CN104998658A - Method for preparing proton-exchange membrane fuel cell oxygen reduction catalyst based on PtNi (111) octahedral single crystal nanoparticles - Google Patents
Method for preparing proton-exchange membrane fuel cell oxygen reduction catalyst based on PtNi (111) octahedral single crystal nanoparticles Download PDFInfo
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Abstract
The invention discloses a method for preparing a proton-exchange membrane fuel cell oxygen reduction catalyst based on PtNi (111) octahedral single crystal nanoparticles, which mainly solves the problem in the prior art that a conventional single-Pt catalyst or a Pt-based catalyst based on bimetallic spherical core-shell-structured nanoparticles is low in activity and poor in Pt atomic efficiency. Meanwhile, the influence factor and the synthesis optimization condition for morphology-controlled PtNi (111) octahedral single crystal nanoparticles are obtained. According to the technical scheme of the invention, platinum acetylacetonate and nickel acetylacetonate are adopted as metal salt precursors, and N, N-dimethylformamide (DMF) is adopted as a crystal face growth control agent. Through the heating reduction process, morphology-controlled PtNi (111) octahedral single crystal nanoparticles are obtained. The morphology-controlled PtNi (111) octahedral single crystal nanoparticles are subjected to ultrasonic dispersion in n-hexane, and then the well dispersed sol is slowly added onto the conductive carbon black of high specific surface area drop by drop through the residual titration process. Therefore, the electro-catalysis specific activity of the obtained oxygen reduction catalyst is high up to 1.5 A/mg Pt, and is improved by 9-10 times compared with that of conventional commercial Pt/C catalysts.
Description
Technical field
The present invention relates to the preparation method of a kind of fuel battery cathode with proton exchange film oxidation raw catalyst, PtNi (111) nano crystal prepared of the method octahedra bimetallic fuel-cell catalyst oxygen reduction activity is high, reduces Pt content and improves the utilization rate of Pt atom.
Background technology
The finiteness of fossil fuel and pollution becoming serious that is non-renewable and that brought by its burning, hydrogen energy source Proton Exchange Membrane Fuel Cells technology, as clean energy resource replacement scheme, has the outstanding advantages such as no pollution, energy work rate height.Predict according to authoritative expert, in 5 ~ 10 years, PEMFC will welcome the development of blowout formula at automotive field: 2016 ~ the year two thousand twenty is the market introduction stage of PEMFC automobile, to realize its large-scale commercial after the year two thousand twenty, the potential commercial value in this field will up to 97,000,000,000 dollars.Proton Exchange Membrane Fuel Cells becomes the focus of the current exploitation of fuel cell in the world, along with the reduction of the production cost of its core component fuel-cell catalyst and the optimization of battery system technology, as the core component on PEMFC, fuel-cell catalyst demand is large, business added value is high, there is wide development and application prospect, be not only the ideal source of electric automobile, and have a wide range of applications in fields such as communications and transportation, portable electronic, Aero-Space, military affairs, family's generating, distributed power generation, power stations.
At present, hydrogen energy source Proton Exchange Membrane Fuel Cells slowly fails really to realize commercial industrial, and the maximum bottleneck limiting the application of its large-scale commercial is catalytic performance and the cost of its Cathodic oxygen reduction (ORR) catalyst.Cathodic oxygen reduction catalyst is because Pt demand is large, and the reasons such as catalytic efficiency is low are the Focal point and difficult points of research always.Therefore, the electrochemical catalyst how preparing high activity low noble metal just becomes the important step (Debe solving fuel cell problem, M.K.Electrocatalyst approaches and challengesfor automotivefuel cells [J] .Nature, 2012,486:43-51).Up to now, Pt remains the most effective catalytic active component of Proton Exchange Membrane Fuel Cells, but Pt resource and scarcity thereof, price is rather stiff are held high, oxygen reduction catalyst Pt content is quite high, and the not high (Banham of catalytic efficiency, D.Feng, F.X.Pei, K.etal.Effect of carbon support nanostructure on the oxygen reduction activity of Pt/C catalysts [J] .Journal ofMaterials ChemistryA, 2013,1:2812-2820).In order to improve above-mentioned defect and reduce its cost, 3d transition metal M element is added (as Fe in Pt, Cr, Co, Ni, Cu etc.), form Pt bimetallic (or three metals) catalyst to can yet be regarded as one comparatively effective method (Rao, C.V.Viswanathan, B.ORRActivity andDirectEthanolFuel Cell Performance of Carbon-Supported Pt-M (M=Fe, Co, and Cr) Alloys Prepared by Polyol ReductionMethod [J] .Journal ofPhysical Chemistry C, 2009, 113:18907-18913) (Xu, Z.Zhang, H. M.Liu, S.S.Facile synthesis of supported Pt-Cu nanoparticles with surface enriched Pt as highly active cathode catalyst for proton exchange membrane fuel cells [J] .International Journal of HydrogenEnergy, 2012, 37:17978-17983), " Anchoring Effect " that produced by it can effective control Pt gathering or running off at carrier surface, make it higher than the stability of pure Pt catalyst.At present the research of Pt bimetallic oxygen reduction catalyst is mainly concentrated on to the nano spherical particle of alloy and nucleocapsid structure, although increase than Pt/C catalyst activity, also reach far away business-like requirement.Because catalytic reaction activity depends on the interaction between reactant and catalyst surface, and the atomic and electronic structures on the catalyst activity component particles surface of different crystal structure is all different, and this affects the catalytic activity of catalyst to a great extent.Therefore, the activity that pattern and crystal structure by regulating and controlling catalyst improve catalyst further becomes ideal mode.
