CN107225254A - A kind of aluminum nanoparticles and preparation method thereof - Google Patents
A kind of aluminum nanoparticles and preparation method thereof Download PDFInfo
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- CN107225254A CN107225254A CN201710214405.9A CN201710214405A CN107225254A CN 107225254 A CN107225254 A CN 107225254A CN 201710214405 A CN201710214405 A CN 201710214405A CN 107225254 A CN107225254 A CN 107225254A
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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
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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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
A kind of aluminum nanoparticles and preparation method thereof, belong to inorganic advanced technical field of nano material.Aluminum nanoparticles, its a diameter of 15~1000 nanometers.Preparation method：Silicon source is added in the organic reaction liquid of ammonium salt, rising temperature for dissolving；Lithium aluminium hydride reduction is added in above-mentioned solution, then obtained mixture is reacted 1~72 hour at a temperature of 100 DEG C~165 DEG C, aluminum nanoparticles suspension is obtained；Separation of solid and liquid is carried out, gained solid is the aluminum nanoparticles.The preparation method of aluminum nanoparticles, using simple and effective solvent-thermal method, makes the aluminum nanoparticles of preparation, granule content is high, and impurity is few.
Description
Technical field
The invention belongs to inorganic advanced technical field of nano material, and in particular to a kind of aluminum nanoparticles and its preparation side
Method.
Background technology
Aluminum nanoparticles refer to that crystallite dimension is nano level ultra-fine aluminum.Compared with traditional energetic material, aluminium is received
Rice corpuscles due to energy density is big, oxygen demand is low and high reactivity and it is unique as propellant and explosive wastewater formula
One of composition.Nano aluminum strengthens shock wave with that can also improve burning velocity after other metal oxide nano-material self assemblies,
It is expected targeted drug being transported to cancer cell, while not damage healthy cells.In addition, the preparation of noble metal nano particles in recent years
It is more ripe with application, but be due to that noble metal cost is higher, the large-scale application of metal nano material is constrained, is compared
Under aluminium as content highest metal in the earth's crust, it is low with cost, be easy to get to the advantages of, be good metal nano material,
It is expected to realize large-scale application.
Material and the continuous improvement of making level with present solar cell, the minority carrier life time of solar cell
It is continuously increased, from the point of view of present business solar cell, in order to which the cost for reducing solar cell improves efficiency, manufacturer also exists
Silicon wafer thickness is constantly reduced to reduce the prices of raw materials, therefore in order to improve the efficiency of battery, it is necessary to consider reduction battery back of the body table
The recombination velocity in face, improves long wave spectral response, so the quality of Al-BSF is special by the output for directly influencing solar cell
Property, particle size is smaller, and aluminium paste contacts better with silicon chip, and alumina particles are smaller in addition, and fusing point is lower, is more easy at a certain temperature
With silica-base material formation sial composite bed, be more conducive to the formation of Al-BSF and improve the output characteristics of solar cell, therefore
Preparing formation of the nano level alumina particles to solar battery aluminum backboard and back surface field has important meaning.
The synthetic method for the metallic aluminium nano material being most widely used at present has mechanical attrition method, gas evaporation sedimentation
With chemical synthesis in liquid phase method.Mechanical attrition method is advantageously implemented volume production, but is easily introduced impurity, and grain shape lack of homogeneity；Gas
Phase condensation method products obtained therefrom purity is high, but equipment requirement is high, and product pattern is difficult to control；Conventional chemical synthesis in liquid phase method,
Possibility is provided for Morphological control, but it reacts too rapid in preparation process, and product particle size is difficult to control.
The content of the invention
To solve the above problems, the present invention proposes a kind of pure aluminum nanoparticles and preparation method thereof.
First aspect present invention provides a kind of pure aluminum nanoparticles, its a diameter of 15~1000 nanometers, further for
The metallic aluminium of face-centered cubic (fcc) crystal formation.
Second aspect of the present invention provides the preparation method of aluminum nanoparticles described above, comprises the following steps：
(1) organic solution of ammonium salt is prepared：Ammonium salt is added in organic solution, the organic reaction containing ammonium salt is configured to
Liquid；
(2) aluminium salt is introduced：Silicon source is added in the organic reaction liquid of above-mentioned ammonium salt, heating makes it fully dissolve；
(3) reducing agent is introduced：Lithium aluminium hydride reduction is added in above-mentioned solution, then by obtained mixture 100 DEG C~
Reacted 1~72 hour at a temperature of 165 DEG C, obtain aluminum nanoparticles suspension；
(4) separation of solid and liquid is carried out to above-mentioned aluminum nanoparticles suspension, gained solid is the aluminum nanoparticles.
