CN103055893A - Supported cobalt-platinum superlattice alloy nano particle composite catalyst and preparation method thereof - Google Patents

Supported cobalt-platinum superlattice alloy nano particle composite catalyst and preparation method thereof Download PDF

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CN103055893A
CN103055893A CN2012105690875A CN201210569087A CN103055893A CN 103055893 A CN103055893 A CN 103055893A CN 2012105690875 A CN2012105690875 A CN 2012105690875A CN 201210569087 A CN201210569087 A CN 201210569087A CN 103055893 A CN103055893 A CN 103055893A
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platinum
cobalt
carbon
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CN103055893B (en
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刘景军
赵艳辉
王峰
李志林
吉静
宋夜
鲍剑明
康建忠
王伟红
覃事永
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Beijing University of Chemical Technology
Bluestar Beijing Chemical Machinery Co Ltd
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Beijing University of Chemical Technology
Bluestar Beijing Chemical Machinery Co Ltd
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Abstract

The invention discloses a supported cobalt-platinum superlattice alloy nano particle composite catalyst used for oxygen reduction reactions in alkaline or acid media and a preparation method of the supported cobalt-platinum superlattice alloy nano particle composite catalyst. The catalyst has an L 12 type superlattice structure. The catalyst has high electrocatalytic activity and stability for the oxygen reduction reactions in the alkaline or acid media, greatly reduces the dosage of precious metal platinum, and meanwhile has the advantage of low cost.

