CN105914381A - Preparation method and application for Pt-Au/GR-SnO<2> methanol fuel cell catalyst - Google Patents

Preparation method and application for Pt-Au/GR-SnO<2> methanol fuel cell catalyst Download PDF

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Publication number
CN105914381A
CN105914381A CN201610492228.6A CN201610492228A CN105914381A CN 105914381 A CN105914381 A CN 105914381A CN 201610492228 A CN201610492228 A CN 201610492228A CN 105914381 A CN105914381 A CN 105914381A
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preparation
catalyst
graphene
graphene oxide
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王尧尧
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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
    • H01M4/9091—Unsupported catalytic particles; loose particulate catalytic materials, e.g. in fluidised state
    • 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
    • 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
    • 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
    • H01M4/928—Unsupported catalytic particles; loose particulate catalytic materials, e.g. in fluidised state
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M8/00—Fuel cells; Manufacture thereof
    • H01M8/10—Fuel cells with solid electrolytes
    • H01M8/1009—Fuel cells with solid electrolytes with one of the reactants being liquid, solid or liquid-charged
    • H01M8/1011—Direct alcohol fuel cells [DAFC], e.g. direct methanol fuel cells [DMFC]
    • 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 relates to the field of a fuel cell catalyst, and particularly to a Pt-Au/GR-SnO<2> methanol fuel cell catalyst and an application thereof. Graphene is partially modified, and an organic functional group is introduced, so that the stability of the graphene structure can be promoted, and the dispersive capacity of nano-alloy particles is improved; therefore, after Pt and Au are formed into the dual-alloy nanoparticles, the nanoparticles can be uniformly dispersed on the surface of a carrier; the utilization rate of Pt and Au is improved while the grain diameter of the metal particles also can be effectively controlled; a little amount of SnO<2> is added to the modified graphene, and the SnO<2> is uniformly dispersed on the surface and in the internal of the graphene; and therefore, the usage amount of the alloy noble metal can be reduced, the activity of the catalyst can be improved, and the stability can be enhanced.

