CN103078123A - Fuel cell catalyst and preparation method thereof - Google Patents
Fuel cell catalyst and preparation method thereof Download PDFInfo
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- CN103078123A CN103078123A CN2013100061602A CN201310006160A CN103078123A CN 103078123 A CN103078123 A CN 103078123A CN 2013100061602 A CN2013100061602 A CN 2013100061602A CN 201310006160 A CN201310006160 A CN 201310006160A CN 103078123 A CN103078123 A CN 103078123A
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- ceo
- ethylene glycol
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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
Abstract
The invention discloses a fuel cell catalyst and a preparation method thereof. The fuel cell catalyst Pt-CeO2/GN takes graphene as a carrier, and Pt-CeO2 is taken as the catalyst of active components, wherein composite nano particles of Pt and CeO2 are uniformly distributed on the surface of the graphene, and the particle size of the Pt is 3-5 nm; the catalytic activity of the fuel cell catalyst is improved by 20-35 percent, compared with the catalytic activity of Pt/GN catalyst; and the electrochemical activity area of the fuel cell catalyst reaches 59.1-66.4 m<2>/g<-1>, and the density of current for catalyzing methanol oxide reaches 279.5-440.1 mA/g<-1>Pt. The preparation method comprises the following steps: graphite oxide and cerium nitrate are dispersed in water, ammonia is used to regulate the pH value, and CeO2/GN is obtained via reaction; and prepared CeO2/GN is dispersed in ethylene glycol solution in an ultraphonic manner, chloroplatinic acid solution is added, the pH value is regulated, and Pt-CeO2/GN catalyst is obtained via reaction. The preparation method disclosed by the invention is simple, can prepare catalysts provided with higher catalytic activity and stability, and has a broad application prospect in the filed of fuel cells.
Description
Technical field
The present invention relates to fuel-cell catalyst and preparation thereof, be specifically related to Pt-CeO
2/ GN Catalysts and its preparation method.
Background technology
Direct methanol fuel cell (DMFC) is one of main path that solves environmental pollution and energy crisis as the green energy resource that cleans, efficient, operating condition is gentle.Yet lower reaction rate has limited the application of DMFC.At present, Pt is catalyticing anode and the negative electrode optimum activity component that reacts, but Pt expensive and easily poisoned by the intermediate product of methanol oxidation (such as CO) and lose catalytic activity at anode is still slower in the kinetics of negative electrode.Therefore, the low year platinum of research and development, high performance catalyst are the key technologies that promotes the fuel cell development.Recent research shows, Pt and transition metal (such as Ru, Pd, Ni etc.) are compounded to form alloy or hud typed catalyst with bimetallic catalytic mechanism, can effectively improve catalytic activity and the poison resistance of catalyst.Also have scholar's research to find that blended metal oxide is (such as CeO in the Pt series catalysts
2, TiO
2, Fe
2O
3Deng) can prevent the reunion of Pt nano particle, metal oxide forms concerted catalysis effect raising catalytic activity with Pt simultaneously.Because CeO
2Cheap, oxygen storage capacity is high, and CeO
2Can provide a good environment by the storage that is changed to oxygen and the transmission of valence state, so scholars are for Pt and CeO
2The performance study of composite catalyst made many work.(M. Aulice Scibioh et al., the Pt-CeO such as Scibioh
2/ C anode catalyst for direct methanol fuel cells, Applied Catalysis B:Environmental, 2008,84 (3), 773-782) adopt the method for fractional steps to make Pt-CeO
2/ C catalyst, CeO in the catalytic oxidation methanol process is found in research
2Play concerted catalysis effect, Pt-CeO with Pt
2Activity and the stability of/C catalyst Oxidation of Methanol are higher than the Pt/C catalyst.
Carrier has larger impact to the performance of catalyst, studies show that the catalytic performance of the Pt/C catalyst of the pure platinum catalyst ratio commerce take carbon nano-tube as carrier exceeds one times.Graphene is a kind of two-dimentional Carbon Materials of the alveolate texture that is comprised of the carbon atom of individual layer, has than the larger specific area of carbon nano-tube and better electronic conduction ability, and be catalyst carrier ideal after carbon black, carbon nano-tube.
Summary of the invention
The object of the present invention is to provide a kind of fuel-cell catalyst with high catalytic activity and stability and preparation method thereof.
