CN109494378A - A kind of preparation method of the catalyst for catalytic fuel cell cathode reaction - Google Patents

A kind of preparation method of the catalyst for catalytic fuel cell cathode reaction Download PDF

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CN109494378A
CN109494378A CN201811515305.0A CN201811515305A CN109494378A CN 109494378 A CN109494378 A CN 109494378A CN 201811515305 A CN201811515305 A CN 201811515305A CN 109494378 A CN109494378 A CN 109494378A
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catalyst
fuel cell
cell cathode
preparation
cathode reaction
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CN109494378B (en
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崔凤娟
邓庆芳
徐蕾
王环宇
赵桦萍
王政军
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Qiqihar 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
    • H01M4/9008—Organic or organo-metallic compounds
    • 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
    • H01M4/8878—Treatment steps after deposition of the catalytic active composition or after shaping of the electrode being free-standing body
    • H01M4/8882—Heat treatment, e.g. drying, baking
    • 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
    • H01M8/08—Fuel cells with aqueous electrolytes
    • H01M8/083—Alkaline fuel cells
    • 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
    • H01M2004/8678—Inert electrodes with catalytic activity, e.g. for fuel cells characterised by the polarity
    • H01M2004/8684—Negative electrodes
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M2300/00—Electrolytes
    • H01M2300/0002—Aqueous electrolytes
    • H01M2300/0014—Alkaline electrolytes
    • 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)
  • Manufacturing & Machinery (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Materials Engineering (AREA)
  • Sustainable Development (AREA)
  • Sustainable Energy (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Catalysts (AREA)

Abstract

A kind of preparation method of the catalyst for catalytic fuel cell cathode reaction, belongs to carbon material preparation technical field.The method is as follows: at room temperature, ionic liquid and melamine are mixed according to certain mass ratio, grinding is uniform, then it places it in tube furnace, it under argon atmosphere, is warming up to 550 DEG C and keeps 3h, then after being warming up to 900 DEG C and calcining 2h, cooled to room temperature is to get the catalyst arrived for catalytic fuel cell cathode reaction.The invention has the advantages that the method for the present invention Heteroatom doping carbon material easy to operate, at low cost, being prepared is used in fuel battery cathod catalyst material.Method of the invention is easy to implement, and experiment instrument is simple.With melamine for the source C and N, ionic liquid BmimPF6For P, F hetero atom source is prepared for N by calcination reaction, and P, F- tri- adulterates carbon material, and as non-metallic cathode oxygen reduction catalyst.

