CN110649300A - Electrolyte of alkaline earth metal doped proton conduction intermediate-temperature solid oxide fuel cell - Google Patents
Electrolyte of alkaline earth metal doped proton conduction intermediate-temperature solid oxide fuel cell Download PDFInfo
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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
- H01M8/1016—Fuel cells with solid electrolytes characterised by the electrolyte material
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- C01P2006/40—Electric properties
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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
- H01M2300/00—Electrolytes
- H01M2300/0017—Non-aqueous electrolytes
- H01M2300/0065—Solid 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
- Y02E60/30—Hydrogen technology
- Y02E60/50—Fuel cells
Abstract
The invention discloses an alkaline earth metal doped proton conduction medium-temperature solid oxide fuel cell electrolyte and a preparation method thereof. The invention adopts a nitrate-sol-gel-combustion method to prepare the proton conduction electrolyte of the intermediate-temperature solid oxide fuel cell with high conductivity, and the relative densities of alkaline earth metal (Mg, Ca, Sr and Ba) doped electrolytes respectively reach 99.42 percent, 99.08 percent, 99.41 percent and 98.94 percent; at wet 5% H2And the electric conductivity of the alloy reaches 0.0154S/cm, 0.0097S/cm, 0.0186S/cm and 0.0102S/cm at 700 ℃ in a mixed atmosphere of 95% Ar.
Description
Technical Field
The invention belongs to the technical field of solid oxide fuel cell materials, and particularly relates to an alkaline earth metal doped proton conduction medium-temperature solid oxide fuel cell electrolyte and a preparation method thereof.
Background
Nowadays, as the population is increasing day by day, the living standard of people is continuously improved and the society develops rapidly, the demand of human beings on energy is greatly increased. Fossil fuels, i.e., coal, oil, natural gas, etc., are the most significant energy sources worldwide. However, these resources have their own reserves limited and their combustion process can present serious environmental problems. Therefore, the subject of modern energy technology is the development of new economic and clean energy sources. The Solid Oxide Fuel Cell (SOFC) is an all-solid-state electrochemical device which directly converts chemical energy into electric energy, is not limited by Carnot cycle, has high working efficiency and environmental friendliness, has the advantages of no corrosion, no leakage, monomer design and the like, and is a clean and environment-friendly energy system device which efficiently utilizes energy in the future of development at present.
SOFCs that have been commercially used today typically operate at 1000 ℃, and operating at such high temperatures presents a number of problems for SOFCs: electrode densification, high requirements on connector materials, poor battery sealing performance, and the like. Therefore, the reduction of the SOFC operating temperature can effectively reduce the cost of the system and improve stability. The traditional electrolyte material is not suitable for working in a medium-temperature environment, and protons have the advantages of small volume and light weight and have lower ion conduction activation energy at medium and low temperature, so the proton conductive oxide is an electrolyte applicable to low-temperature working SOFC. The invention obtains a novel proton conductor oxide material with excellent chemical stability and high proton conductivity by doping alkaline earth metal. The electrolyte material can obtain higher conductivity and excellent chemical stability at the intermediate temperature so as to meet the requirements of the current intermediate-low temperature SOFC electrolyte material.
Disclosure of Invention
The invention aims to provide an alkaline earth metal doped proton conduction intermediate-temperature solid oxide fuel cell electrolyte and a preparation method thereof. The alkaline earth metal doped electrolyte effectively reduces the working temperature of the fuel cell, and has the characteristics of high conductivity, excellent chemical stability and the like.
