CN103949251A - Oxygen reduction catalyst as well as preparation method and application of oxygen reduction catalyst - Google Patents

Oxygen reduction catalyst as well as preparation method and application of oxygen reduction catalyst Download PDF

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CN103949251A
CN103949251A CN201410196011.1A CN201410196011A CN103949251A CN 103949251 A CN103949251 A CN 103949251A CN 201410196011 A CN201410196011 A CN 201410196011A CN 103949251 A CN103949251 A CN 103949251A
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catalyst
mwcnts
ceo
solution
oxygen reduction
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于书平
刘润婷
朱红
韩克飞
汪中明
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Beijing University of Chemical Technology
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Beijing University of Chemical Technology
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    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/30—Hydrogen technology
    • Y02E60/50—Fuel cells

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Abstract

The invention provides an oxygen reduction catalyst. The catalyst is represented as Ag@Pt/MWCNTs-CeO2; a carbon nano tube (MWCNTs) as a carrier; CeO2 doped nuclear shell Ag@Pt acts as an active component; the catalyst is characterized in that CeO2 is uniformly doped into Ag@Pt/MWCNTs; the catalyst serves as a cathode catalyst of a proton exchange membrane fuel cell, and the catalytic activity of the catalyst is improved by 50-70% compared with the Ag@Pt/MWCNTs; the electrochemical active area reaches 67.1-100.0m<2>g<-1>; the current density of catalytic oxygen reduction can reach 4.5-7.0mA.cm<-2>. The preparation method provided by the invention is simple, convenient and feasible, and is easy for industrial application. The prepared Ag@Pt/MWCNTs-CeO2 compound catalyst reduces the load quantity of platinum, so that the cost of the catalyst is reduced greatly.

Description

A kind of oxygen reduction catalyst and its preparation method and application
Technical field
The present invention relates to oxygen reduction catalyst and preparation thereof, be specifically related to a kind of Ag@Pt/MWCNTs-CeO 2catalysts and its preparation method, and this catalyst is used for to fuel battery cathode with proton exchange film catalyst.
Background technology
The advantages such as it is long that Proton Exchange Membrane Fuel Cells (PEMFC) has the life-span, and energy density is high, can at room temperature start, and water is easily got rid of, environmental protection, are having broad application prospects aspect electric automobile, portable power source.At present, platinum base eelctro-catalyst is considered to fuel cell optimum catalyst because having compared with high catalytic performance, yet the cost that platinum base eelctro-catalyst is higher has limited the application of PEMFC.Therefore, researching and developing low year platinum, high performance catalyst is the key technology that promotes Proton Exchange Membrane Fuel Cells development.Recent studies have found that, in Pt based alloy catalyst, mix other metallic elements as: during the metals such as Ni, Cr, Pd, Ag, Cu, Au, this type of double base or multicomponent catalyst not only can reduce the consumption of Pt metal in catalyst, reduce costs, also can be because synergy between other metallic elements and Pt changes Pt surface for the adsorption capacity of oxygen and hydrogen reduction process intermediate state, thus hydrogen reduction efficiency improved.So the emerging catalyst such as Pt alloy, hud typed catalyst have caused people's extensive concern.Also have scholar's research to find, by the doping of metal oxide and platinum group catalyst, not only can reduce the carrying capacity of platinum in catalyst, but also can play the effect that improves catalyst stability and catalytic activity.Due to CeO 2price is lower and have lattice defect, has oxygen room in structure, thereby has higher oxygen storage capacity, therefore in recent years a lot of scholars to Pt and CeO 2the performance study of composite catalyst made much work.
Document: Jerzy Chlistunoff et al., Electrochemical Studies of Novel Pt/Ceria/C Oxygen Reduction Catalysts for Fuel Cells.ECS Transactions, in 2011.1 (41) 2341-2348., the people such as Chlistunoff have prepared a kind of Pt-CeO 2/ C catalyst, finds by research, due to CeO 2good storage oxygen performance, can improve local oxygen partial pressure under the oxidation voltage of Pt, improves its catalytic oxidation-reduction active.
