CN112777624A - Electrolyte material, preparation method and application thereof - Google Patents
Electrolyte material, preparation method and application thereof Download PDFInfo
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- C—CHEMISTRY; METALLURGY
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- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F17/00—Compounds of rare earth metals
- C01F17/20—Compounds containing only rare earth metals as the metal element
- C01F17/206—Compounds containing only rare earth metals as the metal element oxide or hydroxide being the only anion
- C01F17/241—Compounds containing only rare earth metals as the metal element oxide or hydroxide being the only anion containing two or more rare earth metals, e.g. NdPrO3 or LaNdPrO3
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- C01F17/00—Compounds of rare earth metals
- C01F17/30—Compounds containing rare earth metals and at least one element other than a rare earth metal, oxygen or hydrogen, e.g. La4S3Br6
- C01F17/32—Compounds containing rare earth metals and at least one element other than a rare earth metal, oxygen or hydrogen, e.g. La4S3Br6 oxide or hydroxide being the only anion, e.g. NaCeO2 or MgxCayEuO
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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
- H01M8/12—Fuel cells with solid electrolytes operating at high temperature, e.g. with stabilised ZrO2 electrolyte
- H01M8/124—Fuel cells with solid electrolytes operating at high temperature, e.g. with stabilised ZrO2 electrolyte characterised by the process of manufacturing or by the material of the electrolyte
- H01M8/1246—Fuel cells with solid electrolytes operating at high temperature, e.g. with stabilised ZrO2 electrolyte characterised by the process of manufacturing or by the material of the electrolyte the electrolyte consisting of oxides
- H01M8/126—Fuel cells with solid electrolytes operating at high temperature, e.g. with stabilised ZrO2 electrolyte characterised by the process of manufacturing or by the material of the electrolyte the electrolyte consisting of oxides the electrolyte containing cerium oxide
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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
- H01M8/12—Fuel cells with solid electrolytes operating at high temperature, e.g. with stabilised ZrO2 electrolyte
- H01M2008/1293—Fuel cells with solid oxide electrolytes
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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
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Abstract
The invention provides compounds of formula La2‑xMxCe2O7‑δThe application also provides a preparation method and application of the electrolyte material. The electrolyte material provided by the application is doped with a certain amount of alkali metal elements, and La is reserved2Ce2O7Improves La on the premise of excellent chemical stability2Ce2O7The conductivity of the electrolyte improves the output power of the fuel cell, and the output power of the fuel cell doped with the rubidium electrolyte at 700 ℃ is improved by more than 70 percent compared with that of the fuel cell not doped with the rubidium electrolyte.
Description
Technical Field
The invention relates to the technical field of solid oxide fuel cells, in particular to an electrolyte material, a preparation method and application thereof.
Background
Solid Oxide Fuel Cells (SOFC) are attracting more and more attention worldwide as an important sustainable energy production technology, which has advantages of high energy conversion efficiency, environmental friendliness, and wide fuel selectivity.
Proton conductor materials are hot spots of current research because of lower activation energy and hopeful realization of low-temperature operation in SOFC. La2Ce2O7Is used as a stable proton conductor in hydrogen separation and SOFC, and has electrical conductivity higher than BaZrO3Chemical stability is superior to BaCeO3Thus, La is increased2Ce2O7The electrical conductivity of materials is a very important direction of research.
The doping being to increase La2Ce2O7The effective strategy of the conductivity is that under the condition of fixed doping amount, the lower the valence state of the doping element is, the more oxygen vacancies are introduced into the system, and the La is treated2Ce2O7The more advantageous the conductivity increase, the more the output of the constituent cells increases.
Disclosure of Invention
The invention aims to provide an electrolyte material with high conductivity.
In view of the above, the present application provides an electrolyte material represented by formula (I),
La2-xMxCe2O7-δ (Ⅰ)；
wherein x is more than or equal to 0 and less than or equal to 0.20, and delta is the stoichiometric number of oxygen vacancies in the electrolyte material;
m is Li, K, Rb or Cs.
Preferably, the value of x is more than or equal to 0.01 and less than or equal to 0.18.
The application also provides a preparation method of the electrolyte material, which comprises the following steps:
A) la is added according to the stoichiometric ratio of the molecular formula of the electrolyte material2O3Soluble M+Salt, Ce (NO)3)3Mixing the complexing agent and the pH regulator to obtain a complexing solution;
B) and heating the complexing solution until high-temperature self-propagating combustion occurs to obtain primary powder, and sintering the primary powder at a high temperature to obtain the electrolyte material.
