CN103192085B - Method for preparing nano aluminum sheet array with catalysis by high purity graphite - Google Patents
Method for preparing nano aluminum sheet array with catalysis by high purity graphite Download PDFInfo
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- CN103192085B CN103192085B CN201310088242.6A CN201310088242A CN103192085B CN 103192085 B CN103192085 B CN 103192085B CN 201310088242 A CN201310088242 A CN 201310088242A CN 103192085 B CN103192085 B CN 103192085B
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Abstract
The invention discloses a method for preparing a nano aluminum sheet array with catalysis by high purity graphite, relates to a method for preparing a nano aluminum sheet array, and solves the technical problems that a product obtained with a conventional method for preparing a nano aluminum sheet and a nano aluminum sheet array is not uniform in size, and the thickness of the product is difficult to control. The method comprises the steps as follows: firstly, an aluminum sheet is placed into a quartz tube for heat preservation; secondly, a mixed liquid is prepared; thirdly, a milky suspending liquid is prepared; fourthly, high purity graphite is placed into the milky suspending liquid obtained from the third step to form a uniform suspending liquid; and fifthly, the suspending liquid obtained from the fourth step is placed into a hydrothermal reaction kettle, the aluminum sheet treated in the first step is placed into the hydrothermal reaction kettle and dried to obtain the nano aluminum sheet array. The method utilizes the reaction activity of the surface of the high purity natural flake graphite under the hydrothermal condition and adds a surface active agent, so that the array structure of the nano aluminum sheet is formed while the nano aluminum sheet is prepared, and the thickness of the nano aluminum sheet can be controlled in a range from20 nanometers to 50 nanometers.
Description
Technical field
The present invention relates to a kind of preparation method of nano aluminum chip arrays.
Background technology
Nanometer aluminium flake is because it has the characteristic of many novelties, as good reflective, anti-hot property, and the good feature such as electric conductivity and ductility, thereby cause scholar's very big interest.The preparation of nanometer aluminium flake and array thereof has given nanometer aluminium flake new characteristic, makes it have more excellent physics and chemistry characteristic, as optics, catalysis and conductance property etc.At present, the preparation method of metal nanometer sheet mainly concentrates on chemical reduction method and electrodeposition process.The advantage of chemical reduction method is easy preparing nano particle, but in course of reaction, needs to add some additives, is difficult to remove totally, affects product quality, is difficult to control the uniformity of product pattern and size, and nanometer sheet thickness is difficult to control.Electrodeposition process be metal salt solution taking metal nano plate to be prepared as electrolyte, adopts electro-deposition techniques that metal nano plate is grown at cathode surface, thereby prepare metal nano plate, but its thickness is still difficult to control.
Summary of the invention
The object of the invention is in order to solve the existing method products obtained therefrom size of preparing nanometer aluminium flake and array thereof inhomogeneously, the unmanageable technical problem of thickness, provides the preparation method of nano aluminum chip arrays under a kind of high purity graphite catalytic condition.
Under high purity graphite catalytic condition, the preparation method of nano aluminum chip arrays carries out according to following steps:
One, aluminium flake is put into quartz ampoule, then by after quartz ampoule vacuum seal, be warmed up to 500 DEG C with the speed of 5～10 DEG C/point, at 500 DEG C of insulation 1h;
Two, get 0.8～1.6ml ammoniacal liquor, 8～16ml absolute ethyl alcohol and 8～12ml distilled water, stir at ambient temperature, mix 30 minutes, regulating pH value is 9, obtains mixed liquor;
Three, 0.1～0.8ml sorbitan monooleate is splashed in step 2 gained mixed liquor, at room temperature stir 1h with the speed of 150～250 revs/min, form uniform cream;
Four, 0.1～0.2g high purity graphite is put into step 3 gained cream, stirred 30 minutes, form uniform suspension.
Five, step 4 gained suspension is inserted in hydrothermal reaction kettle, the addition of suspension is 4/5 of reactor volume;
Six, will put into the hydrothermal reaction kettle of step 5 through the aluminium flake of step 1 processing, sealing is incubated 12～24h under 120～180 DEG C of conditions, and the aluminium flake after washings thermal response to the pH value of washing lotion is 6～8, dry, obtains nano aluminum chip arrays.
Under high purity graphite catalytic condition of the present invention, the preparation method of nano aluminum chip arrays forms weak alkaline aqueous solution by ammoniacal liquor, second alcohol and water, utilize its oxidation-reduction reaction to aluminium flake surface, utilize the reactivity of high-purity natural crystalline flake graphite at hydrothermal condition lower surface, and add surfactant, thereby make to form its array structure (thickness of nanometer aluminium flake can be controlled in 20～50 nanometers) in preparation nanometer aluminium flake.
