CN113772704A - Preparation method of two-dimensional alumina powder - Google Patents
Preparation method of two-dimensional alumina powder Download PDFInfo
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- CN113772704A CN113772704A CN202111070015.1A CN202111070015A CN113772704A CN 113772704 A CN113772704 A CN 113772704A CN 202111070015 A CN202111070015 A CN 202111070015A CN 113772704 A CN113772704 A CN 113772704A
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- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 title claims abstract description 117
- 239000000843 powder Substances 0.000 title claims abstract description 72
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- 238000000034 method Methods 0.000 claims abstract description 37
- 239000000758 substrate Substances 0.000 claims abstract description 29
- 238000007664 blowing Methods 0.000 claims abstract description 18
- 238000007598 dipping method Methods 0.000 claims abstract description 16
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 13
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 13
- 238000003837 high-temperature calcination Methods 0.000 claims abstract description 7
- 229920001721 polyimide Polymers 0.000 claims description 22
- 238000001035 drying Methods 0.000 claims description 14
- 238000004140 cleaning Methods 0.000 claims description 12
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 11
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- 238000001354 calcination Methods 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- 229920000139 polyethylene terephthalate Polymers 0.000 claims description 6
- 239000005020 polyethylene terephthalate Substances 0.000 claims description 6
- 238000004519 manufacturing process Methods 0.000 claims description 5
- -1 polyethylene terephthalate Polymers 0.000 claims description 5
- 239000011347 resin Substances 0.000 claims description 4
- 229920005989 resin Polymers 0.000 claims description 4
- 239000002245 particle Substances 0.000 claims description 3
- 238000010345 tape casting Methods 0.000 claims description 3
- MXRIRQGCELJRSN-UHFFFAOYSA-N O.O.O.[Al] Chemical compound O.O.O.[Al] MXRIRQGCELJRSN-UHFFFAOYSA-N 0.000 claims description 2
- DPXJVFZANSGRMM-UHFFFAOYSA-N acetic acid;2,3,4,5,6-pentahydroxyhexanal;sodium Chemical compound [Na].CC(O)=O.OCC(O)C(O)C(O)C(O)C=O DPXJVFZANSGRMM-UHFFFAOYSA-N 0.000 claims description 2
- 239000001768 carboxy methyl cellulose Substances 0.000 claims description 2
- 229920001495 poly(sodium acrylate) polymer Polymers 0.000 claims description 2
- 235000019812 sodium carboxymethyl cellulose Nutrition 0.000 claims description 2
- 229920001027 sodium carboxymethylcellulose Polymers 0.000 claims description 2
- NNMHYFLPFNGQFZ-UHFFFAOYSA-M sodium polyacrylate Chemical compound [Na+].[O-]C(=O)C=C NNMHYFLPFNGQFZ-UHFFFAOYSA-M 0.000 claims description 2
- 239000007787 solid Substances 0.000 claims description 2
- 229910001220 stainless steel Inorganic materials 0.000 claims description 2
- 239000010935 stainless steel Substances 0.000 claims description 2
- 239000010408 film Substances 0.000 description 58
- 239000004642 Polyimide Substances 0.000 description 20
- 229920002799 BoPET Polymers 0.000 description 16
- 239000011248 coating agent Substances 0.000 description 8
- 238000000576 coating method Methods 0.000 description 8
- 230000010355 oscillation Effects 0.000 description 8
- 238000007654 immersion Methods 0.000 description 5
- 230000004048 modification Effects 0.000 description 5
- 238000012986 modification Methods 0.000 description 5
- 238000005054 agglomeration Methods 0.000 description 3
- 230000002776 aggregation Effects 0.000 description 3
- 150000003839 salts Chemical class 0.000 description 3
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 239000000945 filler Substances 0.000 description 2
- 238000001027 hydrothermal synthesis Methods 0.000 description 2
- 238000010297 mechanical methods and process Methods 0.000 description 2
- 238000005498 polishing Methods 0.000 description 2
- 238000005245 sintering Methods 0.000 description 2
- 238000003980 solgel method Methods 0.000 description 2
- 238000012876 topography Methods 0.000 description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 238000007605 air drying Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- 239000002738 chelating agent Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000005536 corrosion prevention Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000003618 dip coating Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000005226 mechanical processes and functions Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 238000010926 purge Methods 0.000 description 1
- 239000011819 refractory material Substances 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
- 239000012745 toughening agent Substances 0.000 description 1
- 239000003440 toxic substance Substances 0.000 description 1
