CN110098410B - Synthesis method of cobalt-containing composite cathode material with nano structure - Google Patents
Synthesis method of cobalt-containing composite cathode material with nano structure Download PDFInfo
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Abstract
The invention discloses a method for synthesizing a high-performance cobalt-containing composite cathode material with a solid oxide fuel cell nano structure, which comprises the step of preparing Ce (NO)3)3·6H2O、Gd(NO3)3·6H2Mixing O, complexing agent and deionized water, wherein the complexing agent is a mixture of citric acid and ethylenediamine tetraacetic acid, adding ammonia water, continuously stirring to fully dissolve the mixture, then heating and stirring until the mixture is viscous, and adding PrBa1‑ xCaxCo2O5+δAnd (3) continuously heating and stirring the cathode powder (wherein x is 0-1) to obtain gel, and drying and calcining the gel to obtain the composite cathode material with the nano structure. The invention has the advantages of easily obtained raw materials, simple and stable process, and can obtain the composite cathode particles with nanometer sizes at low preparation cost, the obtained composite cathode material has both electronic conductivity and ionic conductivity, and the nanometer structure of the composite cathode material obviously improves the surface reaction zone of the cathode and shows outstanding electrochemical catalytic activity.
Description
Technical Field
The invention belongs to the technical field of preparation of catalytic materials of fuel cells, and particularly relates to a synthesis method of a high-performance cobalt-containing composite cathode material with a solid oxide fuel cell nano structure.
Background
Solid Oxide Fuel Cells (SOFC) are an important role in the energy structure transformation in the 21 st century, taking advantage of their ability to directly convert chemical energy into electrical energy efficiently and without pollution. The chemical energy of fuels such as hydrogen, synthesis gas and methane is directly converted into electric energy (the cogeneration efficiency is as high as 80%) through electrochemical reaction, and NO caused by direct combustion is avoidedx、SO2And the like. And as one of the key parts of the SOFC, the research on the cathode material can play a significant role in promoting the development of the SOFC. The cobalt-containing perovskite material has outstanding electron/ion mixed conductivity and shows excellent electrochemical catalytic activity in a medium-low temperature region. However, it has some problems of application type, such as surface precipitation of lattice elements, and CO-containing2、SO2And the like, and the long-term stability and thermal cycle stability are poor in an air atmosphere. Recently, the academic community reports a double-layer perovskite cathode material PrBa1-xCaxCo2O5+δ(PBCC) under typical SOFC operating conditions in the presence of CO2Exhibit high ORR catalytic activity and excellent durability in air (Chen Y, Yoo S, Choi Y, et al, A high activity, CO)2-tolerant electrode for the oxygen reduction reaction[J]. Energy &Environmental Science, 2018, 11(9): 2458 and 2458). However, PBCC has a higher phase formation temperature, resulting in a larger particle size and reduced electrocatalytic activity. Gadolinium oxide stabilized cerium oxide (Gd)xCe1-xO2GDC) is a widely used medium and low temperature SOFC electrolyte material with excellent ionic conductivity and surface exchange coefficient. The invention adds GDC into PBCC to increaseAnd adding an effective reaction area of the cathode, and optimizing the ion/electron mixed conductivity and ORR electrochemical catalytic activity of the cathode.
Disclosure of Invention
The invention provides a method for synthesizing a high-performance cobalt-containing composite cathode material with a nano structure of a solid oxide fuel cell. The composite cathode obtained through nano modification can form a fine solid solution with a nano structure at low temperature; meanwhile, the modified body increases the surface active sites of the cathode, optimizes the ORR catalytic activity and obtains the nano-structure composite cathode with high performance and high stability.
The invention is implemented by the following technical scheme:
a method for synthesizing a high-performance solid oxide fuel cell nano-structure cobalt-containing composite cathode material specifically comprises the following steps:
(1) adding Ce (NO)3)3·6H2O、Gd(NO3)3·6H2Mixing O, a complexing agent and deionized water, adding ammonia water, and continuously stirring to fully dissolve all the components to obtain a clear solution;
(2) heating the solution at a certain temperature, adding cathode powder when the solution is evaporated to the bottom and bubbles, and continuously heating and stirring until water is evaporated to obtain gel;
(3) drying the obtained gel at a certain temperature to obtain a composite cathode precursor, grinding the composite cathode precursor, and calcining the ground composite cathode precursor at a certain temperature to obtain a composite cathode material with a nano structure;
the cathode powder is PrBa1-xCaxCo2O5+δWherein x is 0 to 1.
