CN114709457B - 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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- 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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Abstract
The invention provides a double-doped medium-temperature solid oxide fuel cell electrolyte and a preparation method thereof, wherein the medium-temperature solid oxide fuel cell electrolyte with high structural stability and excellent conductivity is prepared by adopting a sol-gel-combustion method, and the chemical formula of the medium-temperature solid oxide fuel cell electrolyte is Sr 10.9 Li 0.1 Mo 3 Ta 1.0 O 23‑δ . The electrolyte has excellent structural stability in medium-high temperature environment, and the ionic conductivity reaches 0.013S/cm at 800 ℃ in air atmosphere, so that the requirement of the medium-temperature solid oxide fuel cell on electrolyte materials is met.
Description
Technical Field
The invention belongs to the technical field of fuel cell electrolytes, and particularly relates to a double-doped medium-temperature solid oxide fuel cell electrolyte and a preparation method thereof.
Background
One of the problems in today's society that is in need of solution is the development of sustainable energy sources to address the environmental crisis raised by global warming and the exploitation of limited natural mineral resources. Advanced energy conversion and storage technologies, such as: fuel cells, lithium batteries, solar cells, and the like are being urgently developed. Fuel cells are one of the most leading technologies in future energy production systems, and have attracted attention for their excellent characteristics of high power generation efficiency, no corrosion, low pollution, etc., and are considered as one of the best green energy schemes.
The Solid Oxide Fuel Cell (SOFC) has the characteristics of high energy conversion efficiency, low cost and good long-term stability. The SOFC can use various carbon-containing fossil fuels as fuels, and the fuels are not directly combusted in the energy conversion process, so that the energy conversion efficiency is greatly improved, and the generation of toxic gases, dust and other pollutants is avoided or reduced. The working temperature of the SOFC is 500-1000 ℃, the byproducts are high-quality heat and water vapor, and the energy utilization rate can be up to about 80% under the condition of combined heat and power supply, and the SOFC has the characteristics of cleanness and high efficiency.
The working temperature of the SOFC which is commercially used at present is generally 1000 ℃, and the long-time running of the cell at the high temperature can cause the electrolyte to react with the electrode to form a high-resistance interface, so that the conductivity is reduced; electrode sintering, porosity and catalytic performance are reduced; the components are cracked due to stress generated at the interface due to the non-uniform thermal expansion coefficient, so that the safety and stability of the battery are greatly reduced. Therefore, lowering the operating temperature of the SOFC is effective in reducing its system cost and improving its stability. The electrolyte material can obtain excellent structural stability and high conductivity at medium and high temperature, and meets the requirements of medium-temperature SOFC electrolyte materials.
Disclosure of Invention
The invention aims to provide a double-doped medium-temperature solid oxide fuel cell electrolyte and a preparation method thereof.
