CN101302040A - A method for preparing nano nickel oxide particles with controllable particle size - Google Patents

Abstract

The invention discloses a method for preparing nanometer nickel oxide particles with controllable particle size, belonging to the technical field of inorganic materials. The method comprises the following steps: 1) According to octylphenol polyoxyethylene ether: n-hexanol: cyclohexane: nickel chloride=3:2:5:1-3 and octylphenol polyoxyethylene ether: n-hexanol: cyclohexane : ammonia water=3: 2: 5: 1-3 weight ratio, prepare nickel chloride microemulsion and ammonia water microemulsion respectively; 2) get the same volume of nickel chloride microemulsion and ammonia water microemulsion, mix under strong stirring, The nickel chloride and ammonia water are fully reacted, statically aged, and the nickel hydroxide precipitate in the lower layer is obtained; 3) the nickel hydroxide precipitate is centrifuged, washed and dried to a constant weight, and then roasted at a high temperature to obtain nano-nickel oxide particles. The particle size prepared by the method is controllable, evenly distributed and regular in shape, which fully meets the practical application requirements of the nano-nickel oxide. It also has the advantages of simple device and easy operation.

Description

A method for preparing nano nickel oxide particles with controllable particle size

1. Technical field

The invention belongs to the technical field of inorganic materials, and in particular relates to a method for preparing nano nickel oxide particles with controllable particle size.

2. Background technology

Nickel oxide is a widely used inorganic material. In nature, nickel oxide has a hexagonal structure and exists in the form of green ore. Like other inorganic nanomaterials, nano-nickel oxide particles have many excellent properties and are widely used in heat-sensitive components, glass, functional ceramics, catalysts, coatings, gas-sensitive components, electronic components, etc. In practical applications, there are strict requirements on the particle size and shape of nano-nickel oxide particles, that is, the particle size should be controlled within a certain range, and the distribution should be uniform, and the particle shape should be regular. At present, there are many methods for preparing nano-nickel oxide particles, such as solid-phase method, gas-phase method and liquid-phase precipitation method. Most of them use the liquid phase precipitation method, but the nano-nickel oxide particles prepared by this method are not only irregular in shape, but also difficult to control in particle size, uneven in distribution, and have a certain degree of agglomeration.

The use of microemulsions to prepare nanoparticles is an effective method developed at the end of the last century. This method prepares nanoparticles through an inverse microemulsion composed of oil phase, co-surfactant, surfactant and water phase. The inverse microemulsion is a thermodynamically stable system. The water nucleus in the microemulsion is essentially a microreactor. The size of the water nucleus can be controlled by selecting a suitable microemulsion system, and the surfactant interface layer has a certain strength, so that Control the size of the microreactor to achieve the purpose of controlling the particle size, distribution and shape of nanoparticles. At the same time, the surfactant coating also solves the problem of nanoparticle agglomeration. However, the method of preparing nano-nickel oxide particles with controllable particle size by inverse microemulsion has not been reported yet.

3. Contents of the invention

The object of the present invention is to provide a method for preparing nano-nickel oxide particles with controllable particle size. The nano-nickel oxide particles prepared by the method have controllable particle size, uniform distribution and regular shape.

The method of the present invention is the microemulsion of nickel chloride microemulsion and ammonia water mixed by oil phase cyclohexane, co-surfactant n-hexanol, surfactant octylphenol polyoxyethylene ether, aqueous phase nickel chloride or ammonia solution. emulsion to prepare nano-nickel oxide particles. Specific steps are as follows:

1) According to octylphenol ethoxylate: n-hexanol: cyclohexane: nickel chloride = 3: 2: 5: 1-3 and octylphenol ethoxylate: n-hexanol: cyclohexane: ammonia water = 3 : 2: 5: 1-3 weight ratio, respectively prepare nickel chloride microemulsion and ammonia water microemulsion;

2) Take the same volume of nickel chloride microemulsion and ammonia water microemulsion, mix under strong stirring, make the nickel chloride and ammonia water in the microemulsion fully react, static aging, get the upper layer of green clear liquid and the lower layer of light green hydrogen nickel oxide precipitation;

3) After centrifuging, washing and drying the nickel hydroxide precipitate to a constant weight, the nano-nickel oxide particles are obtained by roasting at a high temperature.

The stirring time in step 2) is 1 hour.

The centrifugal separation in step 3) is carried out with a centrifuge, the rotating speed is 4000 rpm; the drying temperature is 80°C. ; The calcination temperature is 450° C., and the calcination time is 1 hour.

