CN106853538A - A kind of quick method for preparing particle diameter and the copper nano-particle of morphology controllable - Google Patents
A kind of quick method for preparing particle diameter and the copper nano-particle of morphology controllable Download PDFInfo
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- CN106853538A CN106853538A CN201611177283.2A CN201611177283A CN106853538A CN 106853538 A CN106853538 A CN 106853538A CN 201611177283 A CN201611177283 A CN 201611177283A CN 106853538 A CN106853538 A CN 106853538A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
- B22F1/054—Nanosized particles
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
- B22F1/054—Nanosized particles
- B22F1/0553—Complex form nanoparticles, e.g. prism, pyramid, octahedron
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
Abstract
The present invention principally falls into copper nano-particle preparation field, and in particular to a kind of quick method for preparing particle diameter and the copper nano-particle of morphology controllable.Methods described adds aqueous slkali using ethylene glycol as solvent, using ascorbic acid as reducing agent, with mantoquita as raw material, to realize that reduction prepares copper nano-particle in ethylene glycol solution.When aqueous slkali is ammoniacal liquor or sodium hydroxide solution, the particle size of copper nano-particle can be regulated and controled by controlling the addition of aqueous slkali or mantoquita.When aqueous slkali is ammoniacal liquor, the pattern of copper nano-particle can be regulated and controled by controlling the addition of ammoniacal liquor.The present invention is simple to operate, and a step can be completed, and the reaction time is short, it is not necessary to hot conditions, energy-conserving and environment-protective.Simultaneously, it is not necessary to the surfactant and stabilizer of extra addition particle, the copper nano-particle homogeneous grain diameter for preparing.
Description
Technical field
The present invention principally falls into copper nano-particle preparation field, and in particular to a kind of quickly to prepare particle diameter, shape in the solution
The method of the equal controllable of looks and the excellent copper nano-particle of antioxygenic property, without separately adding any surfactant in reaction
And stabilizer, it is not necessary to more than 100 DEG C of high temperature.
Background technology
Metal nanoparticle has the physics different from its reguline metal material due to the particularity of its size and pattern
Chemical property, has obtained extensively in fields such as catalysis material, nano-device, photoelectric material, semi-conducting material and biomedical materials
General application.However, focusing primarily upon the noble metal nano particles such as gold, silver for the study on the synthesis of metal nanoparticle at present
On.Compared to gold, silver nano-particle, copper nano-particle is more active due to property, easily aoxidizes, therefore reaction condition is more severe
Carve, often need to be carried out under high temperature and inert gas shielding more than 100 DEG C, and need to add various surfactants use
To control the pattern and size of nano-particle, building-up process is cumbersome time-consuming.But meanwhile, copper nano-particle have excellent catalysis,
Optics and electrical conduction performance, and copper aboundresources, it is cheap, have more economic advantages compared with gold, silver nano-particle.It is more next
More researchers begin to focus on the research of copper nano-particle.
The content of the invention
For reported it is relevant prepare copper nano-particle research, course of reaction needs high temperature, adds surfactant
And the shortcoming in reaction time more long, a kind of quick side for preparing particle diameter and the copper nano-particle of morphology controllable of present invention offer
Method, without the addition of higher temperature and surfactant, simply, a step is completed operation the method in half an hour, and is made
The pattern and particle diameter controllable of standby copper nano-particle.
The present invention is achieved by the following technical solutions：
A kind of quick method for preparing particle diameter and the copper nano-particle of morphology controllable, methods described using ethylene glycol as solvent, with
Ascorbic acid adds aqueous slkali as reducing agent, with mantoquita as raw material, is received with realizing that reduction prepares copper in ethylene glycol solution
Rice corpuscles.
Further, when aqueous slkali is ammoniacal liquor or sodium hydroxide solution, the particle size of copper nano-particle can pass through
The addition of control aqueous slkali or mantoquita is regulated and controled.