Description

Supported cobalt platinum superlattices alloy nano particle composite catalyst and preparation method thereof
Technical field
The invention belongs to the energy and material technical field, be specifically related to a kind of supported cobalt platinum superlattices alloy nano particle composite catalyst that is applied to the oxygen reduction reaction and preparation method thereof.
Background technology
Oxygen reduction reaction is one of most important reaction in the contemporary industry field, is indispensable reaction in various fuel cells, metal-air battery, the processing of sewage electroxidation, the chemical industry electrolysis field.Because therefore the dynamic process that the oxygen reduction reaction is slower, needs efficient oxygen reduction reaction catalyst to promote the oxygen reduction reaction acceleration.Oxygen reduction catalyst mainly contains noble metal and alloy catalyst, metal oxide and metallo-chelate catalyst.At present, commercial Pt/C catalyst is the most frequently used oxygen reduction electro-catalyst, has advantages of active high and good stability.But the Pt/C catalyst is expensive, and cost is high, limits its further application in industry.In addition, the electrochemistry poor durability of Pt/C catalyst in highly acid or strongly basic medium, the chemical property decay is serious, can not satisfy the needs of the medium-term and long-term stable operation of actual industrial production.For above commercial Application problem, people have proposed multiple solution at present: the one, with the size Control of platinum and alloy particle thereof at 2～10nm, to give full play to the good hydrogen reduction electro catalytic activity of metal platinum; The 2nd, platinum is loaded on the larger material with carbon element of specific area, improve the hydrogen reduction catalytic performance of unit mass platinum; The 3rd, significantly improve the electro-chemical activity of noble metal catalyst by the precious metal alloys method.Make platinum and other metal alloyizations can not only improve activity and the durability of Pt/C catalyst, significantly reduce the consumption of platinum simultaneously, thereby significantly reduce the cost of catalyst, the Pt resource of saves valuable.Therefore, the alloying of noble metal is one of focus of at present research with activity and the durability that improves the noble metal oxygen reduction eelctro-catalyst.
Summary of the invention
The object of the invention is to solve that the oxygen reduction electro-catalyst activity is low, poor durability, and the problem such as production cost height, a kind of efficient, inexpensive eelctro-catalyst of oxygen reduction reaction and preparation method thereof that is applicable to is provided.In order to realize purpose of the present invention, intend adopting following technical scheme:
One aspect of the present invention relates to a kind of carbon and carries cobalt platinum superlattices alloy nano particle catalyst, it is characterized in that 2 θ have 23.1 ± 0.1 in the described catalyst X-ray diffractogram O, 32.9 ± 0.1 O, 53.1 ± 0.1 OWith 58.6 ± 0.1 OCharacteristic peak; Preferably, described carbon is carbon black.
In a preferred embodiment of the present invention, the mass ratio of cobalt platinum between 1:13 between the 1:1.
In a preferred embodiment of the present invention, the mass ratio of cobalt platinum and carbon carrier is that 1:5 is between the 1:2.
In another preferred embodiment of the present invention, the particle diameter of described cobalt platinum is between 4-10nm.
The present invention also relates to the preparation method of above-mentioned catalyst on the other hand, and it comprises the steps:
(1) ethylene glycol solution of cobalt chloride hexahydrate and chloroplatinic acid is put into the ethylene glycol that contains carbon carrier, more than the ultrasonic 10min, regulate the above-mentioned pH value of glycol reaction system that contains to 8-10, be preferably between the 8.5-9.5, in ultrasonic disintegrator, pulverize 90-120 time with 1400-1800W power, obtain the black slurries, at 30～90 ℃, be preferably under 70～90 ℃ of stirring states and drip NaBH 4Solution, and react 2～4h under this temperature filters slurries at last, the deionized water washing, and drying obtains having the cobalt nano platinum particle of certain alloying level/carbon matrix precursor powder;
(2) preparation-obtained cobalt nano platinum particle/carbon matrix precursor powder is placed alumina crucible; heat-treat under protective atmosphere: the heating rate with 5～10 ℃/min is raised to 600～1000 ℃; and cooling to sample with the furnace room temperature behind constant temperature 0.5h～1.5h under this temperature, obtain carbon and carry cobalt platinum superlattices alloy catalyst.
In a preferred embodiment of the present invention, described carbon carrier is without chemically treated carbon black.
The carbon of the present invention preparation carries cobalt platinum superlattices alloy nano particle and has L12 type platinum cobalt superlattice structure, has improved platinum and and activity and the durability of alloy catalyst.
Description of drawings
The carbon of Fig. 1: embodiment preparation carries the transmission electron microscope photo of platinum cobalt superlattices alloy catalyst, and interior illustration is the alloy particle transmission electron microscope photo, and the even high degree of dispersion of alloy particle is on the carbon carrier surface, and particle size is at 5～10nm.(wherein (a) prepares the transmission electron microscope photo that carbon carries platinum cobalt superlattices alloy catalyst for embodiment 1; (b) prepare the transmission electron microscope photo that carbon carries platinum cobalt superlattices alloy catalyst for embodiment 2; (c) prepare the transmission electron microscope photo that carbon carries platinum cobalt superlattices alloy catalyst for embodiment 3);
The carbon of Fig. 2: embodiment 1,2,3 preparations carries the X-ray diffractogram of platinum cobalt superlattices alloy catalyst, can find out that the diffraction maximum of heat treatment rear catalyst and the diffraction maximum of L12 type CoPt3 are complementary, and illustrate to have formed superlattice structure;
The carbon of Fig. 3: embodiment 3 preparations carries the rotating circular disk curve comparison figure of the hydrogen reduction of cobalt platinum superlattices alloy catalyst and commercial Pt/C (E-TEX) catalyst.The initial hydrogen reduction current potential of prepared cobalt platinum superlattices alloy catalyst is suitable with commercial Pt/C (E-TEX) catalyst as seen from the figure, and its current density is higher than commercial catalysts, and higher catalytic current is arranged.
The specific embodiment
The invention will be further described below in conjunction with embodiment:
Embodiment 1
Figure 2012105690875100002DEST_PATH_IMAGE001
The ethylene glycol solution of the chloroplatinic acid of the cobalt chloride hexahydrate of 7.5mg and 9.3ml 0.01M is put into the 50ml ethylene glycol that contains 100mg Vulcan XC-72 carbon black, ultrasonic 15min, regulating above-mentioned system pH with 1M NaOH solution is 9, in ultrasonic disintegrator, pulverize 99 times with 1600W power, obtain the black slurries, these slurries are put into flask, under 80 ℃ of stirring states, drip the NaBH of 10ml 0.6M 4Solution, and under this temperature, react 3h, at last slurries are filtered, with the deionized water washing, drying obtains the black precursor powder.
Figure 359890DEST_PATH_IMAGE002
With step
Figure 90080DEST_PATH_IMAGE001
Prepared precursor powder places alumina crucible; heat-treat under protective atmosphere: the heating rate with 8 ℃/min is raised to 1000 ℃; and cooling to sample with the furnace room temperature behind the constant temperature 0.5h under this temperature, the carbon that obtains platinum cobalt alloy ratio and be 3:1 carries cobalt platinum superlattices alloy catalyst.
Embodiment 2
Figure 246648DEST_PATH_IMAGE001
The ethylene glycol solution of the chloroplatinic acid of the cobalt chloride hexahydrate of 38.7mg and 5.4ml 0.01M is put into the 50ml ethylene glycol that contains 100mg Vulcan XC-72 carbon black, ultrasonic 15min, regulating above-mentioned system pH with 1M NaOH solution is 9, in ultrasonic disintegrator, pulverize 99 times with 1600W power, obtain the black slurries, these slurries are put into flask, under 80 ℃ of stirring states, drip the NaBH of 10ml 1M 4Solution, and under this temperature, reacted 3 hours, at last slurries are filtered, with deionized water washing, drying, obtain the precursor powder of black.
With step
Figure 393913DEST_PATH_IMAGE001
Prepared precursor powder places alumina crucible; heat-treat under protective atmosphere: the heating rate with 9 ℃/min is raised to 1000 ℃; and cooling to sample with the furnace room temperature behind the constant temperature 0.5h under this temperature, the carbon that obtains platinum cobalt alloy ratio and be 1:3 carries cobalt platinum superlattices alloy catalyst.
Embodiment 3
Figure 527960DEST_PATH_IMAGE001
The ethylene glycol solution of the chloroplatinic acid of the cobalt chloride hexahydrate of 18.9mg and 7.9ml 0.01M is put into the 50ml ethylene glycol that contains 100mg Vulcan XC-72 carbon black, ultrasonic 15min, regulating above-mentioned system pH with NaOH (1M) solution is 9, in ultrasonic disintegrator, pulverize 99 times with 1600W power, obtain the black slurries, these slurries are put into flask, under 80 ℃ of stirring states, drip the NaBH of 10ml 1.2M 4Solution, and under this temperature, react 3h, at last slurries are filtered, with deionized water washing, drying, obtain the precursor powder of black.
Figure 670359DEST_PATH_IMAGE002
With step
Figure 931576DEST_PATH_IMAGE001
Prepared precursor powder places alumina crucible; heat-treat under protective atmosphere: the heating rate with 8 ℃/min is raised to 1000 ℃; and cooling to sample with the furnace room temperature behind the constant temperature 0.5h under this temperature, the carbon that obtains platinum cobalt alloy ratio and be 1:1 carries cobalt platinum superlattices alloy catalyst.
The above be the specific embodiment of the present invention only, but protection scope of the present invention is not limited to this, and any variation or replacement of expecting without creative work all should be encompassed within protection scope of the present invention.Therefore, protection scope of the present invention should be as the criterion with the protection domain that claims were limited.

