CN106312079A - Preparation method of high-brightness nano-scale flakey aluminum powder - Google Patents
Preparation method of high-brightness nano-scale flakey aluminum powder Download PDFInfo
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- CN106312079A CN106312079A CN201510350922.XA CN201510350922A CN106312079A CN 106312079 A CN106312079 A CN 106312079A CN 201510350922 A CN201510350922 A CN 201510350922A CN 106312079 A CN106312079 A CN 106312079A
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Abstract
The invention discloses a preparation method of high-brightness nano-scale flakey aluminum powder, which comprises the following steps: firstly, heating aluminum rods under vacuum to evaporate the aluminum rods on a soluble film substrate to form a nano-scale aluminum film; dissolving the soluble film substrate with a solvent to separate the nano-scale aluminum film from the soluble film substrate, and carrying out stirring and centrifugal separation to obtain nano-scale flakey aluminum powder; and conducting drying and surface modification on the nano-scale flakey aluminum powder to obtain the high-brightness nano-scale flakey aluminum powder. The preparation method adopts a continuous production process; the preparation time is about one hour; the thickness of the prepared high-brightness nano-scale flakey aluminum powder can be precisely controlled; the thicknesses of all points on a powder flake are substantially uniform; the surface of the aluminum powder is flat and smooth; the thickness ranges from 30 to 100 nm; the diameter ranges from 0.1 to 3 [mu]m; the radius-thickness ratio ranges from 30 to 900; the brightness is higher than 120Gs; the light reflectivity is higher than 91%; and the water surface covering power is higher than 12m<2>/g.
Description
Technical field
The present invention relates to metal material field, particularly to the preparation method of a kind of high brightness nano-grade aluminum powder.
Background technology
Flake aluminum is also referred to as aluminum argentum powder, has that good dispersion, adhesive force is strong, color and luster is true to nature exactly likes that silver, luminous reflectance be effective and the feature such as light durable, be widely used in decorating, decorate, pack, color printing, automobile, the field such as motorcycle.Considering in terms of the brightness of flake aluminum, metal sense, flash effect, directional migration and water surface covering force etc., the thickness of flake aluminum preferably controls 30～50nm.This thickness is nano level flake aluminum, and owing to there is bulk effect (i.e. small-size effect) and skin effect so that its water surface covering force is high, dispersibility is fine, adds metallic luster and the flash effect of its uniqueness, and application prospect is the most wide.
At present, atomization-ball-milling technology is all used to produce flake aluminum both at home and abroad, the most first aluminium ingot is added heat fusing, sprays, cool down, obtaining granularity is the spherical of 15～50 μm or class ball aluminum powder, then by aluminium powder classification, recycling the spherical or class ball aluminum powder after multistage ball milling makes classification and become the aluminium powder that thickness is 0.1～0.8 μm, the technique such as the most classified, chemical mechanical polishing prepares flake aluminum.But using this technique to produce flake aluminum and have the disadvantage that one is in mechanical milling process, along with the reduction of aluminum powder particle size, aluminium powder surface easily aoxidizes and dimmed even turns black；Two is due to the restriction of aluminium powder classification technique, and traditional ball-milling method is difficult to prepare the powder sheet that thickness is less；Three is that the aluminium powder thickness distribution that this technique is made is uneven, and powder surface irregularity causes powder surface and edge scattering of light and diffuse-reflectance, has a strong impact on the brightness of powder, color and luster and metal sense；Four is that the water surface covering force of the aluminium powder that this technique is made is relatively low, is usually no more than 1.4m2/ g, unit printing, coating area powder consumption are bigger；Five is complex manufacturing, and the production cycle is long, and the most only ball-milling technology process is accomplished by through 4～6 grades of ball millings, and Ball-milling Time is up to more than 45 hours.
Summary of the invention
It is an object of the invention to the shortcoming overcoming prior art to exist, it is provided that a kind of method using film transition method to prepare the high brightness nano-grade aluminum powder that brightness is high, thickness is thin, water surface covering force is big.
