CN111276705A - Preparation method of metal-supported oxide fuel cell half cell - Google Patents

Preparation method of metal-supported oxide fuel cell half cell Download PDF

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CN111276705A
CN111276705A CN202010009980.7A CN202010009980A CN111276705A CN 111276705 A CN111276705 A CN 111276705A CN 202010009980 A CN202010009980 A CN 202010009980A CN 111276705 A CN111276705 A CN 111276705A
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ysz
metal
nio
substrate
support
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CN111276705B (en
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朱腾龙
倪维婕
马卫华
钟秦
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Nanjing University of Science and Technology
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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
    • H01M4/8803—Supports for the deposition of the catalytic active composition
    • 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
    • H01M4/8647—Inert electrodes with catalytic activity, e.g. for fuel cells consisting of more than one material, e.g. consisting of composites
    • H01M4/8657—Inert electrodes with catalytic activity, e.g. for fuel cells consisting of more than one material, e.g. consisting of composites layered
    • 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
    • H01M8/12—Fuel cells with solid electrolytes operating at high temperature, e.g. with stabilised ZrO2 electrolyte
    • H01M8/1213—Fuel cells with solid electrolytes operating at high temperature, e.g. with stabilised ZrO2 electrolyte characterised by the electrode/electrolyte combination or the supporting material
    • 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
    • H01M8/00—Fuel cells; Manufacture thereof
    • H01M8/10—Fuel cells with solid electrolytes
    • H01M8/12—Fuel cells with solid electrolytes operating at high temperature, e.g. with stabilised ZrO2 electrolyte
    • H01M2008/1293—Fuel cells with solid oxide electrolytes
    • 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
    • H01M2300/0017—Non-aqueous electrolytes
    • H01M2300/0065—Solid electrolytes
    • H01M2300/0068—Solid electrolytes inorganic
    • H01M2300/0071—Oxides
    • 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 Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Manufacturing & Machinery (AREA)
  • Composite Materials (AREA)
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Abstract

The invention discloses a preparation method of a metal-supported oxide fuel cell half cell. The metal support type solid oxide fuel cell half cell has a Ni-Fe I Ni-YSZ I YSZ structure, adopts NiO and Fe2O3The powder is used as raw material, and is sintered at high temperature in the air after being formed to prepare Fe2O3-a NiO metal oxide support matrix; then preparing a NiO-YSZ anode layer on the substrate, and calcining in air; then reducing at high temperature in a reducing atmosphere to obtain a Ni-Fe metal support body and a Ni-YSZ anode, and realizing synchronous shrinkage of the substrate and the anode; and finally, depositing YSZ electrolyte on the surface of the Ni-YSZ, and calcining at 1250 +/-10 ℃ in a reducing atmosphere to realize synchronous shrinkage of the matrix and the electrolyte, thereby obtaining the compact YSZ electrolyte and the high-strength and flat metal support half cell.

