CN108539219A - A kind of sulfur and nitrogen co-doped carbon nanotube carries PtCu alloy catalysts and the preparation method and application thereof - Google Patents

A kind of sulfur and nitrogen co-doped carbon nanotube carries PtCu alloy catalysts and the preparation method and application thereof Download PDF

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CN108539219A
CN108539219A CN201810427091.5A CN201810427091A CN108539219A CN 108539219 A CN108539219 A CN 108539219A CN 201810427091 A CN201810427091 A CN 201810427091A CN 108539219 A CN108539219 A CN 108539219A
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mwcnts
nitrogen
sulfur
ptcu
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CN108539219B (en
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樊友军
唐华果
项胜
孙悦
李佳
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Guangxi Normal 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
    • H01M4/90—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
    • H01M4/90—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
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M8/00—Fuel cells; Manufacture thereof
    • H01M8/10—Fuel cells with solid electrolytes
    • H01M8/1009—Fuel cells with solid electrolytes with one of the reactants being liquid, solid or liquid-charged
    • H01M8/1011—Direct alcohol fuel cells [DAFC], e.g. direct methanol fuel cells [DMFC]
    • 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 discloses a kind of sulfur and nitrogen co-doped carbon nanotubes to carry PtCu alloy catalysts and the preparation method and application thereof, and described method includes following steps：1）PEDOT/PANI copolymer functionalization MWCNTs are heat-treated to prepare sulfur and nitrogen co-doped MWCNTs composite materials；2）With step 1）The sulfur and nitrogen co-doped MWCNTs prepared is that carrier deposits PtCu alloy nanoparticles by solvent thermal reaction approach on its surface, obtains sulfur and nitrogen co-doped MWCNTs and carries PtCu alloy catalysts.This method and process is simple, operating condition is mildly controllable, and the excellent electrochemical performance of obtained material has a good application prospect.Sulfur and nitrogen co-doped MWCNTs prepared by this method, which carries PtCu alloy catalysts, can enhance the electro catalytic activity aoxidized to methanol and stability and the ability for showing excellent resisting CO poison.

Description

A kind of sulfur and nitrogen co-doped carbon nanotube carry PtCu alloy catalysts and preparation method thereof with Using
Technical field
The present invention relates to electro-catalysis and fuel cell field, specifically a kind of sulfur and nitrogen co-doped carbon nanotube carries PtCu alloys Catalyst and the preparation method and application thereof.
Background technology
Currently, carbon black carries Pt base elctro-catalysts（Such as：PtRu/C, Pt/C）Still it is widely used as direct methanol fuel cell （DMFC）Anode electrocatalysis material, however, there are of high cost, methanol oxidation dynamics is low for the precious metals pt in catalyst And the shortcomings of resisting CO poison energy force difference, these unfavorable factors greatly hinder the large-scale commercial application of DMFC.Therefore, How improving the utilization ratio of precious metals pt in catalyst, reduce the cost of catalyst and enhancing its electrocatalysis characteristic is always to be somebody's turn to do The hot issue of area research.
The electrocatalysis characteristic of Pt bases nano particle is strongly depend on the structure and superficiality of used carrier in carried catalyst Matter, for common carbon black support although showing lower resistance and higher specific surface area, existing pore size is small, electrochemical Learn the overall performance that the problems such as stability is poor significantly reduces catalyst.Carbon nanotube because of the high, electric conductivity with specific surface area and The physicochemical properties such as electrochemical stability is excellent, and get more and more people's extensive concerning.However, its surface of original carbon nanotube In chemical inertness, lacks abundant surface-active site and combined with catalyst precursor, be easy to cause catalyst nanoparticles ruler Very little big, the uneven and agglomeration of dispersion, this is obviously unfavorable for the electrochemistry for promoting carbon nanotube base fuel battery catalyst Can, therefore, it is still the direction that people constantly explore to carry out functionalization to carbon nano tube surface to improve its surface nature.