- MYWQGROTKMBNKN-UHFFFAOYSA-N tributoxyalumane Chemical compound [Al+3].CCCC[O-].CCCC[O-].CCCC[O-] MYWQGROTKMBNKN-UHFFFAOYSA-N 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F7/00—Compounds of aluminium
- C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
- C01F7/44—Dehydration of aluminium oxide or hydroxide, i.e. all conversions of one form into another involving a loss of water
- C01F7/441—Dehydration of aluminium oxide or hydroxide, i.e. all conversions of one form into another involving a loss of water by calcination
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/20—Particle morphology extending in two dimensions, e.g. plate-like
Abstract
The invention discloses a preparation method of two-dimensional alumina powder. The transparent aluminum sol is cast to form a film on a flexible substrate by adopting a dipping and pulling method, and the wet film is converted into a hydrated alumina film layer after baking. The hydrated alumina film layer is blown off from the substrate by adopting a pneumatic blowing method and then is broken into hydrated alumina powder. The hydrated alumina powder is converted into two-dimensional alumina powder by high-temperature calcination. The two-dimensional alumina powder prepared by the invention has smooth and flat surface, uniform and controllable thickness, nanoscale and large diameter-thickness ratio.
Description
Technical Field
The invention relates to the technical field of alumina powder, in particular to a preparation method of two-dimensional alumina powder.
Background
The alumina has abundant reserves in nature and low price, has the characteristics of good heat-conducting property, high hardness, high melting point, oxidation resistance, corrosion resistance, high resistivity and the like, and is widely applied to the fields of heat-conducting fillers, polishing powder, toughening agents, refractory materials and the like. The two-dimensional alumina powder with the sheet structure has smooth and flat surface, the thickness is usually in the micron or submicron grade, the radius-thickness ratio is larger, the two-dimensional alumina powder has the excellent performance of common alumina powder, and has the characteristics of strong reflection/shielding capability, easy construction of ordered structures, moderate surface activity and the like, and has great application potential in the fields of heat-conducting fillers, precision polishing, metal corrosion prevention, surface modification and the like.
The common preparation method of the flake alumina comprises the following steps: molten salt processes, sol-gel processes, hydrothermal processes and mechanical processes. The molten salt method is to control the appearance and size of the alumina by controlling molten salt, crystal seeds and additives, the equipment is simple, the production period is short, but the prepared flaky alumina powder is easy to generate mosaic phenomenon, and toxic substances can be discharged or the equipment can be corroded during sintering. The sol-gel method is carried out in solution, the product purity is high, the synthesis temperature is low, but the prepared flaky alumina powder is easy to agglomerate. The flaky alumina powder prepared by the hydrothermal method has high purity, good crystallinity and difficult agglomeration, but has complex process, long production period, harsh reaction conditions and high requirements on equipment. The mechanical method has low cost and easy operation, but the prepared flaky alumina powder has low purity, easy agglomeration, uneven grain diameter and rough surface.
In EP0240952A2(A method for producing a flash material), aluminum tributoxide, butanol and a certain amount of water are mixed to prepare aluminum sol, the aluminum sol is coated on a continuous belt by a roller, a hydrated alumina film layer is obtained by drying, the hydrated alumina film layer is stripped by a scraper, and flaky alumina powder with the particle size of 5-40 μm and the thickness of 1 μm is obtained after high-temperature calcination. The wet film thickness of the patent is larger, and the thickness of the alumina powder is larger. And limited by the limit of processing precision, the hydrated alumina film layer is difficult to be scraped off from the continuous belt by the scraper. The residual hydrated alumina film is superposed with the newly formed hydrated alumina film layer, which will affect the uniformity of the thickness of the flaky alumina powder.
Patent CN108439465A (a method for preparing and loading nano titanium dioxide sol) mixes a titanium source, a solvent, a chelating agent, an acid solution and water to prepare a sol, coats the sol on a substrate, and obtains a titanium dioxide film layer through air drying and sintering. This patent is only concerned with thin film preparation and not with powder preparation.
