CN1669668B - Synchronous load quick film-forming method for nano functional film - Google Patents
Synchronous load quick film-forming method for nano functional film Download PDFInfo
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- CN1669668B CN1669668B CN 200510034020 CN200510034020A CN1669668B CN 1669668 B CN1669668 B CN 1669668B CN 200510034020 CN200510034020 CN 200510034020 CN 200510034020 A CN200510034020 A CN 200510034020A CN 1669668 B CN1669668 B CN 1669668B
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Abstract
The invention provides a method of rapidly forming a nanometer functional film through synchronizing loading, by which can form the even film quickly in the carrier and the drying of the film can be finished at the same time. The method comprise the following steps: a) atomizing the solution or colloidal sols in the reservoir 6 through the pressure air, b) forming the dropping liquid 4 with uniform distribution through the injector 5, c) spraying the liquid 4 on the carrier 3 continuous rotary or moving in a certain speed, meanwhile, the flame 2 of the hot injector 1 in the drying part heat the carrier to 150-400 Deg.c, which makes the film on the carrier drying quickly and forming the even film.
Description
Technical field
The present invention relates to the film build method of the nanometer film of finishing, nano coating and the use of inorganic nano film preparation field.
Background technology
Coat nano coating at common carrier surface, in finishing and modification, have broad application prospects, as on carbon steel, coating nano coating (MoSi
2/ SiC), after heat treatment, the hardness of coating has improved tens times, anti-oxidant and resistance to elevated temperatures also improves greatly, at the nano-titanium oxide rete that plates on glass, glass has self-cleaning net work energy, airborne VOC can degrade under sunshine or UV-irradiation, has photocatalysis performance, on porous carrier, coat the film formed nanofiltration of nanometer, milipore filter is at liquid, gas cleaning, fields such as separation have wide application prospects, can the performance of the rete that is coated be except the composition that depends on film, and the method for film forming also plays a decisive role, stablize uniform rete in the load apace on the carrier, the performance of rete all has much relations with the method for film forming.
In the inoranic membrane field, to modify film, the preparation nanofiltration, milipore filter and other functional membrane, modification at these films, in the preparation process, film build method is to obtain evenly, the key of zero defect film, general film build method has rubbing method, put forward the method for being coated with (dip-coating), dip coating, sedimentation, spraying process etc., it is the coating fluid of 0.05～40% (weight) that Chinese patent " method of forming coating film " (CN1198106) is mentioned with a kind of gravure roller a kind of solid concentration of continuous coating on a kind of supporter, form the film that a kind of dry film thickness is 0.005～1 μ m, Chinese patent CN1359865 deposits on substrate and obtains water white WO with lifting coating method (dip-coating)
3Gas chromism film.Rubbing method, film forming procedure and the dry run of putting forward the method for being coated with (dip-coating), dip coating, sedimentation film forming are all separately carried out, there are membrane thickness unevenness, drying time long and in dry run, occur defective such as crackle easily, especially on porous carrier during film forming, defectives such as crackle, pinprick all appear in film that above-mentioned several method forms easily, need film repeatedly, drying time is long.When adopting sol-gel process on carrier during film forming, film forming and dry cycle reach a couple of days even longer, and require the pore structure of porous carrier, pore size to be complementary with the particle size of colloidal sol, the aperture of carrier is too big, colloidal sol will infiltrate in the carrier duct in film forming procedure and be difficult at surface filming, the aperture of carrier is too little after the carrier surface film forming, occurs rete easily and phenomenon such as peels off, and influences the performance and the stability in use of film forming.
Chinese patent CN1384219 utilizes vacuum film formation apparatus, carries out the film forming of two-layer above multilayer film with the raw material of electron gun heating film.Chinese patent CN1336258 utilizes the internal spray unit-liquid spray nozzle that comprises many apertures to make thin filming at short notice.Chinese patent CN1347137 provides a kind of film build method and film formation device, form on processed substrate by the dropping liquid nozzle that can move in a certain direction and to film, utilize the mobile of substrate solvent atmosphere aspiration to be walked with the suction nozzle that links to each other with vavuum pump, with the thickness uneven phenomenon that suppresses to film, shorten to form and film the required time.These film build methods and film formation device only are suitable for and plate carrier surface film forming, and be inapplicable to the film forming of the carrier of cast or other shape.