Under hydrothermal condition, because gas pressure is along with the rising of temperature is increased, the concentration phase strain that is dissolved in the ammoniacal liquor in the aqueous solution is large.Its atom solid matter direction of metallic aluminium that belongs to cubic system is arranged along [111], now, and because the surface film oxide of aluminium flake under alkaline water heat condition is corroded rapidly along this direction.Along with the increase of Hydro-thermal pressure, metal aluminium flake has been accelerated the dissolution velocity of unstable, generates the meta-aluminic acid of aobvious alkalescence.Meanwhile, due to the redox reaction of high purity graphite under hydrothermal condition, generate aobvious acid carbonate compound, thereby accelerated reaction speed.Thereby reach the controlled preparation of nano aluminum chip arrays by controlling ammonia concn, high purity graphite addition, hydrothermal reaction condition etc.
Brief description of the drawings
Fig. 1 is the XRD collection of illustrative plates of testing under a nano aluminum chip arrays different temperatures of preparing, in figure, A represents the XRD collection of illustrative plates of 120 DEG C of nano aluminum chip arrays, C represents the XRD collection of illustrative plates of 140 DEG C of nano aluminum chip arrays, D represents the XRD collection of illustrative plates of 160 DEG C of nano aluminum chip arrays, and E represents the XRD collection of illustrative plates of 180 DEG C of nano aluminum chip arrays;
Fig. 2 is the scanning electron micrograph of the nano aluminum chip arrays of test two preparations.
Detailed description of the invention
Technical solution of the present invention is not limited to following cited detailed description of the invention, also comprises any combination between each detailed description of the invention.
Detailed description of the invention one: in present embodiment, under high purity graphite catalytic condition, the preparation method of nano aluminum chip arrays carries out according to following steps:
One, aluminium flake is put into quartz ampoule, then by after quartz ampoule vacuum seal, be warmed up to 500 DEG C with the speed of 5～10 DEG C/point, at 500 DEG C of insulation 1h;
Two, get 0.8～1.6ml ammoniacal liquor, 8～16ml absolute ethyl alcohol and 8～12ml distilled water, stir at ambient temperature, mix 30 minutes, regulating pH value is 9, obtains mixed liquor;
Three, 0.1～0.8ml sorbitan monooleate is splashed in step 2 gained mixed liquor, at room temperature stir 1h with the speed of 150～250 revs/min, form uniform cream;
Four, 0.1～0.2g high purity graphite is put into step 3 gained cream, stirred 30 minutes, form uniform suspension.
Five, step 4 gained suspension is inserted in hydrothermal reaction kettle, the addition of suspension is 4/5 of reactor volume;
Six, will put into the hydrothermal reaction kettle of step 5 through the aluminium flake of step 1 processing, sealing is incubated 12～24h under 120～180 DEG C of conditions, and the aluminium flake after washings thermal response to the pH value of washing lotion is 6～8, dry, obtains nano aluminum chip arrays.
Detailed description of the invention two: the purity of what present embodiment was different from detailed description of the invention one is aluminium flake described in step 1 is >=99.5%.Other is identical with detailed description of the invention one.
Detailed description of the invention three: what present embodiment was different from one of detailed description of the invention one or two is to be warmed up to 500 DEG C with the speed of 8 DEG C/point in step 1.Other is identical with one of detailed description of the invention one or two.
Detailed description of the invention four: the concentration of what present embodiment was different from one of detailed description of the invention one to three the is amount of substance of ammoniacal liquor in step 2 is 0.05mol/L.Other is identical with one of detailed description of the invention one to three.
Detailed description of the invention five: the mol ratio of what present embodiment was different from one of detailed description of the invention one to four is in step 2 ammoniacal liquor and absolute ethyl alcohol is 1: 10.Other is identical with one of detailed description of the invention one to four.
Detailed description of the invention six: the purity of what present embodiment was different from one of detailed description of the invention one to five is high purity graphite described in step 4 is 99.5%～99.9%, and average grain diameter is 2 μ m～5 μ m.Other is identical with one of detailed description of the invention one to five.
Detailed description of the invention seven: what present embodiment was different from one of detailed description of the invention one to six is to be incubated 15～22h in step 6 under 130～170 DEG C of conditions.Other is identical with one of detailed description of the invention one to six.
Detailed description of the invention eight: what present embodiment was different from one of detailed description of the invention one to seven is to be incubated 18～21h in step 6 under 140～160 DEG C of conditions.Other is identical with one of detailed description of the invention one to seven.
Detailed description of the invention nine: what present embodiment was different from one of detailed description of the invention one to eight is to be incubated 20h in step 6 under 150 DEG C of conditions.Other is identical with one of detailed description of the invention one to eight.