Disclosure of Invention
Aiming at the problems and the defects of the existing preparation method, the invention aims to provide a novel preparation method of two-dimensional alumina powder.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of two-dimensional alumina powder comprises the following steps: adopting a dipping and pulling method to make the transparent aluminum sol cast on a flexible substrate to form a film, and converting a wet film into a hydrated alumina film layer after baking; the hydrated alumina film layer is blown off from the flexible substrate by adopting a pneumatic blowing method and then is broken into hydrated alumina powder; the hydrated alumina powder is converted into two-dimensional alumina powder by high-temperature calcination.
The method specifically comprises the following steps:
step (1): ultrasonically oscillating and cleaning a flexible substrate in deionized water, drying, ultrasonically oscillating and cleaning in absolute ethyl alcohol, and drying for later use;
step (2): adopting a dipping and pulling method to make the water-soluble resin solution cast into a film on the flexible substrate obtained in the step (1), and drying to obtain a flexible modified substrate;
and (3): adopting a dipping and pulling method to make the transparent aluminum sol form a film on the modified substrate obtained in the step (2) by tape casting, baking and curing to obtain a solid hydrated aluminum oxide film layer;
and (4): blowing off the hydrated alumina film layer obtained in the step (3) from the flexible substrate by using a pneumatic blowing method and breaking the hydrated alumina film layer into two-dimensional hydrated alumina powder;
and (5): and (4) carrying out temperature programming baking on the two-dimensional hydrated alumina powder obtained in the step (4), baking at 200 ℃ to remove most of bound moisture, and then calcining at high temperature to obtain the two-dimensional alumina powder.
Preferably, in the above preparation method, the flexible substrate in step (1) is a Polyimide (PI) film, a heat-resistant polyethylene terephthalate (PET) film, a stainless steel film or an aluminum film.
Preferably, in the above manufacturing method, the flexible substrate is a Polyimide (PI) film or a heat-resistant polyethylene terephthalate (PET) film.
Preferably, in the above preparation method, the water-soluble resin in the step (2) is polyvinyl alcohol, sodium carboxymethylcellulose, or sodium polyacrylate.
Preferably, in the preparation method, the concentration range of the transparent aluminum sol in the step (3) is 0.3-0.5 mol/L, and the diameter range of the colloidal particles is 5-50 nm; the dipping and pulling speed of the transparent alumina sol is 0.3-1.0 mm/s.
Preferably, in the above preparation method, the pneumatic blowing method in step (4) is to blow the hydrated alumina film layer off the flexible substrate by the impact force of compressed air and break the hydrated alumina film layer into hydrated alumina powder.
Preferably, in the above preparation method, the temperature range of the high-temperature calcination in the step (5) is 1100 to 1300 ℃.
Compared with the prior art, the invention has the following beneficial effects:
the invention adopts a dipping and pulling method to form a film on a flexible substrate by tape casting, and utilizes a pneumatic purging method to make a hydrated alumina film layer fall off from the flexible substrate and be broken into hydrated alumina powder. And finally, preparing the two-dimensional alumina powder through high-temperature calcination, wherein the two-dimensional alumina powder has typical two-dimensional characteristics. The invention adopts the combination of the dipping and pulling method and the pneumatic blowing method to prepare the two-dimensional alumina powder, overcomes the defects of larger and uneven thickness, easy agglomeration, rough surface and the like of the common flaky alumina powder, and has the advantages of smooth and flat surface, uniform and controllable thickness, nanoscale diameter-thickness ratio and the like. The two-dimensional alumina powder prepared by the method has smooth and flat surface, uniform and controllable thickness, nanoscale and large diameter-thickness ratio.
Drawings
FIG. 1 is an SEM image of a two-dimensional alumina powder prepared by the present invention.
FIG. 2 is a surface topography of the two-dimensional alumina powder prepared by the present invention.
FIG. 3 is a cross-sectional view of a two-dimensional alumina powder prepared according to the present invention and having a thickness of 300 nm.
Detailed Description
The present invention will be described in detail with reference to specific embodiments.