Summary of the invention
1. the object of the invention is to provide a kind of fuel-cell catalyst of high hydrogen reduction electro catalytic activity, by pattern and the crystal structure of regulation and control PtNi bimetal nano particles, obtain the preparation method of the catalyst of PtNi (111) monocrystalline octahedral structure, while raising oxygen reduction catalytic activity, reduce the content of Pt and improve the utilization rate of Pt atom.
2. the presoma mentioned of the present invention with acetylacetone,2,4-pentanedione platinum and nickel acetylacetonate for part, this is because organic ligand acetylacetone,2,4-pentanedione group changes the reduction potential of metal ion from Thermodynamics, itself and metal nanoparticle generating rate are matched, is conducive to the control of metal nanoparticle size and pattern.
3. the N that mentions of the present invention; dinethylformamide (DMF); as a kind of organic solvent; acetylacetone,2,4-pentanedione platinum containing organic ligand and nickel acetylacetonate can be dissolved according to similar dissolve mutually theory; and there is reducing agent and protectant effect in the reaction, avoid the reunion of nano particle.In addition, DMF also as the high preferred orientation growth promoter of the octahedra nano particle of monocrystalline, controls the pattern of crystal structure.
4. the present invention mention using a certain amount of n-hexane as dispersant ultrasonic disperse Nano sol, adopting the mode of back titration slowly to be dripped by scattered colloidal sol again loads on carbon black-supported, object is that nano particle is uniformly dispersed on carbon black-supported, and monodispersity is good, soilless sticking phenomenon.
5. the catalyst mentioned of the present invention, be mainly used in Proton Exchange Membrane Fuel Cells oxygen reduction reaction, preparation process key step is as described below:
The first step: the configuration of precursor solution.Get a certain amount of N, dinethylformamide is solvent, add 2mmol/L acetylacetone,2,4-pentanedione platinum and 6mmol/L nickel acetylacetonate, ensure that acetylacetone based amount is 0.4mmol:50ml with the ratio of the amount of DMF, then be uniformly mixed, by in the autoclave of above-mentioned mixed liquor impouring glass-lined, sealed by nut;
Second step: the octahedra nano particle synthesis of monocrystalline.The reactor of above-mentioned sealing is inserted in vacuum drying oven temperature, smokes and make vacuum reach 0.8Mpa, be heated to 120 DEG C with the speed of 10 DEG C/min, and keep this temperature about 42 hours;
3rd step: catalyst preparing.Take out reactor and be cooled to normal temperature in a water bath immediately, then in colloidal sol, a certain amount of n-hexane ultrasonic disperse is added 3 hours, obtain grey black sol solution, then will slowly be added drop-wise on conductive black carrier in scattered colloidal sol by the mode of back titration, stir and spend the night about 24 hours;
4th step: washing dry run.Above-mentioned system vacuum filtration is removed water, and replace washing 8 ~ 10 times by ethanol and deionized water, then dry at 80 DEG C in vacuum drying chamber, obtaining platinum load capacity is that the charcoal of 30% (weight ratio) carries PtNi (111) monocrystalline octahedra bimetallic Proton Exchange Membrane Fuel Cells oxygen reduction catalyst.
6. relevant characterization result is as follows:
(1) catalyst activity composition features (TEM) characterization result is as Fig. 1-8.
Beneficial effect
This catalytic benefits is high to oxygen reduction catalytic activity, and Pt content reduces, and does not introduce the impurity elements such as Cl, S of easily causing catalyst poisoning.Wherein when Pt:Ni is than during for 1:3, control the most favourable to PtNi (111) monocrystalline shape of octahedron.When the volume ratio of Pt salt and the total acetylacetone based amount of substance of Ni salt and DMF is 0.4mmol:50ml, control the most favourable to PtNi (111) monocrystalline shape of octahedron.When the mass ratio of platinum content is 30% in catalyst, has and reduce largely.Compared with prior art, commercial at present fuel-cell catalyst is oxidized former (ORR) activity and is only about 0.13 ~ 0.15A/mgPt under high platinum load capacity (Pt content is 70%).The present invention is oxidized former (ORR) activity by the octahedra catalyst of PtNi (111) nano crystal that the pattern and crystal structure regulating and controlling catalyst prepares and reaches 1.5A/mgPt under low platinum load (Pt content is 30%), is much better than current business-like Pt/C fuel-cell catalyst.
