CN105489907A - Carbon-nanotube-loaded platinum-iron superlattice alloy nanoparticles and preparation method therefor - Google Patents
Carbon-nanotube-loaded platinum-iron superlattice alloy nanoparticles and preparation method therefor Download PDFInfo
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- CN105489907A CN105489907A CN201510857841.9A CN201510857841A CN105489907A CN 105489907 A CN105489907 A CN 105489907A CN 201510857841 A CN201510857841 A CN 201510857841A CN 105489907 A CN105489907 A CN 105489907A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/90—Selection of catalytic material
- H01M4/92—Metals of platinum group
- H01M4/921—Alloys or mixtures with metallic elements
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/88—Processes of manufacture
- H01M4/8878—Treatment steps after deposition of the catalytic active composition or after shaping of the electrode being free-standing body
- H01M4/8882—Heat treatment, e.g. drying, baking
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/90—Selection of catalytic material
- H01M4/92—Metals of platinum group
- H01M4/925—Metals of platinum group supported on carriers, e.g. powder carriers
- H01M4/926—Metals of platinum group supported on carriers, e.g. powder carriers on carbon or graphite
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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
Abstract
The invention relates to carbon-nanotube-loaded platinum-iron superlattice alloy nanoparticles used for an oxygen reduction reaction of a proton film fuel cell negative electrode, and a preparation method for the nanoparticles. Chloroplatinic acid and ferrous nitrate are used as a precursor; carbon-nanotube-loaded platinum-iron alloy nanoparticles are obtained by adopting a sodium borohydride reduction method implemented in an ethylene glycol solution; then the carbon-nanotube-loaded alloy nanoparticles are subjected to thermal annealing processing in an inert gas atmosphere to convert the carbon-nanotube-loaded alloy nanoparticles into the carbon-nanotube-loaded platinum-iron superlattice alloy nanoparticles. The method is simple in process, safe in operation, free of reduction gas in the thermal annealing process, and high in controllability; and the activity and the stability of the catalyst oxidization reduction reaction of the obtained product catalyst are both improved at a relative high degree.
Description
Technical field
The invention belongs to eelctro-catalyst field, be specifically related to a kind of carbon nanotube loaded platinum-iron superlattice alloy nano particle as proton membrane fuel battery cathod redox reactions and preparation method thereof.
Background technology
Along with population, the quick growth of industry, environmental pollution and energy shortage problem highlight day by day, and the energy conversion apparatus of exploitation high-efficiency cleaning becomes focus and the difficult point of Present S & T Development.Proton membrane fuel battery is owing to having high-energy-density, and low operating temperature, the features such as transformation efficiency is high, cleanliness without any pollution, portable, receive and pay close attention to widely.But, the electrode reaction of proton membrane fuel battery, especially the redox reactions overpotential of negative electrode is high, dynamics is slow, reaction is difficult to carry out, and therefore often adopts high surface area carbon loading platinum particle as eelctro-catalyst, to improve its electrocatalytic reaction efficiency.Because the cost of platinum is higher, long-play less stable in acid condition, the commercialization of proton membrane fuel battery is subject to high cost, the very big restriction of the problems such as low life-span, and its actual conversion performance and transformation efficiency also need to be improved further.In the method improving charcoal platinum catalyst catalytic performance, platinum and transition metal are compounded to form alloy structure adjustable nanoparticle surface valence bond structure, are increased substantially the catalytic activity of catalyst by cooperative effect.At present, about platinum-cobalt, platinum-iron, platinum-nickel, the alloy nano particle redox reactions catalyst such as platinum-chromium have relevant report.But because proton membrane fuel battery often runs in acid condition, and transition metal in alloy particle is poor at this system stability inferior, and be easy to separated out by acid dissolve and cause catalyst particle structural damage, activity significantly declines.Therefore; random solid solution alloy is converted into ordered intermetallic compound and introduces shell for the protection of easy-soluble component in alloy; the structure of catalyst particle can be improved from atomic scale, thus improve while realizing its catalytic oxygen reduction reaction Activity and stabill.
Summary of the invention
The object of the invention is to solve charcoal, to carry platinum-ferroalloy nano particle catalytic stability in acid system lower, be difficult to the problem of practical application, improved the Atomic Arrangement of alloy by a kind of method simple and easy to operate, improve the Activity and stabill of catalyst redox reactions.
