CN111326741B - Membrane electrode containing ordered catalyst layer and preparation method and application thereof - Google Patents
Membrane electrode containing ordered catalyst layer and preparation method and application thereof Download PDFInfo
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- CN111326741B CN111326741B CN201811527778.2A CN201811527778A CN111326741B CN 111326741 B CN111326741 B CN 111326741B CN 201811527778 A CN201811527778 A CN 201811527778A CN 111326741 B CN111326741 B CN 111326741B
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- H—ELECTRICITY
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- 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
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- 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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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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
- H01M4/88—Processes of manufacture
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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
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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
- H01M8/00—Fuel cells; Manufacture thereof
- H01M8/10—Fuel cells with solid electrolytes
- H01M8/1004—Fuel cells with solid electrolytes characterised by membrane-electrode assemblies [MEA]
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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
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- 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 describes an ordered membrane electrode taking metal nitride/carbide as a carrier and preparation thereof, which comprises the construction of an ordered structure, the formation of the metal nitride/carbide and the assembly of the ordered electrode. First, a sacrificial support Co-OH-CO was prepared3The nanorod array is coated with a metal nitride/carbide layer with good conductivity and high stability; and then the catalyst is loaded on the surface of the metal nitride/carbide layer, and the newly formed structure is subjected to annealing, transfer printing, acid washing and other steps to form a nanotube array structure of the metal nitride/carbide layer @ catalyst, so that the metal nitride/carbide layer @ catalyst can be used for assembling a membrane electrode for a fuel cell. The membrane electrode structure constructed by the invention has the advantages of low catalyst usage amount and high utilization rate, and meanwhile, the carrier in the electrode is corrosion resistant, the electrode stability is high, and the ionic polymer is not required to be used as a proton conductor.
Description
Technical Field
The invention belongs to the field of fuel cells, and particularly relates to a preparation method and application of an ordered membrane electrode of a proton exchange membrane fuel cell.
Background
Proton Exchange Membrane Fuel Cells (PEMFCs) are environment-friendly energy conversion devices with high specific energy, and have been currently used in the fields of new energy vehicles, distributed power stations, aerospace, military industry, etc., but the cost and stability problems have been the short plates of fuel cells.
The membrane electrode is a core component of a fuel cell, a noble metal catalyst Pt used in the membrane electrode is a great source of high cost, and the catalyst Pt/C in the traditional membrane electrode is in a disordered state, the catalyst layer is thick, the utilization rate of the catalyst is low, and mass transfer polarization is large. In order to solve the problems, 3M company provides and constructs an ordered ultrathin membrane electrode (NSTF), a catalyst layer has no proton conductor, and the catalyst layer has the characteristics of microscopic order and excellent mass transfer, and can effectively improve the utilization rate of the catalyst. Therefore, ordered catalytic layers are one of the important directions for future development of fuel cells.
In addition to the 3M company, which uses nonconductive nanowhiskers as supports, metal oxides are also used as catalyst supports in ordered catalytic layers due to their good chemical and electrochemical stability. The article Chemusshem, 2013,6, 659-doped 666 was prepared as TiO2The nanotube array is an ordered electrode structure of a carrier, but poor conductivity is still a disturbing factor. In addition, conductive polymers are also used as carriers, and Polyaniline (PANI) arrays grown on carbon paper are used as carriers in the article Journal of Material Chemistry a, 2017(5), 15260-.
Carbon materials are also used as supports. In the Journal of Power Sources,2014(253) and 104-113, the carbon nanotube array is used as a carrier, and the Pt catalyst is impregnated and reduced and supported, so that the Pt catalyst shows good performance when being applied to a cathode of a proton exchange membrane fuel cell, but the process for preparing the carbon nanotube array by CVD is complex and has high requirements on experimental conditions.