Example 1:
selecting a PI film as a flexible substrate, modifying the PI film by adopting polyvinyl alcohol PVA (5%), wherein the concentration of transparent alumina sol is 0.39 mol/L, the pulling speed is 0.5 mm/s, and the preparation method comprises the following specific steps:
(1) modification of PI film: and (3) placing the PI film in deionized water for ultrasonic oscillation cleaning for 20 min, drying, and placing in absolute ethyl alcohol for ultrasonic oscillation cleaning for 20 min. Coating a PVA solution with the mass fraction of 5% on a PI film at the pulling speed of 0.5 mm/s by adopting a dipping and pulling machine, and baking for 20 min at the temperature of 100 ℃ to obtain a modified PI film;
(2) preparing a hydrated alumina film layer: coating transparent alumina sol with the concentration of 0.39 mol/L on the modified PI film at the speed of 0.5 mm/s by using an immersion drawing machine, and baking for 10 min at the temperature of 80 ℃ to obtain a hydrated alumina film layer;
(3) preparing two-dimensional alumina powder: and blowing off the hydrated alumina film layer attached to the modified PI film by adopting a pneumatic blowing method, crushing the hydrated alumina film layer into hydrated alumina powder, baking the hydrated alumina powder in a muffle furnace at 200 ℃ for 30 min, and calcining the hydrated alumina powder at 1200 ℃ for 2 h to obtain the two-dimensional alumina powder.
The two-dimensional alumina powder prepared by the method has smooth and flat surface, uniform thickness of about 300 nm and large diameter-thickness ratio. The surface topography and the cross-sectional thickness of the two-dimensional alumina powder are respectively shown in fig. 2 and 3.
Example 2:
selecting a PET film as a flexible substrate, modifying the PET film by adopting polyanionic sodium cellulose PAC (0.5 percent), wherein the concentration of transparent alumina sol is 0.45 mol/L, the dipping and pulling speed is 0.5 mm/s, and the preparation method comprises the following specific steps:
(1) modification of PET film: and (3) placing the PET film in deionized water for ultrasonic oscillation cleaning for 20 min, drying, and placing in absolute ethyl alcohol for ultrasonic oscillation cleaning for 20 min. Coating PAC solution with the mass fraction of 0.5% on a PET film by adopting an immersion drawing machine at the drawing speed of 0.5 mm/s, and baking for 10 min at the temperature of 100 ℃ to obtain a modified PET film;
(2) preparing a hydrated alumina film layer: coating transparent aluminum sol with the concentration of 0.45 mol/L on the modified PET film at the speed of 0.5 mm/s by using an immersion drawing machine, and drying for 10 min at the temperature of 80 ℃ to obtain a hydrated alumina film layer;
(3) preparing two-dimensional alumina powder: and blowing off the hydrated alumina film layer attached to the modified PET film by adopting a pneumatic blowing method, crushing the hydrated alumina film layer into hydrated alumina powder, baking the hydrated alumina powder in a muffle furnace at 200 ℃ for 30 min, and calcining the hydrated alumina powder at 1200 ℃ for 2 h to obtain the two-dimensional alumina powder.
The two-dimensional alumina powder prepared by the method has smooth and flat surface, uniform thickness of about 400 nm and large diameter-thickness ratio.
Example 3:
selecting a PI film as a flexible substrate, modifying the PI film by adopting polyvinyl alcohol PVA (6%), wherein the concentration of transparent alumina sol is 0.39 mol/L, the dip-coating rate is 0.3 mm/s, and the preparation method comprises the following specific steps:
(1) modification of PI film: and (3) placing the PI film in deionized water for ultrasonic oscillation cleaning for 20 min, drying, and placing in absolute ethyl alcohol for ultrasonic oscillation cleaning for 20 min. Coating a PVA solution with the mass fraction of 6% on a PI film at the pulling speed of 0.3 mm/s by adopting a dipping and pulling machine, and baking for 25 min at the temperature of 100 ℃ to obtain a modified PI film;
(2) preparing a hydrated alumina film layer: coating transparent alumina sol with the concentration of 0.39 mol/L on the modified PI film at the speed of 0.3 mm/s by adopting an immersion drawing machine, and drying for 10 min at the temperature of 80 ℃ to obtain a hydrated alumina film layer;
(3) preparing two-dimensional alumina powder: and blowing off the hydrated alumina film layer attached to the modified PI film by adopting a pneumatic blowing method, crushing the hydrated alumina film layer into hydrated alumina powder, baking the hydrated alumina powder in a muffle furnace at 200 ℃ for 30 min, and calcining the hydrated alumina powder at 1200 ℃ for 2 h to obtain the two-dimensional alumina powder.