The invention provides a kind of carbon nanotube loaded platinum-iron superlattice alloy nano particle, is black powder, and the nano particle diameter being carried on carbon nano tube surface is 8-20 nanometer.
The present invention also provides the preparation method of above-mentioned carbon nanotube loaded platinum-iron superlattice alloy nano particle, with chloroplatinic acid, ferrous nitrate is as presoma, in ethylene glycol solution, carbon nanotube loaded platinum-ferroalloy nano particle is prepared by sodium borohydride reduction, again by the thermal anneal process under atmosphere of inert gases, make it to transform into carbon nanotube loaded platinum-iron superlattice alloy nano particle.
In a preferred embodiment of the present invention, the concrete steps of above-mentioned preparation method are as follows:
1) by the concentrated sulfuric acid, red fuming nitric acid (RFNA) with volume ratio (3-1): (1-3) mix, carbon nano-tube is added in nitration mixture, is heated to 50-80 ° of C under agitation, reaction 3-10 hour;
2) the mixed liquor deionized water after reaction in step 1) being terminated dilutes, and suction filtration is separated solid-liquid composition, by solid dry 10-24h in the vacuum drying oven of 40-90 ° of C, obtains the carbon nano-tube of acidification;
3) by step 2) in the carbon nano-tube of acidification that obtains by ultrasonic disperse in 30-300mL ethylene glycol, chloroplatinic acid and ferrous nitrate are dissolved in and are above-mentionedly dispersed with in the ethylene glycol of carbon nano-tube, ultrasonic 20-40min is to mix;
4) mixed solution in step 3) is heated under the condition stirred, add sodium borohydride aqueous solution, keep heating to continue reaction 2-5 hour;
5) gained mixed solution in step 4) is carried out suction filtration separation, gained solid is placed in the dry 10-24h of vacuum drying oven of 40-90 ° of C;
6) the dried solid obtained in step 5) is placed in tube furnace, continues to pass into inert gas, be warming up to 400-900 ° of C, insulation 1-1.5h, takes out products therefrom and is carbon nanotube loaded platinum-iron superlattice alloy nano particle after being cooled to room temperature.
In a preferred embodiment of the present invention, the chloroplatinic acid addition described in step 3) is 10-100mg, and described ferrous nitrate addition is 5-80mg.
In a preferred embodiment of the present invention, the reaction temperature of step 4) heating is 70-100 ° of C, and the concentration of described sodium borohydride aqueous solution is 0.1mol/L, and addition is 00-1000mL.
In a preferred embodiment of the present invention, the heat treated heating rate in tube furnace described in step 6) is 3-5 ° of C/min.
The present invention also protects the above-mentioned carbon nanotube loaded platinum-application of iron superlattice alloy nano particle in proton membrane fuel battery cathod redox reactions.
The concentrated sulfuric acid that said method adopts and red fuming nitric acid (RFNA) can adopt commercially available product, as adopt concentration be 98% sulfuric acid and nitric acid to be concentration be 65% nitric acid, carbon nano-tube is that the preparation method of this area routine prepares, as prepared by CVD method.
Adopt method of the present invention to prepare carbon nanotube loaded platinum-iron superlattice alloy nano particle, there is following beneficial effect:
1, present device technique is simple, handling safety, do not need in thermal annealing process to pass into reducibility gas, product crystalline texture can be controlled by the adjustment of presoma ratio, can be controlled the particle diameter of gained nano particle by the adjustment of annealing temperature, the Activity and stabill of products therefrom catalyst redox reactions is improved all largely.
2, adopt in the present invention ethylene glycol as reduction dispersion solvent, suitably can slow down the reduction reaction rate of sodium borohydride, with proof load in carbon nano tube surface particle fine uniform distribute.
Accompanying drawing explanation
Fig. 1 is the transmission electron microscope picture of the carbon nanotube loaded platinum-iron superlattice alloy nano particle of preparation in embodiment 1;
Fig. 2 is the steady-state polarization of the carbon nanotube loaded platinum-iron superlattice alloy nano particle catalytic oxygen reduction reaction of preparation in embodiment 1;
Fig. 3 is carbon nanotube loaded platinum-iron superlattice alloy nano particle, carbon nanotube loaded platinum-iron disordered alloy particle and the steady-state polarization of business platinum/carbon black catalyst before and after stability test prepared by embodiment 1.
