CN104525189A - Polyhedral Pd-Pt alloy nano catalyst and preparation method and application of nano catalyst - Google Patents
Polyhedral Pd-Pt alloy nano catalyst and preparation method and application of nano catalyst Download PDFInfo
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- CN104525189A CN104525189A CN201410832343.4A CN201410832343A CN104525189A CN 104525189 A CN104525189 A CN 104525189A CN 201410832343 A CN201410832343 A CN 201410832343A CN 104525189 A CN104525189 A CN 104525189A
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Abstract
The invention belongs to the technical field of electrochemical energy and relates to a polyhedral Pt-Pd alloy nano catalyst. The preparation method comprises the following steps: by taking octa-aminosilsesquioxane as a stabilizer and taking methanol as a reducing agent, preparing by virtue of a hydrothermal method to obtain the octahedral Pt-Pd alloy nano catalyst with consistent morphology and good dispersity. The polyhedral Pt-Pd alloy nano catalyst has the advantages that the active surface area is large, the catalytic activity is high, harsh conditions are not needed in the reaction, and the operation is simple and feasible. Moreover, the catalyst has huge application prospects in direct formic acid fuel cell anode catalysts.
Description
Technical field
The invention belongs to electrochemical energy technical field, be specifically related to a kind of preparation and application thereof of polyhedron Pt-Pd alloy nano catalyst.
Background technology
Fuel cell, with the advantage such as its high efficiency, high-energy-density, zero-emission, fast startup, is described as the promising High Efficiency Low Pollution Power Generation Technology of 21 century most.Due to the DMFC studied at present exist anode catalyst performance low, easily poisoning, methyl alcohol easily permeate the problems such as Nafion film, methyl alcohol is poisonous, direct methanoic acid fuel cell gets the attention as DMFC substitute.Wherein one of most important critical material of direct methanoic acid fuel cell based on the anode catalyst of Pt and Pt Base Metal.But the noble metal catalyst based on platinum exists the restricted problems such as the finiteness of with high costs and platinum resource, it has become the key factor of restriction direct methanoic acid fuel cell technical development and commercialization process.Therefore, reduce the use amount of noble metal, improve catalytic activity and the stability of catalyst, the manufacturing cost effectively reducing battery becomes and significantly works.
The mode introducing another or two kinds of metals and Pt alloy is the important channel of improving catalyst activity He reducing catalyst cost.In the periodic table of elements, compare other elements in table around Pt, because Pd and Pt has identical face phase cubic structure and theoretical lattice constant relatively, therefore Pd is the selection with the best of Pt alloy.In theory, under proper condition, Pt and Pd can form alloy with any component.Up to the present, researchers have reported a lot of preparation Pt-Pd alloy nano catalyst method, as co-reducing process, and " seed " mediating growth method, and electrochemical displacement method etc.In nano material synthesis, except the component of metal, the pattern of nanocatalyst is also the key factor affecting catalytic performance.Up to the present, the Pt-Pd nano particle of various pattern is in the news and is applied to Oxidation of Formic Acid or hydrogen reduction, comprises hollow ball-shape, nano flower-like, nanometer dendron, concave structure, cube and octahedron etc.
Further research shows, in nano material synthesis, the kind of covering and consumption are the key factors affecting appearance of nano material.In the liquid phase synthesis of metal nano material, covering or surfactant can interact with metal surface, thus change the size of the free energy of different crystal face, and then affect the relative growth rate of different crystal face.This change may cause nano material to produce different-shape.