Studies have shown that in recent years mixes the hetero atoms such as B, N, P and S in carbon nano tube surface structure can significantly increase institute The dispersibility and electro catalytic activity of deposited catalyst nano-particle.In the doped carbon nanometer pipe material of document report, N doping, S mix Miscellaneous or S-N codope is relatively conventional, wherein contains and is assisted in two kinds of heteroatomic S-N codopes carbon nano tube surfaces due to existing Same effect, can further increase the performance of fuel-cell catalyst, and receive the concern of people.So far, related S-N is co-doped with The Research Literature report that miscellaneous carbon nanotube is used as fuel cell electrocatalysis material is few, relates generally to several following documents：(1) 2013《Journal of Materials Chemistry A》S and N codopes carbon nanotube is reported in acid and alkalinity To the research of oxygen reduction reaction performance in medium；(2) 2016 years《Journal of Materials Chemistry A》Report The carbon nanotube of N and S codope partial exfoliations is used for oxygen reduction reaction as three-dimensional structure elctro-catalyst；(3) 2016 years 《RSC Advances》The carbon nanotube for reporting the vertical arrangement of N and S codopes is used for hydrogen reduction electrocatalytic reaction；(4) 2017《Applied Surface Sience》Have studied electro-catalysis of the carbon nanotube to oxygen reduction reaction of N and S codopes Performance；(5) 2018 years《Journal of Colloid and Interface Sience》Report Jie loaded in carbon ball The carbon nanotube of growth in situ N and S codope is used for oxygen reduction reaction electro-catalysis on the cobalt sulfide of hole.Obviously, above-mentioned document report S-N codope carbon nano tube compound materials be both used as the elctro-catalyst of fuel battery negative pole oxygen reduction reaction, and their system It is standby to mostly use chemical vapor deposition greatly or contain heteroatomic small-molecule substance（Such as：Ammonia, urea, thiocarbamide）For the side such as presoma Method obtains, by poly- 3,4-rthylene dioxythiophene（PEDOT）/ polyaniline（PANI）Copolymer functionalized carbon nano-tube into Row is heat-treated to prepare S-N codopes carbon nano tube compound material and be applied to anode of fuel cell electro-catalyst carrier Research is there is not yet document and patent report.
Invention content
The purpose of the present invention is in view of the deficiencies of the prior art, and a kind of sulfur and nitrogen co-doped carbon nanotube is provided carries PtCu and close Au catalyst and the preparation method and application thereof.This method and process is simple, operating condition is mildly controllable, the electrification of obtained material Function admirable is learned, is had a good application prospect.Sulfur and nitrogen co-doped MWCNTs prepared by this method carries PtCu alloy as catalyst Agent can enhance the electro catalytic activity aoxidized to methanol and stability and the ability for showing excellent resisting CO poison.
Realizing the technical solution of the object of the invention is：
A kind of sulfur and nitrogen co-doped carbon nanotube carries the preparation method of PtCu alloy catalysts, unlike the prior art, including Following steps：
1）The multi-walled carbon nanotube of 20mg acidifications is added in equipped with the 20mL three times container of distilled water（MWCNTs）, 2.307g ten Sodium dialkyl sulfate（SDS）, 180 μ L 3,4- ethene dioxythiophenes（EDOT）With 80-200 μ L aniline（ANI）Monomer, under room temperature 20mL 0.02g mL are added dropwise in magnetic agitation after 2 hours−1(NH4)2S2O8Aqueous solution, then reaction 24 hours is continuously stirred, Products therefrom is after centrifugation, washing and vacuum drying, you can PEDOT/PANI copolymer functionalization MWCNTs composite materials are obtained, Then 20mg PEDOT/PANI copolymer functionalization MWCNTs samples are weighed, be placed in quartz tube furnace under protection of argon gas in 800oC is heat-treated 3 hours to get to sulfur and nitrogen co-doped MWCNTs composite materials（S,N-MWCNTs）；
2）According to certain mass ratio in 20mL ethylene glycol（Sulfur and nitrogen co-doped MWCNTs=1/4 PtCu/）It is total that 20mg sulphur nitrogen is added Adulterate the H of MWCNTs, anhydrous cupric sulfate and 19.3mM2PtCl6Solution, and control the H of addition2PtCl6Solution and anhydrous sulphur The atomic ratio of Pt and Cu is Pt in sour copper：Cu=1：0.2-5 is moved into 30mL reaction kettles after being ultrasonically treated 2 hours, in 90oC- It is reacted 24 hours under 200oC, reaction product obtains sulfur and nitrogen co-doped MWCNTs and carry PtCu after centrifugation, washing and vacuum drying Alloy catalyst（PtCu/S,N-MWCNTs）.