Description

A kind of Pt-Au/GR-SnO 2 Methanol fuel cell catalyst preparation method and application
Technical field
The present invention relates to fuel-cell catalyst field, particularly relate to a kind of Pt-Au/ GR-SnO2Methanol fuel cell catalyst and application thereof.
Background technology
Fuel cell is a kind of device that chemical energy is converted into electric energy, has pollution-free, energy transformation ratio advantages of higher.Precious metals pt reserves in nature are very limited, and a large amount of commercial applications using precious metals pt to make fuel cell are restricted because of catalyst resource problem.It addition, use pure Pt to there is the low problem with less stable of anode of fuel cell performance as fuel battery anode catalyst.Au has the highest electrochemical stability, and resource is abundant relative to Pt many.Research about methanol fuel cell anode catalyzer in recent years is concentrated mainly on noble metal catalyst, such as Pt, Pd, Au etc., and non-precious metal catalyst, although mainly including metal carbides and transition metal oxide. the use of non-precious metal catalyst can be substantially reduced battery cost, but its catalytic efficiency does not reaches far away commercialization requirement, and Pt base catalyst is to aoxidize maximally effective catalyst for methyl alcohol up to now, therefore the research of modified catalyst based on Pt has more realistic meaning.Pt is as anode catalyst, the outstanding problem currently faced is for realizing the most considerable catalysis activity, need certain Pt carrying capacity, and reduce Pt consumption, improve catalyst efficiency to be based primarily upon its macroscopic view composition and the modification of pattern, thus cause its microstructure, including micro-scale and the modulation of level density, and then fundamentally solve the key issue that Pt catalyst exists, as catalyst is poisoned by the reactive intermediates such as CO.
Summary of the invention
The problem existed for prior art, the present invention is for the purpose of improving fuel cell electrode performance, increasing catalyst stability, reduction Pt consumption, it is provided that a kind of Pt-Au/ GR-SnO2Fuel battery anode catalyst and preparation method thereof.
A kind of Pt-Au/ GR-SnO2The preparation method of fuel battery anode catalyst, step is as follows:
1) excess sodium borohydrate is joined in the mixed solution of gold-containing compound and sodium citrate, stir, be subsequently adding the H containing diethylene glycol (DEG) (DEG)2PtCl6Solution, continues stirring 3-12 hour, to Pt-Au alloy nanoparticle after centrifugal, vacuum drying；Wherein platinum compound aqueous solution concentration is 10-3mol/L ~10-2 mol/L；A size of 1-4nm received by Pt-Au alloy, and Pt particle diameter is 0.7-3nm；
2) modified Graphene: graphene oxide is soluble in water, ultrasonic disperse, obtain graphene oxide dispersion, be 3-5 by acetic acid regulation dispersion liquid pH value, add ethylenediamine, stir, reaction terminates the washing of rear deionized water, filters；Then by filter cake dispersion and deionization in the solvent with ethanol, add reducing agent, control reaction temperature and be 60-80 DEG C, back flow reaction 4-10 hour, filtering, wash, be dried to obtain the Graphene that ethylenediamine amine is modified, wherein graphene oxide is 1:5-15 with the mass ratio of ethylenediamine；
Wherein, the dispersion liquid concentration of graphene oxide is 1-2mg/ml, and the addition of borane reducing agent sodium hydride is 1-10 times of graphene oxide quality.
3) by SnO2Joining in above-mentioned modified graphene mixed liquor, move in hydrothermal reaction kettle, 80-100 DEG C seals crystallization 2-6 hour, wherein Graphene and SnO2Mass ratio be 40:1-5, i.e. obtain GR-SnO after ultrasonic disperse2Displacement liquid；GR and SnO2Mass ratio is 50:1-10:1.
4) Pt-Au alloy nanoparticle surface is deposited Cu atomic monolayer, then by the Pt-Au alloy of deposition Cu atomic monolayer at GR-SnO by the method deposited by deficient electromotive force2Soaking 15-30min in displacement liquid, uviol lamp, according to 10-30min, obtains Pt-Au/ GR-SnO2Nanocatalyst.
Preferred version as above-mentioned preparation method: described gold compound is the composition of gold chloride, potassium chloroaurate, gold chloride and potassium chloroaurate.
The present invention also provides for Pt-Au/ GR-SnO prepared by said method2Fuel-cell catalyst, by Pt-Au/ GR-SnO2Nano particle forms, and in catalyst, Pt and Au gross mass degree is 10 ~ 20%, and the mol ratio of described Pt Yu Au is 1:(0.3-0.5).Described NaBH4Concentration be 0.1mmolL-1-1molL-1.Described Pt-Au/ GR-SnO2Diameter range is 4-12nm.
