CN109935847A - A kind of preparation method of the loaded platinum base alloy catalyst of low-temperature fuel cell - Google Patents
A kind of preparation method of the loaded platinum base alloy catalyst of low-temperature fuel cell Download PDFInfo
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- CN109935847A CN109935847A CN201711350874.XA CN201711350874A CN109935847A CN 109935847 A CN109935847 A CN 109935847A CN 201711350874 A CN201711350874 A CN 201711350874A CN 109935847 A CN109935847 A CN 109935847A
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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
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- 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
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Abstract
The present invention provides a kind of preparation method of loaded platinum base alloy catalyst, which can be used as Low-Temperature Fuel Cell Catalysts.Preparation method is by support dispersion in solvent, to restore platinum and non-platinum presoma using ethylene glycol as solvent and stabilizer with strong reductant boron hydride, hydrazine hydrate, tetrabutyl boron hydride etc., obtain loaded platinum base alloy nanoparticle.The preparation method that the present invention uses is simple and effective, and no stabilizer difficulty removes problem, and the alloy catalyst being prepared has lesser partial size, uniform particle diameter distribution, while having preferable dispersibility on carrier.In addition, the catalyst can show higher area specific activity and unit mass Pt specific activity to oxygen reduction reaction, the dosage of platinum can be effectively reduced, there is potential application prospect in low-temperature fuel cell.
Description
Technical field
The present invention relates to alloy nano catalyst more particularly to a kind of loaded platinum base alloy of low-temperature fuel cell to be catalyzed
The preparation method of agent.
Background technique
With fossil energy increasingly depleted and environmental pollution and climate change it is increasingly serious, clean energy resource is
Cause the great attention of countries in the world.Proton Exchange Membrane Fuel Cells has cleaning, efficient, power density height and low temperature fast
It the advantages that speed starting, has a wide range of applications in the fields such as vehicle power supply and distributed power generation.But pem fuel is electric
The commercialization in pond is faced with problem at high cost, and wherein catalyst occupies very big specific gravity, because catalyst uses Pt, and the money of Pt
Source is limited, therefore price is very high.In order to reduce the cost of fuel cell, it is necessary to which the dosage for reducing Pt, this requires improve unit
The catalytic activity (mass activity) of quality Pt, the especially catalytic activity of cathodic oxygen reduction, because the dynamics of hydrogen reduction determines
It is a relatively slowly reaction.
It is to improve catalytic oxygen reduction activity that Pt and non-Pt element, which are formed alloy, to reduce having for Pt dosage and cost
One of efficacious prescriptions method.Preparation method in relation to Pt based alloy catalyst is a lot of, such as liquid phase reduction, microemulsion method, electrochemical deposition
Method, vapour deposition process and dipping-high temperature reduction method etc., wherein liquid phase reduction is because production equipment is simple, is conducive to extensive quotient
Industry becomes most widely used one of method.
Using the ethylene glycol with stabilization, easily removed as the reduction of ethylene glycol method of solvent, be developed recently get up one
Kind method, easily controllable metal partial size and dispersion, and it is easy to operate.But ethylene glycol is weak reductant, is unfavorable for restoring non-expensive
Metal is to prepare alloy catalyst.Bo-carsly etc. prepares PtSnO catalyst using reduction of ethylene glycol method, the result shows that, Sn is complete
Portion exists in the form of an oxide, and PtSn alloy is not present.
The strong reductants reduction method such as sodium borohydride is to prepare a kind of most commonly used method of alloy catalyst.Traditional boron
Hydrogenation sodium reduction takes water as a solvent, and guarantees the partial size and dispersion degree of metallic particles by the way that surfactant is added, but still past
Toward there is the problem that catalyst granules is unevenly distributed, alloying pellet is oversized, and the binding force of surfactant and platinum etc.
It is relatively strong, it is difficult to which that washing removal influences catalyst activity.It is complicated for operation by the stable sodium borohydride reduction of surfactant, only
Suitable for small-scale experimental study.
