CN108270024B - Double-doped medium-temperature solid oxide fuel cell electrolyte and preparation method thereof - Google Patents
Double-doped medium-temperature solid oxide fuel cell electrolyte and preparation method thereof Download PDFInfo
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Abstract
The invention adopts a carbonate coprecipitation method to prepare the electrolyte of the proton conduction intermediate-temperature solid oxide fuel cell with high conductivity, and the chemical formula of the electrolyte is La1.9Pr0.05Nd0.05Ce2O7‑δ，0.1>δ>0, the preparation is carried out by adopting a carbonate coprecipitation method, and the relative density reaches 99.9 percent; the electrolyte has conductivity of 0.0081S/cm at 700 deg.C in dry air atmosphere and wet 5% H2The electric conductivity reaches 0.0136S/cm at 700 ℃ in a mixed atmosphere of-95% Ar.
Description
Technical Field
The invention belongs to the technical field of fuel cell materials, and particularly relates to a proton conduction intermediate-temperature solid oxide fuel cell electrolyte with high conductivity and a preparation method thereof.
Background
Energy and environmental issues are major issues facing today's society. At present, it is predominant worldwide
The power generation method mainly burns coal, oil and natural gas. However, these resources are self-reserves limited, and
the combustion process presents serious environmental problems. Therefore, the subject of modern energy technology is to develop new channel
It is beneficial to energy and clean.
Solid Oxide Fuel Cells (SOFC) are one of the effective solutions to alleviate energy problems and their attendant environmental problems. The process of combustion of fossil fuels is an irreversible process, among others
The power supply is accompanied by great waste of efficiency. And the solid oxide fuel cell can bypass combustion
Directly converts chemical energy into electric energy in one process, and the improvement of the efficiency is equal to the energy saving and pollution
The emission reduction of the pollutants, and meanwhile, the reverse process of the SOFC can convert the redundant electric energy into chemical energy, so that the pollution is reduced
Easier to store and transport. Solid oxide fuel cells are increasingly used as clean and efficient energy conversion devices
Is regarded by people as important.
ConventionalSOFCs are often represented by Y2O3Stabilized ZrO2(YSZ) as an electrolyte. Although YSZ is at medium to low temperatures: (<The ionic conductivity at 800 ℃ is very low, and the ionic conductivity meeting the use requirement of SOFCs can be achieved only by working at the high temperature of over 1000 ℃. In a high-temperature working environment, SOFCs have small polarization loss, and do not need to use noble metals as electrode catalysts, but have some problems: the crystal grain of the electrode is coarsened, and the porosity is reduced, so that the activity of the electrode is reduced; the electrolyte and the electrode interdiffuse or react to generate a high-resistance phase, so that the ionic conductivity of the electrolyte is reduced; it is difficult to select a suitable high temperature sealing material. Not only leads to serious attenuation of the battery performance, but also keeps the production cost of the battery high. Therefore, lowering the operating temperature is one of the key issues to reduce production costs and drive the commercialization of SOFCs. However, as the operating temperature of SOFCs decreases, the ohmic resistance of the electrolyte and the polarization resistance of the electrodes increase rapidly, resulting in decreased battery performance. Currently, there are two ways to reduce the ohmic resistance of SOFCs: reducing the film thickness of the electrolyte to reach micron level; improve the conductivity of the existing electrolyte at medium temperature or develop novel medium and low temperature electrolyte. Proton conductors have lower ion conductivity activation energy than oxygen ion conductors, and therefore research on proton conductor electrolytes is an important component in research on low temperature of SOFC. The proton conductor electrolyte can obtain high conductivity under the medium-low temperature working condition so as to meet the requirement of the currently required electrolyte material which can be used for the medium-low temperature SOFC.
Disclosure of Invention
In order to improve the performance of the electrolyte of the medium-low temperature solid oxide fuel cell, a carbonate coprecipitation method is adopted to prepare novel Pr3+And Nd3+Co-doping of La1.9Pr0.05Nd0.05Ce2O7-δThe relative density of the electrolyte sheet after being insulated for 5 hours at 1500 ℃ reaches 99.9 percent; at wet 5% H2The conductivity reaches 0.0136S/cm at 700 ℃ in the mixed atmosphere of-95% Ar, and the electrolyte has the characteristic of effectively reducing the working temperature of the fuel cell.
