CN109841841B - High-temperature fuel cell cathode material and preparation and application thereof - Google Patents
High-temperature fuel cell cathode material and preparation and application thereof Download PDFInfo
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- CN109841841B CN109841841B CN201711221222.6A CN201711221222A CN109841841B CN 109841841 B CN109841841 B CN 109841841B CN 201711221222 A CN201711221222 A CN 201711221222A CN 109841841 B CN109841841 B CN 109841841B
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Abstract
The patent provides a high-temperature fuel cell cathode material and preparation and application thereof. The cathode material is characterized by being formed by compounding YSZ, LNF and LDC, wherein YSZ is preferentially prepared on an electrolyte membrane, the size of YSZ particles is 50-500 nanometers, and the porosity is 20-80%; the size of LNF and LDC particles is 5-100 nanometers, and the LNF and LDC particles are uniformly dispersed on the surface of YSZ particles. On the cathode, active sites of oxygen reduction reaction are distributed among LNF and YSZ and LNF and LDC nano particles, and the oxygen reduction reaction rate is greatly accelerated. The battery adopting the cathode takes air as an oxidant at 800 ℃, and the output power reaches 2W/cm2And (3) stably running for 500 hours without attenuation. The invention can obviously improve the performance and stability of the high-temperature fuel cell and has great significance for promoting the practicability of the high-temperature fuel cell.
Description
Technical Field
The invention relates to the field of high-temperature fuel cells, in particular to a high-temperature fuel cell cathode material and preparation and application thereof.
Background
High temperature fuel cells, also known as Solid Oxide Fuel Cells (SOFC), or ceramic fuel cells, convert the chemical energy of a fuel into electrical energy at high temperatures, and are a highly efficient, clean, low-carbon power generation technology. In recent years, in order to solve the problems of cost, service life, reliability and the like faced by the practical application of high-temperature fuel cells, the development of medium-low temperature solid oxide fuel cells is focused at home and abroad, and the research and development focuses on improving the output power of the cells at medium-low temperature (600-.
The membrane electrode of the high-temperature fuel cell has a sandwich structure, a compact electrolyte membrane is positioned in the middle layer, and porous anode layers and cathode layers are arranged on two sides of the compact electrolyte membrane. The cathode is the position where the oxygen reduction reaction occurs, and plays the roles of transmitting oxygen molecules, electrons and oxygen ions and catalyzing the electrochemical reduction of the oxygen molecules. As the operating temperature decreases, the polarization loss of the cathode increases significantly, resulting in a significant decrease in battery performance, and the development of high performance cathode structures and materials has become a hot issue in the art. The electrochemical performance of the cathode is closely related to its microstructure. For example, increasing the reactive sites on the cathode and increasing the length of the electrode-electrolyte-gas three-phase interface can reduce the loss of activation polarization [ J.Fleig/J.Power Sources 105(2002) 228-; T.Horta, K.Yamaji, N.Sakai, Y.Xiong, T.Kato, H.Yokokawa, T.Kawada/J.Power Sources 106(2002) 224-230), the oxygen ion and electron transport network of the reinforced membrane electrode can greatly reduce ohmic polarization loss, and the reasonable pore size distribution in the electrode is beneficial to the diffusion of hydrogen or oxygen, and the concentration polarization is reduced.
In the preparation of membrane electrodes, a high-temperature co-sintering method is generally adopted to prepare a cathode on an electrolyte membrane. In order to realize good combination between the electrode and the electrolyte, the sintering temperature is generally above 1000 ℃, so that the mesoporous structure of the electrode is single, and the requirements of strengthening gas phase mass transfer, increasing reaction active sites and prolonging the length of a three-phase interface can not be met at the same time. The invention provides a high-temperature fuel cell cathode material, which is a composite cathode consisting of YSZ, LNF and LDC. In the composite cathode, YSZ has a high oxygen ion conductivity, conducting oxygen ions to the electrolyte; LNF has very high electron conductivity and matches the coefficient of thermal expansion of YSZ, can transport electrons; LDC has higher catalytic oxygen reduction activity and catalytic oxygen reduction. In the preparation process of the composite electrode, the YSZ framework with micron-sized macropores is preferentially prepared, the diffusion process of oxygen molecules can be improved, and composite particles with nanoscale LNF and LDC are prepared on the pore channel of the YSZ framework to form a small pore channel, so that the reaction active site can be greatly increased, and the length of a three-phase interface can be prolonged. Thereby realizing higher electrochemical performance output of the cathode.
