CN105702972A - Cathode catalyst for fuel cell and preparation method of cathode catalyst - Google Patents

Cathode catalyst for fuel cell and preparation method of cathode catalyst Download PDF

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Publication number
CN105702972A
CN105702972A CN201610223515.7A CN201610223515A CN105702972A CN 105702972 A CN105702972 A CN 105702972A CN 201610223515 A CN201610223515 A CN 201610223515A CN 105702972 A CN105702972 A CN 105702972A
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catalyst
solution
presoma
cathode catalyst
mass percent
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彭秋明
张志伟
李寒宁
刘娜
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Yanshan University
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
    • H01M4/90—Selection of catalytic material
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
    • H01M4/88—Processes of manufacture
    • 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
    • H01M4/9041—Metals or alloys
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
    • H01M4/90—Selection of catalytic material
    • H01M4/9075—Catalytic material supported on carriers, e.g. powder carriers
    • H01M4/9083—Catalytic material supported on carriers, e.g. powder carriers on carbon or graphite
    • 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
    • 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
    • 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

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Materials Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Catalysts (AREA)

Abstract

The invention relates to a cathode catalyst for a fuel cell. The cathode catalyst comprises the following chemical constituents by mass: 80-99% of Ag and 1-20% of M, wherein the M comprises one or more of elements such as Cu, Ru, Rh, Pd, Cd, Ir, Pt and Au, and the mass percent of each element is same when two or more than two elements are contained. A preparation method of the cathode catalyst for the fuel cell mainly comprises the following steps of separately taking elements of silver, aluminum and the M, preparing the elements to a precursor solution, removing the aluminum in a hydrochloric acid solution, and carrying out electrochemical oxidation and reduction induced growth to obtain the A<g-y>M catalyst. The preparation method has the advantages of simplicity, feasibility, low cost and environmental friendliness, and the prepared electric catalyst is small in grain size and high in electrocatalytic activity.