Claims (7)

1. a carbon carries cobalt platinum superlattices alloy nano particle catalyst, it is characterized in that 2 θ have 23.1 ± 0.1 in the described catalyst X-ray diffractogram O, 32.9 ± 0.1 O, 53.1 ± 0.1 OWith 58.6 ± 0.1 OCharacteristic peak; Preferably, described carbon is carbon black.
2. catalyst according to claim 1, the mass ratio of cobalt platinum between 1:13 between the 1:1.
3. catalyst according to claim 1, the mass ratio of cobalt platinum and carbon carrier is that 1:5 is between the 1:2.
4. catalyst according to claim 1, the particle diameter of described cobalt platinum is between 4-10nm.
5. the preparation method of the described catalyst of claim 1-4 any one, it comprises the steps:
(1) ethylene glycol solution of cobalt chloride hexahydrate and chloroplatinic acid is put into the ethylene glycol that contains carbon carrier, more than the ultrasonic 10min, regulate the above-mentioned pH value of glycol reaction system that contains to 8-10, be preferably between the 8.5-9.5, in ultrasonic disintegrator, pulverize 90-120 time with 1400-1800W power, obtain the black slurries, at 30～90 ℃, be preferably under 70～90 ℃ of stirring states and drip NaBH 4Solution, and react 2～4h under this temperature filters slurries at last, the deionized water washing, and drying obtains having the cobalt nano platinum particle of certain alloying level/carbon matrix precursor powder;
(2) preparation-obtained cobalt nano platinum particle/carbon matrix precursor powder is placed alumina crucible; heat-treat under protective atmosphere: the heating rate with 5～10 ℃/min is raised to 600～1000 ℃; and cooling to sample with the furnace room temperature behind constant temperature 0.5h～1.5h under this temperature, obtain carbon and carry cobalt platinum superlattices alloy catalyst.
6. method for preparing catalyst according to claim 5, described carbon carrier is without chemically treated carbon black.
In the oxygen reduction reaction of the described catalyst of claim 1-4 any one in alkalescence or acid medium as the application of catalyst.
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CN104014810A (en) * 2014-05-29 2014-09-03 燕山大学 Method for manufacturing strepto-shaped cobalt platinum alloy by using octreotide acetate as template
CN104014811A (en) * 2014-05-29 2014-09-03 燕山大学 Method for manufacturing coralline nanometer cobalt by using octreotide acetate as a template
CN104043453A (en) * 2014-01-06 2014-09-17 北京化工大学 Supported cobaltosic oxide nanometer composite catalyst and use thereof
CN104485463A (en) * 2014-12-30 2015-04-01 西北师范大学 Alloy-oxide composite carbon material noble-metal-loaded catalyst and preparation method of catalyst
CN104475126A (en) * 2014-12-11 2015-04-01 北京化工大学 Carbon-supported core-shell type platinum cobalt-platinum catalyst for fuel cells and preparation method for carbon-supported core-shell type platinum cobalt-platinum catalyst
CN105413709A (en) * 2015-12-11 2016-03-23 中国科学院上海高等研究院 Platinum-cobalt nano bimetallic catalyst adopting multi-cubic branched structure as well as preparation method and application of catalyst
CN105489907A (en) * 2015-11-30 2016-04-13 北京化工大学 Carbon-nanotube-loaded platinum-iron superlattice alloy nanoparticles and preparation method therefor
CN105594035A (en) * 2013-08-09 2016-05-18 日产自动车株式会社 Catalyst particles, electrocatalyst using the same, electrolyte membrane-electrode assembly, and fuel cell using the catalyst particles
CN108470920A (en) * 2018-04-08 2018-08-31 北京化工大学 A kind of graphene-supported platinum cobalt tungsten alloy nano-particle composite catalyst and preparation method thereof for acid medium
CN111224118A (en) * 2019-11-15 2020-06-02 一汽解放汽车有限公司 Multi-element doped platinum-based catalyst and preparation method and application thereof
CN115188979A (en) * 2022-08-31 2022-10-14 北京化工大学 Ordered platinum-cobalt intermetallic compound oxidation procatalyst and preparation method and application thereof

