CN115319079A - Method for preparing high-dispersion MLCC nano nickel powder - Google Patents

Method for preparing high-dispersion MLCC nano nickel powder Download PDF

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CN115319079A
CN115319079A CN202210450037.9A CN202210450037A CN115319079A CN 115319079 A CN115319079 A CN 115319079A CN 202210450037 A CN202210450037 A CN 202210450037A CN 115319079 A CN115319079 A CN 115319079A
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drying
water
nickel
melting point
dispersion
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董岩
刘鑫
王玥莹
辛晴
黄柏勋
沈馨怡
潘义庚
蒋建清
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Southeast University
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Abstract

The invention discloses a method for preparing high-dispersion MLCC nano nickel powder, which comprises the steps of firstly preparing mixed aqueous solution containing nickel complex and water-soluble salt, adding organic solvent to precipitate the nickel complex and the water-soluble salt together, then drying the coprecipitate, calcining below the salt melting point to convert the nickel complex in the coprecipitate into nickel oxide, reducing at a high temperature of more than 600 ℃, cooling, washing off the water-soluble salt, and drying to obtain the high-dispersion nano nickel powder. The nano nickel powder prepared by the method has good crystallinity and dispersibility, and the size of the prepared particle is less than 100nm.

Description

Method for preparing high-dispersion MLCC nano nickel powder
Technical Field
The invention relates to preparation of nano materials, in particular to a method for preparing high-dispersion MLCC nano nickel powder.
Background
The metal oxide nanoparticles generally refer to ultrafine oxide particles having a size of 1-100nm, which have a quantum size effect, a volume effect, a surface effect, and a tunnel effect, have very unique properties in thermal, optical, electrical, magnetic, and chemical aspects, and thus are widely used.
The metal oxide nanoparticles are generally prepared by a chemical method, mainly including a sol-gel method, a chemical precipitation method, a micro-emulsion method, a hydrothermal method, a solvothermal method, a spray pyrolysis method and the like. In the high-temperature calcination process, the nanoparticles are very easy to sinter, and dispersed metal oxide nanoparticles cannot be obtained.
To solve the problem of high temperature sintering of nanoparticles, the present group explored a variety of methods using water-soluble salts as isolation media. For example, CN201610365324.4 proposes a method for coating a water-soluble salt shell on the surface of nanoparticles, wherein the salt shell plays a role of isolation during the calcination process, and is removed at the later stage, thereby effectively avoiding the agglomeration and sintering of nanoparticles at high temperature to obtain monodisperse nanoparticles. However, the method has complex process and very low yield. The invention patent CN201610699775.1 firstly prepares hydrosol containing water-soluble salt and oxide precursor nanoparticles, then mixes the hydrosol with a weak-polarity solvent to separate out the water-soluble salt in the form of ultrafine particles, and precipitates together with the precursor particles of the nano oxide, then dries the coprecipitate and calcines below the melting point of the salt to convert the precursor of the nano oxide into the nano oxide, and finally washes away the soluble salt to obtain the nano oxide particles. However, this method requires the preparation of finely dispersed oxide precursor nanoparticles in advance and the preparation of the nanoparticles into a transparent hydrosol, which is complicated in process and low in yield. In patent CN 201810037620.0, metal oxide precursor particles are dispersed and isolated by using potassium sulfate nanoparticles in xylene, and the potassium sulfate is removed by washing after high-temperature calcination, so as to obtain dispersed nanoparticles. The method needs to prepare two materials of nano potassium sulfate and metal oxide precursor nano particles in advance, and the process is more complicated. The invention patent CN 201810037875.7 precipitates a mixed solution of metal sulfate and potassium sulfate in a weak-polarity organic solvent, simultaneously uses polyacrylic acid as a nucleating agent, forms a state that nano potassium sulfate particles are dispersed and isolated in the precipitate, calcines the precipitate at high temperature, decomposes the metal sulfate into metal oxide, and then washes the metal oxide to obtain dispersed metal oxide nano particles. The method has simple process, but the obtained metal oxide particles are coarse and have poor particle size uniformity. The invention patent CN202010125089.X coats a layer of metal-containing xerogel film on the surface of water-soluble salt particles, then calcinates the xerogel film at high temperature to convert the xerogel film into metal oxide nanoparticles, and washes the metal oxide nanoparticles to obtain the highly dispersed metal oxide nanoparticles. However, this method requires a large amount of organic solvent and cannot be recovered, resulting in high production cost. In addition, the research group also proposed a method of impregnating water-soluble salt with metal acetylacetonate (patent CN 2019101041603), but the method has the problems of low preparation efficiency and uneven particle size.
In conclusion, the metal oxide nanoparticles have technical bottleneck of high-temperature sintering in the preparation process, and various methods using water-soluble salts for isolation are tried in the early stage of the subject group, but the methods have the defects of complex process, high raw material cost, low preparation efficiency and the like.
The cerium oxide-based oxide functional nano-particle material has very wide application in the fields of catalysis, solid oxide fuel cells, mechanical polishing, gas sensitive devices and the like, and the cerium oxide is doped with elements such as lanthanum, cobalt, yttrium, gadolinium, nickel, copper, manganese and the like to obtain a non-stoichiometric cerium oxide-based material, namely a cerium oxide crystal contains a large number of crystal defects and oxygen vacancies, and the cerium oxide-based material has extremely high ion mobility and has better oxygen storage capacity and catalytic performance than pure cerium oxide. The preparation method of the cerium oxide-based nanoparticles mainly comprises a solid phase method and a liquid phase method. The solid phase method is obtained by calcining the oxalate, carbonate or basic carbonate corresponding to cerium and doping elements at high temperature, and the like, but the method is simple and easy to implement, and the nano particles are easy to sinter at high temperature, so that the highly dispersed cerium oxide-based nano particles are difficult to prepare; the liquid phase method is a method of obtaining cerium oxide-based nanoparticles or precursors of the cerium oxide-based nanoparticles by performing a physical or chemical process through liquid, and then obtaining the cerium oxide-based nanoparticles through high-temperature calcination. The liquid phase method also has the defects that the sintering of nano particles in the high-temperature calcination process cannot be avoided, the dispersed cerium oxide-based nano particles are difficult to obtain, the method is complicated to operate, the preparation efficiency is low, and impurities are easy to remain.
The performance of yttrium-doped zirconia nano powder is one of the decisive factors of the application performance of the nano-crystalline ceramic material, and the requirement on the dispersibility of the yttrium-doped zirconia nano powder is extremely high besides the requirement that the yttrium-doped zirconia nano powder has a tetragonal crystal structure and small particle size. If the zirconia nano-particles have serious particle agglomeration and sintering defects, the zirconia nano-crystalline ceramic with high density and high strength is difficult to be sintered. The preparation method of the yttrium-doped zirconia nanoparticles mainly comprises a coprecipitation method, a sol-gel method, a hydrothermal method and the like. The coprecipitation method comprises the steps of preparing yttrium salt and zirconium salt into a mixed solution, adding a precipitator to precipitate yttrium and zirconium, and then washing, drying, calcining at high temperature and the like to obtain yttrium-doped zirconia. However, the method cannot avoid the contact and sintering of the nano particles in the high-temperature calcination process, and the highly dispersed yttrium-doped zirconia nano particles are difficult to obtain; the sol-gel method requires that sol containing yttrium and zirconium is prepared first, and then yttrium-doped zirconia is prepared through the processes of gelation, drying, high-temperature calcination decomposition and the like. The method has the disadvantages of high raw material cost, long gel drying period and unsuitability for large-scale production, and the method can not avoid particle sintering in the high-temperature calcination process; the hydrothermal method is to use a reaction kettle to react at high temperature and high pressure to generate yttrium-doped zirconia, and although the method can obtain nanoparticles with good dispersibility, the safety is poor and mass production is difficult.
The ultrathin layer MLCC not only requires the particle size of the nano nickel powder to be fine, but also has extremely high requirements on the particle dispersibility and crystallinity of the nano nickel powder. When the MLCC inner electrode is manufactured, the process of glue discharging in the air is needed, and the nano nickel powder is required to be well crystallized to have good oxidation resistance so as to prevent the nano nickel powder from being oxidized during the glue discharging; meanwhile, the nano nickel powder also needs to have good dispersibility, and cannot have the defects of particle agglomeration or sintering, otherwise, the problems of discontinuity of an inner electrode, electric leakage and the like of the MLCC can be caused. The oxidation resistance of the nano nickel powder depends on the crystallinity, the crystallinity depends on the preparation temperature seriously, and the nickel powder can be prepared at a high temperature of more than 600 ℃ to obtain the nickel powder particles with good crystallinity and compactness. Although nano nickel powder with a particle size of less than 100nm can be prepared by methods such as liquid phase reduction, the preparation temperature is too low (< 100 ℃), the crystallinity is poor, and oxidation occurs at room temperature. At present, the Chemical Vapor Deposition (CVD) method or the Physical Vapor Deposition (PVD) method is adopted for the commercial nanometer nickel powder for MLCC, the prepared nanometer nickel powder is about 100-300nm, and the oxidation resistance and the dispersibility are good, but the CVD method and the PVD method have expensive equipment, complex process and extremely high production cost, and the nanometer nickel powder with the particle size of less than 100nm is difficult to prepare.
Disclosure of Invention
The purpose of the invention is as follows: based on the problems of the prior art, an object of the present invention is to provide a method for preparing highly dispersed metal oxide nanoparticles, which solves the problems of complex process and low efficiency of the prior art.
The invention also aims to provide a preparation method of the cerium oxide-based nano-particles, which solves the problems that the particles are easy to sinter and difficult to uniformly dope in the existing cerium oxide preparation technology.
The invention further aims to provide a method for preparing yttrium-doped zirconia nanoparticles, which solves the problems of hard particle agglomeration, sintering and low preparation efficiency in the existing yttrium-doped zirconia nanoparticle preparation technology.
The invention also aims to provide a method for preparing the high-dispersion MLCC nano nickel powder, which solves the problem that the existing method is difficult to prepare the nano nickel powder with the particle size of less than 100nm, good crystallinity and good dispersibility.
The technical scheme is as follows: in a first aspect, the present invention provides a method for preparing highly dispersed metal oxide nanoparticles, comprising the steps of:
(1) Adding metal salt, water-soluble salt and a complexing agent corresponding to the metal oxide into water to obtain a mixed solution containing the water-soluble salt and the metal complex;
(2) Adding an organic solvent into the mixed solution obtained in the step (1) to precipitate water-soluble salt and the metal complex together to obtain a precipitate of the water-soluble salt isolated metal complex;
(3) Drying the precipitate and calcining at a temperature below the melting point of the water-soluble salt to convert the metal complex into a metal oxide, thereby obtaining water-soluble salt isolated metal oxide nanoparticles;
(4) And washing off water-soluble salt in the calcined product by using deionized water, and drying to obtain the high-dispersion metal oxide nano-particles.
Preferably, the metal oxide is a metal oxide other than alkali metal and alkaline earth metal oxides, and may be any of alumina, titanium oxide, nickel oxide, cobalt oxide, iron oxide, magnesium oxide, copper oxide, tin oxide, indium oxide, cerium oxide, yttrium oxide, europium oxide, zirconium oxide, lanthanum oxide, terbium oxide, dysprosium oxide, and neodymium oxide.
Preferably, the water-soluble salt is any one of sodium chloride, potassium chloride, sodium sulfate, potassium sulfate, sodium carbonate, and potassium carbonate.
Preferably, the metal salt is any one of a metal nitrate, a metal acetate, a metal sulfate, and a metal chloride species corresponding to a metal oxide.
Preferably, the complexing agent is any one of citric acid, sodium citrate, potassium citrate, tartaric acid, sodium tartrate, potassium tartrate, polyacrylic acid, sodium polyacrylate, potassium polyacrylate, ammonium polyacrylate, ethylene diamine tetraacetic acid, sodium ethylene diamine tetracetate, potassium ethylene diamine tetracetate, gluconic acid, sodium gluconate, potassium gluconate, glucoheptonic acid, sodium glucoheptonate, potassium glucoheptonate and ammonia water.
Preferably, the organic solvent is any one of ethanol, propanol, isopropanol, tert-butanol, ethylene glycol methyl ether, ethylene glycol ethyl ether, ethylene glycol butyl ether, diethylene glycol butyl ether, dimethylformamide and dimethyl sulfoxide.
The molar ratio of the water-soluble salt to the metal salt is more than or equal to 1.
The mol ratio of the complexing agent to the metal salt is 0.1-1.
In the above-described embodiment, a mixed solution containing a water-soluble salt and a metal complex is first prepared, and in this mixed solution, the water-soluble salt and the metal complex are uniformly distributed at the molecular or ionic level. When the organic solvent is added, the solubility of the water-soluble salt and the metal complex in the mixed solution is lowered while precipitating out from water, that is, a state where the water-soluble salt isolates the metal complex is formed in the precipitate. Drying the coprecipitate, calcining below the melting point of the salt to convert the metal complex in the coprecipitate into metal oxide, cooling, washing off the water-soluble salt, and drying to obtain the high-dispersion metal oxide nano-particles. In the high-temperature calcination process, the metal oxide nanoparticles are isolated and dispersed by the water-soluble salt all the time, so that the high-temperature sintering of the nanoparticles is effectively avoided, and the high-dispersion nanoparticle material can be prepared.
Another aspect of the present invention provides a method for preparing cerium oxide-based nanoparticles, comprising the steps of:
(1) Dissolving water-soluble salt, cerium salt and doping element salt in water, and adding a complexing agent to prepare a mixed solution of a complex containing cerium and doping elements and the water-soluble salt;
(2) Adding an organic solvent into the mixed solution to separate out a water-soluble salt and a complex of cerium and the doping element together to obtain a coprecipitate, wherein in the precipitate, the complex nano-particles of cerium and the doping element are isolated by the water-soluble salt;
(3) Drying the obtained coprecipitate, and calcining at a temperature of more than 350 ℃ and below the melting point of the water-soluble salt to decompose a complex of cerium and the doping element in the coprecipitate and generate cerium oxide-based nanoparticles, wherein the water-soluble salt still keeps a solid state and plays a role in isolation;
(4) And washing the calcined product with water to remove water-soluble salts, and drying to obtain the high-dispersion cerium oxide-based nano particles.
Wherein the cerium oxide-based nanoparticles have a chemical composition of Ce 1-x M x O 2-y Wherein M is a doping element, M = at least one of La, co, Y, gd, ni, cu or Mn, x is more than or equal to 0 and less than 0.2, Y is a non-stoichiometric number and Y is more than or equal to 0 and less than 0.5.
Preferably, the salt corresponding to cerium and the doping element is nitrate, acetate, sulfate or chloride of cerium and the doping element, and the complex of cerium and the doping element is a complex formed by the complexing agent and cerium and the doping element.
Preferably, the water-soluble salt is potassium sulfate, sodium sulfate, potassium chloride, sodium chloride, potassium carbonate or sodium carbonate.
Preferably, the complexing agent is polyacrylic acid, potassium polyacrylate, sodium polyacrylate, ammonium polyacrylate, citric acid, potassium citrate, sodium citrate, ethylenediaminetetraacetic acid, potassium ethylenediaminetetraacetate, sodium ethylenediaminetetraacetate, tartaric acid, potassium tartrate, sodium tartrate, gluconic acid, potassium gluconate, sodium gluconate, glucoheptonic acid, potassium glucoheptonate or sodium glucoheptonate.
Preferably, the organic solvent is ethanol, isopropanol, propanol, tert-butanol, ethylene glycol ethyl ether, ethylene glycol methyl ether, ethylene glycol butyl ether, diethylene glycol butyl ether, dimethyl sulfoxide or dimethylformamide.
The mass ratio of the water-soluble salt to the cerium salt is more than or equal to 1.
The mol ratio of the complexing agent to the cerium salt is 0.1-1.