The purpose of the present invention is achieved through the following technical solutions:
The method of preparing high brightness nano-grade aluminum powder using film transition method of the present invention, comprises the steps:
(1) heating aluminium bar produces aluminum steam and is deposited in soluble film substrate under vacuum, forms nanometer aluminum film；
(2) dissolve described soluble film substrate with solvent, make described nanometer aluminum film peel off with soluble film substrate, obtain the solidliquid mixture containing aluminum film fragment；
(3) described solidliquid mixture is stirred and separates, obtain nano-grade aluminum powder；
(4) described nano-grade aluminum powder is dried and surface modification treatment, obtains high brightness nano-grade aluminum powder.
In step (1), it it is deposition nanometer aluminum film in the soluble film substrate of movement.
In step (1), described aluminium bar can be selected for aluminum content be 99.7～99.9%, impurity content less than 0.3% thin aluminium bar.
In step (1), described soluble film substrate is collodion membranes.The preparation method of described collodion membranes is: dilutes collodion with ethyl acetate or n-amyl acetate, is then immersed in collodion weak solution by flexible, porous substrate, further take out airing, obtain uniform collodion membranes.Described ethyl acetate or n-amyl acetate are chemical pure ethyl acetate or the n-amyl acetates that content is more than 98.5% (mass percent)；Described collodion is the nitrocellulose content analytical pure collodion more than 5% (mass percent).
In step (2), described solvent can be ethyl acetate or n-amyl acetate.
In step (3), described solidliquid mixture is stirred and separation includes: first with blender by the aluminum film fragment dispersion and fining in described solidliquid mixture, then separate with centrifuge, obtain nano-grade aluminum powder.Also the described nano-grade aluminum powder obtained can be stirred further and separates, the nano-grade aluminum powder obtained by the most under agitation dissolving with solvent, then be centrifuged separating, obtain the purest nano-grade aluminum powder.Described separating step also can repeat repeatedly.
In step (3), described stirring is strength mechanical agitation or ultrasonic agitation.
In step (3), described solvent can be ethyl acetate or n-amyl acetate.
In step (4), described being dried is to use vacuum drier to be dried, and baking temperature is 70～90 DEG C, and drying time is 10～20 minutes.
In step (4), described surface modification treatment is to use hard fatty acids that flake aluminum carries out surface coating modification in drum-type buffing machine, and removes a small amount of dendrite of powder surface.The steel ball of the described built-in φ of drum-type buffing machine 1～3mm.
The present invention compared with prior art has the advantage that and effect:
(1) technique of the present invention is accurately controlled the thickness of flake aluminum, and the thickness of powder sheet surface each point is substantially uniform；
(2) technique of the present invention produces high brightness nano-grade aluminum powder is continuous preparation process, and the production time shortens to about 1 hour；
(3) high brightness nano-grade aluminum powder prepared by technique of the present invention, its surface seldom aoxidizes；
(4) the high brightness nano-grade aluminum powder surfacing prepared by the present invention is smooth, and thickness is 30～100nm, a diameter of 0.1～3 μm, and radius-thickness ratio is 30～900, and luminous reflectance is more than 91%, and brightness is higher than 120Gs, and water surface covering force is more than 12m2/g。
Detailed description of the invention
Below in conjunction with embodiment, the present invention done further detailed description, but embodiments of the present invention are not limited to this.
Embodiment 1
Preparation collodion membranes: nitrocellulose content is more than the analytical pure collodion chemical pure n-amyl acetate dilution of 5%, makes collodion content be down to 2%；Then filter cloth is immersed in collodion weak solution 2 times, collodion membranes after airing, can be formed on filter cloth.
Collodion membranes being put in vacuum coating equipment, evacuation makes the pressure of coating chamber be down to 10-3Pa also makes pressure stability.
The thin aluminium bar that purity is 99.7% is added in aluminum melting pond, forms aluminum steam.
Removing the baffle plate below collodion membranes substrate, make aluminum steam deposit in collodion membranes, coating process continues 5 seconds, obtains the nanometer aluminum film that compact structure, surfacing are smooth.
