CN1790785A - Method for preparing fuel cell nano catalyst with non-metal element - Google Patents
Method for preparing fuel cell nano catalyst with non-metal element Download PDFInfo
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- CN1790785A CN1790785A CNA2005101191030A CN200510119103A CN1790785A CN 1790785 A CN1790785 A CN 1790785A CN A2005101191030 A CNA2005101191030 A CN A2005101191030A CN 200510119103 A CN200510119103 A CN 200510119103A CN 1790785 A CN1790785 A CN 1790785A
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Abstract
The invention provides a preparation method for direct methanol fuel cell catalyst, which comprises: adding sodium dihydrogen hypophosphite into chloroplatinic acid and ruthenic trichloride solution, adjusting pH value and temperature of solution; adding phosphorus into the solution, and obtaining the micro-fine PtP/PtRuP catalyst with 2nm diameter not dependent carbon carrier surface. The testing results show the product has super property. This invention is convenient with high efficiency and low cost.
Description
Technical field
The invention belongs to direct methanol fuel cell Preparation of catalysts method.
Background technology
Direct methanol fuel cell (DMFCs) has caused extensive studies interest at energy circle owing to simple in structure, easy to operate.It is to be electrolyte with the solid polymer proton exchange membrane, directly is fuel with the liquid methanol, and catalytic oxidation methyl alcohol produces the device of CO2 and electric current.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.Therefore, direct methanol fuel cell is suitable for the removable power supply as various uses especially.
Carbon carries platinum, carbon carries the platinum ruthenium and has been widely used as fuel-cell catalyst at present.In order to improve activity, industry thinks that coming the augmenting response area by the mean particle dia that dwindles platinum is a kind of effective means.At present, the preparation method that carbon carries platinum, Pt-Ru/C catalyst mainly is divided into following several: (1) infusion process [(nineteen ninety, the electrochemistry journal, the 35th volume 199-207 page or leaf) J.B.Goodenough, A.Hamnett, B.J.Kennedy, R.Manoharan and S.A.Weeks, Electrochimica Acta, 1990,35,199-207], being the most frequently used method of preparation carrier metal catalyst, promptly directly is maceration extract with the metal salt solution, adopts distinct methods reduction preparation platinum/carbon and platinum ruthenium/carbon catalyst.The method easily causes in the catalyst metallic to be assembled at carrier surface, the wide and skewness one of particle size range, and the decentralization in carrier is low etc., has influenced the best catalytic performance of catalyst.(2) colloid method [(1998 " U.S.'s electrochemistry meeting " 145 volumes, 925-931 page or leaf, and United States Patent (USP): 6232264) T.J.Schmidt, M.Noeske, H.A.Gasteiger, R.J.Behm, P.Britz, and H.Bonnemann, J.Electrochem.Soc., 1998, vol.145,925-931; United StatesPatent:6232264, May, 2001, Charles M.Lukehart] promptly earlier with chloroplatinic acid, platinum ruthenium precursor compounds such as ruthenium trichloride are prepared into the PtRu colloidal compound, as metallo-organic compound colloid or metal oxide colloids, then with colloidal deposition in activated carbon surface, again the said mixture electronation is prepared into platinum/carbon, the platinum ruthenium/carbon eelctro-catalyst.This method can obtain the less catalyst granules of particle diameter, but this class methods preparation process relative complex, and relatively stricter in the preparation process to conditional requests such as temperature, solution concentration, pH value, reaction time.
Summary of the invention
Low in order to solve the fuel-cell catalyst activity, preparation process complicated technology problem the invention provides a kind of preparation method of fuel cell nano catalyst of the high electrocatalytic active that adds nonmetalloid.
