CN104600327B - A kind of preparation method of carbon-supported nano platinum alloy catalyst - Google Patents

A kind of preparation method of carbon-supported nano platinum alloy catalyst Download PDF

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Publication number
CN104600327B
CN104600327B CN201410820939.2A CN201410820939A CN104600327B CN 104600327 B CN104600327 B CN 104600327B CN 201410820939 A CN201410820939 A CN 201410820939A CN 104600327 B CN104600327 B CN 104600327B
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carbon
transition metal
drying
supported nano
nano platinum
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CN104600327A (en
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章俊良
朱凤鹃
沈水云
夏国锋
吴若飞
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Shanghai Jiaotong University
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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
    • 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
    • H01M4/90—Selection of catalytic material
    • H01M4/92—Metals of platinum group
    • H01M4/921—Alloys or mixtures with metallic elements
    • 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 provides a kind of preparation method of carbon-supported nano platinum alloy catalyst；Methods described comprises the following steps：Step 1: Pt/C carbon-supported nano platinum catalysts are dispersed in 3d transition metal salt solutions, Pt/C suspension is prepared into；Step 2: step one gained Pt/C suspension is dried under the conditions of≤80 DEG C, drying sample is obtained；Step 3: drying sample obtained by step 2 is ground, reduction and alloying in reducing atmosphere are placed in；Step 4: product obtained by step 3 is carried out into de- alloy treatment；Carbon-supported nano platinum alloy catalyst is obtained after washing, drying.The advantage of the invention is that preparation method is simple, obtained catalyst alloy particle is evenly distributed on the carbon carrier, uniform component, and catalytic oxidation-reduction performance is high.

Description

A kind of preparation method of carbon-supported nano platinum alloy catalyst
Technical field
The present invention relates to a kind of preparation method of carbon-supported nano platinum alloy catalyst (Pt-alloy/C), belong to materials synthesis And electrochemical technology field.
Background technology
Proton Exchange Membrane Fuel Cells (PEMFC) because its running temperature low (80 DEG C or so), power density is high, it is fast to start, The advantages of power match speed is fast receives significant attention.In the fuel cell of all polymorphic types, H2/ air PEMFC is light vapor Car and the first choice of building energy supply.
At present, it is that catalyst Pt supports demand too to hinder PEMFC wide variety of principal element on automobile Height, so as to cause fuel cell car high expensive, compares with vapour/diesel vehicle and lacks competitiveness.Pt loadings are wherein solved to ask Topic, mainly sets about from reduction negative electrode platinum demand, because it is about 90% that negative electrode platinum, which supports demand accounting, at present.Reduce negative electrode platinum Carrying capacity, inevitable requirement exploitation has high activity, the catalyst of high stability and the utilization rate for improving catalyst.
At present, it is believed to be expected to realize that one of approach of negative electrode platinum carrying capacity reduction is by Pt and 3d transition metal alloys Change, alloying rear catalyst activity can improve more than 2 times.Preparation method about the alloy catalyst is a lot of, and low temperature is organic Liquid phase reduction, microemulsion method, vapour deposition process, electrochemical deposition method and dipping-high temperature reduction method etc., by contrast, has The Patents for closing dipping high temperature reduction method are more, and the equipment and raw material required for this method are commonplace, and process is simple Easily manipulation, is more hopeful to realize that amplification produces and reduces the production cost of alloy catalyst.But current dipping-high temperature reduction legal system Standby alloy catalyst uniform component sex chromosome mosaicism is still than more prominent, and this largely have impact on the homogeneous of alloy catalyst performance Property.
The content of the invention
For defect of the prior art, it is an object of the invention to provide a kind of carbon-supported nano platinum alloy catalyst (Pt- Alloy/C preparation method), overcomes existing dipping-high temperature reduction method technology of preparing to there is problem；The present invention from dispersing mode, The importance such as solvent species and drying mode considers that there is provided a kind of simple carbon-supported nano conjunction for easily realizing catalyst homogeneity Au catalyst (Pt-alloy/C) synthetic method, is distributed using the catalyst alloy particle made by this method on carbon Even, uniform component, and catalytic oxidation-reduction performance is high.