The collodion membranes having plated nanometer aluminum film is immersed in n-amyl acetate solvent, within about 14 minutes, collodion membranes can be made substantially to dissolve, obtain being mixed with the solidliquid mixture of aluminum film fragment.
Then with blender, above-mentioned solidliquid mixture is carried out dispersion and fining, then separate with centrifuge, obtain the flake aluminum primary product of nanometer grade thickness.
Chip level aluminium powder primary product are purified, to remove the collodion membranes of aluminium powder remained on surface, will the flake aluminum primary product of above-mentioned nanometer grade thickness put in blender, add n-amyl acetate, being then turned on blender, low rate mixing 10 minutes, to dissolve the collodion membranes adhered on aluminium powder further, and be centrifuged separating to the solidliquid mixture obtained, it is thus achieved that pure nano-grade aluminum powder.
Using vacuum drier to be dried nano-grade aluminum powder, vacuum about 600mmHg, baking temperature is 85 DEG C, and drying time is 14 minutes.Then dried nano-grade aluminum powder is added in drum-type buffing machine (steel ball of built-in φ 1～3mm), use hard fatty acids that nano-grade aluminum powder is carried out surface coating modification and polishing, remove a small amount of dendrite of powder surface, obtain high brightness nano-grade aluminum powder.
The characteristic of the high brightness nano-grade aluminum powder that the present embodiment prepares is: powder thickness is substantially uniform, average thickness 35nm, and powder sheet surfacing is smooth, a diameter of 0.13～0.7 μm, radius-thickness ratio is 30～160, aluminum content 99.7%, and water surface covering force is 14m2/ g, luminous reflectance is 92%, brightness 134Gs.
Embodiment 2
By the nitrocellulose content analytical pure collodion chemical pure diluted ethyl acetate more than 5%, collodion content is made to be down to 2%.Filter cloth is immersed in collodion weak solution 2 times, collodion membrane after airing, can be formed on filter cloth.Collodion membrane is placed in drying baker drying.
Collodion membrane is put in vacuum coating equipment, then evacuation, make the pressure of coating chamber be down to 10-3Pa is the most stable.
The thin aluminium bar that purity is 99.9% is added in aluminum melting pond, forms aluminum steam；
Removing the baffle plate below collodion membranes, aluminum steam can be deposited with in collodion membranes.The plated film time continues 7 seconds.
The collodion membrane having plated aluminum film is immersed in ethyl acetate solvent, within about 5 minutes, collodion membrane can be made substantially to dissolve.
To by aluminum film fragment and the solidliquid mixture of solution composition, use blender that aluminum film is pulverized further.
To the solidliquid mixture after refinement, use centrifuge to separate, obtain the flake aluminum primary product of nanometer grade thickness.
Putting in blender by the flake aluminum primary product of nanometer grade thickness, add ethyl acetate, be then turned on blender, low rate mixing 6 minutes, to dissolve the collodion membrane of aluminium powder remained on surface further.Solidliquid mixture carries out a centrifugation again.
Use vacuum drier that the flake aluminum of nanometer grade thickness is dried.Vacuum about 600 mmHg, temperature about 85 DEG C, 14 minutes drying times.
To dried nano-grade aluminum powder be added in drum-type buffing machine, and use hard fatty acids that nano-grade aluminum powder carries out surface coating modification and polishing, remove a small amount of dendrite of powder surface.The steel ball of the built-in φ of buffing machine 1～3mm.
The characteristic of gained high brightness nano-grade aluminum powder is: powder thickness is substantially uniform, average thickness 45nm, and powder sheet surfacing is smooth, a diameter of 0.16～0.8 μm, and radius-thickness ratio is 20～150, aluminum content 99.9%, and water surface covering force is 12m2/ g, luminous reflectance is 95%, brightness 148Gs.
Embodiment 3
Preparation collodion membranes: nitrocellulose content is more than the analytical pure collodion chemical pure n-amyl acetate dilution of 5%, makes collodion content be down to 1.5%；Then filter cloth is immersed in collodion weak solution 3 times, collodion membranes after airing, can be formed on filter cloth.
