CN105489907B - A kind of carbon nanotube loaded platinum iron superlattices alloy nano particle and preparation method thereof - Google Patents

A kind of carbon nanotube loaded platinum iron superlattices alloy nano particle and preparation method thereof Download PDF

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CN105489907B
CN105489907B CN201510857841.9A CN201510857841A CN105489907B CN 105489907 B CN105489907 B CN 105489907B CN 201510857841 A CN201510857841 A CN 201510857841A CN 105489907 B CN105489907 B CN 105489907B
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carbon nanotube
superlattices
nanotube loaded
iron
alloy nano
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CN105489907A (en
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王峰
刘海静
宋夜
刘景军
李志林
吉静
窦美玲
覃事永
王伟红
康建忠
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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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    • 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
    • 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
    • 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
    • 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
    • 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 present invention relates to a kind of carbon nanotube loaded platinum iron superlattices alloy nano particle as proton membrane fuel battery cathod redox reactions and preparation method thereof, with chloroplatinic acid, ferrous nitrate is as presoma, carbon nanotube loaded pt-fe alloy nano-particle is prepared in ethylene glycol solution by sodium borohydride reduction, again by the thermal anneal process under atmosphere of inert gases, it is allowed to transform into carbon nanotube loaded platinum iron superlattices alloy nano particle.This method technique is simple, safe operation, and reducibility gas need not be passed through in thermal annealing process, and controllability is strong, and the Activity and stabill of products therefrom catalyst redox reactions is largely improved.