Disclosure of Invention
Based on the above background technology, the invention uses Co-OH-CO3The nano-rod array is used as a sacrificial template, a metal nitride/carbide layer is constructed on the surface of the sacrificial template by adopting a physical vapor deposition technology and is used as a catalyst carrier, then a catalyst is carried on the surface of the sacrificial template, and an ordered electrode structure is formed by annealing or non-annealing treatment, transfer printing and acid washing. Metal nitrides/carbides themselves are often used to prepare metallic bipolar plate coatings for fuel cells due to their good electrical conductivity and chemical and electrochemical stability, and also to take advantage of these properties when used as catalyst supports. The electrode prepared by the invention has the advantages of low catalyst loading capacity, high catalyst utilization rate, good mass transfer, good catalyst layer stability and the like.
The invention aims to prepare a membrane electrode with ordered mass transfer and high catalyst utilization rate. The following technical scheme is adopted:
on one hand, the ordered catalyst layer with the membrane electrode is provided, the microstructure of the catalyst layer is a nano tube arranged in an array, and the inner layer of the tube wall of the nano tube is a carrier; the carrier is at least one of metal nitride or carbide, and the outer layer of the pipe wall is a catalyst; the catalyst is an oxygen reduction catalyst or a hydrogen oxidation catalyst.
Based on the technical scheme, preferably, the thickness of the ordered catalytic layer is 100nm-5 μm, the diameter of the nanotube is 50nm-500nm, the length of the nanotube is 500nm-8 μm, and the thickness of the nanotube wall is 2nm-200 nm.
Based on the technical scheme, preferably, the metal nitride is CrN, TiN, NbN, ZrN, VN, TaN, MoN or WN; the metal carbides CrC, TiC, NbC, ZrC, VC, TaC, MoC and WC; the thickness of the inner layer of the tube wall is 1nm-150nm, and the catalyst is at least one of Pd, Ag, Au, Pt, Ru, Rh, Ni, Co, Ir, Cu, Zn, Fe, Cr, V and Mn.
In another aspect, the present invention provides a method for preparing a membrane electrode comprising the above ordered catalytic layer, the method comprising the steps of:
(1) hydrothermal method for preparing Co-OH-CO vertical to substrate3A nanorod array;
(2) in the Co-OH-CO3The outer surface of the nano rod is deposited with a metal nitride or carbide layer as a carrier to form Co-OH-CO3@ metal nitride/carbide nanorod array structure;
(3) in the Co-OH-CO3The catalyst is supported on the outer surface of the @ metal nitride/carbide nanorod, and then the annealing treatment can be carried out or not carried out to form Co-OH-CO3@ metal nitride/carbide @ catalyst nanorod array structure;
(4) the Co-OH-CO prepared in the step (3)3@ metal nitride/carbide @ catalyst nanorod array is transferred to the proton exchange membrane or the side of the gas diffusion layer with the microporous layer, and the substrate is removed;
(5) and (3) carrying out acid cleaning treatment on the proton exchange membrane or the gas diffusion layer with the catalyst layer after transfer printing to obtain the membrane electrode containing the ordered catalyst layer.
Based on the technical scheme, preferably, Co-OH-CO is prepared by the hydrothermal method in the step (1)3The specific steps of the nanorod array are as follows: preparing a hydrothermal reaction solution, stirring for 10-60min, transferring to a hydrothermal kettle, putting the substrate in the hydrothermal kettle for hydrothermal reaction at 80-180 ℃ for 3-24h to obtain Co-OH-CO3A nanorod array; the hydrothermal reaction solution comprises the following components: co (NO)3)2·6H2O 1-100mmol L-1，NH4F 1-100mmol L-1，CO(NH2)2 1-100mmol L-1B, carrying out the following steps of; the substrate is a nickel sheet, a copper sheet, a stainless steel sheet, a titanium sheet, ceramics or glass.