In conclusion there is an urgent need to develop a kind of simple and effective fuel cell platinum alloy catalyst preparation method.
Summary of the invention
A kind of sodium borohydride reduction that ethylene glycol is stable is provided the purpose of the present invention is overcome the deficiencies in the prior art
Platinum alloy fuel cell catalyst is prepared, the fuel cell platinum alloy catalyst granular size of this method preparation is controllable, partial size divides
Uniform, catalytic activity height is dissipated, operation is simple, and production cost is low, is advantageously implemented large-scale production.
To achieve the above object, the technical solution adopted by the present invention includes the following steps
(1) water solubility Pt presoma and non-Pt precursor mixed solution, the atomic ratio of Pt and non-Pt are prepared with deionized water
For 1:10-10:1, preferably 1:5-5:1.Stirring, is allowed to uniformly mixed.
(2) in ethylene glycol, carrier is added, stirs 10-30min, ultrasonic 30-60min is allowed to evenly dispersed；
(3) dispersion liquid is stirred into 30-60min under 0-90 DEG C of (preferably 25-80 DEG C) reaction temperature, is passed through in whipping process
N2Or Ar, form the inert atmosphere of reaction system；
(4) reducing agent is added in above-mentioned dispersion liquid, Pt and non-Pt precursor mixed solution is then added, so that system
Middle Pt and non-Pt element total mol concentration are 0.5-10mmol/L (preferably 1-5mmol/L), the molar concentration of reducing agent be Pt and
5-100 times (preferably 10-30 times) of non-Pt element total mol concentration.It is reacted under 0-90 DEG C of (preferably 25-80 DEG C) reaction temperature
0.5-24h (preferably 3-12h).
(5) after reaction, be centrifuged or be separated by filtration, successively washed 3-5 times with ethyl alcohol and deionized water respectively, then in
8-20h is dried in vacuo at 60-100 DEG C.
(6) to make platinum alloy catalyst form rich platinum surface layer, 2-5 drop 2mol/L dust technology can be added in when washing, favorably
In formation surface layer richness Pt catalyst (dust technology can also be added without when washing).
The water-soluble Pt presoma is nitrate, amine complex, halogen acids or the halogen acid salt of Pt；Described is water-soluble
Property non-Pt presoma be Ru, Rh, Pd, Au, Ag, Fe, Co, Ni, Cu nitrate, halide, amine complex, halogen acids or hydrogen halogen
Hydrochlorate；The carrier is conductive black, carbon nanotube, graphene, polyaniline, polypyrrole, poly-dopamine or metal nitride.
The reducing agent is one of boron hydride, hydrazine hydrate, tetrabutyl boron hydride or two kinds or more.
Prepared Pt based alloy catalyst is spherical or almost spherical nanoparticle, partial size 1-5nm.
Ethylene glycol doubles as solvent and protective agent, but not as reducing agent；The present invention doubles as solvent and stabilizer with ethylene glycol,
The strong reductants such as sodium borohydride are reducing agent, are prepared for a series of Pt alloy catalysts, preparation method is simple and effective, reaction process
Without adjusting pH, stabilizer is easily removed after reaction, and obtained alloy catalyst has biggish electrochemical surface area, lesser
Partial size and uniform particle diameter distribution, while having good dispersibility on carrier.By changing the type of metal precursor and dense
Degree can prepare the alloy catalyst of various different compositions.The Pt alloy nano particle that the present invention obtains is reducing platinum dosage
Improve oxygen reduction catalytic activity simultaneously, and there is the electrochemical stability better than commercialization Pt/C, fuel cell and other
Electrochemical field has potential application prospect.
Detailed description of the invention
Fig. 1 is the TEM photo of the alloy nano particle of different Pt/Co atomic ratios prepared by the embodiment of the present invention 1.It is shown in figure
Show Pt4Co、Pt3Co、Pt2Co、PtCo、PtCo2Lesser partial size is all had, and there is uniform distribution on the carbon carrier.
