CN108933264A - A kind of conductive black carried noble metal composite material and preparation method and application - Google Patents

A kind of conductive black carried noble metal composite material and preparation method and application Download PDF

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Publication number
CN108933264A
CN108933264A CN201810811451.1A CN201810811451A CN108933264A CN 108933264 A CN108933264 A CN 108933264A CN 201810811451 A CN201810811451 A CN 201810811451A CN 108933264 A CN108933264 A CN 108933264A
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noble metal
conductive black
preparation
composite material
nano particles
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梁长浩
吴守良
刘俊
叶星
叶一星
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Hefei Technology Innovation Engineering Institute of CAS
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Hefei Technology Innovation Engineering Institute of CAS
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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
    • H01M4/8825—Methods for deposition of the catalytic active composition
    • 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
    • H01M4/9041—Metals or alloys
    • 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
    • H01M4/9075—Catalytic material supported on carriers, e.g. powder carriers
    • H01M4/9083—Catalytic material supported on carriers, e.g. powder carriers on carbon or graphite
    • 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
    • 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

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Materials Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Catalysts (AREA)
  • Inert Electrodes (AREA)

Abstract

The present invention provides a kind of preparation methods of conductive black carried noble metal composite material, comprising the following steps: the noble metal target material being immersed in dehydrated alcohol is carried out laser ablation, obtains noble metal nano particles colloidal solution；It is stirred after the noble metal nano particles colloidal solution and conductive black dispersion liquid are mixed, obtains conductive black carried noble metal composite material.Preparation method of the present invention is simple, quick, efficient.Furthermore, the present invention is without using reducing agent and surfactant, the shortcomings that generating by-product contamination when avoiding traditional reducing agent reduction precious metal ion salt specifically avoids the defect that noble metal nano particles surface causes catalytic activity to reduce because of adsorption activity agent molecule.Record according to the embodiment, the quality specific activity for the conductive black carried noble metal composite material that the present invention is prepared are apparently higher than the quality specific activity of commercial conductive black carried noble metal composite material.

