| CPC C01G 31/006 (2013.01) [C25B 1/50 (2021.01); C25B 11/081 (2021.01); B82Y 30/00 (2013.01); B82Y 40/00 (2013.01); C01P 2004/38 (2013.01); C01P 2004/64 (2013.01); C01P 2006/40 (2013.01)] | 4 Claims |
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1. A preparation method for an A-site high-entropy nanometer metal oxide with high conductivity, comprising the following steps:
(1) taking Gd(NO3)3, Er(NO3)3, La(NO3)3, Nd(NO3)3, Y(NO3)3, ZrOSO4, SnC14 and NH4VO3 at a molar ratio of 0.4:0.3:0.4:0.5:0.4:0.7:0.8:0.5 as a solute, and taking and uniformly mixing deionized water, absolute ethyl alcohol and tetrahydrofuran at a mass ratio of 0.3:3:0.5 to obtain a solvent; adding the solute to the solvent, wherein the ratio of the total mass of the solute to that of the solvent is 12.6%; and performing stirring for 5 to 15 minutes to obtain a mixed liquid I for later use;
(2) taking para-phenylene diamine, hydrogenated tallowamine, sorbitol and carbamyl ethyl acetate at a mass ratio of 1-3:0.2-0.4:7-9:0.01-0.03 as a solute I, and adding the solute I to propyl alcohol, wherein the ratio of the total mass of the solute I to that of the propyl alcohol is 7.5%; and performing stirring for 1-3 hours to obtain a mixed liquid II for later use;
(3) taking the mixed liquid I and the mixed liquid II at a mass ratio of 10-8:4-6; heating the mixed liquid I to 50-70° C., and dripping the mixed liquid II into the mixed liquid I under stirring and ultrasonic conditions to obtain a mixture; after the dripping is completed, heating the mixture to a temperature of 85-95° C.; and stopping stirring and maintaining the temperature of 85-95° C. for 3-7 hours, and decreasing the temperature of 85-95° C. to room temperature to obtain a mixed liquid III;
(4) adding the mixed liquid III to an electrolytic cell with using a platinum electrode as an electrode and applying a voltage of 3-7 V to two ends of the electrode, and reacting for 13-17 minutes, to obtain a mixed liquid IV;
(5) heating the mixed liquid IV to a temperature of 55-65° C. under stirring, and dripping another mixed liquid II into the mixed liquid IV, wherein the mass ratio of the mixed liquid II to the mixed liquid IV is 1.05:1.25; and after the dripping is completed, decreasing the temperature of 55-65° C. to room temperature under stirring condition, to obtain a mixed liquid V;
(6) performing shearing treatment on the mixed liquid V by using a shear mulser, to obtain a mixed liquid VI;
(7) performing lyophilization treatment on the mixed liquid VI to obtain a mixture I;
(8) mixing the mixture I and absolute ethyl alcohol at a mass ratio of 1:2 to obtain a mixture II, uniformly stirring the mixture II and performing solvent thermal treatment under a sealing condition at a temperature of 210-230° C. for 18-24 hours; and cooling the reaction to room temperature, collecting the obtained powder by centrifugation, washing the collected powder respectively with deionized water and absolute ethyl alcohol eight times, and drying to obtain a powder I;
(9) uniformly mixing the powder I and ammonium persulfate at a mass ratio of 10:1 to obtain a mixture III, and heating the mixture III to a temperature of 165-175° C. under the sealing condition, and maintaining the temperature of 165-175° C. for 13-15 hours; and cooling the reaction to room temperature, washing the obtained mixed powder with deionized water ten times, and drying to obtain a powder II; and
(10) placing the powder II into a crucible, heating the the powder II to a temperature of 1500-1700° C., and maintaining the temperature of 1500-1700° C. for 7-9 hours; and cooling the reaction to room temperature, to obtain an A-site high-entropy nanometer metal oxide with high conductivity.
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