The two-dimensional alumina powder prepared by the method has smooth and flat surface, uniform thickness of about 800 nm and large diameter-thickness ratio.
Example 4:
selecting a PET film as a flexible substrate, modifying the PET film by adopting polyvinyl alcohol PVA (5%), wherein the concentration of transparent alumina sol is 0.39 mol/L, the dipping and pulling speed is 1.0 mm/s, and the preparation method comprises the following specific steps:
(1) modification of PET film: and (3) placing the PET film in deionized water for ultrasonic oscillation cleaning for 20 min, drying, and placing in absolute ethyl alcohol for ultrasonic oscillation cleaning for 20 min. Coating a PVA solution with the mass fraction of 5% on a PET film by adopting a dipping and drawing machine at the drawing speed of 1.0 mm/s, and drying for 20 min at the temperature of 100 ℃ to obtain a modified PET film;
(2) preparing a hydrated alumina film layer: coating transparent aluminum sol with the concentration of 0.39 mol/L on the modified PET film at the speed of 1.0 mm/s by adopting an immersion drawing machine, and baking for 10 min at the temperature of 80 ℃ to obtain a hydrated alumina film layer;
(3) preparing two-dimensional alumina powder: and blowing off the hydrated alumina film layer attached to the modified PET film by adopting a pneumatic blowing method, crushing the hydrated alumina film layer into hydrated alumina powder, baking the hydrated alumina powder in a muffle furnace at 200 ℃ for 30 min, and calcining the hydrated alumina powder at 1200 ℃ for 2 h to obtain the two-dimensional alumina powder.
The two-dimensional alumina powder prepared by the method has smooth and flat surface, uniform thickness, large diameter-thickness ratio and thickness of about 950 nm.
Claims (8)
1. A preparation method of two-dimensional alumina powder is characterized by comprising the following steps: adopting a dipping and pulling method to make the transparent aluminum sol cast on a flexible substrate to form a film, and converting a wet film into a hydrated alumina film layer after baking; the hydrated alumina film layer is blown off from the flexible substrate by adopting a pneumatic blowing method and then is broken into hydrated alumina powder; the hydrated alumina powder is converted into two-dimensional alumina powder by high-temperature calcination.
2. The method of claim 1, comprising the steps of:
step (1): ultrasonically oscillating and cleaning a flexible substrate in deionized water, drying, ultrasonically oscillating and cleaning in absolute ethyl alcohol, and drying for later use;
step (2): adopting a dipping and pulling method to make the water-soluble resin solution cast into a film on the flexible substrate obtained in the step (1), and drying to obtain a flexible modified substrate;
and (3): adopting a dipping and pulling method to make the transparent aluminum sol form a film on the modified substrate obtained in the step (2) by tape casting, baking and curing to obtain a solid hydrated aluminum oxide film layer;
and (4): blowing off the hydrated alumina film layer obtained in the step (3) from the flexible substrate by using a pneumatic blowing method and breaking the hydrated alumina film layer into two-dimensional hydrated alumina powder;
and (5): and (4) carrying out temperature programming baking on the two-dimensional hydrated alumina powder obtained in the step (4), baking at 200 ℃ to remove most of bound moisture, and then calcining at high temperature to obtain the two-dimensional alumina powder.
3. The method according to claim 1, wherein the flexible substrate of step (1) is a polyimide film, a heat-resistant polyethylene terephthalate film, a stainless steel film or an aluminum film.
4. The production method according to claim 3, wherein the flexible substrate is a polyimide film or a heat-resistant polyethylene terephthalate film.
5. The method according to claim 2, wherein the water-soluble resin in the step (2) is polyvinyl alcohol, sodium carboxymethylcellulose, or sodium polyacrylate.
6. The preparation method according to claim 2, wherein the concentration of the transparent aluminum sol in the step (3) is in the range of 0.3 to 0.5 mol/L, and the diameter of the colloidal particle is in the range of 5 to 50 nm; the dipping and pulling speed of the transparent alumina sol is 0.3-1.0 mm/s.