Description

A kind of conductive black carried noble metal composite material and preparation method and application
Technical field
The present invention relates to catalyst technical field more particularly to a kind of conductive black carried noble metal composite material and its systems Preparation Method and application.
Background technique
It is the basis of the fields such as the energy, environment, fine chemistry industry development using catalyst material as the catalysis technique of core.As A kind of very important catalyst material, loaded noble metal catalyst have wide practical use in fields such as fuel cells. In numerous catalyst carriers, conductive carbon black rich reserves, large specific surface area and stability are high, along with its excellent conduction Property, the favor by numerous researchers.
Currently, there are many report in conductive carbon black area load noble metal nano particles, be mostly using reducing agent (such as: Sodium borohydride, hydrazine hydrate etc.) reduction precious metal ion salt, to obtain noble metal nano particles, but the use of these reducing agents By-product contamination will inevitably be generated.Simultaneously.In order to make noble metal nano particles in catalyst have high degree of dispersion and Ultra-fine partial size is frequently added surfactant (such as: PVP, CTAB) during the preparation process, these active agent molecules are easily inhaled It is attached to the surface of catalyst, occupies the active site of catalyst, reduces its catalytic performance.
Summary of the invention
The purpose of the present invention is to provide a kind of catalytic activity high conductive black carried noble metal composite materials of preparing The application of method and its conductive black carried noble metal composite material in a fuel cell.
In order to achieve the above-mentioned object of the invention, the present invention the following technical schemes are provided:
The present invention provides a kind of preparation methods of conductive black carried noble metal composite material, comprising the following steps:
The noble metal target material being immersed in dehydrated alcohol is subjected to laser ablation, it is molten to obtain noble metal nano particles colloid Liquid；
It is stirred after the noble metal nano particles colloidal solution and conductive black dispersion liquid are mixed, it is negative to obtain conductive black Supported noble metal composite material.
Preferably, the noble metal of the noble metal target material is Pt, Pd, Ag or Au.
Preferably, the dosage of the dehydrated alcohol be dehydrated alcohol liquid level be higher than noble metal target material surface 0.8~ 1.2cm。
Preferably, the optical maser wavelength of the laser ablation is 355nm, 532nm or 1064nm, pulsewidth 7ns, frequency 2 ~20Hz, energy density are 30~300mJ/cm2, the time of laser ablation noble metal target material is 1~30min.
Preferably, the concentration of the conductive black dispersion liquid is 0.5~1.5mg/mL, the noble metal nano particles colloid The concentration of solution is 5 × 10-5~1.5 × 10-3mg/mL。
Preferably, the volume ratio of the noble metal nano particles colloidal solution and conductive black dispersion liquid be (100~ 300):1。
Preferably, the revolving speed of the stirring is 400~600r/min, and the time of the stirring is 8~12min.
The present invention also provides the conductive black carried noble metal composite materials that the preparation method is prepared, including Conductive black and the noble metal nano particles for being supported on the conductive black surface.
Preferably, the partial size of the noble metal nano particles is 1~10nm；The load capacity of the noble metal nano particles is 1wt%~30wt%.
The present invention also provides conductive black carried noble metal composite material the answering as fuel-cell catalyst With.
The present invention provides a kind of preparation methods of conductive black carried noble metal composite material, comprising the following steps: will The noble metal target material being immersed in dehydrated alcohol carries out laser ablation, obtains noble metal nano particles colloidal solution；It will be described expensive It is stirred after metal nanoparticle colloid solution and the mixing of conductive black dispersion liquid, obtains conductive black carried noble metal composite wood Material.The invention firstly uses liquid laser corrode technology corrode noble metal target materials in dehydrated alcohol, obtain surface " cleaning ", ruler Very little uniform and high degree of dispersion noble metal nano particles, are then added conductive black dispersion liquid, can be obtained and lead after being sufficiently stirred Electric carbon black loadings noble metal nano composite material.Preparation method of the present invention is simple, quick, efficient.In addition, the present invention without using Reducing agent and surfactant, when avoiding traditional reducing agent reduction precious metal ion salt the shortcomings that generation by-product contamination, especially The defect which obviate noble metal nano particles surfaces to cause catalytic activity to reduce because of adsorption activity agent molecule.According to embodiment Record, the quality specific activity for the conductive black carried noble metal composite material that the present invention is prepared is apparently higher than commercial lead The quality specific activity of electric carbon black loadings noble metal composite-material.
Detailed description of the invention
Fig. 1 is the TEM figure for the conductive black supporting Pt nano particle that embodiment 1 is prepared；
Fig. 2 is the TEM figure for the conductive black supporting Pt nano particle that embodiment 2 is prepared；