Description

A kind of cathode catalyst for fuel cell and preparation method thereof
Technical field
The invention belongs to field of fuel cell technology, particularly to a kind of fuel-cell catalyst。
Background technology
Nowadays, the overall background that global warming consumes with non-reproducible fossil fuel energy, seriously limit the sustainable development of economic society and the mankind。Therefore, the generation of Renewable Energy Development and memory technology have become as one of current topmost key scientific challenges。In order to tackle this huge challenge, fuel cell becomes the succedaneum of most promising traditional energy。Fuel cell has the advantages such as low in raw material price, aboundresources, theoretical energy density be high, environmentally friendly and completely renewable, and therefore application potential is huge。
The chemical property of battery is had crucial effect by fuel-cell catalyst, also it is weigh the most important mark of battery performance, wherein with platinum and platinum base alloy be representative catalytic performance the most outstanding, yet with the problems such as scarcity of resources, cost intensive and poor stability cause its can not realize large-scale production and business application。Therefore reduce the content of noble metal in catalyst and become the study hotspot of fuel-cell catalyst。
At present, the preparation method of fuel battery cathod catalyst mainly has following several: hydro-thermal method, sol-gel process, microwave polyol method and microemulsion method etc.。The advantage of these methods is that preparation technology is simple, and condition is controlled, and production cost is low。But there is also some inferior positions, the size of such as metal nanoparticle, pattern, dispersibility, stability and the mode of production are but difficult to control。Particle is easily reunited, and causes avtive spot skewness, so catalytic performance instability。In order to better improve the performance of catalyst, it is necessary to the growth pattern of particle is regulated and controled。By regulating and controlling the forming core of particle, growth pattern regulates and controls。By regulating and controlling the forming core of particle, growth pattern, change the Atomic Arrangement structure of its microcosmic, it is possible to prepare the nano metal particles of pattern, size uniform。And then desirably, particle exposes more active site, thus significantly improve the activity of catalyst。This is of great significance for the development tool of catalyst。
At present, preparation about high index polyhedron nanocatalyst both at home and abroad has more report, seminar of Institutes Of Technology Of Taiyuan realizes being prepared for tetrahexahedron iron oxide nanocrystals catalyst (CN104815658A) by controlling the concentration of the phosphate anion in precursor solution, seminar of Xiamen University is prepared for the platinum icosahedron nano crystal catalyst of high catalytic activity (CN101024174A) by the method for electro-deposition, a kind of low-temperature fuel cell nanocrystalline eelctro-catalyst of Pd-Pt polyhedron and preparation method (CN104607183A) have been invented by seminar of University On The Mountain Of Swallows。Basic research shows, the high-index surface of metal single crystal has better catalysis activity relative to low index surface, therefore, prepares the nano-particle of high-index surface, is the important method improving eelctro-catalyst catalysis activity。But, high-index surface in crystal growing process owing to the speed of growth is too fast, it is easy to disappear, finally only remaining low index surface constitute nanocrystal, seriously inhibit catalyst catalysis activity。
Summary of the invention
It is an object of the invention to provide that a kind of preparation method is simple, cost is low, the active high cathode catalyst for fuel cell of catalysis and preparation method thereof。The present invention mainly adopts electrochemical redox induced growth, by scanning under height potential region, regulates the speed of growth of nanocrystal, and then obtains the high-index surface cathode catalyst for fuel cell with high catalytic activity。
The cathode catalyst for fuel cell of the present invention, the mass percent of its chemical composition is Ag80～99%, M1～20%, wherein M includes one or more elements in Cu, Ru, Rh, Pd, Cd, Ir, Pt or Au, when containing two or more element, the mass percent of each element is identical。
