CN1661836A - Method for preparing Pt-Ru/C catalyst in use for direct methanol fuel cell - Google Patents

Method for preparing Pt-Ru/C catalyst in use for direct methanol fuel cell Download PDF

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CN1661836A
CN1661836A CN2005100096984A CN200510009698A CN1661836A CN 1661836 A CN1661836 A CN 1661836A CN 2005100096984 A CN2005100096984 A CN 2005100096984A CN 200510009698 A CN200510009698 A CN 200510009698A CN 1661836 A CN1661836 A CN 1661836A
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carbon
catalyst
preparation
fuel cell
compound
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CN1299375C (en
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尹鸽平
王振波
史鹏飞
程新群
杜春雨
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Harbin Institute of Technology
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Harbin Institute of Technology
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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

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Abstract

The method includes following steps: adding processed carbon carrier into mixed liquor of deionized water and isopropyl alcohol and dispersing them evenly; adding predecessor of Pt and Ru compound into evenly dispersed serum containing carbon, drying the said serum through magnetic stirring under constant temperature 50-80 deg.C; grinding the obtained powder of carbon carried predecessor of Pt and Ru compound for ten minutes; deoxidizing the said carbon carried compound in mixed gas of hydrogen and nitrogen gases for 1-3 hours under 350-420 deg.C. The disclosed (NH4)2PtCl6 or (NH4)2RuCl5 is as solid, possessing lower decomposition temperature. Spongy Pt or Ru generated by deoxidizing the said solid forms skeleton structure in porous so as to raise surface area of electrochemical activity ratio and use rate of catalyst.