The preparation method's of a kind of fuel cell nano catalyst that adds nonmetalloid of the present invention preparation process and condition are as follows:
(1) active carbon is joined in the container of deionized water, making the content of active carbon in prepared catalyst is 40%～90%, ultrasonic 10～40 minutes;
(2) add platinum tetrachloride or platinum acid chloride solution, the content that makes platinum in the catalyst is 10%～60%, stirs;
(3) add ruthenium trichloride, making the content of ruthenium in the catalyst is 7.5%～30%, makes in the prepared catalyst, and platinum ruthenium atom ratio is stirring in 1: 1;
(4) add sodium dihydric hypophosphite, its molal quantity is 10～120 times of platinum molal quantitys in the solution, stirs;
(5) add NaOH or potassium hydroxide solution, regulating the pH value is 8.5～10, stirs;
(6) add thermal agitation, temperature is 85 ℃～95 ℃, and constant temperature 4 hours stops heating, naturally cools to room temperature;
(7) filter, washing, drying at room temperature can get highly active a kind of fuel cell nano catalyst that adds nonmetalloid.
Described a kind of preparation method who adds the fuel cell nano catalyst of nonmetalloid of the present invention can also omit for the 3rd step, and remaining is the same.
A kind of fuel cell nano catalyst that adds nonmetalloid of method preparation of the present invention, its particle diameter is 2.0 ± 0.5nm.
Catalyst with preparation, be prepared into membrane electrode joint body, be assembled into the monomer direct methanol fuel cell, utilize the Arbin fuel battery test system that the monomer direct methanol fuel cell has been carried out performance test, test result shows, aspect peak power output density, commercial E-TEK catalyst is 36.6mW/cm
2A kind of fuel cell nano catalyst that adds nonmetalloid of the present invention has then reached 61.4mW/cm
2Be equivalent to the former about 1.7 times.
Method of the present invention has simple, convenient and practical, realizes miniaturization and decentralized by adding phosphorus (P), utilizes the phosphorus that is added to cut off platinum realization miniaturization with the metallic bond (Metallic Bond) of ruthenium.Except that miniaturization, also produced the effect that particle size distribution range reduces.Catalyst particle size generally is distributed between 2nm～10nm in the past, and scope is bigger.And after the interpolation phosphorus, its distribution has then narrowed down to 2.0 ± 0.5nm.Prepared catalyst is uniformly dispersed on absorbent charcoal carrier, uniform particle diameter, high catalytic activity and controlled advantages such as grain size.
And catalyst of the present invention has very high electro-chemical activity and stability, has improved the utilance of catalyst, has reduced the carrying capacity of catalyst.The method is convenient, efficient, easy operating, and with low cost, can satisfy the development and utilization in electro-catalysis, Proton Exchange Membrane Fuel Cells field, uses, develops value greatly.
Description of drawings:
PtRu/C (20wt%Pt+10wt%Ru) catalyst of accompanying drawing 1 catalyst provided by the invention: PtRuP/C (19.36wt%Pt+9.82wt%Ru+2.38wt%P) and commercial E-TEK company is at 0.5M H
2SO
4+ 1.0M CH
3Cyclic voltammetry curve figure in the OH solution.
PtRu/C (20wt%Pt+10wt%Ru) catalyst of accompanying drawing 2 catalyst provided by the invention: PtRuP/C (19.36wt%Pt+9.82wt%Ru+2.38wt%P) and commercial E-TEK company, the discharge performance figure of the direct methanol fuel cell of assembling, catalyst provided by the invention as can be seen, the battery performance of assembling are higher than the performance of the corresponding catalyst of commercial E-TEK company.
Embodiment.
A certain amount of active carbon is joined in the beaker that fills deionized water, and making the content of active carbon in prepared catalyst is 80wt%, sonicated, add platinum tetrachloride then, the content that makes platinum in the catalyst is 20wt%, stirs, add sodium dihydric hypophosphite, making its molal quantity is 20 times of platinum molal quantitys in the solution, stirs, and adds sodium hydroxide solution, regulating the pH value is 8.5～10.5, begin to add thermal agitation, be heated to 85 ℃～95 ℃, control this temperature range, continue to stir 4 hours, stop heating, naturally cool to room temperature, filter, washing, drying at room temperature can get highly active PtP/C catalyst, and particle diameter is 2.0 ± 0.5nm.Show that by electrochemical oxidation methanol oxidation methanol loop volt-ampere curve this catalyst performance is better than the corresponding eelctro-catalyst of E-TEK company.