With Graphene as conductive carrier in the present invention, there is bigger specific surface area, can effectively adsorb Au-Pt nano particle, and through applicant, Graphene raw material is groped, by Graphene is carried out partially modified, introduce organo-functional group, the stability of graphene-structured can be conducive to, increase the dispersibility of Nanoalloy particle, make Pt Yu Au form alloy nanoparticle structure and may be uniformly dispersed in carrier surface, while improving Pt Yu Au utilization rate, moreover it is possible to effectively control metallic particles particle diameter；And in modified graphene, add SnO2, disperse on the surface of Graphene and inner homogeneous, it is possible to reduce the usage amount of alloyed precious metal, and by being suitably added SnO2I.e. can play the load effect of carrier, but also effective VOID POSITIONS can be formed with alloy Au-Pt nano particle, increase the electron current densities of fuel-cell catalyst, thus increase electron transmission speed, reduce peroxidating current potential, be the preferable selection of electrode catalytic materials.Conductive carrier has gap structure and big surface area, can be with uniform adsorption Au and Au-Pt nano particle so that Pt Yu Au Nanoalloy even particulate dispersion is at carrier surface, while improving Pt Yu Au utilization rate, moreover it is possible to effectively control metallic particles particle diameter.Nanoalloy particle is less, is conducive to improving catalyst activity, improves its stability.
Compared with prior art, the present invention has the following advantages that and beneficial effect:
1) the Pt-Au/ GR-SnO of the present invention2Fuel battery anode catalyst significantly reduces the content of platinum in catalyst, in active component the molar percentage of Pt can as little as 18%, Pt content is only 3wt%, and the resource of gold is the abundantest, thus the catalyst resource problem that current fuel cell is faced can be solved, reduce cost；
2) the Pt-Au/ GR-SnO of the present invention2Fuel battery anode catalyst, oxygen reduction reaction has the most outstanding catalysis activity, compared with commercially available 20wt% Pt/C catalyst, the area activated of catalyst Pt of the present invention improves 5-8 times, and the mass activity of Pt improves 12 times so that fuel battery performance is greatly improved, and through the grapheme material of modification, stability significantly improves, and in fuel cell Long-Time Service, catalysis activity will not reduce；
3) the Pt-Au/ GR-SnO of the present invention2Fuel cell, by adjusting carrier Graphene-SnO2, optimize the dispersion of alloy nanoparticle, efficiently solve the problem that Pt-Au reunion is serious, hence it is evident that improve uniformity and the utilization rate of catalyst surface Nanoalloy particle, drop low-alloyed cost, be conducive to improving the area activated and mass activity of catalyst.
4) catalyst of the application has good CO resistance performance, for pure H2 fuel and the rich H containing CO2Fuel, remains to show the hydroxide activity of excellence.
Detailed description of the invention
Below in conjunction with detailed description of the invention, the present invention is further detailed explanation.
Embodiment 1
1) excess sodium borohydrate is joined in the mixed solution of gold-containing compound and sodium citrate, stir, be subsequently adding the H containing diethylene glycol (DEG) (DEG)2PtCl6Solution, continues stirring 3 hours, to Pt-Au alloy nanoparticle after centrifugal, vacuum drying；Wherein platinum compound aqueous solution concentration is 10-2mol/L；
2) modified Graphene: graphene oxide is soluble in water, ultrasonic disperse, obtain graphene oxide dispersion, be 5 by acetic acid regulation dispersion liquid pH value, add ethylenediamine, stir, reaction terminates the washing of rear deionized water, filters；Then by filter cake dispersion and deionization in the solvent with ethanol, adding reducing agent, controlling reaction temperature is 80 DEG C, back flow reaction 10 hours, filtering, wash, be dried to obtain the Graphene that ethylenediamine amine is modified, wherein graphene oxide is 1:10 with the mass ratio of ethylenediamine；The dispersion liquid concentration of graphene oxide is 1mg/ml, and the addition of borane reducing agent sodium hydride is 3 times of graphene oxide quality.
3) by SnO2Joining in above-mentioned modified graphene mixed liquor, move in hydrothermal reaction kettle, 80 DEG C seal crystallization 2 hours, wherein Graphene and SnO2Mass ratio be 40:3, i.e. obtain GR-SnO after ultrasonic disperse2Displacement liquid；