Summary of the invention
technical problem:technical problem solved by the invention is to provide that a kind of active surface area is large, catalytic activity is high, and reaction does not need exacting terms, and polyhedron Pt-Pd alloy catalyst easy to operation, provides its preparation method and the application in the catalysis of formic acid efficient electric simultaneously.
technical scheme:the method preparing polyhedron Pt-Pd alloy nano catalyst of the present invention, comprises the following steps:
(1) preparation raw material liquid: be in the ratio of 1:1 ~ 9 dispersion solvent that chloroplatinic acid and palladium bichloride dissolution of solid are mixed in methyl alcohol and water in platinum palladium mol ratio; Be the mol ratio of 1:1 ~ 5 by the mol ratio of metal precursor and eight aminosilsesquioxane again, stabilizing agent eight aminosilsesquioxane is added to above-mentioned solution, pH value to 3 ~ 7 of mixed liquor are regulated after sonic oscillation, stirring is kept to make stabilizing agent fully contact complexing with Pd ion with Pt ion, obtain active metal presoma mixed liquor, wherein metal precursor molal quantity is the molal quantity sum of palladium bichloride and chloroplatinic acid;
(2) reduction presoma: the active metal presoma mixed liquor described step (1) prepared is transferred in hydrothermal reaction kettle, and reaction temperature is 90 ~ 170 DEG C, and the reaction time is 5 ~ 10h;
(3) product post processing: by the solid matter in described step (2) product and fluid separation applications, uses water and ethanol repeatedly to clean, in vacuum drying chamber, and heating, drying at 50 ~ 90 DEG C, obtained polyhedron Pt-Pd alloy nano catalyst;
In the preferred version of the inventive method, the water in step (1) and (2) is ultra-pure water.
In the preferred version of the inventive method, for the volume ratio of water and methyl alcohol is 1:1 ~ 6 in step (1) dispersion solvent.
In the preferred version of the inventive method, in step (1), use hydrochloric acid or NaOH adjust ph.
Polyhedron Pt-Pd alloy nano catalyst of the present invention, by the Viability metal precursor mixed liquor of metal Pd, Pt metal and stabilizing agent eight aminosilsesquioxane complexing, then through reduction, Separation of Solid and Liquid, obtain after drying solid product, the mol ratio of described Pt metal and metal Pd is 1:1 ~ 9.
In the preferred version of polyhedron Pt-Pd alloy nano catalyst of the present invention, the mol ratio of metal precursor and eight aminosilsesquioxane is 1:1 ~ 5.
In the preferred version of polyhedron Pt-Pd alloy nano catalyst of the present invention, this catalyst prepares according to said method.
The present invention also comprises the application of above-mentioned polyhedron Pt-Pd alloy nano catalyst in the catalysis of formic acid efficient electric.
The present invention for stabilizing agent, take methyl alcohol as reducing agent with eight aminosilsesquioxane, and prepared the octahedra Pt-Pd nanometer alloy catalyst of consistent appearance, favorable dispersibility by hydrothermal method, this catalyst has polyhedron pattern.Catalyst of the present invention has huge application prospect in direct methanoic acid fuel cell anode catalyst.
beneficial effect:the present invention compared with prior art, has the following advantages:
(1) direct methanoic acid fuel cell solve the anode catalyst performance that DMFC exists low, easily poisoning, methyl alcohol easily permeate the problems such as Nafion film, methyl alcohol are poisonous.
(2) mode of another or two kinds of metals and Pt alloy of introducing, to reduce the use amount of noble metal, effectively reduces the manufacturing cost of battery.
Polyhedron Pt nano particle-Pd alloy catalyst provided by the present invention, with traditional carbon carry Pt-Pd catalyst (Arenz, Physical Chemistry Chemical Physics, 2003; Li, Electrochimica Acta, 2006; Feng, Catalysis Communications, 2011) and other patterns Pt-Pd alloy catalyst (Liu, J. Power Sources, 2009) compare, in catalysis Oxidation of Formic Acid process, polyhedron Pt nano particle-Pd alloy catalyst has lower oxidizing potential, therefore on its surface, formic acid is more easily oxidized, and stable in catalytic performance, lasting.Use eight aminosilsesquioxane as the Morphological control agent of Pt-Pd alloy catalyst in the present invention first, eight aminosilsesquioxane are as a kind of novel organic/inorganic hybridization material, the advantage of hybrid material can be mixed, be played to its nanoscale cage modle skeleton effectively, give the performance that material is outstanding, become the important means preparing high performance material.Naka(Nano Letters, 2002) and Letant(Journal of Physical Chemistry C, 2009) reported and prepare Pd nanosphere by eight aminosilsesquioxane used as stabilizers, but its Morphological control agent as Pt-Pd alloy catalyst still belongs to the first time.Eight aminosilsesquioxane make as Morphological control agent, and nano material preparation process can be made simple; In addition, after having prepared, compare other polymeric complexing agents, eight aminosilsesquioxane can be removed by high speed centrifugation, do not affect the catalytic performance of catalyst.