In the above scheme, a mixed solution containing a complex of cerium and a doping element and a water-soluble salt is prepared first, wherein the cerium and the doping element are uniformly distributed at a molecular or ionic level. The addition of the organic solvent reduces the solubility of the cerium, dopant element complex and water-soluble salt in the solution and precipitates out of the water, thereby forming a state in which the water-soluble salt is dispersed and isolated in the precipitate. Drying the coprecipitate, calcining below the salt melting point to decompose cerium and the doped element complex to obtain doped cerium oxide, and washing to remove water-soluble salt to obtain the high-dispersion cerium oxide-based nanoparticles. In the drying and high-temperature calcining processes, cerium and the doped element complex or cerium oxide-based nanoparticles are always dispersed and isolated by the water-soluble salt, so that the problem of high-temperature sintering of the nanoparticles is effectively solved.
Based on the problems of the preparation method of yttrium-doped zirconia nanoparticles, the method for preparing yttrium-doped zirconia nanoparticles provided by the invention in another aspect comprises the following steps:
(1) Dissolving zirconium salt, yttrium salt, water-soluble salt and a complexing agent in water to obtain a mixed solution, wherein the molar ratio of the yttrium salt to the zirconium salt is 0.03-0.15;
(2) Adding an organic solvent to the mixed solution to obtain a coprecipitate of a water-soluble salt and an yttrium-zirconium complex. Dispersing and isolating the yttrium-zirconium complex nanoparticles in the precipitate by a water-soluble salt;
(3) Drying the coprecipitate, and calcining below the melting point of the water-soluble salt above the decomposition temperature of the yttrium-zirconium complex to convert the yttrium-zirconium complex into yttrium-doped zirconia, wherein the yttrium-doped zirconia nano-particle barium water-soluble salt is separated and dispersed;
(4) And washing and drying the calcined product by using deionized water to obtain the high-dispersion yttrium-doped zirconia nano-particles.
Preferably, the water-soluble salt is potassium sulfate, sodium chloride, potassium chloride, sodium carbonate or potassium carbonate.
Preferably, the complexing agent is polyacrylic acid, ammonium polyacrylate, potassium polyacrylate, sodium polyacrylate, citric acid, potassium citrate, sodium citrate, ethylenediaminetetraacetic acid, sodium ethylenediaminetetraacetate, potassium ethylenediaminetetraacetate, tartaric acid, potassium tartrate, sodium tartrate, gluconic acid, sodium gluconate, potassium gluconate, glucoheptonic acid, sodium glucoheptonate or potassium glucoheptonate.
Preferably, the organic solvent is ethanol, propanol, tert-butanol, isopropanol, ethylene glycol methyl ether, ethylene glycol butyl ether, diethylene glycol butyl ether, ethylene glycol ethyl ether, dimethylformamide or dimethyl sulfoxide.
The molar ratio of the water-soluble salt to the zirconium salt is more than or equal to 1.
The mol ratio of the complexing agent to the zirconium salt is 0.1-1.
In the above scheme, the yttrium and zirconium elements are uniformly distributed in the prepared mixed solution containing yttrium-zirconium complex and water-soluble salt at molecular or ionic level. When the organic solvent is added, the solubility of the water-soluble salt and the yttrium-zirconium complex in the mixed solution is reduced, and the water-soluble salt is precipitated from the solution together, so that the effect of dispersing and isolating the yttrium-zirconium complex is formed in the coprecipitate. In the subsequent high-temperature calcination process, the yttrium-zirconium complex is converted into yttrium-doped zirconia, and finally water-soluble salt is washed away to obtain the highly-dispersed yttrium-doped zirconia nano-particles. In the high-temperature calcination process, the nano particles are effectively isolated and dispersed by the solid water-soluble salt all the time, so that the problem of particle sintering can not occur.
In still another aspect of the present invention, there is provided a method for preparing highly dispersed MLCC nano nickel powder, comprising the steps of:
(1) Adding nickel salt, a complexing agent and water-soluble salt into water to obtain a mixed solution of the water-soluble salt and a nickel complex;
(2) Adding an organic solvent to the mixed solution of the water-soluble salt and the nickel complex to lower the solubility of the water-soluble salt and the nickel complex, thereby obtaining a precipitate. In this precipitate, a water-soluble salt separates and disperses the nickel complex;
(3) Drying the precipitate obtained in the step 2), and calcining the precipitate at a temperature higher than the decomposition temperature of the nickel complex and lower than the melting point of the water-soluble salt to obtain a calcined product. In the calcined product, the nickel complex is converted into nickel oxide, namely a state that water-soluble salt is formed to isolate nickel nano particles;
(4) Reducing the calcined product at a high temperature of more than 600 ℃ and below the melting point of the water-soluble salt to obtain a high-temperature reduced product;
(5) And washing and drying the high-temperature reduction product by using deionized water to obtain the high-dispersion nano nickel powder.
Preferably, the nickel salt is nickel nitrate, nickel sulfate, nickel acetate or nickel chloride, and the water-soluble salt is potassium sulfate, sodium sulfate, potassium chloride, sodium chloride, potassium carbonate or sodium carbonate;
preferably, the organic solvent is ethanol, isopropanol, tert-butanol, propanol, ethylene glycol methyl ether, ethylene glycol ethyl ether, diethylene glycol butyl ether, ethylene glycol butyl ether, dimethylformamide or dimethyl sulfoxide.
Preferably, the complexing agent is ammonia water, ammonium bicarbonate, ammonium carbonate, polyacrylic acid, ammonium polyacrylate, sodium polyacrylate, potassium polyacrylate, citric acid, sodium citrate, potassium citrate, tartaric acid, sodium tartrate, potassium tartrate, ethylene diamine tetraacetic acid, sodium ethylene diamine tetracetate, potassium ethylene diamine tetracetate, gluconic acid, sodium gluconate or potassium gluconate, and the complexing agent and the nickel ions form corresponding complexes.
Preferably, the molar ratio of the water-soluble salt to the nickel salt is not less than 1.
The mol ratio of the complexing agent to the nickel salt is 0.1-1.
In the scheme, the method prepares a mixed solution containing a nickel complex and water-soluble salt, then adds an organic solvent as a precipitator to precipitate the nickel complex and the water-soluble salt together, then calcines the mixture at high temperature and reduces the mixture to convert the nickel complex into metallic nickel, and washes the metallic nickel to remove the water-soluble salt to obtain the high-crystallization high-dispersion nano nickel powder.
Has the advantages that: the nano particles prepared by the method have good dispersibility and crystallinity, the cost is low, the used water-soluble salt and organic solvent do not participate in chemical reaction, the nano particles can be recycled, the process is simple and convenient, the nano particles are very suitable for large-scale production, the requirement on preparation equipment is extremely low, safety problems such as high pressure and the like are not involved, and the universality is strong;
the cerium oxide-based nanoparticles are isolated and dispersed by the solid salt all the time at high temperature, so that the prepared nanoparticles have good dispersibility, element doping is easy to realize in cerium oxide, and cerium oxide-based nanoparticles with different properties can be prepared only by adding elements such as lanthanum, cobalt, yttrium, nickel, copper or manganese and the like when a solution is prepared, and can meet the requirements of ultraviolet absorption materials and catalytic materials;
the yttrium-doped zirconia nano-particles are dispersed and isolated by solid salt all the time in the high-temperature calcination process, and have good dispersibility and high preparation efficiency.
The nano nickel powder prepared by the method has good crystallinity and dispersity, and the size of the prepared particle is less than 100nm.
Drawings
FIG. 1 is a graph of yttrium oxide nanoparticles prepared by the method of example 11, having an average particle size of about 30nm;
FIG. 2 is a graph of zirconia nanoparticles prepared by the method of example 13, having an average particle size of about 30nm;
FIG. 3 is a graph of nickel oxide nanoparticles prepared by the method of example 18, having an average particle size of about 70nm;
FIG. 4 is a graph of cerium oxide nanoparticles prepared by the method of example 23, having an average particle size of about 30nm;
FIG. 5 is a graph of nickel oxide nanoparticles prepared by the method of example 28, having an average particle size of about 60nm;
FIG. 6 is a graph of nickel oxide nanoparticles prepared by the method of example 33, having an average particle size of about 70nm;
FIG. 7 is a graph of cerium oxide nanoparticles prepared in accordance with example 57, having an average particle size of about 20nm;
FIG. 8 is a graph of cerium oxide nanoparticles prepared in example 79, having an average particle size of about 30nm.
FIG. 9 is a cerium oxide-based nanoparticle having an average particle size of about 30nm prepared at 700 ℃ by the method of example 81;
FIG. 10 is a graph of yttrium-doped zirconia nanoparticles having an average particle size of about 30nm prepared at 700 ℃ by the example 125 process;
FIG. 11 is a schematic representation of the reduction of nano-nickel powder prepared at 650 ℃ by the method of example 168, having an average particle size of about 80nm.
Detailed Description
The invention is further illustrated below with reference to examples and figures.
The salts soluble in water can be used as the insulating material in the invention. The water-soluble salt used in the present invention may be sodium chloride, potassium chloride, lithium chloride, cesium chloride, rubidium chloride, lithium sulfate, sodium sulfate, potassium sulfate, cesium sulfate, rubidium sulfate, sodium bromide, potassium bromide, lithium fluoride, sodium fluoride, potassium fluoride, sodium phosphate, sodium metaaluminate, sodium nitrate, potassium nitrate, sodium carbonate, potassium carbonate. From the viewpoint of chemical stability and cost, it is preferable to use sodium chloride, potassium chloride, sodium sulfate, potassium sulfate, sodium carbonate or potassium carbonate.
Metal oxides which do not react chemically with water and the selected salt are suitable. The metal oxide used in the present invention may be magnesium oxide, aluminum oxide, titanium oxide, iron oxide, zirconium oxide, copper oxide, nickel oxide, cobalt oxide, niobium oxide, tin oxide, indium oxide, cerium oxide, yttrium oxide, europium oxide, zirconium oxide, cerium oxide, lanthanum oxide, terbium oxide, dysprosium oxide, or neodymium oxide. From the viewpoint of stability, it is preferable to use aluminum oxide, titanium oxide, nickel oxide, cobalt oxide, iron oxide, magnesium oxide, copper oxide, tin oxide, indium oxide, cerium oxide, yttrium oxide, europium oxide, zirconium oxide, lanthanum oxide, terbium oxide, dysprosium oxide, or neodymium oxide.
In the present invention, either a complexing agent or a complexing method which can form a water-soluble metal complex from a metal is applicable. The complexing agent used in the present invention may be citric acid, sodium citrate, potassium citrate, tartaric acid, sodium tartrate, potassium tartrate, polyacrylic acid, sodium polyacrylate, potassium polyacrylate, ammonium polyacrylate, ethylenediaminetetraacetic acid, sodium ethylenediaminetetraacetate, potassium ethylenediaminetetraacetate, sodium tripolyphosphate, sodium pyrophosphate, sodium hexametaphosphate, sodium aminotriacetate, sodium diethylenetriaminepentacarboxylate, sodium alginate, gluconic acid, sodium gluconate, potassium gluconate, glucoheptonic acid, sodium glucoheptonate, potassium glucoheptonate, hydrolyzed polymaleic anhydride, maleic acid acrylic acid copolymer, ammonia water or ammonium compound. From the viewpoint of chemical stability and cost, the complexing agent preferably uses citric acid, sodium citrate, potassium citrate, tartaric acid, sodium tartrate, potassium tartrate, polyacrylic acid, sodium polyacrylate, potassium polyacrylate, ammonium polyacrylate, ethylenediaminetetraacetic acid, sodium ethylenediaminetetraacetate, potassium ethylenediaminetetraacetate, gluconic acid, sodium gluconate, potassium gluconate, glucoheptonic acid, sodium glucoheptonate, potassium glucoheptonate, or ammonia water.
In the present invention, any organic solvent which is miscible with water and can lower the solubility of the water-soluble salt and the metal complex is suitable. The organic solvent used in the present invention may be pyridine, dioxane, tetrahydrofuran, acetone, methanol, ethanol, propanol, isopropanol, tert-butanol, ethylene glycol methyl ether, ethylene glycol ethyl ether, ethylene glycol butyl ether, diethylene glycol butyl ether, dimethylformamide or dimethyl sulfoxide. From the viewpoint of chemical stability, non-toxicity and economy, ethanol, propanol, isopropanol, tert-butanol, ethylene glycol methyl ether, ethylene glycol ethyl ether, ethylene glycol butyl ether, diethylene glycol butyl ether, dimethylformamide or dimethyl sulfoxide is preferable.
In the invention, the addition amount of the complexing agent is not required to be calculated according to the coordination numbers of the metal and the complexing agent, and even if the addition amount of the complexing agent is less, the metal ions can be completely precipitated. However, when the amount of the complexing agent is too small, the uniformity of the particle size of the obtained nanoparticles is poor, and larger particles are likely to appear. Preferably, the addition amount of the post-complexing agent is 0.1 to 1 time of the mole number of the metal salt.
The method for preparing highly dispersed metal oxide nanoparticles is further illustrated below with reference to specific examples.
Example 1
1L of 0.5M potassium sulfate aqueous solution is prepared, 0.1mol of aluminum nitrate and 0.05mol of citric acid are added, and the mixture is stirred and dissolved into a transparent aqueous solution. Adding 1L ethanol, drying the obtained precipitate, calcining below the melting point of potassium sulfate salt, cooling, washing with deionized water for 2-3 times, and drying to obtain the high-dispersion alumina nano-particles.
Example 2
1L of 0.5M potassium sulfate aqueous solution is prepared, 0.1mol of titanium nitrate and 0.05mol of citric acid are added, and the mixture is stirred and dissolved into a transparent aqueous solution. Adding 1L of ethanol, drying the obtained precipitate, calcining below the melting point of potassium sulfate salt, cooling, washing with deionized water for 2-3 times, and drying to obtain the high-dispersion titanium dioxide nanoparticles.
Example 3
1L of 0.5M potassium sulfate aqueous solution is prepared, 0.1mol of nickel nitrate and 0.05mol of citric acid are added, and the mixture is stirred and dissolved into a transparent aqueous solution. Adding 1L of ethanol, drying the obtained precipitate, calcining below the melting point of potassium sulfate salt, cooling, washing with deionized water for 2-3 times, and drying to obtain the high-dispersion nickel oxide nanoparticles.
Example 4
1L of 0.5M potassium sulfate aqueous solution is prepared, 0.1mol of cobalt nitrate and 0.05mol of citric acid are added, and the mixture is stirred and dissolved into a transparent aqueous solution. Adding 1L of ethanol, drying the obtained precipitate, calcining below the melting point of potassium sulfate salt, cooling, washing with deionized water for 2-3 times, and drying to obtain the high-dispersion cobalt oxide nanoparticles.
Example 5
1L of 0.5M potassium sulfate aqueous solution is prepared, 0.1mol of ferric nitrate and 0.05mol of citric acid are added, and the mixture is stirred and dissolved into a transparent aqueous solution. Adding 1L ethanol, drying the obtained precipitate, calcining below the melting point of potassium sulfate salt, cooling, washing with deionized water for 2-3 times, and drying to obtain the high-dispersion iron oxide nanoparticles.
Example 6
1L of 0.5M potassium sulfate aqueous solution is prepared, 0.1mol of magnesium nitrate and 0.05mol of citric acid are added, and the mixture is stirred and dissolved into a transparent aqueous solution. Adding 1L ethanol, drying the obtained precipitate, calcining below the melting point of potassium sulfate salt, cooling, washing with deionized water for 2-3 times, and drying to obtain the high-dispersion magnesium oxide nanoparticles.
Example 7
1L of 0.5M potassium sulfate aqueous solution is prepared, 0.1mol of copper nitrate and 0.05mol of citric acid are added, and the mixture is stirred and dissolved into a transparent aqueous solution. Adding 1L of ethanol, drying the obtained precipitate, calcining below the melting point of potassium sulfate salt, cooling, washing with deionized water for 2-3 times, and drying to obtain the high-dispersion copper oxide nanoparticles.
Example 8
1L of 0.5M potassium sulfate aqueous solution is prepared, 0.1mol of stannic chloride and 0.05mol of citric acid are added, and the mixture is stirred and dissolved into a transparent aqueous solution. Adding 1L ethanol, drying the obtained precipitate, calcining below the melting point of potassium sulfate salt, cooling, washing with deionized water for 2-3 times, and drying to obtain high-dispersion tin oxide nanoparticles.