Preferably, the complexation isThe agent is citric acid, and the addition amount of the complexing agent is La2O3Soluble M+Salt, Ce (NO)3)3Is 1.5 times of the total molar amount of the metal ions in the solution.
Preferably, the complexing solution further comprises nitric acid.
Preferably, the pH regulator is ammonia water.
Preferably, the high-temperature sintering temperature is 700-900 ℃, and the time is 2-4 h.
The application also provides a solid oxide fuel cell, which comprises a positive electrode, a negative electrode and an electrolyte material, and is characterized in that the electrolyte material is the electrolyte material or the electrolyte material prepared by the preparation method.
The application provides a method as La2-xMxCe2O7-δThe electrolyte material is doped with a certain amount of alkali metal elements, so that La is reserved in the electrolyte material2Ce2O7On the premise of excellent chemical stability, the La content is improved2Ce2O7The conductivity of the electrolyte improves the output power of the fuel cell, and the output power of the fuel cell doped with the rubidium electrolyte at 700 ℃ is improved by more than 70 percent compared with the output power of the fuel cell not doped with the rubidium electrolyte.
Drawings
FIG. 1 is La prepared in each example1.85M0.15Ce2O7-δXRD pattern of material powder;
FIG. 2 is La prepared in each example2Ce2O7Group La1.85K0.15Ce2O7-δGroup La1.85Rb0.15Ce2O7-δGroup and La1.85Cs0.15Ce2O7-δBase single cell section SEM picture;
FIG. 3 is a current-voltage (I-V) and current-power (I-P) curve at 700 ℃ for the single cells prepared in each example;
FIG. 4 is NiO-La of example 41.85Rb0.15Ce2O7-δ|La1.85Rb0.15Ce2O7-δLong term stability of | SSC-SDC cells.
Detailed Description
For a further understanding of the invention, reference will now be made to the preferred embodiments of the invention by way of example, and it is to be understood that the description is intended to further illustrate features and advantages of the invention, and not to limit the scope of the claims.
In view of the application requirements of SOFC and La2Ce2O7The application provides an alkali metal element doped lanthanum cerium oxygen electrolyte material to further improve the conductivity. Specifically, the embodiment of the invention discloses an electrolyte material as shown in a formula (I),
La2-xMxCe2O7-δ (Ⅰ)；
wherein x is more than or equal to 0 and less than or equal to 0.20, and delta is the stoichiometric number of oxygen vacancies in the electrolyte material;
m is Li, K, Rb or Cs.
In the above electrolyte material, x is 0.01. ltoreq. x.ltoreq.0.18, and more specifically, x is 0.15. Said M is more particularly selected from Li, K, Rb or Cs. Delta is the stoichiometric number of oxygen vacancy in the electrolyte material, the content of the delta is not fixed, the delta changes along with the change of experimental environment, and no fixed range exists.
The application also provides a preparation method of the electrolyte material, which comprises the following steps:
A) la is added according to the stoichiometric ratio of the molecular formula of the electrolyte material2O3Soluble M+Salt, Ce (NO)3)3Mixing the complexing agent and the pH regulator to obtain a complexing solution;
B) and heating the complexing solution until high-temperature self-propagating combustion occurs to obtain primary powder, and sintering the primary powder at a high temperature to obtain the electrolyte material.
According to the invention, La is first added according to the formula stoichiometry2O3Soluble M+Salt, Ce (NO)3)3Mixing the complexing agent and the pH regulator to obtain a complexing solution; to make it possible toUniformly mixing the raw materials, and sequentially adding the three main raw materials into an aqueous solution to be stirred until the three main raw materials are fully dissolved; and adding citric acid with the total molar weight of the metal ions being 1.5 times as the complexing agent, dropwise adding ammonia water to adjust the pH of the solution to be neutral, and continuously stirring until the particles are fully complexed to obtain a complexing solution. Nitric acid is also added to fully dissolve the above salts. The stirring is magnetic stirring, and the rotating speed is 100-500 rpm.
And after the complex solution is obtained, heating the complex solution until high-temperature self-propagating reaction occurs, burning the complex solution to obtain primary powder, and sintering the primary components at high temperature to obtain the electrolyte material. The sintering temperature of the high-temperature sintering is 700-900 ℃, and the time is 2-4 h.