Embodiment 2
A certain amount of active carbon is joined in the beaker that fills deionized water, and making the content of active carbon in prepared catalyst is 70wt%, sonicated, add platinum acid chloride solution then, the content that makes platinum in the catalyst is 30wt%, stirs, and adds sodium dihydric hypophosphite, making its molal quantity is 40 times of platinum molal quantitys in the solution, stir, add NaOH or potassium hydroxide solution, regulating the pH value is 8.5～10.5, be heated to 85 ℃～95 ℃, control this temperature range, continue to stir 4 hours, stop heating, naturally cool to room temperature, filter washing, drying at room temperature, can get highly active PtP/C catalyst, particle diameter is 2.0 ± 0.5nm.Show that by electrochemical oxidation methanol oxidation methanol loop volt-ampere curve this catalyst performance is better than the corresponding eelctro-catalyst of E-TEK company
Embodiment 3
A certain amount of active carbon is joined in the beaker that fills deionized water, and making the content of active carbon in prepared catalyst is 60wt%, ultrasonic 10～40 minutes, add platinum acid chloride solution then, the content that makes platinum in the catalyst is 40wt%, stirs, and adds sodium dihydric hypophosphite, making its molal quantity is 80 times of platinum molal quantitys in the solution, stir, add NaOH or potassium hydroxide solution, regulating the pH value is 8.5～10.5, be heated to 85 ℃～95 ℃, control this temperature range, continue to stir 4 hours, stop heating, naturally cool to room temperature, filter washing, drying at room temperature, can get highly active PtP/C catalyst, particle diameter is 2.0 ± 0.5nm.Show that by electrochemical oxidation methanol oxidation methanol loop volt-ampere curve this catalyst performance is better than the corresponding eelctro-catalyst of E-TEK company
Embodiment 4
A certain amount of active carbon is joined in the beaker that fills deionized water, and making the content of active carbon in prepared catalyst is 40wt%, sonicated, add platinum acid chloride solution then, the content that makes platinum in the catalyst is 60wt%, stirs, and adds sodium dihydric hypophosphite, making its molal quantity is 80 times of platinum molal quantitys in the solution, stir, add NaOH or potassium hydroxide solution, regulating the pH value is 8.5～10.5, be heated to 85 ℃～95 ℃, control this temperature range, continue to stir 4 hours, stop heating, naturally cool to room temperature, filter washing, drying at room temperature, can get highly active PtP/C catalyst, particle diameter is 2.0 ± 0.5nm.Show that by electrochemical oxidation methanol oxidation methanol loop volt-ampere curve this catalyst performance is better than the corresponding eelctro-catalyst of E-TEK company
Embodiment 5
A certain amount of active carbon is joined in the beaker that fills deionized water, and making the content of active carbon in prepared catalyst is 80wt%, sonicated, add platinum acid chloride solution then, the content that makes platinum in the catalyst is 12.5wt%, stirs, then add ruthenium trichloride, making the content of ruthenium in the catalyst is 7.5wt%, makes in the prepared catalyst, and platinum ruthenium atom ratio is 1: 1, stir, add sodium dihydric hypophosphite, making its molal quantity is 40 times of platinum molal quantitys in the solution, stirs, add NaOH or potassium hydroxide solution, regulating the pH value is 8.5～10.5, is heated to 85 ℃～95 ℃, controls this temperature range, continue to stir 4 hours, stop heating, naturally cool to room temperature, filter, washing, drying at room temperature can get highly active PtP/C catalyst, and particle diameter is 2.0 ± 0.5nm.Show that by electrochemical oxidation methanol oxidation methanol loop volt-ampere curve this catalyst performance is better than the corresponding eelctro-catalyst of E-TEK company
Embodiment 6