Fuel-cell catalyst provided by the invention is take Graphene as carrier, Pt-CeO
2Catalyst Pt-CeO as active component
2/ GN, Pt and CeO in this catalyst
2Composite nanometer particle be evenly distributed in the Graphene surface, the particle diameter of Pt particle is 3-5 nm.Pt-CeO
2The catalytic activity of/GN catalyst improves 20-35% than the catalytic activity of Pt/GN catalyst; Its electrochemical surface area reaches 59.1-66.4 m
2g
-1, the current density of catalytic oxidation methyl alcohol can reach 279.5-440.1 mA g
-1Pt.(can be used as the performance data of this catalyst).
The concrete preparation process of this fuel-cell catalyst is as follows:
The preparation reference literature of described graphite oxide (S. William et al., Preparation of Graphitic Oxide, J. Am. Chem. Soc., 1958,80,1339).
A. graphite oxide powder (GN) is mixed and ultrasonic being uniformly dispersed according to mass ratio 4-40:1 with cerous nitrate, use 0.1-0.5mol L
-1Ammoniacal liquor or 0.1-0.5mol L
-1Sodium hydroxide solution is regulated pH=8-11, in 80-120 ℃ of back flow reaction 4-6h, and again in 120-160 ℃ of reaction 3-6h, then suction filtration, washing, oven dry obtains the compound that Graphene carries ceria in 40-60 ℃ vacuum drying chamber, uses CeO
2/ GN represents;
B. the CeO that steps A is made
2/ GN joins in the ethylene glycol solution, wherein CeO
2The ratio of/GN and ethylene glycol is 1mg:1-2ml, and ultrasonic dispersion 1-4h adds chloroplatinic acid, wherein CeO
2The ratio of/GN and chloroplatinic acid is 3:1-1:2, the pH value of regulating above-mentioned mixed solution with the ethylene glycol solution of the ethylene glycol solution of NaOH or potassium hydroxide is 9-11, be warming up to 80-120 ℃ of reaction 4-6h, then suction filtration, washing, the dry Pt-CeO that gets in 40-60 ℃ vacuum drying chamber
2/ GN catalyst.
The NaOH mass fraction is 5-10% in the ethylene glycol solution of described NaOH, and the mass fraction of potassium hydroxide is 5-10% in the ethylene glycol solution of potassium hydroxide.
Fig. 1 is the Pt-CeO of embodiment 2 preparations
2/ GN and CeO
2The XRD spectra of/GN, Pt/GN.As seen from the figure, in three curves, 2 θ=23.7 ° are the characteristic diffraction peaks of Graphene; Curve (a) and (c) in, 2 θ=28.7 °, 33.1 °, 47.4 °, 56.4 ° and 76.8 ° are corresponding respectively to be the CeO of face-centred cubic structure
2(200), the diffraction maximum of (220), (311), (222) and (420) crystal face.Curve (b) and (c) in, 2 θ=39.8 °, 46.3 °, 67.8 ° and 81.5 ° are respectively the characteristic diffraction peaks of Pt (111), (200), (220) and (311) crystal face.Pt-CeO
2The characteristic diffraction peak of the Pt of/GN (111) crystal face is than the little and wide Pt-CeO of pure platinum catalyst
2The characteristic diffraction peak of the Pt of/GN (111) crystal face is less and wide than Pt/GN catalyst, calculates Pt-CeO by the Scherrer formula
2The particle diameter of Pt nanoparticle is 4.1nm in the/GN catalyst, the 5.5nm of Pt/GN catalyst.
Fig. 2 is the Pt-CeO of embodiment 2 preparations
2The transmission electron microscope photo of/GN catalyst.By finding out Pt and CeO among the figure a
2Composite nanometer particle be evenly distributed in the Graphene surface, the particle diameter of particle is 3-5nm, and is consistent with XRD result of calculation.Can clearly see Pt (111) and CeO by figure b
2(111) lattice fringe of crystal face, its spacing of lattice is respectively 0.229nm and 0.232nm.
