CN111146456A - Preparation method of composite cathode material for fuel cell - Google Patents

Preparation method of composite cathode material for fuel cell Download PDF

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CN111146456A
CN111146456A CN202010075108.2A CN202010075108A CN111146456A CN 111146456 A CN111146456 A CN 111146456A CN 202010075108 A CN202010075108 A CN 202010075108A CN 111146456 A CN111146456 A CN 111146456A
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composite cathode
cathode material
powder
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CN111146456B (en
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陈孔发
蒋文俊
逄舒淇
江丽贞
邵艳群
王欣
唐电
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Fuzhou 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
    • H01M4/88—Processes of manufacture
    • 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
    • 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
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G51/00—Compounds of cobalt
    • C01G51/006—Compounds containing, besides cobalt, two or more other elements, with the exception of oxygen or hydrogen
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G51/00—Compounds of cobalt
    • C01G51/40—Cobaltates
    • 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
    • H01M4/00—Electrodes
    • H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
    • H01M4/90—Selection of catalytic material
    • H01M4/9016—Oxides, hydroxides or oxygenated metallic salts
    • H01M4/9025—Oxides specially used in fuel cell operating at high temperature, e.g. SOFC
    • H01M4/9033—Complex oxides, optionally doped, of the type M1MeO3, M1 being an alkaline earth metal or a rare earth, Me being a metal, e.g. perovskites
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
    • C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/01—Particle morphology depicted by an image
    • C01P2004/03—Particle morphology depicted by an image obtained by SEM
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/80—Particles consisting of a mixture of two or more inorganic phases
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/40—Electric properties
    • 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 preparation method of a composite cathode material for a fuel cell, belonging to the technical field of preparation of electrode materials of fuel cells. Which is by GdzCe1‑zO2(z is 0 to 1) composite reinforced LaxSr1‑xCoyFe1‑yO3‑δ(x is 0 to 1, and y is 0 to 1). The invention obtainsThe obtained cathode particles have great improvement on the original structure and can show remarkable high catalytic activity. The preparation method has the advantages of simple and easily obtained raw materials and stable process, and can meet the requirements of industrial production.

