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CN-121988749-A - Nano nickel powder and liquid phase preparation method thereof

CN121988749ACN 121988749 ACN121988749 ACN 121988749ACN-121988749-A

Abstract

The application provides a liquid phase preparation method of nano nickel powder, which comprises the following steps of S1 mixing an ethanol solution of a nickel source with hydrazine hydrate, S2 mixing an alkaline ethanol solution with the solution obtained in the step S1, adding a surfactant, S3 reacting the mixed solution obtained in the step S2 under the conditions of stirring and heating, and separating and drying the obtained reaction product to obtain the nano nickel powder. The application also provides the nano nickel powder prepared by the method. According to the application, a nickel source is used as a precursor, hydrazine hydrate is used as a reducing agent, ethanol is used as a solvent, the reaction is carried out under the stirring condition, and the nano nickel powder with the particle size adjustable within the range of 50-300 nm is prepared by regulating and controlling the stirring rate and the surfactant.

Inventors

  • DAI SHUYUN
  • LI TIAN
  • LIU JIE

Assignees

  • 福建贝思科电子材料股份有限公司

Dates

Publication Date
20260508
Application Date
20260324

Claims (10)

  1. 1. The liquid phase preparation method of the nano nickel powder is characterized by comprising the following steps of: S1, mixing an ethanol solution of a nickel source with hydrazine hydrate; s2, mixing the alkaline ethanol solution with the solution obtained in the step S1, and then adding a surfactant; and S3, reacting the mixed solution obtained in the step S2 under the conditions of stirring and heating, and separating and drying the obtained reaction product to obtain the nano nickel powder.
  2. 2. The liquid phase production method according to claim 1, wherein in step S1, the nickel source comprises one or more of nickel acetate, nickel sulfate and nickel chloride, and/or the concentration of the ethanol solution of the nickel source is 0.01 to 0.2mol/L, and/or the molar ratio of the hydrazine hydrate to the nickel source is (5 to 15): 1.
  3. 3. The liquid phase preparation method according to claim 1, wherein in step S2, the preparation method of the alkaline ethanol solution comprises: Dissolving organic alkali or inorganic alkali in ethanol, and stirring to obtain alkaline ethanol solution.
  4. 4. The liquid phase preparation method according to claim 2 or 3, wherein in step S2, the organic or inorganic base in the alkaline ethanol solution includes one or more of sodium hydroxide, potassium hydroxide, and tetramethylammonium hydroxide, and/or the concentration of hydroxyl in the alkaline ethanol solution is 0.1 to 1mol/L.
  5. 5. The method according to claim 4, wherein in the step S2, the volume ratio of the alkaline ethanol solution to the solution obtained in the step S1 is (0.2-0.5): 1, and/or the addition amount of the surfactant is 0.1-10 mmol, and the surfactant comprises one or more of oleic acid, oleylamine and polyethylene glycol.
  6. 6. The method according to claim 1 or 5, wherein in step S2, stirring is further included after the mixing, the stirring time is 1-20 min, and stirring is further included after the surfactant is added, and the stirring time is 1-20 min.
  7. 7. The method according to claim 6, wherein in the step S3, the stirring speed is 0 to 800rpm, and/or the heating temperature is 50 to 150 ℃, and the heating time is 0.5 to 5 hours.
  8. 8. The method according to claim 1, wherein in step S3, the separation is performed by a magnet separation method, and/or the drying is vacuum drying, and the drying temperature is 50-100 ℃ and the time is 2-8 hours.
  9. 9. The nano nickel powder prepared by the liquid phase preparation method according to any one of claims 1 to 8.
  10. 10. The nano-nickel powder according to claim 9, wherein the particle size of the nano-nickel powder is 50-300 nm.

Description

Nano nickel powder and liquid phase preparation method thereof Technical Field The invention relates to the technical field of metal nano powder, in particular to nano nickel powder and a liquid phase preparation method of the nano nickel powder. Background The nano nickel powder is a key metal functional material, and is widely applied to the fields of conductive slurry, catalytic reaction, thick film electrodes of microelectronic devices and microelectronic passive components and the like due to the unique catalytic activity, excellent electrical performance and special magnetic characteristics. In the practical application scene, the particle size and dispersion stability of the nano nickel powder are strictly required in different fields, and the accurate requirements of the fields on the performance can be fully adapted only to the nickel nano particles which meet the specific particle size standard and are uniformly dispersed. The preparation method of the nano nickel powder mainly comprises a mechanical grinding method, a physical vapor deposition method, a chemical vapor deposition method, a thermal plasma treatment method, an electrochemical reduction method, a liquid phase reduction method, a hydrothermal method and the like. Among them, although the gas phase method can efficiently prepare spherical nickel powder, larger particles are often mixed in the product, so that further classification and screening are needed. Although the thermal plasma treatment method can easily produce nano nickel powder, the uniformity of the size of the nickel powder is generally not high enough. In order to solve the problems, researchers carry out various technical adjustments, for example, china patent with publication number of CN105081347A discloses a method for preparing spherical superfine nickel powder with low apparent density and high purity at normal pressure, which takes industrial nickel sulfate as a raw material, adds ammonium sulfate and ammonia water to prepare buffer solution after dissolving in hot water, filters impurities, adds a surfactant, and pours the solution into hydrazine hydrate to form a mixed system, and then adds potassium borohydride/sodium in three steps to finally obtain nickel powder with the particle size of 500-800 nanometers, but the method has complicated steps and larger nickel particle size. The Chinese patent publication No. CN110947979A discloses a method for synthesizing superfine single crystal nickel powder by a solvothermal method, which comprises the steps of adding soluble nickel salt, a stabilizer, a surfactant and a reducing agent into a solvent, transferring the solvent into a high-pressure reaction kettle after dissolution, and obtaining nickel powder with the particle size of 0.1-3 mu m at the reaction temperature of 150-300 ℃ and the reaction pressure of 2-5 atm for 2-6 hours, wherein the method requires high-temperature and high-pressure reaction conditions, and the particle size of the obtained nickel powder is larger. According to the disclosure of the patent, the preparation of the nano nickel powder mainly has the following problems that firstly, the nano nickel powder has a size of submicron level, less reports of nano nickel powder below 100 nanometers are less, and secondly, the uniformity and dispersibility of the powder size are poor, so that the nickel nano particle dispersion liquid is difficult to store for a long time and has unstable performance, and the application of the nickel nano particle dispersion liquid in the fields of multilayer ceramic capacitors, thick film electrodes and the like is limited. Disclosure of Invention The application solves the technical problem of providing a liquid phase preparation method of nano nickel powder, and the preparation method provided by the application prepares nano nickel powder with uniform particle size and good dispersibility. In view of the above, the present application provides a liquid phase preparation method of nano nickel powder, comprising the following steps: S1, mixing an ethanol solution of a nickel source with hydrazine hydrate; s2, mixing the alkaline ethanol solution with the solution obtained in the step S1, and then adding a surfactant; and S3, reacting the mixed solution obtained in the step S2 under the conditions of stirring and heating, and separating and drying the obtained reaction product to obtain the nano nickel powder. In some specific embodiments, in step S1, the nickel source includes one or more of nickel acetate, nickel sulfate and nickel chloride, and/or the concentration of the ethanol solution of the nickel source is 0.01-0.2 mol/L, and/or the molar ratio of the hydrazine hydrate to the nickel source is (5-15): 1. In some specific embodiments, in step S2, the method for preparing the alkaline ethanol solution comprises: Dissolving organic alkali or inorganic alkali in ethanol, and stirring to obtain alkaline ethanol solution. In some embodiments, in step S2, the organi