Detailed description of the invention ten: the baking temperature that what present embodiment was different from one of detailed description of the invention one to nine is in step 6 is 60 DEG C.Other is identical with one of detailed description of the invention one to nine.
Adopt following verification experimental verification effect of the present invention:
Test one:
Under high purity graphite catalytic condition, the preparation method of nano aluminum chip arrays carries out according to following steps:
One, aluminium flake is put into quartz ampoule, then by after quartz ampoule vacuum seal, be warmed up to 500 DEG C with the speed of 8 DEG C/point, at 500 DEG C of insulation 1h;
Two, get 0.9ml ammoniacal liquor, 10ml absolute ethyl alcohol and 11ml distilled water, stir at ambient temperature, mix 30 minutes, regulating pH value is 9, obtains mixed liquor;
Three, 0.5ml sorbitan monooleate is splashed in step 2 gained mixed liquor, at room temperature stir 1h with the speed of 200 revs/min, form uniform cream;
Four, 0.1g high purity graphite is put into step 3 gained cream, stirred 30 minutes, form uniform suspension.
Five, step 4 gained suspension is inserted in hydrothermal reaction kettle, the addition of suspension is 4/5 of reactor volume;
Six, will put into the hydrothermal reaction kettle of step 5 through the aluminium flake of step 1 processing, sealing is incubated 12～24h under 130 DEG C of conditions, and the aluminium flake after washings thermal response to the pH value of washing lotion is 6, dry, obtains nano aluminum chip arrays.
As can be seen from Figure 1, nano aluminum chip arrays composition prepared under different temperatures is identical, does not contain other impurity, illustrates that the method can not introduce the second-phase impurity such as meta-aluminate.
Test two:
Under high purity graphite catalytic condition, the preparation method of nano aluminum chip arrays carries out according to following steps:
One, aluminium flake is put into quartz ampoule, then by after quartz ampoule vacuum seal, be warmed up to 500 DEG C with the speed of 8 DEG C/point, at 500 DEG C of insulation 1h;
Two, get 1ml ammoniacal liquor, 12ml absolute ethyl alcohol and 10ml distilled water, stir at ambient temperature, mix 30 minutes, regulating pH value is 9, obtains mixed liquor;
Three, 0.6ml sorbitan monooleate is splashed in step 2 gained mixed liquor, at room temperature stir 1h with the speed of 200 revs/min, form uniform cream;
Four, 0.15g high purity graphite is put into step 3 gained cream, stirred 30 minutes, form uniform suspension.
Five, step 4 gained suspension is inserted in hydrothermal reaction kettle, the addition of suspension is 4/5 of reactor volume;
Six, will put into the hydrothermal reaction kettle of step 5 through the aluminium flake of step 1 processing, sealing is incubated 12～24h under 140 DEG C of conditions, and the aluminium flake after washings thermal response to the pH value of washing lotion is 6, dry, obtains nano aluminum chip arrays.
As can be seen from Figure 2,, at the next nano aluminum chip arrays of preparing even thickness of this temperature, its average thickness is 30nm.
Test three:
Under high purity graphite catalytic condition, the preparation method of nano aluminum chip arrays carries out according to following steps:
One, aluminium flake is put into quartz ampoule, then by after quartz ampoule vacuum seal, be warmed up to 500 DEG C with the speed of 10 DEG C/point, at 500 DEG C of insulation 1h;
Two, get 1.2ml ammoniacal liquor, 14ml absolute ethyl alcohol and 12ml distilled water, stir at ambient temperature, mix 30 minutes, regulating pH value is 9, obtains mixed liquor;
Three, 0.7ml sorbitan monooleate is splashed in step 2 gained mixed liquor, at room temperature stir 1h with the speed of 200 revs/min, form uniform cream;
Four, 0.2g high purity graphite is put into step 3 gained cream, stirred 30 minutes, form uniform suspension.
Five, step 4 gained suspension is inserted in hydrothermal reaction kettle, the addition of suspension is 4/5 of reactor volume;
Six, will put into the hydrothermal reaction kettle of step 5 through the aluminium flake of step 1 processing, sealing is incubated 12～24h under 160 DEG C of conditions, and the aluminium flake after washings thermal response to the pH value of washing lotion is 6, dry, obtains nano aluminum chip arrays.