Description

A kind of preparation method of the catalyst for catalytic fuel cell cathode reaction
Technical field
The invention belongs to carbon material preparation technical fields, and in particular to a kind of urging for catalytic fuel cell cathode reaction The preparation method of agent.
Background technique
Fossil fuel also brings environmental pollution and the energy while economy for bringing human prosperity is with efficiently living Crisis, in order to pursue clean new energy, fuel cell is considered as environmentally protective low emission and is most possibly to replace in this century For depleted one of the energy technology of fossil fuel.However, fuel cell core reaction-O2On cathod catalyst Oxygen reduction reaction (ORR) dynamic process is very slow, needs to occur quickly in the case where effective catalyst is catalyzed.Currently, The highest ORR elctro-catalyst of activity be still it is expensive, reserves are limited, the Pt series catalysts of selectivity and stability difference, cause Fuel cell is not widely used yet so far.Therefore it is urged for novel ORR electricity efficient, stable, inexpensive, that selectivity is good The research and development of agent have very important effect to promotion commercializing fuel cells.
Summary of the invention
It is at high cost, unstable, selective and steady that the purpose of the present invention is to solve current fuel battery cathod catalysts The problem of qualitative difference provides a kind of preparation method of catalyst for catalytic fuel cell cathode reaction.
To achieve the above object, the technical solution adopted by the present invention is as follows:
A kind of preparation method of the catalyst for catalytic fuel cell cathode reaction, the method specific steps are such as Under:
At room temperature, ionic liquid and melamine are mixed according to the mass ratio of 0.3~2.0:1, grinding uniformly, then will It is placed in tube furnace, under argon atmosphere, is warming up to 550 DEG C and keeps 3h, then after being warming up to 900 DEG C and calcining 2h, natural It is cooled to room temperature to get the catalyst for catalytic fuel cell cathode reaction is arrived.
The beneficial effect of the present invention compared with the existing technology is: the method for the present invention is easy to operate, it is at low cost, be prepared Heteroatom doping carbon material is in fuel battery cathod catalyst material.Method of the invention is easy to implement, tests instrument used Device is simple.With melamine for the source C and N, ionic liquid Bmim PF6For P, F hetero atom source is prepared for N by calcination reaction, P, F- tri- adulterates carbon material, and as non-metallic cathode oxygen reduction catalyst.Its pattern and structure are aobvious by scanning electron Micro mirror, transmission electron microscope and X-ray diffraction technology are characterized, and are investigated by linear voltammetric scan method and chronoamperometry Hydrogen reduction catalytic performance under its alkaline condition, and be compared with business Pt/C catalyst, by verifying it to cathodic oxygen reduction Reaction shows more high catalytic activity, more high stability, higher methanol tolerant.In the preparation of doping type carbon material and fuel cell electricity Catalytic field has important value and significance.
Detailed description of the invention
Fig. 1 is CM1.5- 900 XRD spectra；
Fig. 2 is CM1.5The full peak spectrogram of -900 XPS；
Fig. 3 is CM1.5- 900 SEM figure；
Fig. 4 is CM1.5- 900 TEM figure；
Fig. 5 is respectively in saturation N2And O20.1M KOH and O2ORR cyclic voltammetric polarization curve in/METHANOL MEDIUM Figure；
Fig. 6 is CM1.5The stability comparison diagram of -900 and Pt/C catalyst；
Fig. 7 is CM under different rotating speeds1.5The ORR polarization curve of -900 modification rotating disk electrode (r.d.e) RDE；
Fig. 8 is CM1.5Koutevky-Levich polarization curve under -900 different potentials.
Specific embodiment
Further description of the technical solution of the present invention with reference to the accompanying drawings and examples, and however, it is not limited to this, All to be modified to technical solution of the present invention or equivalent replacement, range without departing from the spirit of the technical scheme of the invention should all Cover within the protection scope of the present invention.
Heteroatom doping carbon material itself has certain hydrogen reduction performance and can be used as non-metallic catalyst, heteroatomic Incorporation increases active site, improves electro catalytic activity.Heteroatom doping carbon material has price low as ORR catalyst The characteristics of honest and clean, stability is high and methanol tolerance function admirable.Ionic liquid is the liquid being composed entirely of ions, in room temperature or room The substance being made of ion being in a liquid state at warm temperature nearby, due to its good stability and its insignificant volatility and Its entire carbonisation is very simple, therefore is widely used in the synthesis field of carbon material at present, mixes at the same time as hetero atom Miscellaneous raw material is modified carbon material surface and effectively improves carbon material performance.
The reaction that cathode occurs in a fuel cell is: 1/2O2+2H++2e----H2O；Alkaline fuel cell is electricity with KOH Xie Zhi, oxygen are oxidant, condition of nitrogen gas lower electrode surface covering catalyst non-oxidation process；Methanol: using methanol as anode In fuel cell, methanol can be through diaphragm from anode diffusion to cathode, and oxidation reaction occurs on cathod catalyst, generation Intermediate particulate CO is easy to make catalyst poisoning, can reduce the activity and stability of catalyst, to influence fuel cell entirety Performance and efficiency.
Specific embodiment 1: present embodiment record is a kind of catalyst for catalytic fuel cell cathode reaction Preparation method, specific step is as follows for the method:
At room temperature, ionic liquid and melamine are mixed according to the mass ratio of 0.3~2.0:1, is placed in agate mortar Grinding uniformly, is then placed it in aluminium oxide porcelain boat, is put into tube furnace, under argon atmosphere, be warming up to 550 DEG C and keep 3h, then after being warming up to 900 DEG C and calcining 2h, cooled to room temperature is to get to urging for catalytic fuel cell cathode reaction Agent is expressed as CMx- 900 (mass ratio of x=ILs/MA, conventional expression of the ILs for document used in this field herein, meanings Calcination temperature is indicated for ionic liquid, 900, CM represents carbon material).Melamine is as carbon and nitrogen in the present invention It simultaneously plays a supporting role in source.