Based on the above technical solution, preferably, the surface deposition method in step (2) is Physical Vapor Deposition (PVD); the catalyst loading mode in the step (3) is at least one of chemical reduction, electrodeposition, magnetron sputtering, evaporation, thermal decomposition or atomic deposition, and is calculated by the area of a membrane electrode; the loading amount of the catalyst is 1 mu g-10mg cm-2。
Based on the above technical solution, preferably, the step (3) is: in the Co-OH-CO3The catalyst is supported on the outer surface of the @ metal nitride/carbide nanorod, and then annealing treatment is carried out to form Co-OH-CO3@ metal nitride/carbide @ catalyst nanorod array structure; the annealing temperature is 100-1000 ℃, and the annealing time is 10min-48 h; annealing atmosphere is H2、N2Ar or He, said atmosphere containing H2When H is present2The content of (A) is 1 vol.% to 99 vol.%, and H2The flow rate is 10sccm to 200 sccm.
Based on the technical scheme, the transfer printing mode in the step (4) is preferably hot-press transfer printing, the transfer printing temperature is 20-200 ℃, the transfer printing pressure is 0.05-50 MPa, and the transfer printing time is 0.5-60 min.
Based on the technical scheme, preferably, the solution used in the acid washing in the step (5) is HCl or H2SO4、HNO3、HclO4The concentration of at least one of the solutions is 0.01M-5M, the pickling time is 1min-24h, and the pickling temperature is 20-90 ℃.
In another aspect, the invention provides an application of the membrane electrode comprising the ordered catalytic layer prepared by the method, wherein the membrane electrode is used for an anode and/or a cathode of a proton membrane fuel cell, and no ionic polymer is required to be added in the catalytic layer to serve as a proton conductor.
Advantageous effects
The membrane electrode containing the ordered catalyst layer prepared by the invention has the characteristics of low Pt loading capacity, high catalyst utilization rate and excellent mass transfer.
Drawings
FIG. 1 is a flow chart of the preparation of the ordered electrode of example 1.
FIG. 2 Co-OH-CO prepared in example 13Cross-sectional view of nanorod array.
Figure 3 is a graph of the I-V performance of the ordered electrode prepared in example 1 in a proton exchange membrane fuel cell.
FIG. 4 shows Co-OH-CO prepared in example 23Section view of @ TiN nanorod array.
FIG. 5 is a schematic view ofCo-OH-CO prepared in example 23@ TiN nanorod array top view.
FIG. 6 is a cross-sectional view of the ordered electrode catalyst layer after transfer and acid washing in example 2.
Figure 7 is a graph of the I-V performance of the ordered electrode prepared in example 2 in a proton exchange membrane fuel cell.
Detailed Description
The following examples further illustrate the invention
Example 1
Step 1: growing Co-OH-CO on the surface of the stainless steel sheet3A nanorod array. Reaction temperature 120 ℃, reaction solution: reaction solution: 20mM Co (NO)3)2·6H2O,20mM NH4F,40mM CO(NH2)2The array was 5 μm in length and 200-300nm in diameter.
Step 2: by physical vapor deposition on Co-OH-CO3And a CrN layer is deposited on the surface of the nanorod array and is used as a catalyst carrier. Physical vapor deposition adopts a multi-arc ion plating mode, the target material is a Cr target, and the ultimate vacuum pressure is 3 multiplied by 10- 3Pa, working pressure 0.8Pa, Ar gas flow rate 250sccm, N2The flow rate is 250sccm, the bias voltage is 100V, the focusing coil current is 0.4A, the arc coil current is 1A, the working current is 50A, and the time is 15 min. To obtain Co-OH-CO3@ CrN nanorod array.
And step 3: in the presence of Co-OH-CO3The surface of the @ CrN nanorod array adopts a physical vapor deposition method to load a catalyst Pt. The mode of physical vapor deposition adopts a magnetron sputtering mode, and the ultimate vacuum pressure is 3.8 multiplied by 10-3Pa, working pressure of 0.8Pa, power of 120W, Ar gas flow of 400sccm, and time of 15 min. And carrying out annealing treatment on the array at 400 ℃ in an atmosphere of 5% H2/Ar for 1H.