Document: Lim D-H et al., Effect of ceria nanoparticles into the Pt/C catalyst as cathode material on the electrocatalytic activity and durability for low-temperature fuel cell.Applied Catalysis B:Environmental, 20101 (94), in 85-96., the people such as Lim study and find CeO 2itself there is the effect of storage oxygen, and be distributed near CeO Pt 2just in time can in hydrogen reduction process, play the effect of oxygen buffering area, the deficiency of oxygen in make-up catalyst hydrogen reduction process, thus improved the catalytic performance of catalyst, rather than new avtive spot is provided
Summary of the invention
The object of the present invention is to provide oxygen reduction catalyst of a kind of low platinum carrying capacity and high catalytic activity and preparation method thereof, and this catalyst is used as to fuel battery cathode with proton exchange film catalyst.
Oxygen reduction catalyst provided by the invention, is expressed as: Ag@Pt/MWCNTs-CeO 2, be that to take CNT (MWCNTs) be carrier, CeO 2the catalyst that the hud typed Ag@Pt of doping is active component, this catalyst is CeO 2uniform Doped is in Ag@Pt/MWCNTs; By this catalyst, as fuel battery cathode with proton exchange film catalyst, its catalytic activity improves 50-70% than the catalytic activity of Ag@Pt/MWCNTs, and its electrochemical surface area reaches 67.1-100.0m 2g -1, the current density of catalytic oxidation-reduction can reach 4.5-7.0mAcm -2.
The concrete preparation process of this oxygen reduction catalyst is as follows:
A is dispersed in silver nitrate, natrium citricum and multi-walled carbon nano-tubes in deionized water, to prepare suspension A, making the wherein molar concentration of silver nitrate is 1-6mmol/L, the molar concentration of natrium citricum is 20-50mmol/L, the mass concentration of multi-walled carbon nano-tubes is 1-3g/L, sodium borohydride/ethanolic solution that dropping and suspension A volume ratio are 1:30-60 wherein again, filter, dry, obtain Ag/MWCNTs; In sodium borohydride/ethanolic solution, the content of sodium borohydride is 100-300mmol/L;
The Ag/MWCNTs making is dispersed in and in ethylene glycol solution, prepares suspension B by 1-3g/L, ultrasonic dispersion 1-4h, add the platinum acid chloride solution that accounts for suspension B volume parts 0.5-1%, with the KOH/ ethylene glycol solution of 2-10%, regulate pH=5-10 again, be warming up to 60-120 ℃ of reaction 3-6h, filter, dry, obtain Ag@Pt/MWCNTs;
B. the cerous nitrate solution that is 0.1-1.0mmol/L by concentration 0.1mol L -1ammoniacal liquor or 0.1mol L -1sodium hydroxide solution regulates pH=7-11, adds in high-temperature high-pressure reaction kettle, and first at 60-90 ℃, reaction 2-6h, then at 110-160 ℃ of reaction 3-6h, after filtration, washing, the dry CeO that obtains 2;
C. the CeO that Ag@Pt/MWCNTs steps A being made and step B obtain 2mass ratio with 4-8:1 joins in ethanolic solution, and ultrasonic dispersion 1-4h filters, and in the vacuum drying chamber of 50-80 ℃, dry 5-15h, obtains Ag@Pt/MWCNTs-CeO 2composite catalyst.
Fig. 1 is the CeO of embodiment 1 preparation 2with Ag@Pt/MWCNTs-CeO 2xRD spectra.At a, in two curves of b, during 2 θ=26 ℃, corresponding first strong peak is the characteristic diffraction peak of carrier multi-walled carbon nano-tubes.Curve b and standard card (PDF card04-0802) are contrasted, in 2 θ=39.8 °, 46.2 °, 67.4 ° and 81.3 ° corresponding be the characteristic diffraction peak of face-centred cubic structure Pt, corresponding crystal face is respectively (111), (200), (220), (311).Curve b is Ag@Pt/MWCNTs-CeO 2the XRD spectra of catalyst, the characteristic diffraction peak of curve b metal A g does not occur, illustrates that metal A g has become kernel, has been wrapped in its inside by Pt metal shell.As can be seen from the figure, in composite construction, to go out peak obvious for each characteristic peak, well-formed.