Accompanying drawing explanation
Fig. 1 is the electron microscope picture of polyhedron Pt1Pd9 alloy nano particle in embodiment 1.
Fig. 2 be in embodiment 1 polyhedron Pt1Pd9 alloy nano particle at 0.5MH
2sO
4cyclic voltammetry curve in+0.5MHCOOH solution.
Fig. 3 is the electron microscope picture of polyhedron Pt3Pd7 alloy nano particle in embodiment 2.
Fig. 4 be in embodiment 2 polyhedron Pt3Pd7 alloy nano particle at 0.5MH
2sO
4cyclic voltammetry curve in+0.5MHCOOH solution.
Fig. 5 is the electron microscope picture of polyhedron Pt5Pd5 alloy nano particle in embodiment 3.
Fig. 6 be in embodiment 3 polyhedron Pt5Pd5 alloy nano particle at 0.5MH
2sO
4cyclic voltammetry curve in+0.5MHCOOH solution.
Detailed description of the invention
Be described in detail below by the technical scheme of embodiment to invention.
The preparation of embodiment 1, Pt1Pd9 alloy
Get the mixed liquor (volume ratio of methyl alcohol and water is 1:1) that 5.2mg chloroplatinic acid solid and 15.9mg palladium bichloride solid (platinum palladium is than being 1:9) are dissolved in methyl alcohol and water; 117.3mg eight aminosilsesquioxane (mol ratio of metal precursor and eight aminosilsesquioxane is 1:1) is added again in above-mentioned solution, 1mol/L hydrochloric acid solution is used to regulate the pH value to 5 of above-mentioned mixed liquor after sonic oscillation, keep stirring to be that stabilizing agent fully contacts complexing with Pd ion with Pt ion, obtain active metal presoma mixed liquor; Be transferred in hydrothermal reaction kettle by the material liquid of preparation, reaction temperature is 90 ~ 170 DEG C, and the reaction time is 10h; By the nano material after reduction and fluid separation applications, water and ethanol is used repeatedly to clean, in vacuum drying chamber, at 50 ~ 90 DEG C, by solid matter heating, drying, obtained polyhedron Pt1Pd9 alloy nano catalyst.
Be scattered in ultra-pure water by a certain amount of PtPd alloy, getting 10ul sample drop at diameter is on 3mm glass-carbon electrode, after drying completely under room temperature, goes the Nafion dissolution homogeneity of 2ul to be coated on catalyst surface, and namely room temperature can be used as working electrode and use after drying.
Polyhedron PtPd alloy is observed to the effect of formic acid efficient catalytic as shown in Figure 1 and Figure 2 for embodiment 1.
The preparation of embodiment 2, Pt3Pd7 alloy
Get the mixed liquor (volume ratio of methyl alcohol and water is 3:1) that 15.5mg chloroplatinic acid solid and 12.5mg palladium bichloride solid (platinum palladium is than being 3:7) are dissolved in methyl alcohol and water; 234.6mg eight aminosilsesquioxane (mol ratio of metal precursor and eight aminosilsesquioxane is 1:5) is added again in above-mentioned solution, 1mol/L hydrochloric acid solution is used to regulate the pH value to 3 of above-mentioned mixed liquor after sonic oscillation, keep stirring to make stabilizing agent fully contact complexing with Pd ion with Pt ion, obtain active metal presoma mixed liquor; Be transferred in hydrothermal reaction kettle by the material liquid of preparation, reaction temperature is 90 ~ 170 DEG C, and the reaction time is 6h; By the nano material after reduction and fluid separation applications, water and ethanol is used repeatedly to clean, in vacuum drying chamber, at 50 ~ 90 DEG C, by solid matter heating, drying, obtained polyhedron Pt3Pd7 alloy nano catalyst.
