CN115692740A - Method for preparing solid oxide fuel cell composite electrode by direct impregnation - Google Patents
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- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- 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
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Abstract
The invention discloses a method for preparing a solid oxide fuel cell composite electrode by directly dipping ceramic nanorods, which comprises the steps of firstly synthesizing GDC ceramic nanorods by one step by a hydrothermal method, and then mixing the obtained GDC ceramic nanorods with deionized water, absolute ethyl alcohol and PVP to form turbid liquid for dipping an LSM fiber electrode, thereby obtaining the LSM-GDC composite electrode with a nano structure. Compared with the traditional nitrate impregnation method, the method avoids the step of high-temperature calcination, greatly shortens the preparation flow of the battery, and the composite electrode surface nanorods obtained by impregnation by the method are uniformly distributed, so that the cathode surface active sites are increased, and the cathode Oxygen Reduction Reaction (ORR) activity is improved.
Description
Technical Field
The invention belongs to the field of solid oxide fuel cells, and particularly relates to a method for preparing a composite cathode of a solid oxide fuel cell by directly dipping ceramic nanorods.
Background
The Solid Oxide Fuel Cell (SOFC) can directly convert chemical energy in fuel into electric energy, the power generation efficiency can reach 65%, and the combined power generation efficiency with a thermoelectric linkage system can reach 85%. Cathode materials for SOFCs include mainly perovskite structured oxides and metal-based ceramic composite cathode materials, including particularly manganates such as LSM. In the early research stage, the SOFC mainly operates in the temperature range of 800-1000 ℃, the high temperature accelerates the ion transmission and electrode reaction in the electrolyte, and the battery can realize high power output. However, the high-temperature working environment also brings various problems to the SOFC, such as higher running cost, poor sealing performance, poor chemical compatibility and the like, so that the working temperature needs to be reduced to a middle-temperature region of 600-800 ℃. LSM is a pure electronic conductor at medium and low temperatures, lacks oxygen vacancies, and ORR occurs only at the interface of the cathode and electrolyte, hindering its application at medium and low temperatures. The cerium oxide-based material, especially GDC, has high ionic conductivity at medium-low working temperature, and can effectively transfer reaction sites from an LSM electrode/YSZ electrolyte interface to an LSM electrode/GDC nanorod interface in an electrode body by preparing the LSM-GDC composite cathode, thereby enhancing the ORR activity of the cathode.
The method for preparing the nano-structure composite cathode material at present generally comprises the steps of preparing a porous framework, then impregnating a precursor solution containing nitrate on the surface of a substrate material, and calcining the mixture at a certain temperature to form a phase. However, such a preparation method has many problems, such as poor chemical compatibility of two phases during calcination, low cyclic impregnation-calcination efficiency, poor continuity and uniformity of surface attachments, and the like. The direct ceramic particle impregnation method can reduce the cycle times required by impregnation-calcination, does not need subsequent high-temperature calcination steps, shortens the electrode preparation time, and adopts the direct ceramic particle impregnation to prepare the composite cathode, so that the electrochemical activity, the stability and other properties of the LSM cathode can be optimized, the overall performance of the SOFC cathode is further improved, and the direct ceramic particle impregnation method has a better application prospect.
Disclosure of Invention
The invention aims to provide a method for preparing a solid oxide fuel cell composite electrode by directly impregnating ceramic nanorods. The introduction of the nano rod can increase the surface active sites of the cathode, improve the ORR activity and ensure that the cathode has high performance and high stability. Compared with the traditional nitrate impregnation method, the method avoids the traditional high-temperature calcination step, and greatly shortens the preparation process of the battery.