Specific embodiment 2: a kind of catalysis for catalytic fuel cell cathode reaction described in specific embodiment one The preparation method of agent, the ionic liquid are 1- normal-butyl -3- methylimidazole hexafluorophosphate (Bmim PF6), with ionic liquid Body is as P, F hetero atom source.
Specific embodiment 3: a kind of catalysis for catalytic fuel cell cathode reaction described in specific embodiment one The preparation method of agent, heating is is warming up to 550 DEG C from room temperature with the heating rate of 5 DEG C/min for the first time, second of heating rate For 10 DEG C/min.
Embodiment 1:
A kind of preparation method of the catalyst for catalytic fuel cell cathode reaction, the method specific steps are such as Under:
At room temperature, ionic liquid and melamine are mixed according to the mass ratio of 1.5:1, is placed in agate mortar and grinds It is even, it then places it in aluminium oxide porcelain boat, is put into tube furnace, under argon atmosphere, from room temperature with the heating speed of 5 DEG C/min Rate is warming up to 550 DEG C and keeps 3h, then after being warming up to 900 DEG C with the heating rate of 10 DEG C/min and calcined 2h, naturally cools to Room temperature is expressed as CM to get to the catalyst for catalytic fuel cell cathode reactionx- 900 (mass ratio of x=ILs/MA, ILs herein is the conventional expression of document used in this field, and meaning is ionic liquid).The ionic liquid is 1- normal-butyl- 3- methylimidazole hexafluorophosphate (Bmim PF6), using ionic liquid as P, F hetero atom source.Melamine is as carbon and nitrogen source And it plays a supporting role.
X-ray diffraction technology, transmission electron microscope, scanning electron microscopy are carried out to the product that the present embodiment is prepared Mirror and X-ray photoelectron spectroscopic analysis are characterized.Characterization result is as follows:
As can be seen from Figure 1 CM1.5- 900 there is diffraction maximum 2 θ=23 ° and 42.6 °, correspond respectively to carbon-based (002) and (101) crystal face, the two diffraction maximums are to moving to left compared with graphene, this is because the heteroatomic electronegativity of doping It is bigger than the electronegativity of carbon, cause crystalline structure to deform, active site increases the increase of lamellar structure disordering, forms unordered crystalline substance State carbon causes part lattice deformability crystallinity relatively low, and the catalytic activity ratio of the structure of this pattern is free of heteroatomic catalysis Activity wants high.
As shown in Figure 3 and Figure 4, by scanning electron microscope and transmission electron microscope, it can be observed that CM1.5-900 Pattern have lamellate structure, and there is the unordered fold of multilayer to stack, the structure of this Disordered Layer is conducive to electronics Transmitting, by Fig. 3 it can be observed that its pattern is unordered folded laminar rather than block agglomerated together after high-temperature calcination Shape material, such pattern can be such that active site increases, and be conducive to the utilization rate for improving bioactive molecule.
Learnt by current progress, to catalytic activity play a key effect be increase active site.Miscellaneous original The introducing of son is conducive to increasing for active site, electro catalytic activity is improved, by Fig. 2, it can be observed that CM1.5It is each in -900 The distribution situation of element, CM1.5- 900 are mainly made of five kinds of elements of C, O, N, P, F, and peak position is 284.8eV respectively (C1s)、398.7eV(N1s)、531.4eV(O1s)、134.1eV(P2p)、684.7eV(F1s)。
Catalyst prepared by the present invention is dispersed in 0.5%nafion aqueous solution, concentration 5mg/mL, ultrasonic disperse 1 Hour, then take 6 microlitres of dispersant liquid drops on the glass-carbon electrode that diameter is 3mm, catalyst loadings 0.423mg/cm2, It is dry at room temperature to use.It is that 50mV/s measures CM to sweep speed using 0.1M KOH as electrolytic solution1.5The cyclic voltammetric of -900 materials (CV) oxygen reduction reaction catalytic activity of the curve to research material, such as CM in Fig. 51.5-900N2Corresponding curve can be seen Out, in N2CV curve does not show apparent redox peaks in the KOH solution of saturation；On the contrary, in O2The 0.1M KOH solution of saturation In, such as CM in Fig. 51.5-900O2It is shown, CM1.5Obviously occur on the CV curve of -900 materials spike potential -0.29V cathode also Parent peak shows CM1.5- 900 materials are to O2Reduction have certain catalytic capability.Methanol is added after oxygen saturation, obtains Curve corresponds to the CM in Fig. 51.5- 900MeOH, it can be seen that this kind of catalyst has good methanol tolerance penetrating power.Fig. 7 The LSV curve for being material in 0.1M KOH solution under different rotating speeds, with the increase of revolving speed, limiting current density also increases therewith Greatly, this is because biggish revolving speed can shorten the diffusion length of reactant, the take-off potential of ORR working electrode is about -0.125V, Kinetic test shows that electron transfer number about 3.7 (Fig. 8) in the ORR of the catalyst, predominantly 4 electronics courses, nitrogen phosphorus fluorine are co-doped with Miscellaneous phase, which mutually acts synergistically, is conducive to the absorption of the mass transfer and oxygen of charge, has good anti-first after chrono-amperometric is tested The penetrating power of alcohol and higher stability (Fig. 5 and Fig. 6).
Embodiment 2:
BmimPF6The preparation of the CMx-900 material of/melamine different proportion (mass ratio):
2 grams of melamines are taken, the BmimPF that quality is 3 grams is added6It is constantly ground in agate mortar uniformly mixed Material, is put into tube furnace calcines after mixing by (30min), argon gas protection, argon gas flow velocity 100sscm, with 5 DEG C/min's Rate is warming up to 550 DEG C, keeps after calcining 3h at 550 DEG C, change argon gas flow velocity is 250sscm, then with the rate of 10 DEG C/min 900 DEG C are warming up to, keeps after calcining 2h at 900 DEG C, is cooled to room temperature, black product is collected and is ground, resulting material It is denoted as CM1.5-900。