Fig. 2 (a) is the Electronic Speculum picture of the Ag@Pt/MWCNTs catalyst of embodiment 2 preparations.As can be seen from the figure, the even surface that must be distributed in MWCNTs of Ag Pt nano particle.Fig. 2 (b) is the Ag@Pt/MWCNT-CeO of embodiment 2 preparations 2composite construction catalyst.CeO in figure 2for the blocky-shaped particle of diameter 600nm, and be inserted into and between Ag@Pt/MWCNT, formed a uniform composite construction.
By cyclic voltammetry curve method and a linear volt-ampere scanning method, fuel-cell catalyst is carried out to the sign of chemical property, the results are shown in Figure 3 and 4, from Fig. 3,4: Ag@Pt/MWCNTs-CeO 2catalytic activity to be significantly higher than Ag@Pt/MWCNTs, its electrochemical surface area can reach 97.2m 2g -1, and the CeO that adulterated 2catalyst there is obvious high limit electric current, illustrate under the existence of cerium oxide, increased the concentration of partial oxygen.In hydrogen reduction process, cerium oxide has maintained higher reaction rate as the source of supply of O.
Beneficial effect: the Ag@Pt/MWCNTs-CeO that the present invention is prepared 2composite catalyst has not only reduced the load capacity of platinum, has reduced catalyst cost, meanwhile, and the CeO of doping 2under oxidation or reducing condition, CeO 2/ Ce 2o 3between the circulation of redox reaction occur, be easy to picked-up and discharge O, and can produce unsettled oxygen room in this process, body phase oxygen species have relatively high mobility, and the circulation in oxygen room produces and bury in oblivion and impel oxonium ion to flow, can promote the absorption of oxygen in oxygen reduction reaction process and dissociate, promoting the generation of oxygen reduction reaction, thereby improving the catalytic activity of catalyst.Its electrochemical surface area can reach 97.2m 2g -1, the current density of catalytic oxidation-reduction can reach 4.8mAcm -2.The preparation method who adopts is simple and easy to do, is easy to commercial Application.
Accompanying drawing explanation
Fig. 1 is the CeO of embodiment 1 preparation 2with Ag@Pt/MWCNTs-CeO 2xRD spectra.Wherein a is CeO 2xRD curve, b is Ag@Pt/MWCNTs-CeO 2xRD curve.
Fig. 2 is Ag@Pt/MWCNTs and the Ag@Pt/MWCNTs-CeO of embodiment 2 preparations 2stereoscan photograph.A is the stereoscan photograph of Ag@Pt/MWCNTs, and b is Ag@Pt/MWCNTs-CeO 2stereoscan photograph.
Fig. 3 is Ag@Pt/MWCNTs and the Ag@Pt/MWCNTs-CeO of embodiment 3 preparations 2cyclic voltammetry curve.A is the cyclic voltammetry curve of Ag@Pt/MWCNTs, and b is Ag@Pt/MWCNTs-CeO 2cyclic voltammetry curve.
Fig. 4 is Ag@Pt/MWCNTs and the Ag@Pt/MWCNTs-CeO of the preparation of embodiment 2 preparations 2polarization curve.A is the polarization curve of Ag@Pt/MWCNTs, and b is Ag@Pt/MWCNTs-CeO 2polarization curve.
The specific embodiment
Embodiment 1
A. the silver nitrate of 100mg, 1.0g natrium citricum and 100mg multi-walled carbon nano-tubes are dispersed in deionized water, ultrasonic 1h obtains the black suspension of homogeneous, then drips wherein 100mmol/L sodium borohydride/ethanolic solution of 10ml, obtains Ag/MWCNTs; The Ag/MWCNTs making is dispersed in 20ml ethylene glycol solution, and ultrasonic dispersion 1h, adds the platinum acid chloride solution of 2ml, and the KOH/ ethylene glycol solution with 2% regulates pH=5, is warming up to 60 ℃ of reaction 3h, obtains Ag@Pt/MWCNTs.