In order to realize the purpose, the invention adopts the following technical scheme:
a method for preparing a solid oxide fuel cell composite electrode by directly dipping ceramic nanorods comprises the following steps:
(1) Ce (NO) 3 ) 3 ·6H 2 O and Gd (NO) 3 ) 3 ·6H 2 Dissolving O in deionized water, and adding a surfactant to prepare a solution A; dissolving a certain amount of mineralizer in deionized water to prepare solution B; dropwise adding the solution B into the solution A until no precipitate is generated, placing the solution B into a hydrothermal kettle, reacting at a certain temperature, centrifugally separating the precipitate after the reaction is finished, washing with distilled water, and drying to obtain Gd 0.1 Ce 0.9 O 1.95 (GDC) ceramic nanorods;
(2) Adding the obtained ceramic nano-rod into a mixed solution of deionized water and absolute ethyl alcohol, adding a dispersing agent, stirring to obtain a uniformly dispersed suspension, and then directly dipping La into the suspension 0.8 Sr 0.2 MnO 3-δ And (LSM) drying the (LSM) fiber electrode at a certain temperature to obtain the LSM-GDC composite electrode with the nano structure.
Further, the surfactant used in the step (1) is polyethylene glycol 400 (PEG-400), and the dosage of the surfactant is 0.1 to 1 percent of the total mass of the solution A.
Further, the mineralizer in the step (1) is KOH, and the concentration of the prepared solution B is 1-12M.
Further, the reaction temperature in the step (1) is 80-200 ℃, and the reaction time is 12-24 h.
Further, the volume ratio of the deionized water to the absolute ethyl alcohol in the mixed solution in the step (2) is 1 to 9.
Further, the dispersant in the step (2) is PVP, and the dosage of the dispersant accounts for 0.1 to 1 percent of the total mass of the obtained suspension.
Further, the content of the ceramic nano-rods in the suspension obtained in the step (2) is 0.1 to 0.3M.
Further, the amount of the suspension used in the impregnation in the step (2) is from 1 to 5 mg. Cm -2 。
Further, the drying temperature in the step (2) is 80-150 ℃, and the drying time is 1-5 h.
The LSM-GDC composite electrode prepared by the method can be used as a cathode material of a solid oxide fuel cell.
The invention has the following remarkable advantages:
(1) The method adopts a hydrothermal method to synthesize the GDC ceramic nanorods in one step, GDC can directly form a phase in a hydrothermal kettle, a subsequent calcination phase forming step is not needed, and energy consumption is reduced.
(2) The fiber structure cathode and the nano-rod-shaped GDC have high specific surface area, can provide a longer three-phase reaction interface, and increase the surface active sites of the cathode, thereby improving the ORR activity.
(3) Compared with the traditional nitrate impregnation method, the method for directly impregnating the ceramic nanorods avoids the subsequent calcining step, reduces the energy consumption and avoids the adverse chemical reaction possibly generated by high-temperature calcination. Meanwhile, the traditional method needs cyclic impregnation to improve the uniformity of surface particles, and the direct ceramic nanorod impregnation can realize uniform distribution of the surface particles through one-time impregnation, so that the time for preparing the electrode is greatly shortened.
Drawings
FIG. 1 is a transmission electron microscope image of GDC nanorods synthesized in example 1;
FIG. 2 is a transmission electron micrograph of GDC nanoparticles synthesized in comparative example 1;
FIG. 3 is a graph showing adsorption and desorption curves of GDC nanorods synthesized in example 1 and GDC nanoparticles synthesized in comparative example 1;
fig. 4 is an SEM cross-sectional profile of a pure LSM cathode prepared in example 2;
fig. 5 is an SEM cross-sectional topography of the LSM-GDC composite cathode prepared in example 3;
fig. 6 is a graph showing the results of stability test of a full cell assembled using cathodes prepared in example 2 and example 3;
fig. 7 is an SEM sectional view of the LSM-GDC composite cathode prepared in comparative example 2.