Example 9
1L of 0.5M potassium sulfate aqueous solution is prepared, 0.1mol of indium chloride and 0.05mol of citric acid are added, and the mixture is stirred and dissolved into a transparent aqueous solution. Adding 1L of ethanol, drying the obtained precipitate, calcining below the melting point of potassium sulfate salt, cooling, washing with deionized water for 2-3 times, and drying to obtain the high-dispersion indium oxide nanoparticles.
Example 10
1L of 0.5M potassium sulfate aqueous solution is prepared, 0.1mol of cerium nitrate and 0.05mol of citric acid are added, and the mixture is stirred and dissolved into a transparent aqueous solution. Adding 1L of ethanol, drying the obtained precipitate, calcining below the melting point of potassium sulfate salt, cooling, washing with deionized water for 2-3 times, and drying to obtain the high-dispersion cerium oxide nanoparticles.
Example 11
1L of 0.5M potassium sulfate aqueous solution is prepared, 0.1mol of yttrium nitrate and 0.05mol of citric acid are added, and the mixture is stirred and dissolved into a transparent aqueous solution. Adding 1L ethanol, drying the obtained precipitate, calcining below the melting point of potassium sulfate salt, cooling, washing with deionized water for 2-3 times, and drying to obtain the high-dispersion yttrium oxide nanoparticles.
Example 12
1L of 0.5M potassium sulfate aqueous solution is prepared, 0.1mol of europium nitrate and 0.05mol of citric acid are added, and the mixture is stirred and dissolved into a transparent aqueous solution. Adding 1L ethanol, drying the obtained precipitate, calcining below the melting point of potassium sulfate salt, cooling, washing with deionized water for 2-3 times, and drying to obtain the high-dispersion europium oxide nanoparticles.
Example 13
1L of 0.5M potassium sulfate aqueous solution is prepared, 0.1mol of zirconium nitrate and 0.05mol of citric acid are added, and the mixture is stirred and dissolved into a transparent aqueous solution. Adding 1L of ethanol, drying the obtained precipitate, calcining below the melting point of potassium sulfate salt, cooling, washing with deionized water for 2-3 times, and drying to obtain the high-dispersion zirconium oxide nanoparticles.
Example 14
1L of 0.5M potassium sulfate aqueous solution is prepared, 0.1mol of lanthanum nitrate and 0.05mol of citric acid are added, and the mixture is stirred and dissolved into a transparent aqueous solution. Adding 1L ethanol, drying the obtained precipitate, calcining below the melting point of potassium sulfate salt, cooling, washing with deionized water for 2-3 times, and drying to obtain the high-dispersion lanthanum oxide nano-particles.
Example 15
1 liter of 0.5M potassium sulfate aqueous solution is prepared, 0.1mol of terbium nitrate and 0.05mol of citric acid are added, and the mixture is stirred and dissolved into transparent aqueous solution. And adding 1 liter of ethanol, drying the obtained precipitate, calcining below the melting point of potassium sulfate salt, cooling, washing with deionized water for 2-3 times, and drying to obtain the high-dispersion terbium oxide nanoparticles.
Example 16
1L of 0.5M potassium sulfate aqueous solution is prepared, 0.1mol of dysprosium nitrate and 0.05mol of citric acid are added, and the mixture is stirred and dissolved into transparent aqueous solution. Adding 1L of ethanol, drying the obtained precipitate, calcining below the melting point of potassium sulfate, cooling, washing with deionized water for 2-3 times, and drying to obtain the high-dispersion dysprosium oxide nano-particles.
Example 17
1L of 0.5M potassium sulfate aqueous solution is prepared, 0.1mol of neodymium nitrate and 0.05mol of citric acid are added, and the mixture is stirred and dissolved into a transparent aqueous solution. Adding 1L of ethanol, drying the obtained precipitate, calcining below the melting point of potassium sulfate salt, cooling, washing with deionized water for 2-3 times, and drying to obtain the high-dispersion neodymium oxide nanoparticles.
Example 18
1L of 0.5M potassium sulfate aqueous solution is prepared, 0.1mol of nickel nitrate and 0.05mol of sodium ethylene diamine tetracetate are added, and the mixture is stirred and dissolved into a transparent aqueous solution. Adding 1L of ethanol, drying the obtained precipitate, calcining below the melting point of potassium sulfate salt, cooling, washing with deionized water for 2-3 times, and drying to obtain the high-dispersion nickel oxide nanoparticles.
Example 19
1L of 0.5M potassium sulfate aqueous solution is prepared, 0.1mol of nickel acetate and 0.05mol of sodium ethylene diamine tetracetate are added, and the mixture is stirred and dissolved into a transparent aqueous solution. Adding 1L of ethanol, drying the obtained precipitate, calcining below the melting point of potassium sulfate salt, cooling, washing with deionized water for 2-3 times, and drying to obtain the high-dispersion nickel oxide nanoparticles.
Example 20
1L of 0.5M potassium sulfate aqueous solution is prepared, 0.1mol of nickel chloride and 0.05mol of sodium ethylene diamine tetracetate are added, and the mixture is stirred and dissolved into a transparent aqueous solution. Adding 1L ethanol, drying the obtained precipitate, calcining below the melting point of potassium sulfate salt, cooling, washing with deionized water for 2-3 times, and drying to obtain the high-dispersion nickel oxide nanoparticles.
Example 21
1L of 0.5M potassium sulfate aqueous solution is prepared, 0.1mol of nickel sulfate and 0.05mol of sodium ethylene diamine tetracetate are added, and the mixture is stirred and dissolved into a transparent aqueous solution. Adding 1L ethanol, drying the obtained precipitate, calcining below the melting point of potassium sulfate salt, cooling, washing with deionized water for 2-3 times, and drying to obtain the high-dispersion nickel oxide nanoparticles.
Example 22
1L of 0.5M potassium sulfate aqueous solution is prepared, 0.1mol of cerium nitrate and 0.05mol of sodium ethylene diamine tetracetate are added, and the mixture is stirred and dissolved into a transparent aqueous solution. Adding 1L of ethanol, drying the obtained precipitate, calcining below the melting point of potassium sulfate salt, cooling, washing with deionized water for 2-3 times, and drying to obtain the high-dispersion cerium oxide nanoparticles.
Example 23
1L of 0.5M potassium sulfate aqueous solution is prepared, 0.1mol of cerium acetate and 0.05mol of sodium ethylene diamine tetracetate are added, and the mixture is stirred and dissolved into a transparent aqueous solution. Adding 1L of ethanol, drying the obtained precipitate, calcining below the melting point of potassium sulfate salt, cooling, washing with deionized water for 2-3 times, and drying to obtain the high-dispersion cerium oxide nanoparticles.
Example 24
1L of 0.5M potassium sulfate aqueous solution is prepared, 0.1mol of cerium chloride and 0.05mol of sodium ethylene diamine tetracetate are added, and the mixture is stirred and dissolved into a transparent aqueous solution. Adding 1L of ethanol, drying the obtained precipitate, calcining below the melting point of potassium sulfate salt, cooling, washing with deionized water for 2-3 times, and drying to obtain the high-dispersion cerium oxide nanoparticles.
Example 25
1L of 0.5M potassium sulfate aqueous solution is prepared, 0.1mol of cerium sulfate and 0.05mol of sodium ethylene diamine tetracetate are added, and the mixture is stirred and dissolved into a transparent aqueous solution. Adding 1L of ethanol, drying the obtained precipitate, calcining below the melting point of potassium sulfate salt, cooling, washing with deionized water for 2-3 times, and drying to obtain the high-dispersion cerium oxide nanoparticles.
Example 26
1L of 1M sodium sulfate aqueous solution is prepared, 0.1mol of nickel nitrate and 0.1mol of ammonia water are added, and the mixture is stirred and dissolved into a transparent aqueous solution. Adding 1L of ethanol, drying the obtained precipitate, calcining below the melting point of sodium sulfate, cooling, washing with deionized water for 2-3 times, and drying to obtain the high-dispersion nickel oxide nanoparticles.
Example 27
1L of 1M sodium sulfate aqueous solution is prepared, 0.1mol of nickel nitrate and 0.1mol of citric acid are added, and the mixture is stirred and dissolved into a transparent aqueous solution. Adding 1L of ethanol, drying the obtained precipitate, calcining below the melting point of sodium sulfate, cooling, washing with deionized water for 2-3 times, and drying to obtain the high-dispersion nickel oxide nanoparticles.
Example 28
1L of 1M sodium sulfate aqueous solution is prepared, 0.1mol of nickel nitrate and 0.1mol of sodium citrate are added, and the mixture is stirred and dissolved into a transparent aqueous solution. Adding 1L of ethanol, drying the obtained precipitate, calcining below the melting point of sodium sulfate, cooling, washing with deionized water for 2-3 times, and drying to obtain the high-dispersion nickel oxide nanoparticles.
Example 29
1L of 1M sodium sulfate aqueous solution is prepared, 0.1mol of nickel nitrate and 0.1mol of potassium citrate are added, and the mixture is stirred and dissolved into a transparent aqueous solution. Adding 1L of ethanol, drying the obtained precipitate, calcining below the melting point of sodium sulfate, cooling, washing with deionized water for 2-3 times, and drying to obtain the high-dispersion nickel oxide nanoparticles.
Example 30
1L of 1M aqueous solution of sodium sulfate was prepared, and 0.1mol of nickel nitrate and 0.1mol of tartaric acid were added thereto and dissolved by stirring to obtain a transparent aqueous solution. Adding 1L of ethanol, drying the obtained precipitate, calcining below the melting point of sodium sulfate, cooling, washing with deionized water for 2-3 times, and drying to obtain the high-dispersion nickel oxide nanoparticles.
Example 31
1L of 1M aqueous solution of sodium sulfate was prepared, and 0.1mol of nickel nitrate and 0.1mol of sodium tartrate were added thereto and dissolved by stirring to obtain a transparent aqueous solution. Adding 1L of ethanol, drying the obtained precipitate, calcining below the melting point of sodium sulfate, cooling, washing with deionized water for 2-3 times, and drying to obtain the high-dispersion nickel oxide nanoparticles.
Example 32
1L of 1M sodium sulfate aqueous solution is prepared, 0.1mol of nickel nitrate and 0.1mol of potassium tartrate are added, and the mixture is stirred and dissolved into a transparent aqueous solution. Adding 1L of ethanol, drying the obtained precipitate, calcining below the melting point of sodium sulfate, cooling, washing with deionized water for 2-3 times, and drying to obtain the high-dispersion nickel oxide nanoparticles.
Example 33
1L of 1M sodium sulfate aqueous solution is prepared, 0.1mol of nickel nitrate and 0.1mol of polyacrylic acid are added, and the mixture is stirred and dissolved into a transparent aqueous solution. Adding 1L of ethanol, drying the obtained precipitate, calcining below the melting point of sodium sulfate, cooling, washing with deionized water for 2-3 times, and drying to obtain the high-dispersion nickel oxide nanoparticles.
Example 34
1L of 1M sodium sulfate aqueous solution is prepared, 0.1mol of nickel nitrate and 0.1mol of sodium polyacrylate are added, and the mixture is stirred and dissolved into a transparent aqueous solution. Adding 1L of ethanol, drying the obtained precipitate, calcining below the melting point of sodium sulfate, cooling, washing with deionized water for 2-3 times, and drying to obtain the high-dispersion nickel oxide nanoparticles.
Example 35
1L of 1M sodium sulfate aqueous solution is prepared, 0.1mol of nickel nitrate and 0.1mol of potassium polyacrylate are added, and the mixture is stirred and dissolved into a transparent aqueous solution. Adding 1L of ethanol, drying the obtained precipitate, calcining below the melting point of sodium sulfate, cooling, washing with deionized water for 2-3 times, and drying to obtain the high-dispersion nickel oxide nanoparticles.
Example 36
1L of 1M sodium sulfate aqueous solution is prepared, 0.1mol of nickel nitrate and 0.1mol of ammonium polyacrylate are added, and the mixture is stirred and dissolved into a transparent aqueous solution. Adding 1L of ethanol, drying the obtained precipitate, calcining below the melting point of sodium sulfate, cooling, washing with deionized water for 2-3 times, and drying to obtain the high-dispersion nickel oxide nanoparticles.
Example 37
1L of 1M sodium sulfate aqueous solution is prepared, 0.1mol of nickel nitrate and 0.1mol of ethylenediamine tetraacetic acid are added, and the mixture is stirred and dissolved into a transparent aqueous solution. Adding 1L of ethanol, drying the obtained precipitate, calcining below the melting point of sodium sulfate, cooling, washing with deionized water for 2-3 times, and drying to obtain the high-dispersion nickel oxide nanoparticles.
Example 38
1L of 1M sodium sulfate aqueous solution is prepared, 0.1mol of nickel nitrate and 0.1mol of sodium ethylene diamine tetracetate are added, and the mixture is stirred and dissolved into a transparent aqueous solution. Adding 1L of ethanol, drying the obtained precipitate, calcining below the melting point of sodium sulfate, cooling, washing with deionized water for 2-3 times, and drying to obtain the high-dispersion nickel oxide nanoparticles.
Example 39
1L of 1M sodium sulfate aqueous solution is prepared, 0.1mol of nickel nitrate and 0.1mol of potassium ethylene diamine tetraacetate are added, and the mixture is stirred and dissolved into transparent aqueous solution. Adding 1L of ethanol, drying the obtained precipitate, calcining below the melting point of sodium sulfate, cooling, washing with deionized water for 2-3 times, and drying to obtain the high-dispersion nickel oxide nanoparticles.
Example 40
1L of 1M sodium sulfate aqueous solution is prepared, 0.1mol of nickel nitrate and 0.1mol of gluconic acid are added, and the mixture is stirred and dissolved into transparent aqueous solution. Adding 1L of ethanol, drying the obtained precipitate, calcining below the melting point of sodium sulfate, cooling, washing with deionized water for 2-3 times, and drying to obtain the high-dispersion nickel oxide nanoparticles.
EXAMPLE 41
1L of 1M sodium sulfate aqueous solution is prepared, 0.1mol of nickel nitrate and 0.1mol of sodium gluconate are added, and the mixture is stirred and dissolved into a transparent aqueous solution. Adding 1L of ethanol, drying the obtained precipitate, calcining below the melting point of sodium sulfate, cooling, washing with deionized water for 2-3 times, and drying to obtain the high-dispersion nickel oxide nanoparticles.
Example 42
1L of 1M sodium sulfate aqueous solution is prepared, 0.1mol of nickel nitrate and 0.1mol of potassium gluconate are added, and the mixture is stirred and dissolved into a transparent aqueous solution. Adding 1L of ethanol, drying the obtained precipitate, calcining below the melting point of sodium sulfate, cooling, washing with deionized water for 2-3 times, and drying to obtain the high-dispersion nickel oxide nanoparticles.
Example 43
1L of 1M sodium sulfate aqueous solution is prepared, 0.1mol of nickel nitrate and 0.1mol of glucoheptonic acid are added, and the mixture is stirred and dissolved into a transparent aqueous solution. Adding 1L of ethanol, drying the obtained precipitate, calcining below the melting point of sodium sulfate, cooling, washing with deionized water for 2-3 times, and drying to obtain the high-dispersion nickel oxide nanoparticles.
Example 44
1L of 1M sodium sulfate aqueous solution is prepared, 0.1mol of nickel nitrate and 0.1mol of sodium glucoheptonate are added, and the mixture is stirred and dissolved into a transparent aqueous solution. Adding 1L of ethanol, drying the obtained precipitate, calcining below the melting point of sodium sulfate, cooling, washing with deionized water for 2-3 times, and drying to obtain the high-dispersion nickel oxide nanoparticles.
Example 45
1L of a 1M aqueous solution of sodium sulfate was prepared, and 0.1mol of nickel nitrate and 0.1mol of potassium gluceptate were added thereto and dissolved by stirring to obtain a transparent aqueous solution. Adding 1L of ethanol, drying the obtained precipitate, calcining below the melting point of sodium sulfate, cooling, washing with deionized water for 2-3 times, and drying to obtain the high-dispersion nickel oxide nanoparticles.
