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CN-122011878-A - Preparation method for synthesizing high-entropy spinel oxide coating with electromagnetic wave absorption and corrosion resistance at low temperature

CN122011878ACN 122011878 ACN122011878 ACN 122011878ACN-122011878-A

Abstract

The invention discloses a preparation method for synthesizing a high-entropy spinel oxide coating with electromagnetic wave absorption and corrosion resistance at low temperature, which adopts a hydrothermal method to prepare the high-entropy spinel oxide, has the advantages of simple and feasible process, low synthesis temperature, simple and convenient operation and low cost, and the prepared high-entropy spinel oxide powder material has high purity, can be directly sintered and molded and realizes the electromagnetic wave absorption function, and meanwhile, the high-entropy spinel oxide powder is doped into a resin coating, so that the corrosion resistance of the coating is effectively improved, thereby obtaining a novel coating with electromagnetic wave absorption and corrosion resistance, and effectively solving the problem that the electromagnetic wave absorption coating on the surface of a metal substrate is easy to corrode in the prior art.

Inventors

  • QIAN JUNJIE
  • MA DANDAN
  • Cao Suhang
  • ZHANG XIAOZHEN
  • ZHOU XIAOLING
  • WANG YONGQING

Assignees

  • 景德镇陶瓷大学

Dates

Publication Date
20260512
Application Date
20260119

Claims (8)

  1. 1. The preparation method for synthesizing the high-entropy spinel oxide coating with electromagnetic wave absorption and corrosion resistance at low temperature is characterized by comprising the following steps of: (1) Preparation of nickel-copper-zinc-manganese cobaltate high-entropy spinel oxide precursor liquid (1-1) Dissolving a cobalt source, a nickel source, a copper source, a zinc source and a manganese source in water according to a molar ratio of cobalt to nickel to copper to zinc to manganese=6-10:1-3:1-3, and uniformly stirring to obtain a mixed solution; (1-2) adding urea into the mixed solution according to the molar ratio of cobalt to urea=1:3-6, and stirring for 30-60 min until the solution is uniformly mixed to obtain nickel-copper-zinc-manganese-cobaltate precursor liquid; (2) Preparation of nickel-copper-zinc-manganese cobaltate high-entropy spinel oxide powder material (2-1) Placing the nickel-copper-zinc-manganese cobaltate precursor liquid into a hydrothermal reaction kettle, and performing hydrothermal reaction at the temperature of 95-145 ℃ for 6-30 hours to obtain a reaction product; (2-2) after centrifugal cleaning and drying, heating to 300-600 ℃ at a rate of 2-5 ℃ per minute for sintering treatment, wherein the heat preservation time is 1-3 hours, so as to obtain the high-entropy spinel oxide powder material; (3) Preparation of high-entropy spinel oxide coating with electromagnetic wave absorption and corrosion resistance (3-1) Adding the high-entropy spinel oxide powder material into a coating, and uniformly stirring to obtain a mixed coating with the high-entropy spinel oxide powder material content of 2-10%; And (3-2) polishing, washing and drying the surface of the metal substrate, coating the mixed coating on the surface of the metal substrate, and standing and solidifying to obtain the high-entropy spinel oxide coating with electromagnetic wave absorption and corrosion resistance.
  2. 2. The method for preparing the high-entropy spinel oxide coating with electromagnetic wave absorption and corrosion resistance by low-temperature synthesis according to claim 1, wherein the stirring time in the step (1) is 20-40 min.
  3. 3. The method for preparing the high-entropy spinel oxide coating with electromagnetic wave absorption and corrosion resistance by low temperature synthesis according to claim 1, wherein the reaction product in the step (2-2) is centrifugally washed 3-5 times with water, centrifugally washed 3-5 times with absolute ethyl alcohol, and dried at 60-80 ℃ for 10-24 hours.
  4. 4. The method for preparing the spinel oxide coating with high entropy and electromagnetic wave absorption and corrosion resistance by low temperature synthesis according to claim 1, wherein the coating thickness of the mixed coating in the step (3-2) is 90-110 μm, and the mixed coating is allowed to stand and solidify for 8-24 hours at room temperature.
  5. 5. The method for preparing the high-entropy spinel oxide coating with electromagnetic wave absorption and corrosion resistance according to claim 1, wherein the cobalt source is cobalt nitrate, cobalt chloride, cobalt acetate or cobalt sulfate, the nickel source is nickel nitrate, nickel chloride, nickel acetate or nickel sulfate, the copper source is copper nitrate, copper chloride, copper acetate or copper sulfate, the zinc source is zinc nitrate, zinc chloride, zinc acetate or zinc sulfate, and the manganese source is manganese nitrate, manganese chloride, manganese acetate or manganese sulfate.
  6. 6. The method for preparing the high-entropy spinel oxide coating with electromagnetic wave absorption and corrosion resistance according to claim 1, wherein the high-entropy spinel oxide powder material obtained in the step (2) is in a fluffy sphere shape and is evenly distributed in O, co, zn, cu, ni, mn.
  7. 7. The method for preparing the high-entropy spinel oxide coating with electromagnetic wave absorption and corrosion resistance by low-temperature synthesis according to claim 1 is characterized in that the high-entropy spinel oxide powder material obtained in the step (2) has the microwave absorption performance that the wave absorption loss is-55.75 to-18.56 dB when the frequency is 16.86-17.98 GHz and the matching thickness is 1.70-2.07 mm, and the effective wave absorption bandwidth is 7.13-8.11 GHz when the matching thickness is 2.04-2.79 mm.
  8. 8. The method for preparing the high-entropy spinel oxide coating with electromagnetic wave absorption and corrosion resistance according to claim 1, wherein the high-entropy spinel oxide coating is subjected to salt spray test under the condition of 5% mass fraction of sodium chloride solution, and the salt spray corrosion resistance time is at least 9 days.