Detailed Description
A method for preparing a solid oxide fuel cell composite electrode by directly dipping ceramic nanorods comprises the following steps:
(1) Adding Ce (NO) according to the required element proportion 3 ) 3 ·6H 2 O and Gd (NO) 3 ) 3 ·6H 2 Dissolving O in deionized water, and adding PEG-400 to prepare a solution A, wherein the content of the PEG-400 is 0.1 to 1wt%; dissolving a certain amount of mineralizer in deionized water to prepare a solution B with the concentration of 1-12M; dropwise adding the solution B into the solution A until no precipitate is generated, placing the solution B into a hydrothermal kettle, reacting at 80-200 ℃ for 12-24h, centrifugally separating the precipitate after the reaction is finished, washing the precipitate with distilled water, and drying to obtain Gd 0.1 Ce 0.9 O 1.95 (GDC) ceramic nanorods;
(2) Adding the obtained ceramic nanorod into a mixed solution of deionized water and absolute ethyl alcohol (1 to 9, v/v), adding a dispersant PVP (polyvinyl pyrrolidone), and stirring to obtain a uniformly dispersed suspension, wherein the content of the ceramic nanorod is 0.1 to 0.3M, and the content of the PVP is 0.1 to 1wt%; then, the concentration of the solution is 1 to 5 mg/cm -2 Amount of La directly impregnated with the suspension 0.8 Sr 0.2 MnO 3-δ And (LSM) drying the (LSM) fiber electrode at the temperature of 80 to 150 ℃ for 1 to 5 hours to obtain the LSM-GDC composite electrode with the nano structure.
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: preparation of GDC ceramic nanorod
(1) Adding 0.009mol Ce (NO) into the beaker 3 ) 3 ·6H 2 O、0.001mol Gd(NO 3 ) 3 ·6H 2 O and 100ml of deionized water, and PEG-400 is added as a surfactant, and the mixture is stirred continuously to be fully dissolved, wherein the adding amount of the PEG-400 accounts for 0.5 percent of the total mass of the solution;
(2) Adding 0.2mol of KOH and 100ml of deionized water into another beaker, and uniformly stirring;
(3) Dropwise adding the solution obtained in the step (2) into the solution obtained in the step (1), putting the solution into a hydrothermal kettle after no precipitate is generated, putting the hydrothermal kettle into a drying oven, and reacting for 24 hours at 200 ℃;
(4) And after the reaction is finished, cooling the hydrothermal kettle to room temperature along with the furnace, centrifugally separating out precipitate, washing the precipitate with deionized water until the pH is =7, putting the washed precipitate into an oven, and drying for 2 hours at 80 ℃ to obtain the GDC material.
FIG. 1 is a transmission electron micrograph of the synthesized GDC material. As shown in the figure, the obtained GDC material is a nanorod, and the average particle size of the nanorod is 5.34nm.
Comparative example 1: preparation of GDC ceramic nanoparticles
(1) Adding 0.009mol Ce (NO) into the beaker 3 ) 3 ·6H 2 O、0.001mol Gd(NO 3 ) 3 ·6H 2 Continuously stirring O and 100ml of deionized water to fully dissolve the O and the deionized water;
(2) Adding 0.2mol of KOH and 100ml of deionized water into another beaker, and uniformly stirring;
(3) Dropwise adding the solution obtained in the step (2) into the solution obtained in the step (1), putting the solution into a hydrothermal kettle after no precipitate is generated, putting the hydrothermal kettle into an oven, and reacting for 24 hours at 200 ℃;
(4) And after the reaction is finished, cooling the hydrothermal kettle to room temperature along with the furnace, centrifugally separating out precipitate, washing the precipitate with deionized water until the pH is =7, putting the washed precipitate into an oven, and drying for 2 hours at 80 ℃ to obtain the GDC material.
FIG. 2 is a transmission electron micrograph of the synthesized GDC material. As shown, the resulting GDC material was round particles with an average particle size of 5.52nm.
Fig. 3 is a graph showing adsorption and desorption curves of the synthesized GDC nanorods and GDC nanoparticles. As shown in the figure, obtainedThe specific surface areas of the GDC nanorods and the nanoparticles are 151.40m respectively 2 (iv)/g and 74.09m 2 The/g proves that the nanorod structure has high specific surface area, can obviously increase the surface active sites of the cathode, improves the ORR activity and enhances the electrochemical activity of the composite cathode.