4) Pt-Au alloy nanoparticle surface is deposited Cu atomic monolayer, then by the Pt-Au alloy of deposition Cu atomic monolayer at GR-SnO by the method deposited by deficient electromotive force2Soaking 20min in displacement liquid, uviol lamp, according to 30min, obtains Pt-Au/ GR-SnO2Nanocatalyst, wherein the mol ratio of Pt Yu Au is 1:0.3.
Embodiment 2
1) excess sodium borohydrate is joined in the mixed solution of gold-containing compound and sodium citrate, stir, be subsequently adding the H containing diethylene glycol (DEG) (DEG)2PtCl6Solution, continues stirring 5 hours, to Pt-Au alloy nanoparticle after centrifugal, vacuum drying；Wherein platinum compound aqueous solution concentration is 10-3mol/L；
2) modified Graphene: graphene oxide is soluble in water, ultrasonic disperse, obtain graphene oxide dispersion, be 4 by acetic acid regulation dispersion liquid pH value, add ethylenediamine, stir, reaction terminates the washing of rear deionized water, filters；Then by filter cake dispersion with the solvent of deionization and ethanol, adding reducing agent, controlling reaction temperature is 60 DEG C, back flow reaction 8 hours, filters, washs, is dried to obtain the Graphene that ethylenediamine amine is modified, and wherein graphene oxide is 1:15 with the mass ratio of ethylenediamine；The dispersion liquid concentration of graphene oxide is 1mg/ml, and the addition of borane reducing agent sodium hydride is 5 times of graphene oxide quality.
3) by SnO2Joining in above-mentioned modified graphene mixed liquor, move in hydrothermal reaction kettle, 100 DEG C seal crystallization 2 hours, wherein Graphene and SnO2Mass ratio be 40:5, i.e. obtain GR-SnO after ultrasonic disperse2Displacement liquid；
4) Pt-Au alloy nanoparticle surface is deposited Cu atomic monolayer, then by the Pt-Au alloy of deposition Cu atomic monolayer at GR-SnO by the method deposited by deficient electromotive force2Soaking 30min in displacement liquid, uviol lamp, according to 30min, obtains Pt-Au/ GR-SnO2Nanocatalyst, wherein the mol ratio of Pt Yu Au is 1:0.5.
The Pt-Au/ GR-SnO of the present invention2The catalyst performance to methanol catalytic oxidation, solution to be measured: 0.5mol/LH2SO4+1.0mol/LCH3OH At 50Mv/s, quality measurement specific activity (ma/mg Pt) is 1375-1401at 0.75V, exceeds 2-3 times than catalyst such as conventional PtRu/CNT, PtFe/CNT, it may be possible to owing to being doped with a certain amount of transition metal oxide SnO in the Graphene modified at ethylenediamine2, reduce the particle diameter of catalyst particle, improve dispersibility, and the Irreversible Adsorption of intermediate can also be weakened, changing carriers affect affects lattice and the electro transfer of metal, thus improves activity and the stability of catalyst.
Additionally, now there are some researches show that Pd/Pt catalyst peak current density is 376 mA mg- 1, it is Pt/XC-72R (51 mA•mg- 1) more than 7 times, and the catalyst of the present invention can reach about 30 times of common Pt/XC-72R, and effect is fairly obvious.
The present invention is also by prepared Pt-Au/ GR-SnO2Catalyst, is evaluated CO tolerance catalysts and investigates, and uses fixed bed continuous flowing reactive evaluating apparatus to evaluate its catalytic performance: air speed is 9000 mL h-1·g-1, in gas, CO concentration is 1%, O2Concentration is 1 %, H2 Concentration is 45%, and remaining is He gas.
Table 1 different catalysts is to CO reaction evaluating
CO conversion ratio 100%, temperature 24 hours conversion ratios of 40 DEG C of reactions 24 hours conversion ratios of 60 DEG C of reactions
Pt-Au0.3/ GR-SnO2 50℃ 80% 88%
Pt-Au0.5/GR-SnO2 59℃ 80% 87%
Pt-Au/GR 110℃ 68% 60%
The unmodified GR of Pt-Au/ 90℃ 75% 68%
Pt-Au/C 120℃ 43% 37%
Be can be seen that by form, in gas of the present invention, CO conversion ratio is higher, and reaction temperature is relatively low, only just can reach 100% conversion ratio at 50 DEG C, show that in reactive alloys component, CO absorption can effectively oxidize away, and operating for a long time was maintained to higher CO conversion through 24 hours.
The above; it is only the detailed description of the invention of the present invention; but protection scope of the present invention is not limited thereto; any those of ordinary skill in the art are in the technical scope that disclosed herein; the change can expected without creative work or replacement, all should contain within protection scope of the present invention.Therefore, protection scope of the present invention should be as the criterion with the protection domain that claims are limited.