The present invention is achieved by the following technical solutions：
The present invention relates to a kind of preparation method of carbon-supported nano platinum alloy catalyst (Pt-alloy/C), the preparation method Comprise the following steps：
Step 1: Pt/C carbon-supported nano platinum catalysts are dispersed in 3d transition metal salt solutions, Pt/C suspensions are prepared into Liquid；
Step 2: step one gained Pt/C suspension is dried under the conditions of≤80 DEG C, drying sample is obtained；
Step 3: drying sample obtained by step 2 is ground, reduction and alloying in reducing atmosphere are placed in；
Step 4: product obtained by step 3 is carried out into de- alloy treatment；Obtain producing carbon-supported nano platinum after washing, drying Alloy catalyst (Pt-alloy/C).
Preferably, in step one, the scattered method is the one or more in standard machinery stirring, shearing, ultrasound.
Preferably, in step one, described 3d transition metal salt solutions include 3d transition metal salts, non-3d transition metal Salt, solvent；
Preferably, the 3d transition metal salts include the nitrate, sulfate, chlorination of copper, cobalt, nickel, iron, manganese and chromium Salt, carbonate, acetate, formates or oxalates.
Preferably, the non-3d transition metal salts include palladium, rhodium, iridium, osmium, ruthenium, the chloride of gold, bromide or chlorine complexing Hydrochlorate.
Preferably, the palladium, rhodium, iridium, osmium, ruthenium, the chlorine complexing hydrochlorate of gold include palladium bichloride, palladium bromide, potassium chloropalladate, vinegar The sour potassium of the sour ammonium of sour palladium, rhodium chloride, chlorine rhodium, chlordene rhodium, iridous chloride, iridic chloride, chloro-iridic acid, potassium osmate, chlordene osmic acid Potassium, ruthenium trichloride, ruthenium hydrochloride ammonium, gold chloride, gold trichloride, sodium terachloraurate or tetra chlorauric acid ammonia.
Preferably, solvent is water, isopropanol, ethanol, methanol, ether, acetone, N, N- in the 3d transition metal salt solutions One or more of mixed solvents in dimethylformamide, ethylene glycol, glycerine.
Preferably, the metallic atom of the 3d transition metal salts, non-3d transition metal salts in 3d transition metal salt solutions Molar concentration is respectively 0.20~1.0mol/L, 0.01~0.15mol/L.
Preferably, step one, the quality of the Pt/C carbon-supported nanos platinum catalyst and solvent in 3d transition metal salt solutions Than for 1：(5~20).
Preferably, in step 2, described drying means is natural drying, heat drying, freeze-drying, vacuum drying or Spray drying.
Preferably, in step 3, described alloying temperature is 600~1000 DEG C；The alloying is referred specifically in alloy At a temperature of change, the metal formation in Platinum Nanoparticles in Pt/C carbon-supported nano platinum catalysts on carbon carrier and the 3d solution being reduced is closed Gold.
Preferably, in step 3, the reducing atmosphere is specially H2/N2Mixed gas or H2/ Ar mixed gas；Its In, the volume fraction of hydrogen is less than 20%.
Preferably, in step 4, the method for the de- alloy treatment includes acidleach and takes off alloy or the de- alloy of electrochemistry；Washing Mode include filter membrane dialysis or filter type；Drying mode includes vacuum drying, spray drying, freeze-drying or common Heat drying.
Preferably, the acidleach takes off the sulfuric acid or nitric acid that alloy uses 1M, and condition is 60~80 DEG C, 12~48h.
Compared with prior art, the present invention has following beneficial effect：
(1) by changing, the solvent of 3d transition metal salt solutions is constituted the present invention and solvent burden ratio can be significantly improved and received Composition, distribution and the performance uniformity of rice alloy catalyst；
(2) present invention can significantly improve conjunction by improving the dispersing technology of the 3d transition metal salt suspensioning liquids containing Pt/C Composition, distribution and the performance uniformity of Au catalyst；
(3) present invention can improve the reduction of alloy catalyst by optimized alloy temperature range and de- alloy condition (ORR) catalytic activity is reacted, the quality specific activity measured under 0.9V voltages is 0.40A/mgPt, area specific activity is 0.66mA/ cmPt 2。
Brief description of the drawings
By reading the detailed description made with reference to the following drawings to non-limiting example, further feature of the invention, Objects and advantages will become more apparent upon：
Fig. 1 is Pt-alloy/C TEM photos；
Pt mass specific activity and the graph of a relation of cell voltage that Fig. 2 obtains for fuel cell test.