Fig. 3 is the TEM figure for the conductive black supporting Pt nano particle that embodiment 3 is prepared；
Fig. 4 is the conductive black supporting Pt nano particle and commercialization Pt/C (20wt%) catalyst that embodiment 2 is prepared In the 0.5M H of nitrogen saturation2SO4Cyclic voltammetry curve figure in solution；
Fig. 5 is the conductive black supporting Pt nano particle and commercialization Pt/C (20wt%) catalyst that embodiment 2 is prepared In 0.5M H2SO4+0.5M CH3Cyclic voltammetry curve figure in OH solution；
Fig. 6 is the TEM figure that the conductive black that embodiment 4 is prepared loads Pd nano particle.
Specific embodiment
The present invention provides a kind of preparation methods of conductive black carried noble metal composite material, comprising the following steps:
The noble metal target material being immersed in dehydrated alcohol is subjected to laser ablation, it is molten to obtain noble metal nano particles colloid Liquid；
It is stirred after the noble metal nano particles colloidal solution and conductive black dispersion liquid are mixed, it is negative to obtain conductive black Supported noble metal composite material.
In the present invention, if without specified otherwise, all raw material components are commercial product well known to those skilled in the art.
The noble metal target material being immersed in dehydrated alcohol is carried out laser ablation by the present invention, obtains noble metal nano particles glue Liquid solution.In the present invention, the composition of noble metal is preferably Pt, Pd, Ag or Au in the noble metal target material.
In the present invention, the purity of the noble metal target material is preferably > 99.99%；The present invention is preferably to the noble metal Target uses after being polished；The present invention is to the no any special restriction of polishing, using known to those skilled in the art Bruting process polished and achieve the purpose that make the surface of noble metal target material smooth.
In the present invention, the dosage of the dehydrated alcohol is preferably that the liquid level of dehydrated alcohol is higher than noble metal target material surface At 0.8~1.2cm, more preferably 0.9~1.1cm.
In the present invention, the height can guarantee to have when noble metal target material in laser ablation dehydrated alcohol highest molten Lose efficiency.
In the present invention, the optical maser wavelength of the laser ablation is 355nm, 532nm or 1064nm；The laser ablation Pulsewidth is preferably 7ns,；The frequency of the laser ablation is preferably 2~20Hz, more preferably 5~15Hz, most preferably 8~ 12Hz；The energy density of the laser ablation is preferably 30~300mJ/cm2, more preferably 50~250mJ/cm2, most preferably 80~150mJ/cm2；The time of the laser ablation is preferably 1~30min, more preferably 3~20min, most preferably 5~ 15min。
In the present invention, the mass concentration of noble metal is preferably 5 × 10 in the noble metal nano particles colloidal solution-5~ 1.5×10-3Mg/mL, more preferably 3 × 10-4~10-3Mg/mL, most preferably 5 × 10-4~8 × 10-4mg/mL。
After obtaining noble metal nano particles colloidal solution, the present invention is by the noble metal nano particles colloidal solution and conduction It is stirred after carbon black dispersion liquid mixing, obtains conductive black carried noble metal composite material.In the present invention, the conductive black point The solvent of dispersion liquid is preferably dehydrated alcohol；In the present invention, the concentration of the conductive black dispersion liquid is preferably 0.5~1.5mg/ ML, more preferably 0.8~1.2mg/mL.In the present invention, the noble metal nano particles colloidal solution and conductive black disperse The volume ratio of liquid is preferably (100~300): 1, more preferably (150~250): 1, most preferably (180~220): 1.
Order by merging and blended sliver of the present invention to the noble metal nano particles colloidal solution and conductive black dispersion liquid Part does not have any special restriction, is mixed using mixed process well known to those skilled in the art.
In the present invention, the revolving speed of the stirring is preferably 400~600r/min, more preferably 450~550r/min；Institute The time for stating stirring is preferably 8~12min, more preferably 9~11min.
In the present invention, the stirring can make noble metal nano particles in conductive black surface uniform adsorption, and then make Noble metal nano particles are uniformly supported on conductive black surface.
The present invention also provides the conductive black carried noble metal composite materials that the preparation method is prepared, including lead Electric carbon black and the noble metal nano particles for being supported on the conductive black surface.
In the present invention, the partial size of noble metal nano particles is preferably in the conductive black carried noble metal composite material 1~10nm, more preferably 2~4nm；The load capacity of the noble metal nano particles is preferably 1wt%~30wt%, more preferably 5wt%~25wt%, most preferably 10wt%~20wt%.
Application the present invention also provides the conductive black carried noble metal composite material as fuel-cell catalyst.
Below with reference to embodiment to conductive black carried noble metal composite material and preparation method provided by the invention into Row detailed description, but they cannot be interpreted as limiting the scope of the present invention.
Embodiment 1
The Pt target (purity > 99.99%) that surface polishes smooth is placed in polytetrafluoroethylene (PTFE) pot bottom, it is anhydrous that 20mL is added Ethyl alcohol to liquid level exceeds target material surface 1cm；