Further, when aqueous slkali is ammoniacal liquor, the pattern of copper nano-particle can be entered by controlling the addition of ammoniacal liquor
Row regulation and control.
Further, the described method comprises the following steps：
（1）Using ethylene glycol as solvent, the ethylene glycol solution of ascorbic acid and the ethylene glycol solution of mantoquita are respectively configured；
（2）Ethylene glycol solution, the ethylene glycol solution of mantoquita, the appropriate aqueous slkali of ascorbic acid are sequentially added in a reservoir, are stirred
Mix and heating response for a period of time；
（3）By step（2）Reacted solution is cooled to room temperature, centrifugation, is washed with deionized, and is disperseed with deionized water, i.e.,
The dispersion liquid of copper nano-particle is obtained, after drying, copper nano-particle powder can be obtained, the copper nano-particle powder has certain particle diameter big
Small and particle morphology.
Further, step（1）In, the concentration of the ethylene glycol solution of the ascorbic acid for preparing is rubbed for 0.04
You/0.22 mol/L is risen to, the concentration of the mantoquita for preparing is 5 mM/ls to 70 mM/ls.
Further, step（1）In, the mantoquita for using is Salzburg vitriol, anhydrous cupric sulfate, acetylacetone copper, chlorine
Change copper or copper nitrate.
Further, step（2）In, the aqueous slkali for using is ammoniacal liquor or sodium hydroxide solution；
When the aqueous slkali use ammoniacal liquor when, control concentration of the ammoniacal liquor in reaction system be 0.05 mol/L to 0.5 mole/
Rise；
When the aqueous slkali use sodium hydroxide solution when, control concentration of the NaOH in reaction system be 0.02 mole/
Rise to 0.25 mol/L.
Further, in step（2）In, the ethylene glycol of the ethylene glycol solution of the ascorbic acid of addition and the mantoquita for adding is molten
Liquid product is equal.
Further, step（2）In, heating response temperature is 65 DEG C to 100 DEG C, time of heating response for 5 minutes extremely
30 minutes.
Further, the particle size range of the copper nano-particle that methods described is prepared is 50-800 nanometers；Methods described
The pattern of the copper nano-particle for preparing can be regulated to the flower-shaped spheroid of rice krispies by irregular cube, and pattern is uniform,
Homogeneous grain diameter.
Advantageous Effects of the invention：
Patent methods described of the present invention replaces the aqueous solution molten as reaction in the building-up process of copper nano-particle from ethylene glycol
Agent, reduces the oxidized possibility of copper nano-particle；From ascorbic acid as reducing agent, compared to conventional sodium borohydride, hydrazine
Class reducing agent, with more preferable bio-compatibility, mitigates environmental pollution burden.
From ammoniacal liquor as pH adjusting agent, the on the one hand reduction of the influence regulation and control ascorbic acid using ammoniacal liquor to system pH
Ability, on the other hand using ammoniacal liquor and the coordination of copper ion, controls the nucleation and growth speed of copper nano-particle.
This reaction method, without extra nitrogen protection, without separately adding any surfactant, only by simply changing
Raw material proportioning i.e. can by the size of copper nano-particle in a big way it is interior regulated and controled, and the pattern of copper nano-particle can also
Regulated and controled from irregular polyhedronses to the flower-shaped ball-type of rice krispies, the nano-particles size for obtaining is homogeneous；And due to being lived without surface
Property agent, therefore washing step is simple, and the yield and purity of product are higher.
Because in copper nano-particle forming process, ascorbic acid molecule and glycol molecule can be adsorbed in copper nano-particle
Surface, plays a part of good stable particle, and by centrifuge washing, the aqueous dispersions of copper nano-particle can be under air-proof condition
Long-time stable is preserved.
In addition, this reaction can be smoothed out when temperature is less than 100 DEG C, the reaction time only needs 5 to 30 minutes, subtracts significantly
The energy consumption of course of reaction is lacked.Whole operation is simple, and repeatability is high.