Ce (NO) added in step (1)3)3·6H2O and Gd (NO)3)3·6H2The molar ratio of O is (0.4-0.99) to (0.01-0.6).
The preparation method of the complexing agent in the step (1) comprises the following steps: a mixture of citric acid and EDTA in a molar ratio of (0.1-2.5) to (0.1-2).
The addition amount of the complexing agent in the step (1) is that the molar ratio of EDTA to metal cations in the solution is (1-10) to 1.
And (2) after ammonia water is added in the step (1), the pH value of the clear solution is 4-10.
The heating temperature in the step (2) is 50-500 ℃.
The adding amount of the cathode powder in the step (2) is 10-99% of the weight of the finally obtained composite cathode material.
The temperature for drying the gel in the step (3) is 50-500 ℃, and the drying time is 0.1-50 hours.
The calcining temperature in the step (3) is 400-1200 ℃, and the calcining time is 0.1-20 hours.
The solid oxide fuel cell cathode material is prepared by the method.
The invention has the obvious advantages that
1. The GDC nitrate precursor and the PBCC double perovskite powder are uniformly mixed at the atomic scale by a sol-gel method, and a solid solution is formed at a low temperature, so that the composite cathode powder with a fine nano structure is obtained.
2. The GDC nanometer modifier greatly increases the reaction area of the cathode, improves the ORR catalytic activity and greatly improves the electrical property and stability of the cathode.
3. The preparation method of the composite cathode material provided by the invention has the advantages of easily available raw materials, low equipment requirement and simple and stable preparation process.
Drawings
Figure 1 is a STEM-EDS elemental plane scan of the 20wt% GDC-modified PBCC cathode material obtained in example 1.
Figure 2 is an SEM surface topography map of the 20wt% GDC-modified PBCC cathode material obtained in example 1.
Figure 3 is a discharge curve at different temperatures for a full cell assembled with the 20wt% GDC modified PBCC cathode material obtained in example 1.
FIG. 4 is a 500mA cm full cell assembled with 20wt% GDC modified PBCC cathode material obtained in example 1 at 700 deg.C-2The stability curve was tested for 100h under discharge conditions.
FIG. 5 is pure PrBa without modification0.8Ca0.2Co2O5＋δOf the cathodeSEM surface topography.
FIG. 6 is pure PrBa without modification0.8Ca0.2Co2O5＋δThe cathode assembled full cell is at 750 deg.C and 500mA cm-2The discharge curve was tested before and after 20 hours.
Figure 7 is a discharge curve at 750 ℃ for full cells assembled with GDC-modified PBCC cathode materials of different proportions made in accordance with the present invention.
Detailed Description
The invention is further illustrated by the following examples, without restricting its scope to the following embodiments.
Example 1
(1) Firstly Pr (NO)3)3·6H2O、Ba(NO3)2、Ca(NO3)2·4H2O、Co(NO3)2·6H2Mixing O, CA and EDTA with deionized water according to the molar ratio of 1:0.8:0.2:2:6:4, adding 28wt% ammonia water, and continuously stirring to fully dissolve the mixture, wherein the ratio of the adding volume of the 28wt% ammonia water to the mole number of the EDTA is 10ml:0.01 mol;
(2) continuously stirring the clear solution obtained in the step (1) at 375 ℃, putting the clear solution into an oven to dry all water after the solution forms gel, and then calcining the gel at 1050 ℃ for 5 hours to prepare PBCC cathode powder;
(3) adding Ce (NO)3)3·6H2O、Gd(NO3)3·6H2Mixing O, CA and EDTA with deionized water according to a molar ratio of 0.8:0.2:9:6, adding 28wt% ammonia water, and continuously stirring to fully dissolve the mixture, wherein the addition of the 28wt% ammonia water is used for adjusting the pH value of the solution to 6;
(4) continuously stirring the clarified solution obtained in the step (3) at 250 ℃, adding PBCC cathode powder prepared in the step (2) when the solution is evaporated to the bottom and bubbles, and continuously heating and stirring until the water is evaporated to dryness to obtain mixture gel;
(5) and (4) drying the gel obtained in the step (4) in an oven at 180 ℃ for 10 hours, and then calcining the gel at 650 ℃ for 3 hours to obtain the composite cathode material with the nano structure. Wherein, the PBCC cathode powder accounts for 80 percent of the total mass of the nano composite cathode material.