Disclosure of Invention
The invention provides a high-temperature fuel cell cathode material and preparation and application thereof.
The cathode material of the high-temperature fuel cell is characterized in that:
the cathode material is composed of YSZ (8% mol Y)2O3Stabilized ZrO2)，LNF(LaNi0.6Fe0.4O3) And LDC (La)0.45Ce0.55O2) Wherein YSZ is preferentially prepared on the electrolyte membrane, and the particle size of YSZ is50-500 nm, porosity 20-80%; the size of LNF and LDC particles is 5-100 nanometers, the LNF and LDC particles are uniformly dispersed on the surface of YSZ particles, the mass ratio of LNF to LDC is 20: 80-80: 20, and the mass ratio of the sum of LNF and LDC to YSZ is 30: 70-70: 30.
The size of YSZ particles is preferably 100-300 nanometers, and the porosity is preferably 35-55%;
the LNF particle size is preferably 20-50 nanometers, and the LDC particle size is preferably 10-30 nanometers;
the mass ratio of the LNF to the LDC is preferably 40: 60-60: 40, and the mass ratio of the sum of the LNF and the LDC to the YSZ is preferably 45: 55-55: 45;
the preparation method of the cathode material of the high-temperature fuel cell comprises the following specific processes:
(A) firstly, ultrasonically and uniformly mixing YSZ powder with a proper amount of n-butyl alcohol, PVB (polyvinyl butyral), fish oil, a pore-forming agent and a binder to obtain YSZ slurry, coating the YSZ slurry on a two-in-one YSZ electrolyte membrane consisting of an anode and an electrolyte, and sintering at the firing temperature of 1100-1300 ℃ for 2-5 hours to obtain a YSZ particle framework;
(B) then, preparing an LNF and LDC composite precursor solution: weighing nitrates of La, Ni, Fe and Ce metal ions according to a stoichiometric ratio, dissolving the nitrates into deionized water, adding a complexing agent after the nitrates are completely dissolved, adjusting the pH of a system to clarify the system, and controlling the total concentration of the metal ions in a precursor solution to be 0.5-2 mol/L;
(C) and (C) finally, soaking the LNF and LDC composite precursor solution prepared in the step (B) into a YSZ particle skeleton, sintering at 800 ℃ for 1h, repeatedly soaking the precursor solution, and sintering at 800 ℃ until the mass ratio of the sum of the mass of the LNF and the LDC to the mass of the YSZ particle skeleton reaches a target value, thereby obtaining the cathode material.
The pore-forming agent in the step (A) is graphite and/or polymethyl methacrylate (PMMA), the binder is one of polyvinyl alcohol (PVA) or ethyl cellulose, the firing temperature is preferably 1100-1200 ℃, and the adding proportion of the YSZ powder to the n-butyl alcohol, the PVB, the fish oil, the pore-forming agent and the binder is 15: 47.5: 15: 0.5: 15: 7-20: 35: 20: 1: 20: 4 (mass ratio).
In the step (B), the complexing agent is one or more than two of citric acid, ethylene diamine tetraacetic acid and urea, the total concentration of metal ions in the precursor solution is preferably controlled to be 0.5-2mol/L, and the pH value is adjusted to be 5-6 by ammonia water.
The cathode material and the preparation method thereof are suitable for tubular, flat plate and flat tube type high-temperature fuel cells.
The invention has the beneficial effects that:
the invention provides a high-temperature fuel cell cathode material and preparation and application thereof. At 800 ℃, air is taken as an oxidant, and the output power reaches 2W/cm2And after running for 500h, the performance of the battery is not attenuated.