Compared with the preparation method of the copper nano-particle reported, the present invention has advantage following prominent：Course of reaction without
Need the addition of surfactant；Reaction time is short；Reaction is not required to high temperature；Particle size is controllable（Be, for example, less than 100 nanometers, 100 to
200 nanometers, 200 to 500 nanometers, more than 500 nanometers）；Product morphology can be regulated to the flower-shaped spheroid of rice krispies by irregular cube,
And pattern is uniform, homogeneous grain diameter.
Brief description of the drawings
Fig. 1 is a kind of quick method schematic diagram for preparing particle diameter and the copper nano-particle of morphology controllable；
Reference：1. it is reaction vessel, be 2. reaction raw materials, be 3. polyhedral copper nano-particle, is 4. the flower-shaped ball of rice krispies
Body copper nano-particle.
Specific embodiment
In order to make the purpose , technical scheme and advantage of the present invention be clearer, it is right below in conjunction with drawings and Examples
The present invention is explained in further detail.It should be appreciated that specific implementation described herein is used only for explaining the present invention, not
For limiting the present invention.
Conversely, the present invention covers any replacement done in spirit and scope of the invention being defined by the claims, repaiies
Change, equivalent method and scheme.Further, in order that the public has a better understanding to the present invention, below to of the invention thin
It is detailed to describe some specific detail sections in section description.Part without these details for a person skilled in the art
Description can also completely understand the present invention.
As shown in figure 1, a kind of quick method for preparing particle diameter and the copper nano-particle of morphology controllable, methods described include with
Lower step：
（1）Using ethylene glycol as solvent, the ethylene glycol solution of ascorbic acid and the ethylene glycol solution of mantoquita are respectively configured；Preparation is obtained
The concentration of the ethylene glycol solution of the ascorbic acid for obtaining is 0.04 mol/L to 0.22 mol/L, the copper for preparing
The concentration of salt is 5 mM/ls to 70 mM/ls；The mantoquita for using is Salzburg vitriol, anhydrous cupric sulfate, levulinic
Ketone copper, copper chloride or copper nitrate.
（2）Ethylene glycol solution, the ethylene glycol solution of mantoquita, the appropriate alkali soluble of ascorbic acid are sequentially added in a reservoir
Liquid, stir and heating response for a period of time；The aqueous slkali for using is ammoniacal liquor or sodium hydroxide solution；
When the aqueous slkali use ammoniacal liquor when, control concentration of the ammoniacal liquor in reaction system be 0.05 mol/L to 0.5 mole/
Rise；When the aqueous slkali uses sodium hydroxide solution, it is 0.02 mol/L to control concentration of the NaOH in reaction system
To 0.25 mol/L；
The ethylene glycol solution of the ascorbic acid of addition is equal with the ethylene glycol solution volume of the mantoquita for adding.
Heating response temperature is 65 DEG C to 100 DEG C, and the time of heating response is 5 minutes to 30 minutes.
（3）By step（2）Reacted solution is cooled to room temperature, centrifugation, is washed with deionized, with deionized water point
Dissipate, obtain final product the dispersion liquid of copper nano-particle, the copper nano-particle existed containing energy long-time stable in the dispersion liquid.
Can be to step（3）The dispersion liquid for preparing is dried, and obtains copper nano-particle powder, prepared by methods described
The particle size range of the copper nano-particle of acquisition is 50-800 nanometers.The pattern of the copper nano-particle that methods described is prepared can
The flower-shaped spheroid of rice krispies is regulated to by irregular cube, and pattern is uniform, homogeneous grain diameter.
Embodiment 1
A kind of quick method for preparing particle diameter and the copper nano-particle of morphology controllable, the described method comprises the following steps：
（1）Using ethylene glycol as solvent, the ethylene glycol solution of ascorbic acid and the ethylene glycol solution of mantoquita are respectively configured；Preparation is obtained
The concentration of the ethylene glycol solution of the ascorbic acid for obtaining is 0.22 mol/L, and the mantoquita for selecting in the present embodiment is five water
Copper sulphate is closed, the concentration of the ethylene glycol solution of the Salzburg vitriol for preparing is 0.022 mol/L.