The preparation method of above-mentioned cathode catalyst for fuel cell is as follows:
1, raw material:
(1) silver presoma: AgNO3；
(2) aluminum presoma: AlCl3；
(3) M presoma: M includes: Cu, Ru, Rh, Pd, Cd, Ir, Pt or Au, M presoma is chloride or the noble metal acid of metal；
(4) reducing agent: what include in ethylene glycol, sodium borohydride, 1mol/L D/W, 1mol/L aqueous ascorbic acid is any。
2, preparation process:
(1) it is Ag-xAl-yM by the mass percent of above-mentioned raw materials, wherein: the mass percent of x is 0.1～10%, the mass percent of y is 1～20%, surplus is the ratio of Ag, take the precursor solution that silver presoma, aluminum presoma become mass concentration to be 10g/L with M precursor power respectively, be the ratio of 1:10 according to precursor solution with reducing agent volume ratio, reducing agent is added drop-wise in precursor solution, at magnetic stirring apparatus moderate-speed mixer 300r/min, stir 30min；
(2) step (1) solution is put in stainless steel high temperature reactor, at 200 DEG C, heat 2h；
(3) step (2) being obtained product deionized water repeatedly to wash, wash unnecessary ion and reducing agent reaches about PH=7 to solution, centrifugal, at 60 DEG C, dry 12h, obtains Ag-xAl-yM；
(4) add the ratio of 1mgAg-xAl-yM in the hydrochloric acid solution that every ml concn is 3mol/L, the Ag-xAl-yM obtained is joined hydrochloric acid solution, at magnetic stirring apparatus moderate-speed mixer 300r/min, stir 30min；
(5) step (4) being obtained product deionized water repeatedly to wash, reach about PH=7 to solution, centrifugal, at 60 DEG C, dry 12h, obtains Ag-M catalyst；
(6) catalyst uniform load step (5) obtained is on glass-carbon electrode, at 0.1MHClO4In, sweep limits is-0.2V～0.8VvsSCE, scanning 100 circle, and Ag-M catalyst can be made to be attached on glass-carbon electrode。
The present invention compared with prior art has the advantage that
1, under ensureing catalysis activity premise, the consumption of noble metal is decreased, the catalyst cost being substantially reduced；
2. electrocatalyst particles size is little, and electro catalytic activity is high。Electrochemical redox induced growth generates multiaspect height defect binary catalyst, has the catalysis activity higher than business platinum carbon；
3. catalyst activity component variation, can pass through the change regulation and control of metal precursor kind and consumption, prepare multiple catalysts component。
4. preparation method is simple, easy, environmental friendliness。The solvent, the reducing agent that use in preparation process are safe and nontoxic, environmentally safe。
Accompanying drawing explanation
Fig. 1 is the ORR performance comparison figure of Ag-1Pt nanocatalyst and Pt/C in the embodiment of the present invention 1。
Fig. 2 is the specific activity comparison diagram of Ag-10Pd10Cu nanocatalyst and Pt/C in the embodiment of the present invention 2。
Fig. 3 is the mass activity comparison diagram of Ag-10Pd10Cu nanocatalyst and Pt/C in the embodiment of the present invention 2。
Detailed description of the invention
Embodiment 1
1, take mass concentration respectively and be the AgNO of 10g/L3Solution 9.89ml, AlCl3Solution 0.01ml and H2PtCl6Solution 0.1ml, prepares into precursor solution, takes 1mol/L ascorbic acid solution 100ml, is added drop-wise in precursor solution, at magnetic stirring apparatus moderate-speed mixer 300r/min, stirs 30min；
2, the solution of step 1 is put in stainless steel high temperature reactor, at 200 DEG C, heat 2h；
3, step 2 obtaining product repeatedly washed product deionized water repeatedly wash, wash unnecessary ion and reducing agent reaches about PH=7 to solution, centrifugal, at 60 DEG C, dry 12h, obtains Ag-0.1Al-1Pt。
4. 10mgAg-0.1Al-1Pt is joined the hydrochloric acid solution that 10mL concentration is 3mol/L, at magnetic stirring apparatus moderate-speed mixer 300r/min, stirs 30min；
5. step 4 obtaining product deionized water repeatedly wash, reach about PH=7 to solution, centrifugal, at 60 DEG C, dry 12h, obtains Ag-1Pt catalyst。
6. by above-mentioned catalyst uniform load on glass-carbon electrode, at 0.1MHClO4In, sweep limits is-0.2V～0.8VvsSCE, scanning 100 circle, and Ag-1Pt catalyst can be made to be attached on glass-carbon electrode。