Using convex lens by pulse laser focusing to Pt target material surface, optical maser wavelength be 355nm, pulsewidth 7ns, frequency For 10Hz, energy density 100mJ/cm2Under conditions of, it carries out laser ablation and handles 5min, it is molten to obtain Pt nano-particle colloid Liquid；
By the dehydrated alcohol dispersion for the conductive black that the Pt nanoparticle colloid solution and 100 microlitres of concentration are 1mg/mL Liquid mixing, obtains conductive black supporting Pt nano particle after stirring 10min with the revolving speed of 500r/min.
Fig. 1 is that the TEM of the conductive black supporting Pt nano particle schemes, and as seen from the figure, the conductive black supporting Pt is received The average grain diameter of Pt nano particle is 2nm in rice grain.The load capacity of Pt is 5wt% in the embodiment.
Embodiment 2
The Pt target (purity > 99.99%) that surface polishes smooth is placed in polytetrafluoroethylene (PTFE) pot bottom, it is anhydrous that 20mL is added Ethyl alcohol to liquid level exceeds target material surface 1cm；
Using convex lens by pulse laser focusing to Pt target material surface, optical maser wavelength be 355nm, pulsewidth 7ns, frequency For 20Hz, energy density 100mJ/cm2Under conditions of, it carries out laser ablation and handles 10min, it is molten to obtain Pt nano-particle colloid Liquid；
By the dehydrated alcohol dispersion for the conductive black that the Pt nanoparticle colloid solution and 100 microlitres of concentration are 1mg/mL Liquid mixing, obtains conductive black supporting Pt nano particle after stirring 10min with the revolving speed of 500r/min.
Fig. 2 is that the TEM of the conductive black supporting Pt nano particle schemes, and as seen from the figure, the conductive black supporting Pt is received The average grain diameter of Pt nano particle is 2nm in rice grain.The load capacity of Pt is 20wt% in the embodiment.
Fig. 4 is conductive black supporting Pt nano particle of the present invention and commercialization Pt/C (20wt%) catalyst in nitrogen The 0.5M H of saturation2SO4Cyclic voltammetry curve figure in solution；As seen from the figure, in -0.2 to 0.12V potential range, two kinds Catalyst shows apparent hydrogen suction-desorption peaks.By the absorption electricity for integrate to hydrogen desorption peak area available hydrogen Measure QH, utilize ECSA=QH/ (0.21 × [Pt]) is estimated that the electrochemical surface area of catalyst.The results show that of the invention The electrochemical surface area of the conductive black supporting Pt nano particle is 820.4cm2/mgpt, it is higher than commercialization Pt/C The 706.4cm of (20wt%) catalyst2/mgpt。
Fig. 5 is conductive black supporting Pt nano particle of the present invention and commercialization Pt/C (20wt%) in 0.5M H2SO4+ 0.5M CH3Cyclic voltammetry curve figure in OH solution；As seen from the figure, conductive black supporting Pt nano particle of the present invention Higher electro catalytic activity is shown to methanol oxidation, quality specific activity is 785.3mA/mgpt, hence it is evident that it is higher than commercialization Pt/C The 513mA/mg of (20wt%) catalystpt。
Embodiment 3
The Pt target (purity > 99.99%) that surface polishes smooth is placed in polytetrafluoroethylene (PTFE) pot bottom, it is anhydrous that 20mL is added Ethyl alcohol to liquid level exceeds target material surface 1cm；
Using convex lens by pulse laser focusing to Pt target material surface, optical maser wavelength be 532nm, pulsewidth 7ns, frequency For 10Hz, energy density 130mJ/cm2Under conditions of, it carries out laser ablation and handles 10min, it is molten to obtain Pt nano-particle colloid Liquid；
By the dehydrated alcohol dispersion for the conductive black that the Pt nanoparticle colloid solution and 100 microlitres of concentration are 1mg/mL Liquid mixing, obtains conductive black supporting Pt nano particle after stirring 10min with the revolving speed of 500r/min.
Fig. 3 is that the TEM of the conductive black supporting Pt nano particle schemes, and as seen from the figure, the conductive black supporting Pt is received The average grain diameter of Pt nano particle is 3.5nm in rice grain.The load capacity of Pt is 18wt% in the embodiment.
Embodiment 4
The Pd target (purity > 99.99%) that surface polishes smooth is placed in polytetrafluoroethylene (PTFE) pot bottom, it is anhydrous that 20mL is added Ethyl alcohol to liquid level exceeds target material surface 1cm；
Using convex lens by pulse laser focusing to Pd target material surface, optical maser wavelength be 355nm, pulsewidth 7ns, frequency For 10Hz, energy density 100mJ/cm2Under conditions of, it carries out laser ablation and handles 2min, it is molten to obtain Pd nano-particle colloid Liquid；
By the dehydrated alcohol dispersion for the conductive black that the Pd nanoparticle colloid solution and 100 microlitres of concentration are 1mg/mL Liquid mixing obtains conductive black load Pd nano particle after stirring 10min with the revolving speed of 500r/min.
Fig. 6 is the TEM figure that the conductive black loads Pd nano particle, and as seen from the figure, the conductive black load Pd receives The average grain diameter of Pd nano particle is 1.6nm in rice grain.The load capacity of Pd is 3wt% in the embodiment.
As seen from the above embodiment, the catalytic performance for the conductive black carried noble metal composite material that the present invention is prepared Higher than commercial conductive black carried noble metal composite material.
The above is only a preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art For member, various improvements and modifications may be made without departing from the principle of the present invention, these improvements and modifications are also answered It is considered as protection scope of the present invention.