In preferred embodiments, step (1) described ammonium salt is aniline, methylphenylamine, triphenylamine, oleyl amine, 18
One of amine and hexadecyldimethyl benzyl ammonium tertiary amine；The one kind or many of described organic reagent in toluene, mesitylene, butyl ether
Kind, using preceding need carry out water removal deoxygenation handle.
In preferred embodiments, the silicon source described in step (2) be one of aluminium chloride, aluminium acetylacetonate, aluminum acetate or
Their mixtures.
In preferred embodiments, step (1) (2) (3) is carried out or carried out under an inert atmosphere in glove box.
In preferred embodiments, the separation of solid and liquid described in step (4) comprises the following steps：First centrifugal concentrating, surpass again
Sound wash, be finally dried in vacuo, wherein used in supersound washing process cleaning solution be acetone, methanol, ether in one kind or
Several mixtures.
In preferred embodiments, the mol ratio of ammonium salt and aluminium element is 1：(0.1~3), aluminium element is silicon source and gone back
Total aluminium element in former agent lithium aluminium hydride reduction.
In preferred embodiments, when using aluminium chloride as source of aluminium, the concentration of the aluminium chloride for (1~
10) mol ratio of mol/L, aluminium chloride and lithium aluminium hydride reduction is 1：(2~5)；When using aluminium acetylacetonate or aluminum acetate as described
During silicon source, the concentration of the aluminium acetylacetonate or aluminum acetate is (0.1~10) mol/L, aluminium acetylacetonate or aluminum acetate and hydrogenation
The mol ratio of aluminium lithium is 1：(2~5).
In preferred embodiments, as increase connect in organic amine on nitrogen side chain number come aluminium nanometer obtained by reducing
The size of particle；Or, when using same ammonium salt, gained aluminium nanometer is reduced as improving it with the mol ratio of silicon source
The size of grain.
The present invention achieves following beneficial effect：
1st, the aluminum nanoparticles in the present invention yet there are no open report, and its diameter can be as small as 15nm.
2nd, aluminum nanoparticles prepared by preparation method of the invention, its particle size Independent adjustable, wherein particle size can
To obtain the aluminum nanoparticles of different-grain diameter by changing the species and corresponding concentration of ammonium salt.According to the change of ammonium salt species
Different with corresponding concentration, the size of aluminum nanoparticles can reach 15nm.
3rd, relative to aluminium nano material prior art preparation method, the preparation method of aluminum nanoparticles of the invention,
Using simple and effective solvent-thermal method, make the aluminum nanoparticles of preparation, granule content is high, and impurity is few.
Brief description of the drawings
A figures are SEM (SEM) figures of aluminum nanoparticles prepared by embodiment 1 in Fig. 1, wherein aluminium nanometer
The diameter of grain is about (900 ± 50) nm.
B figures are SEM (SEM) figures of aluminum nanoparticles prepared by embodiment 2 in Fig. 1, wherein aluminium nanometer
The diameter of grain is about (400 ± 20) nm.
C figures are SEM (SEM) figures of aluminum nanoparticles prepared by embodiment 3 in Fig. 1, wherein aluminium nanometer
The diameter of grain is about (60 ± 10) nm.
D figures are SEM (SEM) figures of aluminum nanoparticles prepared by embodiment 4 in Fig. 1, wherein aluminium nanometer
The diameter of grain is about (20 ± 5) nm.
E figures are SEM (SEM) figures of aluminum nanoparticles prepared by embodiment 5 in Fig. 1, wherein aluminium nanometer
The diameter of grain is about (15 ± 5) nm.
F figures are SEM (SEM) figures of aluminum nanoparticles prepared by embodiment 6 in Fig. 1, wherein aluminium nanometer
The diameter of grain is about (25 ± 5) nm.