In order to achieve the purpose, the invention adopts the following technical scheme:
Nd1.85Mg0.15Ce2O7+δ、Nd1.85Ca0.15Ce2O7+δ、Nd1.85Sr0.15Ce2O7+δ、Nd1.85Ba0.15Ce2O7+δ，0>δ>the preparation method of-0.075 is as follows:
1) respectively press Nd1.85Mg0.15Ce2O7+δ、Nd1.85Ca0.15Ce2O7+δ、Nd1.85Sr0.15Ce2O7+δ、Nd1.85Ba0.15Ce2O7+δWeighing Nd (NO) according to the stoichiometric ratio of3)3·nH2O (AR)、Ce(NO3)3·6H2O (AR)、Mg(NO3)2·6H2O (AR)、Ca(NO3)2·6H2O (AR)、Sr(NO3)2·6H2O (AR) and Ba (NO)3)2·6H2O (AR), and weighing citric acid according to the molar ratio of the metal cations to the citric acid of 1: 1.5;
2) respectively dissolving the nitrate and the citric acid in the step 1) by using deionized water;
3) stirring and mixing the corresponding nitrate solution, and finally adding a citric acid solution serving as a complexing agent;
4) respectively dropwise adding ammonia water with the mass concentration of 15% -20% into the obtained solution to adjust the pH value of the solution to 7;
5) putting the mixed solution obtained in the step 4) into a constant-temperature magnetic stirrer, heating to 70 ℃, and then keeping stirring at 70 ℃ until gel is formed;
6) transferring the gel into an evaporating dish, and heating the evaporating dish on an electric furnace until self-propagating combustion occurs to form fluffy oxide powder;
7) heating the obtained oxide powder to 800 +/-10 ℃, preserving heat for 3 +/-0.1 hours, and then naturally cooling to form Nd1.85Mg0.15Ce2O7+δ、Nd1.85Ca0.15Ce2O7+δ、Nd1.85Sr0.15Ce2O7+δ、Nd1.85Ba0.15Ce2O7+δPowder;
8) the prepared Nd1.85Mg0.15Ce2O7+δ、Nd1.85Ca0.15Ce2O7+δ、Nd1.85Sr0.15Ce2O7+δ、Nd1.85Ba0.15Ce2O7+δFully grinding the powder, putting the powder into a die, preparing a wafer with the diameter of 12 +/-0.1 mm and the thickness of 2 +/-0.1 mm under the pressure of 150MPa, heating the wafer to 800 ℃ at the speed of 5 ℃ per minute, heating to 1500 +/-10 ℃ at the speed of 3 ℃ per minute, and preserving the temperature for 5 +/-0.1 hours to obtain the electrolyte wafer of the intermediate-temperature solid oxide fuel cell.
The invention has the following remarkable advantages: nd doped with alkaline earth metal (Mg, Ca, Sr, Ba)2Ce2O7The solid electrolyte of the proton conductor fully reduces the working temperature of the electrolyte; and in CO2And H2O has good stability. Nd doped with Mg, Ca, Sr and Ba2Ce2O7The relative density of the electrolyte reaches 99.42 percent, 99.08 percent, 99.41 percent and 98.94 percent respectively; at wet 5% H2The electric conductivity of the Nd alloy reaches 0.0154S/cm, 0.0097S/cm, 0.0186S/cm and 0.0102S/cm respectively at 700 ℃ in the mixed atmosphere of 95% Ar, and the electric conductivity is higher than that of the pure Nd prepared by the same method2Ce2O7The relative density of the composite material is 97.14 percent, and the conductivity is 0.0086S/cm. The working temperature of the conductive coating has high conductivity in the range of medium temperature (500 ℃ -800 ℃).
Drawings
FIG. 1 shows Nd2Ce2O7、Nd1.85Mg0.15Ce2O7+δ、Nd1.85Ca0.15Ce2O7+δ、Nd1.85Sr0.15Ce2O7+δAnd Nd1.85Ba0.15Ce2O7+δAt 5% H wet2And a conductivity chart in a 95% Ar mixed atmosphere.
FIG. 2 shows Nd2Ce2O7、Nd1.85Mg0.15Ce2O7+δ、Nd1.85Ca0.15Ce2O7+δ、Nd1.85Sr0.15Ce2O7+δAnd Nd1.85Ba0.15Ce2O7+δXRD patterns after different atmosphere maintenance.
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.