Collodion membranes being put in vacuum coating equipment, evacuation makes the pressure of coating chamber be down to 10-3Pa also stabilizes it.
The thin aluminium bar that purity is not less than 99.7% adds in aluminum melting pond, forms aluminum steam.
Removing the baffle plate below collodion membranes, aluminum steam can be deposited with in collodion membranes, and coating process continues 5 seconds, obtains the nanometer aluminum film that compact structure, surfacing are smooth.
The collodion membranes having plated nanometer aluminum film is immersed in n-amyl acetate solvent, within about 14 minutes, collodion membranes can be made substantially to dissolve, obtain being mixed with the solidliquid mixture of aluminum film fragment.
Then with blender, above-mentioned solidliquid mixture is carried out dispersion and fining, then separate with centrifuge, obtain the flake aluminum primary product of nanometer grade thickness.
Chip level aluminium powder primary product are purified, to remove the collodion membranes of aluminium powder remained on surface, will the flake aluminum primary product of above-mentioned nanometer grade thickness put in blender, add n-amyl acetate, being then turned on blender, low rate mixing 10 minutes, to dissolve the collodion membranes adhered on aluminium powder further, and be centrifuged separating to the solidliquid mixture obtained, obtain pure nano-grade aluminum powder.
Using vacuum drier to be dried nano-grade aluminum powder, vacuum about 700mmHg, baking temperature is 80 DEG C, and drying time is 10 minutes.Then dried nano-grade aluminum powder is added in drum-type buffing machine (steel ball of built-in φ 1～3mm), use hard fatty acids that nano-grade aluminum powder is carried out surface coating modification and polishing, remove a small amount of dendrite of powder surface, obtain high brightness nano-grade aluminum powder.
The characteristic of the high brightness nano-grade aluminum powder that the present embodiment prepares is: powder thickness is substantially uniform, average thickness 35nm, and powder sheet surfacing is smooth, a diameter of 0.13～0.7 μm, radius-thickness ratio is 30～160, aluminum content 99.7%, and water surface covering force is 15m2/ g, luminous reflectance is 93%, brightness 143Gs.
Embodiment 4
By the nitrocellulose content analytical pure collodion chemical pure diluted ethyl acetate more than 5%, collodion content is made to be down to 1.5%.Filter cloth is immersed in collodion weak solution 3 times, collodion membrane after airing, can be formed on filter cloth.Collodion membrane is placed in drying baker drying.
Collodion membrane is put in vacuum coating equipment, then evacuation, make the pressure of coating chamber be down to 10-3Pa is the most stable.
The thin aluminium bar that purity is 99.9% is added in aluminum melting pond, to form aluminum steam.
Removing the baffle plate below collodion membranes, aluminum steam can be deposited with in collodion membranes.The plated film time is 7 seconds.
The collodion membrane having plated aluminum film is immersed in ethyl acetate solvent, within about 5 minutes, collodion membrane can be made substantially to dissolve.
To by aluminum film fragment and the solidliquid mixture of solution composition, use blender that aluminum film fragment is pulverized further.
To the solidliquid mixture after refinement, use centrifuge to separate, obtain the flake aluminum primary product of nanometer grade thickness.
Putting in blender by the flake aluminum primary product of nanometer grade thickness, add ethyl acetate, be then turned on blender, low rate mixing 6 minutes, to dissolve the collodion membranes of aluminium powder remained on surface further.Solidliquid mixture carries out a centrifugation again.
Use vacuum drier that the flake aluminum of nanometer grade thickness is dried.Vacuum about 700mmHg, temperature about 80 DEG C, 10 minutes drying times.
To dried nano-grade aluminum powder be added in drum-type buffing machine, and use hard fatty acids that nano-grade aluminum powder carries out surface coating modification and polishing, remove a small amount of dendrite of powder surface.The steel ball of the built-in φ of buffing machine 1～3mm.