Claims (3)

1. a kind of preparation method of the catalyst for catalytic fuel cell cathode reaction, it is characterised in that: the method tool Steps are as follows for body:
At room temperature, ionic liquid and melamine are mixed according to the mass ratio of 0.3~2.0:1, grinding uniformly, is then set It in tube furnace, under argon atmosphere, is warming up to 550 DEG C and keeps 3h, then after being warming up to 900 DEG C and calcining 2h, natural cooling To room temperature to get the catalyst arrived for catalytic fuel cell cathode reaction.
2. a kind of preparation method of catalyst for catalytic fuel cell cathode reaction according to claim 1, special Sign is: the ionic liquid is 1- normal-butyl -3- methylimidazole hexafluorophosphate.
3. a kind of preparation method of catalyst for catalytic fuel cell cathode reaction according to claim 1, special Sign is: heating for the first time to be warming up to 550 DEG C from room temperature with the heating rate of 5 DEG C/min, second of heating rate be 10 DEG C/ min。
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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115036519A (en) * 2022-07-04 2022-09-09 上海电气集团股份有限公司 Fluorine-doped porous carbon, microporous layer, gas diffusion layer, preparation method and application

Citations (5)

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Publication number Priority date Publication date Assignee Title
DE102006054737A1 (en) * 2006-11-21 2008-05-29 Volkswagen Ag Use of an ionic liquid based on fluorinated or partially fluorinated alkyl phosphorus/phosphine, phosphonic- or alkyl sulfonic-acid, or di- or triacid derivatives as an electrolyte to prepare fuel cell membrane or its electrode assemblies
CN101601151A (en) * 2007-02-08 2009-12-09 巴斯夫欧洲公司 The electrochemical element that contains melamine/formaldehyde foamed plastic
CN104525235A (en) * 2014-12-18 2015-04-22 华南理工大学 Nitrogen-doped graphene catalyst as well as preparation method and application thereof
CN106374117A (en) * 2016-11-25 2017-02-01 天津工业大学 Preparation of N and P co-doped nonmetallic oxygen reduction catalyst
CN107394215A (en) * 2017-07-14 2017-11-24 西北师范大学 A kind of preparation and application of the functional carbon material of Heteroatom doping

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE102006054737A1 (en) * 2006-11-21 2008-05-29 Volkswagen Ag Use of an ionic liquid based on fluorinated or partially fluorinated alkyl phosphorus/phosphine, phosphonic- or alkyl sulfonic-acid, or di- or triacid derivatives as an electrolyte to prepare fuel cell membrane or its electrode assemblies
CN101601151A (en) * 2007-02-08 2009-12-09 巴斯夫欧洲公司 The electrochemical element that contains melamine/formaldehyde foamed plastic
CN104525235A (en) * 2014-12-18 2015-04-22 华南理工大学 Nitrogen-doped graphene catalyst as well as preparation method and application thereof
CN106374117A (en) * 2016-11-25 2017-02-01 天津工业大学 Preparation of N and P co-doped nonmetallic oxygen reduction catalyst
CN107394215A (en) * 2017-07-14 2017-11-24 西北师范大学 A kind of preparation and application of the functional carbon material of Heteroatom doping

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115036519A (en) * 2022-07-04 2022-09-09 上海电气集团股份有限公司 Fluorine-doped porous carbon, microporous layer, gas diffusion layer, preparation method and application

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