CN101944620B - Fuel cell catalyst with multi-component composite as carrier and preparation method - Google Patents
Fuel cell catalyst with multi-component composite as carrier and preparation method Download PDFInfo
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- CN101944620B CN101944620B CN2010102425667A CN201010242566A CN101944620B CN 101944620 B CN101944620 B CN 101944620B CN 2010102425667 A CN2010102425667 A CN 2010102425667A CN 201010242566 A CN201010242566 A CN 201010242566A CN 101944620 B CN101944620 B CN 101944620B
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- 239000003054 catalyst Substances 0.000 title claims abstract description 34
- 238000002360 preparation method Methods 0.000 title claims abstract description 25
- 239000000446 fuel Substances 0.000 title abstract description 7
- 239000002131 composite material Substances 0.000 title abstract description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 22
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 21
- 239000003575 carbonaceous material Substances 0.000 claims abstract description 19
- 239000000463 material Substances 0.000 claims abstract description 17
- 150000001875 compounds Chemical class 0.000 claims abstract description 15
- 238000000034 method Methods 0.000 claims abstract description 14
- 238000011065 in-situ storage Methods 0.000 claims abstract description 9
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 18
- 239000000243 solution Substances 0.000 claims description 15
- 239000012065 filter cake Substances 0.000 claims description 12
- 238000002203 pretreatment Methods 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- 239000000126 substance Substances 0.000 claims description 8
- 230000001105 regulatory effect Effects 0.000 claims description 6
- 238000000967 suction filtration Methods 0.000 claims description 6
- 229910052751 metal Inorganic materials 0.000 claims description 4
- 239000002184 metal Substances 0.000 claims description 4
- 229910000667 (NH4)2Ce(NO3)6 Inorganic materials 0.000 claims description 2
- 239000012266 salt solution Substances 0.000 claims description 2
- 229910052684 Cerium Inorganic materials 0.000 claims 1
- 229910052759 nickel Inorganic materials 0.000 claims 1
- 229910052718 tin Inorganic materials 0.000 claims 1
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Substances [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 abstract description 38
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 abstract description 22
- 229920000049 Carbon (fiber) Polymers 0.000 abstract description 14
- 239000004917 carbon fiber Substances 0.000 abstract description 14
- 229910052697 platinum Inorganic materials 0.000 abstract description 12
- 239000006229 carbon black Substances 0.000 abstract description 6
- 229910044991 metal oxide Inorganic materials 0.000 abstract description 6
- 150000004706 metal oxides Chemical class 0.000 abstract description 6
- 229910006404 SnO 2 Inorganic materials 0.000 abstract description 3
- 238000006243 chemical reaction Methods 0.000 abstract description 3
- 239000011165 3D composite Substances 0.000 abstract description 2
- 239000003638 chemical reducing agent Substances 0.000 abstract description 2
- 238000001556 precipitation Methods 0.000 abstract description 2
- 238000006722 reduction reaction Methods 0.000 abstract description 2
- 239000011159 matrix material Substances 0.000 abstract 2
- 229910020599 Co 3 O 4 Inorganic materials 0.000 abstract 1
- 239000002041 carbon nanotube Substances 0.000 abstract 1
- 229910021393 carbon nanotube Inorganic materials 0.000 abstract 1
- 239000004005 microsphere Substances 0.000 abstract 1
- GNRSAWUEBMWBQH-UHFFFAOYSA-N nickel(II) oxide Inorganic materials [Ni]=O GNRSAWUEBMWBQH-UHFFFAOYSA-N 0.000 abstract 1
- 238000005979 thermal decomposition reaction Methods 0.000 abstract 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 12
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 8
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 8
- 229910001260 Pt alloy Inorganic materials 0.000 description 5
- 239000007789 gas Substances 0.000 description 5
- 238000001816 cooling Methods 0.000 description 4
- 239000008367 deionised water Substances 0.000 description 4
- 229910021641 deionized water Inorganic materials 0.000 description 4
- 238000001035 drying Methods 0.000 description 4
- 230000007935 neutral effect Effects 0.000 description 4
- 229910017604 nitric acid Inorganic materials 0.000 description 4