Description

Direct methanol fuel cell Pt-Ru/C Preparation of catalysts method
Technical field:
The present invention relates to a kind of preparation method of direct methanol fuel cell anode catalyst.
Background technology:
Direct methanol fuel cell (DMFC) is a fuel with liquid state or gaseous methanol, need not external reformer unit, have energy conversion efficiency height, pollution-free, noiselessness, system configuration is simple, energy density is high and fuel carries and replenishes advantages such as convenient, be specially adapted to the vehicles, compact power and extremely people pay close attention to.The research of direct methanol fuel cell mainly concentrates in the research of anode catalyst and resistance alkoxide polymer dielectric film at present; DMFC is not high, the serious polarization of electroxidation activity of methyl alcohol at low temperatures, is the main cause of its loss in efficiency, needs further to improve the activity of methyl alcohol anode electrocatalyst.The Pt-Ru binary catalyst has the ability of ability that anti-preferably CO poisons and higher methanol electro-oxidizing, has obtained using widely in DMFC.But this catalyst costs an arm and a leg, resource-constrained, thus cause direct methanol fuel cell to hold at high price, be difficult to realize commercialization.Therefore people wish to improve as much as possible activity and the utilization rate of metallic catalyst, reduce the cost of catalyst.At present, people mainly concentrate in the improvement of traditional preparation process method the research of catalyst, and the catalytic activity of Pt-Ru/C catalyst is subjected to multiple factor affecting.And Pt and Ru compound presoma are very remarkable to the performance impact of catalyst, and adopt preparation method's difference of the catalyst of different presomas.The extensive presoma that adopts of people is H at present 2PtCl 6And RuCl 3, adopting immersion reduction method, the catalyst particle size of preparation is bigger, and the utilance of catalyst is lower.With Pt (NH 3) 4Cl 2, Pt (NH 3) 2(NO 2) 2And Ru (NH 3) 4Cl 2Adopt the methods such as ion-exchange or electrochemical reduction Deng for presoma, can prepare small size, the catalyst that catalytic activity is higher; But Pt (NH 3) 4Cl 2, Pt (NH 3) 2(NO 2) 2And Ru (NH 3) 4Cl 2Difficult Deng the presoma preparation, and price is very expensive.Therefore it is more suitable to seek, and the presoma of cheap Pt-Ru catalyst becomes the task of top priority in the direct methanol fuel cell research work.
Summary of the invention:
The purpose of this invention is to provide a kind of direct methanol fuel cell Pt-Ru/C Preparation of catalysts method, it is simple that this method has preparation technology, the catalyst activity of preparation and utilance height, the characteristics that cost is low.Method of the present invention realizes by following step: one, carbon carrier is carried out following processing: 1. carbon carrier is placed high-pressure steam to handle 3-12 hour, carbon carrier is taken out the final vacuum drying; 2. the carbon carrier that steam treatment is crossed is heated to 400-1000 ℃ of processing 1-3 hour in the tube furnace inert gas; Two, the carbon carrier with above-mentioned processing joins in the mixed solution of deionized water and isopropyl alcohol, is uniformly dispersed; Three, Pt and Ru compound presoma are joined in the finely dispersed carbon containing slurries, Pt and Ru compound presoma are dispersed on the carbon carrier; Four, finely dispersed carbon is carried Pt and Ru compound presoma slurries make its drying under 50-80 ℃ of constant temperature magnetic agitation; Five, the carbon that obtains is carried Pt and Ru compound precursor powder, in agate mortar, ground 10 minutes; Six, carbon is carried Pt and Ru compound in the mist of hydrogen and argon gas, temperature is that reduction promptly obtained the Pt-Ru/C catalyst that direct methanol fuel cell is used in 1-3 hour under the 350-420 ℃ of condition.The VulcanXC-72 carbon dust that described carbon carrier is produced for Cabot company.Described Pt and Ru compound presoma are (NH 4) 2PtCl 6Or (NH 4) 2RuCl 5Described and (NH 4) 2RuCl 5The Pt presoma that matches is H 2PtCl 6, Pt (NH 3) 4Cl 2Or Pt (NH 3) 2(NO 2) 2Described and (NH 4) 2PtCl 6The Ru presoma that matches is Ru (OH) 3, Ru (NO 3) 2, RuCl 3Or Ru (NH 3) 4Cl 2The pressure of described step 1 mesohigh steam is 0.1～1.5MPa.Inert gas in the described step 1 is the mist of hydrogen and argon gas, and the volume ratio of its hydrogen and argon gas is 1: 1.The volume ratio of its deionized water of the mixed solution of deionized water and isopropyl alcohol and isopropyl alcohol is 1: 1 in the described step 2.The present invention (NH 4) 2PtCl 6Or (NH 4) 2RuCl 5Be solid, more easily preparation, and have lower decomposition temperature; The good main cause of Pt-Ru/C catalyst performance take it as presoma is (NH 4) 2PtCl 6Or (NH 4) 2RuCl 5The spongy Pt or the Ru that generate after the reduction have formed the cellular skeleton structure, improve the electrochemically active specific surface area of catalyst, are conducive to simultaneously the diffusion of methyl alcohol in catalyst, improve the utilization rate of catalyst.This spongy porous Pt-Ru particle is bigger, for about 10nm.It is simple that the present invention has preparation technology, the catalyst activity of preparation and utilance height, the advantage that cost is low.
Embodiment:
