after centrifugation product is placed in into oven drying processing；
5）PtCoFe alloy powders and WC-C powder mechanical mixtures are obtained into the nano combined oxygen reduction catalysts of PtCoFe/WC-C.
2. the preparation method of PtCoFe/WC-C oxygen reduction catalysts according to claim 1, it is characterised in that：The step
Rapid 1）In, platinum source is chloroplatinic acid, and cobalt source is cobalt chloride, and source of iron is iron chloride, by their mixed solutions with sodium borohydride powder
It is dissolved in preparation PtCoFe mixed solutions in ethylene glycol solution；PtCoFe/WC-C powder solvent-thermal method is prepared with mechanical mixing,
Make the solvent-thermal method of reducing agent with ethylene glycol, the formation of product thing phase, the size of particle diameter, form can be controlled, product it is scattered
Property is also preferable.
3. the preparation method of PtCoFe/WC-C oxygen reduction catalysts according to claim 1, it is characterised in that：The step
Rapid 2）In, ultrasonic power is 80%, and ultrasonic time is 1 hour.
4. the preparation method of PtCoFe/WC-C oxygen reduction catalysts according to claim 1, it is characterised in that：The step
Rapid 3）In, centrifugal speed is 10000 rpm, and centrifugation time is 3 minutes.
5. the preparation method of PtCoFe/WC-C oxygen reduction catalysts according to claim 1, it is characterised in that：The step
Rapid 4）In, heating-up temperature is 60 DEG C, and the heat time is 5 hours；In the catalyst of preparation the ratio of tri- kinds of materials of Pt, Co, Fe according to
Secondary is 1：1：1（mg/ mg /mg）.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109888306A (en) * | 2019-03-13 | 2019-06-14 | 西南大学 | The preparation method of WC enhancing PtCoTe oxygen reduction catalyst |
| CN109921045A (en) * | 2017-12-12 | 2019-06-21 | 中国科学院大连化学物理研究所 | It is a kind of using platinum black as the preparation and application of the oxygen electrode catalyst of carrier |
| CN110676469A (en) * | 2019-08-26 | 2020-01-10 | 宁德师范学院 | Carbon-supported platinum-based nanomaterial |
| CN112691687A (en) * | 2020-11-27 | 2021-04-23 | 浙江工业大学 | WC-C palladium-loaded composite material and preparation method and application thereof |
| CN113991130A (en) * | 2021-10-27 | 2022-01-28 | 西安热工研究院有限公司 | Polyacrylonitrile fiber loaded cobalt-nickel alloy composite oxygen reduction catalytic material and preparation method thereof |
| WO2024036823A1 (en) * | 2022-08-19 | 2024-02-22 | 昂华（上海）自动化工程股份有限公司 | Pressurizing and shaping apparatus for battery cell |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109921045A (en) * | 2017-12-12 | 2019-06-21 | 中国科学院大连化学物理研究所 | It is a kind of using platinum black as the preparation and application of the oxygen electrode catalyst of carrier |
| CN109921045B (en) * | 2017-12-12 | 2021-07-20 | 中国科学院大连化学物理研究所 | Preparation and application of oxygen electrode catalyst with platinum black as carrier |
| CN109888306A (en) * | 2019-03-13 | 2019-06-14 | 西南大学 | The preparation method of WC enhancing PtCoTe oxygen reduction catalyst |
| CN110676469A (en) * | 2019-08-26 | 2020-01-10 | 宁德师范学院 | Carbon-supported platinum-based nanomaterial |
| CN110676469B (en) * | 2019-08-26 | 2020-10-27 | 宁德师范学院 | Carbon-supported platinum-based nanomaterial |
| CN112691687A (en) * | 2020-11-27 | 2021-04-23 | 浙江工业大学 | WC-C palladium-loaded composite material and preparation method and application thereof |
| CN113991130A (en) * | 2021-10-27 | 2022-01-28 | 西安热工研究院有限公司 | Polyacrylonitrile fiber loaded cobalt-nickel alloy composite oxygen reduction catalytic material and preparation method thereof |
| CN113991130B (en) * | 2021-10-27 | 2024-01-19 | 西安热工研究院有限公司 | Polyacrylonitrile fiber supported cobalt-nickel alloy composite oxygen reduction catalytic material and preparation method thereof |
| WO2024036823A1 (en) * | 2022-08-19 | 2024-02-22 | 昂华（上海）自动化工程股份有限公司 | Pressurizing and shaping apparatus for battery cell |
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Application publication date: 20171024 |