In order to achieve the above purpose, the invention adopts the following technical scheme:
a double-doped medium-temperature solid oxide fuel cell electrolyte has a chemical formula of Sr 10.9 Li 0.1 Mo 3 Ta 1.0 O 23-δ ，0≤δ≤1.1。
The preparation method comprises the following steps:
Sr 10.9 Li 0.1 Mo 3 Ta 1.0 O 23-δ the preparation method of the electrolyte powder comprises the following steps:
1) According to Sr 10.9 Li 0.1 Mo 3 Ta 1.0 O 23-δ Is to weigh Ta 2 O 5 ，Sr(NO 3 ) 2 ，LiNO 3 ，(NH 4 ) 6 Mo 7 O 24 ·4H 2 O, and weighing ethylene glycol and citric acid according to the molar ratio of metal cations to ethylene glycol and citric acid of 1:2:2;
2) Sr (NO) 3 ) 2 ，LiNO 3 ，(NH 4 ) 6 Mo 7 O 24 ·4H 2 Adding O and citric acid into distilled water respectively for dissolution;
3) The Sr (NO) obtained in the step 2) is reacted with 3 ) 2 Solution, liNO 3 Solution, (NH) 4 ) 6 Mo 7 O 24 ·4H 2 The O solution is poured into the citric acid solution in turn, and then Ta is added into the solution 2 O 5 Dripping glycol;
4) Dropwise adding ammonia water with the mass concentration of 15% -20% into the solution to adjust the pH value of the solution to 7-8;
5) Heating the mixed solution obtained in the step 4) to 80 ℃ in a constant-temperature magnetic stirrer, and then keeping the temperature at 80 ℃ for continuous stirring until gel is formed;
6) Transferring the gel into an evaporation dish, and heating on an electric furnace until fluffy oxide powder is formed;
7) Heating the obtained oxide powder to 800+ -10deg.C, maintaining for 2+ -0.1 hr to eliminate residual organic matters, and cooling with furnace at 1100+ -10deg.C for 12+ -0.1 hr to form Sr 10.9 Li 0.1 Mo 3 Ta 1.0 O 23-δ A powder;
Sr 10.9 Li 0.1 Mo 3 Ta 1.0 O 23-δ the preparation method of the electrolyte sheet comprises the following steps:
sr to be prepared 10.9 Li 0.1 Mo 3 Ta 1.0 O 23-δ Ball milling the powder for 10 hours, drying, adding a proper amount of PVB (10 wt.%) as an adhesive, grinding uniformly, taking a proper amount of PVB, pouring the mixture into a mould, preparing a wafer with the diameter of 12+/-0.1 mm and the thickness of 1+/-0.1 mm under the pressure of 100MPa, heating the wafer to 500 ℃ +/-10 ℃ at the speed of 3 ℃/min, preserving heat for 1 hour, discharging the adhesive, heating the wafer to 1300+/-10 ℃ at the speed of 3 ℃/min, and preserving heat for 12+/-0.1 hour to obtain compact Sr 10.9 Li 0.1 Mo 3 Ta 1.0 O 23-δ Electrolyte discs.
The invention has the advantages that:
double layer perovskite oxide Sr 11 Mo 4 O 23 The oxygen ion mobility is high due to the defective frame, so that the oxygen ion mobility can be applied to a solid oxide fuel cell as an electrolyte. But Sr 11 Mo 4 O 23 Unstable phase structure and Sr at 400 DEG C 11 Mo 4 O 23 → SrMoO 4 With a concomitant sharp drop in conductivity, which greatly limits the application of such materials. Aiming at the defects of the material, the invention prepares the novel Sr double-doped with lithium and tantalum by a sol-gel-combustion method 10.9 Li 0.1 Mo 3 Ta 1.0 O 23-δ Electrolyte which does not undergo phase transition at SOFC operating temperature 600-800 ℃, still maintains double perovskite structure, and has higher conductivity than Sr 11 Mo 4 O 23 (8.72X10 at 800 ℃ C.) -3 S/cm). Sr at 800 ℃ under air atmosphere 10.9 Li 0.1 Mo 3 Ta 1.0 O 23-δ The ion conductivity of (C) reaches 0.013S/cm. Thus Sr 10.9 Li 0.1 Mo 3 Ta 1.0 O 23-δ The electrolyte has the characteristics of good structural stability, excellent conductivity and the like, and is a medium-temperature SOFC oxygen ion conductor electrolyte with great potential.
The advantages are that: sr (Sr) 10.9 Li 0.1 Mo 3 Ta 1.0 O 23-δ The electrolyte is a pure oxygen ion conductor, and at the service temperature of the SOFC, sr is always kept 11 Mo 4 O 23 Is perovskite structure of (2) and does not generate Sr 11 Mo 4 O 23 → SrMoO 4 Has the characteristics of stable structure and high conductivity, and is suitable for being applied to medium-temperature solid oxide fuel cells.
The application is as follows: as an electrolyte for a medium temperature solid oxide fuel cell.