In order to achieve the purpose, the invention adopts the following technical scheme:
a dual-doped medium-temperature solid oxide fuel cell electrolyte with a chemical formula of La1.9Pr0.05Nd0.05Ce2O7-δ，0.1>δ>0. The preparation method is characterized by adopting a carbonate coprecipitation method and comprises the following steps:
(I) La1.9Pr0.05Nd0.05Ce2O7-δThe preparation of (1):
1) preparing a solution: according to La1.9Pr0.05Nd0.05Ce2O7-δ，0.1>δ>0, stoichiometric weighing of La (NO)3)3·6H2O、Pr(NO3)3·6H2O、Nd(NO3)3·6H2O、Ce(NO3)3·6H2O, weighing ammonium bicarbonate according to the molar ratio of metal ions to the ammonium bicarbonate of 1:2, respectively adding the nitrate into deionized water for dissolving to prepare solutions with different metal ion concentrations, and dissolving the ammonium bicarbonate into the deionized water to prepare a solution with the concentration of 0.1 mol/L;
La(NO3)3·6H2O、Pr(NO3)3·6H2O、Nd(NO3)3·6H2O、Ce(NO3)3·6H2the metal ion concentration of the O solution is 0.3mol/L, 0.1mol/L and 0.5mol/L respectively, then the nitrate solution is mixed and added with deionized water to be diluted until the metal ion concentration is 0.1 mol/L;
2) precipitation reaction: respectively measuring the solutions obtained in the step 1) according to the volume ratio of the metal ion solution to the ammonium bicarbonate solution of 1:4, uniformly stirring the ammonium bicarbonate solution under the condition of water bath at 60 ℃, slowly dripping the metal ion solution into the ammonium bicarbonate solution, and continuously stirring for 30min to obtain a white suspension;
3) and (3) centrifugal washing of a precipitated product: subpackaging the white suspension obtained in the step 2) into 50ml centrifuge tubes, centrifuging at the speed of 8500rpm for 6min to obtain white precipitates, adding deionized water, repeatedly washing twice, finally adding absolute ethyl alcohol, and repeatedly washing twice;
4) drying the white precipitate obtained in the step 3) in an oven at 70 ℃ for 12 h;
5) heating the oxide powder obtained in the step 4) to 800 +/-10 ℃, preserving heat for 3 +/-0.1 hours, and then naturally cooling to form La1.9Pr0.05Nd0.05Ce2O7-δPowder;
(II) preparation of electrolyte
Subjecting the obtained La1.9Pr0.05Nd0.05Ce2O7-δPutting the powder into a die, preparing a wafer under the pressure of 200MPa, heating the wafer to 1500 +/-10 ℃ at the speed of 3 ℃ per minute, and preserving the heat for 5 +/-0.1 hours to obtain the electrolyte wafer.
The product has the advantages and the application:
(1) the advantages are that: protons have the advantages of small volume and light weight, and have lower ion conduction activation energy at medium and low temperatures, so proton-conducting oxides are an electrolyte applicable to SOFCs operating at low temperatures. La2Ce2O7As a proton conductor in CO2And H2Good stability in O, but poor conductivity (5% H in wet)2The electric conductivity at 700 ℃ under the mixed atmosphere of-95% Ar is only 0.0083S/cm), the invention passes through A position Pr3+And Nd3+Co-doping to obtain La1.9Pr0.05Nd0.05Ce2O7-δ（0.1>δ>0) Has better conductivity, the conductivity reaches 0.0081S/cm at 700 ℃ in dry air atmosphere and reaches 5% of wet H2The conductivity reaches 0.0136S/cm at 700 ℃ in the mixed atmosphere of-95% Ar, and the electrolyte is suitable for being applied to medium-low temperature solid oxide fuel cell electrolytes.
(2) The application is as follows: the electrolyte is used for an intermediate-temperature solid oxide fuel cell.
Drawings
FIG. 1 is La1.9Pr0.05Nd0.05Ce2O7-δThe conductivity-temperature relationship curve of the electrolyte under the dry air atmosphere;
FIG. 2 is La1.9Pr0.05Nd0.05Ce2O7-δElectrolyte at 5% H wet2-electrical conductivity-temperature dependence in a 95% Ar mixed atmosphere.