As it is shown in figure 1, the LSV curve comparison of Ag-1Pt catalyst and commercial Pt/C catalyst。It can be seen that all commercial Pt/C catalyst corrigendums of ratio of the starting point position of Ag-1Pt catalyst and half wave potential, Limited diffusion current density is close。Illustrate that the catalytic performance of Ag-1Pt catalyst is better than commercial Pt/C catalyst。
Embodiment 2
1, take mass concentration respectively and be the AgNO of 10g/L3Solution 7ml, AlCl3Solution 1ml, H2PdCl6Solution 1ml and CuCl2Solution 1ml, prepares into precursor solution, takes 1mol/L D/W 100ml, is added drop-wise in precursor solution, at magnetic stirring apparatus moderate-speed mixer 300r/min, stirs 30min；
2, the solution of step 1 is put in stainless steel high temperature reactor, at 200 DEG C, heat 2h；
3, step 2 obtaining product repeatedly washed product deionized water repeatedly wash, wash unnecessary ion and reducing agent reaches about PH=7 to solution, centrifugal, at 60 DEG C, dry 12h, obtains Ag-10Al-10Pd10Cu。
4,10mgAg-10Al-10Pd10Cu is joined the hydrochloric acid solution that 10mL concentration is 3mol/L, at magnetic stirring apparatus moderate-speed mixer 300r/min, stir 30min；
5, step 4 obtaining product deionized water repeatedly to wash, reach about PH=7 to solution, centrifugal, at 60 DEG C, dry 12h, obtains Ag-10Pd10Cu catalyst。
6, by above-mentioned catalyst uniform load on glass-carbon electrode, at 0.1MHClO4In, sweep limits is-0.2V～0.8VvsSCE, scanning 100 circle, and Ag-10Pd10Cu catalyst can be made to be attached on glass-carbon electrode。
Specific activity and the mass activity of Ag-10Pd10Cu catalyst and commercial Pt/C catalyst contrast as shown in Figures 2 and 3。It can be seen that when 0.3V and 0.4V, the specific activity of Ag-10Pd10Cu catalyst and mass activity are all significantly better than commercial Pt/C catalyst。Illustrate that the catalytic performance of Ag-10Pd10Cu catalyst is better than commercial Pt/C catalyst。
Embodiment 3
1, take mass concentration respectively and be the AgNO of 10g/L3Solution 9.3ml, AlCl3Solution 0.1ml, HAuCl4Solution 0.2ml, RuCl3Solution 0.2ml and CdCl2Solution 0.2ml, prepares into precursor solution, takes sodium borohydride aqueous solution 100ml, is added drop-wise in precursor solution, at magnetic stirring apparatus moderate-speed mixer 300r/min, stirs 30min；
2, step 1 solution is transferred in stainless steel high temperature reactor, at 200 DEG C, heat 2h；
3, step 2 obtaining product repeatedly washed product deionized water repeatedly wash, wash unnecessary ion and reducing agent reaches about PH=7 to solution, centrifugal, at 60 DEG C, dry 12h, obtains Ag-Al-2Au2Ru2Cd。
4,10mgAg-Al-2Au2Ru2Cd is joined the hydrochloric acid solution that 10mL concentration is 3mol/L, at magnetic stirring apparatus moderate-speed mixer 300r/min, stir 30min；
5, step 4 obtaining product deionized water repeatedly to wash, reach about PH=7 to solution, centrifugal, at 60 DEG C, dry 12h, obtains Ag-2Au2Ru2Cd catalyst。
6, by above-mentioned catalyst uniform load on glass-carbon electrode, at 0.1MHClO4In, sweep limits is-0.2V～0.8VvsSCE, scanning 100 circle, and Ag-2Au2Ru2Cd catalyst can be made to be attached on glass-carbon electrode。
Embodiment 4
1, take mass concentration respectively and be the AgNO of 10g/L3Solution 8.5ml, AlCl3Solution 0.5ml, H2PtCl6Solution 0.25ml, CuCl2Solution 0.25ml, RhCl3Solution 0.25ml and IrCl3Solution 0.25ml, prepares into precursor solution, takes glycol water 100ml, is added drop-wise in precursor solution, at magnetic stirring apparatus moderate-speed mixer 300r/min, stirs 30min；
2, step 1 solution is transferred in stainless steel high temperature reactor, at 200 DEG C, heat 2h；
3, step 2 obtaining product repeatedly washed product deionized water repeatedly wash, wash unnecessary ion and reducing agent reaches about PH=7 to solution, centrifugal, at 60 DEG C, dry 12h, obtains Ag-5Al-2.5Pt2.5Cu2.5Rh2.5Ir。
4,10mgAg-5Al-2.5Pt2.5Cu2.5Rh2.5Ir is joined the hydrochloric acid solution that 10mL concentration is 3mol/L, at magnetic stirring apparatus moderate-speed mixer 300r/min, stir 30min；
5, step 4 obtaining product deionized water repeatedly to wash, reach about PH=7 to solution, centrifugal, at 60 DEG C, dry 12h, obtains Ag-2.5Pt2.5Cu2.5Rh2.5Ir catalyst。
6, by above-mentioned catalyst uniform load on glass-carbon electrode, at 0.1MHClO4In, sweep limits is-0.2V～0.8VvsSCE, and scanning 100 circle, namely Ag-2.5Pt2.5Cu2.5Rh2.5Ir catalyst is attached on glass-carbon electrode。