Summary of the invention
The objective of the invention is to defective at the prior art existence, provide a kind of not only can plate but also can carrier at cast on the synchronized loading fast filming method of loaded with nano functional membrane, these carriers can be the pipe or the sheets of various potteries, metal, and the pipe of these potteries, metal or sheet can be porous, densification, smooth and coarse.And film forming and drying finish synchronously, shortened film forming and dry cycle greatly.The distinctive film technique of the present invention can be in several minutes or tens of minutes forms the dry coating of uniform film thickness, flawless, controllable film thickness at carrier surface, require the inoranic membrane of low (＜400 ℃) for sintering temperature, also can a step obtain sintered membrane, not need follow-up sintering process.
The synchronized loading fast filming method of nano functional film of the present invention comprises the steps:
(1) preliminary treatment of carrier: the carrier that cleaning will plated film, remove pollutants such as floating dust, oil stain, oven dry is fixed in the carrier movement mechanism;
(2) film forming: the colloidal sol or the solution that will contain the required active component of nanometer film are poured in the fluid reservoir, utilize air compressor machine or pressure-air (or nitrogen) with the quick atomizing spraying of the drop at nozzle place at rotation or the carrier surface that moves, form a rete at carrier surface;
(3) rete drying: in the spraying film forming, the flame of hot nozzle is heated to 150-400 ℃ with carrier on carrier, makes the even rete of the dry simultaneously and rapidly formation of rete that loads on the carrier;
(4) film sintering.
After described film sintering is meant film forming, put into the high temperature furnace sintering, form stable, firm rete.
For the inoranic membrane of sintering temperature requirement low (＜400 ℃), the flame of hot nozzle can be with the film sintering of load on the carrier in heating carrier.
The rete drying of the film forming of described step (2) and step (3) hockets, and carrier is in whole film forming and dry run rotation or mobile continuously.
Described carrier is the pipe or the sheet of various potteries, metal material.The pipe of materials such as these potteries, metal or sheet can be porous, densification, smooth or coarse.
The present invention has following advantage compared with the prior art:
(1) colloidal sol or the solution that contains the nanometer film active component is atomized by gases at high pressure, and the particle in colloidal sol or the solution evenly disperses, and does not assemble, and can form uniform rete at carrier surface.
(2) in the atomizing film forming, the flame of hot nozzle is heated to 150-400 ℃ with bearer synchronization, makes the even rete of the dry simultaneously and rapidly formation of rete that loads on the carrier.
(3) whole film and dry run in, carrier is all the time with rotation at the uniform velocity or move, each moment the thickness of rete extremely thin, drying can be finished in moment, can effectively prevent defectives such as crackle that the rete dry run very easily occurs, pinprick.
(4) flame of hot nozzle can be with the synchronous sintering of the film of load on the carrier in heating carrier.
Description of drawings
Fig. 1 is the schematic diagram at the outer tube wall loaded with nano functional membrane of tubular carrier.
Fig. 2 is the schematic diagram at the inner tubal wall loaded with nano functional membrane of tubular carrier.
Fig. 3 is in the schematic diagram of the area load nano functional film of chip carrier (the be placed in both sides of carrier of atomizing and heater.
Fig. 4 is that (atomizing and heater place the same side of carrier at the schematic diagram of the area load nano functional film of chip carrier.