- XTUSEBKMEQERQV-UHFFFAOYSA-N propan-2-ol;hydrate Chemical compound O.CC(C)O XTUSEBKMEQERQV-UHFFFAOYSA-N 0.000 description 4
- 238000010992 reflux Methods 0.000 description 4
- 238000005406 washing Methods 0.000 description 4
- 239000012528 membrane Substances 0.000 description 2
- 231100000572 poisoning Toxicity 0.000 description 2
- 230000000607 poisoning effect Effects 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000011149 active material Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005518 electrochemistry Effects 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 239000002574 poison Substances 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
Classifications
-
- 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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- Inert Electrodes (AREA)
Abstract
一种多元复合物为载体的燃料电池催化剂及制备方法，涉及一种燃料电池催化剂及制备方法。本发明采用粒状碳材料(C1)与线状碳材料(C2)的混合材料作为碳基体材料，在这两种基体材料上采用沉淀热分解法制备碳载体和氧化物的复合载体MOx-(C1+C2)，然后再采用原位化学还原法制备Pt/MOx-(C1+C2)催化剂。MOx为CeO2、SnO2、Co3O4或NiO。C1为碳黑、碳微球或介孔碳。C2为碳纤维或碳纳米管。线状碳材料与粒状碳材料的结合形成了三维复合网络结构，加大了催化剂的三相反应活性区；掺杂的金属氧化物增强了催化剂的抗CO能力，提高了铂的利用率。The invention relates to a fuel cell catalyst and a preparation method with a multi-component compound as a carrier, relating to a fuel cell catalyst and a preparation method. The present invention adopts the mixed material of granular carbon material (C1) and linear carbon material (C2) as the carbon matrix material, adopts the precipitation thermal decomposition method on these two matrix materials to prepare the composite carrier MO x -( C1+C2), and then prepare Pt/MO x -(C1+C2) catalyst by in-situ chemical reduction method. MO x is CeO 2 , SnO 2 , Co 3 O 4 or NiO. C1 is carbon black, carbon microspheres or mesoporous carbon. C2 is carbon fiber or carbon nanotube. The combination of linear carbon materials and granular carbon materials forms a three-dimensional composite network structure, which increases the three-phase reaction active area of the catalyst; the doped metal oxide enhances the anti-CO ability of the catalyst and improves the utilization rate of platinum.
Description
Technical field
The present invention relates to a kind of fuel-cell catalyst and preparation method.
Background technology
Fuel cell has characteristics such as operating temperature is low, energy efficiency is high, no electrolyte corrosion, is a research focus in electrochemistry and energy science field.Study of Catalyst is one of the most challenging task in the Proton Exchange Membrane Fuel Cells research.Big quantity research proves that the cathode and anode catalyst of the catalyst based battery that acts as a fuel of Pt has shown good catalytic action.Yet the price of metal platinum and the shortage in source have limited the catalyst based application of Pt.Therefore, the amount that reduces the use noble metal catalyst is one of key factor that effectively reduces the fuel cell manufacture cost, and its solution is through using the appropriate carriers material to possess high dispersive and high efficiency catalyst to be arranged.
People generally adopt carbon black as catalyst carrier at present; This is because carbon black has higher specific surface area and has good electrical conductivity and preferable pore structure; Help improving metal platinum microparticulate property; But the utilance of platinum still can be very not high, and an important reasons is the micropore that a large amount of platinum or platinum alloy particulate enter into carbon surface, because this part platinum or the platinum alloy that are buried can not contact with proton conductor; Therefore be difficult to form more three-phase reaction interface, thereby reduce the utilance of platinum.In addition; Because platinum or platinum alloy directly link to each other with carbon, in preparation membrane electrode process, proton exchange resins can not enter into the position between platinum or platinum alloy and the carbon; This has reduced the phase reaction district on the one hand; On the other hand in battery operated process and since CO poison platinum or platinum alloy reduced activity.
Summary of the invention
Technical problem to be solved by this invention is that the utilance of raising platinum increases poisoning of anti-CO.
Technical scheme of the present invention:
A kind of the multiple element compound is the fuel-cell catalyst of carrier, and this catalyst is expressed as Pt/MOx-(C1+C2), MO
xBe metal oxide, carrier is the complex of granular carbon material and wire material with carbon element.