（2）Step is sequentially added in a reservoir（1）The ethylene glycol solution of the ascorbic acid for preparing, the ethylene glycol of mantoquita
Solution, appropriate aqueous slkali, stir and heating response, and heating response temperature is 85 DEG C, and the time of heating response is 30 minutes；
Wherein, the volume phase of the ethylene glycol solution of the ethylene glycol solution of the ascorbic acid of addition and the Salzburg vitriol for adding
Deng being 6 milliliters；
Wherein, the aqueous slkali of addition is the ammonia spirit that mass percent is 2.5%, and addition is 1 milliliter；Now, ammoniacal liquor is anti-
It is 0.102 mol/L to answer the concentration in system.
（3）By step（2）Reacted solution is cooled to room temperature, is centrifuged 5 minutes under conditions of 8000 revs/min, spends
Ion water washing, gained precipitation is disperseed with deionized water, so washing three times, is disperseed with deionized water, obtains final product copper nano-particle
Dispersion liquid, bottling, sealed membrane sealing preserve.
Alternatively, it is also possible to the dispersion liquid of the copper nano-particle is dried, copper nano-particle powder can be obtained, copper nanometer
Particle powder particle diameter is about 200 nanometers, and particle morphology is polyhedron.
Embodiment 2
A kind of quick method for preparing particle diameter and the copper nano-particle of morphology controllable, the described method comprises the following steps：
（1）Using ethylene glycol as solvent, the ethylene glycol solution of ascorbic acid and the ethylene glycol solution of mantoquita are respectively configured；Preparation is obtained
The concentration of the ethylene glycol solution of the ascorbic acid for obtaining is 0.22 mol/L, and the mantoquita for selecting in the present embodiment is five water
Copper sulphate is closed, the concentration of the ethylene glycol solution of the Salzburg vitriol for preparing is 0.03 mol/L.
（2）Step is sequentially added in a reservoir（1）The ethylene glycol solution of the ascorbic acid for preparing, the ethylene glycol of mantoquita
Solution, appropriate aqueous slkali, stirring are placed in carrying out heating response in oil bath, and heating response temperature is 85 DEG C, heating response
Time is 30 minutes；
Wherein, the volume phase of the ethylene glycol solution of the ethylene glycol solution of the ascorbic acid of addition and the Salzburg vitriol for adding
Deng being 6 milliliters；
Wherein, the aqueous slkali of addition is the ammonia spirit that mass percent is 2.5%, and addition is 1 milliliter；Now, ammoniacal liquor is anti-
It is 0.102 mol/L to answer the concentration in system.
（3）By step（2）Reacted solution is cooled to room temperature, is centrifuged 5 minutes under conditions of 8000 revs/min, spends
Ion water washing, gained precipitation is disperseed with deionized water, so washing three times, is disperseed with deionized water, obtains final product copper nano-particle
Dispersion liquid, bottling, sealed membrane sealing preserve.
Alternatively, it is also possible to the dispersion liquid of the copper nano-particle is dried, copper nano-particle powder can be obtained, copper nanometer
Particle powder particle diameter is about 300 nanometers, and particle morphology is polyhedron.
By comparing embodiment 1 and the experimental result of embodiment 2, by regulating and controlling Salzburg vitriol（In mantoquita
It is a kind of）Addition, be capable of the particle size of Effective Regulation copper nano-particle.
Embodiment 3
A kind of quick method for preparing particle diameter and the copper nano-particle of morphology controllable, the described method comprises the following steps：
（1）Using ethylene glycol as solvent, the ethylene glycol solution of ascorbic acid and the ethylene glycol solution of mantoquita are respectively configured；Preparation is obtained
The concentration of the ethylene glycol solution of the ascorbic acid for obtaining is 0.22 mol/L, and the mantoquita for selecting in the present embodiment is five water
Copper sulphate is closed, the concentration of the ethylene glycol solution of the Salzburg vitriol for preparing is 0.03 mol/L.