Description

Preparation method of metal-supported oxide fuel cell half cell
Technical Field
The invention belongs to the technical field of fuel cells, and relates to a preparation method of a metal support type oxide fuel cell half cell.
Background
The fuel cell is an electrochemical power generation device which directly converts chemical energy in fuel into electric energy with high efficiency and environmental friendliness, and compared with the traditional power generation and power supply technology, the fuel cell has very obvious advantages in the aspects of power generation efficiency (45-60%), noise control and vehicle endurance mileage. The Solid Oxide Fuel Cell (SOFC) works at high temperature (600-1000 ℃) and can directly adopt various fuels such as hydrogen, synthetic gas, natural gas, liquefied petroleum gas, methanol, ethanol and the like to efficiently generate electricity. The SOFC adopts all-solid-state and modular design, and has wide application prospect in the fields of small-sized portable power supplies, vehicle extended-range power supplies, household combined heat and power supplies, distributed power generation systems and the like.
The preparation of single cells with high performance and high stability is an important foundation for realizing the construction of the SOFC cell stack and the integration of a power generation system. The traditional SOFC single cell with ceramic base has the defects of low strength, difficult sealing, high cost and the like, and the commercialization process of the SOFC is seriously hindered. The metal material is used as the support body of the SOFC single cell, so that the cost can be reduced, the rapid start and the efficient packaging can be realized, the mechanical strength of the single cell can be obviously improved, and the high-performance operation at medium and low temperature (600-800 ℃) can be expected to be realized. Therefore, metal supported solid oxide fuel cells (MS-SOFCs) are currently the heat generation point of research.
The metal support battery generally adopts a structure of a metal support anode electrolyte cathode, the support material comprises 300/400 series stainless steel, hastelloy alloy, Ni-Fe alloy and the like, the electrolyte generally comprises YSZ (yttria-stabilized zirconia) and GDC/SDC (gadolinium oxide/samarium oxide-doped cerium oxide), and the anode generally adopts Ni-YSZ/GDC metal ceramic composite material. Because the metal support body can not be calcined at high temperature in the air atmosphere, the MS-SOFC single cell still faces technical bottlenecks of complex preparation process, higher cost and the like. At present, the mismatch of sintering shrinkage between a metal support and an oxide ceramic electrolyte is a major challenge in the development of a metal-supported single cell, and the following approaches are available for preparing a metal-supported SOFC dense electrolyte:
(1) the advanced film forming process includes the first preparation of metal support and the subsequent preparation of dense electrolyte through chemical deposition, electrochemical deposition and other steps. The metal support has the advantages of high strength, good forming and high flatness; the disadvantages are complex technical process, high cost and low production efficiency (packer M C. progress in metal-supported solid oxide fuels: A review [ J ]. Journal of Power Sources,2010,195(15): 4570-4582.).
(2) In the traditional wet ceramic process, oxide powder of a support body and electrolyte are co-sintered in an oxidizing atmosphere, and then the oxide support body is reduced into metal. However, during the reduction process, the metal oxide support has a large shrinkage deformation, which leads to battery deformation and electrolyte cracking (Cho H J, KimK J, Park Y M, et al. Flexibesolid oxide cells supported on thin and porous metal [ J ]. International journal of Hydrogen Energy,2016,41(22): 9577-.
(3) In the traditional wet ceramic process, the metal powder of the support body and the electrolyte are sintered together in a reducing atmosphere. However, the high-Temperature calcination shrinkage of the metal support in a reducing atmosphere is much higher than that of the electrolyte, resulting in deformation of the battery, cracking and peeling of the electrolyte, and scale-up of the production is difficult to achieve (y.zhou, h.wu, t.luo, et al., a Nanostructured Architecture for reduced-Temperature Oxide Fuel Cells [ J ]. Advanced Energy Materials,2015,5 (11)).
Therefore, the development of low cost and easy to implement electrolyte densification processes is an important direction of current stage MS-SOFC research.
Disclosure of Invention
In order to solve the problem that the shrinkage of the conventional metal support and oxide ceramic electrolyte is not matched in the co-sintering and reducing processes, the invention provides a preparation method of a metal support type oxide fuel cell half cell.
The technical scheme of the invention is as follows:
the preparation method of the metal support type oxide fuel cell half cell comprises the following specific steps:
(1) preparing a metal oxide substrate: mixing Fe2O3Mixing with NiO powder according to the molar ratio of 1:1 to prepare the formed Fe2O3Pre-firing the NiO substrate for 1-5 hours at 1100-1200 ℃ in an air atmosphere to obtain a metal oxide support body matrix;
(2) depositing the NiO-YSZ suspension or slurry on the surface of the metal oxide support body substrate, and firing for 1-5 hours in an air atmosphere at 1100-1200 ℃ to obtain an oxide support body;
(3) subjecting the oxide support to 10% H in a reducing atmosphere2Preserving the heat for 1-5 hours at 800-900 ℃ under 90% of Ar to obtain a reduced Ni-Fe support body and a Ni-YSZ anode;