Figure 1 is a STEM-EDS elemental plane scan of the 20wt% GDC modified PBCC cathode material obtained in this example. As shown in the figure, the GDC and PBCC contain elements uniformly distributed and have fine particle sizes.
Figure 2 is an SEM surface topography of the 20wt% GDC modified PBCC cathode material obtained in this example. As shown, the composite cathode particles have reached nanometer size.
Figure 3 is a discharge curve at different temperatures for a full cell assembled with the 20wt% GDC modified PBCC cathode material obtained in this example. As shown in the figure, the maximum power density of the battery at 750 ℃, 700 ℃, 650 ℃ and 600 ℃ respectively reaches 1.427, 1.019, 1.565 and 0.283W cm-2。
FIG. 4 shows the assembly of a full cell at 750 deg.C and 500 mA-cm with 20wt% GDC modified PBCC cathode material obtained in this example-2The stability curve was tested for 100h under discharge conditions. As shown, there was almost no degradation in the cell performance during the test, and the output voltage reached 0.945V.
Example 2
(1) Firstly Pr (NO)3)3·6H2O、Ba(NO3)2、Ca(NO3)2·4H2O、Co(NO3)2·6H2Mixing O, CA and EDTA with deionized water according to the molar ratio of 1:0.8:0.2:2:6:4, adding 28wt% ammonia water, and continuously stirring to fully dissolve the mixture, wherein the ratio of the adding volume of the 28wt% ammonia water to the mole number of the EDTA is 10ml:0.01 mol;
(2) continuously stirring the clear solution obtained in the step (1) at 375 ℃, putting the clear solution into an oven to dry all water after the solution forms gel, and then calcining the gel at 1050 ℃ for 5 hours to prepare PBCC cathode powder;
(3) adding Ce (NO)3)3·6H2O、Gd(NO3)3·6H2Mixing O, CA and EDTA with deionized water according to a molar ratio of 0.8:0.2:9:6, adding 28wt% ammonia water, and continuously stirring to fully dissolve the mixture, wherein the addition of the 28wt% ammonia water is used for adjusting the pH value of the solution to 6;
(4) continuously stirring the clarified solution obtained in the step (3) at 250 ℃, adding PBCC cathode powder prepared in the step (2) when the solution is evaporated to the bottom and bubbles, and continuously heating and stirring until the water is evaporated to dryness to obtain mixture gel;
(5) and (4) drying the gel obtained in the step (4) in an oven at 180 ℃ for 10 hours, and then calcining the gel at 650 ℃ for 3 hours to obtain the composite cathode material with the nano structure. Wherein the PBCC cathode powder accounts for 90 percent of the total mass of the nano composite cathode material.
Example 3
(1) Firstly Pr (NO)3)3·6H2O、Ba(NO3)2、Ca(NO3)2·4H2O、Co(NO3)2·6H2Mixing O, CA and EDTA with deionized water according to the molar ratio of 1:0.8:0.2:2:6:4, adding 28wt% ammonia water, and continuously stirring to fully dissolve the mixture, wherein the ratio of the adding volume of the 28wt% ammonia water to the mole number of the EDTA is 10ml:0.01 mol;
(2) continuously stirring the clear solution obtained in the step (1) at 375 ℃, putting the clear solution into an oven to dry all water after the solution forms gel, and then calcining the gel at 1050 ℃ for 5 hours to prepare PBCC cathode powder;
(3) adding Ce (NO)3)3·6H2O、Gd(NO3)3·6H2Mixing O, CA and EDTA with deionized water according to a molar ratio of 0.8:0.2:9:6, adding 28wt% ammonia water, and continuously stirring to fully dissolve the mixture, wherein the addition of the 28wt% ammonia water is used for adjusting the pH value of the solution to 6;
(4) continuously stirring the clarified solution obtained in the step (3) at 250 ℃, adding PBCC cathode powder prepared in the step (2) when the solution is evaporated to the bottom and bubbles, and continuously heating and stirring until the water is evaporated to dryness to obtain mixture gel;
(5) and (4) drying the gel obtained in the step (4) in an oven at 180 ℃ for 10 hours, and then calcining the gel at 650 ℃ for 3 hours to obtain the composite cathode material with the nano structure. Wherein the PBCC cathode powder accounts for 70 percent of the total mass of the nano composite cathode material.