A certain amount of active carbon is joined in the beaker that fills deionized water, and making the content of active carbon in prepared catalyst is 70wt%, sonicated, add platinum acid chloride solution then, the content that makes platinum in the catalyst is 20wt%, stirs, then add ruthenium trichloride, making the content of ruthenium in the catalyst is 10wt%, makes in the prepared catalyst, and platinum ruthenium atom ratio is 1: 1, stir, add sodium dihydric hypophosphite, making its molal quantity is 60 times of platinum molal quantitys in the solution, stirs, add NaOH or potassium hydroxide solution, regulating the pH value is 8.5～10.5, is heated to 85 ℃～95 ℃, controls this temperature range, continue to stir 4 hours, stop heating, naturally cool to room temperature, filter, washing, drying at room temperature can get highly active PtP/C, PtRuP/C catalyst, particle diameter are 2.0 ± 0.5nm.Show that by electrochemical oxidation methanol oxidation methanol loop volt-ampere curve this catalyst performance is better than the corresponding eelctro-catalyst of E-TEK company
Embodiment 7
A certain amount of active carbon is joined in the beaker that fills deionized water, and making the content of active carbon in prepared catalyst is 55wt%, sonicated, add platinum acid chloride solution then, the content that makes platinum in the catalyst is 30wt%, stirs, then add ruthenium trichloride, making the content of ruthenium in the catalyst is 15wt%, makes in the prepared catalyst, and platinum ruthenium atom ratio is 1: 1, stir, add sodium dihydric hypophosphite, making its molal quantity is 80 times of platinum molal quantitys in the solution, stirs, add NaOH or potassium hydroxide solution, regulating the pH value is 8.5～10.5, is heated to 85 ℃～95 ℃, controls this temperature range, continue to stir 4 hours, stop heating, naturally cool to room temperature, filter, washing, drying at room temperature can get highly active PtP/C, PtRuP/C catalyst, particle diameter are 2.0 ± 0.5nm.Show that by electrochemical oxidation methanol oxidation methanol loop volt-ampere curve this catalyst performance is better than the corresponding eelctro-catalyst of E-TEK company
Embodiment 8
A certain amount of active carbon is joined in the beaker that fills deionized water, and making the content of active carbon in prepared catalyst is 55wt%, sonicated, add platinum acid chloride solution then, the content that makes platinum in the catalyst is 30wt%, stirs, and then adds ruthenium trichloride, the content that makes ruthenium in the catalyst is 15wt%, make in the prepared catalyst, platinum ruthenium atom ratio is stirring in 1: 1, adds sodium dihydric hypophosphite, making its molal quantity is 100 times of platinum molal quantitys in the solution, stir, add NaOH or potassium hydroxide solution, regulating the pH value is 8.5～10.5, be heated to 85 ℃～95 ℃, control this temperature range, continue to stir 4 hours, stop heating, naturally cool to room temperature, filter washing, drying at room temperature, can get highly active PtP/C, PtRuP/C catalyst, particle diameter are 2.0 ± 0.5nm.Show that by electrochemical oxidation methanol oxidation methanol loop volt-ampere curve this catalyst performance is better than the corresponding eelctro-catalyst of E-TEK company
Embodiment 9
A certain amount of active carbon is joined in the beaker that fills deionized water, and making the content of active carbon in prepared catalyst is 40wt%, sonicated, add platinum acid chloride solution then, the content that makes platinum in the catalyst is 40wt%, stirs, then add ruthenium trichloride, making the content of ruthenium in the catalyst is 20wt%, makes in the prepared catalyst, and platinum ruthenium atom ratio is 1: 1, stir, add sodium dihydric hypophosphite, making its molal quantity is 120 times of platinum molal quantitys in the solution, stirs, add NaOH or potassium hydroxide solution, regulating the pH value is 8.5～10.5, is heated to 85 ℃～95 ℃, controls this temperature range, continue to stir 4 hours, stop heating, naturally cool to room temperature, filter, washing, drying at room temperature can get highly active PtP/C, PtRuP/C catalyst, particle diameter are 2.0 ± 0.5nm.Show that by electrochemical oxidation methanol oxidation methanol loop volt-ampere curve this catalyst performance is better than the corresponding eelctro-catalyst of E-TEK company