Example 1
Nd1.85Mg0.15Ce2O7+δ、Nd1.85Ca0.15Ce2O7+δ、Nd1.85Sr0.15Ce2O7+δ、Nd1.85Ba0.15Ce2O7+δ，0>δ>-0.075 preparation method:
1) respectively press Nd1.85Mg0.15Ce2O7+δ、Nd1.85Ca0.15Ce2O7+δ、Nd1.85Sr0.15Ce2O7+δ、Nd1.85Ba0.15Ce2O7+δWeighing Nd (NO) according to the stoichiometric ratio of3)3·nH2O (AR)、Ce(NO3)3·6H2O (AR)、Mg(NO3)2·6H2O (AR)、Ca(NO3)2·6H2O (AR)、Sr(NO3)2·6H2O (AR) and Ba (NO)3)2·6H2O (AR), and weighing citric acid according to the molar ratio of the metal cations to the citric acid of 1: 1.5;
2) respectively dissolving the nitrate and the citric acid in the step 1) by using deionized water;
3) stirring and mixing the corresponding nitrate solution uniformly, and finally adding a citric acid solution serving as a complexing agent;
4) respectively dropwise adding ammonia water with the mass concentration of 15% -20% into the obtained solution to adjust the pH value of the solution to 7;
5) putting the mixed solution obtained in the step 4) into a constant-temperature magnetic stirrer, heating to 70 ℃, and then keeping stirring at 70 ℃ until gel is formed;
6) transferring the gel into an evaporating dish, and heating the evaporating dish on an electric furnace until self-propagating combustion occurs to form fluffy oxide powder;
7) heating the obtained oxide powder to 800 +/-10 ℃, preserving heat for 3 +/-0.1 hours, and then naturally cooling to form Nd1.85Mg0.15Ce2O7+δ、Nd1.85Ca0.15Ce2O7+δ、Nd1.85Sr0.15Ce2O7+δ、Nd1.85Ba0.15Ce2O7+δPowder;
8) the prepared Nd1.85Mg0.15Ce2O7+δ、Nd1.85Ca0.15Ce2O7+δ、Nd1.85Sr0.15Ce2O7+δ、Nd1.85Ba0.15Ce2O7+δFully grinding the powder, putting the powder into a die, preparing a wafer with the diameter of 12 +/-0.1 mm and the thickness of 2 +/-0.1 mm under the pressure of 150MPa, heating the wafer to 800 ℃ at the speed of 5 ℃ per minute, heating to 1500 +/-10 ℃ at the speed of 3 ℃ per minute, and preserving the temperature for 5 +/-0.1 hours to obtain the high-performance medium-temperature solid oxide fuel cell electrolyte wafer.
Specifically, the method comprises the following steps:
1 mol of Nd1.85Mg0.15Ce2O7+δ、Nd1.85Ca0.15Ce2O7+δAnd Nd1.85Sr0.15Ce2O7+δ、Nd1.85Ba0.15Ce2O7+δThe preparation of (1):
preparation of 1 mol of Nd1.85Mg0.15Ce2O7+δ
1.85 mol of Nd (NO) was weighed3)3·nH2O: 1.85 × 330.25=610.96 g
Weighing 2 moles of Ce (NO)3)3·6H2O: 2 × 434.22=868.44 g
0.15 mol of Mg (NO) was weighed out3)2·6H2O: 0.15 × 256.41=38.4615 g
Weighing 6 moles of citric acid: 6 × 210.14=1260.84 g
Adding Nd (NO)3)3·nH2O，Ce(NO3)3·6H2O，Mg(NO3)2·6H2Dissolving O and citric acid in deionized water;
uniformly stirring and mixing the nitrate solution, finally adding a citric acid solution serving as a complexing agent, and dropwise adding ammonia water to adjust the pH value to 7;
heating the mixed solution to 70 ℃ in a constant-temperature magnetic stirrer, and continuously stirring at 70 ℃ until gel is formed;
transferring the gel into an evaporating dish, and placing the evaporating dish on an electric furnace for heating until self-propagating combustion occurs to form oxide powder;
heating the powder to 800 +/-10 ℃, preserving the heat for 3 +/-0.1 hours, and naturally cooling to form Nd1.85Mg0.15Ce2O7+δAnd (3) powder.
Same procedure for preparing 1 mol Nd1.85Ca0.15Ce2O7+δ、Nd1.85Sr0.15Ce2O7+δ、Nd1.85Ba0.15Ce2O7+δ(ii) a 0.15 mol of Ca (NO)3)2·6H2O: 0.15 × 236.15=35.4225 g, 0.15 mol of Sr (NO)3)2·6H2O: 0.15 × 211.63=31.7445 g, 0.15 mol of Ba (NO)3)2·6H2O: 0.15 × 261.34=39.201 grams.
Preparation of the wafer: prepared Nd1.85Mg0.15Ce2O7+δ、Nd1.85Ca0.15Ce2O7+δ、Nd1.85Sr0.15Ce2O7+δAnd Nd1.85Ba0.15Ce2O7+δPutting the powder into a die, preparing a wafer with the diameter of 12mm +/-0.1 mm and the thickness of 2mm +/-0.1 mm under the pressure of 150MPa, heating the wafer to 800 ℃ at the heating speed of 5 ℃ per minute, heating to 1500 ℃ at the heating speed of 3 ℃ per minute, and preserving the heat for 5 +/-0.1 hours to obtain the required electrolyte wafer.