And 4, step 4: and (4) transferring and acid washing. Transferring the array with the catalyst to a Nafion211 membrane with the transfer pressure of 4MPa, and pickling to obtain an ordered catalyst layer with 0.5mol L acid solution-1Sulfuric acid solution as cathode. The anode used commercial GDE (0.1 mg)Pt/cm2) Application to proton exchange membrane fuel cellsIn (1). Battery operating temperature: 80 ℃; h2Flow 50mL min-1；O2Flow 100mL min-1，PH2/PO2＝2bar/2bar。
FIG. 2 Co-OH-CO prepared in example 13The cross section of the nanorod array is shown, and the length of the nanorods is 4 mu m; FIG. 3 is a graph of I-V performance of the ordered electrode prepared in example 1 in a PEM fuel cell, as seen at H2-O2Under the condition, the maximum power density is 360mW cm-2。
Example 2
Step 1: growing Co-OH-CO on the surface of the stainless steel sheet3A nanorod array. Reaction temperature 120 ℃, reaction solution: reaction solution: 20mM Co (NO)3)2·6H2O,20mM NH4F,40mM CO(NH2)2The array was 5 μm in length and 200-300nm in diameter.
Step 2: by physical vapor deposition on Co-OH-CO3And a layer of TiC is deposited on the surface of the nanorod array and is used as a catalyst carrier. Physical vapor deposition adopts a multi-arc ion plating mode, the target materials are Ti target and C target, and the ultimate vacuum pressure is 3 multiplied by 10-3Pa, working pressure 0.8Pa, Ar gas flow rate 250sccm, N2The flow rate is 250sccm, the bias voltage is 100V, the focusing coil current is 0.4A, the arc coil current is 1A, the working current is 50A, and the time is 15 min. To obtain Co-OH-CO3@ TiC nanorod array.
And step 3: in the presence of Co-OH-CO3The surface of the @ TiC nanorod array adopts a physical vapor deposition method to load a catalyst Pt. The mode of physical vapor deposition adopts a magnetron sputtering mode, and the ultimate vacuum pressure is 3.8 multiplied by 10-3Pa, working pressure of 0.8Pa, power of 120W, Ar gas flow of 400sccm, and time of 15 min.
And 4, step 4: and (4) transferring and acid washing. Transferring the array with the catalyst to a Nafion211 membrane with the transfer pressure of 4MPa, and pickling to obtain an ordered catalyst layer with 0.5mol L acid solution-1Sulfuric acid solution as cathode. The anode used commercial GDE (0.1 mg)Pt/cm2) The method is applied to proton exchange membrane fuel cells. Battery operationWorking temperature: 80 ℃; h2Flow 50mL min-1；O2Flow 100mL min-1，PH2/PO22bar/2 bar. FIG. 4 shows Co-OH-CO prepared in example 23The section view of the @ TiN nanorod array can show that the diameter of the nanorod is 4 mu m; FIG. 5 shows Co-OH-CO prepared in example 23The top view of the @ TiN nanorod array shows that the diameter of the nanorod is 200nm and 300 nm; FIG. 6 is a cross-sectional view of the ordered electrode catalyst layer after transfer and acid washing in example 2, wherein the catalyst layer is about 800nm thick; FIG. 7 is a graph of I-V performance of the ordered electrode prepared in example 2 in a PEM fuel cell showing a maximum power density of 470mW cm-2。
Claims (9)
1. A preparation method of a membrane electrode comprising an ordered catalytic layer is characterized in that,
the microstructure of the catalyst layer is a nanotube arranged in an array, the inner layer of the tube wall of the nanotube is at least one of metal nitride or metal carbide, and the outer layer of the tube wall is a catalyst; the catalyst is an oxygen reduction catalyst or a hydrogen oxidation catalyst;
the method comprises the following steps:
(1) hydrothermal method for preparing Co-OH-CO vertical to substrate3A nanorod array;
(2) in the Co-OH-CO3Depositing metal nitride or carbide on the outer surface of the nano rod to form Co-OH-CO3@ metal nitride/carbide nanorod array structure;
(3) in the Co-OH-CO3The catalyst is supported on the outer surface of the @ metal nitride/carbide nanorod to form Co-OH-CO3@ metal nitride/carbide @ catalyst nanorod array structure;
(4) the Co-OH-CO prepared in the step (3)3@ metal nitride/carbide @ catalyst nanorod array is transferred to the proton exchange membrane or the side of the gas diffusion layer with the microporous layer, and the substrate is removed;
(5) acid cleaning treatment is carried out on the proton exchange membrane or the gas diffusion layer with the catalyst layer after transfer printing, and the membrane electrode containing the ordered catalyst layer is obtained;
the step (3) is as follows: in the Co-OH-CO3The catalyst is supported on the outer surface of the @ metal nitride/carbide nanorod, and then annealing treatment is carried out to form Co-OH-CO3@ metal nitride/carbide @ catalyst nanorod array structure; the annealing temperature is 100-1000 ℃, and the annealing time is 10min-48 h.