A certain amount of active carbon is joined in the beaker that fills deionized water, and making the content of active carbon in prepared catalyst is 70wt%, sonicated, add platinum tetrachloride solution then, the content that makes platinum in the catalyst is 20wt%, stirs, and then adds ruthenium trichloride, the content that makes ruthenium in the catalyst is 10wt%, make in the prepared catalyst, platinum ruthenium atom ratio is stirring in 1: 1, adds sodium dihydric hypophosphite, making its molal quantity is 40 times of platinum molal quantitys in the solution, stir, add NaOH or potassium hydroxide solution, regulating the pH value is 8.5～10.5, be heated to 85 ℃～95 ℃, control this temperature range, continue to stir 4 hours, stop heating, naturally cool to room temperature, filter washing, drying at room temperature, can get highly active PtP/C, PtRuP/C catalyst, particle diameter are 2.0 ± 0.5nm.Show that by electrochemical oxidation methanol oxidation methanol loop volt-ampere curve this catalyst performance is better than the corresponding eelctro-catalyst of E-TEK company
Embodiment 11
A certain amount of active carbon is joined in the beaker that fills deionized water, and making the content of active carbon in prepared catalyst is 55wt%, sonicated, add platinum tetrachloride solution then, the content that makes platinum in the catalyst is 30wt%, stirs, and then adds ruthenium trichloride, the content that makes ruthenium in the catalyst is 15wt%, make in the prepared catalyst, platinum ruthenium atom ratio is stirring in 1: 1, adds sodium dihydric hypophosphite, making its molal quantity is 80 times of platinum molal quantitys in the solution, stir, add NaOH or potassium hydroxide solution, regulating the pH value is 8.5～10.5, be heated to 85 ℃～95 ℃, control this temperature range, continue to stir 4 hours, stop heating, naturally cool to room temperature, filter washing, drying at room temperature, can get highly active PtP/C, PtRuP/C catalyst, particle diameter are 2.0 ± 0.5nm.Show that by electrochemical oxidation methanol oxidation methanol loop volt-ampere curve this catalyst performance is better than the corresponding eelctro-catalyst of E-TEK company.
Embodiment 12
A certain amount of active carbon is joined in the beaker that fills deionized water, and making the content of active carbon in prepared catalyst is 40wt%, sonicated, add platinum tetrachloride solution then, the content that makes platinum in the catalyst is 40wt%, stirs, and then adds ruthenium trichloride, the content that makes ruthenium in the catalyst is 20wt%, make in the prepared catalyst, platinum ruthenium atom ratio is stirring in 1: 1, adds sodium dihydric hypophosphite, making its molal quantity is 100 times of platinum molal quantitys in the solution, stir, add NaOH or potassium hydroxide solution, regulating the pH value is 8.5～10.5, be heated to 85 ℃～95 ℃, control this temperature range, continue to stir 4 hours, stop heating, naturally cool to room temperature, filter washing, drying at room temperature, can get highly active PtP/C, PtRuP/C catalyst, particle diameter are 2.0 ± 0.5nm.Show that by electrochemical oxidation methanol oxidation methanol loop volt-ampere curve this catalyst performance is better than the corresponding eelctro-catalyst of E-TEK company.
Claims (2)
1. direct methanol fuel cell Preparation of catalysts method is characterized in that preparation process and condition are as follows:
(1) active carbon is joined in the container of deionized water, making the content of active carbon in prepared catalyst is 40%～90%, ultrasonic 10～40 minutes;
(2) add platinum tetrachloride or platinum acid chloride solution, the content that makes platinum in the catalyst is 10%～60%, stirs;
(4) add sodium dihydric hypophosphite, its molal quantity is 10～120 times of platinum molal quantitys in the solution, stirs;
(5) add NaOH or potassium hydroxide solution, regulating the pH value is 8.5～10, stirs;
(6) add thermal agitation, temperature is 85 ℃～95 ℃, and constant temperature 4 hours stops heating, naturally cools to room temperature;
(7) filter, washing, drying at room temperature can get highly active a kind of direct methanol fuel cell catalyst.