The present invention prepares the octahedra nano particle of PtNi (111) monocrystalline, part precious metals pt is replaced with transition metal Ni, on the one hand by the consumption adding effectively minimizing Pt of Ni, shorten the interatomic spacing of lattice of Pt-Pt adding of Ni in addition, be conducive to the Dissociative of oxygen, and in catalyst, the loss of a small amount of Ni can cause the roughening of Pt atomic surface, makes specific surface area active increase, is conducive to the raising of catalyst activity.
Accompanying drawing explanation
Fig. 1-2 is that Pt:Ni (atomic ratio) is for preparing the transmission electron microscope picture of sample during 1:1;
Fig. 3-4 is that Pt:Ni (atomic ratio) is for preparing the transmission electron microscope picture of sample during 1:2;
Fig. 5-6 is that Pt:Ni (atomic ratio) is for preparing the transmission electron microscope picture of sample during 1:3; When Pt:Ni atomic ratio is 1:3, nano particle presents (111) monocrystalline octahedral structure of rule.
Fig. 7 be under the different PtNi proportioning of the present invention catalyst in linear scan voltammogram and catalyst quality specific activity result.Quality is at 0.9V/RHE, 0.1mol/LHClO than activity data
4as electrolyte, 1600rpm, 20mV/s sweep in the three-electrode system under speed and obtain, and wherein during Pt:Ni=1:3, activity is preferably 1.5A/mgPt.
Fig. 8 is catalyst circulation voltammogram under the different PtNi proportioning of the present invention.
Detailed description of the invention
The present invention is further described below:
Experimental raw: acetylacetone,2,4-pentanedione platinum (Guiyan Platium Co., Ltd); Nickel acetylacetonate (Aladdin); DMF (Xilong Chemical Co., Ltd analyzes pure); N-hexane (Xilong Chemical Co., Ltd analyzes pure); Conductive black (Cabot, XC-72).
Embodiment 1: take acetylacetone,2,4-pentanedione platinum 39.3mg, nickel acetylacetonate 77.1mg, puts into 50mL DMF and fully dissolves, and wherein Pt:Ni atomic ratio is 1:3.Mixed liquor is placed in autoclave, and heat 42 hours at 120 DEG C in baking oven, then gained solution cool to room temperature adds 50mL n-hexane, ultrasonic 3 hours and control bath temperature and be no more than 30 DEG C.Then the colloidal sol of above-mentioned high degree of dispersion is added drop-wise in 28.2mg conductive black solution in the mode of back titration, stirs after 48 hours, static filtration, and to use deionized water and ethanol alternately clean, be finally placed in vacuum drying oven at 60 DEG C drying 6 hours.This product catalyst oxidation former (ORR) activity value is about 1.50A/mg.
Embodiment 2: take acetylacetone,2,4-pentanedione platinum 39.3mg, nickel acetylacetonate 51.4mg, puts into 37.5mL DMF and fully dissolves, and wherein Pt:Ni atomic ratio is 1:2.Mixed liquor is placed in autoclave, and heat 42 hours at 120 DEG C in baking oven, then gained solution cool to room temperature adds 25mL n-hexane, ultrasonic 3 hours and control bath temperature and be no more than 30 DEG C.Then the colloidal sol of above-mentioned high degree of dispersion is added drop-wise in 34.0mg conductive black solution in the mode of back titration, stirs 48 hours, static filtration, use deionized water and ethanol alternately to clean to products obtained therefrom, be finally placed in vacuum drying oven drying 6 hours at 60 DEG C.Products obtained therefrom oxidation former (ORR) activity is about 0.95A/mg.
Embodiment 3: take acetylacetone,2,4-pentanedione platinum 39.3mg, nickel acetylacetonate 25.7mg, puts into 25mL DMF and fully dissolves, and wherein Pt:Ni atomic ratio is 1:1.Mixed liquor is placed in autoclave, and heat 42 hours at 120 DEG C in baking oven, then gained solution cool to room temperature adds 50mL n-hexane, ultrasonic 3 hours and control bath temperature and be no more than 30 DEG C.Then the colloidal sol of above-mentioned high degree of dispersion is added drop-wise in 40.0mg conductive black solution in the mode of back titration, stirs 48 hours, static filtration, use deionized water and ethanol alternately to clean to products obtained therefrom, be finally placed in vacuum drying oven drying 6 hours at 60 DEG C.Products obtained therefrom oxidation former (ORR) activity is about 0.7A/mg.