Embodiment
In order to make object of the present invention, technical scheme and advantage clearly understand, below in conjunction with specific embodiment, the present invention is further elaborated.Should be appreciated that specific embodiment described herein only in order to explain the present invention, and be not construed as limiting the invention.
embodiment 1
1) by the 150mL concentrated sulfuric acid, 50mL red fuming nitric acid (RFNA) mixes, and adds in nitration mixture, is heated to 70 ° of C under agitation, react 1g carbon nano-tube 5 hours;
2) mixed liquor after reaction in step 1) being terminated slowly adds in 1000mL deionized water under agitation, is separated solid-liquid composition, by solid dry 12h in the vacuum drying oven of 60 ° of C, obtains the carbon nano-tube of acidification by suction filtration;
3) get step 2) in the carbon nano-tube 50mg of acidification that obtains, be placed in there-necked flask, add 100mL ethylene glycol, ultrasonic disperse 30min, 33.5mg chloroplatinic acid and 12mg ferrous nitrate are dissolved in and are above-mentionedly dispersed with in the ethylene glycol of carbon nano-tube, continue ultrasonic 30min to mix;
4) mixed solution in step 3) is heated to 80 ° of C under the condition stirred, adds 500mL, the sodium borohydride aqueous solution of 0.1mol/L, keep heating to continue reaction 3 hours;
5) gained mixed solution in step 4) is carried out suction filtration separation, gained solid is placed in the dry 12h of vacuum drying oven of 80 ° of C;
6) the dried solid obtained in step 5) is placed in tube furnace, continue to pass into inert gas, rise to 650 ° of C with the programming rate of 5 ° of C/min, insulation 1h, taking out products therefrom after being cooled to room temperature, is carbon nanotube loaded platinum-iron superlattice alloy nano particle.
Obtained carbon nanotube loaded platinum-iron superlattice alloy nano particle catalyst thus, average particle size is 10 nanometers, and be nucleocapsid structure, core is
l1
0type platinum-iron superlattice structure, shell is that the pure pt atom arrangement of three atomic layers forms.As seen from Figure 1, particle is nucleocapsid structure, and core is the platinum be alternately arranged layer by layer, iron atom, and shell is the pt atom of three atomic layers.As seen from Figure 2, compared with carbon nanotube loaded platinum-iron disordered alloy particle and business platinum/carbon black catalyst, take-off potential and the half wave potential of its catalytic oxygen reduction reaction are shuffled, and catalytic activity improves.From Fig. 3 relatively, the catalytic stability of carbon nanotube loaded platinum-iron superlattice alloy nano particle is significantly improved.
embodiment 2
1) by the 120mL concentrated sulfuric acid, 40mL red fuming nitric acid (RFNA) mixes, and adds in nitration mixture, is heated to 60 ° of C under agitation, react 0.8g carbon nano-tube 10 hours;
2) mixed liquor after reaction in step 1) being terminated slowly adds in 1000mL deionized water under agitation, is separated solid-liquid composition, by solid dry 10h in the vacuum drying oven of 80 ° of C, obtains the carbon nano-tube of acidification by suction filtration;
3) get step 2) in the carbon nano-tube 80mg of acidification that obtains, be placed in there-necked flask, add 150mL ethylene glycol, ultrasonic disperse 30min, 38.6mg chloroplatinic acid and 15.2mg ferrous nitrate are dissolved in and are above-mentionedly dispersed with in the ethylene glycol of carbon nano-tube, continue ultrasonic 30min to mix;
4) mixed solution in step 3) is heated to 80 ° of C under the condition stirred, adds 300mL, the sodium borohydride aqueous solution of 0.1mol/L, keep heating to continue reaction 3 hours;
5) gained mixed solution in step 4) is carried out suction filtration separation, gained solid is placed in the dry 24h of vacuum drying oven of 60 ° of C;
6) the dried solid obtained in step 5) is placed in tube furnace, continue to pass into inert gas, rise to 750 ° of C with the programming rate of 3 ° of C/min, insulation 1h, taking out products therefrom after being cooled to room temperature, is carbon nanotube loaded platinum-iron superlattice alloy nano particle.
Obtained carbon nanotube loaded platinum-iron superlattice alloy nano particle thus, average particle size is 15 nanometers, and be nucleocapsid structure, core is
l1
0type platinum-iron superlattice structure, shell is that the pure pt atom arrangement of three atomic layers forms.