2. a kind of direct methanol fuel cell Preparation of catalysts method as claimed in claim 1 has increased by the 3rd step, it is characterized in that preparation process and condition are as follows:
(1) active carbon is joined in the container of deionized water, making the content of active carbon in prepared catalyst is 40%～90%, ultrasonic 10～40 minutes;
(2) add platinum tetrachloride or platinum acid chloride solution, the content that makes platinum in the catalyst is 10%～60%, stirs;
(3) add ruthenium trichloride, making the content of ruthenium in the catalyst is 7.5%～30%, makes in the prepared catalyst, and platinum ruthenium atom ratio is stirring in 1: 1;
(4) add sodium dihydric hypophosphite, its molal quantity is 10～120 times of platinum molal quantitys in the solution, stirs;
(5) add NaOH or potassium hydroxide solution, regulating the pH value is 8.5～10, stirs;
(6) add thermal agitation, temperature is 85 ℃～95 ℃, and constant temperature 4 hours stops heating, naturally cools to room temperature;
(7) filter, washing, drying at room temperature can get highly active a kind of direct methanol fuel cell catalyst.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US8168348B2 (en) | 2007-12-04 | 2012-05-01 | Hanwha Chemical Corporation | Process for the electrochemical catalysts of fuel cells based on polymer electrolytes |
| CN104001536A (en) * | 2014-06-10 | 2014-08-27 | 西北师范大学 | Method for preparing non-load palladium alloy electrocatalyst on gas-solution interface |
| CN113410472A (en) * | 2021-06-03 | 2021-09-17 | 扬州大学 | Alcohol fuel cell anode catalyst and preparation method thereof |
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| CN102365775B (en) * | 2009-03-12 | 2014-08-13 | 戴姆勒股份公司 | Platinum phosphide as a cathode catalyst for pemfcs and phosphorous treatment of catalysts for fuel cell |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JP2003157857A (en) * | 2001-11-20 | 2003-05-30 | Toyota Central Res & Dev Lab Inc | Electrode catalyst body for fuel cell, air electrode for fuel cell using it, and evaluating method of its catalystic activity |
| JP2003308849A (en) * | 2002-04-12 | 2003-10-31 | Tanaka Kikinzoku Kogyo Kk | Catalyst for fuel electrode of high polymer solid electrolyte fuel cell |
| JP2005005257A (en) * | 2003-05-20 | 2005-01-06 | Nissan Motor Co Ltd | Air electrode catalyst for fuel cell, and manufacturing method therefor |
| CN1323450C (en) * | 2005-07-05 | 2007-06-27 | 北京科技大学 | Method of preparing catalyst for anode of fuel cell of direct alcohols |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US8168348B2 (en) | 2007-12-04 | 2012-05-01 | Hanwha Chemical Corporation | Process for the electrochemical catalysts of fuel cells based on polymer electrolytes |
| CN101641816B (en) * | 2007-12-04 | 2012-05-23 | 韩华石油化学株式会社 | Process for the electrochemical catalysts of fuel cells based on polymer electrolytes |
| CN104001536A (en) * | 2014-06-10 | 2014-08-27 | 西北师范大学 | Method for preparing non-load palladium alloy electrocatalyst on gas-solution interface |
| CN113410472A (en) * | 2021-06-03 | 2021-09-17 | 扬州大学 | Alcohol fuel cell anode catalyst and preparation method thereof |
| CN113410472B (en) * | 2021-06-03 | 2024-05-07 | 扬州大学 | Anode catalyst of alcohol fuel cell and preparation method thereof |
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