Example 2: preparation of LSM cathode
(1) Mixing deionized water and DMF at a volume ratio of 50;
(2) Adding La (NO) in stoichiometric ratio 3 ) 3 ·6H 2 O、Sr(NO 3 ) 2 、Mn(NO 3 ) 2 Dissolving the mixture in the mixed solution obtained in the step (1) to obtain a mixed solution with the nitrate concentration of 0.22mol/L, and magnetically stirring the mixed solution until the solution is clear to obtain an LSM electrostatic spinning solution;
(3) Transferring the LSM electrostatic spinning solution prepared in the step (2) into a 10mL injector, connecting the injector to a flow pump, controlling the feeding rate of the solution to be 0.2mL/h, using a stainless steel needle as a nozzle, carrying out electrostatic spinning under 17kV voltage, rotating a collecting roller to collect a fiber precursor, and calcining the fiber precursor at 900 ℃ for 3 hours to prepare the LSM fiber;
(4) Ultrasonically and uniformly mixing 0.05g of the LSM fiber prepared in the step (3) with a binder (0.1 g of PVP is dispersed in 2ml of ethanol) to obtain LSM cathode slurry;
(5) Preparing an anode NiO-YSZ support body by a dry pressing method, and sintering for 2 hours at 1000 ℃; then spin-coating a layer of 12-micron-thick AFL anode functional layer on one side of the anode support body, and calcining for 2 hours at 600 ℃; then spin-coating a layer of YSZ electrolyte layer with the thickness of 10 mu m on the AFL functional layer;
(6) 10 μ L of the cathode slurry was applied by dropping onto YSZ electrolyte (controlled area 0.22 cm) 2 ) And then placing the cell piece on a stirring table, heating the cell piece to 80 ℃, placing the cell piece in a muffle furnace after ethanol is volatilized, and carrying out heat treatment at 600 ℃ for 2 hours to obtain the LSM cathode.
Fig. 4 is an SEM cross-sectional topography of the prepared pure LSM cathode. As can be seen in the figure, the LSM cathode skeleton surface is clean.
Example 3: preparation of LSM-GDC composite electrode
(1) Taking 1ml of ionized water and 1ml of absolute ethyl alcohol by using a liquid-moving gun to prepare a solvent, then adding 0.1g of the GDC nanorod prepared in the example 1 and PVP, and continuously stirring to uniformly disperse all components to obtain a suspension, wherein the content of the PVP is 1wt%;
(2) The dosage is 3.0mg cm -2 And (3) adding the suspension obtained in the step (2) to the LSM cathode prepared in the embodiment 2, and drying at 80 ℃ for 2 hours to obtain the LSM-GDC cathode with the nano structure.
Fig. 5 is an SEM sectional view of the prepared LSM-GDC cathode. Comparing with fig. 4, it can be seen that the surface of the LSM cathode skeleton is uniformly coated with a GDC nanorod coating, which illustrates that the present invention can form a uniform dip coating on the LSM cathode skeleton. The addition of the GDC nanorods can effectively transfer reaction sites from an LSM electrode/YSZ electrolyte interface to an LSM electrode/GDC nanorod interface in the electrode main body, provide more active sites and improve the ORR activity of the cathode.
FIG. 6 shows the total cell assembled by using the cathodes prepared in example 2 and example 3 at 0.5A cm -2 And a discharge curve after discharging for 5h at 750 ℃. As shown in the figure, the maximum power density of the batteries prepared by the pure LSM cathode and the LSM-GDC composite cathode after the stability test is 0.34W cm -2 And 0.5 W.cm -2 。
Comparative example 2: preparation of composite electrode
(1) Taking 1ml of ionized water and 1ml of absolute ethyl alcohol by using a liquid-moving gun to prepare a solvent, then adding 0.1g of GDC nano-particles prepared in the comparative example 1 and PVP, and continuously stirring to uniformly disperse all the components to obtain a suspension, wherein the content of the PVP is 1wt%;
(2) The dosage is 3.0mg cm -2 And (3) adding the suspension obtained in the step (2) to the LSM cathode prepared in the example 2, and drying at 80 ℃ for 2 hours to obtain the LSM-GDC cathode.