(4) depositing a YSZ suspension or slurry on the surface of the reduced metal support at 3% H2Sintering the substrate and the electrolyte for 2 to 5 hours at 1250 +/-10 ℃ in a protective atmosphere of-97% Ar to realize synchronous shrinkage of the substrate and the electrolyte, and obtaining the metal-supported solid oxide fuel cell half cell.
In step (1) of the present invention, Fe2O3Shaping of the-NiO substrate Using methods conventionally used in the art, e.g. shaping Fe by dry pressing, casting or slip casting2O3-a NiO substrate.
In step (2) of the present invention, the NiO-YSZ suspension or slurry is deposited on the surface of the metal oxide support substrate by a method conventionally used in the art, for example, by dropping or screen printing or spraying the NiO-YSZ suspension or slurry on the surface of the fired metal support.
In step (4) of the present invention, the YSZ suspension or slurry is deposited on the surface of the reduced metal support by a method conventionally used in the art, for example, by dropping or screen printing or spraying the YSZ suspension or slurry on the surface of the reduced metal support.
Compared with the prior art, the invention has the following advantages:
(1) the metal oxide is adopted as precursor powder, so that the production process flow is simple and the cost is low; after preparing a NiO-YSZ anode layer on a metal oxide substrate, co-sintering in a reducing atmosphere to obtain a flat and high-strength support; meanwhile, the support body shrinks for the first time, so that the shrinkage rate of the support body under high-temperature sintering is adjusted, and the contact combination of the metal layer and the anode layer is promoted.
(2) Preparing YSZ electrolyte on the support body which is reduced and contracted for the first time, calcining at 1250 +/-10 ℃ under protective atmosphere to realize synchronous contraction of the support body and the electrolyte, obtaining the metal support type solid oxide fuel cell half cell with the Ni-Fe | Ni-YSZ | YSZ structure and high strength and high flatness, and obtaining compact electrolyte at lower sintering temperature.
Drawings
Fig. 1 is a schematic diagram of a process for preparing a metal-supported oxide fuel cell half cell of the present invention.
FIG. 2 is a sectional scanning electron micrograph of a half cell of example 1.
FIG. 3 is a partially enlarged SEM image of an electrolyte in example 1.
FIG. 4 is a sectional scanning electron micrograph of a half cell of comparative example 1.
Detailed Description
The present invention will be described in more detail with reference to the following examples and the accompanying drawings.
Example 1
The structure of the metal-supported oxide fuel cell half cell of the present invention comprises: the preparation method comprises the following steps of preparing a porous Ni-Fe alloy support layer, a microporous Ni-8YSZ anode functional layer and a compact 8YSZ electrolyte layer:
(1) mixing Fe2O3And NiO powder were weighed in a molar ratio of 1:1, and graphite in an amount of 10% by mass was added thereto, followed by ball-milling and mixing at a speed of 300 revolutions per minute for 24 hours. The dried powder was pressed into small round pieces of 19mm in diameter, each about 0.8g of powder, by a tablet press, and held at a pressure of 300MPa for 1 minute. Then pre-firing at 1100 ℃ in an air atmosphere, and preserving heat for 2 hours to obtain a metal oxide support substrate;
(2) preparing NiO-YSZ suspension with the mass fraction of 10%, weighing 2g of NiO powder and 2g of YSZ powder, adding 33mL of isopropanol and 11mL of ethanol, and carrying out ball-milling mixing for 48 hours;
(3) dripping the NiO-YSZ suspension on a fired metal oxide support substrate, dripping 160uL of the NiO-YSZ suspension for each time, dripping four times, naturally drying the NiO-YSZ suspension, calcining the NiO-YSZ suspension for 1 hour at 400, 600, 800 and 1100 ℃ for each time to remove organic matters in the suspension, and finally sintering the NiO-YSZ suspension for the first time in an air atmosphere at 1150 ℃;
(4) then at 10% H2Reducing for 2h at 800 ℃ under an Ar atmosphere of-90 percent;
(5) preparing YSZ suspension with the mass fraction of 10%, weighing 4g of YSZ powder, adding 33mL of isopropanol and 11mL of ethanol, and carrying out ball milling and mixing for 48 hours;
(6) dropping YSZ suspension on reduced anode layer Ni-YSZ, dropping 160uL each time, dropping four times, naturally drying, calcining at 400 deg.C each time for 30 min, and calcining at 3% H2Sintering at 1250 ℃ for 4 hours under an Ar atmosphere of-97%.
This example results in a half cell having a Ni-Fe alloy support (-180 μm), Ni-YSZ anode functional layer (-45 μm), and dense 8YSZ electrolyte layer (-30 μm) structure. The half cell prepared in this example had an overall shrinkage of 22%, while the support layer without first reduction was at 3% H2The shrinkage after calcination at 1250 ℃ for 2 hours in an Ar atmosphere of-97% was 39%. The sectional scanning electron microscope image of the half cell is shown in fig. 2, and it can be seen that the contact of each part of the prepared half cell is good, and the electrolyte layer in fig. 3 is dense.
Comparative example 1
This comparative example is substantially the same as example 1, except that the calcination temperature in step (6) was 1350 ℃, and the cross-sectional scanning electron microscope image of the half cell is shown in fig. 4, which shows that the electrolyte YSZ layer was substantially destroyed and cracked more at higher calcination temperatures.
The above description is a preferred embodiment of the present invention, but the present invention should not be limited to the disclosure of the embodiment and the drawings. All equivalents and modifications which do not depart from the spirit of the invention as disclosed are deemed to be within the scope of the invention.