Embodiment one: the method for present embodiment realizes by following step: one, carbon carrier is carried out following processing: 1. carbon carrier is placed high-pressure steam to handle 3-12 hour, carbon carrier is taken out the final vacuum drying; 2. the carbon carrier that steam treatment is crossed is heated to 400-1000 ℃ of processing 1-3 hour in the tube furnace inert gas; Two, the carbon carrier with above-mentioned processing joins in the mixed solution of deionized water and isopropyl alcohol, is uniformly dispersed; Three, Pt and Ru compound presoma are joined in the finely dispersed carbon containing slurries, Pt and Ru compound presoma are dispersed on the carbon carrier; Four, finely dispersed carbon is carried Pt and Ru compound presoma slurries make its drying under 50-80 ℃ of constant temperature magnetic agitation; Five, the carbon that obtains is carried Pt and Ru compound precursor powder, in agate mortar, ground 10 minutes; Six, carbon is carried Pt and Ru compound in the mist of hydrogen and argon gas, temperature is that reduction promptly obtained the Pt-Ru/C catalyst that direct methanol fuel cell is used in 1-3 hour under the 350-420 ℃ of condition.The Vulcan XC-72 carbon dust that described carbon carrier is produced for Cabot company.Described Pt and Ru compound presoma are (NH 4) 2PtCl 6Or (NH 4) 2RuCl 5Described and (NH 4) 2RuCl 5The Pt presoma that matches is H 2PtCl 6, Pt (NH 3) 4Cl 2Or Pt (NH 3) 2(NO 2) 2Described and (NH 4) 2PtCl 6The Ru presoma that matches is Ru (OH) 3, Ru (NO 3) 2, RuCl 3Or Ru (NH 3) 4Cl 2The pressure of described step 1 mesohigh steam is 0.1～1.5MPa.Inert gas in the described step 1 is the mist of hydrogen and argon gas, and the volume ratio of its hydrogen and argon gas is 1: 1.The volume ratio of its deionized water of the mixed solution of deionized water and isopropyl alcohol and isopropyl alcohol is 1: 1 in the described step 2.
The specific embodiment two: take by weighing the Vulcan XC-72 carbon dust that 200mg process steam and heat treated Cabot company produce, join in the mixed solution of deionized water and isopropyl alcohol, be uniformly dispersed; Add 87.8mg (NH 4) 2PtCl 6With 25.7mg Ru (OH) 3, it is dispersed on the carbon carrier, dry under 60 ℃ of temperature constant magnetic stirrings, obtain carbon and carry (NH 4) 2PtCl 6And Ru (OH) 3Powder ground 10 minutes in agate mortar.Carbon with gained carries (NH then 4) 2PtCl 6And Ru (OH) 3Powder places tube furnace, in the mist (volume ratio is 1: 1) of hydrogen and argon gas, temperature is under 360 ℃ the condition, and reductase 12 hour.Make the Pt-Ru/C catalyst, particle diameter is 8-10nm, and electrochemically active specific surface area is 81.22m 2/ g.
The specific embodiment three: take by weighing the Vulcan XC-72 carbon dust that 200mg process steam and heat treated Cabot company produce, join in the mixed solution of deionized water and isopropyl alcohol, be uniformly dispersed; Add 87.8mg (NH 4) 2PtCl 6With 0.84ml 0.2mol/L RuCl 3, it is dispersed on the carbon carrier, dry under 80 ℃ of temperature constant magnetic stirrings, obtain carbon and carry (NH 4) 2PtCl 6And RuCl 3Powder ground 10 minutes in agate mortar.Carbon with gained carries (NH then 4) 2PtCl 6And RuCl 3Powder places tube furnace, in the mist (volume ratio is 1: 1) of hydrogen and argon gas, temperature is under 400 ℃ of conditions, and reductase 12 hour.Make the Pt-Ru/C catalyst, particle diameter is 8-10nm, and electrochemically active specific surface area is 89.81m 2/ g.
The specific embodiment four: take by weighing the Vulcan XC-72 carbon dust that 200mg process steam and heat treated Cabot company produce, join in the mixed solution of deionized water and isopropyl alcohol, be uniformly dispersed; Add 87.8mg (NH 4) 2PtCl 6With 1.84ml 0.0917mol/L Ru (NO 3) 2, it is dispersed on the carbon carrier, dry under 70 ℃ of temperature constant magnetic stirrings, obtain carbon and carry (NH 4) 2PtCl 6And Ru (NO 3) 2Powder ground 10 minutes in agate mortar.Carbon with gained carries (NH then 4) 2PtCl 6And Ru (NO 3) 2Powder places tube furnace, in the mist (volume ratio is 1: 1) of hydrogen and argon gas, temperature is under 360 ℃ of conditions, and reductase 12 hour.Make the Pt-Ru/C catalyst, particle diameter is 9-11nm, and electrochemically active specific surface area is 78.53m 2/ g.
The specific embodiment five: take by weighing the Vulcan XC-72 carbon dust that 200mg process steam and heat treated Cabot company produce, join in the mixed solution of deionized water and isopropyl alcohol, be uniformly dispersed; Add 43.5mg (NH 4) 2RuCl 5With 1.46ml 0.1158mol/L H 2PtCl 6, it is dispersed on the carbon carrier, dry under 70 ℃ of temperature constant magnetic stirrings, obtain carbon and carry (NH 4) 2RuCl 5And H 2PtCl 6Powder ground 10 minutes in agate mortar.Carbon with gained carries (NH then 4) 2RuCl 5And H 2PtCl 6Powder places tube furnace, in the mist (volume ratio is 1: 1) of hydrogen and argon gas, temperature is under 380 ℃ of conditions, and reductase 12 .5 hour.Make the Pt-Ru/C catalyst, particle diameter is 7-9nm, and electrochemically active specific surface area is 69.78m 2/ g.
The specific embodiment six: take by weighing the Vulcan XC-72 carbon dust that 200mg process steam and heat treated Cabot company produce, join in the mixed solution of deionized water and isopropyl alcohol, be uniformly dispersed; Add 43.5mg (NH 4) 2RuCl 5With 6.78ml 0.0249mol/L Pt (NH 3) 4Cl 2, it is dispersed on the carbon carrier, dry under 50 ℃ of temperature constant magnetic stirrings, obtain carbon and carry (NH 4) 2RuCl 5And Pt (NH 3) 4Cl 2Powder ground 10 minutes in agate mortar.Carbon with gained carries (NH then 4) 2RuCl 5And Pt (NH 3) 4Cl 2Powder places tube furnace, in the mist (volume ratio is 1: 1) of hydrogen and argon gas, temperature is under 370 ℃ of conditions, and reductase 12 hour.Make the Pt-Ru/C catalyst, particle diameter is 7-9nm, and electrochemically active specific surface area is 75.68m 2/ g.
The specific embodiment seven: take by weighing the Vulcan XC-72 carbon dust that 200mg process steam and heat treated Cabot company produce, join in the mixed solution of deionized water and isopropyl alcohol, be uniformly dispersed; Add 43.5mg (NH 4) 2RuCl 5With 6.77ml 0.0249mol/L Pt (NH 3) 2(NO 2) 2, it is dispersed on the carbon carrier, dry under 50 ℃ of temperature constant magnetic stirrings, obtain carbon and carry (NH 4) 2RuCl 5And Pt (NH 3) 2(NO 2) 2Powder ground 10 minutes in agate mortar.Carbon with gained carries (NH then 4) 2RuCl 5And Pt (NH 3) 2(NO 2) 2Powder places tube furnace, in the mist (volume ratio is 1: 1) of hydrogen and argon gas, temperature is under 360 ℃ of conditions, and reductase 12 hour.Make the Pt-Ru/C catalyst, particle diameter is 8-11nm, and electrochemically active specific surface area is 92.8m 2/ g.