The application also provides the application of the electrolyte material in the solid oxide fuel cell, and the electrolyte material is used as the electrolyte material of the solid oxide fuel cell. In practical application, the working temperature of the solid oxide fuel cell is 500-700 ℃.
The output power of the solid oxide fuel cell is greatly improved, and the temperature of 700 ℃ reaches 1065mWcm-2And the performance of the battery is improved by 76 percent compared with that of an undoped battery. Meanwhile, the electrolyte material disclosed by the invention is simple in preparation process and low in cost, and is beneficial to large-scale industrial use. The battery prepared by the invention has good output stability and provides possibility for practical application.
For further understanding of the present invention, the following examples are given to illustrate the composite material and the preparation method thereof, and the scope of the present invention is not limited by the following examples.
Example 1: la1.85K0.15Ce2O7-δPreparation of powder
According to La1.85K0.15Ce2O7-δWeighing La according to the stoichiometric ratio2O3、KNO3、Ce(NO3)3Dissolving in dilute nitric acid, stirring until the solution is fully dissolved, wherein the purity of the medicine is analytically pure or higher; adding citric acid ions with the total molar weight of the metal ions being 1.5 times as the complexing agent, dropwise adding ammonia water to adjust the pH of the solution to be neutral, and keepingStirring until the particles are fully complexed; transferring the precursor solution to a crucible, and heating the crucible by using an electric furnace until high-temperature self-propagating combustion occurs to obtain precursor powder; putting the burnt powder into a muffle furnace to be calcined for 2 hours at 700 ℃ to obtain the electrolyte La1.85K0.15Ce2O7-δAnd (3) powder materials.
Example 2: la1.85Cs0.15Ce2O7-δPreparation of powder
According to La1.85Cs0.15Ce2O7-δWeighing La according to the stoichiometric ratio2O3、CsNO3、Ce(NO3)3Dissolving in dilute nitric acid, stirring until the solution is fully dissolved, wherein the purity of the medicine is analytically pure or higher; adding citric acid ions with the total molar weight of the metal ions being 1.5 times as that of the metal ions as a complexing agent, dropwise adding ammonia water to adjust the pH value of the solution to be neutral, and continuously stirring until the particles are fully complexed; transferring the precursor solution to a crucible, and heating the crucible by using an electric furnace until high-temperature self-propagating combustion occurs to obtain precursor powder; putting the burnt powder into a muffle furnace to be calcined for 2 hours at 700 ℃ to obtain the electrolyte La1.85Cs0.15Ce2O7-δAnd (3) powder materials.
Example 3: la1.85Rb0.15Ce2O7-δPreparation of powder
According to La1.85Rb0.15Ce2O7-δWeighing La according to the stoichiometric ratio2O3、RbNO3、Ce(NO3)3Dissolving in dilute nitric acid, stirring until the solution is fully dissolved, wherein the purity of the medicine is analytically pure or higher; adding citric acid ions with the total molar weight of the metal ions being 1.5 times as that of the metal ions as a complexing agent, dropwise adding ammonia water to adjust the pH value of the solution to be neutral, and continuously stirring until the particles are fully complexed; transferring the precursor solution to a crucible, and heating the crucible by using an electric furnace until high-temperature self-propagating combustion occurs to obtain precursor powder; putting the burnt powder into a muffle furnace to be calcined for 2 hours at 700 ℃ to obtain the electrolyte La1.85Rb0.15Ce2O7-δAnd (3) powder materials.
FIG. 1 shows La electrolytes prepared in examples 1 to 31.85K0.15Ce2O7-δPowder material and electrolyte La1.85Cs0.15Ce2O7-δPowder material and electrolyte La1.85Rb0.15Ce2O7-δPowder material and La2Ce2O7An XRD pattern of (a), wherein, La1.85K0.15Ce2O7-δThe marker is LKCO, La1.85Cs0.15Ce2O7-δMarked as LCCO, La1.85Rb0.15Ce2O7-δLabeled as LRCO, La2Ce2O7Labeled LCO; as shown in fig. 1, a series of products obtained by the one-step synthesis method have no impurity phase, which indicates that the target electrolyte product can be obtained by simple one-step synthesis.