The method of the present invention uses the inverse microemulsion system composed of nickel chloride or ammonia water, cyclohexane, n-hexanol, and octylphenol polyoxyethylene ether as a nanoreactor, and the precipitation reaction occurs through the nickel chloride and ammonia water in the nanoreactor , to prepare high-quality nano-scale nickel oxide particles. The prepared particles have controllable particle size, uniform distribution and regular shape. The characteristics are as follows: Structural phase: cubic structure nickel oxide, no impurity phase; particle size: 11-28nm; particle shape: approximately spherical, fully meeting the requirements of nano-nickel oxide in practical applications. It also has the advantages of simple device and easy operation.

4. Specific implementation

Example 1:

1) According to octylphenol ethoxylate: n-hexanol: cyclohexane: nickel chloride = 3: 2: 5: 1 and octylphenol ethoxylate: n-hexanol: cyclohexane: ammonia water = 3: 2 :5:1 weight ratio, respectively prepare nickel chloride microemulsion and ammonia water microemulsion, wherein the concentrations of nickel chloride and ammonia water are respectively: 0.1mol/L and 0.2mol/L.

2) Take the same volume of nickel chloride microemulsion and ammonia water microemulsion, mix under strong stirring, the stirring time is 1 hour, make the nickel chloride and ammonia water in the microemulsion fully react, static aging, get the upper layer of green clear liquid and the lower layer of light green nickel hydroxide precipitate;

3) Separate the above-mentioned nickel hydroxide precipitate with a centrifuge at a speed of 4000 rpm, wash with ethanol, dry at a temperature of 80°C to constant weight, and roast at a high temperature of 450°C for 1 hour to obtain nano-nickel oxide particles .

It has been measured that its constituent phase is a single nickel oxide phase with an average particle size of 11nm.

Example 2:

1) According to octylphenol ethoxylate: n-hexanol: cyclohexane: nickel chloride = 3: 2: 5: 2 and octylphenol ethoxylate: n-hexanol: cyclohexane: ammonia water = 3: 2 :5:2 weight ratio, respectively prepare nickel chloride microemulsion and ammonia water microemulsion, wherein the concentrations of nickel chloride and ammonia water are respectively: 0.1mol/L and 0.2mol/L.

Step 2), 3) are identical with embodiment 1.

It is measured that its constituent phase is a single nickel oxide phase with an average particle size of 20nm.

Example 3:

1) According to octylphenol ethoxylate: n-hexanol: cyclohexane: nickel chloride = 3: 2: 5: 3 and octylphenol ethoxylate: n-hexanol: cyclohexane: ammonia water = 3: 2 : 5: 3 weight ratio, respectively prepare nickel chloride microemulsion and ammonia water microemulsion, wherein the concentrations of nickel chloride and ammonia water are respectively: 0.1mol/L and 0.2mol/L.

Step 2), 3) are identical with embodiment 1.

It is measured that its constituent phase is a single nickel oxide phase with an average particle size of 28nm.

Claims (5)

1, a kind of method for preparing particle diameter-controllable nano-nickel oxide particle is characterized in that: comprise the steps:

1) according to polyoxyethylene octylphenol ether: n-hexyl alcohol: hexanaphthene: nickelous chloride=3: 2: 5: 1-3 and polyoxyethylene octylphenol ether: n-hexyl alcohol: hexanaphthene: the weight ratio of ammoniacal liquor=3: 2: 5: 1-3, prepare nickelous chloride microemulsion and ammonia microemulsion respectively;

2) get nickelous chloride microemulsion and ammonia microemulsion, under violent stirring, mix, nickelous chloride and ammoniacal liquor are fully reacted with volume, static ageing, lower floor's nickel hydroxide precipitate;

3) with after above-mentioned nickel hydroxide precipitate centrifugation, washing and be dried to constant weight, promptly get nano nickel oxide particles through high-temperature roasting.

2, a kind of method for preparing particle diameter-controllable nano-nickel oxide particle according to claim 1 is characterized in that: step 2) in churning time be 1 hour.

3, a kind of method for preparing particle diameter-controllable nano-nickel oxide particle according to claim 1 and 2 is characterized in that: centrifugation adopts whizzer to carry out in the step 3), and rotating speed is 4000 rev/mins.

4, a kind of method for preparing particle diameter-controllable nano-nickel oxide particle according to claim 1 and 2, it is characterized in that: drying temperature is 80 ℃ in the step 3).

5, a kind of method for preparing particle diameter-controllable nano-nickel oxide particle according to claim 1 and 2, it is characterized in that: maturing temperature is 450 ℃ in the step 3), roasting time is 1 hour.