A figures are more scattered aluminum nanoparticles SEM (SEM) figures prepared by embodiment 7 in Fig. 2.Fig. 2
Middle b figures are its partial enlargement pictures, it can be seen that nano particle favorable dispersibility, particle diameter is about (50 ± 5)
nm。
C figures are more scattered aluminum nanoparticles SEM (SEM) figures prepared by embodiment 8 in Fig. 2.Fig. 2
Middle d figures are its partial enlargement pictures, it can be seen that nano particle favorable dispersibility, particle diameter is about (80 ± 5)
nm。
Fig. 3 is X-ray powder diffraction (XRD) figure of aluminum nanoparticles prepared by the embodiment of the present invention 4.Therefrom can be clear and definite
Know, material of the present invention is the metallic aluminium of face-centered cubic (fcc) crystal formation.And have no other impurities peak, it is sufficient to illustrate to be closed
There is higher purity into sample.
Fig. 4 is x-ray photoelectron power spectrum (XPS) figure that aluminum nanoparticles prepared by the embodiment of the present invention 4 are measured, X-ray
XPS Analysis analysis is the significant surfaces analytical technology for confirming material surface chemical composition and its element chemistry state.Figure
4 can clearly find out the relative scale of aluminium and its oxide, and aluminum oxide is almost invisible, and degree of oxidation is weak.
Fig. 5 is SEM (SEM) figure of aluminum nanoparticles prepared by embodiment 9；
Fig. 6 is SEM (SEM) figure of aluminum nanoparticles prepared by embodiment 10；
Fig. 7 is SEM (SEM) figure of aluminum nanoparticles prepared by embodiment 11；
Embodiment
The present invention will be described in further detail with reference to the accompanying drawings and examples, it should be appreciated that implements in detail below
What example was merely exemplary, and it is nonrestrictive.
Embodiment 1
0.10ml aniline is added in the toluene after 20ml water removal deoxygenations, uniform, formation mixed solution is thoroughly mixed,
It is placed in 50ml flasks.Then 0.13g aluminum chloride powders are added in mixed solution, is warming up to 80 DEG C, is sufficiently stirred for so that chlorine
Change aluminium to be completely dissolved, then add 0.075g lithium aluminium hydride reduction powder in the flask, being stirred vigorously makes it be sufficiently mixed with solution.
Flask is placed in oil bath pan into 120 DEG C to react 4 hours, then takes out and is placed in natural cooling in air.By the solution after cooling
Pour into centrifuge tube and centrifuge 20min under 8000rpm, remove supernatant.Then the suspension after 15mL acetone dispersion concentrations is used,
Ultrasonic 5min, 8000rpm centrifuge washing；Repeat three times.Vacuum drying, starvation preserves stand-by.Accompanying drawing 1a is this reality
Apply the SEM figures of the aluminum nanoparticles of example preparation.Experimental result is：Diameter is about (900 ± 50) nm.
Embodiment 2
0.37ml aniline is added in the toluene after 20ml water removal deoxygenations, uniform, formation mixed solution is thoroughly mixed,
It is placed in 50ml flasks.Then 0.32g acetylacetone,2,4-pentanediones aluminium powder is added in mixed solution, is warming up to 80 DEG C, is sufficiently stirred for making
Obtain aluminium chloride to be completely dissolved, then add 0.075g lithium aluminium hydride reduction powder in the flask, being stirred vigorously makes it abundant with solution
Mixing.Flask is placed in oil bath pan into 120 DEG C to react 4 hours, then takes out and is placed in natural cooling in air.After cooling
Solution pours into centrifuge tube and centrifuges 20min under 8000rpm, removes supernatant.Then with outstanding after 15mL acetone dispersion concentrations
Float, ultrasonic 5min, 8000rpm centrifuge washings；Repeat three times.Vacuum drying, starvation preserves stand-by.Accompanying drawing 1b is
The SEM figures of aluminum nanoparticles manufactured in the present embodiment.Experimental result is：Diameter is about (400 ± 20) nm.
Embodiment 3
1ml methylphenylamines are added in the toluene after 20ml water removal deoxygenations, uniform, formation mixing is thoroughly mixed
Solution, is placed in 50ml flasks.Then 0.63g aluminum chloride powders are added in mixed solution, is warming up to 80 DEG C, is sufficiently stirred for making
Obtain aluminium chloride to be completely dissolved, then add 0.57g lithium aluminium hydride reduction powder in the flask, being stirred vigorously makes it fully be mixed with solution
Close.Flask is placed in oil bath pan into 120 DEG C to react 4 hours, then takes out and is placed in natural cooling in air.Will be molten after cooling
Liquid pours into centrifuge tube and centrifuges 20min under 8000rpm, removes supernatant.Then the suspension after 15mL acetone dispersion concentrations is used
Thing, ultrasonic 5min, 8000rpm centrifuge washings；Repeat three times.Vacuum drying, starvation preserves stand-by.Accompanying drawing 1c is this
The SEM figures of aluminum nanoparticles prepared by embodiment.Experimental result is：Diameter is about (60 ± 10) nm.