Example 4
(1) Firstly, the method is carried outPr(NO3)3·6H2O、Ba(NO3)2、Ca(NO3)2·4H2O、Co(NO3)2·6H2Mixing O, CA and EDTA with deionized water according to the molar ratio of 1:0.8:0.2:2:6:4, adding 28wt% ammonia water, and continuously stirring to fully dissolve the mixture, wherein the ratio of the adding volume of the 28wt% ammonia water to the mole number of the EDTA is 10ml:0.01 mol;
(2) continuously stirring the clear solution obtained in the step (1) at 375 ℃, putting the clear solution into an oven to dry all water after the solution forms gel, and then calcining the gel at 1050 ℃ for 5 hours to prepare PBCC cathode powder;
(3) adding Ce (NO)3)3·6H2O、Gd(NO3)3·6H2Mixing O, CA and EDTA with deionized water according to a molar ratio of 0.8:0.2:9:6, adding 28wt% ammonia water, and continuously stirring to fully dissolve the mixture, wherein the addition of the 28wt% ammonia water is used for adjusting the pH value of the solution to 6;
(4) continuously stirring the clarified solution obtained in the step (3) at 250 ℃, adding PBCC cathode powder prepared in the step (2) when the solution is evaporated to the bottom and bubbles, and continuously heating and stirring until the water is evaporated to dryness to obtain mixture gel;
(5) and (4) drying the gel obtained in the step (4) in an oven at 180 ℃ for 10 hours, and then calcining the gel at 650 ℃ for 3 hours to obtain the composite cathode material with the nano structure. Wherein the PBCC cathode powder accounts for 60 percent of the total mass of the nano composite cathode material.
FIG. 5 is pure PrBa without modification0.8Ca0.2Co2O5＋δSEM surface topography of the cathode. Compared with FIG. 2, the overall particle size is much larger, which shows that the method of the present invention can improve the cathode powder structure.
FIG. 6 is pure PrBa without modification0.8Ca0.2Co2O5＋δThe cathode assembled full cell is at 750 deg.C and 500mA cm-2The discharge curve was tested before and after 20 hours. As shown in the figure, the maximum power densities of the battery at 0 hour and 20 hours are 0.770 and 0.611W cm-2。
FIG. 7 is an embodimentThe discharge curves of all batteries assembled by the GDC modified PBCC cathode powder with different proportions prepared in examples 1-4 are 750 ℃. As shown in the figure, the maximum power densities of 10 wt%, 20wt%, 30wt% and 40wt% respectively reach 1.065, 1.503, 1.579 and 1.771W cm-2Much higher than the maximum power density shown in fig. 6. The method of the invention can greatly increase the performance of the cathode.
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 (7)
1. A synthesis method of a high-performance solid oxide fuel cell nano-structure cobalt-containing composite cathode material is characterized by comprising the following steps:
(1) adding Ce (NO)3)3·6H2O、Gd(NO3)3·6H2Mixing O, a complexing agent and deionized water, adding ammonia water, and continuously stirring to fully dissolve all the components to obtain a clear solution;
(2) heating the solution at a certain temperature, adding cathode powder when the solution is evaporated to the bottom and bubbles, and continuously heating and stirring until water is evaporated to obtain gel;
(3) drying the obtained gel at a certain temperature to obtain a composite cathode precursor, grinding the composite cathode precursor, and calcining the ground composite cathode precursor at a certain temperature to obtain a composite cathode material with a nano structure;
the cathode powder is PrBa0.8Ca0.2Co2O5＋δ；
The heating temperature in the step (2) is 50-500 ℃;
in the step (3), the drying temperature of the gel is 50-500 ℃, and the drying time is 0.1-50 hours;
the calcining temperature in the step (3) is 650 ℃, and the calcining time is 0.1-20 hours.
2. The method of synthesis according to claim 1, characterized in that: ce (NO) added in step (1)3)3·6H2O andGd(NO3)3·6H2the molar ratio of O is (0.4-0.99) to (0.01-0.6).
3. The synthesis method according to claim 1, wherein the complexing agent in step (1) is prepared by the following steps: a mixture of citric acid and EDTA in a molar ratio of (0.1-2.5) to (0.1-2).
4. The synthesis method according to claim 1, wherein the complexing agent is added in the step (1) in a molar ratio of EDTA to metal cations in the solution of (1-10): 1.
5. The synthesis method according to claim 1, wherein the pH value of the clear solution is 4-10 after the ammonia water is added in the step (1).
6. The method of synthesis according to claim 1, characterized in that: the adding amount of the cathode powder in the step (2) is 10-99% of the weight of the finally obtained composite cathode material.
7. A solid oxide fuel cell cathode material made according to the method of claim 1.
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