Description

Preparation method for synthesizing high-entropy spinel oxide coating with electromagnetic wave absorption and corrosion resistance at low temperature Technical Field The invention relates to the technical field of electromagnetic wave absorbing materials, in particular to a preparation method for synthesizing a high-entropy spinel oxide coating with electromagnetic wave absorbing and corrosion resisting properties at low temperature. Background With the continuous progress of technology and the improvement of life demands of people, in military equipment and civil equipment (such as naval vessel surfaces, torpedo surfaces, inner shell surfaces of mobile phones, etc.), it is required to coat the surfaces of substrates with a coating having an electromagnetic wave absorption function. However, when the electromagnetic wave absorbing coating on the surface of the substrate is in severe environments such as humidity, acid-base salt and the like for a long time, the performance of the wave absorbing material is reduced or the service life of the wave absorbing material is influenced. Therefore, there is an urgent need to develop a coating having both electromagnetic wave absorption and corrosion resistance properties to solve this technical problem. Disclosure of Invention The invention aims to overcome the defects of the prior art, and provides a preparation method for synthesizing a spinel oxide coating with high entropy and electromagnetic wave absorption and corrosion resistance at low temperature, so as to effectively solve the problem that the electromagnetic wave absorption coating on the surface of a metal substrate is easy to corrode in the prior art. The aim of the invention is realized by the following technical scheme: The invention provides a preparation method for synthesizing a high-entropy spinel oxide coating with electromagnetic wave absorption and corrosion resistance at low temperature, which comprises the following steps: (1) Preparation of nickel-copper-zinc-manganese cobaltate high-entropy spinel oxide precursor liquid (1-1) Dissolving a cobalt source, a nickel source, a copper source, a zinc source and a manganese source in water according to a molar ratio of cobalt to nickel to copper to zinc to manganese=6-10:1-3:1-3, and uniformly stirring to obtain a mixed solution; (1-2) adding urea into the mixed solution according to the molar ratio of cobalt to urea=1:3-6, and stirring for 30-60 min until the solution is uniformly mixed to obtain nickel-copper-zinc-manganese-cobaltate precursor liquid; (2) Preparation of nickel-copper-zinc-manganese cobaltate high-entropy spinel oxide powder material (2-1) Placing the nickel-copper-zinc-manganese cobaltate precursor liquid into a hydrothermal reaction kettle, and performing hydrothermal reaction at the temperature of 95-145 ℃ for 6-30 hours to obtain a reaction product; (2-2) after centrifugal cleaning and drying, heating to 300-600 ℃ at a rate of 2-5 ℃ per minute for sintering treatment, wherein the heat preservation time is 1-3 hours, so as to obtain the high-entropy spinel oxide powder material; (3) Preparation of high-entropy spinel oxide coating with electromagnetic wave absorption and corrosion resistance (3-1) Adding the high-entropy spinel oxide powder material into a coating, and uniformly stirring to obtain a mixed coating with the high-entropy spinel oxide powder material content of 2-10%; And (3-2) polishing, washing and drying the surface of the metal substrate, coating the mixed coating on the surface of the metal substrate, and standing and solidifying to obtain the high-entropy spinel oxide coating with electromagnetic wave absorption and corrosion resistance. Further, in the step (1), the stirring time is 20-40 min. And (3) centrifugally cleaning the reaction product in the step (2-2) with water for 3-5 times, centrifugally cleaning the reaction product with absolute ethyl alcohol for 3-5 times, and drying the reaction product at the temperature of 60-80 ℃ for 10-24 hours. And (3) setting the coating thickness of the mixed coating in the step (3-2) to 90-110 mu m, and standing and curing for 8-24 hours at room temperature. In the above scheme, the cobalt source is cobalt nitrate, cobalt chloride, cobalt acetate or cobalt sulfate, the nickel source is nickel nitrate, nickel chloride, nickel acetate or nickel sulfate, the copper source is copper nitrate, copper chloride, copper acetate or copper sulfate, the zinc source is zinc nitrate, zinc chloride, zinc acetate or zinc sulfate, and the manganese source is manganese nitrate, manganese chloride, manganese acetate or manganese sulfate. The high-entropy spinel oxide powder material obtained in the step (2) is in a plush spherical shape, O, co, zn, cu, ni, mn is uniformly distributed, and the microwave absorption performance is that when the frequency is 16.86-17.98 GHz, the matching thickness is 1.70-2.07 mm, the wave absorption loss is-55.75-18.56 dB, and when the matching thicknes