Example 46
1L of 1M aqueous solution of sodium sulfate was prepared, and 0.1mol of nickel nitrate and 0.1mol of potassium glucoheptonate were added and dissolved by stirring to obtain a transparent aqueous solution. Adding 1L of ethanol, drying the obtained precipitate, calcining below the melting point of sodium sulfate, cooling, washing with deionized water for 2-3 times, and drying to obtain the high-dispersion nickel oxide nanoparticles.
Example 47
1L of 2M sodium carbonate aqueous solution is prepared, 0.5mol of nickel nitrate and 0.5mol of polyacrylic acid are added, and the mixture is stirred and dissolved into transparent aqueous solution. Adding 1L ethanol, drying the obtained precipitate, calcining below the melting point of sodium carbonate salt, cooling, washing with deionized water for 2-3 times, and drying to obtain the high-dispersion nickel oxide nano-particles.
Example 48
1L of 2M sodium carbonate aqueous solution is prepared, 0.5mol of nickel nitrate and 0.5mol of polyacrylic acid are added, and the mixture is stirred and dissolved into transparent aqueous solution. Adding 1L of propanol, drying the obtained precipitate, calcining below the melting point of sodium carbonate salt, cooling, washing with deionized water for 2-3 times, and drying to obtain the high-dispersion nickel oxide nano-particles.
Example 49
1L of 2M sodium carbonate aqueous solution is prepared, 0.5mol of nickel nitrate and 0.5mol of polyacrylic acid are added, and the mixture is stirred and dissolved into transparent aqueous solution. Adding 1L of isopropanol, drying the obtained precipitate, calcining below the melting point of sodium carbonate salt, cooling, washing with deionized water for 2-3 times, and drying to obtain the high-dispersion nickel oxide nano-particles.
Example 50
1L of 2M sodium carbonate aqueous solution is prepared, 0.5mol of nickel nitrate and 0.5mol of polyacrylic acid are added, and the mixture is stirred and dissolved into transparent aqueous solution. Adding 1L of tertiary butanol, drying the obtained precipitate, calcining below the melting point of sodium carbonate salt, cooling, washing with deionized water for 2-3 times, and drying to obtain the high-dispersion nickel oxide nano-particles.
Example 51
1L of 2M sodium carbonate aqueous solution is prepared, 0.5mol of nickel nitrate and 0.5mol of polyacrylic acid are added, and the mixture is stirred and dissolved into transparent aqueous solution. Adding 2 liters of ethylene glycol monomethyl ether, drying the obtained precipitate, calcining below the melting point of sodium carbonate salt, cooling, washing with deionized water for 2-3 times, and drying to obtain the high-dispersion nickel oxide nano-particles.
Example 52
1L of 2M sodium carbonate aqueous solution is prepared, 0.5mol of nickel nitrate and 0.5mol of polyacrylic acid are added, and the mixture is stirred and dissolved into transparent aqueous solution. Adding 2 liters of ethylene glycol ethyl ether, drying the obtained precipitate, calcining below the melting point of sodium carbonate salt, cooling, washing with deionized water for 2-3 times, and drying to obtain the high-dispersion nickel oxide nano-particles.
Example 53
1L of 2M sodium carbonate aqueous solution is prepared, 0.5mol of nickel nitrate and 0.5mol of polyacrylic acid are added, and the mixture is stirred and dissolved into transparent aqueous solution. Adding 2 liters of ethylene glycol monobutyl ether, drying the obtained precipitate, calcining below the melting point of sodium carbonate salt, cooling, washing for 2-3 times by deionized water, and drying to obtain the high-dispersion nickel oxide nano-particles.
Example 54
1L of 2M sodium carbonate aqueous solution is prepared, 0.5mol of nickel nitrate and 0.5mol of polyacrylic acid are added, and the mixture is stirred and dissolved into transparent aqueous solution. Adding 2 liters of diethylene glycol butyl ether, drying the obtained precipitate, calcining below the melting point of sodium carbonate salt, cooling, washing for 2-3 times by using deionized water, and drying to obtain the high-dispersion nickel oxide nano-particles.
Example 55
1L of 2M sodium carbonate aqueous solution is prepared, 0.5mol of nickel nitrate and 0.5mol of polyacrylic acid are added, and the mixture is stirred and dissolved into transparent aqueous solution. Adding 2 liters of dimethylformamide, drying the obtained precipitate, calcining below the melting point of sodium carbonate salt, cooling, washing with deionized water for 2-3 times, and drying to obtain the high-dispersion nickel oxide nano-particles.
Example 56
1L of 2M sodium carbonate aqueous solution is prepared, 0.5mol of nickel nitrate and 0.5mol of polyacrylic acid are added, and the mixture is stirred and dissolved into transparent aqueous solution. Adding 2 liters of dimethyl sulfoxide, drying the obtained precipitate, calcining below the melting point of sodium carbonate salt, cooling, washing for 2-3 times by deionized water, and drying to obtain the high-dispersion nickel oxide nano-particles.
Example 57
1L of 2M sodium carbonate aqueous solution is prepared, 0.5mol of cerium nitrate and 0.5mol of polyacrylic acid are added, and the mixture is stirred and dissolved into transparent aqueous solution. Adding 1L of ethanol, drying the obtained precipitate, calcining below the melting point of sodium carbonate salt, cooling, washing with deionized water for 2-3 times, and drying to obtain the high-dispersion cerium oxide nano-particles.
Example 48
1L of 2M sodium carbonate aqueous solution is prepared, 0.5mol of cerium nitrate and 0.5mol of polyacrylic acid are added, and the mixture is stirred and dissolved into transparent aqueous solution. Adding 1L of propanol, drying the obtained precipitate, calcining below the melting point of sodium carbonate salt, cooling, washing with deionized water for 2-3 times, and drying to obtain the high-dispersion cerium oxide nano-particles.
Example 59
1L of 2M sodium carbonate aqueous solution is prepared, 0.5mol of cerium nitrate and 0.5mol of polyacrylic acid are added, and the mixture is stirred and dissolved into transparent aqueous solution. Adding 1L of isopropanol, drying the obtained precipitate, calcining below the melting point of sodium carbonate salt, cooling, washing with deionized water for 2-3 times, and drying to obtain the high-dispersion cerium oxide nano-particles.
Example 60
1L of 2M sodium carbonate aqueous solution is prepared, 0.5mol of cerium nitrate and 0.5mol of polyacrylic acid are added, and the mixture is stirred and dissolved into transparent aqueous solution. Adding 1L of tertiary butanol, drying the obtained precipitate, calcining below the melting point of sodium carbonate salt, cooling, washing with deionized water for 2-3 times, and drying to obtain the high-dispersion cerium oxide nano-particles.
Example 61
1L of 2M sodium carbonate aqueous solution is prepared, 0.5mol of cerium nitrate and 0.5mol of polyacrylic acid are added, and the mixture is stirred and dissolved into transparent aqueous solution. Adding 2 liters of ethylene glycol monomethyl ether, drying the obtained precipitate, calcining below the melting point of sodium carbonate salt, cooling, washing with deionized water for 2-3 times, and drying to obtain the high-dispersion cerium oxide nano-particles.
Example 62
1L of 2M sodium carbonate aqueous solution is prepared, 0.5mol of cerium nitrate and 0.5mol of polyacrylic acid are added, and the mixture is stirred and dissolved into transparent aqueous solution. Adding 2 liters of ethylene glycol ethyl ether, drying the obtained precipitate, calcining below the melting point of sodium carbonate salt, cooling, washing with deionized water for 2-3 times, and drying to obtain the high-dispersion cerium oxide nano-particles.
Example 63
1L of 2M sodium carbonate aqueous solution is prepared, 0.5mol of cerium nitrate and 0.5mol of polyacrylic acid are added, and the mixture is stirred and dissolved into transparent aqueous solution. Adding 2 liters of ethylene glycol monobutyl ether, drying the obtained precipitate, calcining below the melting point of sodium carbonate salt, cooling, washing with deionized water for 2-3 times, and drying to obtain the high-dispersion cerium oxide nano-particles.
Example 64
1L of 2M sodium carbonate aqueous solution is prepared, 0.5mol of cerium nitrate and 0.5mol of polyacrylic acid are added, and the mixture is stirred and dissolved into transparent aqueous solution. Adding 2 liters of diethylene glycol monobutyl ether, drying the obtained precipitate, calcining below the melting point of sodium carbonate salt, cooling, washing for 2-3 times by deionized water, and drying to obtain the high-dispersion cerium oxide nano-particles.
Example 65
1L of 2M sodium carbonate aqueous solution is prepared, 0.5mol of cerium nitrate and 0.5mol of polyacrylic acid are added, and the mixture is stirred and dissolved into transparent aqueous solution. Adding 2 liters of dimethylformamide, drying the obtained precipitate, calcining below the melting point of sodium carbonate salt, cooling, washing with deionized water for 2-3 times, and drying to obtain the high-dispersion cerium oxide nano-particles.
Example 66
1L of 2M sodium carbonate aqueous solution is prepared, 0.5mol of cerium nitrate and 0.5mol of polyacrylic acid are added, and the mixture is stirred and dissolved into transparent aqueous solution. Adding 2L of dimethyl sulfoxide, drying the obtained precipitate, calcining below the melting point of sodium carbonate salt, cooling, washing with deionized water for 2-3 times, and drying to obtain the high-dispersion cerium oxide nano-particles.
Example 67
1L of 2M potassium carbonate aqueous solution is prepared, 0.5mol of cerium nitrate is added, and the mixture is stirred and dissolved into a transparent aqueous solution. Adding 2 liters of dimethyl sulfoxide, drying the obtained precipitate, calcining below the melting point of potassium carbonate, cooling, washing with deionized water for 2-3 times, and drying to obtain the high-dispersion cerium oxide nano-particles.
Example 68
1L of 2M sodium chloride aqueous solution is prepared, 1mol of cerium nitrate and 1mol of polyacrylic acid are added, and the mixture is stirred and dissolved into transparent aqueous solution. Adding 2 liters of ethanol, drying the obtained precipitate, calcining below the melting point of sodium chloride, cooling, washing with deionized water for 2-3 times, and drying to obtain the high-dispersion cerium oxide nano-particles.
Example 69
1L of 2M potassium chloride aqueous solution is prepared, 1mol of cerium nitrate and 1mol of polyacrylic acid are added, and the mixture is stirred and dissolved into transparent aqueous solution. Adding 2 liters of ethanol, drying the obtained precipitate, calcining below the melting point of sodium chloride, cooling, washing with deionized water for 2-3 times, and drying to obtain the high-dispersion cerium oxide nano-particles.
Example 70
1L of 2M sodium carbonate aqueous solution is prepared, 0.5mol of nickel nitrate and 0.5mol of polyacrylic acid are added, and the mixture is stirred and dissolved into transparent aqueous solution. Adding 2L of dimethyl sulfoxide, drying the obtained precipitate, calcining below the melting point of sodium carbonate salt, cooling, washing with deionized water for 2-3 times, and drying to obtain the high-dispersion nickel oxide nano-particles.
Example 71
1L of 2M potassium carbonate aqueous solution is prepared, 0.5mol of nickel nitrate and 0.5mol of polyacrylic acid are added, and the mixture is stirred and dissolved into a transparent aqueous solution. Adding 2L of dimethyl sulfoxide, drying the obtained precipitate, calcining below the melting point of potassium carbonate, cooling, washing with deionized water for 2-3 times, and drying to obtain the high-dispersion nickel oxide nanoparticles.
Example 72
1L of 2M sodium chloride aqueous solution is prepared, 1mol of nickel nitrate and 1mol of polyacrylic acid are added, and the mixture is stirred and dissolved into transparent aqueous solution. Adding 2 liters of ethanol, drying the obtained precipitate, calcining below the melting point of sodium chloride salt, cooling, washing with deionized water for 2-3 times, and drying to obtain the high-dispersion nickel oxide nano-particles.
Example 73
1L of 2M potassium chloride aqueous solution is prepared, 1mol of nickel nitrate and 1mol of polyacrylic acid are added, and the mixture is stirred and dissolved into transparent aqueous solution. Adding 2L ethanol, drying the obtained precipitate, calcining below the melting point of potassium chloride salt, cooling, washing with deionized water for 2-3 times, and drying to obtain the high-dispersion nickel oxide nanoparticles.
Example 74
1L of 2M sodium sulfate aqueous solution is prepared, 1mol of nickel nitrate and 0.1mol of polyacrylic acid are added, and the mixture is stirred and dissolved into transparent aqueous solution. Adding 1L of ethanol, drying the obtained precipitate, calcining below the melting point of sodium sulfate, cooling, washing with deionized water for 2-3 times, and drying to obtain the high-dispersion nickel oxide nanoparticles.
Example 75
1L of 2M sodium sulfate aqueous solution is prepared, 1mol of nickel nitrate and 0.1mol of polyacrylic acid are added, and the mixture is stirred and dissolved into transparent aqueous solution. Adding 1L of ethanol, drying the obtained precipitate, calcining below the melting point of sodium sulfate, cooling, washing with deionized water for 2-3 times, and drying to obtain the high-dispersion nickel oxide nanoparticles.
Example 76
1L of 2M sodium sulfate aqueous solution is prepared, 1mol of nickel nitrate and 0.5mol of polyacrylic acid are added, and the mixture is stirred and dissolved into transparent aqueous solution. Adding 1L of ethanol, drying the obtained precipitate, calcining below the melting point of sodium sulfate, cooling, washing with deionized water for 2-3 times, and drying to obtain the high-dispersion nickel oxide nanoparticles.
Example 77
1L of 2M sodium sulfate aqueous solution is prepared, 1mol of nickel nitrate and 1mol of polyacrylic acid are added, and the mixture is stirred and dissolved into transparent aqueous solution. Adding 1L of ethanol, drying the obtained precipitate, calcining below the melting point of sodium sulfate, cooling, washing with deionized water for 2-3 times, and drying to obtain the high-dispersion nickel oxide nanoparticles.
Example 78
1L of 2M sodium sulfate aqueous solution is prepared, 1mol of cerium nitrate and 0.1mol of polyacrylic acid are added, and the mixture is stirred and dissolved into transparent aqueous solution. Adding 1L of ethanol, drying the obtained precipitate, calcining below the melting point of sodium sulfate, cooling, washing with deionized water for 2-3 times, and drying to obtain the high-dispersion cerium oxide nanoparticles.
Example 79
1L of 2M sodium sulfate aqueous solution is prepared, 1mol of cerium nitrate and 0.5mol of polyacrylic acid are added, and the mixture is stirred and dissolved into transparent aqueous solution. Adding 1L of ethanol, drying the obtained precipitate, calcining below the melting point of sodium sulfate, cooling, washing with deionized water for 2-3 times, and drying to obtain the high-dispersion cerium oxide nanoparticles.
Example 80
1L of 2M sodium sulfate aqueous solution is prepared, 1mol of cerium nitrate and 1mol of polyacrylic acid are added, and the mixture is stirred and dissolved into transparent aqueous solution. Adding 1L of ethanol, drying the obtained precipitate, calcining below the melting point of sodium sulfate, cooling, washing with deionized water for 2-3 times, and drying to obtain the high-dispersion cerium oxide nanoparticles.
Morphology tests were performed on the nanoparticles prepared in examples 11, 13, 18, 23, 28, 33, 57 and 79, and the results are shown in fig. 1 to 8, which show that the dispersibility is good.
In the absence of the water-soluble salt of the above example, the aqueous solution of the metal complex is highly stable and does not precipitate when an organic solvent is added. However, in the above embodiment, when the water-soluble salt is dissolved again in the aqueous solution of the metal complex, the dissolution property of the metal complex changes, and the metal complex precipitates together with the water-soluble salt after the addition of the organic solvent, and forms a state in which the metal complex is isolated and dispersed by the water-soluble salt, which is also a novel point of the above embodiment.
The preparation method of the cerium oxide-based nanoparticles is specifically described below with reference to specific examples.
Example 81
1 liter of 0.5M potassium sulfate solution is prepared by deionized water, and 0.1mol of cerium nitrate, 0.001mol of lanthanum nitrate, 0.001mol of cobalt nitrate and 0.05mol of polyacrylic acid are added and stirred for dissolution. Adding 1L of ethanol to obtain a precipitate, drying, calcining below the melting point of potassium sulfate, cooling, washing with water for 2-3 times, and drying to obtain the high-dispersion cerium oxide-based nanoparticles.