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
La1.9Pr0.05Nd0.05Ce2O7-δ(LPNC) production method
(I) La1.9Pr0.05Nd0.05Ce2O7-δThe preparation of (1):
1) preparing a solution: according to La1.9Pr0.05Nd0.05Ce2O7-δ，0.1>δ>0, stoichiometric weighing of La (NO)3)3·6H2O、Pr(NO3)3·6H2O、Nd(NO3)3·6H2O、Ce(NO3)3·6H2O, weighing ammonium bicarbonate according to the molar ratio of metal ions to the ammonium bicarbonate of 1:2, respectively adding the nitrate into deionized water for dissolving to prepare solutions with different metal ion concentrations, and dissolving the ammonium bicarbonate into the deionized water to prepare a solution with the concentration of 0.1 mol/L;
La(NO3)3·6H2O、Pr(NO3)3·6H2O、Nd(NO3)3·6H2O、Ce(NO3)3·6H2the metal ion concentration of the O solution is 0.3mol/L, 0.1mol/L and 0.5mol/L respectively, then the nitrate solution is mixed and added with deionized water to be diluted until the metal ion concentration is 0.1 mol/L;
2) precipitation reaction: respectively measuring the solutions obtained in the step 1) according to the volume ratio of the metal ion solution to the ammonium bicarbonate solution of 1:4, uniformly stirring the ammonium bicarbonate solution under the condition of water bath at 60 ℃, slowly dripping the metal ion solution into the ammonium bicarbonate solution, and continuously stirring for 30min to obtain a white suspension;
3) and (3) centrifugal washing of a precipitated product: subpackaging the white suspension obtained in the step 2) into 50ml centrifuge tubes, centrifuging at the speed of 8500rpm for 6min to obtain white precipitates, adding deionized water, repeatedly washing twice, finally adding absolute ethyl alcohol, and repeatedly washing twice;
4) drying the white precipitate obtained in the step 3) in an oven at 70 ℃ for 12 h;
5) heating the oxide powder obtained in the step 4) to 800 +/-10 ℃, preserving heat for 3 +/-0.1 hours, and then naturally cooling to form La1.9Pr0.05Nd0.05Ce2O7-δPowder;
(II) preparation of electrolyte
Subjecting the obtained La1.9Pr0.05Nd0.05Ce2O7-δPutting the powder into a die, preparing a wafer under the pressure of 200MPa, heating the wafer to 1500 +/-10 ℃ at the speed of 3 ℃ per minute, and preserving the heat for 5 +/-0.1 hours to obtain the electrolyte wafer.
Specifically, the method comprises the following steps:
1mol of La1.9Pr0.05Nd0.05Ce2O7-δPreparation of (LPNC):
1.9 mol of La (NO) was weighed out3)3·6H2O: 1.9 × 433.00=822.7 g
0.05 mole of Pr (NO) was weighed3)3·6H2O: 0.05 × 435.01=21.7505 g
Weigh 0.05 mol of Nd (NO)3)3·6H2O: 0.05 × 438.35=21.9175 g
Weighing 2 moles of Ce (NO)3)3·6H2O: 2 × 434.22=868.440 g
Weighing 8 moles of ammonium bicarbonate: 8 × 79.06=632.48 g
Adding La (NO)3)3·6H2O、Pr(NO3)3·6H2O、Nd(NO3)3·6H2O、Ce(NO3)3·6H2Respectively adding deionized water to dissolve O and ammonium bicarbonate;
slowly dripping the metal ion solution into an ammonium bicarbonate solution respectively;
heating the mixed solution to 60 deg.C in a stirrer, and stirring at 60 deg.C for 30 min;
centrifuging and washing the white suspension at a centrifuging speed of 8500rpm for 6min to obtain a white precipitate, adding deionized water, repeatedly washing twice, finally adding absolute ethyl alcohol, and repeatedly washing twice; then drying the powder at 70 ℃ for 12 h;
heating the powder to 800 + -10 deg.C, keeping the temperature for 3 + -0.1 hr, and naturally cooling to obtain La1.9Pr0.05Nd0.05Ce2O7-δAnd (3) powder.
Example 2
Preparation of the wafer: la prepared in example 11.9Pr0.05Nd0.05Ce2O7-δPutting the powder into a die, preparing a wafer under the pressure of 200MPa, heating the wafer to 1500 +/-10 ℃ at the heating speed of 3 ℃ per minute, and keeping the temperature for 5 +/-0.1 hours to obtain the required electrolyte sheet.
Conductivity test method:
the ac conductance of the electrolyte was measured by the two-terminal method. La obtained after sintering at 1500 + -1 deg.C for 5 + -0.1 hr1.9Pr0.05Nd0.05Ce2O7-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. And connecting the current collectors at the two ends with an alternating current impedance instrument by using silver wires. The AC impedance meter is an electrochemical workstation with Interface1000 type of GARY electrochemical instrument, the AC amplitude potential is 10mV, the measurement frequency range is 0.1Hz-1MHz, the temperature range for measuring the AC impedance is 350-750 ℃, and the AC impedance is measured in a dry air atmosphere or in a wet 5% H2Measured under a mixed atmosphere of-95% Ar, and EIS was measured every 50 ℃. The conductivity is calculated using the following formula:
wherein, sigma is electrolyte conductivity, S/cm;
h is the thickness of the electrolyte sheet in cm;
r is electrolyte resistance with unit omega;
s is the cross-sectional area of the electrolyte sheet in cm2。
The ionic conductivity at 700 deg.C in dry air atmosphere is 0.0081S/cm, and the ionic conductivity in wet 5% H2The ionic conductivity at 700 ℃ in a mixed atmosphere of-95% Ar was 0.0136S/cm.