Embodiment
With reference to specific embodiment, the present invention is described in detail.Following examples will be helpful to the technology of this area Personnel further understand the present invention, but the invention is not limited in any way.It should be pointed out that to the ordinary skill of this area For personnel, without departing from the inventive concept of the premise, various modifications and improvements can be made.These belong to the present invention Protection domain.
Embodiment 1
The present embodiment is related to a kind of preparation method of carbon-supported nano platinum alloy catalyst (Pt-alloy/C), methods described bag Include following steps：
Step 1,6g Pt/C carbon-supported nanos platinum catalyst (platinum content is 30wt%) is added under standard machinery stirring condition It is added to (the NO containing Co3)2·6H2O 16.17g and HAuCl4·3H2O 0.47g 60ml water, alcohol mixed solution (water and ethanol Volume ratio be 2:1) it is, follow-up that the dispersing mode being combined, ultrasonic 30mins, standard machinery are stirred with standard machinery using ultrasound 30mins is stirred, is repeated twice, obtains suspension；
Step 2, the suspension in step 1 is heated to 80 DEG C, freeze-day with constant temperature 12h under standard machinery stirring condition；
Step 3, the drying sample in step 2 is ground, is subsequently placed in 10%H2/N2In gaseous mixture, 800 DEG C, perseverance are heated to Warm 12h；
Step 4, the sample obtained in step 3 is placed in 80 DEG C of 1M HNO3De- alloy treatment 48h, washed in solution Filter and 80 DEG C of vacuum drying 8h.
Effect：The TEM photos of the prepared catalyst of embodiment 1 are as shown in figure 1, distribution ratio of the alloy nanoparticle on carbon It is more uniform.The quality specific activity measured under 0.9V voltages is as shown in Fig. 2 its value is 0.40A/mgPt。
Embodiment 2
The present embodiment is the change case of embodiment 1, other implementation condition be the same as Examples 1, and change part is：In step 1 Solvent, pure water solvent is changed to by the mixed solvent of water and ethanol.
Effect：The quality specific activity that carbon-supported nano platinum alloy catalyst manufactured in the present embodiment is measured under 0.9V voltages is 0.31A/mgPt。
Embodiment 3
The present embodiment is the change case of embodiment 1, other implementation condition be the same as Examples 1, and change part is：In step 4 Acid solution, by 1M HNO3Solution is changed to 1M H2SO4Solution.
Effect：The quality specific activity that carbon-supported nano platinum alloy catalyst manufactured in the present embodiment is measured under 0.9V voltages is 0.30A/mgPt。
Embodiment 4
The present embodiment is the change case of embodiment 2, other implementation condition be the same as Examples 2, and change part is only that：Step 2 In drying mode, by heat drying be changed to freeze-drying.
Effect：The quality specific activity measured under 0.9V voltages is 0.34A/mgPt。
Embodiment 5
The present embodiment is the change case of embodiment 1, other implementation condition be the same as Examples 1, and change part is：In step 3 Alloying temperature be changed to 900 DEG C by 800 DEG C.
Effect：The quality specific activity that carbon-supported nano platinum alloy catalyst manufactured in the present embodiment is measured under 0.9V voltages is 0.34A/mgPt。
Embodiment 6
The present embodiment is the change case of embodiment 1, other implementation condition be the same as Examples 1, and change part is：In step 3 Alloying temperature be changed to 700 DEG C by 800 DEG C.
Effect：The quality specific activity that carbon-supported nano platinum alloy catalyst manufactured in the present embodiment is measured under 0.9V voltages is 0.30A/mgPt。
Embodiment 7
The present embodiment is the change case of embodiment 1, and other conditions are same as Example 1, and change part is：In step 1, Co(NO3)2·6H2O concentration is 0.20mol/L, HAuCl4·3H2O concentration is 0.15mol/L.