Embodiment 4
1.23g triphenylamines are added in the trimethylbenzene after 20ml water removal deoxygenations, stirring makes it fully dissolve, and formation contains ammonium
The solution of salt, is placed in 50ml flasks.Then 2.0g acetic acid aluminium powders are added in the solution, is warming up to 80 DEG C, is sufficiently stirred for
So that aluminium chloride is completely dissolved, then 1.52g lithium aluminium hydride reduction powder is added in the flask, being stirred vigorously makes it abundant with solution
Mixing.Flask is placed in oil bath pan into 165 DEG C to react 4 hours, then takes out and is placed in natural cooling in air.After cooling
Solution pours into centrifuge tube and centrifuges 20min under 8000rpm, removes supernatant.Then with outstanding after 15mL acetone dispersion concentrations
Float, ultrasonic 5min, 8000rpm centrifuge washings；Repeat three times.Vacuum drying, starvation preserves stand-by.Accompanying drawing 1d is
The SEM figures of aluminum nanoparticles manufactured in the present embodiment.Experimental result is：Diameter is about (20 ± 5) nm.
Embodiment 5
1.3ml oleyl amines are added in the trimethylbenzene after 20ml water removal deoxygenations, is thoroughly mixed uniformly, forms mixing molten
Liquid, is placed in 50ml flasks.Then by 0.13g aluminum chloride powders add mixed solution in, be warming up to 80 DEG C, be sufficiently stirred for so that
Aluminium chloride is completely dissolved, and then adds 0.19g lithium aluminium hydride reduction powder in the flask, and being stirred vigorously makes it fully be mixed with solution
Close.Flask is placed in oil bath pan into 140 DEG C to react 4 hours, then takes out and is placed in natural cooling in air.Will be molten after cooling
Liquid pours into centrifuge tube and centrifuges 20min under 8000rpm, removes supernatant.Then the suspension after 15mL acetone dispersion concentrations is used
Thing, ultrasonic 5min, 8000rpm centrifuge washings；Repeat three times.Vacuum drying, starvation preserves stand-by.Accompanying drawing 1e is this
The SEM figures of aluminum nanoparticles prepared by embodiment.Experimental result is：Diameter is about (15 ± 5) nm.
Embodiment 6
3.4ml octadecylamines are added in the trimethylbenzene after 20ml water removal deoxygenations, is thoroughly mixed uniformly, forms mixing molten
Liquid, is placed in 50ml flasks.Then by 0.65g aluminum chloride powders add mixed solution in, be warming up to 80 DEG C, be sufficiently stirred for so that
Aluminium chloride is completely dissolved, and then adds 0.38g lithium aluminium hydride reduction powder in the flask, and being stirred vigorously makes it fully be mixed with solution
Close.Flask is placed in oil bath pan into 140 DEG C to react 4 hours, then takes out and is placed in natural cooling in air.Will be molten after cooling
Liquid pours into centrifuge tube and centrifuges 20min under 8000rpm, removes supernatant.Then the suspension after 15mL acetone dispersion concentrations is used
Thing, ultrasonic 5min, 8000rpm centrifuge washings；Repeat three times.Vacuum drying, starvation preserves stand-by.Accompanying drawing 1f is this
The SEM figures of aluminum nanoparticles prepared by embodiment.Experimental result is：Diameter is about (25 ± 5) nm.
Embodiment 7
0.07ml hexadecyldimethyl benzyl ammoniums tertiary amine is added in the toluene after 20ml water removal deoxygenations, is thoroughly mixed
It is even, mixed solution is formed, is placed in 50ml flasks.Then 0.26g aluminum chloride powders are added in mixed solution, is warming up to 80
DEG C, it is sufficiently stirred for so that aluminium chloride is completely dissolved, then adding 0.23g lithium aluminium hydride reduction powder in the flask, being stirred vigorously makes
It is sufficiently mixed with solution.Flask is placed in oil bath pan into 120 DEG C to react 4 hours, then take out be placed in it is naturally cold in air
But.Solution after cooling is poured into centrifuge tube and centrifuges 20min under 8000rpm, supernatant is removed.Then with 15mL acetone point
Dissipate the suspension after concentration, ultrasonic 5min, 8000rpm centrifuge washings；Repeat three times.Vacuum drying, starvation is preserved
It is stand-by.Accompanying drawing 2a is the SEM figures of aluminum nanoparticles manufactured in the present embodiment.B figures are its partial enlargement pictures in Fig. 2, from figure
As can be seen that nano particle favorable dispersibility, experimental result is：Diameter is about (50 ± 5) nm.