B. by the cerous nitrate solution of 0.1mmol/L 0.1mol L -1ammonia spirit regulates pH=7, solution poured in high-temperature high-pressure reaction kettle, and first at 60 ℃, reaction 2h, then at 110 ℃ of reaction 3h.Then through suction filtration, washing, be dried to obtain CeO 2.
C. the Ag@Pt/MWCNTs and the CeO that steps A are made 2mass ratio with 4:1 joins in ethanolic solution, ultrasonic dispersion 1h, and later suction filtration, in the vacuum drying chamber of 50 ℃, dry 5h obtains Ag@Pt/MWCNTs-CeO 2composite catalyst.
Embodiment 2
A. the silver nitrate of 150mg, 2.0g natrium citricum and 120mg multi-walled carbon nano-tubes are dispersed in deionized water, ultrasonic 2h obtains the black suspension of homogeneous, then drips wherein 200mmol/L sodium borohydride/ethanolic solution of 20ml, obtains Ag/MWCNTs; The Ag/MWCNTs making is dispersed in 60ml ethylene glycol solution, and ultrasonic dispersion 2h, adds the platinum acid chloride solution of 5ml, and the KOH/ ethylene glycol solution with 7% regulates pH=8, is warming up to 90 ℃ of reaction 4h, obtains Ag@Pt/MWCNTs.
B. by the cerous nitrate solution of 0.5mmol/L 0.1mol L -1ammonia spirit regulates pH=9, solution poured in high-temperature high-pressure reaction kettle, and first at 70 ℃, reaction 4h, then at 130 ℃ of reaction 4h.Then through suction filtration, washing, be dried to obtain CeO 2.
C. Ag@Pt/MWCNTs steps A being made and CeO2 join in ethanolic solution with the mass ratio of 5:1, ultrasonic dispersion 2h, and later suction filtration, in the vacuum drying chamber of 60 ℃, dry 10h obtains Ag@Pt/MWCNTs-CeO 2composite catalyst.
The Ag@Pt/MWCNTs-CeO that the Ag/MWCNTs respectively steps A being obtained and step C obtain 2adopt cyclic voltammetry to carry out chemical property contrast test
Pretreatment of glassy carbon electrode: respectively by 5mgAg/MWCNTs and Ag@Pt/MWCNTs-CeO 2with 0.9ml absolute ethyl alcohol and 0.1ml5%Nafion solution wiring solution-forming, ultrasonic 1h in ultrasonic cleaner, is dispersed in mixed solution catalyst afterwards; With liquid-transfering gun, pipette 10 μ l catalyst solutions in glass-carbon electrode surface, under room temperature, dry.
Test is carried out in three-electrode system, with above-mentioned surface, containing the glass-carbon electrode of catalyst, makes working electrode (d=5mm), and reference electrode is Ag/AgCl electrode, to electrode, is platinum filament, with the H of 0.5mol/L 2sO 4solution is done electrolyte.Adsorption peak or desorption peaks by the hydrogen in resulting cyclic voltammetry curve are carried out integration, obtain the electro-chemical activity surface area (ESA) of catalyst reaction, and formula is as follows:
ESA＝Q H/(2.1×Pt)
Q in formula h(Cm -2) be the electric weight of every square of Miboplatin surface desorption hydrogen, Pt (gm -2) for covering on glass-carbon electrode the content of Pt in catalyst.The unit of ESA is m 2/ g is one of performance important indicator of weighing by catalyst.The results are shown in Figure 3,
As seen from Figure 3, Ag@Pt/MWCNTs-CeO 2catalytic activity to be significantly higher than Ag@Pt/MWCNTs, Ag@Pt/MWCNTs-CeO 2electrochemical surface area can reach 97.2m 2g -1, the electrochemical surface area of Ag@Pt/MWCNTs is 66.15m 2g -1
Embodiment 3
A. the silver nitrate of 200mg, 3.6g natrium citricum and 300mg multi-walled carbon nano-tubes are dispersed in deionized water, ultrasonic 3h obtains the black suspension of homogeneous, then drips wherein 300mmol/L sodium borohydride/ethanolic solution of 40ml, obtains Ag/MWCNTs; The Ag/MWCNTs making is dispersed in 100ml ethylene glycol solution, and ultrasonic dispersion 4h, adds the platinum acid chloride solution of 10ml, and the KOH/ ethylene glycol solution with 10% regulates pH=10, is warming up to 120 ℃ of reaction 6h, obtains Ag@Pt/MWCNTs.