Fig. 2 is the PtCo/C alloy catalyst and Johnson of different Pt/Co atomic ratios prepared by the embodiment of the present invention 1
Cyclic voltammetric (CV) curve of Matthey company 20%Pt/C (JM) catalyst.Solution is N2The 0.1M HClO of saturation4, scanning
Speed is 50mVs-1, room temperature test.Compared with Pt/C (JM), the reduction spike potential of Pt alloy surface oxide is shuffled, explanation
Pt alloy surface oxide is easier to remove, so that the reaction rate of ORR is accelerated.
Fig. 3 is the PtCo/C alloy catalyst and Johnson of different Pt/Co atomic ratios prepared by the embodiment of the present invention 1
Hydrogen reduction polarization (ORR) curve of Matthey company 20%Pt/C (JM) catalyst.Solution is O2The 0.1M HClO of saturation4, sweep
Retouching speed is 10mVs-1, forward scan, RDE revolving speed is 1600rpm, room temperature test.The PtCo/C it can be seen from hydrogen reduction curve
The half wave potential of alloy is higher than Pt/C (J M).
Fig. 4 is the Pt Co/C alloy catalyst and 20%Pt/C of different Pt/Co atomic ratios prepared by the embodiment of the present invention 1
(JM) unit mass Pt catalytic activity of the catalyst in hydrogen reduction polarization (ORR) curve test at 0.9V (vs.R HE).As a result
It has been shown that, Pt Co/C catalyst towards oxygen reduction reaction prepared by the embodiment of the present invention 1 show higher catalytic activity.
Fig. 5 is Pt Ni alloy nano particle TEM photo prepared by the embodiment of the present invention 2.The average grain diameter of particle is
1.5nm。
Fig. 6 is Pt Ni alloy nano particle TEM photo prepared by the embodiment of the present invention 3.The average grain diameter of particle is
1.7nm。
Fig. 7 is Pt Ni/C catalyst prepared by the embodiment of the present invention 3 and 20%Pt/C (JM) catalyst in rotating circular disk electricity
CV curve and polarization curves of oxygen reduction in the test of pole (RDE).CV test is N with electrolyte2The 0.1M HClO of saturation4, scanning speed
Degree is 50mVs-1.It is O that polarization curves of oxygen reduction, which tests electrolyte used,2The 0.1M HClO of saturation4, sweeping speed is 10mVs-1, just
To scanning, RDE revolving speed is 1600rpm, and test carries out at room temperature, and total metal load amount is 20ug cm on electrode-2。
Fig. 8 is that Pt Ni/C catalyst prepared by the embodiment of the present invention 3 declines with the acceleration of 20%Pt/C (JM) catalyst half-cell
The unit mass Pt catalytic activity for subtracting front and back compares.
Specific embodiment
Embodiment 1:
(1) by H2PtCl6·6H2O and CoCl2·6H2O is dissolved in 2ml deionized water, and the atomic ratio of Pt and Co is 4:1, and 3:
1,2:1,1:1,1:2.Stirring, is allowed to uniformly mixed.
(2) in ethylene glycol, carrier is added, stirs 10min, ultrasonic 30min is allowed to evenly dispersed；
(3) 30min is stirred at room temperature in dispersion liquid, is passed through N in whipping process2Or Ar, form the inertia of reaction system
Atmosphere；
(4) reducing agent is added in above-mentioned dispersion liquid, Pt and Co precursor mixed solution is then added, stirs at room temperature
Mix 3h.So that Pt and Co element total mol concentration is respectively 3.6mmol/L, 3.75mmol/L, 3.9mmol/L in system,
4.2mmol/L and 4.95mmol/L, the molar concentration of reducing agent are the 18.5,17.8 of Pt and Co element total mol concentration respectively,
17.4,16.6,14.9 times.
(5) after reaction, it is centrifuged or is separated by filtration, successively washed 3 times with ethyl alcohol and deionized water respectively, then in 80
10h is dried in vacuo at DEG C.