Claims (10)

1. a kind of preparation method of conductive black carried noble metal composite material, comprising the following steps:
The noble metal target material being immersed in dehydrated alcohol is subjected to laser ablation, obtains noble metal nano particles colloidal solution；
It is stirred after the noble metal nano particles colloidal solution and conductive black dispersion liquid are mixed, it is expensive to obtain conductive black load Metallic composite.
2. preparation method as described in claim 1, which is characterized in that the noble metal of the noble metal target material be Pt, Pd, Ag or Au。
3. preparation method as described in claim 1, which is characterized in that the dosage of the dehydrated alcohol is the liquid level of dehydrated alcohol Higher than 0.8~1.2cm of noble metal target material surface.
4. preparation method as claimed in claim 1 or 2, which is characterized in that the optical maser wavelength of the laser ablation be 355nm, 532nm or 1064nm, pulsewidth 7ns, frequency are 2~20Hz, and energy density is 30~300mJ/cm2, laser ablation noble metal The time of target is 1~30min.
5. preparation method as described in claim 1, which is characterized in that the concentration of the conductive black dispersion liquid be 0.5~ 1.5mg/mL, the concentration of the noble metal nano particles colloidal solution are 5 × 10-5~1.5 × 10-3mg/mL。
6. preparation method as claimed in claim 5, which is characterized in that the noble metal nano particles colloidal solution and conductive charcoal The volume ratio of black dispersion liquid is (100~300): 1.
7. preparation method as described in claim 1, which is characterized in that the revolving speed of the stirring is 400~600r/min, described The time of stirring is 8~12min.
8. the conductive black carried noble metal composite material that the described in any item preparation methods of claim 1~7 are prepared, packet Include conductive black and the noble metal nano particles for being supported on the conductive black surface.
9. conductive black carried noble metal composite material as claimed in claim 8, which is characterized in that the noble metal nano The partial size of grain is 1~10nm；The load capacity of the noble metal nano particles is 1wt%~30wt%.
10. application of the conductive black carried noble metal composite material as fuel-cell catalyst described in claim 8 or 9.
CN201810811451.1A 2018-07-23 2018-07-23 A kind of conductive black carried noble metal composite material and preparation method and application Pending CN108933264A (en)

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CN110649294A (en) * 2019-09-25 2020-01-03 新源动力股份有限公司 Method for characterizing surface polymer electrolyte coverage of Pt/C catalyst for fuel cell
CN114734051A (en) * 2022-04-21 2022-07-12 中国科学院合肥物质科学研究院 Method for in-situ preparation of ultra-small precious metal and non-precious metal alloy on carbon carrier
CN114828397A (en) * 2022-04-21 2022-07-29 华南理工大学 Preparation method and application of conductive metal carbon paste

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CN110649294A (en) * 2019-09-25 2020-01-03 新源动力股份有限公司 Method for characterizing surface polymer electrolyte coverage of Pt/C catalyst for fuel cell
CN114734051A (en) * 2022-04-21 2022-07-12 中国科学院合肥物质科学研究院 Method for in-situ preparation of ultra-small precious metal and non-precious metal alloy on carbon carrier
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Application publication date: 20181204