Drawings
FIG. 1 is Sr 11 Mo 4 O 23 XRD contrast patterns before and after incubation at 800 ℃ for 24 hours. Sr (Sr) 11 Mo 4 O 23 After the tablets were incubated at 800℃for 24 hours, they had been completely converted to SrMoO 4 ；
FIG. 2 shows Sr prepared according to the present invention 10.9 Li 0.1 Mo 3 Ta 1.0 O 23-δ XRD contrast patterns before and after incubation at 800 ℃ for 24 hours. Sr of the invention 10.9 Li 0.1 Mo 3 Ta 1.0 O 23-δ The electrolyte is kept at 800 ℃ for 24 hoursThe original structure is maintained;
FIG. 3 is Sr 11 Mo 4 O 23 And Sr 10.9 Li 0.1 Mo 3 Ta 1.0 O 23-δ Total conductivity profile of electrolyte at different test temperatures. Sr (Sr) 10.9 Li 0.1 Mo 3 Ta 1.0 O 23-δ The conductivity of the electrolyte is obviously higher than that of Sr 11 Mo 4 O 23 Conductivity of the electrolyte. At 800 ℃, sr 10.9 Li 0.1 Mo 3 Ta 1.0 O 23-δ The conductivity of the electrolyte reaches 0.013S/cm.
Detailed Description
The following examples are provided to illustrate the above features and advantages of the present invention. The method of the invention is a conventional method in the art unless specifically stated otherwise.
Example 1
1.Sr 10.9 Li 0.1 Mo 3 Ta 1.0 O 23-δ The preparation method of the electrolyte powder comprises the following steps:
1) According to Sr 10.9 Li 0.1 Mo 3 Ta 1.0 O 23-δ Is to weigh Ta 2 O 5 ，Sr(NO 3 ) 2 ，LiNO 3 ，(NH 4 ) 6 Mo 7 O 24 ·4H 2 O, and weighing ethylene glycol and citric acid according to the molar ratio of metal cations to ethylene glycol and citric acid of 1:2:2;
2) Sr (NO) 3 ) 2 ，LiNO 3 ，(NH 4 ) 6 Mo 7 O 24 ·4H 2 Adding O and citric acid into distilled water respectively for dissolution;
3) The Sr (NO) obtained in the step 2) is reacted with 3 ) 2 Solution, liNO 3 Solution, (NH) 4 ) 6 Mo 7 O 24 ·4H 2 The O solution is poured into the citric acid solution in turn, and then Ta is added into the solution 2 O 5 Dripping glycol;
4) Dropwise adding ammonia water with the mass concentration of 15% -20% into the solution to adjust the pH value of the solution to 7-8;
5) Heating the mixed solution obtained in the step 4) to 80 ℃ in a constant-temperature magnetic stirrer, and then keeping the temperature at 80 ℃ for continuous stirring until gel is formed;
6) Transferring the gel into an evaporation dish, and heating on an electric furnace until fluffy oxide powder is formed;
7) Heating the obtained oxide powder to 800+ -10deg.C, maintaining for 2+ -0.1 hr to eliminate residual organic matters, and cooling with furnace at 1100+ -10deg.C for 12+ -0.1 hr to form Sr 10.9 Li 0.1 Mo 3 Ta 1.0 O 23-δ A powder;
2.Sr 10.9 Li 0.1 Mo 3 Ta 1.0 O 23-δ the preparation method of the electrolyte sheet comprises the following steps:
sr to be prepared 10.9 Li 0.1 Mo 3 Ta 1.0 O 23-δ Ball milling the powder for 10 hours, drying, adding a proper amount of PVB (10 wt.%) as an adhesive, grinding uniformly, taking a proper amount of PVB, pouring the mixture into a mould, preparing a wafer with the diameter of 12+/-0.1 mm and the thickness of 1+/-0.1 mm under the pressure of 100MPa, heating the wafer to 500+/-10 ℃ at the speed of 3 ℃/min, preserving heat for 1 hour, heating the wafer to 1300+/-10 ℃ at the speed of 3 ℃/min, and preserving heat for 12+/-0.1 hour to obtain compact Sr 10.9 Li 0.1 Mo 3 Ta 1.0 O 23-δ Electrolyte discs.