B. by the cerous nitrate solution of 1.0mmol/L 0.1mol L -1sodium hydroxide solution regulates pH=11, solution poured in high-temperature high-pressure reaction kettle, and first at 90 ℃, reaction 6h, then at 160 ℃ of reaction 6h.Then through suction filtration, washing, be dried to obtain CeO 2.
C. the Ag@Pt/MWCNTs and the CeO that steps A are made 2mass ratio with 8:1 joins in ethanolic solution, ultrasonic dispersion 4h, and later suction filtration, in the vacuum drying chamber of 80 ℃, dry 15h obtains Ag@Pt/MWCNTs-CeO 2composite catalyst.
The sample that adopts linear volt-ampere scanning method to obtain steps A, C carries out chemical property contrast test
The same cyclic voltammetry of pretreatment of glassy carbon electrode.
Test is carried out in three-electrode system, with above-mentioned surface, containing the glass-carbon electrode of catalyst, makes working electrode (d=5mm), and reference electrode is Ag/AgCl electrode, is platinum filament, at the H of 0.5mol/L to electrode 2sO 4the continual oxygen that passes in solution, after the concentration of oxygen in solution reaches capacity, starts the sweep test of linear volt-ampere, the supply that keeps oxygen in test process.Sweep speed is 5mV/s, and the scope of test voltage is-0.2-0.8V that the rotating speed of rotating circular disk is 1600rpm/min.Test result is shown in Fig. 4
Ag@Pt/MWCNTs-CeO as seen from Figure 4 2with respect to the hydrogen reduction take-off potential of the Ag@Pt/MWCNTs 40mV that shuffled.Ag@Pt/MWCNTs-CeO 2the limiting current density of curve is significantly higher than Ag@Pt/MWCNTs.CeO has adulterated 2catalyst there is obvious high limit electric current, illustrate under the existence of cerium oxide, increased the concentration of partial oxygen.In hydrogen reduction process, cerium oxide has maintained higher reaction rate as the source of supply of O.

Claims (3)

1. a preparation method for oxygen reduction catalyst, concrete preparation process is as follows:
A is dispersed in silver nitrate, natrium citricum and multi-walled carbon nano-tubes in deionized water, to prepare suspension A, making the wherein molar concentration of silver nitrate is 1-6mmol/L, the molar concentration of natrium citricum is 20-50mmol/L, the mass concentration of multi-walled carbon nano-tubes is 1-3g/L, sodium borohydride/ethanolic solution that dropping and suspension A volume ratio are 1:30-60 wherein again, filter, dry, obtain Ag/MWCNTs; In sodium borohydride/ethanolic solution, the content of sodium borohydride is 100-300mmol/L;
The Ag/MWCNTs making is dispersed in and in ethylene glycol solution, prepares suspension B by 1-3g/L, ultrasonic dispersion 1-4h, add the platinum acid chloride solution that accounts for suspension B volume parts 0.5-1%, with the KOH/ ethylene glycol solution of 2-10%, regulate pH=5-10 again, be warming up to 60-120 ℃ of reaction 3-6h, filter, dry, obtain Ag@Pt/MWCNTs;
B. the cerous nitrate solution that is 0.1-1.0mmol/L by concentration 0.1mol L -1ammoniacal liquor or 0.1mol L -1sodium hydroxide solution regulates pH=7-11, adds in high-temperature high-pressure reaction kettle, and first at 60-90 ℃, reaction 2-6h, then at 110-160 ℃ of reaction 3-6h, after filtration, washing, the dry CeO that obtains 2;
C. the CeO that Ag@Pt/MWCNTs steps A being made and step B obtain 2mass ratio with 4-8:1 joins in ethanolic solution, and ultrasonic dispersion 1-4h filters, and in the vacuum drying chamber of 50-80 ℃, dry 5-15h, obtains Ag@Pt/MWCNTs-CeO 2composite catalyst.