Example 4: la1.85M0.15Ce2O7-δPreparation of (M ═ K, Rb, Cs) -based single cells
Anode NiO-La of single fuel cell1.85M0.15Ce2O7-δThe same combustion method as described above for citrate was used for SSC-SDC cathode powder; sintered phase NiO-La1.85M0.15Ce2O7-δMixing with 20% wt of starch, adding an ethanol solvent, ball-milling for 12 hours, and drying to obtain anode powder; SSC-SDC (6: 4 wt%) powder is added into proper ethyl cellulose terpineol, and the mixture is fully ground to obtain cathode slurry.
Using a uniaxial co-pressing mode to press a trace amount of La1.85M0.15Ce2O7-δPressed in NiO-La1.85M0.15Ce2O7-δAnd co-firing the surface of the green wafer for 5 hours at 1300 ℃ in a muffle furnace to obtain the half cell.
Coating the cathode slurry on the center of the prepared half-cell electrolyte membrane by a screen printing method, and then co-firing at 900 ℃ for 2h to obtain NiO-La1.85M0.15Ce2O7-δ|La1.85M0.15Ce2O7-δI SSC-SDC single cell. As shown in FIG. 2, the single cell electrolyte layer prepared by the above procedure was less doped with La2Ce2O7The electrolyte layer is more compact, the porous anode and the porous cathode are tightly combined with the electrolyte, and the battery has a good microstructure.
In a home-made test system, the time is 40mL min-1H of flow velocity2(～3％H2O) as fuel gas test cell; the anode side of the single cell is sealed at the pipe orifice of the self-made ceramic device by conductive adhesive, the cathode uses silver paste to collect current and uses a fine silver wire to lead out the current when the cell works; the I-V and I-P curves of the cells were measured using a dc electronic load.
FIG. 3 shows La1.85K0.15Ce2O7-δGroup La1.85Rb0.15Ce2O7-δGroup and La1.85Cs0.15Ce2O7-δThe maximum output power of the basic single cell at 700 ℃ is 916mWcm-2、1065mWcm-2And 903mWcm-2Undoped La2Ce2O7The maximum output power of the basic single cell at 700 ℃ is 604mWcm-2The improvement is respectively 51.66%, 76.32% and 49.50%.
Selecting the La with the highest output power1.85Rb0.15Ce2O7-δThe cell stability test was performed on the base cell under the conditions of 600 c and 0.7V, and fig. 4 shows that the cell can stably output for more than 200h under the conditions.
The above description of the embodiments is only intended to facilitate the understanding of the method of the invention and its core idea. It should be noted that, for those skilled in the art, it is possible to make various improvements and modifications to the present invention without departing from the principle of the present invention, and those improvements and modifications also fall within the scope of the claims of the present invention.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (8)
1. An electrolyte material as shown in a formula (I),
La2-xMxCe2O7-δ (Ⅰ)；
wherein x is more than or equal to 0 and less than or equal to 0.20, and delta is the stoichiometric number of oxygen vacancies in the electrolyte material;
m is Li, K, Rb or Cs.
2. The electrolyte material of claim 1, wherein x is 0.01. ltoreq. x.ltoreq.0.18.
3. The method for producing the electrolyte material according to claim 1, comprising the steps of:
A) la is added according to the stoichiometric ratio of the molecular formula of the electrolyte material2O3Soluble M+Salt, Ce (NO)3)3Mixing the complexing agent and the pH regulator to obtain a complexing solution;
B) and heating the complexing solution until high-temperature self-propagating combustion occurs to obtain primary powder, and sintering the primary powder at a high temperature to obtain the electrolyte material.
4. The method according to claim 3, wherein the complexing agent is citric acid, and the amount of the complexing agent added is the La2O3Soluble M+Salt, Ce (NO)3)3Is 1.5 times of the total molar amount of the metal ions in the solution.
5. The method according to claim 3, wherein the complexing solution further comprises nitric acid.
6. The method according to claim 3, wherein the pH adjuster is ammonia water.
7. The preparation method according to claim 3, wherein the high-temperature sintering temperature is 700-900 ℃ and the time is 2-4 h.
8. A solid oxide fuel cell comprising a positive electrode, a negative electrode and an electrolyte material, wherein the electrolyte material is the electrolyte material according to any one of claims 1 to 2 or the electrolyte material prepared by the preparation method according to any one of claims 3 to 7.
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Application publication date: 20210511 |