Embodiment 8
0.33ml oleyl amines are added in the trimethylbenzene after 20ml water removal deoxygenations, is thoroughly mixed uniformly, forms mixing molten
Liquid, is placed in 50ml flasks.Then by 0.26g aluminum chloride powders add mixed solution in, be warming up to 80 DEG C, be sufficiently stirred for so that
Aluminium chloride is completely dissolved, and then adds 0.23g lithium aluminium hydride reduction powder in the flask, and being stirred vigorously makes it fully be mixed with solution
Close.Flask is placed in oil bath pan into 120 DEG C to react 4 hours, then takes out and is placed in natural cooling in air.Will be molten after cooling
Liquid pours into centrifuge tube and centrifuges 20min under 8000rpm, removes supernatant.Then the suspension after 15mL acetone dispersion concentrations is used
Thing, ultrasonic 5min, 8000rpm centrifuge washings；Repeat three times.Vacuum drying, starvation preserves stand-by.Accompanying drawing 2c is this
The SEM figures of aluminum nanoparticles prepared by embodiment.D figures are its partial enlargement pictures in Fig. 2, it can be seen that nanometer
Grain favorable dispersibility, experimental result is：Diameter is about (80 ± 5) nm.
Embodiment 9
0.5ml methylphenylamines are added in the toluene after 20ml water removal deoxygenations, is thoroughly mixed uniformly, forms mixed
Solution is closed, is placed in 50ml flasks.Then 0.63g aluminum chloride powders are added in mixed solution, is warming up to 80 DEG C, is sufficiently stirred for
So that aluminium chloride is completely dissolved, then 0.57g lithium aluminium hydride reduction powder is added in the flask, being stirred vigorously makes it abundant with solution
Mixing.Flask is placed in oil bath pan into 120 DEG C to react 4 hours, then takes out and is placed in natural cooling in air.After cooling
Solution pours into centrifuge tube and centrifuges 20min under 8000rpm, removes supernatant.Then with outstanding after 15mL acetone dispersion concentrations
Float, ultrasonic 5min, 8000rpm centrifuge washings；Repeat three times.Vacuum drying, starvation preserves stand-by.Accompanying drawing 5 is
The SEM figures of aluminum nanoparticles manufactured in the present embodiment.
Embodiment 10
0.49g triphenylamines are added in the trimethylbenzene after 20ml water removal deoxygenations, stirring makes it fully dissolve, and formation contains ammonium
The solution of salt, is placed in 50ml flasks.Then 1.3g aluminum chloride powders are added in the solution, is warming up to 80 DEG C, is sufficiently stirred for
So that aluminium chloride is completely dissolved, then 1.52g lithium aluminium hydride reduction powder is added in the flask, being stirred vigorously makes it abundant with solution
Mixing.Flask is placed in oil bath pan into 165 DEG C to react 4 hours, then takes out and is placed in natural cooling in air.After cooling
Solution pours into centrifuge tube and centrifuges 20min under 8000rpm, removes supernatant.Then with outstanding after 15mL acetone dispersion concentrations
Float, ultrasonic 5min, 8000rpm centrifuge washings；Repeat three times.Vacuum drying, starvation preserves stand-by.Accompanying drawing 6 is
The SEM figures of aluminum nanoparticles manufactured in the present embodiment.