The prepared fuel-cell catalyst of the present invention has important application aspect fuel cell.The sign of fuel-cell catalyst being carried out chemical property adopts the cyclic voltammetry curve method usually.The method of testing of cyclic voltammetry curve is: adopt three-electrode system, reference electrode is saturated calomel electrode, is platinum electrode to electrode, and work electrode uses the polytetrafluoroethylene glass-carbon electrode.Catalyst to be tested and absolute ethyl alcohol and Nafion solution are made into mixed serum, drip on the glass-carbon electrode with micro syringe, natural drying in air at room temperature, obtain work electrode.Used electrolyte is 0.5mol L
-1H
2SO
4Solution or 0.5mol L
-1H
2SO
4With 1 mol L
-1The methyl alcohol mixed solution.Before test, in solution, lead to first nitrogen (N
2) 30min is to remove the partial oxidation in the solution, sweep limits is-0.2-1.2V (relative saturation calomel electrode) that potential scanning speed is 50mV s
-1In cyclic voltammetry curve, near the peak-0.1V is the oxidation peak of hydrogen, and the peak of 0.4-0.45V is the Reduction of oxygen peak, and the size of the integral area at redox peak represents respectively carries out for what of redox reaction electric weight.And can be calculated the electrochemistry oxygen active area of the Pt of unit mass by the integral area at the redox peak in the cyclic voltammetry curve of catalyst, concrete formula is as follows:
EAS(m
2?g
-1)=Q
H/(2.1×[Pt])
Catalyst circulation volt-ampere curve test result is seen Fig. 3 and Fig. 4.
As seen from Figure 3, CeO
2/ GN does not almost have catalytic activity, Pt-CeO
2The catalytic activity of/GN catalyst is apparently higher than the catalytic activity of Pt/GN catalyst, Pt-CeO
2The electrochemical surface area of/GN catalyst is 66.4 m
2g
-1
At 0.5mol L
-1H
2SO
4With 1 mol L
-1The cyclic voltammetry curve characterization result is seen Fig. 4 in the methyl alcohol mixed solution, can find out CeO by curve a among the figure
2/ GN does not almost have catalytic activity, Pt-CeO to methyl alcohol
2The catalyst of/GN is compared with the Pt/GN catalyst, and the ability of catalytic oxidation methyl alcohol significantly improves, and the forward scan density peak value can reach 440.1mA mg
-1Pt, than Pt/GN height 251.2 mA mg
-1Pt.
Beneficial effect: the present invention adopts CeO
2/ GN composite nanoparticle prepares Pt-CeO as carrier
2/ GN, on the one hand CeO
2Cheap, oxygen storage capacity is high, can make the Pt nanoparticulate dispersed more even, the ratio that Pt is exposed in the oxygen increases, on the other hand CeO
2Can pass through Ce
3+With Ce
4+Variation of valence is O
2Transmission provides a good environment, can play with Pt the effect of concerted catalysis, effectively the carrying out of accelerating oxidation reduction reaction.Use CeO
2The Graphene of modifying is as the Pt-CeO of carrier preparation
2/ GN catalyst, its electrochemical surface area can reach 66.4m
2g
-1, the current density of catalytic oxidation methyl alcohol can reach 440.1 mA g
-1Pt.
Description of drawings
Fig. 1 is the Pt-CeO of embodiment 2 preparations
2/ GN and CeO
2The XRD spectra of/GN, Pt/GN.Wherein a is CeO
2The XRD curve of/GN, b are the XRD curve of Pt/GN, and c is Pt-CeO
2The XRD curve of/GN.
Fig. 2 is the Pt-CeO of embodiment 2 preparations
2The TEM photo of/GN.A is common transmission electron microscope picture, and b is the high power transmission electron microscope picture.
Fig. 3 is that the catalyst of embodiment 2 preparation is at 0.5mol L
-1H
2SO
4Cyclic voltammetry curve in the solution.A is CeO among the figure
2The cyclic voltammetry curve of/GN, b are the cyclic voltammetry curve of Pt/GN, and c is Pt-CeO
2/ GN cyclic voltammetry curve.
Fig. 4 is that the catalyst of embodiment 2 preparation is at 0.5mol L
-1H
2SO
4With 1 mol L
-1Cyclic voltammetry curve in the methyl alcohol mixed solution.A is CeO among the figure
2The cyclic voltammetry curve of/GN, b are the cyclic voltammetry curve of Pt/GN, and c is Pt-CeO
2/ GN cyclic voltammetry curve.
Embodiment
Embodiment 1
A. take by weighing the 2g graphite powder, add successively the dense H of 46ml
2SO
4, 0.5g NaNO
3With 6g KMnO
4, the control reaction temperature is at stirring reaction 1h below 10 ℃.There-necked flask moved on in 35 ℃ of water-baths react 0.5h, slowly drip the 92ml deionized water.Be warming up to rapidly 95 ℃ of reaction 0.5h, add 30% the H of 20ml
2O
2Stop reaction.Product is neutral with 5% hydrochloric acid solution and deionized water washing, and 80 ℃ of dryings obtain graphite oxide.