The sulfur and nitrogen co-doped MWCNTs made from above-mentioned preparation method carries PtCu alloy catalysts（PtCu/S,N- MWCNTs）.
The sulfur and nitrogen co-doped MWCNTs made from above-mentioned preparation method carries PtCu alloy catalysts（PtCu/S,N-MWCNTs） Application in direct methanol fuel cell.
The size of catalytic nanoparticle, dispersion degree and utilization ratio are carried with catalyst used in fuel cell electro-catalyst Body and its surface nature are closely related, sulfur and nitrogen co-doped to prepare by being heat-treated PEDOT/PANI copolymer functionalization MWCNTs Carbon nano tube compound material and using it as the carrier of catalytic nanoparticle, can be substantially reduced the ruler of PtCu alloy nanoparticles It is very little, its dispersion degree and utilization ratio are improved, while can also be each by sulfur and nitrogen co-doped MWCNTs carriers and PtCu nano particles Strong electron interaction changes the surface electron states of Pt between ingredient, to significantly enhance catalyst to methanol oxygen The electro catalytic activity of change, the ability of stability and resisting CO poison.
The technical program in-situ polymerization PEDOT/PANI functionalized copolymers first on the surfaces MWCNTs of acidification, obtain Then PEDOT/PANI copolymer functionalization MWCNTs composite materials use PEDOT/PANI copolymer functionalization MWCNTs samples, Sulfur and nitrogen co-doped MWCNTs composite materials are prepared, finally using sulfur and nitrogen co-doped MWCNTs composite materials obtained as carrier deposit PtCu alloy nanoparticles, and then obtain sulfur and nitrogen co-doped MWCNTs and carry PtCu alloy catalysts.
It is sulfur and nitrogen co-doped made from PEDOT/PANI copolymer functionalization MWCNTs to be heat-treated according to the technical program MWCNTs composite materials, which are carrier, can not only deposit acquisition dispersion degree and the good PtCu alloy nanoparticles of homogeneity, moreover it is possible to The electron interaction between each ingredient of catalytic nanoparticle and carrier is significantly improved, to change the surface of Pt in catalyst Electronic state.Prepared sulfur and nitrogen co-doped MWCNTs, which carries PtCu alloy catalysts, can be remarkably reinforced the electro-catalysis aoxidized to methanol Activity and stability, and show the ability of excellent resisting CO poison.
This method and process is simple, operating condition is mildly controllable, the excellent electrochemical performance of obtained material, has good Application prospect.Sulfur and nitrogen co-doped MWCNTs prepared by this method, which carries PtCu alloy catalysts, can enhance and aoxidized to methanol Electro catalytic activity and stability and the ability for showing excellent resisting CO poison.