The characteristic of gained high brightness nano-grade aluminum powder is: powder thickness is substantially uniform, average thickness 45nm, and powder sheet surfacing is smooth, a diameter of 0.16～0.8 μm, and radius-thickness ratio is 20～150, aluminum content 99.9%, and water surface covering force is 12m2/ g, luminous reflectance is 91%, brightness 125Gs.
Claims (9)
1. the preparation method of a high brightness nano-grade aluminum powder, it is characterised in that comprise the steps: that (1) is heated aluminium bar under vacuum and produced aluminum steam and be deposited in soluble film substrate, form nanometer aluminum film；(2) dissolve described soluble film substrate with solvent, make described nanometer aluminum film peel off with soluble film substrate, obtain the solidliquid mixture containing aluminum film fragment；(3) described solidliquid mixture is stirred and separates, obtain nano-grade aluminum powder；(4) described nano-grade aluminum powder is dried and surface modification treatment, obtains high brightness nano-grade aluminum powder.
The method of preparing high brightness nano-grade aluminum powder using film transition method the most according to claim 1, it is characterised in that: in step 1, described soluble film substrate is collodion membranes.
The method of preparing high brightness nano-grade aluminum powder using film transition method the most according to claim 2, it is characterised in that: the preparation method of described collodion membranes is dilute by ethyl acetate or n-amyl acetate
Release collodion, then flexible, porous substrate is immersed in collodion weak solution, further take out airing, obtain uniform collodion membranes.
The method of preparing high brightness nano-grade aluminum powder using film transition method the most according to claim 1, it is characterised in that: in step 2, described solvent is ethyl acetate or n-amyl acetate.
The method of preparing high brightness nano-grade aluminum powder using film transition method the most according to claim 1, it is characterized in that: in step 3, described solidliquid mixture is stirred and separates include first with blender by the aluminum film fragment dispersion and fining in described solidliquid mixture, separate with centrifuge again, obtain nano-grade aluminum powder.
The method of preparing high brightness nano-grade aluminum powder using film transition method the most according to claim 5, it is characterised in that: described nano-grade aluminum powder stirred further and separates, the most under agitation using
Nano-grade aluminum powder obtained by solvent dissolving, then be centrifuged separating, obtain the nano-grade aluminum powder of more clean surface；Described further stirring and separating step are repeated more than once.
The method of preparing high brightness nano-grade aluminum powder using film transition method the most according to claim 6, it is characterised in that: described solvent is ethyl acetate or n-amyl acetate.
The method of preparing high brightness nano-grade aluminum powder using film transition method the most according to claim 1, it is characterised in that: in step 4, described being dried is to use vacuum drier to be dried, and baking temperature is 70～90 DEG C, and drying time is 10～20 minutes.
The method of preparing high brightness nano-grade aluminum powder using film transition method the most according to claim 1, it is characterized in that: in step 4, described surface modification treatment is to use hard fatty acids that flake aluminum carries out surface coating modification in drum-type buffing machine, and removes a small amount of dendrite of powder surface.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106623901A (en) * | 2016-12-19 | 2017-05-10 | 北京化工大学 | Aluminum nanosheet and preparation method and application thereof |
| CN108971508A (en) * | 2018-07-24 | 2018-12-11 | 安徽澳雅合金有限公司 | A kind of method controlling nanometer aluminium powder pattern and partial size and its chemical additives used |
| CN115945692A (en) * | 2023-03-14 | 2023-04-11 | 长春黄金研究院有限公司 | Preparation method of water-soluble solid gold colloid |
-
2015
- 2015-06-24 CN CN201510350922.XA patent/CN106312079A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106623901A (en) * | 2016-12-19 | 2017-05-10 | 北京化工大学 | Aluminum nanosheet and preparation method and application thereof |
| CN108971508A (en) * | 2018-07-24 | 2018-12-11 | 安徽澳雅合金有限公司 | A kind of method controlling nanometer aluminium powder pattern and partial size and its chemical additives used |
| CN115945692A (en) * | 2023-03-14 | 2023-04-11 | 长春黄金研究院有限公司 | Preparation method of water-soluble solid gold colloid |
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