Claims (9)

1. a Pt-Au/GR-SnO2The preparation method of catalyst, it is characterised in that comprise the following steps:
(1) Pt-Au alloy nanoparticle；
(2) ethylenediamine amine modified graphene: graphene oxide is soluble in water, ultrasonic disperse, obtain graphene oxide dispersion, be 3-5 by acetic acid regulation dispersion liquid pH value, add ethylenediamine, stir, reaction terminates the washing of rear deionized water, filters；Then by filter cake dispersion and deionization in the solvent with ethanol, addition sodium borohydride, 60-80 DEG C, back flow reaction 4-10 hour, filters；
(3) by SnO2Join in above-mentioned modified graphene mixed liquor, after ultrasonic disperse, after sealing crystallization, i.e. obtain GR-SnO2Displacement liquid；
(4) Pt-Au alloy nanoparticle surface is deposited Cu atomic monolayer, then by the Pt-Au alloy of deposition Cu atomic monolayer at GR-SnO2Soaking about 15-30min in displacement liquid, uviol lamp is according to about 10-30min.
2. preparation method as claimed in claim 1, it is characterised in that Pt and Au gross mass degree is 10 ~ 20%, and the mol ratio of described Pt Yu Au is 1:(0.3-0.5), Pt-Au/ GR-SnO2Diameter range is about 4-12nm.
3. preparation method as claimed in claim 1, it is characterised in that in catalyst, Pt nano particle diameter is about 0.7-3nm.
4. preparation method as claimed in claim 1 or 2, it is characterised in that the detailed process of step (1) is: is joined by excess sodium borohydrate in the mixed solution of gold-containing compound and sodium citrate, stirs, be subsequently adding the H containing diethylene glycol (DEG) (DEG)2PtCl6Solution, continues stirring 3-12 hour, to Pt-Au alloy nanoparticle after centrifugal, vacuum drying.
5. preparation method as claimed in claim 3, it is characterised in that GR:SnO2Mass ratio is 50:1-10:1.
6. preparation method as claimed in claim 1, it is characterised in that in step (2), the dispersion liquid concentration of graphene oxide is 1-2mg/ml, and the addition of borane reducing agent sodium hydride is 1-10 times of graphene oxide quality.
7. preparation method as claimed in claim 5, it is characterised in that: in step (2), graphene oxide is 1:5-15 with the mass ratio of ethylenediamine.
8. the preparation method as described in claim 5 or 6, it is characterised in that described gold-containing compound is the compositions such as gold chloride, potassium chloroaurate, gold chloride and potassium chloroaurate.
9. the catalyst that preparation method as claimed in claim 1 obtains is in methanol fuel cell, aminic acid fuel battery course of reaction.
CN201610492228.6A 2016-06-29 2016-06-29 Preparation method and application for Pt-Au/GR-SnO<2> methanol fuel cell catalyst Pending CN105914381A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108671929A (en) * 2018-05-02 2018-10-19 大连理工大学 A kind of preparation method of extra small nanometer alloy catalyst for electro-catalysis water decomposition oxygen evolution reaction
CN109560295A (en) * 2018-12-28 2019-04-02 哈尔滨工业大学 Composite catalyst and the preparation method and application thereof based on FeNC catalyst Yu Pt-C catalyst
CN110165227A (en) * 2019-05-15 2019-08-23 北京化工大学 A kind of PtAu nanocatalyst and preparation method thereof with controllable active site spacing

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103084175A (en) * 2013-01-31 2013-05-08 武汉大学 Pt-Au@Pt core-shell structure fuel cell cathode catalyst and preparation method thereof

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103084175A (en) * 2013-01-31 2013-05-08 武汉大学 Pt-Au@Pt core-shell structure fuel cell cathode catalyst and preparation method thereof

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108671929A (en) * 2018-05-02 2018-10-19 大连理工大学 A kind of preparation method of extra small nanometer alloy catalyst for electro-catalysis water decomposition oxygen evolution reaction
CN108671929B (en) * 2018-05-02 2021-05-11 大连理工大学 Preparation method of ultra-small nano alloy catalyst for electrocatalytic water decomposition oxygen evolution reaction
CN109560295A (en) * 2018-12-28 2019-04-02 哈尔滨工业大学 Composite catalyst and the preparation method and application thereof based on FeNC catalyst Yu Pt-C catalyst
CN110165227A (en) * 2019-05-15 2019-08-23 北京化工大学 A kind of PtAu nanocatalyst and preparation method thereof with controllable active site spacing

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Application publication date: 20160831