Example 82
1L of 0.5M potassium sulfate solution is prepared by deionized water, and 0.1mol of cerium nitrate, 0.001mol of yttrium nitrate, 0.001mol of gadolinium nitrate and 0.05mol of polyacrylic acid are added and stirred for dissolution. Adding 1L of ethanol to obtain a precipitate, drying, calcining below the melting point of potassium sulfate, cooling, washing with water for 2-3 times, and drying to obtain the high-dispersion cerium oxide-based nanoparticles.
Example 83
1 liter of 0.5M potassium sulfate solution is prepared by deionized water, and 0.1mol of cerium nitrate, 0.001mol of nickel nitrate, 0.001mol of copper nitrate, 0.001mol of manganese nitrate and 0.05mol of polyacrylic acid are added and stirred for dissolution. Adding 1L of ethanol to obtain a precipitate, drying, calcining below the melting point of potassium sulfate, cooling, washing with water for 2-3 times, and drying to obtain the high-dispersion cerium oxide-based nanoparticles.
Example 84
1L of 0.5M potassium sulfate solution is prepared by deionized water, and 0.1mol of cerium nitrate and 0.05mol of polyacrylic acid are added and stirred for dissolution. Adding 1L of ethanol to obtain a precipitate, drying, calcining below the melting point of potassium sulfate, cooling, washing with water for 2-3 times, and drying to obtain the high-dispersion cerium oxide-based nanoparticles.
Example 85
1L of 0.5M potassium sulfate solution is prepared by deionized water, and 0.1mol of cerium acetate, 0.01mol of lanthanum acetate and 0.05mol of polyacrylic acid are added and stirred for dissolution. Adding 1L of ethanol to obtain a precipitate, drying, calcining below the melting point of potassium sulfate, cooling, washing with water for 2-3 times, and drying to obtain the high-dispersion cerium oxide-based nanoparticles.
Example 86
1L of 0.5M potassium sulfate solution is prepared by deionized water, and 0.1mol of cerium sulfate, 0.01mol of lanthanum sulfate and 0.05mol of polyacrylic acid are added and stirred for dissolution. Adding 1L of ethanol to obtain a precipitate, drying, calcining below the melting point of potassium sulfate, cooling, washing with water for 2-3 times, and drying to obtain the high-dispersion cerium oxide-based nanoparticles.
Example 87
1L of 0.5M potassium sulfate solution is prepared by deionized water, and 0.1mol of cerium chloride, 0.01mol of lanthanum chloride and 0.05mol of polyacrylic acid are added and stirred for dissolution. Adding 1L of ethanol to obtain a precipitate, drying, calcining below the melting point of potassium sulfate, cooling, washing with water for 2-3 times, and drying to obtain the high-dispersion cerium oxide-based nanoparticles.
Example 88
1L of 0.5M potassium sulfate solution is prepared by deionized water, and 0.1mol of cerium nitrate, 0.01mol of lanthanum nitrate and 0.1mol of polyacrylic acid are added and stirred for dissolution. Adding 1L of ethanol to obtain a precipitate, drying, calcining below the melting point of potassium sulfate, cooling, washing with water for 2-3 times, and drying to obtain the high-dispersion cerium oxide-based nanoparticles.
Example 89
1L of 0.5M potassium sulfate solution is prepared by deionized water, and 0.1mol of cerium nitrate, 0.01mol of lanthanum nitrate and 0.1mol of potassium polyacrylate are added and stirred for dissolution. Adding 1L of ethanol to obtain a precipitate, drying, calcining below the melting point of potassium sulfate, cooling, washing with water for 2-3 times, and drying to obtain the high-dispersion cerium oxide-based nanoparticles.
Example 90
1L of 0.5M potassium sulfate solution is prepared by deionized water, and 0.1mol of cerium nitrate, 0.01mol of lanthanum nitrate and 0.1mol of sodium polyacrylate are added and stirred for dissolution. Adding 1L of ethanol to obtain a precipitate, drying, calcining below the melting point of potassium sulfate, cooling, washing with water for 2-3 times, and drying to obtain the high-dispersion cerium oxide-based nanoparticles.
Example 91
1L of 0.5M potassium sulfate solution is prepared by deionized water, and 0.1mol of cerium nitrate, 0.01mol of lanthanum nitrate and 0.1mol of ammonium polyacrylate are added and stirred for dissolution. Adding 1L of ethanol to obtain a precipitate, drying, calcining below the melting point of potassium sulfate, cooling, washing with water for 2-3 times, and drying to obtain the high-dispersion cerium oxide-based nanoparticles.
Example 92
1L of 0.5M potassium sulfate solution is prepared by deionized water, and 0.1mol of cerium nitrate, 0.01mol of lanthanum nitrate and 0.1mol of citric acid are added and stirred for dissolution. Adding 1L of ethanol to obtain a precipitate, drying, calcining below the melting point of potassium sulfate, cooling, washing with water for 2-3 times, and drying to obtain the high-dispersion cerium oxide-based nanoparticles.
Example 93
1L of 0.5M potassium sulfate solution is prepared by deionized water, and 0.1mol of cerium nitrate, 0.01mol of lanthanum nitrate and 0.1mol of potassium citrate are added and stirred for dissolution. Adding 1L of ethanol to obtain a precipitate, drying, calcining below the melting point of potassium sulfate, cooling, washing with water for 2-3 times, and drying to obtain the high-dispersion cerium oxide-based nanoparticles.
Example 94
1L of 0.5M potassium sulfate solution is prepared by deionized water, and 0.1mol of cerium nitrate, 0.01mol of lanthanum nitrate and 0.1mol of sodium citrate are added and stirred for dissolution. Adding 1L of ethanol to obtain a precipitate, drying, calcining below the melting point of potassium sulfate, cooling, washing with water for 2-3 times, and drying to obtain the high-dispersion cerium oxide-based nanoparticles.
Example 95
1L of 0.5M potassium sulfate solution is prepared by deionized water, and 0.1mol of cerium nitrate, 0.01mol of lanthanum nitrate and 0.05mol of ethylenediamine tetraacetic acid are added and stirred for dissolution. Adding 1L of ethanol to obtain a precipitate, drying, calcining below the melting point of potassium sulfate, cooling, washing with water for 2-3 times, and drying to obtain the high-dispersion cerium oxide-based nanoparticles.
Example 96
1L of 0.5M potassium sulfate solution is prepared by deionized water, and 0.1mol of cerium nitrate, 0.01mol of lanthanum nitrate and 0.1mol of potassium ethylene diamine tetraacetate are added and stirred for dissolution. Adding 1L of ethanol to obtain a precipitate, drying, calcining below the melting point of potassium sulfate, cooling, washing with water for 2-3 times, and drying to obtain the high-dispersion cerium oxide-based nanoparticles.
Example 97
1L of 0.5M potassium sulfate solution is prepared by deionized water, and 0.1mol of cerium nitrate, 0.01mol of lanthanum nitrate and 0.1mol of sodium ethylene diamine tetracetate are added and stirred for dissolution. Adding 1L of ethanol to obtain a precipitate, drying, calcining below the melting point of potassium sulfate, cooling, washing with water for 2-3 times, and drying to obtain the high-dispersion cerium oxide-based nanoparticles.
Example 98
1L of 0.5M potassium sulfate solution is prepared by deionized water, and 0.1mol of cerium nitrate, 0.01mol of lanthanum nitrate and 0.1mol of tartaric acid are added and stirred for dissolution. Adding 1L of ethanol to obtain a precipitate, drying, calcining below the melting point of potassium sulfate, cooling, washing with water for 2-3 times, and drying to obtain the high-dispersion cerium oxide-based nanoparticles.
Example 99
1L of 0.5M potassium sulfate solution is prepared by deionized water, and 0.1mol of cerium nitrate, 0.01mol of lanthanum nitrate and 0.1mol of potassium tartrate are added and stirred for dissolution. Adding 1L of ethanol to obtain a precipitate, drying, calcining below the melting point of potassium sulfate, cooling, washing with water for 2-3 times, and drying to obtain the high-dispersion cerium oxide-based nanoparticles.
Example 100
1L of 0.5M potassium sulfate solution is prepared by deionized water, and 0.1mol of cerium nitrate, 0.01mol of lanthanum nitrate and 0.1mol of sodium tartrate are added and stirred for dissolution. Adding 1L of ethanol to obtain a precipitate, drying, calcining below the melting point of potassium sulfate, cooling, washing with water for 2-3 times, and drying to obtain the high-dispersion cerium oxide-based nanoparticles.
Example 101
1L of 0.5M potassium sulfate solution is prepared by deionized water, and 0.1mol of cerium nitrate, 0.01mol of lanthanum nitrate and 0.1mol of gluconic acid are added and stirred for dissolution. Adding 1L of ethanol to obtain a precipitate, drying, calcining below the melting point of potassium sulfate, cooling, washing with water for 2-3 times, and drying to obtain the high-dispersion cerium oxide-based nanoparticles.
Example 102
1L of 0.5M potassium sulfate solution is prepared by deionized water, and 0.1mol of cerium nitrate, 0.01mol of lanthanum nitrate and 0.1mol of potassium gluconate are added and stirred for dissolution. Adding 1L of ethanol to obtain a precipitate, drying, calcining below the melting point of potassium sulfate, cooling, washing with water for 2-3 times, and drying to obtain the high-dispersion cerium oxide-based nanoparticles.
Example 103
1 liter of 0.5M potassium sulfate solution is prepared by deionized water, and 0.1mol of cerium nitrate, 0.01mol of lanthanum nitrate and 0.1mol of sodium gluconate are added and stirred for dissolution. Adding 1L of ethanol to obtain a precipitate, drying, calcining below the melting point of potassium sulfate, cooling, washing with water for 2-3 times, and drying to obtain the high-dispersion cerium oxide-based nanoparticles.
Example 104
1L of 0.5M potassium sulfate solution is prepared by deionized water, and 0.1mol of cerium nitrate, 0.01mol of lanthanum nitrate and 0.1mol of glucoheptonic acid are added and stirred for dissolution. Adding 1L of ethanol to obtain a precipitate, drying, calcining below the melting point of potassium sulfate, cooling, washing with water for 2-3 times, and drying to obtain the high-dispersion cerium oxide-based nanoparticles.
Example 105
1L of 0.5M potassium sulfate solution is prepared by deionized water, and 0.1mol of cerium nitrate, 0.01mol of lanthanum nitrate and 0.1mol of potassium glucoheptonate are added and stirred for dissolution. Adding 1L of ethanol to obtain a precipitate, drying, calcining below the melting point of potassium sulfate, cooling, washing with water for 2-3 times, and drying to obtain the high-dispersion cerium oxide-based nanoparticles.
Example 106
1L of 0.5M potassium sulfate solution is prepared by deionized water, and 0.1mol of cerium nitrate, 0.01mol of lanthanum nitrate and 0.1mol of sodium glucoheptonate are added and stirred for dissolution. Adding 1L of ethanol to obtain a precipitate, drying, calcining below the melting point of potassium sulfate, cooling, washing with water for 2-3 times, and drying to obtain the high-dispersion cerium oxide-based nanoparticles.
Example 107
1L of 1M sodium sulfate solution is prepared by deionized water, and 0.5mol of cerous nitrate, 0.01mol of lanthanum nitrate and 0.5mol of polyacrylic acid are added and stirred for dissolution. Adding 2L of ethanol to obtain a precipitate, drying, calcining below the melting point of sodium sulfate, cooling, washing with water for 2-3 times, and drying to obtain the high-dispersion cerium oxide-based nanoparticles.
Example 108
1L of 1M sodium sulfate solution is prepared by deionized water, and 0.5mol of cerous nitrate, 0.01mol of lanthanum nitrate and 0.5mol of polyacrylic acid are added and stirred for dissolution. Adding 2L of isopropanol to obtain a precipitate, drying, calcining below the melting point of sodium sulfate, cooling, washing with water for 2-3 times, and drying to obtain the high-dispersion cerium oxide-based nanoparticles.
Example 109
1L of 1M sodium sulfate solution is prepared by deionized water, and 0.5mol of cerous nitrate, 0.01mol of lanthanum nitrate and 0.5mol of polyacrylic acid are added and stirred for dissolution. Adding 2 liters of propanol to obtain a precipitate, drying, calcining below the melting point of sodium sulfate, cooling, washing with water for 2-3 times, and drying to obtain the high-dispersion cerium oxide-based nano-particles.
Example 110
1L of 1M sodium sulfate solution is prepared by deionized water, and 0.5mol of cerium nitrate, 0.01mol of lanthanum nitrate and 0.5mol of polyacrylic acid are added and stirred for dissolution. Adding 2 liters of tertiary butanol to obtain a precipitate, drying, calcining below the melting point of sodium sulfate, cooling, washing with water for 2-3 times, and drying to obtain the high-dispersion cerium oxide-based nano-particles.
Example 111
1L of 1M sodium sulfate solution is prepared by deionized water, and 0.5mol of cerous nitrate, 0.01mol of lanthanum nitrate and 0.5mol of polyacrylic acid are added and stirred for dissolution. Adding 2 liters of ethylene glycol ethyl ether to obtain a precipitate, drying, calcining below the melting point of sodium sulfate, cooling, washing with water for 2-3 times, and drying to obtain the high-dispersion cerium oxide-based nano particles.
Example 112
1L of 1M sodium sulfate solution is prepared by deionized water, and 0.5mol of cerium nitrate, 0.01mol of lanthanum nitrate and 0.5mol of polyacrylic acid are added and stirred for dissolution. Adding 2 liters of ethylene glycol monomethyl ether to obtain a precipitate, drying, calcining below the melting point of sodium sulfate, cooling, washing with water for 2-3 times, and drying to obtain the high-dispersion cerium oxide-based nano particles.
Example 113
1L of 1M sodium sulfate solution is prepared by deionized water, and 0.5mol of cerium nitrate, 0.01mol of lanthanum nitrate and 0.5mol of polyacrylic acid are added and stirred for dissolution. Adding 2 liters of ethylene glycol monobutyl ether to obtain a precipitate, drying, calcining below the melting point of sodium sulfate, cooling, washing with water for 2-3 times, and drying to obtain the high-dispersion cerium oxide-based nano-particles.
Example 114
1L of 1M sodium sulfate solution is prepared by deionized water, and 0.5mol of cerium nitrate, 0.01mol of lanthanum nitrate and 0.5mol of polyacrylic acid are added and stirred for dissolution. Adding 2L of diethylene glycol monobutyl ether to obtain a precipitate, drying, calcining below the melting point of sodium sulfate, cooling, washing with water for 2-3 times, and drying to obtain the high-dispersion cerium oxide-based nano particles.
Example 115
1L of 1M sodium sulfate solution is prepared by deionized water, and 0.5mol of cerous nitrate, 0.01mol of lanthanum nitrate and 0.5mol of polyacrylic acid are added and stirred for dissolution. Adding 2L dimethyl sulfoxide to obtain precipitate, drying, calcining below the melting point of sodium sulfate, cooling, washing with water for 2-3 times, and drying to obtain high-dispersion cerium oxide-based nanoparticles.
Example 116
1L of 2M potassium carbonate solution is prepared with deionized water, and 0.5mol of cerium nitrate is added and dissolved with stirring. Adding 2 liters of dimethyl sulfoxide to obtain a precipitate, drying, calcining below the melting point of potassium carbonate, cooling, washing with water for 2-3 times, and drying to obtain the high-dispersion cerium oxide-based nano-particles.
Example 117
1L of 1M sodium chloride solution is prepared by deionized water, and 0.5mol of cerium nitrate, 0.01mol of lanthanum nitrate and 0.5mol of polyacrylic acid are added and stirred for dissolution. Adding 2L of ethanol to obtain a precipitate, drying, calcining below the melting point of sodium chloride, cooling, washing with water for 2-3 times, and drying to obtain the high-dispersion cerium oxide-based nanoparticles.
Example 118
1L of 1M potassium chloride solution is prepared by deionized water, and 0.5mol of cerium nitrate, 0.01mol of lanthanum nitrate and 0.5mol of polyacrylic acid are added and stirred for dissolution. Adding 2 liters of ethanol to obtain a precipitate, drying, calcining below the melting point of potassium chloride salt, cooling, washing with water for 2-3 times, and drying to obtain the high-dispersion cerium oxide-based nano-particles.