Embodiment 2:
(1) by water-soluble Pt presoma K2PtCl4With Ni presoma NiCl2·6H2O (please provide specific example) is dissolved in 2ml
In deionized water, the atomic ratio of Pt and Ni are 1:2.Stirring, is allowed to uniformly mixed.
(2) in ethylene glycol, carrier is added, stirs 10min, ultrasonic 30min is allowed to evenly dispersed；
(3) 30min is stirred at room temperature in dispersion liquid, is passed through N in whipping process2Or Ar, form the inertia of reaction system
Atmosphere；
(4) reducing agent is added in above-mentioned dispersion liquid, Pt and Ni precursor mixed solution is then added, stirs at room temperature
12h is mixed, so that Pt and Ni element total concentration is 6mmol/L in system, the molar concentration of reducing agent is Pt and Ni element total moles
12.7 times of concentration.
(5) after reaction, it is centrifuged or is separated by filtration, successively washed 5 times with ethyl alcohol and deionized water respectively, and wash every time
2-5 drop 2mol/L dust technology is added when washing, is then dried in vacuo 10h at 80 DEG C.
Embodiment 3:
(1) by Na2PtCl6·6H2O and Ni (NO3)2·6H2O molten (please provide specific example) is in 2ml deionized water, Pt
Atomic ratio with Ni is 1:2.Stirring, is allowed to uniformly mixed.
(2) in ethylene glycol, carrier is added, stirs 10min, ultrasonic 30min is allowed to evenly dispersed；
(3) 30min is stirred at room temperature in dispersion liquid, is passed through N in whipping process2Or Ar, form the inertia of reaction system
Atmosphere；
(4) reducing agent is added in above-mentioned dispersion liquid, Pt and Ni precursor mixed solution is then added, so that in system
Pt and Ni element total concentration is 6mmol/L, and the molar concentration of reducing agent is 12.7 times of Pt and Ni element total mol concentration.80
3h is stirred under DEG C reaction temperature.
(5) after reaction, it is centrifuged or is separated by filtration, successively washed 4 times with ethyl alcohol and deionized water respectively, then in 60
12h is dried in vacuo at DEG C.
Claims (8)
1. a kind of low-temperature fuel cell preparation method of loaded platinum base alloy catalyst, which is characterized in that preparation method packet
Include following steps,
1) water solubility Pt presoma and non-Pt precursor mixed solution are prepared with deionized water, stirred evenly；The original of Pt and non-Pt
Son is than being 1:10-10:1；
2) in ethylene glycol, carrier is added, stirs 10-30min, ultrasonic 30-60min, is allowed to evenly dispersed formation dispersion liquid；
3) dispersion liquid is passed through N in 0-90 DEG C of stirring 30-60min, whipping process2Or Ar, form the indifferent gas of reaction system
Atmosphere；
4) reducing agent is added in above-mentioned dispersion liquid, Pt presoma and non-Pt precursor mixed solution is then added, then exists
0.5-24h is reacted at 0-90 DEG C；Pt and non-Pt element total mol concentration are 0.5-10mmol/L in system, reducing agent it is mole dense
Degree is 5-100 times of Pt and non-Pt element total mol concentration；
5) it after reaction, is centrifuged or is separated by filtration, successively washed 3-5 times with ethyl alcohol and deionized water respectively, then in 60-
8-20h is dried in vacuo at 100 DEG C.
2. preparation method described in accordance with the claim 1, which is characterized in that the water-soluble Pt presoma used is the nitric acid of Pt
Salt, amine complex, halogen acids or halogen acid salt；The non-Pt presoma of water solubility used is Ru, Rh, Pd, Au, Ag, Fe, Co, Ni,
Nitrate, halide, amine complex, halogen acids or the halogen acid salt of one of Cu or two kinds or more；Carrier be conductive black,
Carbon nanotube, graphene, polyaniline, one of polypyrrole, poly-dopamine or metal nitride or two kinds or more, Pt and non-Pt
Metal quality load capacity is 10wt%-20wt%.