（2）Step is sequentially added in a reservoir（1）The ethylene glycol solution of the ascorbic acid for preparing, the ethylene glycol of mantoquita
Solution, appropriate aqueous slkali, stir and heating response, and heating response temperature is 85 DEG C, and the time of heating response is 30 minutes；
Wherein, the volume phase of the ethylene glycol solution of the ethylene glycol solution of the ascorbic acid of addition and the Salzburg vitriol for adding
Deng being 6 milliliters；
Wherein, the aqueous slkali of addition is the ammonia spirit that mass percent is 2.5%, and addition is 0.5 milliliter；Now, ammoniacal liquor exists
Concentration in reaction system is 0.053 mol/L.
（3）By step（2）Reacted solution is cooled to room temperature, is centrifuged 5 minutes under conditions of 8000 revs/min, spends
Ion water washing, gained precipitation is disperseed with deionized water, so washing three times, is disperseed with deionized water, obtains final product copper nano-particle
Dispersion liquid, bottling, sealed membrane sealing preserve.
Alternatively, it is also possible to the dispersion liquid of the copper nano-particle is dried, copper nano-particle powder can be obtained, copper nanometer
Particle powder particle diameter is about 600 nanometers, and particle morphology is the flower-shaped spheroid of rice krispies.
By comparing embodiment 2 and the experimental result of embodiment 3, by regulating and controlling the addition of alkali lye, can be effective
Regulate and control the pattern of copper nano-particle.
Embodiment 4
A kind of quick method for preparing particle diameter and the copper nano-particle of morphology controllable, the described method comprises the following steps：
（1）Using ethylene glycol as solvent, the ethylene glycol solution of ascorbic acid and the ethylene glycol solution of mantoquita are respectively configured；Preparation is obtained
The concentration of the ethylene glycol solution of the ascorbic acid for obtaining is 0.11 mol/L, and the mantoquita for selecting in the present embodiment is five water
Copper sulphate is closed, the concentration of the ethylene glycol solution of the Salzburg vitriol for preparing is 0.03 mol/L.
（2）Step is sequentially added in a reservoir（1）The ethylene glycol solution of the ascorbic acid for preparing, the ethylene glycol of mantoquita
Solution, appropriate aqueous slkali, stir and heating response, and heating response temperature is 85 DEG C, and the time of heating response is 30 minutes；
Wherein, the volume phase of the ethylene glycol solution of the ethylene glycol solution of the ascorbic acid of addition and the Salzburg vitriol for adding
Deng being 6 milliliters；
Wherein, the aqueous slkali of addition is the ammonia spirit that mass percent is 2.5%, and addition is 1 milliliter；Now, ammoniacal liquor is anti-
It is 0.102 mol/L to answer the concentration in system.
（3）By step（2）Reacted solution is cooled to room temperature, is centrifuged 5 minutes under conditions of 8000 revs/min, spends
Ion water washing, gained precipitation is disperseed with deionized water, so washing three times, is disperseed with deionized water, obtains final product copper nano-particle
Dispersion liquid, bottling, sealed membrane sealing preserve.
Alternatively, it is also possible to the dispersion liquid of the copper nano-particle is dried, copper nano-particle powder can be obtained, copper nanometer
Particle powder particle diameter is about 300 nanometers, and particle morphology is polyhedron.
By comparing embodiment 2 and embodiment 4, change the addition of the ethylene glycol solution of ascorbic acid, will not be right
Particle diameter and the pattern change of copper nano-particle produce influence.Thus, it is only required to the concentration that control the ethylene glycol solution of bad hematic acid is
In the range of 0.04 mol/L to 0.22 mol/L.