Example 119
1L of 1M sodium carbonate solution is prepared by deionized water, and 0.5mol of cerium nitrate, 0.01mol of lanthanum nitrate and 0.5mol of polyacrylic acid are added and stirred for dissolution. Adding 2 liters of ethanol to obtain a precipitate, drying, calcining below the melting point of sodium carbonate salt, cooling, washing with water for 2-3 times, and drying to obtain the high-dispersion cerium oxide-based nano-particles.
Example 120
1L of 1M potassium carbonate solution is prepared by deionized water, and 0.5mol of cerium nitrate, 0.01mol of lanthanum nitrate and 0.5mol of polyacrylic acid are added and stirred for dissolution. Adding 2L ethanol to obtain precipitate, oven drying, calcining below the melting point of potassium carbonate, cooling, washing with water for 2-3 times, and drying to obtain high-dispersion cerium oxide-based nanoparticles.
Example 121
1L of 1M sodium sulfate solution is prepared by deionized water, and 0.5mol of cerium acetate, 0.01mol of lanthanum acetate and 0.5mol of polyacrylic acid are added and stirred for dissolution. Adding 2L of ethanol to obtain a precipitate, drying, calcining below the melting point of sodium sulfate, cooling, washing with water for 2-3 times, and drying to obtain the high-dispersion cerium oxide-based nanoparticles.
Example 122
1L of 1M sodium sulfate solution is prepared by deionized water, and 0.5mol of cerium acetate, 0.01mol of lanthanum acetate and 0.05mol of polyacrylic acid are added and stirred for dissolution. Adding 2L of ethanol to obtain a precipitate, drying, calcining below the melting point of sodium sulfate, cooling, washing with water for 2-3 times, and drying to obtain the high-dispersion cerium oxide-based nanoparticles.
Example 123
1L of 1M sodium sulfate solution is prepared by deionized water, and 0.5mol of cerium acetate, 0.01mol of lanthanum acetate and 0.25mol of polyacrylic acid are added and stirred for dissolution. Adding 2L of ethanol to obtain a precipitate, drying, calcining below the melting point of sodium sulfate, cooling, washing with water for 2-3 times, and drying to obtain the high-dispersion cerium oxide-based nanoparticles.
Example 124
1 liter of 1M sodium sulfate solution is prepared by deionized water, and 0.5mol of cerium acetate, 0.01mol of lanthanum acetate, 0.01mol of cobalt acetate, 0.01mol of yttrium acetate, 0.01mol of gadolinium acetate, 0.01mol of nickel acetate, 0.01mol of copper acetate, 0.01mol of manganese acetate and 0.25mol of polyacrylic acid are added and stirred for dissolution. Adding 2L of ethanol to obtain a precipitate, drying, calcining below the melting point of sodium sulfate, cooling, washing with water for 2-3 times, and drying to obtain the high-dispersion cerium oxide-based nanoparticles.
If the water-soluble salt described in the above examples is not added to the aqueous solution of the complex of cerium and the dopant element, the solution stability is high and precipitation does not occur when the organic solvent is added. However, after the cerium oxide-based nanoparticles are dissolved in the water-soluble salt, the solubility of the complex of cerium and the dopant element is changed significantly, and the complex of cerium and the dopant element precipitates out together with the water-soluble salt, which is one of the important factors for efficiently preparing the cerium oxide-based nanoparticles in the above embodiment.
The method of making yttrium doped zirconia nanoparticles is further illustrated by the specific examples below.
Example 125
1 liter of 0.5M potassium sulfate aqueous solution is prepared, and 0.1mol of zirconium nitrate, 0.01mol of yttrium nitrate and 0.05mol of polyacrylic acid are added and stirred to be dissolved. Adding 1L of ethanol while stirring to obtain a precipitate, drying, calcining below the melting point of potassium sulfate, washing with water for 2-3 times, and drying to obtain the high-dispersion yttrium-doped zirconia nanoparticles.
Example 126
1L of 0.5M potassium sulfate aqueous solution is prepared, and 0.1mol of zirconium acetate, 0.01mol of yttrium nitrate and 0.05mol of polyacrylic acid are added and stirred to dissolve. Adding 1L of ethanol while stirring to obtain a precipitate, drying, calcining below the melting point of potassium sulfate, washing with water for 2-3 times, and drying to obtain the high-dispersion yttrium-doped zirconia nanoparticles.
Example 127
1L of 0.5M potassium sulfate aqueous solution is prepared, and 0.1mol of zirconium chloride, 0.01mol of yttrium nitrate and 0.05mol of polyacrylic acid are added and stirred to dissolve. Adding 1L of ethanol while stirring to obtain a precipitate, drying, calcining below the melting point of potassium sulfate, washing with water for 2-3 times, and drying to obtain the high-dispersion yttrium-doped zirconia nanoparticles.
Example 128
1L of 0.5M potassium sulfate aqueous solution is prepared, and 0.1mol of zirconium oxychloride, 0.01mol of yttrium nitrate and 0.05mol of polyacrylic acid are added and stirred to dissolve. Adding 1L of ethanol while stirring to obtain a precipitate, drying, calcining below the melting point of potassium sulfate, washing with water for 2-3 times, and drying to obtain the high-dispersion yttrium-doped zirconia nanoparticles.
Example 129
1L of 0.5M potassium sulfate aqueous solution is prepared, and 0.1mol of zirconium nitrate, 0.01mol of yttrium acetate and 0.05mol of polyacrylic acid are added and stirred to dissolve. Adding 1L of ethanol while stirring to obtain a precipitate, drying, calcining below the melting point of potassium sulfate, washing with water for 2-3 times, and drying to obtain the high-dispersion yttrium-doped zirconia nanoparticles.
Example 130
1L of 0.5M potassium sulfate aqueous solution is prepared, and 0.1mol of zirconium nitrate, 0.01mol of yttrium sulfate and 0.05mol of polyacrylic acid are added and stirred to dissolve. Adding 1L of ethanol while stirring to obtain a precipitate, drying, calcining below the melting point of potassium sulfate, washing with water for 2-3 times, and drying to obtain the high-dispersion yttrium-doped zirconia nanoparticles.
Example 131
1L of 0.5M potassium sulfate aqueous solution is prepared, and 0.1mol of zirconium nitrate, 0.01mol of yttrium chloride and 0.05mol of polyacrylic acid are added and stirred to dissolve. Adding 1L of ethanol while stirring to obtain a precipitate, drying, calcining below the melting point of potassium sulfate, washing with water for 2-3 times, and drying to obtain the high-dispersion yttrium-doped zirconia nanoparticles.
Example 132
1L of 0.5M potassium sulfate aqueous solution is prepared, and 0.1mol of zirconium nitrate, 0.003mol of yttrium nitrate and 0.05mol of polyacrylic acid are added and stirred to dissolve. Adding 1L of ethanol while stirring to obtain a precipitate, drying, calcining below the melting point of potassium sulfate, washing with water for 2-3 times, and drying to obtain the high-dispersion yttrium-doped zirconia nanoparticles.
Example 133
1 liter of 0.5M potassium sulfate aqueous solution is prepared, and 0.1mol of zirconium nitrate, 0.015mol of yttrium nitrate and 0.05mol of polyacrylic acid are added and stirred to be dissolved. Adding 1L of ethanol while stirring to obtain a precipitate, drying, calcining below the melting point of potassium sulfate, washing with water for 2-3 times, and drying to obtain the high-dispersion yttrium-doped zirconia nanoparticles.
Example 134
1L of 0.5M potassium sulfate aqueous solution is prepared, and 0.1mol of zirconium nitrate, 0.01mol of yttrium nitrate and 0.05mol of ammonium polyacrylate are added and stirred for dissolution. Adding 1L of ethanol while stirring to obtain a precipitate, drying, calcining below the melting point of potassium sulfate, washing with water for 2-3 times, and drying to obtain the high-dispersion yttrium-doped zirconia nanoparticles.
Example 135
1L of 0.5M potassium sulfate aqueous solution is prepared, and 0.1mol of zirconium nitrate, 0.01mol of yttrium nitrate and 0.05mol of potassium polyacrylate are added and stirred for dissolution. Adding 1L of ethanol while stirring to obtain a precipitate, drying, calcining below the melting point of potassium sulfate, washing with water for 2-3 times, and drying to obtain the high-dispersion yttrium-doped zirconia nanoparticles.
Example 136
1L of 0.5M potassium sulfate aqueous solution is prepared, and 0.1mol of zirconium nitrate, 0.01mol of yttrium nitrate and 0.05mol of sodium polyacrylate are added and stirred for dissolution. Adding 1L of ethanol while stirring to obtain a precipitate, drying, calcining below the melting point of potassium sulfate, washing with water for 2-3 times, and drying to obtain the high-dispersion yttrium-doped zirconia nanoparticles.
Example 137
1 liter of 0.5M potassium sulfate aqueous solution is prepared, and 0.1mol of zirconium nitrate, 0.01mol of yttrium nitrate and 0.05mol of citric acid are added and stirred to be dissolved. Adding 1L of ethanol while stirring to obtain a precipitate, drying, calcining below the melting point of potassium sulfate, washing with water for 2-3 times, and drying to obtain the high-dispersion yttrium-doped zirconia nanoparticles.
Example 138
1L of 0.5M potassium sulfate aqueous solution is prepared, and 0.1mol of zirconium nitrate, 0.01mol of yttrium nitrate and 0.05mol of potassium citrate are added and stirred to dissolve. Adding 1L of ethanol while stirring to obtain a precipitate, drying, calcining below the melting point of potassium sulfate, washing with water for 2-3 times, and drying to obtain the high-dispersion yttrium-doped zirconia nanoparticles.
Example 139
1 liter of 0.5M potassium sulfate aqueous solution is prepared, and 0.1mol of zirconium nitrate, 0.01mol of yttrium nitrate and 0.05mol of sodium citrate are added and stirred to be dissolved. Adding 1L of ethanol while stirring to obtain a precipitate, drying, calcining below the melting point of potassium sulfate, washing with water for 2-3 times, and drying to obtain the high-dispersion yttrium-doped zirconia nanoparticles.
Example 140
1L of 0.5M potassium sulfate aqueous solution is prepared, and 0.1mol of zirconium nitrate, 0.01mol of yttrium nitrate and 0.05mol of ethylenediamine tetraacetic acid are added and stirred to dissolve. Adding 1L of ethanol while stirring to obtain a precipitate, drying, calcining below the melting point of potassium sulfate, washing with water for 2-3 times, and drying to obtain the high-dispersion yttrium-doped zirconia nanoparticles.
Example 141
1 liter of 0.5M potassium sulfate aqueous solution is prepared, and 0.1mol of zirconium nitrate, 0.01mol of yttrium nitrate and 0.05mol of sodium ethylene diamine tetracetate are added and stirred for dissolution. Adding 1L of ethanol while stirring to obtain a precipitate, drying, calcining below the melting point of potassium sulfate, washing with water for 2-3 times, and drying to obtain the high-dispersion yttrium-doped zirconia nanoparticles.
Example 142
1L of 0.5M potassium sulfate aqueous solution is prepared, and 0.1mol of zirconium nitrate, 0.01mol of yttrium nitrate and 0.05mol of potassium ethylenediamine tetraacetate are added and stirred for dissolution. Adding 1L of ethanol while stirring to obtain a precipitate, drying, calcining below the melting point of potassium sulfate, washing with water for 2-3 times, and drying to obtain the high-dispersion yttrium-doped zirconia nanoparticles.
Example 143
1L of 0.5M potassium sulfate aqueous solution is prepared, and 0.1mol of zirconium nitrate, 0.01mol of yttrium nitrate and 0.05mol of tartaric acid are added and stirred to dissolve. Adding 1L of ethanol while stirring to obtain a precipitate, drying, calcining below the melting point of potassium sulfate, washing with water for 2-3 times, and drying to obtain the high-dispersion yttrium-doped zirconia nanoparticles.
Example 144
1L of 0.5M potassium sulfate aqueous solution is prepared, and 0.1mol of zirconium nitrate, 0.01mol of yttrium nitrate and 0.05mol of potassium tartrate are added and stirred to dissolve. Adding 1L of ethanol while stirring to obtain a precipitate, drying, calcining below the melting point of potassium sulfate, washing with water for 2-3 times, and drying to obtain the high-dispersion yttrium-doped zirconia nanoparticles.
Example 145
1 liter of 0.5M potassium sulfate aqueous solution is prepared, and 0.1mol of zirconium nitrate, 0.01mol of yttrium nitrate and 0.05mol of gluconic acid are added and stirred for dissolution. Adding 1L of ethanol while stirring to obtain a precipitate, drying, calcining below the melting point of potassium sulfate, washing with water for 2-3 times, and drying to obtain the high-dispersion yttrium-doped zirconia nanoparticles.
Example 146
1L of 0.5M potassium sulfate aqueous solution is prepared, and 0.1mol of zirconium nitrate, 0.01mol of yttrium nitrate and 0.05mol of sodium gluconate are added and stirred for dissolution. Adding 1L of ethanol while stirring to obtain a precipitate, drying, calcining below the melting point of potassium sulfate, washing with water for 2-3 times, and drying to obtain the high-dispersion yttrium-doped zirconia nanoparticles.
Example 147
1L of 0.5M potassium sulfate aqueous solution is prepared, and 0.1mol of zirconium nitrate, 0.01mol of yttrium nitrate and 0.05mol of potassium gluconate are added and stirred to dissolve. Adding 1L of ethanol while stirring to obtain a precipitate, drying, calcining below the melting point of potassium sulfate, washing with water for 2-3 times, and drying to obtain the high-dispersion yttrium-doped zirconia nanoparticles.
Example 148
1 liter of 0.5M potassium sulfate aqueous solution is prepared, and 0.1mol of zirconium nitrate, 0.01mol of yttrium nitrate and 0.05mol of glucoheptonic acid are added and stirred to be dissolved. Adding 1L of ethanol while stirring to obtain a precipitate, drying, calcining below the melting point of potassium sulfate, washing with water for 2-3 times, and drying to obtain the high-dispersion yttrium-doped zirconia nanoparticles.
Example 149
1 liter of 0.5M potassium sulfate aqueous solution is prepared, and 0.1mol of zirconium nitrate, 0.01mol of yttrium nitrate and 0.05mol of sodium glucoheptonate are added and stirred to be dissolved. Adding 1L of ethanol while stirring to obtain a precipitate, drying, calcining below the melting point of potassium sulfate, washing with water for 2-3 times, and drying to obtain the high-dispersion yttrium-doped zirconia nanoparticles.
Example 150
1L of 0.5M potassium sulfate aqueous solution is prepared, and 0.1mol of zirconium nitrate, 0.01mol of yttrium nitrate and 0.05mol of potassium glucoheptonate are added and dissolved with stirring. Adding 1L of ethanol while stirring to obtain a precipitate, drying, calcining below the melting point of potassium sulfate, washing with water for 2-3 times, and drying to obtain the high-dispersion yttrium-doped zirconia nanoparticles.
Example 151
1L of 1M sodium sulfate aqueous solution was prepared, and 0.2mol of zirconium nitrate, 0.02mol of yttrium nitrate and 0.2mol of polyacrylic acid were added and dissolved with stirring. Adding 2 liters of propanol while stirring to obtain a precipitate, drying, calcining below the melting point of sodium sulfate, washing with water for 2-3 times, and drying to obtain the high-dispersion yttrium-doped zirconia nano-particles.
Example 152
1L of 1M sodium sulfate aqueous solution was prepared, and 0.2mol of zirconium nitrate, 0.02mol of yttrium nitrate and 0.2mol of polyacrylic acid were added and dissolved with stirring. Adding 2 liters of tertiary butanol while stirring to obtain a precipitate, drying, calcining below the melting point of sodium sulfate, washing with water for 2-3 times, and drying to obtain the high-dispersion yttrium-doped zirconia nano-particles.