B. get in the graphite oxide and the ultrasonic 100ml of the being dispersed in ultra-pure water of 25.2mg cerous nitrate of 90mg, ultrasonic 30min moves into there-necked flask in the oil bath pan, is warming up to 80 ℃, uses 0.1mol L
-1The pH=8 of ammoniacal liquor regulator solution, constant temperature backflow 4h pours solution in the reactor into while hot, reacts 4h under 120 ℃ of conditions.With product suction filtration, washing, 40 ℃ of lower vacuumizes obtain CeO
2/ GN.
C. take by weighing 26.2mg CeO
2/ GN adds 26ml ethylene glycol and 17.4mg chloroplatinic acid, ultrasonic dispersion 1h in there-necked flask, there-necked flask is moved in 80 ℃ of oil bath pans, be that the pH value that the ethylene glycol solution of 5% potassium hydroxide is regulated above-mentioned mixed solution is 9 with mass fraction, stirring and refluxing reaction 4h, washs to get Pt-CeO at suction filtration
2/ GN catalyst.
Be used for the Pt/GN of contrast test according to traditional immersion reduction method preparation, concrete steps are as follows: 40mg graphite oxide and 26.6mg chloroplatinic acid are dispersed in the 50ml ultra-pure water, and ultrasonic 1h adds the 0.2g citric acid, after stirring, drips 20ml 0.1g ml
-1NaBH
4, react 6h under the normal temperature, suction filtration, washing, 50 ℃ of vacuumizes obtain the Pt/GN catalyst.
A. step is with embodiment 1
B. get in the graphite oxide and the ultrasonic 100ml of the being dispersed in ultra-pure water of 12.6mg cerous nitrate of 95mg, ultrasonic 1h moves into there-necked flask in the oil bath pan, be warming up to 120 ℃, with the pH=11 of ammoniacal liquor regulator solution, constant temperature backflow 6h, while hot solution is poured in the reactor, under 160 ℃ of conditions, reacted 6h.With product suction filtration, washing, 50 ℃ of lower vacuumizes obtain CeO
2/ GN.
C. take by weighing 44.8mg CeO
2/ GN adds 40ml ethylene glycol and 30mg chloroplatinic acid in there-necked flask, ultrasonic dispersion 2h moves into there-necked flask in 120 ℃ of oil bath pans, is that the ethylene glycol solution of 5% NaOH is regulated pH=11 with concentration, and stirring and refluxing is reacted 6h, suction filtration, washs to get Pt-CeO
2/ GN catalyst
Embodiment 3
A, the B step is with embodiment 1
C. take by weighing 44.8mg CeO
2/ GN adds 50ml ethylene glycol and 30mg chloroplatinic acid in there-necked flask, ultrasonic dispersion 2h moves into there-necked flask in 90 ℃ of oil bath pans, is 5% potassium hydroxide ethylene glycol solution adjusting pH=10 with concentration, stirring and refluxing reaction 6h, and filtering and washing gets Pt-CeO
2/ GN catalyst.
Claims (3)
1. a fuel-cell catalyst is take Graphene as carrier, Pt-CeO
2Catalyst as active component is expressed as Pt-CeO
2/ GN, wherein GN represents Graphene; Pt and CeO in this catalyst
2Composite nanometer particle be evenly distributed in the Graphene surface, the particle diameter of Pt particle is 3-5nm.
2. fuel-cell catalyst according to claim 1, its catalytic activity improves 20-35% than the catalytic activity of Pt/GN catalyst; Its electrochemical surface area reaches 59.1-66.4 m
2g
-1, the current density of catalytic oxidation methyl alcohol reaches 279.5-440.1 mA g
-1Pt.
3. method for preparing fuel-cell catalyst claimed in claim 1, concrete preparation process is as follows:
A. the graphite oxide powder is mixed and ultrasonic being uniformly dispersed according to mass ratio 4-40:1 with cerous nitrate, use 0.1-0.5mol L
-1Ammoniacal liquor or 0.1-0.5mol L
-1Sodium hydroxide solution is regulated pH=8-11, in 80-120 ℃ of back flow reaction 4-6h, and again in 120-160 ℃ of reaction 3-6h, then suction filtration, washing, oven dry obtains the compound that Graphene carries ceria in 40-60 ℃ vacuum drying chamber, uses CeO
2/ GN represents;
B. the CeO that steps A is made
2/ GN joins in the ethylene glycol solution, wherein CeO
2The ratio of/GN and ethylene glycol is 1mg:1-2ml, and ultrasonic dispersion 1-4h adds chloroplatinic acid, wherein CeO
2The ratio of/GN and chloroplatinic acid is 3:1-1:2, the pH value of regulating above-mentioned mixed solution with the ethylene glycol solution of the ethylene glycol solution of NaOH or potassium hydroxide is 9-11, be warming up to 80-120 ℃ of reaction 4-6h, then suction filtration, washing, the dry Pt-CeO that gets in 40-60 ℃ vacuum drying chamber
2/ GN catalyst;
The NaOH mass fraction is 5-10% in the ethylene glycol solution of described NaOH, and the mass fraction of potassium hydroxide is 5-10% in the ethylene glycol solution of potassium hydroxide.