Embodiment 5
A kind of quick method for preparing particle diameter and the copper nano-particle of morphology controllable, the described method comprises the following steps：
（1）Using ethylene glycol as solvent, the ethylene glycol solution of ascorbic acid and the ethylene glycol solution of mantoquita are respectively configured；Preparation is obtained
The concentration of the ethylene glycol solution of the ascorbic acid for obtaining is 0.22 mol/L, and the mantoquita for selecting in the present embodiment is nitric acid
Copper, the concentration of the ethylene glycol solution of the copper nitrate for preparing is 0.022 mol/L.
（2）Step is sequentially added in a reservoir（1）The ethylene glycol solution of the ascorbic acid for preparing, the ethylene glycol of mantoquita
Solution, appropriate aqueous slkali, stir and heating response, and heating response temperature is 85 DEG C, and the time of heating response is 30 minutes；
Wherein, the ethylene glycol solution of the ascorbic acid of addition is equal with the volume of the ethylene glycol solution of the copper nitrate for adding, and is 6
Milliliter；
Wherein, the aqueous slkali of addition is the ammonia spirit that mass percent is 2.5%, and addition is 1 milliliter；Now, ammoniacal liquor is anti-
It is 0.102 mol/L to answer the concentration in system.
（3）By step（2）Reacted solution is cooled to room temperature, is centrifuged 5 minutes under conditions of 8000 revs/min, spends
Ion water washing, gained precipitation is disperseed with deionized water, so washing three times, is disperseed with deionized water, obtains final product copper nano-particle
Dispersion liquid, bottling, sealed membrane sealing preserve.
Alternatively, it is also possible to the dispersion liquid of the copper nano-particle is dried, copper nano-particle powder can be obtained, copper nanometer
Particle powder particle diameter is about 200 nanometers, and particle morphology is polyhedron.
By comparative example 1 and example 5, changing the species of mantoquita can equally be obtained the polyhedron copper of same particle size
Nano-particle.
Embodiment 6
A kind of quick method for preparing particle diameter and the copper nano-particle of morphology controllable, the described method comprises the following steps：
（1）Using ethylene glycol as solvent, the ethylene glycol solution of ascorbic acid and the ethylene glycol solution of mantoquita are respectively configured；Preparation is obtained
The concentration of the ethylene glycol solution of the ascorbic acid for obtaining is 0.22 mol/L, and the mantoquita for selecting in the present embodiment is five water
Copper sulphate is closed, the concentration of the ethylene glycol solution of the Salzburg vitriol for preparing is 0.022 mol/L.
（2）Step is sequentially added in a reservoir（1）The ethylene glycol solution of the ascorbic acid for preparing, the ethylene glycol of mantoquita
Solution, appropriate aqueous slkali, stir and heating response, and heating response temperature is 85 DEG C, and the time of heating response is 30 minutes；
Wherein, the volume phase of the ethylene glycol solution of the ethylene glycol solution of the ascorbic acid of addition and the Salzburg vitriol for adding
Deng being 6 milliliters；
Wherein, the aqueous slkali of addition is the sodium hydroxide solution that concentration is 1.33 mol/Ls, and addition is 0.5 milliliter；Now,
Concentration of the NaOH in reaction system is 0.05 mol/L.
（3）By step（2）Reacted solution is cooled to room temperature, is centrifuged 5 minutes under conditions of 8000 revs/min, spends
Ion water washing, gained precipitation is disperseed with deionized water, so washing three times, is disperseed with deionized water, obtains final product copper nano-particle
Dispersion liquid, bottling, sealed membrane sealing preserve.
Alternatively, it is also possible to the dispersion liquid of the copper nano-particle is dried, copper nano-particle powder can be obtained, copper nanometer
Particle powder particle diameter is about 200 nanometers, and particle morphology is polyhedron.
By comparative example 1 and example 6, the species for changing alkali can also equally be obtained polyhedron copper nano-particle.