7. The method according to claim 2, wherein the pneumatic blowing method in the step (4) is to blow the hydrated alumina film layer off the flexible substrate by using the impact force of compressed air and to break the hydrated alumina film layer into hydrated alumina powder.
8. The method according to claim 2, wherein the high-temperature calcination in the step (5) is carried out at a temperature ranging from 1100 to 1300 ℃.
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Citations (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5312789A (en) * | 1987-05-27 | 1994-05-17 | Minnesota Mining And Manufacturing Company | Abrasive grits formed of ceramic, impregnation method of making the same and products made therewith |
| CN101092307A (en) * | 2007-04-20 | 2007-12-26 | 江苏省陶瓷研究所有限公司 | Filter plate of porous ceramic covered by Nano ceramic membrane filter, and fabricating method |
| CN101444725A (en) * | 2008-12-26 | 2009-06-03 | 上海师范大学 | Method for preparing load type titanium dioxide photocatalytic film |
| CN101531469A (en) * | 2009-04-13 | 2009-09-16 | 浙江大学 | Transparent lyophobic alumina film and preparation method thereof |
| CN102861618A (en) * | 2011-07-07 | 2013-01-09 | 中国石油化工股份有限公司 | Preparation method of alumina supporter |
| CN103803814A (en) * | 2013-12-27 | 2014-05-21 | 东华大学 | Preparation method of transparent super-hydrophobic coating |
| CN105513795A (en) * | 2016-01-19 | 2016-04-20 | 同济大学 | Hydrated alumina dielectric thin film with solid electrolyte function and preparation thereof |
| CN107245323A (en) * | 2017-01-10 | 2017-10-13 | 白鸽磨料磨具有限公司 | Production method of alumina abrasive and products thereof |
| CN107814817A (en) * | 2016-09-13 | 2018-03-20 | 三星电子株式会社 | Aluminium compound, by using its formed film method and manufacture IC-components method |
| CN109319813A (en) * | 2018-11-09 | 2019-02-12 | 中山大学 | A kind of preparation method of two dimensional oxidation aluminium powder |
| CN109487245A (en) * | 2018-12-14 | 2019-03-19 | 华南理工大学 | A kind of preparation method of super-hydrophobic aqua oxidation aluminium film |
-
2021
- 2021-09-13 CN CN202111070015.1A patent/CN113772704A/en active Pending
Patent Citations (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5312789A (en) * | 1987-05-27 | 1994-05-17 | Minnesota Mining And Manufacturing Company | Abrasive grits formed of ceramic, impregnation method of making the same and products made therewith |
| CN101092307A (en) * | 2007-04-20 | 2007-12-26 | 江苏省陶瓷研究所有限公司 | Filter plate of porous ceramic covered by Nano ceramic membrane filter, and fabricating method |
| CN101444725A (en) * | 2008-12-26 | 2009-06-03 | 上海师范大学 | Method for preparing load type titanium dioxide photocatalytic film |
| CN101531469A (en) * | 2009-04-13 | 2009-09-16 | 浙江大学 | Transparent lyophobic alumina film and preparation method thereof |
| CN102861618A (en) * | 2011-07-07 | 2013-01-09 | 中国石油化工股份有限公司 | Preparation method of alumina supporter |
| CN103803814A (en) * | 2013-12-27 | 2014-05-21 | 东华大学 | Preparation method of transparent super-hydrophobic coating |
| CN105513795A (en) * | 2016-01-19 | 2016-04-20 | 同济大学 | Hydrated alumina dielectric thin film with solid electrolyte function and preparation thereof |
| CN107814817A (en) * | 2016-09-13 | 2018-03-20 | 三星电子株式会社 | Aluminium compound, by using its formed film method and manufacture IC-components method |
| CN107245323A (en) * | 2017-01-10 | 2017-10-13 | 白鸽磨料磨具有限公司 | Production method of alumina abrasive and products thereof |
| CN109319813A (en) * | 2018-11-09 | 2019-02-12 | 中山大学 | A kind of preparation method of two dimensional oxidation aluminium powder |
| CN109487245A (en) * | 2018-12-14 | 2019-03-19 | 华南理工大学 | A kind of preparation method of super-hydrophobic aqua oxidation aluminium film |
Non-Patent Citations (1)
| Title |
|---|
| 苗虎等: "原子层沉积技术发展概况", 《真空》 * |
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