Specific:
(one) 1 mole Sr 10.9 Li 0.1 Mo 3 Ta 1.0 O 23-δ Preparation of electrolyte powder:
1) 2306.771g (10.9 mol) of Sr (NO 3 ) 2 ，6.895g(0.1mol) LiNO 3 ，529.654g(0.42mol) (NH 4 ) 6 Mo 7 O 24 ·4H 2 O，220.990g(0.5mol) Ta 2 O 5 1862.100g (30 mol) of ethylene glycol and 6304.200g (30 mol) of citric acid;
2) Sr (NO) 3 ) 2 ，LiNO 3 ，(NH 4 ) 6 Mo 7 O 24 ·4H 2 O and citric acid fractionAdding into distilled water respectively for dissolution;
3) The Sr (NO) obtained in the step 2) is reacted with 3 ) 2 Solution, liNO 3 Solution, (NH) 4 ) 6 Mo 7 O 24 ·4H 2 The O solution is poured into the citric acid solution in turn, and then Ta is added into the solution 2 O 5 Dripping glycol;
4) Dropwise adding ammonia water with the concentration of 15wt% into the solution to adjust the pH value of the solution to 7;
5) Heating the mixed solution obtained in the step 4) to 80 ℃ in a constant-temperature magnetic stirrer, and then keeping the temperature at 80 ℃ for continuous stirring until gel is formed;
6) Transferring the gel into an evaporation dish, and heating on an electric furnace until fluffy oxide powder is formed;
7) Heating the obtained oxide powder to 800 deg.C, maintaining for 2 hr to eliminate residual organic matters, maintaining at 1100 deg.C for 12 hr, and cooling with furnace to form Sr 10.9 Li 0.1 Mo 3 Ta 1.0 O 23-δ A powder;
(II) Sr 10.9 Li 0.1 Mo 3 Ta 1.0 O 23-δ The preparation method of the electrolyte sheet comprises the following steps:
sr to be prepared 10.9 Li 0.1 Mo 3 Ta 1.0 O 23-δ Ball milling the powder for 10 hours, drying, adding a proper amount of PVB (10 wt.%) as an adhesive, grinding uniformly, pouring a proper amount of PVB into a mould, preparing a wafer with a diameter of 12mm and a thickness of 1mm under a pressure of 100MPa, heating the wafer to 500 ℃ at a speed of 3 ℃/min, preserving heat for 1 hour, and then heating to 1300 ℃ at a speed of 3 ℃/min, preserving heat for 12 hours to obtain compact Sr 10.9 Li 0.1 Mo 3 Ta 1.0 O 23-δ Electrolyte discs.
The conductivity test method comprises the following steps:
the alternating current conductance of the electrolyte was measured using a two terminal method. Sintering at 1300 ℃ for 12 hours to obtain Sr 10.9 Li 0.1 Mo 3 Ta 1.0 O 23-δ The electrolyte wafer is coated with silver paste on both sides and then at 40Roasting for 2 hours at 0 ℃ to obtain the silver electrode. Silver electrodes at two ends are connected with an alternating current impedance meter by silver wires. The alternating current impedance meter is an Interface 1000 electrochemical workstation of Gamry company, the disturbance potential is 30mV, the measuring frequency range is 0.1Hz-1MHz, the measuring temperature is 450-800 ℃, and the measuring is carried out at 50 ℃ intervals in the air atmosphere. The conductivity was calculated using the following formula:
wherein sigma is electrolyte conductivity, S/cm;
h is the thickness of the electrolyte sheet, and the unit cm;
r is electrolyte resistance, unit omega;
s is the cross-sectional area of the electrolyte sheet, in cm 2 。
The foregoing description is only of the preferred embodiments of the invention, and all changes and modifications that come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein.