Effect：The quality specific activity that carbon-supported nano platinum alloy catalyst manufactured in the present embodiment is measured under 0.9V voltages is 0.43A/mgPt。
Embodiment 8
The present embodiment is the change case of embodiment 1, and other conditions are same as Example 1, and change part is：In step 1, 3d transition metal salts are copper chloride, and non-3d transition metal salts are iridic chloride.
Effect：The quality specific activity that carbon-supported nano platinum alloy catalyst manufactured in the present embodiment is measured under 0.9V voltages is 0.41A/mgPt。
Embodiment 9
The present embodiment is the change case of embodiment 1, and other conditions are same as Example 1, and change part is：In step 1, The mass ratio of Pt/C carbon-supported nanos platinum catalyst and solvent is 1:5.
Effect：The quality specific activity that carbon-supported nano platinum alloy catalyst manufactured in the present embodiment is measured under 0.9V voltages is 0.44A/mgPt。
Embodiment 10
The present embodiment is the change case of embodiment 1, and other conditions are same as Example 1, and change part is：In step 1, The mass ratio of Pt/C carbon-supported nanos platinum catalyst and solvent is 1:20.
Effect：The quality specific activity that carbon-supported nano platinum alloy catalyst manufactured in the present embodiment is measured under 0.9V voltages is 0.40A/mgPt。
Embodiment 11
The present embodiment is the change case of embodiment 1, and other conditions are same as Example 1, and change part is：In step 1, In step 3, alloying temperature is 600 DEG C.
Effect：The quality specific activity that carbon-supported nano platinum alloy catalyst manufactured in the present embodiment is measured under 0.9V voltages is 0.34A/mgPt。
Embodiment 12
The present embodiment is the change case of embodiment 1, and other conditions are same as Example 1, and change part is：In step 1, In step 3, alloying temperature is 1000 DEG C.
Effect：The quality specific activity that carbon-supported nano platinum alloy catalyst manufactured in the present embodiment is measured under 0.9V voltages is 0.38A/mgPt 2。
Comparative example 1
This comparative example is the comparative example of embodiment 1, other condition be the same as Examples 1, and difference is：It is molten in step 1 Agent volume is changed into 300ml from 60ml, and the quality of Pt/C carbon-supported nano platinum catalysts is 30g, now Co (NO3)2·6H2O concentration is small In 0.2mol/L, HAuCl4·3H2O concentration is less than 0.01mol/L.
Effect：The quality specific activity that is measured under 0.9V voltages of carbon-supported nano platinum alloy catalyst prepared by this comparative example is 0.28A/mgPt。
Comparative example 2
This comparative example is the comparative example of embodiment 1, other condition be the same as Examples 1, and difference is：Conjunction in step 3 Aurification temperature is changed to 1200 DEG C by 800 DEG C.
Effect：The quality specific activity that is measured under 0.9V voltages of carbon-supported nano platinum alloy catalyst prepared by this comparative example is 0.20A/mgPt。
Comparative example 3
This comparative example is the comparative example of embodiment 1, other condition be the same as Examples 1, and difference is：It is de- in step 4 The time of alloy treatment is changed into 6h from 48h.
Effect：The quality specific activity that is measured under 0.9V voltages of carbon-supported nano platinum alloy catalyst prepared by this comparative example is 0.31A/mgPt。
Comparative example 4
This comparative example is the comparative example of embodiment 1, other condition be the same as Examples 1, and difference is：Perseverance in step 4 The warm time is changed into 55h from 48h.
Effect：The quality specific activity that is measured under 0.9V voltages of carbon-supported nano platinum alloy catalyst prepared by this comparative example is 0.26A/mgPt。
Comparative example 5
This comparative example is the comparative example of embodiment 1, other condition be the same as Examples 1, and difference is：Perseverance in step 4 The warm time is changed into 10h from 48h..
Effect：The quality specific activity that is measured under 0.9V voltages of carbon-supported nano platinum alloy catalyst prepared by this comparative example is 0.30A/mgPt。
Comparative example 6
This comparative example is the comparative example of comparative example 1, and difference is, the Pt/C carbon-supported nano platinum catalysts of this comparative example Processing without step one to four, directly detects performance：The quality specific activity measured under 0.9V voltages is 0.13A/mgPt。
The specific embodiment of the present invention is described above.It is to be appreciated that the invention is not limited in above-mentioned Particular implementation, those skilled in the art can make various deformations or amendments within the scope of the claims, this not shadow Ring the substance of the present invention.