Observe polyhedron PtPd alloy to the effect of formic acid efficient catalytic as shown in Figure 3, Figure 4 for embodiment 2, load electrode preparation method is with embodiment 1.
The preparation of embodiment 3, Pt5Pd5 alloy
Get the mixed liquor (volume ratio of methyl alcohol and water is 6:1) that 25.9mg chloroplatinic acid solid and 8.9mg palladium bichloride solid (platinum palladium is than being 5:5) are dissolved in methyl alcohol and water; 234.6mg eight aminosilsesquioxane (mol ratio of metal precursor and eight aminosilsesquioxane is 1:2) is added again in above-mentioned solution, 1mol/L hydrochloric acid solution is used to regulate the pH value to 7 of above-mentioned mixed liquor after sonic oscillation, keep stirring to make stabilizing agent fully contact complexing with Pd ion with Pt ion, obtain active metal presoma mixed liquor; Be transferred in hydrothermal reaction kettle by the material liquid of preparation, reaction temperature is 90 ~ 170 DEG C, and the reaction time is 5h; By the nano material after reduction and fluid separation applications, water and ethanol is used repeatedly to clean, in vacuum drying chamber, at 50 ~ 90 DEG C, by solid matter heating, drying, obtained polyhedron Pt5Pd5 alloy nano catalyst.
Observe polyhedron PtPd alloy to the effect of formic acid efficient catalytic as shown in Figure 5, Figure 6 for embodiment 3, load electrode preparation method is with embodiment 1.
Above-described embodiment is only the preferred embodiment of the present invention; be noted that for those skilled in the art; under the premise without departing from the principles of the invention; some improvement and equivalent replacement can also be made; these improve the claims in the present invention and are equal to the technical scheme after replacing, and all fall into protection scope of the present invention.
Claims (8)
1. prepare the method for polyhedron Pt-Pd alloy nano catalyst for one kind: it is characterized in that, the method comprises the following steps:
(1) preparation raw material liquid: be in the ratio of 1:1 ~ 9 dispersion solvent that chloroplatinic acid and palladium bichloride dissolution of solid are mixed in methyl alcohol and water in platinum palladium mol ratio; Be the mol ratio of 1:1 ~ 5 by the mol ratio of metal precursor and eight aminosilsesquioxane again, stabilizing agent eight aminosilsesquioxane is added to above-mentioned solution, pH value to 3 ~ 7 of mixed liquor are regulated after sonic oscillation, keep stirring to make stabilizing agent fully contact complexing with Pd ion with Pt ion, obtain active metal presoma mixed liquor;
(2) reduction presoma: the active metal presoma mixed liquor described step (1) prepared is transferred in hydrothermal reaction kettle, and reaction temperature is 90 ~ 170 DEG C, and the reaction time is 5 ~ 10h;
(3) product post processing: by the solid matter in described step (2) product and fluid separation applications, uses water and ethanol repeatedly to clean, in vacuum drying chamber, and heating, drying at 50 ~ 90 DEG C, obtained polyhedron Pt-Pd alloy nano catalyst.
2. prepare the method for polyhedron Pt-Pd alloy nano catalyst as claimed in claim 1, it is characterized in that: the water in described step (1) and (2) is ultra-pure water.
3. prepare the method for polyhedron Pt-Pd alloy nano catalyst as claimed in claim 1 or 2, it is characterized in that: for the volume ratio of water and methyl alcohol is 1:1 ~ 6 in described step (1) dispersion solvent.
4. prepare the method for polyhedron Pt-Pd alloy nano catalyst as claimed in claim 1 or 2, it is characterized in that: in described step (1), use hydrochloric acid or NaOH adjust ph.