3. preparation method described in accordance with the claim 1, which is characterized in that the reducing agent is boron hydride, hydrazine hydrate, four fourths
One of base boron hydride or two kinds or more.
4. preparation method described in accordance with the claim 1, which is characterized in that when non-Pt presoma is base metal presoma,
In step 4), 2-5 drop 2mol/L dust technology can be added in when washing.
5. preparation method described in accordance with the claim 1, which is characterized in that reaction temperature is preferably 25-80 DEG C in step 4).
6. according to preparation method described in claim 1 or 4, which is characterized in that being stirred to react the time in step 4) is preferably 3-
12h。
7. preparation method described in accordance with the claim 1, which is characterized in that in step 5), Pt and non-Pt element total mol concentration
Preferably 1-5mmol/L.
8. preparation method described in accordance with the claim 1, it is characterised in that: prepared Pt based alloy catalyst is spherical or close
Like nano spherical particle, partial size 1-5nm.
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| CN110404531A (en) * | 2019-08-30 | 2019-11-05 | 北京邮电大学 | A kind of method of the reducing loaded noble metal catalyst for obtaining atom level dispersion of one step |
| CN110676469A (en) * | 2019-08-26 | 2020-01-10 | 宁德师范学院 | Carbon-supported platinum-based nanomaterial |
| CN110718695A (en) * | 2019-11-11 | 2020-01-21 | 北京化工大学 | Platinum-based catalytic system for formic acid fuel cell and preparation method thereof |
| CN110943234A (en) * | 2019-12-31 | 2020-03-31 | 南京工业大学 | High-performance platinum alloy catalyst based on magnetic regulation and control and preparation method thereof |
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| CN110404531A (en) * | 2019-08-30 | 2019-11-05 | 北京邮电大学 | A kind of method of the reducing loaded noble metal catalyst for obtaining atom level dispersion of one step |
| CN110718695A (en) * | 2019-11-11 | 2020-01-21 | 北京化工大学 | Platinum-based catalytic system for formic acid fuel cell and preparation method thereof |
| CN111146460A (en) * | 2019-12-30 | 2020-05-12 | 一汽解放汽车有限公司 | Fuel cell alloy catalyst, preparation method thereof and application thereof in fuel cell |
| CN110943234B (en) * | 2019-12-31 | 2022-09-20 | 南京工业大学 | High-performance platinum alloy catalyst based on magnetic regulation and control and preparation method thereof |
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| CN111054334A (en) * | 2020-01-16 | 2020-04-24 | 浙江高成绿能科技有限公司 | Preparation method of high-activity supported binary alloy catalyst |
| CN112201798A (en) * | 2020-09-01 | 2021-01-08 | 深圳航天科技创新研究院 | Metal catalyst, mass preparation method thereof and fuel cell |
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| CN114618482A (en) * | 2020-12-11 | 2022-06-14 | 中国科学院大连化学物理研究所 | Preparation method of platinum-rhodium alloy, preparation method of platinum-rhodium alloy catalyst and application of platinum-rhodium alloy catalyst |
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| CN113258090A (en) * | 2021-06-23 | 2021-08-13 | 南京大学 | Transition metal doped Pt/C fuel cell catalyst and preparation method thereof |
| CN114420956A (en) * | 2021-11-19 | 2022-04-29 | 东北电力大学 | Preparation method of anode electrocatalyst CuNi/C of direct methanol fuel cell |
| CN114420956B (en) * | 2021-11-19 | 2024-03-29 | 东北电力大学 | Preparation method of direct methanol fuel cell anode electrocatalyst CuNi/C |
| CN115240899A (en) * | 2022-08-05 | 2022-10-25 | 广东顺德弘暻电子有限公司 | Low-cost, low-sheet-resistance and high-stability thick film resistor paste and preparation method thereof |
| CN115966716A (en) * | 2023-01-10 | 2023-04-14 | 福州大学 | Preparation method of metal nitride stable Pt-based alloy fuel cell catalyst |
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