Claims (4)

1. The preparation method of the metal support type oxide fuel cell half cell is characterized by comprising the following specific steps of:
(1) preparing a metal oxide substrate: mixing Fe2O3Mixing with NiO powder according to the molar ratio of 1:1 to prepare the formed Fe2O3Pre-sintering a-NiO substrate at 1100-1200 ℃ in air atmosphere for 1-5 hoursThen, obtaining a metal oxide support matrix;
(2) depositing the NiO-YSZ suspension or slurry on the surface of the metal oxide support body substrate, and firing for 1-5 hours in an air atmosphere at 1100-1200 ℃ to obtain an oxide support body;
(3) subjecting the oxide support to 10% H in a reducing atmosphere2Preserving the heat for 1-5 hours at 800-900 ℃ under 90% of Ar to obtain a reduced Ni-Fe support body and a Ni-YSZ anode;
(4) depositing a YSZ suspension or slurry on the surface of the reduced metal support at 3% H2Sintering the substrate and the electrolyte for 2 to 5 hours at 1250 +/-10 ℃ in a protective atmosphere of-97% Ar to realize synchronous shrinkage of the substrate and the electrolyte, and obtaining the metal-supported solid oxide fuel cell half cell.
2. The method according to claim 1, wherein in the step (1), Fe2O3The formation of the-NiO substrate is carried out by dry pressing, casting or grouting.
3. The method of claim 1, wherein in step (2), the NiO-YSZ suspension or slurry is deposited on the surface of the metal oxide support substrate by depositing the NiO-YSZ suspension or slurry on the surface of the fired metal support substrate by drop coating or screen printing or spraying.
4. The method of claim 1, wherein the step (4) of depositing the YSZ suspension or slurry on the surface of the reduced metal support is carried out by depositing the YSZ suspension or slurry on the surface of the reduced metal support by drop coating or screen printing or spraying.
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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113054215A (en) * 2021-03-19 2021-06-29 东睦新材料集团股份有限公司 Method for manufacturing metal support plate for fuel cell

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CN113054215A (en) * 2021-03-19 2021-06-29 东睦新材料集团股份有限公司 Method for manufacturing metal support plate for fuel cell

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