Detailed description of the preferred embodiment
Example 1 the cathode material was prepared from YSZ-LNF-LDC: YSZ, LNF (LaNi)0.6Fe0.4O3) And LDC (La)0.45Ce0.55O2) And compounding. YSZ powder is 8YSZ (8% mol of Y) produced by TOSOH corporation of Japan2O3Stabilized ZrO2) The YSZ particle size is 100 nanometers, the porosity is 45 percent, the LNF particle size is 30 nanometers, the LDC particle size is 20 nanometers, and the mass ratio of the LNF to the LDC is 50:50, the mass ratio of the sum of the LNF and LDC to the YSZ is 50: 50. The preparation process of the cathode is as follows:
(A) firstly, ultrasonically and uniformly mixing YSZ powder with a proper amount of n-butyl alcohol, PVB, fish oil, graphite and polyvinyl alcohol (PVA) according to a mass ratio of 15: 47.5: 15: 0.5: 15: 7, obtaining YSZ slurry, coating the YSZ slurry on a two-in-one YSZ electrolyte membrane, and sintering at the firing temperature of 1200 ℃ for 2h to obtain a YSZ particle framework;
(B) then, preparing an LNF and LDC composite precursor solution: according to the mass ratio of LNF to LDC of 50:50, nitrate of La, Ni, Fe and Ce metal ions is weighed and dissolved in deionized water, complexing agent citric acid (the molar ratio of the metal ions to the citric acid is 1:1) is added after the nitrate is completely dissolved, ammonia water (1/5 of the total volume) is used for adjusting the pH of the system to be clear, and the total concentration of the metal ions in the precursor solution is controlled to be 1 mol/L;
(C) and finally, dipping the precursor solution in the step B) into a YSZ particle skeleton, sintering at 800 ℃ for 1h, repeatedly dipping the precursor solution, and sintering at 800 ℃ until the mass ratio of the sum of the LNF and the LDC to the YSZ particle skeleton reaches 50:50, thereby obtaining the cathode material. The cathode material and the preparation method thereof are suitable for tubular, flat plate and flat tube type high-temperature fuel cells.
The cathode material is applied to a flat-plate anode-supported battery, and the output power reaches 2.20W/cm at 800 ℃ by taking air as an oxidant2And after running for 500h, the performance of the battery is not attenuated.
Example 2 the cathode material was compounded with YSZ-LNF-LDC. The YSZ particle size is 500 nanometers, the porosity is 50 percent, the LNF particle size is 50 nanometers, the LDC particle size is 30 nanometers, and the mass ratio of the LNF to the LDC is 60:40, the mass ratio of the sum of the LNF and LDC to YSZ was 55: 45. The preparation process of the cathode is as follows:
(A) firstly, ultrasonically and uniformly mixing YSZ powder with a proper amount of n-butyl alcohol, PVB, fish oil, polymethacrylic acid and ethyl cellulose, wherein the mass ratio is 20: 35: 20: 1: 20: 4, obtaining YSZ slurry, coating the YSZ slurry on a two-in-one YSZ electrolyte membrane, and sintering at the firing temperature of 1150 ℃ for 3 hours to obtain a YSZ particle framework;
(B) then, preparing an LNF and LDC composite precursor solution: according to the mass ratio of LNF to LDC of 60:40, nitrate of La, Ni, Fe and Ce metal ions is weighed and dissolved in deionized water, complexing agent ethylene diamine tetraacetic acid (the molar ratio of the metal ions to citric acid is 1:1) is added after the nitrate is completely dissolved, ammonia water (1/5 of the total volume) is used for adjusting the pH of the system to clarify the nitrate, and the total concentration of the metal ions in the precursor solution is controlled to be 2 mol/L;
(C) and finally, dipping the precursor solution in the step 2) into a YSZ particle framework, sintering at 800 ℃ for 1h, repeatedly dipping the precursor solution, and sintering at 800 ℃ until the mass ratio of the sum of the LNF and the LDC to the YSZ particle framework reaches 55:45, thereby obtaining the cathode material.