Claims (3)
1. A method for preparing a double-doped medium-temperature solid oxide fuel cell electrolyte, which is characterized by comprising the following steps:
1) According to Sr 10.9 Li 0.1 Mo 3 Ta 1.0 O 23-δ Is to weigh Ta 2 O 5 ，Sr(NO 3 ) 2 ，LiNO 3 ，(NH 4 ) 6 Mo 7 O 24 ·4H 2 O, and weighing ethylene glycol and citric acid according to the molar ratio of metal cations to ethylene glycol and citric acid of 1:2:2, wherein delta is more than or equal to 0 and less than or equal to 1.1;
2) Sr (NO) 3 ) 2 ，LiNO 3 ，(NH 4 ) 6 Mo 7 O 24 ·4H 2 Adding O and citric acid into distilled water respectively for dissolution;
3) The Sr (NO) obtained in the step 2) is reacted with 3 ) 2 ，LiNO 3 ，(NH 4 ) 6 Mo 7 O 24 ·4H 2 The O solution is poured into the citric acid solution in turn, and then Ta is added into the solution 2 O 5 Dripping glycol;
4) Dropwise adding ammonia water with the mass concentration of 15% -20% into the solution to adjust the pH value of the solution to 7-8;
5) Heating the mixed solution obtained in the step 4) to 80 ℃ in a constant-temperature magnetic stirrer, and then keeping the temperature at 80 ℃ for continuous stirring until gel is formed;
6) Transferring the gel into an evaporation dish, and heating until fluffy oxide powder is formed;
7) Heating the obtained oxide powder to 800+ -10deg.C, maintaining for 2+ -0.1 hr to eliminate residual organic matters, and cooling with furnace at 1100+ -10deg.C for 12+ -0.1 hr to form Sr 10.9 Li 0.1 Mo 3 Ta 1.0 O 23-δ Electrolyte powder.
2. A double doped intermediate temperature solid oxide fuel cell electrolyte prepared according to the method of claim 1, wherein the fuel cell electrolyte has the chemical formula Sr 10.9 Li 0.1 Mo 3 Ta 1.0 O 23-δ ，0≤δ≤1.1。
3. Use of an electrolyte according to claim 2, characterized in that: for solid oxide fuel cells, the operating temperature of the cell is 800 ℃ ± 10 ℃.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102593467A (en) * | 2012-03-05 | 2012-07-18 | 北京科技大学 | High-conductivity double-perovskite-type anode material and preparation method thereof |
| CN106935889A (en) * | 2017-05-04 | 2017-07-07 | 福州大学 | A kind of intermediate temperature solid oxide fuel cell electrolyte of oxygen ion conduction |
| CN109742414A (en) * | 2019-01-09 | 2019-05-10 | 渤海大学 | A kind of intermediate temperature solid oxide fuel cell cathode material and the preparation method and application thereof |
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| US10020515B2 (en) * | 2016-07-14 | 2018-07-10 | Institute of Nuclear Energy Research, Atomic Energy Council, Executive Yuan, R.O.C. | Strontium magnesium molybdenum oxide material having double perovskite structure and method for preparing the same |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102593467A (en) * | 2012-03-05 | 2012-07-18 | 北京科技大学 | High-conductivity double-perovskite-type anode material and preparation method thereof |
| CN106935889A (en) * | 2017-05-04 | 2017-07-07 | 福州大学 | A kind of intermediate temperature solid oxide fuel cell electrolyte of oxygen ion conduction |
| CN109742414A (en) * | 2019-01-09 | 2019-05-10 | 渤海大学 | A kind of intermediate temperature solid oxide fuel cell cathode material and the preparation method and application thereof |
Non-Patent Citations (1)
| Title |
|---|
| "Preparation and characterization of Ta and monovalent alkali metals (Li, Na, K) co-doping on Sr11Mo4O23 electrolyte for solid oxide fuel cells";Xian Pan, et al.;《Journal of Alloys and Compounds》;第938卷;168482 * |
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