Conductivity test method:
the ac conductance of the electrolyte was measured by the two-terminal method. Nd obtained after sintering at 1500 +/-10 ℃ for 5 +/-0.1 hours1.85Mg0.15Ce2O7+δ、Nd1.85Ca0.15Ce2O7+δ、Nd1.85Sr0.15Ce2O7+δ、Nd1.85Ba0.15Ce2O7+δCoating silver paste on two sides of the electrolyte wafer, and then roasting for 2h at 450 ℃ to obtain the silver electrode. Silver electrodes at two ends are connected with an alternating current impedance instrument by silver wires. The AC impedance meter is an interfacial 1000 electrochemical workstation manufactured by Gamry of America, the application potential is 10mV, the frequency range is measured to be 1Hz-1MHz, the temperature for measuring the AC conductance is 350-700 ℃, and the measurement is carried out once every 50 ℃ in the air atmosphere. The conductivity is calculated using the following formula:
wherein, sigma is electrolyte conductivity, S/cm;
h is the thickness of the electrolyte sheet, cm;
r is electrolyte resistance, omega;
s is the cross section area of the electrolyte sheet in cm2。
Nd1.85Mg0.15Ce2O7+δ、Nd1.85Ca0.15Ce2O7+δAnd Nd1.85Sr0.15Ce2O7+δ、Nd1.85Ba0.15Ce2O7+δAt wet 5% H2The ion conductivity of the Nd and 95 percent Ar mixed atmosphere at 700 ℃ respectively reaches 0.0154S/cm, 0.0097S/cm, 0.0186S/cm and 0.0102S/cm, and the Nd is pure2Ce2O7The concentration of the solution is 0.0086S/cm at 700 ℃ in an air atmosphere.
FIG. 1 shows Nd2Ce2O7、Nd1.85Mg0.15Ce2O7+δ、Nd1.85Ca0.15Ce2O7+δ、Nd1.85Sr0.15Ce2O7+δAnd Nd1.85Ba0.15Ce2O7+δAt 5% H wet2And a conductivity test chart at different temperatures in a 95% Ar mixed atmosphere. As can be seen from the figure, the ionic conductivities at 700 ℃ reach 0.0154S/cm, 0.0097S/cm, 0.0186S/cm and 0.0102S/cm respectively, while pure Nd2Ce2O7The concentration of the solution is 0.0086S/cm at 700 ℃ in an air atmosphere.
FIG. 2 shows Nd2Ce2O7(NDC)、Nd1.85Mg0.15Ce2O7+δ(NMDC)、Nd1.85Ca0.15Ce2O7+δ(NCDC)、Nd1.85Sr0.15Ce2O7+δ(NSDC) and Nd1.85Ba0.15Ce2O7+δ(NBDC) samples were separately in different atmospheres: the heat preservation in water at 80 ℃ for 24 hours, the heat preservation in wet hydrogen at 700 ℃ for 24 hours, and the heat preservation in carbon dioxide at 700 ℃ for 24 hours, then XRD shows that: nd doped with alkaline earth metal (Mg, Ca, Sr, Ba)2Ce2O7The electrolyte has good stability in different atmospheres.
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 (4)
1. An electrolyte for an intermediate-temperature solid oxide fuel cell, characterized in that: alkaline earth metal doped proton conducting electrolyte with chemical formula of Nd1.85M0.15Ce2O7+δ，0>δ>-0.075, M is one of Mg, Ca, Sr, Ba.
2. A method of preparing the electrolyte of claim 1, wherein: a nitrate-sol-gel-combustion method is adopted.
3. The method of claim 2, wherein: the method comprises the following specific steps:
(1) adding a citric acid solution into a mixed solution of Nd, Ce and an alkaline earth metal nitrate;
(2) dropwise adding ammonia water, and adjusting the pH value of the solution to 7;
(3) magnetically stirring at constant temperature of 70 ℃ until gel is formed, and heating until self-propagating combustion occurs to form fluffy oxide powder;
(4) heating the oxide powder to 800 +/-10 ℃, preserving heat for 3 +/-0.1 hours, naturally cooling, fully grinding, and preparing a wafer with the diameter of 12 +/-0.1 mm and the thickness of 2 +/-0.1 mm under the pressure of 150 MPa; heating to 800 ℃ at the speed of 5 ℃ per minute, heating to 1500 +/-10 ℃ at the speed of 3 ℃ per minute, and preserving the heat for 5 +/-0.1 hours to obtain the electrolyte of the intermediate-temperature solid oxide fuel cell.
4. The method of claim 3, wherein: the molar ratio of the metal cations to the citric acid is 1: 1.5; the mass concentration of the ammonia water is 15-20%.
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Cited By (2)
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| WO2022145659A1 (en) * | 2020-12-31 | 2022-07-07 | Samsung Electro-Mechanics Co., Ltd. | All-solid-state battery |
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