The specific embodiment
Embodiment 1
Woelm Alumina pipe 3 is cleaned, remove pollutants such as floating dust, oil stain, oven dry is fixed in the carrier movement mechanism, the boehmite colloidal sol that will be feedstock production with the aluminium isopropoxide is poured (as accompanying drawing 1) in the fluid reservoir 6 into, start carrier movement mechanism, Woelm Alumina pipe 3 is rotated continuously with 200 rev/mins rotating speed, open air valve, utilize high pressure nitrogen that the drop at nozzle 5 places is atomized into Woelm Alumina pipe 3 outer surfaces that vaporific drop 4 is sprayed on rotation fast, after 5 seconds, form one deck liquid film at carrier surface.Regulate flame 2 sizes of hot nozzle 1, make the carrier surface temperature be controlled at 400 ℃, make the rete rapid draing that is carried on the carrier, after 3 seconds, the flame 2 of hot nozzle 1 is turned down, continuation is atomized into vaporific drop 4 fast with the drop at nozzle 5 places and is sprayed on carrier 3 surfaces with the certain speed rotation, form the liquid film of new one deck on carrier 3 surfaces, so film load and drying hocket, obtained the gama-alumina nanometer film of uniform film thickness after 40 seconds on Woelm Alumina pipe 3 surfaces, and in drying, the flame 2 of nozzle 1 has also been finished the sintering process to nanometer gama-alumina nanometer film synchronously.This gama-alumina nanometer film aperture is 3-5nm, can be used for the ultrafiltration of liquid and separating of gas.
Embodiment 2
Porous metals titanium pipe is cleaned, remove floating dust, pollutants such as oil stain, oven dry is fixed in the carrier movement mechanism, the titanium oxide sol that will be feedstock production with the butyl titanate is poured (as accompanying drawing 2) in the fluid reservoir 6 into, start carrier movement mechanism, porous metals titanium pipe 3 is rotated continuously with 500 rev/mins rotating speed, the flame 2 that utilizes hot nozzle 1 to produce is controlled at about 250 ℃ the carrier surface fixed temperature, open air valve, utilize pressure-air that the drop at nozzle 5 places is atomized into the inner surface that vaporific drop 4 is sprayed on the porous metals titanium oxide pipe 3 of rotation fast, inner surface at carrier 3 forms one deck liquid film, the ultra-thin rete that forms in a certain local surfaces of carrier of rotation is immediately by dry simultaneously and rapidly, obtained the TiOx nano film of uniform film thickness after 2 minutes at the inner surface of porous metals titanium pipe 3, the aperture is about 3nm, can be used for the purification and the photocatalysis of air.
Embodiment 3
Glass plate is cleaned, remove pollutants such as floating dust, oil stain, oven dry is fixed in the carrier movement mechanism, moves with the velocity level of 10cm/sec..Pour titanium oxide sol in the fluid reservoir 6 (as accompanying drawing 3), start air compressor machine, utilize compressed air that the drop at nozzle 5 places is atomized into vaporific drop 4 fast and be sprayed on glass plate 3 surfaces of at the uniform velocity moving, form one deck retes on carrier 3 surfaces.Regulate the flame size of hot nozzle, make the carrier surface temperature reach 150 ℃, the rete that is carried on the surface is dried simultaneously and forms dry even rete, has obtained the titanium oxide layer of uniform film thickness after 1 minute on the glass plate surface.The sheet glass of this loaded with nano titanium oxide layer has self-cleaning net work energy such as organic pollution in the photocatalytic degradation air.
Embodiment 4
Potsherd is cleaned, remove pollutants such as floating dust, oil stain, oven dry is fixed in the carrier movement mechanism, moves with the velocity level of 20cm/sec..Pour titanium oxide sol in the fluid reservoir 6 (as accompanying drawing 4), start air compressor machine, utilize compressed air that the drop at nozzle 5 places is atomized into vaporific drop 4 fast and be sprayed on potsherd 3 surfaces, in the time of the spraying film forming, the flame of hot nozzle forms a rete at carrier surface after 2 seconds.The flame 2 of regulating hot nozzle 1 is heated to 200 ℃ with potsherd, and the liquid film drying with thermal Ceramics sheet surface forms rete fast, simultaneously the flame of hot nozzle can be further with the oxidation titanium film sintering of drying.After 45 seconds, formed the nano oxidized titanium film of layer of even at carrier surface.The potsherd of this loaded with nano oxidation titanium film has good in cleaning and bacteria resistance function.