Embodiment 7
A kind of quick method for preparing particle diameter and the copper nano-particle of morphology controllable, the described method comprises the following steps：
（1）Using ethylene glycol as solvent, the ethylene glycol solution of ascorbic acid and the ethylene glycol solution of mantoquita are respectively configured；Preparation is obtained
The concentration of the ethylene glycol solution of the ascorbic acid for obtaining is 0.22 mol/L, and the mantoquita for selecting in the present embodiment is five water
Copper sulphate is closed, the concentration of the ethylene glycol solution of the Salzburg vitriol for preparing is 0.03 mol/L.
（2）Step is sequentially added in a reservoir（1）The ethylene glycol solution of the ascorbic acid for preparing, the ethylene glycol of mantoquita
Solution, appropriate aqueous slkali, stir and heating response, and heating response temperature is 90 DEG C, and the time of heating response is 30 minutes；
Wherein, the volume phase of the ethylene glycol solution of the ethylene glycol solution of the ascorbic acid of addition and the Salzburg vitriol for adding
Deng being 6 milliliters；
Wherein, the aqueous slkali of addition is the ammonia spirit that mass percent is 2.5%, and addition is 1 milliliter；Now, ammoniacal liquor is anti-
It is 0.102 mol/L to answer the concentration in system.
（3）By step（2）Reacted solution is cooled to room temperature, is centrifuged 5 minutes under conditions of 8000 revs/min, spends
Ion water washing, gained precipitation is disperseed with deionized water, so washing three times, is disperseed with deionized water, obtains final product copper nano-particle
Dispersion liquid, bottling, sealed membrane sealing preserve.
Alternatively, it is also possible to the dispersion liquid of the copper nano-particle is dried, copper nano-particle powder can be obtained, copper nanometer
Particle powder particle diameter is about 300 nanometers, and particle morphology is polyhedron.
By comparative example 2 and example 7, reaction temperature changes in the range of 65 DEG C -100 DEG C, to copper nano-particle
Pattern and particle diameter do not influence.
Embodiment 8
A kind of quick method for preparing particle diameter and the copper nano-particle of morphology controllable, the described method comprises the following steps：
（1）Using ethylene glycol as solvent, the ethylene glycol solution of ascorbic acid and the ethylene glycol solution of mantoquita are respectively configured；Preparation is obtained
The concentration of the ethylene glycol solution of the ascorbic acid for obtaining is 0.22 mol/L, and the mantoquita for selecting in the present embodiment is five water
Copper sulphate is closed, the concentration of the ethylene glycol solution of the Salzburg vitriol for preparing is 0.03 mol/L.
（2）Step is sequentially added in a reservoir（1）The ethylene glycol solution of the ascorbic acid for preparing, the ethylene glycol of mantoquita
Solution, appropriate aqueous slkali, stir and heating response, and heating response temperature is 85 DEG C, and the time of heating response is 10 minutes；
Wherein, the volume phase of the ethylene glycol solution of the ethylene glycol solution of the ascorbic acid of addition and the Salzburg vitriol for adding
Deng being 6 milliliters；
Wherein, the aqueous slkali of addition is the ammonia spirit that mass percent is 2.5%, and addition is 0.5 milliliter；Now, ammoniacal liquor exists
Concentration in reaction system is 0.053 mol/L.
（3）By step（2）Reacted solution is cooled to room temperature, is centrifuged 5 minutes under conditions of 8000 revs/min, spends
Ion water washing, gained precipitation is disperseed with deionized water, so washing three times, is disperseed with deionized water, obtains final product copper nano-particle
Dispersion liquid, bottling, sealed membrane sealing preserve.
Alternatively, it is also possible to the dispersion liquid of the copper nano-particle is dried, copper nano-particle powder can be obtained, copper nanometer
Particle powder particle diameter is about 600 nanometers, and particle morphology is the flower-shaped spheroid of rice krispies.