The application is as follows: the electrolyte is used for an intermediate-temperature solid oxide fuel cell.
La1.9Pr0.05Nd0.05Ce2O7-δThe conductivity-temperature relationship of the electrolyte is shown in fig. 1 and fig. 2.
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 (2)
1. The electrolyte of the double-doped medium-temperature solid oxide fuel cell is characterized in that the electrolyte has a chemical formula of La1.9Pr0.05Nd0.05Ce2O7-δ，0.1>δ>0。
2. The preparation method of the electrolyte of the double-doped medium-temperature solid oxide fuel cell according to claim 1, which is characterized by adopting a carbonate coprecipitation method, and the preparation method comprises the following steps:
(I) La1.9Pr0.05Nd0.05Ce2O7-δThe preparation of (1):
1) preparing a solution: according to La1.9Pr0.05Nd0.05Ce2O7-δ，0.1>δ>0, stoichiometric weighing of La (NO)3)3·6H2O、Pr(NO3)3·6H2O、Nd(NO3)3·6H2O、Ce(NO3)3·6H2O, weighing ammonium bicarbonate according to the molar ratio of the total mole of all metal ions to the ammonium bicarbonate of 1:2, respectively adding the nitrate into deionized water for dissolving to prepare solutions with different metal ion concentrations, and dissolving the ammonium bicarbonate into the deionized water to prepare a solution with the concentration of 0.1 mol/L;
La(NO3)3·6H2O、Pr(NO3)3·6H2O、Nd(NO3)3·6H2O、Ce(NO3)3·6H2the metal ion concentration of the O solution is respectively 0.3mol/L, 0.1mol/L and 0.5mol/L, then the nitrate solution is mixed and added with deionized water to be diluted until the metal ion concentration is 0.1 mol/L;
2) precipitation reaction: respectively measuring the solutions obtained in the step 1) according to the volume ratio of the metal ion solution to the ammonium bicarbonate solution of 1:4, uniformly stirring the ammonium bicarbonate solution under the condition of water bath at 60 ℃, slowly dripping the metal ion solution into the ammonium bicarbonate solution, and continuously stirring for 30min to obtain a white suspension;
3) and (3) centrifugal washing of a precipitated product: subpackaging the white suspension obtained in the step 2) into 50ml centrifuge tubes, centrifuging at the speed of 8500rpm for 6min to obtain white precipitates, adding deionized water, repeatedly washing twice, finally adding absolute ethyl alcohol, and repeatedly washing twice;
4) drying the white precipitate obtained in the step 3) in an oven at 70 ℃ for 12 h;
5) heating the oxide powder obtained in the step 4) to 800 +/-10 ℃, preserving heat for 3 +/-0.1 hours, and then naturally cooling to form La1.9Pr0.05Nd0.05Ce2O7-δPowder;
(II) preparation of electrolyte
Subjecting the obtained La1.9Pr0.05Nd0.05Ce2O7-δPutting the powder into a die, preparing a wafer under the pressure of 200MPa, heating the wafer to 1500 +/-10 ℃ at the speed of 3 ℃ per minute, and preserving the heat for 5 +/-0.1 hours to obtain the electrolyte wafer.
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| CN106684412A (en) * | 2017-01-11 | 2017-05-17 | 福州大学 | Proton conduction intermediate-temperature solid oxide fuel cell electrolyte and preparation method thereof |
| CN107221690A (en) * | 2017-06-07 | 2017-09-29 | 福州大学 | A kind of codope intermediate temperature solid oxide fuel cell electrolyte |
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| SG11201504840XA (en) * | 2012-12-19 | 2015-07-30 | Lg Fuel Cell Systems Inc | Fuel cell system with interconnect |
| CN107134584B (en) * | 2017-04-24 | 2020-06-12 | 福州大学 | Medium-temperature solid oxide fuel cell electrolyte and preparation method thereof |
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| CN107221690A (en) * | 2017-06-07 | 2017-09-29 | 福州大学 | A kind of codope intermediate temperature solid oxide fuel cell electrolyte |
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