Claims (4)
1. the synchronized loading fast filming method of a nano functional film is characterized in that comprising the steps:
(1) preliminary treatment of carrier: the carrier that cleaning will plated film, remove floating dust, oil stain, oven dry is fixed in the carrier movement mechanism;
(2) film forming: the colloidal sol or the solution that will contain the required active component of nano functional film are poured in the fluid reservoir, utilize air compressor machine or pressure-air with the quick atomizing spraying of the drop at nozzle place at rotation or the carrier surface that moves, form a rete at carrier surface;
(3) rete drying: in the spraying film forming, the flame of hot nozzle is heated to 150-400 ℃ with carrier on carrier, makes the even rete of the dry simultaneously and rapidly formation of rete that loads on the carrier;
(4) film sintering.
2. method according to claim 1 is characterized in that the film forming of step (2) and the rete drying of step (3) hocket, and carrier is in whole film forming and dry run rotation or mobile continuously.
3. method according to claim 1 and 2 is characterized in that requiring to be lower than 400 ℃ inoranic membrane for sintering temperature, and the flame of hot nozzle is in heating carrier, with the film sintering of load on the carrier.
4. method according to claim 3 is characterized in that described carrier is the pipe or the sheet of pottery, metal material.
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| Application Number | Priority Date | Filing Date | Title |
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| CN 200510034020 CN1669668B (en) | 2005-04-08 | 2005-04-08 | Synchronous load quick film-forming method for nano functional film |
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| CN 200510034020 CN1669668B (en) | 2005-04-08 | 2005-04-08 | Synchronous load quick film-forming method for nano functional film |
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| CN1669668A CN1669668A (en) | 2005-09-21 |
| CN1669668B true CN1669668B (en) | 2011-05-04 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| US8586138B2 (en) * | 2011-01-19 | 2013-11-19 | Halliburton Energy Services, Inc. | Method of coating a porous substrate with a thermoplastic material from the outside of the substrate |
| CN102126830B (en) * | 2011-03-02 | 2013-04-10 | 东莞宏威数码机械有限公司 | Titanium dioxide slurry spraying device and method |
| CN110274803A (en) * | 2019-05-30 | 2019-09-24 | 中国科学院金属研究所 | Can accuracy controlling nanometer grade thickness forming thin film thickness and area film-forming method |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1450123A (en) * | 2003-04-28 | 2003-10-22 | 西安交通大学 | Process for preparing nano structured titanium dioxide photocatalyst coating |
| CN1506164A (en) * | 2002-12-11 | 2004-06-23 | 中国科学院广州能源研究所 | Rotating, soaking and pulling process of preparing photocatalyst film on circular tube as substrate |
| CN1556548A (en) * | 2004-01-08 | 2004-12-22 | 西安交通大学 | Preparation method of large surface area carbon nano pipe film for field emitting display cathode |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1506164A (en) * | 2002-12-11 | 2004-06-23 | 中国科学院广州能源研究所 | Rotating, soaking and pulling process of preparing photocatalyst film on circular tube as substrate |
| CN1450123A (en) * | 2003-04-28 | 2003-10-22 | 西安交通大学 | Process for preparing nano structured titanium dioxide photocatalyst coating |
| CN1556548A (en) * | 2004-01-08 | 2004-12-22 | 西安交通大学 | Preparation method of large surface area carbon nano pipe film for field emitting display cathode |
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Owner name: GUANGZHOU PUREEASY HI-TEC. CO., LTD. Free format text: FORMER OWNER: SOUTH CHINA UNIVERSITY OF TECHNOLOGY Effective date: 20131108 |
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Effective date of registration: 20131108 Address after: Guangzhou Science City of Guangdong province 510663 City Nanxiang Road No. 52 Patentee after: Guangzhou Pureeasy Hi-tec. Co., Ltd. Address before: 510640 Tianhe District, Guangdong, No. five road, No. 381, Patentee before: South China University of Technology |