Description

Preparation method of composite cathode material for fuel cell
Technical Field
The invention belongs to the technical field of preparation of fuel cell electrode materials, and particularly relates to a preparation method of a high-efficiency composite cathode material for a fuel cell.
Background
The fuel cell is an electrochemical power generation device, can efficiently and cleanly convert chemical energy of fuel into electric energy, wherein the Solid Oxide Fuel Cell (SOFC) has unique advantages, such as adopting an all-solid-state ceramic device, and avoiding electrolyte corrosion and leakage; and modular design can be adopted, so that the design and production cost is reduced. The cathode is an important component of the SOFC, and the performance of the SOFC is closely linked to the catalytic activity, electrical conductivity, and microstructure of the cathode. Desirable high performance cathodes need to have excellent electrochemical catalytic activity, high electrochemical reaction area, and good electron conductivity and ion mixing conductivity properties. In recent years, researchers have tried various methods to prepare high performance SOFC cathode materials, such as building composite cathodes by adding ion conductors.
Gadolinium oxide doped cerium oxide (Gd)zCe1-zO2GDC and z are 0-1) is a widely applied medium-low temperature SOFC electrolyte material, and has excellent ionic conductivity and surface exchange coefficient. Patent CN 110098410A uses colloid modification method to apply GDC nano-particles to double-layer perovskite cathode material PrBa1-λCaλCo2O5+δIn the (PBCC) (wherein lambda is 0-1), the redox of PBCC is obviously improvedElectrochemical catalytic activity of the original reaction (ORR). However, PBCC materials are still in the experimental development stage, and many technical problems still remain to be solved, such as the required sintering temperature is too high, the thermal expansion coefficient matching with the electrolyte material is poor (Hou J, Miao L, Hui J, et al A novel in situ differentiation strategy to a novel high performance for low temperature processing and reducing of solid oxide cells [ J]. Journal of Materials Chemistry A, 2018, 6(22): 10411-10420）。
LaxSr1-xCoyFe1-yO3-δ(LSCF, x is 0-1, y is 0-1) is the most successful intermediate temperature SOFC cathode material at present, has excellent electron/ion conductivity and electrochemical catalytic activity, and achieves the condition of industrial use (ConceiOLD, Silva A M, Ribeiro N F P, et al, Combustion synthesis of La)0.7Sr0.3Co0.5Fe0.5O3(LSCF) porous materials for application as cathode in IT-SOFC[J]Materials Research Bulletin, 2011, 46(2): 308-. However, the conventional electrode preparation process needs high-temperature sintering (900-. A nano-scale coated electrode can be prepared by a dipping method, but The process is complex and needs to be subjected to a plurality of dipping-pre-burning processes (Tomov R I, Mitchel-Williams T B, Maher R, et al, The synergy effect of cobalt oxide and Gd-CeO2dual infiltration in LSCF/CGO cathodes[J]Journal of Materials Chemistry A, 2018, 6(12): 5071-5081). Patent CN 108091885a prepares perovskite oxide or fluorite oxide on the cathode by an impregnation method, which comprises coating cathode slurry on the electrolyte, sintering at high temperature, and then dropping nitrate solution into the cathode, which has the same phenomena of complex preparation process and uneven impregnation concentration gradient as the aforementioned impregnation method. While patent CN 102420332A is in LaNi0.6Fe0.4O3-δCeO is coated on the cathode2The method for preparing the Cr poison resistant cathode comprises the steps of coating cathode slurry on an electrolyte, sintering at high temperature, and infiltrating the cathodeIn CeO2In the solution, but it is not uniformly stirred in the soaking process, and LaNi0.6Fe0.4O3-δThe electrode is subjected to high-temperature sintering treatment before coating, so that the phenomena of large cathode particles, uneven coating and the like are easy to occur.
The method modifies the GDC nano-particles onto the LSCF particles which are not subjected to high-temperature sintering by a sol-gel method, so as to form a fine composite cathode, and prepares the fine composite cathode on the surface of an electrolyte by an electrochemical polarization method under the condition of medium temperature (600-plus-850 ℃) in the subsequent battery assembly process, thereby avoiding the high-temperature sintering process, inhibiting the growth of electrode particles, improving the effective reaction area and the ionic conductivity of the cathode, and improving the output performance of the battery.
Disclosure of Invention
The invention aims to provide a high-efficiency preparation method of a composite cathode material for a fuel cell, aiming at the defects of the prior art. The composite cathode powder is constructed through a sol modification process, so that the cathode microstructure is improved, the effective reaction area and the surface exchange coefficient of the LSCF cathode are obviously improved, and the electrochemical catalytic performance of the LSCF cathode is further improved.
In order to achieve the purpose, the invention adopts the following technical scheme:
a composite cathode material for fuel cell is prepared from the cerium oxide (Gd) stabilized by nano-class gadolinium oxidezCe1-zO2Z is 0-1) is modified in LaxSr1-xCoyFe1-yO3-δ(x is 0-1, y is 0-1) to prepare the ion-conducting enhanced composite cathode material. The method comprises the following specific steps:
(1) weighing a certain amount of Ce (NO)3)3·6H2O and Gd (NO)3)3·6H2Pouring O solid powder into a beaker, adding deionized water, mixing, adding a certain amount of complexing agent and ammonia water solution, pouring the obtained mixture into the beaker filled with deionized water, and mixing and stirring at room temperature to obtain a colored clear solution;
(2) adding the colored clear solution obtained in the step (1) at the temperature of 20-600 DEG CHeating, and adding La when the balance of the solution is 50-100 mLxSr1-xCoyFe1-yO3-δ(LSCF) powder, stirring and mixing to obtain colored gel; ce in salt solution in the process3+With Gd3+Attached to the LSCF surface layer;
(3) and (3) drying the colored gel obtained in the step (2) in an oven at 50-600 ℃ for 0.1-50 hours, transferring the dried black fluffy gel into a mortar for grinding, placing the black fluffy gel into a crucible, calcining the black fluffy gel for 0.1-20 hours at 400-1200 ℃ in a high-temperature furnace, reacting surface salt ions with oxygen to form fluorite-structured oxide in the process, taking out the fluorite-structured oxide, and finely grinding the fluorite-structured oxide to obtain the LSCF ion enhanced cathode powder modified by GDC.