Granular carbon material comprises: carbon black, carbosphere or mesoporous carbon, the wire material with carbon element comprises: carbon fiber or CNT.
Metal oxide MO
xComprise: SnO
2, CeO
2, NiO or Co
3O
4
A kind of the multiple element compound is the preparation method of the fuel-cell catalyst of carrier, and this preparation method's step is:
Step 1 is to the pre-treatment of granular carbon material and wire material with carbon element;
Step 2, the preparation molar concentration is the SnCl of 0.01～0.1mol/L
2, (NH
4)
2Ce (NO
3)
6, Ni (NO
3)
2Or Co (NO
3)
2Solution;
Step 3, by granular carbon material: the wire material with carbon element is that 1～10: 1 mass ratio mixes, and joins in the container, adds isopropyl alcohol and water, and its volume ratio is 1: 3, and ultrasonic dispersing is even;
Step 4 slowly drips the metal salt solution that step 2 is prepared, and ultrasonic dispersing is even, and regulating the pH value is 6.5～9.5, ultrasonic stirring, and suction filtration obtains filter cake;
Step 5, filter cake in vacuum is dry, at N
2Decomposed 1～3 hour under following 200 ℃～500 ℃ temperature of gas shiled, promptly get required the multiple element compound carrier MOx-(C1+C2);
Step 6 with the multiple element compound carrier MOx-(C1+C2) of step 5 gained, obtains Pt/MOx-(C1+C2) catalyst through the in-situ chemical reducing process.
The present invention compares the beneficial effect that is had with prior art: the present invention adopts the composite material of wire material with carbon element and granular carbon material as catalyst carrier, on these two kinds of basis materials, adopts the precipitation heat decomposition method to prepare the complex carrier MO of carbon carrier and oxide
x-(C1+C2), and then adopt in-situ chemical reduction method for preparing Pt/MO
x-(C1+C2) catalyst; Have like this between wire material with carbon element and the granular carbon material and the Pt of bigger draw ratio and formed three-dimensional composite network structure; Active material Pt and collector and intermembranous being in contact with one another of proton have been increased; The composite catalyzing agent carrier of processing at some metal oxides that mix on the carbon back can promote the absorption of active OH on the Pt electrode and the desorption of CO, has increased poisoning of anti-CO, has improved the utilance of platinum.
Embodiment
A kind of the multiple element compound is the fuel-cell catalyst of carrier, and this catalyst is expressed as Pt/MOx-(C1+C2), MO
xBe metal oxide, support C is the complex of granular carbon material C1 and wire material with carbon element C2.
Described granular carbon material C1 comprises: carbon black, carbosphere or mesoporous carbon, wire material with carbon element C2 comprises: carbon fiber or CNT.
Described metal oxide MO
xComprise: SnO
2, CeO
2, NiO or Co
3O
4
A kind of the multiple element compound is preparation method's the execution mode of the fuel-cell catalyst of carrier:
Embodiment one
A kind of the multiple element compound is the preparation method of the fuel-cell catalyst of carrier, and this preparation method may further comprise the steps:
Step 1 is the pre-treatment of carbon black (ValcanXC-72) to granular carbon material C1:
With the granular carbon material ValcanXC-72 0.5h that in acetone, refluxes; Filter then, wash, after the drying, with 2mol/L nitric acid dousing 24h, then with deionized water wash to neutral; Use 5% hydrogen peroxide backflow 2h again, filter, washing, dry, grind subsequent use.
To wire material with carbon element C2 is the pre-treatment of CNT (CNTS):
CNTS at room temperature is soaked in the red fuming nitric acid (RFNA), stirs 12h, at 80 ℃ of refluxed 2h, with the mixed liquor natural cooling, filter then, vacuumize 12h grinds subsequent use.
Step 2, the preparation molar concentration is the SnCl of 0.01mol/L
2Solution;
Step 3 is got the ValcanXC-7230mg that step 1 handles by 1: 1 mass ratio and mixed with CNTS 30mg, joins in the there-necked flask of 150ml the adding isopropyl alcohol: the 40ml isopropanol water solution of water=1: 3, ultrasonic dispersing is even.