Description

A kind of carbon nanotube loaded platinum-iron superlattices alloy nano particle and preparation method thereof
Technical field
The invention belongs to elctro-catalyst field, and in particular to one kind is used as proton membrane fuel battery cathod redox reactions Carbon nanotube loaded platinum-iron superlattices alloy nano particle and preparation method thereof.
Background technology
With population, industrial rapid growth, environmental pollution and energy shortage problem increasingly highlight, and develop high-efficiency cleaning Energy conversion apparatus turns into the focus and difficult point of Present S ＆ T Development.Proton membrane fuel battery is low due to high-energy-density Operation temperature, transformation efficiency are high, cleanliness without any pollution, it is portable the features such as, it is of great interest.However, proton membrane fuel is electric The redox reactions overpotential of the electrode reaction in pond, especially negative electrode is high, and dynamics is slow, and reaction is difficult to, therefore past Toward high surface area carbon loading platinum particle is used as elctro-catalyst, to improve its electrocatalytic reaction efficiency.Due to platinum The cost of category is higher, in acid condition long-play less stable, the commercialization of proton membrane fuel battery by height into Originally, very big limitation the problems such as the low life-span, its actual conversion performance and transformation efficiency also need further to be improved.Carried improving charcoal In the method for platinum catalyst catalytic performance, platinum and transition metal are compounded to form alloy structure and can adjust nanoparticle surface valence link Structure, the catalytic activity of catalyst is increased substantially by cooperative effect.At present, on platinum-cobalt, platinum-iron, palladium-nickel, platinum-chromium Deng the existing relevant report of alloy nano particle redox reactions catalyst.But because proton membrane fuel battery is often in acid Property under the conditions of run, and the transition metal in alloy particle is poor in the system stability inferior, it is easy to is analysed by acid dissolving Go out and cause catalyst particle structural damage, activity significantly declines.Therefore, random solid solution alloy is converted into orderly metal Between compound and be introduced into shell be used for protect easy-soluble component in alloy, can from atomic scale improve catalyst particle structure, Improved so as to realize while its catalytic oxygen reduction reaction Activity and stabill.
The content of the invention
It is relatively low it is an object of the invention to solve charcoal load platinum-ferroalloy nano-particle catalytic stability in acid system, The problem of being difficult to practical application, the Atomic Arrangement of alloy is improved by a kind of method simple and easy to operate, improves catalyst The Activity and stabill of redox reactions.
The present invention provides a kind of carbon nanotube loaded platinum-iron superlattices alloy nano particle, is black powder, is carried on carbon The nano particle diameter of nanotube surface is 8-20 nanometers.
The present invention also provides the preparation method of above-mentioned carbon nanotube loaded platinum-iron superlattices alloy nano particle, with chlorine platinum Acid, ferrous nitrate are prepared in ethylene glycol solution carbon nanotube loaded as presoma, by sodium borohydride reduction Platinum-ferroalloy nano-particle, then by the thermal anneal process under atmosphere of inert gases, it is allowed to transform into carbon nanotube loaded Platinum-iron superlattices alloy nano particle.
In a preferred embodiment of the present invention, above-mentioned preparation method comprises the following steps that：
1）By the concentrated sulfuric acid, concentrated nitric acid with volume ratio（3-1）:（1-3）Mixing, CNT is added in nitration mixture, stirred Under the conditions of be heated to 50-80 °C, react 3-10 hours；
2）By step 1）Mixed liquor after middle reaction terminates is diluted with deionized water, separation solid-liquid composition is filtered, by solid 10-24 h are dried in 40-90 °C of vacuum drying oven, obtain the CNT of acidification；
3）By step 2）In the obtained CNT of acidification by ultrasonic disperse in 30-300 mL ethylene glycol, By chloroplatinic acid and ferrous nitrate be dissolved in it is above-mentioned be dispersed with the ethylene glycol of CNT, ultrasonic 20-40 min are with well mixed；
4）By step 3）In mixed solution heated under conditions of stirring, add sodium borohydride aqueous solution, keep heating Continue to react 2-5 hours；
5）By step 4）Middle gained mixed solution carries out suction filtration separation, and gained solid is placed in 40-90 °C of vacuum drying oven Dry 10-24 h；
6）By step 5）In obtained dried solid be placed in tube furnace, be continually fed into inert gas, be warming up to 400-900 °C, 1-1.5 h are incubated, taking-up products therefrom is that carbon nanotube loaded platinum-iron superlattices close after being cooled to room temperature Golden nanometer particle.
In a preferred embodiment of the present invention, step 3）Described chloroplatinic acid addition is 10-100 mg, described Ferrous nitrate addition is 5-80 mg.
In a preferred embodiment of the present invention, step 4）The reaction temperature of heating is 70-100 °C, described boron hydrogen The concentration for changing sodium water solution is 0.1mol/L, and addition is 00-1000 mL.
In a preferred embodiment of the present invention, step 6）The described heating rate being heat-treated in tube furnace is 3- 5°C/min。
The present invention also protects above-mentioned carbon nanotube loaded platinum-iron superlattices alloy nano particle cloudy in proton membrane fuel battery Application in the redox reactions of pole.
The above method use the concentrated sulfuric acid and concentrated nitric acid can use commercially available product, as use concentration for 98% sulfuric acid And nitric acid is the nitric acid that concentration is 65%, CNT is that the conventional preparation method in this area is prepared, such as by CVD side It is prepared by method.
Carbon nanotube loaded platinum-iron superlattices alloy nano particle is prepared using the method for the present invention, had beneficial below Effect：
1st, present device technique is simple, safe operation, reducibility gas need not be passed through in thermal annealing process, by preceding The adjustment for driving body ratio can control product crystalline texture, the particle diameter of nano-particle as obtained by the adjustment of annealing temperature is controllable, The Activity and stabill of products therefrom catalyst redox reactions is largely improved.
2nd, reduction dispersion solvent is used as using ethylene glycol in the present invention, can suitably slows down the reduction reaction speed of sodium borohydride Rate, with proof load in carbon nano tube surface particle fine uniform be distributed.
Brief description of the drawings
Fig. 1 is the transmission electron microscope picture of the carbon nanotube loaded platinum-iron superlattices alloy nano particle prepared in embodiment 1；
Fig. 2 is that the carbon nanotube loaded platinum-iron superlattices alloy nano particle catalytic oxygen reduction prepared in embodiment 1 is anti- The steady-state polarization answered；
Fig. 3 be embodiment 1 prepare carbon nanotube loaded platinum-iron superlattices alloy nano particle, carbon nanotube loaded platinum- Iron disordered alloy particle and business platinum/steady-state polarization of the carbon black catalyst before and after stability test.
Embodiment
In order to make the purpose , technical scheme and advantage of the present invention be clearer, below in conjunction with specific embodiment, to this Invention is further elaborated.It should be appreciated that specific embodiment described herein is only to explain the present invention, without structure Into limitation of the present invention.
Embodiment 1
1）By the 150 mL concentrated sulfuric acids, the mixing of 50 mL concentrated nitric acids, 1g CNTs are added in nitration mixture, under agitation 70 °C are heated to, is reacted 5 hours；
2）By step 1）Mixed liquor after middle reaction terminates is slowly added in 1000 mL deionized waters under agitation, Solid-liquid composition is separated by filtering, solid is dried into 12 h in 60 °C of vacuum drying oven, obtains the carbon nanometer of acidification Pipe；
3）Take step 2）In the obtained mg of CNT 50 of acidification, be placed in three-necked flask, add 100 mL second Glycol, the min of ultrasonic disperse 30,33.5 mg chloroplatinic acids and 12 mg ferrous nitrates are dissolved in the above-mentioned CNT that is dispersed with In ethylene glycol, continue 30 min of ultrasound with well mixed；
4）By step 3）In mixed solution be heated to 80 °C under conditions of stirring, add 500 mL, 0.1 mol/L Sodium borohydride aqueous solution, keep heating continue reaction 3 hours；
5）By step 4）Middle gained mixed solution carries out suction filtration separation, and gained solid is placed in 80 °C of vacuum drying oven and done Dry 12 h；
6）By step 5）In obtained dried solid be placed in tube furnace, inert gas is continually fed into, with 5 °C/min Programming rate rise to 650 °C, be incubated 1 h, products therefrom taken out after being cooled to room temperature, be that carbon nanotube loaded platinum-iron is super brilliant Lattice alloy nano particle.
Thus carbon nanotube loaded platinum-iron superlattices alloy nano particle catalyst is made, average particle size is received for 10 Rice, is core shell structure, core isL10Type platinum-iron superlattice structure, shell be the pure pt atom arrangement of three atomic layers and Into.As seen from Figure 1, particle is core shell structure, and core is the platinum being alternately arranged layer by layer, and iron atom, shell is three The pt atom of atomic layer.As seen from Figure 2, it is catalyzed with carbon nanotube loaded platinum-iron disordered alloy particle and business platinum/carbon black Agent is compared, and the take-off potential and half wave potential of its catalytic oxygen reduction reaction are shuffled, and catalytic activity improves.Can by Fig. 3 comparison Know, the catalytic stability of carbon nanotube loaded platinum-iron superlattices alloy nano particle is significantly improved.
Embodiment 2
1）By the 120 mL concentrated sulfuric acids, the mixing of 40 mL concentrated nitric acids, 0.8 g CNTs are added in nitration mixture, in stirring bar 60 °C are heated under part, is reacted 10 hours；
2）By step 1）Mixed liquor after middle reaction terminates is slowly added in 1000 mL deionized waters under agitation, Solid-liquid composition is separated by filtering, solid is dried into 10 h in 80 °C of vacuum drying oven, obtains the carbon nanometer of acidification Pipe；
3）Take step 2）In the obtained mg of CNT 80 of acidification, be placed in three-necked flask, add 150 mL Ethylene glycol, the min of ultrasonic disperse 30,38.6 mg chloroplatinic acids and 15.2 mg ferrous nitrates are dissolved in and above-mentioned are dispersed with carbon nanometer In the ethylene glycol of pipe, continue 30 min of ultrasound with well mixed；
4）By step 3）In mixed solution be heated to 80 °C under conditions of stirring, add 300 mL, 0.1 mol/ L sodium borohydride aqueous solution, heating is kept to continue reaction 3 hours；
5）By step 4）Middle gained mixed solution carries out suction filtration separation, and gained solid is placed in 60 °C of vacuum drying oven and done Dry 24 h；
6）By step 5）In obtained dried solid be placed in tube furnace, be continually fed into inert gas, with 3 °C/ Min programming rate rises to 750 °C, is incubated 1 h, takes out products therefrom after being cooled to room temperature, be carbon nanotube loaded platinum-iron Superlattices alloy nano particle.
Thus carbon nanotube loaded platinum-iron superlattices alloy nano particle is made, average particle size is 15 nanometers, is core Shell structure, core areL10Type platinum-iron superlattice structure, shell are that the pure pt atom arrangement of three atomic layers forms.
Embodiment above describes general principle, principal character and the advantages of the present invention of the present invention.The present invention is not by upper State the limitation of embodiment, merely illustrating the principles of the invention described in above-described embodiment and specification, and can not be with any side Formula limits the scope of the present invention, and without departing from the scope of the present invention, various changes and modifications of the present invention are possible, this A little changes and improvements are all included in claimed scope.