Claims (8)

1, direct methanol fuel cell Pt-Ru/C Preparation of catalysts method, it is characterized in that it realizes by following step: one, carbon carrier is carried out following processing: 1. carbon carrier is placed high-pressure steam to handle 3-12 hour, carbon carrier is taken out the final vacuum drying; 2. the carbon carrier that steam treatment is crossed is heated to 400-1000 ℃ of processing 1-3 hour in the tube furnace inert gas; Two, the carbon carrier with above-mentioned processing joins in the mixed solution of deionized water and isopropyl alcohol, is uniformly dispersed; Three, Pt and Ru compound presoma are joined in the finely dispersed carbon containing slurries, Pt and Ru compound presoma are dispersed on the carbon carrier; Four, finely dispersed carbon is carried Pt and Ru compound presoma slurries make its drying under 50-80 ℃ of constant temperature magnetic agitation; Five, the carbon that obtains is carried Pt and Ru compound precursor powder, in agate mortar, ground 10 minutes; Six, carbon is carried Pt and Ru compound in the mist of hydrogen and argon gas, temperature is that reduction promptly obtained the Pt-Ru/C catalyst that direct methanol fuel cell is used in 1-3 hour under the 350-420 ℃ of condition.
2, DMFC according to claim 1 is characterized in that with the preparation method of Pt-Ru/C catalyst described Pt and Ru compound presoma are (NH 4) 2PtCl 6Or (NH 4) 2RuCl 5
3, DMFC according to claim 1 is characterized in that described and (NH with the preparation method of Pt-Ru/C catalyst 4) 2RuCl 5The Pt presoma that matches is H 2PtCl 6, Pt (NH 3) 4Cl 2Or Pt (NH 3) 2(NO 2) 2
4, DMFC according to claim 1 is characterized in that described and (NH with the preparation method of Pt-Ru/C catalyst 4) 2PtCl 6The Ru presoma that matches is Ru (OH) 3, Ru (NO 3) 2, RuCl 3Or Ru (NH 3) 4Cl 2
5, direct methanol fuel cell according to claim 1 Pt-Ru/C Preparation of catalysts method, the pressure that it is characterized in that described step 1 mesohigh steam is 0.1～1.5MPa.
6, direct methanol fuel cell according to claim 1 is characterized in that with Pt-Ru/C Preparation of catalysts method the inert gas in the described step 1 is the mist of hydrogen and argon gas, and the volume ratio of its hydrogen and argon gas is 1: 1.
7, direct methanol fuel cell according to claim 1 is with Pt-Ru/C Preparation of catalysts method, it is characterized in that deionized water and its deionized water of mixed solution of isopropyl alcohol and the volume ratio of isopropyl alcohol are 1: 1 in the described step 2.
8, direct methanol fuel cell according to claim 1 Pt-Ru/C Preparation of catalysts method, the particle diameter that it is characterized in that described Pt-Ru/C catalyst is 8-11nm.
CNB2005100096984A 2005-02-01 2005-02-01 Method for preparing Pt-Ru/C catalyst in use for direct methanol fuel cell Expired - Fee Related CN1299375C (en)