Claims (10)
1. the preparation method of nano aluminum chip arrays under high purity graphite catalytic condition, is characterized in that the preparation method of nano aluminum chip arrays under high purity graphite catalytic condition carries out according to following steps:
One, aluminium flake is put into quartz ampoule, then by after quartz ampoule vacuum seal, be warmed up to 500 DEG C with the speed of 5～10 DEG C/point, at 500 DEG C of insulation 1h;
Two, get 0.8～1.6ml ammoniacal liquor, 8～16ml absolute ethyl alcohol and 8～12ml distilled water, stir at ambient temperature, mix 30 minutes, regulating pH value is 9, obtains mixed liquor;
Three, 0.1～0.8ml sorbitan monooleate is splashed in step 2 gained mixed liquor, at room temperature stir 1h with the speed of 150～250 revs/min, form uniform cream;
Four, 0.1～0.2g high purity graphite is put into step 3 gained cream, stirred 30 minutes, form uniform suspension;
Five, step 4 gained suspension is inserted in hydrothermal reaction kettle, the addition of suspension is 4/5 of reactor volume;
Six, will put into the hydrothermal reaction kettle of step 5 through the aluminium flake of step 1 processing, sealing is incubated 12～24h under 120～180 DEG C of conditions, and the aluminium flake after washings thermal response to the pH value of washing lotion is 6～8, dry, obtains nano aluminum chip arrays.
2. the preparation method of nano aluminum chip arrays under high purity graphite catalytic condition according to claim 1, the purity that it is characterized in that aluminium flake described in step 1 is >=99.5%.
3. according to the preparation method of nano aluminum chip arrays under high purity graphite catalytic condition described in claim 1 or 2, it is characterized in that being warmed up to 500 DEG C with the speed of 8 DEG C/point in step 1.
4. according to the preparation method of nano aluminum chip arrays under high purity graphite catalytic condition described in claim 1 or 2, the concentration that it is characterized in that the amount of substance of ammoniacal liquor in step 2 is 0.05mol/L.
5. according to the preparation method of nano aluminum chip arrays under high purity graphite catalytic condition described in claim 1 or 2, it is characterized in that in step 2, the mol ratio of ammoniacal liquor and absolute ethyl alcohol is 1: 10.
6. according to the preparation method of nano aluminum chip arrays under high purity graphite catalytic condition described in claim 1 or 2, the purity that it is characterized in that high purity graphite described in step 4 is 99.5%～99.9%, and average grain diameter is 2 μ m～5 μ m.
7. according to the preparation method of nano aluminum chip arrays under high purity graphite catalytic condition described in claim 1 or 2, it is characterized in that under 130～170 DEG C of conditions, being incubated 15～22h in step 6.
8. according to the preparation method of nano aluminum chip arrays under high purity graphite catalytic condition described in claim 1 or 2, it is characterized in that under 140～160 DEG C of conditions, being incubated 18～21h in step 6.
9. according to the preparation method of nano aluminum chip arrays under high purity graphite catalytic condition described in claim 1 or 2, it is characterized in that under 150 DEG C of conditions, being incubated 20h in step 6.
10. according to the preparation method of nano aluminum chip arrays under high purity graphite catalytic condition described in claim 1 or 2, it is characterized in that the baking temperature in step 6 is 60 DEG C.
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Citations (5)
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| JPS5569204A (en) * | 1978-11-14 | 1980-05-24 | Sumitomo Metal Mining Co Ltd | Production of germanium-gallium alloy particle |
| US6325909B1 (en) * | 1999-09-24 | 2001-12-04 | The Governing Council Of The University Of Toronto | Method of growth of branched carbon nanotubes and devices produced from the branched nanotubes |
| CN102142550A (en) * | 2011-02-25 | 2011-08-03 | 浙江大学 | Compound nano material of graphene nano slice and WS2 and preparation method thereof |
| CN102142548A (en) * | 2011-02-25 | 2011-08-03 | 浙江大学 | Compound nano material of graphene and MoS2 and preparation method thereof |
| CN102233433A (en) * | 2010-05-08 | 2011-11-09 | 中国科学院合肥物质科学研究院 | Micron semisphere composed of silver nano-flakes as well as preparation method and use thereof |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5569204A (en) * | 1978-11-14 | 1980-05-24 | Sumitomo Metal Mining Co Ltd | Production of germanium-gallium alloy particle |
| US6325909B1 (en) * | 1999-09-24 | 2001-12-04 | The Governing Council Of The University Of Toronto | Method of growth of branched carbon nanotubes and devices produced from the branched nanotubes |
| CN102233433A (en) * | 2010-05-08 | 2011-11-09 | 中国科学院合肥物质科学研究院 | Micron semisphere composed of silver nano-flakes as well as preparation method and use thereof |
| CN102142550A (en) * | 2011-02-25 | 2011-08-03 | 浙江大学 | Compound nano material of graphene nano slice and WS2 and preparation method thereof |
| CN102142548A (en) * | 2011-02-25 | 2011-08-03 | 浙江大学 | Compound nano material of graphene and MoS2 and preparation method thereof |
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