The cathode material is applied to a flat plateThe plate type anode is supported on a cell, air is taken as an oxidant at 800 ℃, and the output power reaches 2.05W/cm2And after running for 500h, the performance of the battery is not attenuated.
Claims (8)
1. The cathode material of the high-temperature fuel cell is characterized in that the cathode material is formed by compounding YSZ, LNF and LDC, wherein YSZ is firstly prepared on an electrolyte membrane, the size of YSZ particles is 50-500 nanometers, and the porosity is 20-80%; the size of LNF and LDC particles is 5-100 nanometers, the LNF and LDC particles are uniformly dispersed on the surface of YSZ particles, the mass ratio of LNF to LDC is 20: 80-80: 20, and the mass ratio of the sum of LNF and LDC to YSZ is 30: 70-70: 30.
2. The cathode material according to claim 1, wherein: the size of YSZ particles is 100-300 nanometers, and the porosity is 35-55 percent.
3. The cathode material of claim 1, wherein the LNF particle size is 20-50 nm and the LDC particle size is 10-30 nm.
4. The cathode material according to claim 1, wherein the mass ratio of LNF to LDC is 40: 60-60: 40, and the mass ratio of the sum of LNF and LDC to YSZ is 45: 55-55: 45.
5. The preparation method of the cathode material of the high-temperature fuel cell according to claim 1, comprising the following steps:
(A) firstly, ultrasonically and uniformly mixing YSZ powder with a proper amount of n-butyl alcohol, PVB (polyvinyl butyral), fish oil, a pore-forming agent and a binder to obtain YSZ slurry, coating the YSZ slurry on a two-in-one YSZ electrolyte membrane consisting of an anode and an electrolyte, and firing at the temperature of 1100-1300 DEG CoSintering for 2-5h under C to obtain a YSZ particle framework;
(B) then, preparing an LNF and LDC composite precursor solution: weighing nitrates of La, Ni, Fe and Ce metal ions according to a stoichiometric ratio, dissolving the nitrates into deionized water, adding a complexing agent after the nitrates are completely dissolved, adjusting the pH of a system to clarify the system, and controlling the total concentration of the metal ions in a precursor solution to be 0.5-2 mol/L;
(C) finally, the composite precursor solution of LNF and LDC prepared in the step (B) is dipped into the YSZ particle skeleton at 800oC sintering for 1h, repeatedly dipping the precursor solution at 800oAnd C, sintering until the mass ratio of the sum of the LNF and the LDC to the YSZ particle skeleton reaches a target value, and obtaining the cathode material.
6. The method according to claim 5, wherein the pore-forming agent in step (A) is graphite and/or polymethyl methacrylate (PMMA), the binder is one of polyvinyl alcohol (PVA) or ethyl cellulose, and the firing temperature is 1100-1200-oC, the adding mass ratio of YSZ powder to n-butyl alcohol, PVB, fish oil, pore-forming agent and binder is 15: 47.5: 15: 0.5: 15: 7-20: 35: 20: 1: 20: 4.
7. the preparation method according to claim 5, wherein the complexing agent in step (B) is one or more of citric acid, ethylenediamine tetraacetic acid and urea, the total concentration of metal ions in the precursor solution is controlled to be 0.5-2mol/L, and the pH value is adjusted to 5-6 by ammonia water.
8. Use of a high temperature fuel cell cathode material as claimed in any one of claims 1 to 6, wherein: the cathode material is suitable for tube type, flat plate type and flat tube type high-temperature fuel cells.
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| CN111621807B (en) * | 2020-05-28 | 2022-04-29 | 华中科技大学 | Electrode material of quasi-symmetrical solid oxide electrolytic cell and preparation method and application thereof |
| CN113523268B (en) * | 2021-05-28 | 2023-02-14 | 嘉庚创新实验室 | Metal fuel particle, metal fuel block and battery thereof |
| CN114045520B (en) * | 2021-12-15 | 2023-05-26 | 中国科学院大连化学物理研究所 | Oxygen electrode for solid oxide electrolysis hydrogen production and preparation method thereof |
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