By comparative example 3 and example 8, reaction time change in 5-30 minutes, to the pattern of copper nano-particle
And particle diameter does not influence.
Claims (10)
1. a kind of quick method for preparing particle diameter and the copper nano-particle of morphology controllable, it is characterised in that methods described is with second two
Alcohol adds aqueous slkali as solvent, using ascorbic acid as reducing agent, with mantoquita as raw material, to realize in ethylene glycol solution
Middle reduction prepares copper nano-particle.
2. a kind of quick method for preparing particle diameter and the copper nano-particle of morphology controllable according to claim 1, its feature exists
In when aqueous slkali is ammoniacal liquor or sodium hydroxide solution, the particle size of copper nano-particle can be by controlling aqueous slkali or copper
The addition of salt is regulated and controled.
3. a kind of quick method for preparing particle diameter and the copper nano-particle of morphology controllable according to claim 1, its feature exists
In when aqueous slkali is ammoniacal liquor, the pattern of copper nano-particle can be regulated and controled by controlling the addition of ammoniacal liquor.
4. a kind of quick method for preparing particle diameter and the copper nano-particle of morphology controllable according to claim 1, its feature exists
In the described method comprises the following steps：
（1）Using ethylene glycol as solvent, the ethylene glycol solution of ascorbic acid and the ethylene glycol solution of mantoquita are respectively configured；
（2）Ethylene glycol solution, the ethylene glycol solution of mantoquita, the appropriate aqueous slkali of ascorbic acid are sequentially added in a reservoir, are stirred
Mix and heating response for a period of time；
（3）By step（2）Reacted solution is cooled to room temperature, centrifugation, is washed with deionized, and is disperseed with deionized water, i.e.,
The dispersion liquid of copper nano-particle is obtained, after drying, copper nano-particle powder can be obtained, the copper nano-particle powder has certain particle diameter big
Small and particle morphology.
5. a kind of quick method for preparing particle diameter and the copper nano-particle of morphology controllable according to claim 4, its feature exists
In step（1）In, the concentration of the ethylene glycol solution of the ascorbic acid for preparing for 0.04 mol/L to 0.22 mole/
Rise, the concentration of the mantoquita for preparing is 5 mM/ls to 70 mM/ls.
6. a kind of quick method for preparing particle diameter and the copper nano-particle of morphology controllable according to claim 4, its feature exists
In step（1）In, the mantoquita for using is Salzburg vitriol, anhydrous cupric sulfate, acetylacetone copper, copper chloride or copper nitrate.
7. a kind of quick method for preparing particle diameter and the copper nano-particle of morphology controllable according to claim 4, its feature exists
In step（2）In, the aqueous slkali for using is ammoniacal liquor or sodium hydroxide solution；
When the aqueous slkali use ammoniacal liquor when, control concentration of the ammoniacal liquor in reaction system be 0.05 mol/L to 0.5 mole/
Rise；
When the aqueous slkali use sodium hydroxide solution when, control concentration of the NaOH in reaction system be 0.02 mole/
Rise to 0.25 mol/L.
8. a kind of quick method for preparing particle diameter and the copper nano-particle of morphology controllable according to claim 4, its feature exists
In in step（2）In, the ethylene glycol solution of the ascorbic acid of addition is equal with the ethylene glycol solution volume of the mantoquita for adding.
9. a kind of quick method for preparing particle diameter and the copper nano-particle of morphology controllable according to claim 4, its feature exists
In step（2）In, heating response temperature is 65 DEG C to 100 DEG C, and the time of heating response is 5 minutes to 30 minutes.
10. a kind of quick method for preparing particle diameter and the copper nano-particle of morphology controllable according to claim 1, its feature exists
In the particle size range of the copper nano-particle that methods described is prepared is 50-800 nanometers；The copper that methods described is prepared is received
The pattern of rice corpuscles can be regulated to the flower-shaped spheroid of rice krispies by irregular cube, and pattern is uniform, homogeneous grain diameter.
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