Embodiment 11
0.7ml hexadecyldimethyl benzyl ammoniums tertiary amine is added in the toluene after 20ml water removal deoxygenations, is thoroughly mixed uniformly,
Mixed solution is formed, is placed in 50ml flasks.Then 0.26g aluminum chloride powders are added in mixed solution, is warming up to 80 DEG C, fills
Point stirring cause aluminium chloride be completely dissolved, then 0.23g lithium aluminium hydride reduction powder is added in the flask, be stirred vigorously make its with it is molten
Liquid is sufficiently mixed.Flask is placed in oil bath pan into 120 DEG C to react 4 hours, then takes out and is placed in natural cooling in air.Will be cold
But the solution after pours into centrifuge tube and centrifuges 20min under 8000rpm, removes supernatant.Then 15mL acetone dispersion concentrations are used
Suspension afterwards, ultrasonic 5min, 8000rpm centrifuge washings；Repeat three times.Vacuum drying, starvation preserves stand-by.It is attached
Fig. 7 is the SEM figures of aluminum nanoparticles manufactured in the present embodiment.
Each experimental data shown in the drawings, it is that yardstick is uniform fully to demonstrate the material of the invention synthesized, favorable dispersibility
Metal aluminum nanoparticles, be an important breakthrough of aluminum metallic material preparation field.
Claims (8)
1. a kind of aluminum nanoparticles, it is characterised in that be pure aluminum nanoparticles, its a diameter of 15~1000 nanometers.
2. according to the aluminum nanoparticles described in claim 1, it is characterised in that the metallic aluminium of face-centered cubic (fcc) crystal formation.
3. prepare the method for the aluminum nanoparticles described in claim 1, it is characterised in that comprise the following steps：
(1) organic solution of ammonium salt is prepared：Ammonium salt is added in organic solution, the organic reaction liquid containing ammonium salt is configured to；
(2) aluminium salt is introduced：Silicon source is added in the organic reaction liquid of above-mentioned ammonium salt, heating makes it fully dissolve；
(3) reducing agent is introduced：Lithium aluminium hydride reduction is added in above-mentioned solution, then by obtained mixture at 100 DEG C~165 DEG C
At a temperature of react 1~72 hour, obtain aluminum nanoparticles suspension；
(4) separation of solid and liquid is carried out to above-mentioned aluminum nanoparticles suspension, gained solid is the aluminum nanoparticles.
4. method according to claim 3, it is characterised in that the separation of solid and liquid described in step (4) comprises the following steps：First
Centrifugal concentrating, again supersound washing, are finally dried in vacuo, wherein used in supersound washing process cleaning solution be acetone, ice methanol,
One of ether or their mixture.
5. method according to claim 3, it is characterised in that the silicon source described in step (1) is aluminium chloride, acetylacetone,2,4-pentanedione
One of aluminium, aluminum acetate or their mixtures；The ammonium salt is that the ammonium salt is aniline, methylphenylamine, triphenylamine, oleyl amine, ten
One of eight amine and hexadecyldimethyl benzyl ammonium tertiary amine；The one kind or many of the organic solvent in toluene, mesitylene, butyl ether
Kind.
6. method according to claim 3, it is characterised in that the mol ratio of ammonium salt and aluminium element is 1：(0.1~3), aluminium
Element is aluminium element total in silicon source and reducing agent lithium aluminium hydride reduction.
7. method according to claim 5, it is characterised in that when using aluminium chloride as source of aluminium, the chlorination
The concentration of aluminium is (1~10) mol/L, and the mol ratio of aluminium chloride and lithium aluminium hydride reduction is 1：(2~5)；When using aluminium acetylacetonate or
When aluminum acetate is as source of aluminium, the concentration of the aluminium acetylacetonate or aluminum acetate is (0.1~10) mol/L, aluminium acetylacetonate
Or the mol ratio of aluminum acetate and lithium aluminium hydride reduction is 1：(2~5).
8. method according to claim 3, it is characterised in that by increase connect in organic amine on nitrogen the number of side chain come
The size of reduction gained aluminum nanoparticles；Or, when using same ammonium salt, dropped by improving it with the mol ratio of silicon source
The size of low gained aluminum nanoparticles.
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| CN111069588A (en) * | 2018-10-22 | 2020-04-28 | 吉林大学 | Aluminum nanoparticles and method for preparing same |
| CN111069588B (en) * | 2018-10-22 | 2022-09-13 | 吉林大学 | Aluminum nanoparticles and method for preparing same |
| CN114560485A (en) * | 2022-03-19 | 2022-05-31 | 长沙宁曦新材料有限公司 | Preparation method of superfine alumina |
| CN114560485B (en) * | 2022-03-19 | 2024-03-22 | 长沙宁曦新材料有限公司 | Preparation method of superfine alumina |
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Application publication date: 20171003 |