Claims (4)

1. a kind of carbon nanotube loaded platinum-iron superlattices alloy nano particle, it is characterised in that be prepared via a method which Arrive：
1）By the concentrated sulfuric acid, concentrated nitric acid with volume ratio（3-1）:（1-3）Mixing, CNT is added in nitration mixture, in stirring condition Under be heated to 50-80 °C, react 3-10 hours；
2）By step 1）Mixed liquor after middle reaction terminates is diluted with deionized water, separation solid-liquid composition is filtered, by solid in 40- 10-24 h are dried in 90 °C of vacuum drying oven, obtain the CNT of acidification；
3）By step 2）In the obtained CNT of acidification by ultrasonic disperse in 30-300 mL ethylene glycol, by chlorine Platinic acid and ferrous nitrate be dissolved in it is above-mentioned be dispersed with the ethylene glycol of CNT, ultrasonic 20-40 min are with well mixed；
4）By step 3）In mixed solution heated under conditions of stirring, add sodium borohydride aqueous solution, keep heating continue React 2-5 hours；
5）By step 4）Middle gained mixed solution carries out suction filtration separation, and gained solid is placed in 40-90 °C of vacuum drying oven and dried 10-24 h；
6）By step 5）In obtained dried solid be placed in tube furnace, be continually fed into inert gas, be warming up to 400-900 °C, 1-1.5 h are incubated, taking-up products therefrom is carbon nanotube loaded platinum-iron superlattices alloy nanoparticle after being cooled to room temperature Son；
Step 3）Described chloroplatinic acid addition is 10-100 mg, and described ferrous nitrate addition is 5-80 mg.
2. preparation method according to claim 1, it is characterised in that step 4）The reaction temperature of heating is 70-100 °C, The concentration of described sodium borohydride aqueous solution is 0.1mol/L, and addition is 300-1000 mL.
3. preparation method according to claim 1, it is characterised in that step 6）The described liter being heat-treated in tube furnace Warm speed is 3-5 °C/min.
4. carbon nanotube loaded platinum-iron superlattices alloy nano particle any one of claim 1-3 fires in proton membrane Expect the application in cell cathode redox reactions.
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CN107069053B (en) * 2017-02-03 2019-06-18 沈阳理工大学 A method of preparing pt-fe alloy catalyst
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
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
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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