2. the oxygen reduction catalyst that prepared by method according to claim 1, is expressed as: Ag Pt/MWCNTs-CeO 2, be to take CNT as carrier, CeO 2the catalyst that the hud typed Ag@Pt of doping is active component, this catalyst is CeO 2uniform Doped is in Ag@Pt/MWCNTs.
3. the application of an oxygen reduction catalyst claimed in claim 2, this catalyst is applied to fuel battery cathode with proton exchange film catalyst, the catalytic activity of its catalyst improves 50-70% than Ag@Pt/MWCNTs, and its electrochemical surface area reaches 67.1-100.0m 2g -1, the current density of catalytic oxidation-reduction reaches 4.5-7.0mAcm -2.
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CN105244511A (en) * 2015-09-29 2016-01-13 北京化工大学 Alloy electrocatalyst and preparation method thereof
CN105797725A (en) * 2016-04-10 2016-07-27 刘义林 Pt/WO3-CNTs (carbon nanotubes) catalyst prepared with hydro-thermal synthesis method
CN105797726A (en) * 2016-04-10 2016-07-27 郑叶芳 Method for preparing Pt/WO3-CNTs (carbon nanotubes) catalyst by adopting hydro-thermal synthesis
CN105797724A (en) * 2016-04-10 2016-07-27 刘义林 Pt/WO3-CNTs (carbon nanotubes) catalyst
CN108428904A (en) * 2018-04-04 2018-08-21 北京航空航天大学 One kind hydrotalcite oxygen reduction catalyst of silver-based containing cerium and the preparation method and application thereof
CN108923049A (en) * 2018-07-19 2018-11-30 深圳大学 A kind of oxygen reduction reaction catalyst and preparation method and application
CN114530608A (en) * 2021-12-17 2022-05-24 深圳航天科技创新研究院 Catalyst for fuel cell, preparation method thereof and fuel cell
CN115739156A (en) * 2022-11-24 2023-03-07 中汽创智科技有限公司 Catalyst carrier and preparation method and application thereof

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CN105244511A (en) * 2015-09-29 2016-01-13 北京化工大学 Alloy electrocatalyst and preparation method thereof
CN105797725A (en) * 2016-04-10 2016-07-27 刘义林 Pt/WO3-CNTs (carbon nanotubes) catalyst prepared with hydro-thermal synthesis method
CN105797726A (en) * 2016-04-10 2016-07-27 郑叶芳 Method for preparing Pt/WO3-CNTs (carbon nanotubes) catalyst by adopting hydro-thermal synthesis
CN105797724A (en) * 2016-04-10 2016-07-27 刘义林 Pt/WO3-CNTs (carbon nanotubes) catalyst
CN108428904A (en) * 2018-04-04 2018-08-21 北京航空航天大学 One kind hydrotalcite oxygen reduction catalyst of silver-based containing cerium and the preparation method and application thereof
CN108428904B (en) * 2018-04-04 2020-05-08 北京航空航天大学 Cerium-silver-containing hydrotalcite oxygen reduction catalyst and preparation method and application thereof
CN108923049A (en) * 2018-07-19 2018-11-30 深圳大学 A kind of oxygen reduction reaction catalyst and preparation method and application
CN108923049B (en) * 2018-07-19 2021-07-20 深圳大学 Oxygen reduction reaction catalyst, preparation method and application
CN114530608A (en) * 2021-12-17 2022-05-24 深圳航天科技创新研究院 Catalyst for fuel cell, preparation method thereof and fuel cell
CN114530608B (en) * 2021-12-17 2023-07-07 深圳航天科技创新研究院 Catalyst for fuel cell, preparation method of catalyst and fuel cell
CN115739156A (en) * 2022-11-24 2023-03-07 中汽创智科技有限公司 Catalyst carrier and preparation method and application thereof

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Application publication date: 20140730