Description of the drawings
Fig. 1 is the flow diagram for preparing sulfur and nitrogen co-doped carbon nanotube in embodiment and carrying PtCu alloy catalysts；
Fig. 2-(A) is the TEM figures that the sulfur and nitrogen co-doped MWCNTs prepared in embodiment carries PtCu alloy catalysts；
Fig. 2-(B) is that the sulfur and nitrogen co-doped MWCNTs prepared in embodiment carries the grain size statistical Butut of PtCu alloy catalysts；
Fig. 3 is the PtCu/S, N-MWCNTs, Pt/S prepared in embodiment, N-MWCNTs, Pt/N-MWCNTs, Pt/S-MWCNTs With business Pt/C catalyst in 0.5M CH3OH + 0.5M H2SO4Cyclic voltammetry curve schematic diagram in solution.
Specific implementation mode
The content of present invention is further elaborated with reference to the accompanying drawings and examples, but is not limitation of the invention.
Embodiment：
Referring to Fig.1, a kind of sulfur and nitrogen co-doped carbon nanotube carries the preparation method of PtCu alloy catalysts, includes the following steps：
1）The multi-walled carbon nanotube of 20mg acidifications is added in equipped with the 20mL three times container of distilled water（MWCNTs）, 2.307g ten Sodium dialkyl sulfate（SDS）, 180 μ L 3,4- ethene dioxythiophenes（EDOT）With 80-200 μ L aniline（ANI）Monomer, under room temperature 20mL 0.02g mL are added dropwise in magnetic agitation after 2 hours−1(NH4)2S2O8Aqueous solution, then reaction 24 hours is continuously stirred, Products therefrom is after centrifugation, washing and vacuum drying, you can PEDOT/PANI copolymer functionalization MWCNTs composite materials are obtained, Then 20mg PEDOT/PANI copolymer functionalization MWCNTs samples are weighed, be placed in quartz tube furnace under protection of argon gas in 800oC is heat-treated 3 hours to get to sulfur and nitrogen co-doped MWCNTs composite materials（S,N-MWCNTs）；
2）According to certain mass ratio in 20 mL ethylene glycol（Sulfur and nitrogen co-doped MWCNTs=1/4 PtCu/）20mg sulphur nitrogen is added The H of codope MWCNTs, anhydrous cupric sulfate and 19.3mM2PtCl6Solution, and control the H of addition2PtCl6Solution and anhydrous The atomic ratio of Pt and Cu is Pt in copper sulphate：Cu=1：0.2-5 is moved into 30mL reaction kettles after being ultrasonically treated 2 hours, in 90oC- It is reacted 24 hours under 200oC, reaction product obtains sulfur and nitrogen co-doped MWCNTs and carry PtCu after centrifugation, washing and vacuum drying Alloy catalyst（PtCu/S,N-MWCNTs）.
The sulfur and nitrogen co-doped MWCNTs made from above-mentioned preparation method carries PtCu alloy catalysts（PtCu/S,N- MWCNTs）.
The sulfur and nitrogen co-doped MWCNTs made from above-mentioned preparation method carries PtCu alloy catalysts（PtCu/S,N-MWCNTs） Application in direct methanol fuel cell.
As shown in Fig. 2-(A), Fig. 2-(B), tem analysis shows that PtCu nano particles are in sulphur in this example prepared catalyst It is uniformly dispersed on nitrogen co-doped MWCNTs, average grain diameter 2.87nm, hence it is evident that other PtCu less than current document report are urged Agent.
Compare prepared PtCu/S by cyclic voltammetry and chronoamperometry, it is N-MWCNTs, sulfur and nitrogen co-doped MWCNTs carries Pt（It is denoted as Pt/S, N-MWCNTs）, N doping MWCNTs carry Pt（It is denoted as Pt/N-MWCNTs）, sulfur doping MWCNTs Carry Pt（It is denoted as Pt/S-MWCNTs）The electrocatalysis characteristic that methanol is aoxidized with business Pt/C catalyst, the results showed that, this example is made The electro catalytic activity that standby PtCu/S, N-MWCNTs catalyst aoxidize methanol is respectively Pt/S, N-MWCNTs, Pt/N- 1.5,2,2.1 and 4.2 times of MWCNTs, Pt/S-MWCNTs and business Pt/C catalyst, in addition, PtCu/S, N-MWCNTs are catalyzed Agent also shows excellent methanol oxidizing and electrochemical stability, as shown in figure 3, different catalysts are set forth in 0.5M CH3OH + 0.5M H2SO4Cyclic voltammetry curve in solution.