Fig. 7 is an SEM cross-sectional topography of the prepared LSM-GDC cathode. As can be seen in comparison with fig. 5, GDC ceramic nanoparticles are stacked on the LSM cathode skeleton and fail to form a uniform coating, further illustrating the better impregnation effect with nanorods.
The above description is only a preferred embodiment of the present invention, and all the equivalent changes and modifications made according to the claims of the present invention should be covered by the present invention.
Claims (10)
1. A method for preparing a solid oxide fuel cell composite electrode by directly dipping ceramic nanorods is characterized by comprising the following steps: the method comprises the following steps:
(1) Ce (NO) 3 ) 3 ·6H 2 O and Gd (NO) 3 ) 3 ·6H 2 Dissolving O in deionized water, and adding a surfactant to prepare a solution A; dissolving a certain amount of mineralizer in deionized water to prepare solution B; dropwise adding the solution B into the solution A until no precipitate is generated, placing the solution B into a hydrothermal kettle, reacting at a certain temperature, centrifugally separating the precipitate after the reaction is finished, washing with distilled water, and drying to obtain Gd 0.1 Ce 0.9 O 1.95 Ceramic nanorods;
(2) Adding the obtained ceramic nano-rod into a mixed solution of deionized water and absolute ethyl alcohol, adding a dispersing agent, stirring to obtain a uniformly dispersed suspension, and then directly dipping La into the suspension 0.8 Sr 0.2 MnO 3-δ And drying the fiber electrode at a certain temperature to obtain the LSM-GDC composite electrode with the nano structure.
2. The method for preparing the composite electrode of the solid oxide fuel cell by directly impregnating the ceramic nanorod according to claim 1, wherein the method comprises the following steps: in the step (1), the surfactant is polyethylene glycol 400, and the dosage of the surfactant accounts for 0.1 to 1 percent of the total mass of the solution A.
3. The method for preparing the composite electrode of the solid oxide fuel cell by directly impregnating the ceramic nanorods according to claim 1, wherein: the mineralizer in the step (1) is KOH, and the concentration of the prepared solution B is 1 to 12M.
4. The method for preparing the composite electrode of the solid oxide fuel cell by directly impregnating the ceramic nanorods according to claim 1, wherein: the reaction temperature in the step (1) is 80-200 ℃, and the reaction time is 12-24 h.
5. The method for preparing the composite electrode of the solid oxide fuel cell by directly impregnating the ceramic nanorods according to claim 1, wherein: and (3) the volume ratio of the deionized water to the absolute ethyl alcohol in the mixed solution in the step (2) is 1 to 9.
6. The method for preparing the composite electrode of the solid oxide fuel cell by directly impregnating the ceramic nanorods according to claim 1, wherein: in the step (2), the dispersing agent is PVP, and the using amount of the dispersing agent accounts for 0.1-1% of the total mass of the obtained suspension.
7. The method for preparing the composite electrode of the solid oxide fuel cell by directly impregnating the ceramic nanorod according to claim 1, wherein the method comprises the following steps: the content of the ceramic nano-rods in the suspension obtained in the step (2) is 0.1 to 0.3M.
8. The method for preparing the composite electrode of the solid oxide fuel cell by directly impregnating the ceramic nanorods according to claim 1, wherein: when the impregnation is carried out in the step (2), the dosage of the suspension is 1 to 5 mg-cm -2 。
9. The method for preparing the composite electrode of the solid oxide fuel cell by directly impregnating the ceramic nanorods according to claim 1, wherein: the drying temperature in the step (2) is 80 to 150 ℃, and the time is 1 to 5 hours.
10. Use of a composite electrode prepared by the method of claim 1 as a cathode material for a solid oxide fuel cell.
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