Example 153
1L of 1M sodium sulfate aqueous solution is prepared, and 0.2mol of zirconium nitrate, 0.02mol of yttrium nitrate and 0.2mol of polyacrylic acid are added and dissolved by stirring. Adding 2 liters of isopropanol while stirring to obtain a precipitate, drying, calcining below the melting point of sodium sulfate, washing with water for 2-3 times, and drying to obtain the high-dispersion yttrium-doped zirconia nano-particles.
Example 154
1L of 1M sodium sulfate aqueous solution was prepared, and 0.2mol of zirconium nitrate, 0.02mol of yttrium nitrate and 0.2mol of polyacrylic acid were added and dissolved with stirring. Adding 2 liters of ethylene glycol monomethyl ether while stirring to obtain a precipitate, drying, calcining below the melting point of sodium sulfate, washing with water for 2-3 times, and drying to obtain the high-dispersion yttrium-doped zirconia nano-particles.
Example 155
1L of 1M sodium sulfate aqueous solution is prepared, and 0.2mol of zirconium nitrate, 0.02mol of yttrium nitrate and 0.2mol of polyacrylic acid are added and dissolved by stirring. Adding 2 liters of ethylene glycol ethyl ether while stirring to obtain a precipitate, drying, calcining below the melting point of sodium sulfate, washing with water for 2-3 times, and drying to obtain the high-dispersion yttrium-doped zirconia nano-particles.
Example 156
1L of 1M sodium sulfate aqueous solution was prepared, and 0.2mol of zirconium nitrate, 0.02mol of yttrium nitrate and 0.2mol of polyacrylic acid were added and dissolved with stirring. Adding 2 liters of ethylene glycol monobutyl ether while stirring to obtain a precipitate, drying, calcining below the melting point of sodium sulfate, washing with water for 2-3 times, and drying to obtain the high-dispersion yttrium-doped zirconia nano-particles.
Example 157
1L of 1M sodium sulfate aqueous solution was prepared, and 0.2mol of zirconium nitrate, 0.02mol of yttrium nitrate and 0.2mol of polyacrylic acid were added and dissolved with stirring. Adding 2 liters of diethylene glycol butyl ether while stirring to obtain a precipitate, drying, calcining below the melting point of sodium sulfate, washing with water for 2-3 times, and drying to obtain the high-dispersion yttrium-doped zirconia nano-particles.
Example 158
1L of 1M sodium sulfate aqueous solution is prepared, and 0.2mol of zirconium nitrate, 0.02mol of yttrium nitrate and 0.2mol of polyacrylic acid are added and dissolved by stirring. Adding 2 liters of dimethylformamide while stirring to obtain a precipitate, drying, calcining below the melting point of sodium sulfate, washing with water for 2-3 times, and drying to obtain the high-dispersion yttrium-doped zirconia nano-particles.
Example 159
1L of 1M sodium sulfate aqueous solution is prepared, and 0.2mol of zirconium nitrate, 0.02mol of yttrium nitrate and 0.2mol of polyacrylic acid are added and dissolved by stirring. Adding 2 liters of dimethyl sulfoxide while stirring to obtain a precipitate, drying, calcining below the melting point of sodium sulfate, washing with water for 2-3 times, and drying to obtain the high-dispersion yttrium-doped zirconia nano-particles.
Example 160
1L of 1M potassium carbonate aqueous solution is prepared, and 0.2mol of zirconium acetate and 0.02mol of yttrium acetate are added and dissolved with stirring. Adding 2 liters of dimethyl sulfoxide while stirring to obtain a precipitate, drying, calcining below the melting point of potassium carbonate, washing with water for 2-3 times, and drying to obtain the high-dispersion yttrium-doped zirconia nano-particles.
Example 161
1L of 1M sodium chloride aqueous solution is prepared, 0.2mol of zirconium acetate, 0.02mol of yttrium acetate and 0.2mol of polyacrylic acid are added and stirred for dissolution. Adding 2 liters of ethanol while stirring to obtain a precipitate, drying, calcining below the melting point of sodium chloride, washing with water for 2-3 times, and drying to obtain the high-dispersion yttrium-doped zirconia nano-particles.
Example 162
1L of 1M potassium chloride aqueous solution is prepared, and 0.2mol of zirconium acetate, 0.02mol of yttrium acetate and 0.2mol of polyacrylic acid are added and stirred for dissolution. Adding 2 liters of ethanol while stirring to obtain a precipitate, drying, calcining below the melting point of potassium chloride salt, washing with water for 2-3 times, and drying to obtain the high-dispersion yttrium-doped zirconia nano-particles.
Example 163
1L of 1M sodium carbonate aqueous solution is prepared, 0.2mol of zirconium acetate, 0.02mol of yttrium acetate and 0.2mol of polyacrylic acid are added and stirred for dissolution. Adding 2 liters of ethanol while stirring to obtain a precipitate, drying, calcining below the melting point of sodium carbonate salt, washing with water for 2-3 times, and drying to obtain the high-dispersion yttrium-doped zirconia nano-particles.
Example 164
1L of 1M potassium carbonate aqueous solution is prepared, 0.2mol of zirconium acetate, 0.02mol of yttrium acetate and 0.2mol of polyacrylic acid are added and stirred to dissolve. Adding 2 liters of ethanol while stirring to obtain a precipitate, drying, calcining below the melting point of potassium carbonate, washing with water for 2-3 times, and drying to obtain the high-dispersion yttrium-doped zirconia nano-particles.
Example 165
1L of 1M sodium sulfate aqueous solution is prepared, and 0.2mol of zirconium acetate, 0.02mol of yttrium acetate and 0.2mol of polyacrylic acid are added and stirred to dissolve. Adding 2 liters of dimethyl sulfoxide while stirring to obtain a precipitate, drying, calcining below the melting point of sodium sulfate, washing with water for 2-3 times, and drying to obtain the high-dispersion yttrium-doped zirconia nano-particles.
Example 166
1L of 1M sodium sulfate aqueous solution is prepared, and 0.2mol of zirconium acetate, 0.02mol of yttrium acetate and 0.02mol of polyacrylic acid are added and stirred to dissolve. Adding 2 liters of dimethyl sulfoxide while stirring to obtain a precipitate, drying, calcining below the melting point of sodium sulfate, washing with water for 2-3 times, and drying to obtain the high-dispersion yttrium-doped zirconia nano-particles.
Example 167
1L of 1M sodium sulfate aqueous solution is prepared, and 0.2mol of zirconium acetate, 0.02mol of yttrium acetate and 0.1mol of polyacrylic acid are added and stirred to dissolve. Adding 2 liters of dimethyl sulfoxide while stirring to obtain a precipitate, drying, calcining below the melting point of sodium sulfate, washing with water for 2-3 times, and drying to obtain the high-dispersion yttrium-doped zirconia nano-particles.
When only the aqueous solution of the yttrium-zirconium complex is used, the stability is very good without the water-soluble salt described in the above examples, and precipitation does not occur by adding an organic solvent such as ethanol. The addition of the water-soluble salt greatly changes the solubility of the cerium complex, and the cerium complex and the water-soluble salt are precipitated together after the organic solvent is added and are separated and dispersed by the water-soluble salt, which is one of the main reasons that the yttrium-doped zirconia nanoparticles can be efficiently prepared in the above embodiment.
The method for preparing the highly dispersed MLCC nano nickel powder is further described by the specific examples.
Example 168
1L of 0.5M potassium sulfate aqueous solution is prepared, 0.1mol of nickel nitrate and 0.05mol of polyacrylic acid are added, and the mixture is stirred and dissolved. Then adding 1L ethanol to generate precipitation, drying, calcining in the air at a temperature of above 300 ℃ and below the melting point of potassium sulfate, calcining in a reducing atmosphere at a temperature of above 600 ℃ and below the melting point of potassium sulfate, cooling, washing with deionized water for 2-3 times, and drying to obtain the high-dispersion nano nickel powder.
Example 169
1L of 0.5M potassium sulfate aqueous solution is prepared, 0.1mol of nickel sulfate and 0.05mol of polyacrylic acid are added, and the mixture is stirred and dissolved. Then adding 1L ethanol to generate precipitation, drying, calcining in the air at a temperature of above 300 ℃ and below the melting point of potassium sulfate, calcining in a reducing atmosphere at a temperature of above 600 ℃ and below the melting point of potassium sulfate, cooling, washing with deionized water for 2-3 times, and drying to obtain the high-dispersion nano nickel powder.
Example 170
1L of 0.5M potassium sulfate aqueous solution is prepared, 0.1mol of nickel acetate and 0.05mol of polyacrylic acid are added, and the mixture is stirred and dissolved. Then adding 1L ethanol to generate precipitation, drying, calcining in the air at a temperature of above 300 ℃ and below the melting point of potassium sulfate, calcining in a reducing atmosphere at a temperature of above 600 ℃ and below the melting point of potassium sulfate, cooling, washing with deionized water for 2-3 times, and drying to obtain the high-dispersion nano nickel powder.
Example 171
1L of 0.5M potassium sulfate aqueous solution is prepared, 0.1mol of nickel chloride and 0.05mol of polyacrylic acid are added, and the mixture is stirred and dissolved. Then adding 1L ethanol to generate precipitation, drying, calcining in the air at a temperature of above 300 ℃ and below the melting point of potassium sulfate, calcining in a reducing atmosphere at a temperature of above 600 ℃ and below the melting point of potassium sulfate, cooling, washing with deionized water for 2-3 times, and drying to obtain the high-dispersion nano nickel powder.
Example 172
1L of 0.5M potassium sulfate aqueous solution is prepared, and then 0.1mol of nickel nitrate and 0.1mol of ammonia water are added and stirred for dissolution. And then adding 1 liter of ethanol to generate precipitation, drying, calcining at a temperature of above 300 ℃ in the air and below the melting point of potassium sulfate, calcining at a temperature of above 600 ℃ in a reducing atmosphere and below the melting point of potassium sulfate, cooling, washing with deionized water for 2-3 times, and drying to obtain the high-dispersion nano nickel powder.
Example 173
1L of 0.5M potassium sulfate aqueous solution is prepared, 0.1mol of nickel nitrate and 0.1mol of ammonium bicarbonate are added, and the mixture is stirred and dissolved. And then adding 1 liter of ethanol to generate precipitation, drying, calcining at a temperature of above 300 ℃ in the air and below the melting point of potassium sulfate, calcining at a temperature of above 600 ℃ in a reducing atmosphere and below the melting point of potassium sulfate, cooling, washing with deionized water for 2-3 times, and drying to obtain the high-dispersion nano nickel powder.
Example 174
1L of 0.5M potassium sulfate aqueous solution is prepared, and then 0.1mol of nickel nitrate and 0.1mol of ammonium carbonate are added and stirred to dissolve. And then adding 1 liter of ethanol to generate precipitation, drying, calcining at a temperature of above 300 ℃ in the air and below the melting point of potassium sulfate, calcining at a temperature of above 600 ℃ in a reducing atmosphere and below the melting point of potassium sulfate, cooling, washing with deionized water for 2-3 times, and drying to obtain the high-dispersion nano nickel powder.
Example 175
1L of 0.5M potassium sulfate aqueous solution is prepared, 0.1mol of nickel nitrate and 0.1mol of polyacrylic acid are added, and stirring is carried out to dissolve. And then adding 1 liter of ethanol to generate precipitation, drying, calcining at a temperature of above 300 ℃ in the air and below the melting point of potassium sulfate, calcining at a temperature of above 600 ℃ in a reducing atmosphere and below the melting point of potassium sulfate, cooling, washing with deionized water for 2-3 times, and drying to obtain the high-dispersion nano nickel powder.
Example 176
1L of 0.5M potassium sulfate aqueous solution is prepared, 0.1mol of nickel nitrate and 0.1mol of ammonium polyacrylate are added, and stirring is carried out to dissolve. Then adding 1L ethanol to generate precipitation, drying, calcining in the air at a temperature of above 300 ℃ and below the melting point of potassium sulfate, calcining in a reducing atmosphere at a temperature of above 600 ℃ and below the melting point of potassium sulfate, cooling, washing with deionized water for 2-3 times, and drying to obtain the high-dispersion nano nickel powder.
Example 177
1L of 0.5M potassium sulfate aqueous solution is prepared, 0.1mol of nickel nitrate and 0.05mol of sodium polyacrylate are added, and the mixture is stirred and dissolved. And then adding 1 liter of ethanol to generate precipitation, drying, calcining at a temperature of above 300 ℃ in the air and below the melting point of potassium sulfate, calcining at a temperature of above 600 ℃ in a reducing atmosphere and below the melting point of potassium sulfate, cooling, washing with deionized water for 2-3 times, and drying to obtain the high-dispersion nano nickel powder.
Example 178
1L of 0.5M potassium sulfate aqueous solution is prepared, 0.1mol of nickel nitrate and 0.05mol of potassium polyacrylate are added, and the mixture is stirred and dissolved. And then adding 1 liter of ethanol to generate precipitation, drying, calcining at a temperature of above 300 ℃ in the air and below the melting point of potassium sulfate, calcining at a temperature of above 600 ℃ in a reducing atmosphere and below the melting point of potassium sulfate, cooling, washing with deionized water for 2-3 times, and drying to obtain the high-dispersion nano nickel powder.
Example 179
1L of 0.5M potassium sulfate aqueous solution is prepared, 0.1mol of nickel nitrate and 0.1mol of citric acid are added, and the mixture is stirred and dissolved. And then adding 1 liter of ethanol to generate precipitation, drying, calcining at a temperature of above 300 ℃ in the air and below the melting point of potassium sulfate, calcining at a temperature of above 600 ℃ in a reducing atmosphere and below the melting point of potassium sulfate, cooling, washing with deionized water for 2-3 times, and drying to obtain the high-dispersion nano nickel powder.
Example 180
1L of 0.5M potassium sulfate aqueous solution is prepared, 0.1mol of nickel nitrate and 0.1mol of sodium citrate are added, and stirring and dissolving are carried out. Then adding 1L ethanol to generate precipitation, drying, calcining in the air at a temperature of above 300 ℃ and below the melting point of potassium sulfate, calcining in a reducing atmosphere at a temperature of above 600 ℃ and below the melting point of potassium sulfate, cooling, washing with deionized water for 2-3 times, and drying to obtain the high-dispersion nano nickel powder.
Example 181
1L of 0.5M potassium sulfate aqueous solution is prepared, 0.1mol of nickel nitrate and 0.1mol of potassium citrate are added, and stirring is carried out to dissolve the potassium sulfate aqueous solution. Then adding 1L ethanol to generate precipitation, drying, calcining in the air at a temperature of above 300 ℃ and below the melting point of potassium sulfate, calcining in a reducing atmosphere at a temperature of above 600 ℃ and below the melting point of potassium sulfate, cooling, washing with deionized water for 2-3 times, and drying to obtain the high-dispersion nano nickel powder.
Example 182
1L of 0.5M potassium sulfate aqueous solution is prepared, 0.1mol of nickel nitrate and 0.1mol of tartaric acid are added, and the mixture is stirred and dissolved. Then adding 1L ethanol to generate precipitation, drying, calcining in the air at a temperature of above 300 ℃ and below the melting point of potassium sulfate, calcining in a reducing atmosphere at a temperature of above 600 ℃ and below the melting point of potassium sulfate, cooling, washing with deionized water for 2-3 times, and drying to obtain the high-dispersion nano nickel powder.
Example 183
1L of 0.5M potassium sulfate aqueous solution is prepared, and then 0.1mol of nickel nitrate and 0.1mol of sodium tartrate are added and stirred for dissolution. Then adding 1L ethanol to generate precipitation, drying, calcining in the air at a temperature of above 300 ℃ and below the melting point of potassium sulfate, calcining in a reducing atmosphere at a temperature of above 600 ℃ and below the melting point of potassium sulfate, cooling, washing with deionized water for 2-3 times, and drying to obtain the high-dispersion nano nickel powder.
Example 184
1L of 0.5M potassium sulfate aqueous solution is prepared, 0.1mol of nickel nitrate and 0.1mol of potassium tartrate are added, and the mixture is stirred and dissolved. Then adding 1L ethanol to generate precipitation, drying, calcining in the air at a temperature of above 300 ℃ and below the melting point of potassium sulfate, calcining in a reducing atmosphere at a temperature of above 600 ℃ and below the melting point of potassium sulfate, cooling, washing with deionized water for 2-3 times, and drying to obtain the high-dispersion nano nickel powder.