Prepared PtCu/S, N-MWCNTs, Pt/S, N-MWCNTs, Pt/ are compared by electrochemistry CO stripping voltammetries The performance of the resisting CO poison of N-MWCNTs, Pt/S-MWCNTs and business Pt/C catalyst.As a result it points out, CO is in PtCu/S, N- Initial oxidation current potential on MWCNTs catalyst（0.42V）Respectively than Pt/S, N-MWCNTs（0.44V）、Pt/N-MWCNTs （0.47V）, Pt/S-MWCNTs（0.5V）With business Pt/C（0.52V）Catalyst is negative to have moved 20,50,80 and 100mV, this shows Sulfur and nitrogen co-doped MWCNTs prepared by this example carries the ability that PtCu alloy catalysts have excellent resisting CO poison.

Claims (3)

1. a kind of sulfur and nitrogen co-doped carbon nanotube carries the preparation method of PtCu alloy catalysts, characterized in that include the following steps：
1）The multi-walled carbon nanotube of 20mg acidifications is added in equipped with the 20mL three times container of distilled water（MWCNTs）, 2.307g ten Sodium dialkyl sulfate（SDS）, 180 μ L 3,4- ethene dioxythiophenes（EDOT）With 80-200 μ L aniline（ANI）Monomer, under room temperature 20mL 0.02g mL are added dropwise in magnetic agitation after 2 hours−1(NH4)2S2O8Aqueous solution, then reaction 24 hours is continuously stirred, Products therefrom is after centrifugation, washing and vacuum drying, you can PEDOT/PANI copolymer functionalization MWCNTs composite materials are obtained, Then 20mg PEDOT/PANI copolymer functionalization MWCNTs samples are weighed, be placed in quartz tube furnace under protection of argon gas in 800oC is heat-treated 3 hours to get to sulfur and nitrogen co-doped MWCNTs composite materials（S,N-MWCNTs）；
2）According to certain mass ratio in 20mL ethylene glycol（Sulfur and nitrogen co-doped MWCNTs=1/4 PtCu/）It is total that 20mg sulphur nitrogen is added Adulterate the H of MWCNTs, anhydrous cupric sulfate and 19.3mM2PtCl6Solution, and control the H of addition2PtCl6Solution and anhydrous sulphur The atomic ratio of Pt and Cu is Pt in sour copper：Cu=1：0.2-5 is moved into 30mL reaction kettles after being ultrasonically treated 2 hours, in 90oC- It is reacted 24 hours under 200oC, reaction product obtains sulfur and nitrogen co-doped MWCNTs and carry PtCu after centrifugation, washing and vacuum drying Alloy catalyst（PtCu/S,N-MWCNTs）.
2. sulfur and nitrogen co-doped MWCNTs made from the preparation method described in claim 1 carries PtCu alloy catalysts（PtCu/S,N- MWCNTs）.
3. sulfur and nitrogen co-doped MWCNTs described in claim 2 carries PtCu alloy catalysts（PtCu/S,N-MWCNTs）In direct first Application in alcohol fuel battery.
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CN117219794A (en) * 2023-09-15 2023-12-12 佛山职业技术学院 Nitrogen-sulfur co-doped porous carbon nanofiber-loaded PtCu alloy particle, and preparation method and application thereof
CN117219794B (en) * 2023-09-15 2024-03-19 佛山职业技术学院 Nitrogen-sulfur co-doped porous carbon nanofiber-loaded PtCu alloy particle, and preparation method and application thereof

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