Step 4 slowly drips the SnCl that step 2 is prepared
2Solution, ultrasonic dispersing is even, and regulating the pH value is 9.5, ultrasonic stirring, suction filtration obtains filter cake;
Step 5, filter cake in vacuum is dry, at N
2Decomposed 1 hour under the following 500 ℃ temperature of gas shiled, promptly get complex carrier SnO
2-(ValcanXC-72R+CNTS);
Step 6 obtains Pt/SnO with step 5 gained complex carrier through the in-situ chemical reducing process
2-(ValcanXC-72+CNTS) catalyst.
Embodiment two
A kind of the multiple element compound is the preparation method of the fuel-cell catalyst of carrier, and this preparation method comprises that step is:
Step 1 is the pre-treatment of carbosphere to granular carbon material C1:
With the carbosphere 0.5h that in acetone, refluxes, filter then, wash, after the drying, with 2mol/L nitric acid dousing 24h, then with deionized water wash to neutral, use 5% hydrogen peroxide backflow 2h again, filter, washing, dry, grind subsequent use.
To wire material with carbon element C2 is the pre-treatment of carbon fiber:
Carbon fiber at room temperature is soaked in the red fuming nitric acid (RFNA), stirs 12h, at 80 ℃ of refluxed 2h, with the mixed liquor natural cooling, filter then, vacuumize 12h grinds subsequent use.
Step 2, the preparation molar concentration is the (NH of 0.1mol/L
4)
2Ce (NO
3)
6Solution;
Step 3 is got the carbosphere 100mg that step 1 handles by 10: 1 mass ratio and mixed with carbon fiber 1mg, joins in the there-necked flask of 150ml the adding isopropyl alcohol: the 40ml isopropanol water solution of water=1: 3, ultrasonic dispersing is even.
Step 4 slowly drips (the NH that step 2 is prepared
4)
2Ce (NO
3)
6Solution, ultrasonic dispersing is even, and regulating the pH value is 6.5, ultrasonic stirring, suction filtration obtains filter cake;
Step 5, filter cake in vacuum is dry, at N
2Decomposed 2 hours under the following 200 ℃ temperature of gas shiled, promptly get complex carrier CeO
2-(carbosphere+carbon fiber);
Step 6 obtains Pt/CeO with step 5 gained complex carrier through the in-situ chemical reducing process
2-(carbosphere+carbon fiber) catalyst.
Embodiment three
A kind of the multiple element compound is the preparation method of the fuel-cell catalyst of carrier, and this preparation method comprises that step is:
Step 1 is the pre-treatment of mesoporous carbon to granular carbon material C1:
With the mesoporous carbon 0.5h that in acetone, refluxes, filter then, wash, after the drying, with 2mol/L nitric acid dousing 24h, then with deionized water wash to neutral, use 5% hydrogen peroxide backflow 2h again, filter, washing, dry, grind subsequent use.
To wire material with carbon element C2 is the pre-treatment of CNT (CNTS):
CNTS at room temperature is soaked in the red fuming nitric acid (RFNA), stirs 12h, at 80 ℃ of refluxed 2h, with the mixed liquor natural cooling, filter then, vacuumize 12h grinds subsequent use.
Step 2, the preparation molar concentration is the Ni (NO of 0.05mol/L
3)
2Solution;
Step 3 is got the mesoporous carbon 50mg that step 1 handles by 5: 1 mass ratio and mixed with CNTS 10mg, joins in the there-necked flask of 150ml the adding isopropyl alcohol: the 40ml isopropanol water solution of water=1: 3, ultrasonic dispersing is even.