Claims (2)

1. a cathode catalyst for fuel cell, it is characterized in that: the mass percent of its chemical composition is Ag80～99%, M1～20%, wherein M includes one or more elements in Cu, Ru, Rh, Pd, Cd, Ir, Pt or Au, when containing two or more element, the mass percent of each element is identical。
2. the preparation method of the cathode catalyst for fuel cell of claim 1, it is characterised in that: it comprises the steps:
(1) raw material:
1. silver presoma: AgNO3；
2. aluminum presoma: AlCl3；
3. M presoma: M includes: Cu, Ru, Rh, Pd, Cd, Ir, Pt or Au, M presoma is chloride or the noble metal acid of metal；
4. reducing agent: what include in ethylene glycol, sodium borohydride, 1mol/L D/W, 1mol/L aqueous ascorbic acid is any。
(2) preparation process:
1. it is Ag-xAl-yM by the mass percent of above-mentioned raw materials, wherein: the mass percent of x is 0.1～10%, the mass percent of y is 1～20%, surplus is the ratio of Ag, take the precursor solution that silver presoma, aluminum presoma become mass concentration to be 10g/L with M precursor power respectively, be the ratio of 1:10 according to precursor solution with reducing agent volume ratio, reducing agent is added drop-wise in precursor solution, at magnetic stirring apparatus moderate-speed mixer 300r/min, stir 30min；
2. step 1. solution is put in stainless steel high temperature reactor, at 200 DEG C, heat 2h；
2. 3. step obtaining product deionized water repeatedly wash, wash unnecessary ion and reducing agent reaches about PH=7 to solution, centrifugal, at 60 DEG C, dry 12h, obtains Ag-xAl-yM；
4. add the ratio of 1mgAg-xAl-yM in the hydrochloric acid solution that every ml concn is 3mol/L, the Ag-xAl-yM obtained is joined hydrochloric acid solution, at magnetic stirring apparatus moderate-speed mixer 300r/min, stir 30min；
4. 5. step obtaining product deionized water repeatedly wash, reach about PH=7 to solution, centrifugal, at 60 DEG C, dry 12h, obtains Ag-M catalyst；
6. catalyst uniform load step 5. obtained is on glass-carbon electrode, at 0.1MHClO4In, sweep limits is-0.2V～0.8VvsSCE, scanning 100 circle, and Ag-M catalyst can be made to be attached on glass-carbon electrode。
CN201610223515.7A 2016-04-12 2016-04-12 Cathode catalyst for fuel cell and preparation method of cathode catalyst Pending CN105702972A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107262114A (en) * 2017-06-30 2017-10-20 西南大学 The preparation method of liberation of hydrogen catalyst is combined based on PtAuFe/C in sulfuric acid electrolyte
CN107293757A (en) * 2017-07-05 2017-10-24 西南大学 The preparation method of PtCoFe/WC C oxygen reduction catalysts
CN107887618A (en) * 2017-09-27 2018-04-06 姚乃元 A kind of carbon-based platinum silver palladium ternary alloy catalyst and preparation method thereof

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CN105032412A (en) * 2015-08-06 2015-11-11 厦门大学 Silver/platinum alloy nanometer material with porous hollow structure and preparing method thereof
CN105261766A (en) * 2015-09-09 2016-01-20 华侨大学 PdAg alloy nanotube positive catalyst of direct direct ethanol fuel cell and preparation method of PdAg alloy nanotube positive catalyst

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US20130029252A1 (en) * 2011-07-28 2013-01-31 Man-Yin Lo Fuel cell and electrocatalyst
CN105032412A (en) * 2015-08-06 2015-11-11 厦门大学 Silver/platinum alloy nanometer material with porous hollow structure and preparing method thereof
CN105261766A (en) * 2015-09-09 2016-01-20 华侨大学 PdAg alloy nanotube positive catalyst of direct direct ethanol fuel cell and preparation method of PdAg alloy nanotube positive catalyst

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107262114A (en) * 2017-06-30 2017-10-20 西南大学 The preparation method of liberation of hydrogen catalyst is combined based on PtAuFe/C in sulfuric acid electrolyte
CN107262114B (en) * 2017-06-30 2019-12-10 西南大学 Preparation method of PtAuFe/C composite hydrogen evolution catalyst based on sulfuric acid electrolyte
CN107293757A (en) * 2017-07-05 2017-10-24 西南大学 The preparation method of PtCoFe/WC C oxygen reduction catalysts
CN107887618A (en) * 2017-09-27 2018-04-06 姚乃元 A kind of carbon-based platinum silver palladium ternary alloy catalyst and preparation method thereof
CN107887618B (en) * 2017-09-27 2020-07-24 姚乃元 Carbon-based platinum-silver-palladium ternary alloy catalyst and preparation method thereof

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Application publication date: 20160622