Embodiment 4: take acetylacetone,2,4-pentanedione platinum 117.9mg, nickel acetylacetonate 25.7mg, puts into 50mL DMF and fully dissolves, and wherein Pt:Ni atomic ratio is 3:1.Mixed liquor is placed in autoclave, heat 42 hours at 120 DEG C in baking oven, then gained solution cool to room temperature adds 50mL n-hexane, ultrasonic 3 hours and control bath temperature and be no more than 30 DEG C, then the colloidal sol of above-mentioned high degree of dispersion is added drop-wise in 64.9mg conductive black solution in the mode of back titration, stirs 48 hours, static filtration, use deionized water and ethanol alternately to clean to products obtained therefrom, be finally placed in vacuum drying oven drying 6 hours at 60 DEG C.Products obtained therefrom oxidation former (ORR) activity is about 0.20A/mg.
Claims (7)
1. the preparation method of the octahedra Proton Exchange Membrane Fuel Cells oxygen reduction catalyst of PtNi (111) nano crystal, it is characterized in that: select acetylacetone,2,4-pentanedione platinum and nickel acetylacetonate to be slaine presoma, with N, dinethylformamide and DMF are solvent, obtain the octahedra nano particle of PtNi (111) monocrystalline by heat reduction, then ultrasonic disperse loads on high-specific surface area conductive black carrier and obtains super-active catalyst of fuel batter with proton exchange film.
2. by the preparation method of the octahedra Proton Exchange Membrane Fuel Cells oxygen reduction catalyst of PtNi according to claim 1 (111) nano crystal, it is characterized in that: make described slaine presoma utilize solvent thermal reaction to prepare the octahedra Nano sol of PtNi (111) monocrystalline at a certain temperature.
3. by the preparation method of the octahedra Proton Exchange Membrane Fuel Cells oxygen reduction catalyst of PtNi according to claim 1 (111) nano crystal, it is characterized in that: the atomic ratio selecting Pt and Ni is 1:1,1:2,1:3 or 3:1.
4. by the preparation method of the octahedra Proton Exchange Membrane Fuel Cells oxygen reduction catalyst of PtNi according to claim 1 (111) nano crystal, it is characterized in that: select N, dinethylformamide is monocrystalline octahedral crystal face growth directed agents and reducing agent, and the volume ratio of Pt salt and the total acetylacetone based amount of substance of Ni salt and DMF is 0.4mmol:50ml.
5., by the preparation method of the octahedra Proton Exchange Membrane Fuel Cells oxygen reduction catalyst of PtNi according to claim 1 (111) nano crystal, it is characterized in that: when in catalyst, the mass ratio of platinum content is 30%.
6. by the preparation method of the octahedra Proton Exchange Membrane Fuel Cells oxygen reduction catalyst of PtNi according to claim 2 (111) nano crystal, it is characterized in that: using a certain amount of n-hexane as dispersant, join in the Nano sol of acquisition after ultrasonic 3 hours, then by the mode of back titration scattered colloidal sol slowly dripped and load on the carbon black-supported of high-specific surface area.
7. a preparation method for the octahedra Proton Exchange Membrane Fuel Cells oxygen reduction catalyst of PtNi (111) nano crystal, is characterized in that concrete steps are:
The first step: the configuration of precursor solution:
Get a certain amount of N, dinethylformamide is solvent, add 2mmol/L acetylacetone,2,4-pentanedione platinum and 6mmol/L nickel acetylacetonate, ensure that acetylacetone based amount is 0.4mmol:50ml with the ratio of the amount of DMF, then be uniformly mixed, by in the autoclave of above-mentioned mixed liquor impouring glass-lined, sealed by nut;
Second step: the octahedra nano particle synthesis of monocrystalline:
The reactor of above-mentioned sealing is inserted in vacuum drying oven temperature, smokes and make vacuum reach 0.8Mpa, be heated to 120 DEG C with the speed of 10 DEG C/min, and keep this temperature about 42 hours;
3rd step: catalyst preparing:
Take out reactor and be cooled to normal temperature in a water bath immediately, then in colloidal sol, a certain amount of n-hexane ultrasonic disperse is added 3 hours, obtain grey black sol solution, then will slowly be added drop-wise on conductive black carrier in scattered colloidal sol by the mode of back titration, stir and spend the night about 24 hours;
4th step: washing dry run:
Above-mentioned system vacuum filtration is removed water, and replace washing 8 ~ 10 times by ethanol and deionized water, then dry at 80 DEG C in vacuum drying chamber, obtain platinum load capacity weight ratio be 30% charcoal carry PtNi (111) monocrystalline octahedra bimetallic Proton Exchange Membrane Fuel Cells oxygen reduction catalyst.
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