Ce (NO) added in step (1)3)3·6H2O and Gd (NO)3)3·6H2The molar ratio of O is (0.1-0.9) to (0.01-0.5).
In the step (1), the addition amount of the complexing agent is 1-15 times of the total mole number of metal cations in the solution; the complexing agent is a mixture of citric acid and EDTA, and the molar ratio of the citric acid to the EDTA is (0.1-1.5) to (0.1-1).
The mass ratio of the total using amount of the deionized water to the complexing agent in the step (1) is (1-15): 1.
And (2) adding an ammonia water solution to adjust the pH of the solution to 2-12, wherein the mass concentration of the ammonia water solution is 25%.
La in step (2)xSr1-xCoyFe1-yO3-δThe adding amount of the powder is 1-99% of the mass of the obtained composite cathode material.
The invention has the obvious advantages that
1. The GDC/LSCF composite cathode synthesized by the sol-gel method has a high reaction area, and can remarkably improve the performance of the solid oxide fuel cell cathode.
2. Particles having nanostructures in general tend to agglomerate, thereby affecting their dispersibility and utilization. The invention takes LSCF as a framework to play a role of uniform dispersion, gives play to the flexibility and the easy operability of a polymer carrier, reduces the probability of cathode agglomeration, and can also generate a stronger synergistic effect by utilizing the surface recombination of polymer micro-nano sizes to improve the catalytic efficiency.
3. The preparation method of the composite cathode material provided by the invention has the advantages of easily available raw materials, simple and stable preparation process.
Drawings
Fig. 1 is an SEM surface topography of pure LSCF cathode powder.
FIG. 2 is an SEM image of 10wt% GDC-modified LSCF composite cathode powder obtained in example 1.
FIG. 3 is the XRD pattern of 20wt% GDC modified LSCF composite cathode powder obtained in example 2.
FIG. 4 is a graph comparing the single cell performance of 20wt% GDC modified LSCF composite cathode powder obtained in example 2 and pure LSCF cathode powder under the working condition of 750 ℃.
Detailed Description
In order to make the present invention more comprehensible, the technical solutions of the present invention are further described below with reference to specific embodiments, but the present invention is not limited thereto.
Preparation of LSCF powder:
(1) adding 5.1g La (NO)3)3·6H2O、1.7g Sr(NO3)2、1.2g Co(NO3)2·6H2O、6.5g Fe(NO3)3·9H2Adding O, 11.5g of citric acid and 11.7g of EDTA powder into a beaker, mixing with 500mL of deionized water, slowly pouring 24mL of 25% ammonia water solution, and stirring to fully dissolve, wherein the pH is measured to be = 5;
(2) and (3) heating the stirred colored solution to 300 ℃, putting the solution into an oven for drying after the solution is completely converted into gel, and calcining the solution at 950 ℃ for 5 hours to obtain the pure LSCF cathode powder.
FIG. 1 is an SEM surface topography of the prepared pure LSCF cathode powder. As shown in the figure, the particle size is not uniform, the agglomeration phenomenon is serious, and the dispersion is not uniform.
EXAMPLE 1 preparation of LSCF/GDC composite powder
(1) 0.02g (4.6X 10) was weighed-5mol）Gd(NO3)3·6H2O、0.22g（4.8×10-4mol）Ce(NO3)3·6H2O、0.33g（1.7×10-3mol) citric acid, 0.33g (1.1X 10)-3mol) EDTA is put into a beaker, 100mL of deionized water is poured, 0.7mL of 25% ammonia water solution is slowly poured, the mixture is continuously stirred at room temperature to be fully dissolved, and the pH value of the detection solution is 6;
(2) heating and stirring the obtained light yellow solution at 180 ℃, adding a certain amount of LSCF cathode powder when the water content is 50mL, keeping the temperature unchanged, and stirring and mixing to obtain black fluffy cathode precursor gel;
(3) and (3) drying the obtained precursor gel in an oven at 180 ℃ for 10 hours, taking out the massive precursor, grinding the massive precursor into powder, putting the powder into a crucible, calcining the powder in a high-temperature furnace at 750 ℃ for 2 hours, taking out the powder, and finely grinding the powder to obtain the LSCF ion enhanced fuel cell cathode powder coated with 10wt% of GDC.
FIG. 2 is an SEM image of 10wt% GDC-modified LSCF fuel cell cathode powder obtained in example 1. As shown in the figure, the particles are nanoscale, and GDC and LSCF particles are orderly stacked and uniformly distributed, which shows that the method of the present invention can improve the cathode powder microstructure.
EXAMPLE 2 preparation of LSCF/GDC composite powder
(1) 0.04g (9.2X 10) was weighed out-5mol）Gd(NO3)3·6H2O、0.44g（9.6×10-4mol）Ce(NO3)3·6H2O、0.66g（3.4×10-3mol) citric acid, 0.68g (2.2X 10)-3mol) EDTA in a beaker, pouring 200mL of deionized water, slowly pouring 0.14mL of ammonia water solution (the concentration is 25 percent), continuously stirring at room temperature to fully dissolve the EDTA, and detecting the pH value of the solution to be 6;
(2) heating and stirring the obtained light yellow solution at 180 ℃, adding a certain amount of LSCF cathode powder when the water content is 50mL, keeping the temperature unchanged, and stirring and mixing to obtain black fluffy cathode precursor gel;
(3) and (3) drying the obtained precursor gel in an oven at 180 ℃ for 10 hours, taking out the massive precursor, grinding the massive precursor into powder, putting the powder into a crucible, calcining the powder in a high-temperature furnace at 750 ℃ for 2 hours, taking out the powder, and finely grinding the powder to obtain the LSCF ion enhanced fuel cell cathode powder coated with the GDC with the content of 20 wt%.
Figure 3 is the XRD pattern of the LSCF fuel cell cathode powder modified with 20wt% GDC obtained in example 2. As shown, both GDC and LSCF are in phase and no miscellaneous items are generated.
FIG. 4 is a graph comparing the single cell performance of 20wt% GDC modified LSCF composite cathode powder obtained in example 2 and pure LSCF cathode powder under the working condition of 750 ℃. As shown, the maximum power density of the GDC-modified LSCF was 0.91W-cm-2The maximum power density of pure LSCF is 0.60 W.cm-2Therefore, the power of the composite cathode material prepared by the invention is obviously improved.
The above description is only a preferred embodiment of the present invention, and all equivalent changes and modifications made in accordance with the claims of the present invention should be covered by the present invention.