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Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101337183B (en) * 2008-08-15 2010-06-23 哈尔滨工业大学 Preparation method of direct methanol fuel cell cathode catalyst
CN101306364B (en) * 2008-07-04 2010-10-06 北京科技大学 Preparation method of direct methanol fuel cell anode catalyst
US7902111B2 (en) 2006-02-07 2011-03-08 Samsung Sdi Co., Ltd. Supported catalyst for fuel cell, method of preparing the same, electrode for fuel cell including the supported catalyst, and fuel cell including the electrode
CN101219402B (en) * 2006-05-16 2011-04-20 三星Sdi株式会社 Supported catalyst, method of preparing the same, and fuel cell using the same
CN101826623B (en) * 2009-12-14 2012-09-26 汕头大学 Preparation method of PEMFC Pt-Ru/c catalyst
CN103296288A (en) * 2013-06-07 2013-09-11 苏州诺信创新能源有限公司 Preparation method of catalyst electrode of microorganism fuel cell
CN109267121A (en) * 2018-11-20 2019-01-25 大连理工大学 A kind of method that composite electrodeposition prepares PtM/C catalyst
CN113437317A (en) * 2021-06-24 2021-09-24 国家电投集团氢能科技发展有限公司 Anti-reversal catalyst for fuel cell and preparation method thereof
CN114108012A (en) * 2021-12-07 2022-03-01 湖南大学 Method for constructing secondary amine compound through electrocatalytic C-N reduction coupling

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JPS62163746A (en) * 1986-01-13 1987-07-20 Nippon Engeruharudo Kk Platinum alloy electrode catalyst and electrode for acidic electrolyte fuel cell using same
JP2001062296A (en) * 1999-08-31 2001-03-13 Suzuki Motor Corp Electrode catalyst for fuel cell and method for selecting candidate metal element
CN1181583C (en) * 2001-04-10 2004-12-22 大连新源动力股份有限公司 Anti-CO compound catalystic layer for proteon-exchange membrane fuel cell and its preparation
CN1111083C (en) * 2001-05-18 2003-06-11 清华大学 Method for preparing CO poisoning resisting platinum-ruthenium electro-catalyst
CN1547280A (en) * 2003-12-16 2004-11-17 中国科学院长春应用化学研究所 Preparation method of direct methanol fuel cell electrode

Cited By (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US7902111B2 (en) 2006-02-07 2011-03-08 Samsung Sdi Co., Ltd. Supported catalyst for fuel cell, method of preparing the same, electrode for fuel cell including the supported catalyst, and fuel cell including the electrode
CN101219402B (en) * 2006-05-16 2011-04-20 三星Sdi株式会社 Supported catalyst, method of preparing the same, and fuel cell using the same
US7994088B2 (en) 2006-05-16 2011-08-09 Samsung Sdi Co., Ltd. Supported catalyst, method of preparing the same, and fuel cell using the same
CN101306364B (en) * 2008-07-04 2010-10-06 北京科技大学 Preparation method of direct methanol fuel cell anode catalyst
CN101337183B (en) * 2008-08-15 2010-06-23 哈尔滨工业大学 Preparation method of direct methanol fuel cell cathode catalyst
CN101826623B (en) * 2009-12-14 2012-09-26 汕头大学 Preparation method of PEMFC Pt-Ru/c catalyst
CN103296288A (en) * 2013-06-07 2013-09-11 苏州诺信创新能源有限公司 Preparation method of catalyst electrode of microorganism fuel cell
CN109267121A (en) * 2018-11-20 2019-01-25 大连理工大学 A kind of method that composite electrodeposition prepares PtM/C catalyst
CN113437317A (en) * 2021-06-24 2021-09-24 国家电投集团氢能科技发展有限公司 Anti-reversal catalyst for fuel cell and preparation method thereof
CN113437317B (en) * 2021-06-24 2022-01-28 国家电投集团氢能科技发展有限公司 Anti-reversal catalyst for fuel cell and preparation method thereof
CN114108012A (en) * 2021-12-07 2022-03-01 湖南大学 Method for constructing secondary amine compound through electrocatalytic C-N reduction coupling

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