Example 185
1L of 0.5M potassium sulfate aqueous solution is prepared, 0.1mol of nickel nitrate and 0.05mol of ethylene diamine tetraacetic acid are added, and stirring and dissolving are carried out. Then adding 1L ethanol to generate precipitation, drying, calcining in the air at a temperature of above 300 ℃ and below the melting point of potassium sulfate, calcining in a reducing atmosphere at a temperature of above 600 ℃ and below the melting point of potassium sulfate, cooling, washing with deionized water for 2-3 times, and drying to obtain the high-dispersion nano nickel powder.
Example 186
1L of 0.5M potassium sulfate aqueous solution is prepared, 0.1mol of nickel nitrate and 0.05mol of sodium ethylene diamine tetracetate are added, and the mixture is stirred and dissolved. Then adding 1L ethanol to generate precipitation, drying, calcining in the air at a temperature of above 300 ℃ and below the melting point of potassium sulfate, calcining in a reducing atmosphere at a temperature of above 600 ℃ and below the melting point of potassium sulfate, cooling, washing with deionized water for 2-3 times, and drying to obtain the high-dispersion nano nickel powder.
Example 187
1L of 0.5M potassium sulfate aqueous solution is prepared, 0.1mol of nickel nitrate and 0.05mol of potassium ethylene diamine tetraacetate are added, and the mixture is stirred and dissolved. And then adding 1 liter of ethanol to generate precipitation, drying, calcining at a temperature of above 300 ℃ in the air and below the melting point of potassium sulfate, calcining at a temperature of above 600 ℃ in a reducing atmosphere and below the melting point of potassium sulfate, cooling, washing with deionized water for 2-3 times, and drying to obtain the high-dispersion nano nickel powder.
Example 188
1 liter of 0.5M potassium sulfate aqueous solution is prepared, and then 0.1mol of nickel nitrate and 0.1mol of gluconic acid are added and stirred for dissolution. And then adding 1 liter of ethanol to generate precipitation, drying, calcining at a temperature of above 300 ℃ in the air and below the melting point of potassium sulfate, calcining at a temperature of above 600 ℃ in a reducing atmosphere and below the melting point of potassium sulfate, cooling, washing with deionized water for 2-3 times, and drying to obtain the high-dispersion nano nickel powder.
Example 189
1L of 0.5M potassium sulfate aqueous solution is prepared, 0.1mol of nickel nitrate and 0.1mol of sodium gluconate are added, and stirring and dissolving are carried out. Then adding 1L ethanol to generate precipitation, drying, calcining in the air at a temperature of above 300 ℃ and below the melting point of potassium sulfate, calcining in a reducing atmosphere at a temperature of above 600 ℃ and below the melting point of potassium sulfate, cooling, washing with deionized water for 2-3 times, and drying to obtain the high-dispersion nano nickel powder.
Example 190
1L of 0.5M potassium sulfate aqueous solution is prepared, 0.1mol of nickel nitrate and 0.1mol of potassium gluconate are added, and the mixture is stirred and dissolved. And then adding 1 liter of ethanol to generate precipitation, drying, calcining at a temperature of above 300 ℃ in the air and below the melting point of potassium sulfate, calcining at a temperature of above 600 ℃ in a reducing atmosphere and below the melting point of potassium sulfate, cooling, washing with deionized water for 2-3 times, and drying to obtain the high-dispersion nano nickel powder.
Example 191
1L of 1M sodium sulfate aqueous solution is prepared, and then 0.5mol of nickel nitrate and 0.5mol of polyacrylic acid are added and stirred to dissolve. And then adding 2 liters of ethanol to generate a precipitate, drying, calcining at a temperature of above 300 ℃ in the air and below the melting point of sodium sulfate, calcining at a temperature of above 600 ℃ in a reducing atmosphere and below the melting point of sodium sulfate, cooling, washing with deionized water for 2-3 times, and drying to obtain the high-dispersion nano nickel powder.
Example 192
1L of 1M sodium sulfate aqueous solution is prepared, 0.5mol of nickel nitrate and 0.5mol of polyacrylic acid are added, and the mixture is stirred and dissolved. Then adding 2 liters of isopropanol to generate precipitation, drying, calcining at the temperature of more than 300 ℃ in the air and below the melting point of sodium sulfate, calcining at the temperature of more than 600 ℃ in a reducing atmosphere and below the melting point of sodium sulfate, cooling, washing with deionized water for 2-3 times, and drying to obtain the high-dispersion nano nickel powder.
Example 193
1L of 1M sodium sulfate aqueous solution is prepared, and then 0.5mol of nickel nitrate and 0.5mol of polyacrylic acid are added and stirred to dissolve. Then adding 2L of tertiary butanol to generate precipitation, drying, calcining in the air at a temperature of above 300 ℃ and below the melting point of sodium sulfate, calcining in a reducing atmosphere at a temperature of above 600 ℃ and below the melting point of sodium sulfate, cooling, washing with deionized water for 2-3 times, and drying to obtain the high-dispersion nano nickel powder.
Example 194
1L of 1M sodium sulfate aqueous solution is prepared, 0.5mol of nickel nitrate and 0.5mol of polyacrylic acid are added, and the mixture is stirred and dissolved. Then adding 2L of propanol to generate precipitation, drying, calcining in the air at a temperature of above 300 ℃ and below the melting point of sodium sulfate, calcining in a reducing atmosphere at a temperature of above 600 ℃ and below the melting point of sodium sulfate, cooling, washing with deionized water for 2-3 times, and drying to obtain the high-dispersion nano nickel powder.
Example 195
1L of 1M sodium sulfate aqueous solution is prepared, 0.5mol of nickel nitrate and 0.5mol of polyacrylic acid are added, and the mixture is stirred and dissolved. Then 2 liters of ethylene glycol monomethyl ether is added to generate precipitation, the precipitation is calcined in the air at the temperature of more than 300 ℃ and below the melting point of sodium sulfate after being dried, the calcination is carried out at the temperature of more than 600 ℃ and below the melting point of sodium sulfate in a reducing atmosphere, the cooling is carried out, the washing is carried out for 2 to 3 times by deionized water, and the high-dispersion nano nickel powder can be obtained after the drying.
Example 196
1L of 1M sodium sulfate aqueous solution is prepared, and then 0.5mol of nickel nitrate and 0.5mol of polyacrylic acid are added and stirred to dissolve. Then adding 2 liters of ethylene glycol ethyl ether to generate precipitation, calcining at the temperature of more than 300 ℃ in the air and below the melting point of sodium sulfate after drying, calcining at the temperature of more than 600 ℃ in a reducing atmosphere and below the melting point of sodium sulfate, washing for 2-3 times by deionized water after cooling, and drying to obtain the high-dispersion nano nickel powder.
Example 197
1L of 1M sodium sulfate aqueous solution is prepared, and then 0.5mol of nickel nitrate and 0.5mol of polyacrylic acid are added and stirred to dissolve. Then adding 2 liters of diethylene glycol monobutyl ether to generate precipitation, calcining at the temperature of more than 300 ℃ in the air and below the melting point of sodium sulfate after drying, calcining at the temperature of more than 600 ℃ and below the melting point of sodium sulfate in a reducing atmosphere, washing for 2-3 times by deionized water after cooling, and drying to obtain the high-dispersion nano nickel powder.
Example 198
1L of 1M sodium sulfate aqueous solution is prepared, 0.5mol of nickel nitrate and 0.5mol of polyacrylic acid are added, and the mixture is stirred and dissolved. Then adding 2 liters of ethylene glycol monobutyl ether to generate precipitation, calcining at the temperature of more than 300 ℃ in the air and below the melting point of sodium sulfate after drying, calcining at the temperature of more than 600 ℃ and below the melting point of sodium sulfate in a reducing atmosphere, washing for 2-3 times by deionized water after cooling, and drying to obtain the high-dispersion nano nickel powder.
Example 199
1L of 1M sodium sulfate aqueous solution is prepared, 0.5mol of nickel nitrate and 0.5mol of polyacrylic acid are added, and the mixture is stirred and dissolved. Then adding 2L of dimethylformamide to generate precipitation, drying, calcining in the air at a temperature of above 300 ℃ and below the melting point of sodium sulfate, calcining in a reducing atmosphere at a temperature of above 600 ℃ and below the melting point of sodium sulfate, cooling, washing with deionized water for 2-3 times, and drying to obtain the high-dispersion nano nickel powder.
Example 200
1L of 1M sodium sulfate aqueous solution is prepared, 0.5mol of nickel nitrate and 0.5mol of polyacrylic acid are added, and the mixture is stirred and dissolved. Then adding 2 liters of dimethyl sulfoxide to generate precipitation, drying, calcining at the temperature of more than 300 ℃ in the air and below the melting point of sodium sulfate, calcining at the temperature of more than 600 ℃ in a reducing atmosphere and below the melting point of sodium sulfate, cooling, washing with deionized water for 2-3 times, and drying to obtain the high-dispersion nano nickel powder.
Example 201
1L of 1M sodium chloride aqueous solution is prepared, 0.5mol of nickel nitrate and 0.5mol of polyacrylic acid are added, and stirring is carried out to dissolve. Then adding 2 liters of ethanol to generate precipitation, drying, calcining at the temperature of more than 300 ℃ in the air and below the melting point of sodium chloride, calcining at the temperature of more than 600 ℃ in a reducing atmosphere and below the melting point of sodium chloride, cooling, washing with deionized water for 2-3 times, and drying to obtain the high-dispersion nano nickel powder.
Example 202
1L of 1M potassium chloride aqueous solution is prepared, 0.5mol of nickel nitrate and 0.5mol of polyacrylic acid are added, and the mixture is stirred and dissolved. Then adding 2 liters of ethanol to generate precipitation, drying, calcining at the temperature of more than 300 ℃ in the air and below the melting point of potassium chloride salt, calcining at the temperature of more than 600 ℃ in a reducing atmosphere and below the melting point of potassium chloride, cooling, washing with deionized water for 2-3 times, and drying to obtain the high-dispersion nano nickel powder.
Example 203
1L of 1M sodium carbonate aqueous solution is prepared, 0.5mol of nickel nitrate and 0.5mol of polyacrylic acid are added, and stirring is carried out to dissolve. Then adding 2 liters of ethanol to generate precipitation, drying, calcining at the temperature of more than 300 ℃ in the air and below the melting point of sodium carbonate salt, calcining at the temperature of more than 600 ℃ and below the melting point of sodium carbonate in a reducing atmosphere, cooling, washing with deionized water for 2-3 times, and drying to obtain the high-dispersion nano nickel powder.
Example 204
1L of 1M potassium carbonate aqueous solution is prepared, 0.5mol of nickel nitrate and 0.5mol of polyacrylic acid are added, and the mixture is stirred and dissolved. Then adding 2 liters of ethanol to generate precipitation, drying, calcining at the temperature of more than 300 ℃ in the air and below the melting point of potassium carbonate, calcining at the temperature of more than 600 ℃ and below the melting point of potassium carbonate in a reducing atmosphere, cooling, washing with deionized water for 2-3 times, and drying to obtain the high-dispersion nano nickel powder.
Example 205
1L of 1M potassium carbonate aqueous solution is prepared, and then 0.5mol of nickel nitrate is added and dissolved by stirring. Then adding 2 liters of dimethyl sulfoxide to generate precipitation, drying, calcining at the temperature of more than 300 ℃ in the air and below the melting point of potassium carbonate, calcining at the temperature of more than 600 ℃ in a reducing atmosphere and below the melting point of potassium carbonate, cooling, washing with deionized water for 2-3 times, and drying to obtain the high-dispersion nano nickel powder.
Example 206
1L of 0.5M potassium sulfate aqueous solution is prepared, 0.1mol of nickel nitrate and 0.1mol of polyacrylic acid are added, and stirring is carried out to dissolve. Then adding 1L ethanol to generate precipitation, drying, calcining in the air at a temperature of above 300 ℃ and below the melting point of potassium sulfate, calcining in a reducing atmosphere at a temperature of above 600 ℃ and below the melting point of potassium sulfate, cooling, washing with deionized water for 2-3 times, and drying to obtain the high-dispersion nano nickel powder.
Example 207
1L of 0.5M potassium sulfate aqueous solution is prepared, 0.1mol of nickel nitrate and 0.01mol of polyacrylic acid are added, and the mixture is stirred and dissolved. Then adding 1L ethanol to generate precipitation, drying, calcining in the air at a temperature of above 300 ℃ and below the melting point of potassium sulfate, calcining in a reducing atmosphere at a temperature of above 600 ℃ and below the melting point of potassium sulfate, cooling, washing with deionized water for 2-3 times, and drying to obtain the high-dispersion nano nickel powder.
If the aqueous solution of the nickel complex does not contain the water-soluble salts described in the above examples, the stability is high and precipitation does not occur by adding an organic solvent. However, when water-soluble salt is dissolved in the nickel complex aqueous solution, the dissolution property of the nickel complex can be obviously changed, and the nickel complex can be precipitated together with the water-soluble salt and separated by the dispersion of the water-soluble salt, which is one of the key factors for effectively preparing the high-dispersion nano nickel powder.
The above examples are only preferred embodiments of the present invention, it should be noted that: it will be apparent to those skilled in the art that various modifications and equivalents can be made without departing from the spirit of the invention, and it is intended that all such modifications and equivalents fall within the scope of the invention as defined in the claims.

Claims (7)

1. A method for preparing high-dispersion MLCC nano nickel powder is characterized by comprising the following steps:
(1) Adding nickel salt, a complexing agent and water-soluble salt into water to obtain a mixed solution of the water-soluble salt and a nickel complex;
(2) Adding an organic solvent to the mixed solution of the water-soluble salt and the nickel complex to lower the solubility of the water-soluble salt and the nickel complex, thereby obtaining a precipitate. In this precipitate, a water-soluble salt separates and disperses the nickel complex;
(3) Drying the precipitate obtained in the step 2), and calcining the precipitate at a temperature higher than the decomposition temperature of the nickel complex and lower than the melting point of the water-soluble salt to obtain a calcined product. In the calcined product, the nickel complex is converted into nickel oxide, namely a state that water-soluble salt is formed to isolate nickel nano particles;
(4) Reducing the calcined product at a high temperature of more than 600 ℃ and below the melting point of the water-soluble salt to obtain a high-temperature reduced product;
(5) And washing and drying the high-temperature reduction product by using deionized water to obtain the high-dispersion nano nickel powder.
2. The method for preparing highly dispersed MLCC nano nickel powder according to claim 1, wherein the nickel salt is any one of nickel nitrate, nickel sulfate, nickel acetate, nickel chloride.
3. The method for preparing highly dispersed MLCC nano nickel powder according to claim 1, wherein the water soluble salt is any one of potassium sulfate, sodium sulfate, potassium chloride, sodium chloride, potassium carbonate, and sodium carbonate.
4. The method for preparing the highly dispersed MLCC nano nickel powder according to claim 1, wherein the organic solvent is any one of ethanol, isopropanol, t-butanol, propanol, ethylene glycol methyl ether, ethylene glycol ethyl ether, diethylene glycol butyl ether, ethylene glycol butyl ether, dimethylformamide, dimethylsulfoxide.
5. The method for preparing highly dispersed MLCC nano nickel powder as claimed in claim 1, wherein the complexing agent is any one of ammonia water, ammonium bicarbonate, ammonium carbonate, polyacrylic acid, ammonium polyacrylate, sodium polyacrylate, potassium polyacrylate, citric acid, sodium citrate, potassium citrate, tartaric acid, sodium tartrate, potassium tartrate, ethylenediaminetetraacetic acid, sodium ethylenediaminetetraacetate, potassium ethylenediaminetetraacetate, gluconic acid, sodium gluconate, potassium gluconate.
6. The method for preparing high-dispersion MLCC nano nickel powder according to claim 1, wherein the molar ratio of the water-soluble salt to the nickel salt is not less than 1.
7. The method for preparing the highly dispersed MLCC nano nickel powder as claimed in claim 1, wherein the molar ratio of the complexing agent to the nickel salt is 0.1 to 1.
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