Embodiment above describes general principle of the present invention, principal character and advantage of the present invention.The present invention is not restricted to the described embodiments; what describe in above-described embodiment and specification just illustrates principle of the present invention; and can not limit the scope of the invention by any way; without departing from the scope of the present invention; the present invention also has various changes and modifications, and these changes and improvements are all listed in claimed scope.
Claims (7)
1. carbon nanotube loaded platinum-iron superlattice alloy nano particle, it is characterized in that, be black powder, and the nano particle diameter being carried on carbon nano tube surface is 8-20 nanometer.
2. the preparation method of carbon nanotube loaded platinum according to claim 1-iron superlattice alloy nano particle, it is characterized in that, with chloroplatinic acid, ferrous nitrate is as presoma, in ethylene glycol solution, carbon nanotube loaded platinum-ferroalloy nano particle is prepared by sodium borohydride reduction, again by the thermal anneal process under atmosphere of inert gases, make it to transform into carbon nanotube loaded platinum-iron superlattice alloy nano particle.
3. preparation method according to claim 2, is characterized in that, concrete steps are as follows:
1) by the concentrated sulfuric acid, red fuming nitric acid (RFNA) with volume ratio (3-1): (1-3) mix, carbon nano-tube is added in nitration mixture, is heated to 50-80 ° of C under agitation, reaction 3-10 hour;
2) the mixed liquor deionized water after reaction in step 1) being terminated dilutes, and suction filtration is separated solid-liquid composition, by solid dry 10-24h in the vacuum drying oven of 40-90 ° of C, obtains the carbon nano-tube of acidification;
3) by step 2) in the carbon nano-tube of acidification that obtains by ultrasonic disperse in 30-300mL ethylene glycol, chloroplatinic acid and ferrous nitrate are dissolved in and are above-mentionedly dispersed with in the ethylene glycol of carbon nano-tube, ultrasonic 20-40min is to mix;
4) mixed solution in step 3) is heated under the condition stirred, add sodium borohydride aqueous solution, keep heating to continue reaction 2-5 hour;
5) gained mixed solution in step 4) is carried out suction filtration separation, gained solid is placed in the dry 10-24h of vacuum drying oven of 40-90 ° of C;
6) the dried solid obtained in step 5) is placed in tube furnace, continues to pass into inert gas, be warming up to 400-900 ° of C, insulation 1-1.5h, takes out products therefrom and is carbon nanotube loaded platinum-iron superlattice alloy nano particle after being cooled to room temperature.
4. preparation method according to claim 3, is characterized in that, the chloroplatinic acid addition described in step 3) is 10-100mg, and described ferrous nitrate addition is 5-80mg.
5. preparation method according to claim 3, is characterized in that, the reaction temperature of step 4) heating is 70-100 ° of C, and the concentration of described sodium borohydride aqueous solution is 0.1mol/L, and addition is 00-1000mL.
6. preparation method according to claim 3, is characterized in that, the heat treated heating rate in tube furnace described in step 6) is 3-5 ° of C/min.
7. the carbon nanotube loaded platinum according to claim 1-application of iron superlattice alloy nano particle in proton membrane fuel battery cathod redox reactions.
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| CN107069053A (en) * | 2017-02-03 | 2017-08-18 | 沈阳理工大学 | A kind of method for preparing pt-fe alloy catalyst |
| CN109037606A (en) * | 2018-06-22 | 2018-12-18 | 合肥国轩高科动力能源有限公司 | A kind of carbon coating porous silicon Antaciron composite negative pole material and its preparation, application |
| CN109935847A (en) * | 2017-12-15 | 2019-06-25 | 中国科学院大连化学物理研究所 | A kind of preparation method of the loaded platinum base alloy catalyst of low-temperature fuel cell |
| CN113373345A (en) * | 2021-06-07 | 2021-09-10 | 中氢新能(北京)新能源技术研究院有限公司 | Supported superfine PtCoP ternary alloy nanoparticle for electrocatalytic methanol oxidation and preparation method thereof |
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| CN113373345A (en) * | 2021-06-07 | 2021-09-10 | 中氢新能(北京)新能源技术研究院有限公司 | Supported superfine PtCoP ternary alloy nanoparticle for electrocatalytic methanol oxidation and preparation method thereof |
| CN113373345B (en) * | 2021-06-07 | 2022-05-17 | 中氢新能(北京)新能源技术研究院有限公司 | Supported superfine PtCoP ternary alloy nanoparticle for electrocatalytic methanol oxidation and preparation method thereof |
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