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Cited By (10)
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|---|---|---|---|---|
| CN103831102A (en) * | 2014-03-14 | 2014-06-04 | 哈尔滨工业大学 | Preparation method of graphene catalyst |
| CN103831103A (en) * | 2014-03-14 | 2014-06-04 | 哈尔滨工业大学 | Graphene aerogel catalyst and preparation method thereof |
| CN104841454A (en) * | 2015-04-22 | 2015-08-19 | 南京理工大学 | Preparation method of Pd-Fe2O3/GO composite material |
| CN105244511A (en) * | 2015-09-29 | 2016-01-13 | 北京化工大学 | Alloy electrocatalyst and preparation method thereof |
| CN105948032A (en) * | 2016-07-04 | 2016-09-21 | 烟台市烯能新材料股份有限公司 | Method for etching multilayer graphene |
| CN108630956A (en) * | 2018-04-26 | 2018-10-09 | 哈尔滨师范大学 | A kind of direct methanoic acid fuel cell palladium-based catalyst carrier and preparation method thereof |
| CN108767280A (en) * | 2018-06-22 | 2018-11-06 | 西安交通大学 | A kind of Pt nano particles/hydroxyl carbon cerium mine nano-cluster/graphene composite material and preparation method thereof |
| CN109524679A (en) * | 2018-11-07 | 2019-03-26 | 北京化工大学 | A kind of efficient electric catalysis methanol oxidized fuel cell catalyst and preparation method thereof |
| CN110890558A (en) * | 2019-11-05 | 2020-03-17 | 中新国际联合研究院 | Supported platinum-based core-shell catalyst and preparation method thereof |
| CN113224323A (en) * | 2021-05-17 | 2021-08-06 | 安徽师范大学 | Three-dimensional flower-shaped ultrathin two-dimensional Ce and B doped Pt nanosheet and preparation method and application thereof |
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| CN103831102A (en) * | 2014-03-14 | 2014-06-04 | 哈尔滨工业大学 | Preparation method of graphene catalyst |
| CN104841454A (en) * | 2015-04-22 | 2015-08-19 | 南京理工大学 | Preparation method of Pd-Fe2O3/GO composite material |
| CN105244511A (en) * | 2015-09-29 | 2016-01-13 | 北京化工大学 | Alloy electrocatalyst and preparation method thereof |
| CN105948032A (en) * | 2016-07-04 | 2016-09-21 | 烟台市烯能新材料股份有限公司 | Method for etching multilayer graphene |
| CN108630956B (en) * | 2018-04-26 | 2021-01-29 | 哈尔滨师范大学 | Palladium-based catalyst carrier for direct formic acid fuel cell and preparation method thereof |
| CN108630956A (en) * | 2018-04-26 | 2018-10-09 | 哈尔滨师范大学 | A kind of direct methanoic acid fuel cell palladium-based catalyst carrier and preparation method thereof |
| CN108767280A (en) * | 2018-06-22 | 2018-11-06 | 西安交通大学 | A kind of Pt nano particles/hydroxyl carbon cerium mine nano-cluster/graphene composite material and preparation method thereof |
| CN108767280B (en) * | 2018-06-22 | 2020-10-27 | 西安交通大学 | Pt nanoparticle/hydroxyl cerite nanocluster/graphene composite material and preparation method thereof |
| CN109524679A (en) * | 2018-11-07 | 2019-03-26 | 北京化工大学 | A kind of efficient electric catalysis methanol oxidized fuel cell catalyst and preparation method thereof |
| CN109524679B (en) * | 2018-11-07 | 2021-06-25 | 北京英维深技术有限公司 | High-efficiency electrocatalytic methanol oxidation fuel cell catalyst and preparation method thereof |
| CN110890558A (en) * | 2019-11-05 | 2020-03-17 | 中新国际联合研究院 | Supported platinum-based core-shell catalyst and preparation method thereof |
| CN113224323A (en) * | 2021-05-17 | 2021-08-06 | 安徽师范大学 | Three-dimensional flower-shaped ultrathin two-dimensional Ce and B doped Pt nanosheet and preparation method and application thereof |
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