Claims (5)

1. a kind of preparation method of carbon-supported nano platinum alloy catalyst, it is characterised in that the preparation method comprises the following steps：
Step 1: Pt/C carbon-supported nano platinum catalysts are dispersed in 3d transition metal salt solutions, Pt/C suspension is prepared into；
Step 2: step one gained Pt/C suspension is dried under the conditions of≤80 DEG C, drying sample is obtained；
Step 3: drying sample obtained by step 2 is ground, reduction and alloying in reducing atmosphere are placed in；
Step 4: product obtained by step 3 is carried out into de- alloy treatment；The catalysis of carbon-supported nano platinum alloy is obtained after washing, drying Agent；
In step one, described 3d transition metal salt solutions include 3d transition metal salts, non-3d transition metal salts, solvent；It is described 3d transition metal salts include cobalt, nickel, the nitrate of iron, sulfate, chlorate, carbonate, acetate, formates or oxalates； The non-3d transition metal salts include ruthenium, the chloride of gold, bromide or chlorine complexing hydrochlorate；The solvent is the mixed of water and ethanol Bonding solvent；
In step one, the Pt/C carbon-supported nanos platinum catalyst is 1 with the mass ratio of solvent in 3d transition metal salt solutions：(5~ 20)；
In step one, the metallic atom of the 3d transition metal salts, non-3d transition metal salts in 3d transition metal salt solutions rubs Your concentration is respectively 0.20~1.0mol/L, 0.01~0.15mol/L；
In step 3, the temperature of the alloying is 800 DEG C；
In step 4, the method for the de- alloy treatment takes off alloy for acidleach；The acidleach takes off the nitric acid that alloy uses 1M, condition For 80 DEG C, 48h.
2. the preparation method of carbon-supported nano platinum alloy catalyst according to claim 1, it is characterised in that in step one, The scattered method is the one or more in mechanical agitation, shearing, ultrasound.
3. the preparation method of carbon-supported nano platinum alloy catalyst according to claim 1, it is characterised in that in step 2, The method of the drying includes freeze-drying, vacuum drying or is spray-dried.
4. the preparation method of carbon-supported nano platinum alloy catalyst according to claim 1, it is characterised in that in step 3, The reducing atmosphere is specially H2/N2Mixed gas or H2/ Ar mixed gas；Wherein, the volume fraction of hydrogen is less than 20%.
5. the preparation method of carbon-supported nano platinum alloy catalyst according to claim 1, it is characterised in that in step 4, The mode of washing includes filter membrane dialysis or filter type；Drying mode include vacuum drying, spray drying, freeze-drying or Common heating is dried.
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CN107088415B (en) * 2017-04-10 2020-05-08 南京大学 Preparation method of platinum alloy nano powder catalyst
CN106960962B (en) * 2017-04-26 2019-11-15 北京化工大学 A kind of platinum base of polyaniline-coated carbon carrier takes off alloy fuel cell catalyst and preparation method thereof
CN109390592B (en) * 2017-08-04 2021-12-31 上海汽车集团股份有限公司 Membrane electrode and preparation method thereof
CN108786791A (en) * 2018-06-10 2018-11-13 江苏经贸职业技术学院 A method of synthesis pt atom cluster is heat-treated based on complexing
CN111092235B (en) * 2019-12-27 2021-01-15 苏州擎动动力科技有限公司 Platinum-cobalt alloy catalyst and preparation method thereof
CN111725525B (en) * 2020-06-18 2022-03-15 上海交通大学 Carbon-supported monodisperse Pt-Ni nanoparticle catalyst prepared by electrodeposition and preparation and application thereof
CN114361478A (en) * 2021-12-17 2022-04-15 华南理工大学 Fuel cell carbon-supported platinum-based anti-reversal catalyst with small amount of highly-dispersed iridium surface modification, and preparation method and application thereof
CN114784305A (en) * 2022-02-16 2022-07-22 同济大学 Multi-component platinum alloy carbon-supported catalyst doped with non-metallic elements and preparation method thereof

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