5. a polyhedron Pt-Pd alloy nano catalyst, it is characterized in that: this catalyst is by the Viability metal precursor mixed liquor of metal Pd, Pt metal and stabilizing agent eight aminosilsesquioxane complexing, then through reduction, Separation of Solid and Liquid, obtain after drying solid product, the mol ratio of described Pt metal and metal Pd is 1:1 ~ 9.
6. polyhedron Pt-Pd alloy nano catalyst as claimed in claim 5, is characterized in that: the mol ratio of described metal precursor and eight aminosilsesquioxane is 1:1 ~ 5.
7. as claim: the polyhedron Pt-Pd alloy nano catalyst as described in 5 or 6, is characterized in that: this catalyst method according to claim 1,2,3 or 4 prepares.
8. the application of polyhedron Pt-Pd alloy nano catalyst in the catalysis of formic acid efficient electric described in claim 5,6 or 7.
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Cited By (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN105013475A (en) * | 2015-06-03 | 2015-11-04 | 东南大学 | Mono-dispersed Pd-Pt nano-catalyst and preparation method therefor |
CN105081308A (en) * | 2015-08-24 | 2015-11-25 | 中国科学院上海高等研究院 | Curved-surface Pt-based nanometer bimetallic material with and preparation method and application thereof |
CN107887619A (en) * | 2017-10-27 | 2018-04-06 | 北京航天动力研究所 | A kind of Pt Pd alloy catalysts of morphology controllable and preparation method and application |
CN108630948A (en) * | 2017-03-17 | 2018-10-09 | 天津大学 | A kind of preparation method of octahedron palladium platinum catalyst with core-casing structure |
CN110444774A (en) * | 2018-05-03 | 2019-11-12 | 中国科学院深圳先进技术研究院 | A kind of alloy nano cage catalyst and its preparation method and application |
CN113948729A (en) * | 2021-10-20 | 2022-01-18 | 江苏大学 | Preparation method of binary metal platinum-palladium prismatic catalyst and application of catalyst in direct methanol fuel cell |
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JP2011090916A (en) * | 2009-10-23 | 2011-05-06 | Hitachi Maxell Ltd | Anode catalyst for fuel cell, method of manufacturing the same, and membrane electrode assembly |
CN103056380A (en) * | 2012-12-28 | 2013-04-24 | 南通大学 | Method for self-assembling and preparing bismuth metal nanowire through octa-amino silsesquioxane |
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Cited By (9)
Publication number | Priority date | Publication date | Assignee | Title |
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CN105013475A (en) * | 2015-06-03 | 2015-11-04 | 东南大学 | Mono-dispersed Pd-Pt nano-catalyst and preparation method therefor |
CN105081308A (en) * | 2015-08-24 | 2015-11-25 | 中国科学院上海高等研究院 | Curved-surface Pt-based nanometer bimetallic material with and preparation method and application thereof |
CN108630948A (en) * | 2017-03-17 | 2018-10-09 | 天津大学 | A kind of preparation method of octahedron palladium platinum catalyst with core-casing structure |
CN108630948B (en) * | 2017-03-17 | 2020-11-03 | 天津大学 | Preparation method of octahedral palladium-platinum core-shell structure catalyst |
CN107887619A (en) * | 2017-10-27 | 2018-04-06 | 北京航天动力研究所 | A kind of Pt Pd alloy catalysts of morphology controllable and preparation method and application |
CN107887619B (en) * | 2017-10-27 | 2020-05-08 | 北京航天动力研究所 | Morphology-controllable Pt-Pd alloy catalyst and preparation method and application thereof |
CN110444774A (en) * | 2018-05-03 | 2019-11-12 | 中国科学院深圳先进技术研究院 | A kind of alloy nano cage catalyst and its preparation method and application |
CN110444774B (en) * | 2018-05-03 | 2022-09-23 | 中国科学院深圳先进技术研究院 | Alloy nano cage catalyst and preparation method and application thereof |
CN113948729A (en) * | 2021-10-20 | 2022-01-18 | 江苏大学 | Preparation method of binary metal platinum-palladium prismatic catalyst and application of catalyst in direct methanol fuel cell |
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