Claims (8)

1. A preparation method of a composite cathode material for a fuel cell is characterized by comprising the following steps: using GdzCe1-zO2To LaxSr1- xCoyFe1-yO3-δModifying to prepare the ion-conducting enhanced composite cathode material; wherein z is 0-1, x is 0-1, and y is 0-1.
2. The method of preparing a composite cathode material according to claim 1, wherein: the method comprises the following specific steps:
(1) weighing a certain amount of Ce (NO)3)3·6H2O and Gd (NO)3)3·6H2Adding deionized water into O solid powder, mixing, adding a certain amount of complexing agent and ammonia water solution, pouring the obtained mixture into a beaker filled with deionized water, and mixing and stirring at room temperature to obtain a colored clear solution;
(2) heating the colored clear solution obtained in the step (1) at the temperature of 20-600 ℃,adding La when the balance of the solution is 50-100 mLxSr1-xCoyFe1-yO3-δStirring and mixing the powder to obtain colored gel;
(3) and (3) drying, grinding, calcining and grinding the colored gel obtained in the step (2) again to obtain the ion-enhanced composite cathode powder.
3. The method of preparing a composite cathode material according to claim 2, characterized in that: ce (NO) added in step (1)3)3·6H2O and Gd (NO)3)3·6H2The molar ratio of O is (0.1-0.9) to (0.01-0.5).
4. The method of preparing a composite cathode material according to claim 2, characterized in that: in the step (1), the addition amount of the complexing agent is 1-15 times of the total mole number of metal cations in the solution;
the complexing agent is a mixture of citric acid and EDTA, and the molar ratio of the citric acid to the EDTA is (0.1-1.5) to (0.1-1).
5. The method of preparing a composite cathode material according to claim 2, characterized in that: the mass ratio of the total using amount of the deionized water to the complexing agent in the step (1) is (1-15): 1.
6. The method of preparing a composite cathode material according to claim 2, characterized in that: and (2) adding an ammonia water solution to adjust the pH of the solution to 2-12, wherein the mass concentration of the ammonia water solution is 25%.
7. The method of preparing a composite cathode material according to claim 2, characterized in that: la in step (2)xSr1- xCoyFe1-yO3-δThe adding amount of the powder is 1-99% of the mass of the obtained composite cathode material.
8. The method of preparing a composite cathode material according to claim 2, characterized in that: the drying temperature in the step (3) is 50-600 ℃, and the drying time is 0.1-50 hours; the calcining temperature is 400-1200 ℃ and the calcining time is 0.1-20 hours.
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CN112670521A (en) * 2020-12-28 2021-04-16 哈尔滨工业大学 Method for improving stability of solid oxide fuel cell cathode based on stress design
CN113555562A (en) * 2021-06-29 2021-10-26 南京理工大学 Composite cathode structure working in wide oxygen atmosphere and preparation method thereof
CN115064712A (en) * 2022-08-03 2022-09-16 盐城工学院 Preparation method of nanoparticle-coated composite cathode material

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112290034A (en) * 2019-07-26 2021-01-29 南京理工大学 Anode material of solid oxide fuel cell and preparation method thereof
CN112290034B (en) * 2019-07-26 2022-09-20 南京理工大学 Anode material of solid oxide fuel cell and preparation method thereof
CN112670521A (en) * 2020-12-28 2021-04-16 哈尔滨工业大学 Method for improving stability of solid oxide fuel cell cathode based on stress design
CN113555562A (en) * 2021-06-29 2021-10-26 南京理工大学 Composite cathode structure working in wide oxygen atmosphere and preparation method thereof
CN115064712A (en) * 2022-08-03 2022-09-16 盐城工学院 Preparation method of nanoparticle-coated composite cathode material
CN115064712B (en) * 2022-08-03 2023-11-17 盐城工学院 Preparation method of nanoparticle coated composite cathode material

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