Step 4 slowly drips the Ni (NO that step 2 is prepared
3)
2Solution, ultrasonic dispersing is even, and regulating the pH value is 9.5, ultrasonic stirring, suction filtration obtains filter cake;
Step 5, filter cake in vacuum is dry, at N
2Decomposed 3 hours under the following 300 ℃ temperature of gas shiled, promptly get complex carrier NiO-(mesoporous carbon+CNTS);
Step 6 obtains the Pt/NiO-(catalyst of mesoporous carbon+CNTS) with step 5 gained complex carrier through the in-situ chemical reducing process
Embodiment four
A kind of the multiple element compound is the preparation method of the fuel-cell catalyst of carrier, and this preparation method comprises that step is:
Step 1 is the pre-treatment of carbosphere to granular carbon material C1:
With the carbosphere 0.5h that in acetone, refluxes, filter then, wash, after the drying, with 2mol/L nitric acid dousing 24h, then with deionized water wash to neutral, use 5% hydrogen peroxide backflow 2h again, filter, washing, dry, grind subsequent use.
To wire material with carbon element C2 is the pre-treatment of carbon fiber:
Carbon fiber at room temperature is soaked in the red fuming nitric acid (RFNA), stirs 12h, at 80 ℃ of refluxed 2h, with the mixed liquor natural cooling, filter then, vacuumize 12h grinds subsequent use.
Step 2, the preparation molar concentration is the Co (NO of 0.1mol/L
3)
2Solution;
Step 3 is got the carbosphere 30mg that step 1 handles by 3: 1 mass ratio and mixed with carbon fiber 10mg, joins in the there-necked flask of 150ml the adding isopropyl alcohol: the 40ml isopropanol water solution of water=1: 3, ultrasonic dispersing is even.
Step 4 slowly drips the Co (NO that step 2 is prepared
3)
2Solution, ultrasonic dispersing is even, and regulating the pH value is 8, ultrasonic stirring, suction filtration obtains filter cake;
Step 5, filter cake in vacuum is dry, at N
2Decomposed 2 hours under the following 300 ℃ temperature of gas shiled, promptly get complex carrier Co
3O
4(carbosphere+carbon fiber);
Step 6 obtains Pt/Co with step 5 gained complex carrier through the in-situ chemical reducing process
3O
4-(carbosphere+carbon fiber) catalyst.
Carbosphere, mesoporous carbon are from Beijing University of Chemical Technology, and carbon fiber and CNT are from Tsing-Hua University.
The method of the patent that the described in-situ chemical reducing process of the step 6 in all execution modes all adopts (02155256.8 and 02155255.X) record realizes.
Claims (1)
1. the preparation method that the multiple element compound is the fuel-cell catalyst of carrier is characterized in that, this preparation process is:
Step 1 is to the pre-treatment of granular carbon material (C1) and wire material with carbon element (C2);
Step 2, the preparation molar concentration is the SnCl of 0.01～0.1mol/L
2, (NH
4)
2Ce (NO
3)
6, Ni (NO
3)
2Or Co (NO
3)
2Solution;
Step 3, by granular carbon material C1: wire material with carbon element C2 is that the mass ratio of 1～10:1 mixes, and joins in the container, adds isopropyl alcohol and water, and its volume ratio is 1:3, and ultrasonic dispersing is even;
Step 4 slowly drips the metal salt solution that step 2 is prepared, and ultrasonic dispersing is even, and regulating the pH value is 6.5～9.5, ultrasonic stirring, and suction filtration obtains filter cake;
Step 5, filter cake in vacuum is dry, at N
2Decomposed 1～3 hour under following 200 ℃～500 ℃ temperature of gas shiled, promptly get required the multiple element compound carrier MOx-(C1+C2), the M among the MOx represents Sn, Ce, Ni or Co;
Step 6 with the multiple element compound carrier MOx-(C1+C2) of step 5 gained, obtains Pt/ MOx-(C1+C2) catalyst through the in-situ chemical reducing process.
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| CN2010102425667A CN101944620B (en) | 2010-08-02 | 2010-08-02 | Fuel cell catalyst with multi-component composite as carrier and preparation method |
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|---|---|---|---|
| CN2010102425667A CN101944620B (en) | 2010-08-02 | 2010-08-02 | Fuel cell catalyst with multi-component composite as carrier and preparation method |
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| CN101944620A CN101944620A (en) | 2011-01-12 |
| CN101944620B true CN101944620B (en) | 2012-10-31 |
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| CN102773095A (en) * | 2012-08-03 | 2012-11-14 | 上海锦众信息科技有限公司 | Method for preparing platinum-based catalyst for fuel cell |
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