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US10847811B2 (en) 2013-08-09 2020-11-24 Nissan Motor Co., Ltd. Catalyst particle, and electrode catalyst, electrolyte membrane-electrode assembly, and fuel cell using the same
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US10014532B2 (en) 2013-08-09 2018-07-03 Nissan Motor Co., Ltd. Catalyst particle, and electrode catalyst, electrolyte membrane-electrode assembly, and fuel cell using the same
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EP3032624A4 (en) * 2013-08-09 2016-07-27 Nissan Motor Catalyst particles, and electrocatalyst, electrolyte membrane-electrode assembly, and fuel cell using such catalyst particles
CN104043453B (en) * 2014-01-06 2015-12-09 北京化工大学 A kind of support type cobaltosic oxide nano composite catalyst and application
CN104043453A (en) * 2014-01-06 2014-09-17 北京化工大学 Supported cobaltosic oxide nanometer composite catalyst and use thereof
CN104014811A (en) * 2014-05-29 2014-09-03 燕山大学 Method for manufacturing coralline nanometer cobalt by using octreotide acetate as a template
CN104014811B (en) * 2014-05-29 2016-03-02 燕山大学 A kind of octreotide acetate that utilizes is for the method for Template preparation coralloid nano cobalt
CN104014810A (en) * 2014-05-29 2014-09-03 燕山大学 Method for manufacturing strepto-shaped cobalt platinum alloy by using octreotide acetate as template
CN104014810B (en) * 2014-05-29 2016-08-17 燕山大学 A kind of method utilizing octreotide acetate to prepare the spherical cobalt-platinum alloy of chain for template
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CN104485463A (en) * 2014-12-30 2015-04-01 西北师范大学 Alloy-oxide composite carbon material noble-metal-loaded catalyst and preparation method of catalyst
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CN105489907B (en) * 2015-11-30 2018-02-13 北京化工大学 A kind of carbon nanotube loaded platinum iron superlattices alloy nano particle and preparation method thereof
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CN105413709A (en) * 2015-12-11 2016-03-23 中国科学院上海高等研究院 Platinum-cobalt nano bimetallic catalyst adopting multi-cubic branched structure as well as preparation method and application of catalyst
CN105413709B (en) * 2015-12-11 2018-01-30 中国科学院上海高等研究院 A kind of platinum cobalt nanometer bi-metal catalyst of more cubes of dendritic morphologies and its preparation method and application
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