2. The method of claim 1 comprising the preparation of a sequenced membrane electrode, wherein: the thickness of the ordered catalytic layer is 100nm-5 μm, the diameter of the nanotube is 50nm-500nm, the length of the nanotube is 500nm-8 μm, and the thickness of the nanotube wall is 2nm-200 nm.
3. The method of claim 1, wherein the metal nitride is CrN, TiN, NbN, ZrN, VN, TaN, MoN, WN; the metal carbides CrC, TiC, NbC, ZrC, VC, TaC, MoC and WC; the thickness of the inner layer of the tube wall is 1nm-150nm, and the catalyst is at least one of Pd, Ag, Au, Pt, Ru, Rh, Ni, Co, Ir, Cu, Zn, Fe, Cr, V and Mn.
4. The method of claim 1 comprising the preparation of a sequenced membrane electrode, wherein: the hydrothermal method for preparing Co-OH-CO in step (1)3The specific steps of the nanorod array are as follows: preparing a hydrothermal reaction solution, stirring for 10-60min, transferring to a hydrothermal kettle, putting the substrate in the hydrothermal kettle for hydrothermal reaction at 80-180 ℃ for 3-24h to obtain Co-OH-CO3A nanorod array; the hydrothermal reaction solution comprises the following components: co (NO)3)2·6H2O 1-100mmol L-1，NH4F 1-100mmol L-1，CO(NH2)2 1-100mmol L-1(ii) a The substrate is a nickel sheet, a copper sheet, a stainless steel sheet, a titanium sheet, ceramics or glass.
5. According to claimThe method for preparing a membrane electrode comprising a sequence according to claim 1, wherein: the surface deposition method in the step (2) is Physical Vapor Deposition (PVD); the catalyst supporting mode in the step (3) is at least one of chemical reduction, electrodeposition, magnetron sputtering, evaporation, thermal decomposition or atomic deposition; the loading amount of the catalyst is 1 mu g-10mg cm-2。
6. The method of claim 1 wherein the annealing atmosphere is H2、N2Ar or He, said atmosphere containing H2When H is present2The content of (A) is 1 vol.% to 99 vol.%, and H2The flow rate is 10sccm to 200 sccm.
7. The method of claim 1 comprising the preparation of a sequenced membrane electrode, wherein: the transfer printing mode in the step (4) is hot-pressing transfer printing, the transfer printing temperature is 20-200 ℃, the transfer printing pressure is 0.05-50 MPa, and the transfer printing time is 0.5-60 min.
8. The method of claim 1 comprising the preparation of a sequenced membrane electrode, wherein: the solution used in the acid washing in the step (5) is HCl and H2SO4、HNO3、HClO4The concentration of at least one of the solutions is 0.01M-5M, the pickling time is 1min-24h, and the pickling temperature is 20-90 ℃.
9. The use of a membrane electrode comprising ordered catalytic layers prepared by the preparation method of claim 1, wherein: the membrane electrode is used for an anode and/or a cathode of a proton membrane fuel cell.
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