CN1775379A - Ultrasonic auxiliary drying method and apparatus for solution filming process - Google Patents

Abstract

The present invention relates to a new-type dry film-forming method and its device in the solution film-forming process. Said method includes ink-jet printing process, screen-printing process and whirl coating process, and adds ultrasonic treatment process, its device includes ultrasonic generator, film-forming sample base plate, conductive medium and protection device, etc.

Description

A kind of ultrasonic auxiliary drying method and device thereof that is used for solution film forming process

Technical field

The invention belongs to the solution film forming technical field, be specifically related to a kind of a kind of novel dried film build method and device that is used for solution process (Liquid Process) system film, be applicable to using inkjet printing (Ink-jet printing, IJP) drop of technology, serigraphy (Screen printing) technology and spin-coating method (Spin-coating) deposit or liquid film carry out subsequent drying processing film forming, in order to improve the uniformity of organic matter film forming, perhaps control the reunion of particle in the dry run.

Background technology

In the modern industry, people utilize the solution process to form required various function films more and more.So-called solution process is exactly through handling, such as being dispersed into nano level molecule material requested, be dissolved in the corresponding solvent then, utilize again other equipment with this solution deposition at substrate surface, treat solvent evaporation after, can form required film at substrate surface.

The film build method of solution process comprises a variety of means, such as common spin-coating method (Spin-coating), promptly utilize the spin coating instrument to revolve and get rid of film forming, in semiconductor industry and optical storage field extensive use, also a kind of system membrane means commonly used in the laboratory, people utilize spin-coating method to prepare metallic film again now, mainly are to utilize the solution that is dispersed with metal nanoparticle to get rid of to be coated with drying and forming-film.Such as the Au film that is used for OTFT (OTFT) electrode with the nanoparticles solution preparation of Au ^[1]But along with other utilize the development of solution process masking technique, spin-coating method has also demonstrated its weak point day by day.The film that spin-coating method is made is very thin, and is strict to working environment, needs the better purifying space of higher level, and to the utilization rate of material less than 1%, waste is serious, especially can't form pattern, and is powerless for the film forming of elaborate figure.

So people have been developed inkjet printing again, and (Ink-jet printing, IJP), serigraphy (Screen printing) etc. is used for the solution film forming technology, prepares various films with fine pattern.Serigraphy is to utilize printing technology, by repeatedly printing, and drying, last film forming, professor Jabbour of U.S. Arizona university once adopted this technology to prepare PLED (polymeric light-emitting device), was used for polymer film forming ^[2], comparatively complicated but printing forms the thin-film process of labyrinth, influence factor is a lot of and overcome a difficulty, and also is in the research exploratory stage now.

Inkjet technology also has a long history, and 1833, Savart just observes from the liquid miniflow of nozzle ejection can form drop of the same size ^[3]1878, Rayleigh carried out detailed mathematical description and exploration to this phenomenon for the first time ^[3].1951 in year, Siemens company has applied for the patent of invention of first practical ink-jet apparatus, and has made the ink mist recording instrument of first record analog voltage signal.To late 1970s, succeeded in developing practical inkjet technology, then promoted the use of rapidly, become the important means of publication and printing at present.Inkjet technology has the ability of desirable multicolour patternization, be fit to the baroque meticulous film of preparation, positioning accuracy can reach micron order, and to environmental requirement comparatively spin-coating method prepare loose, utilization rate to material is also very high, reaches more than 98%, meets very much green development thought, therefore, this technology is considered to very promising a kind of film preparation means.

Inkjet technology has been used to various solution film forming process, to prepare dissimilar films.1998, the people such as professor Yang Yang of U.S. UCLA at first propose inkjet technology can be used for full-color high molecule electroluminescent preparation of devices, and had prepared first PLED device ^[4]Inkjet technology is widely used in preparation high molecular polymer film afterwards, comprise Britain CDT, the Seiko-Epson of Japan, Philips, DuPont Display, Litrex, Covion, companies such as Toshiba have dropped into inkjet printing methods and have prepared in the exploitation of full-color PLED device, have obtained some phasic results.Be not only aspect PLED, in other respects, inkjet technology has been given full play to the advantage of solution process film forming, is used to prepare the colored filter (Color filter) that LCD uses ^[5], OTFT (Organic TFT) ^[6-7], metal electrode (Metal electrodes) ^[9]And three-dimensional divider wall (Walls) ^[10]Deng, all obtained good result.

Though inkjet printing has many benefits, in the technology of solution process system film, also exist the problem that much presses for solution.Wherein very important one is exactly the homogeneity question of film forming.Drop is spraying after on the substrate, rely on the solvent evaporation, make solute stay film forming, the evaporation process of solvent will be to the generation decisive influence such as uniformity of solute film forming, generally like this, evaporation along with solvent, because the edge evaporation is very fast, solution can flow to the edge, causes dry back to form intermediate thin, the film morphology that the edge is thick is commonly called as " coffee ring " (Coffee ring) ^[11], perhaps form the thin form in opposite thick middle both sides ^[12], for the PLED device, this will have a strong impact on the luminous uniformity of pixel, therefore, wait to improve with the uniformity of film of the high molecular polymer pixel of inkjet technology preparation is anxious, and the novel one-tenth membrane technology that exploitation can be used for this is very necessary.

Prepare metal electrode or the divider wall structure also can run into similar problem with inkjet technology.Particle after we require to reunite in the metallic film is as much as possible little, and is crosslinked mutually because little and fine and close even metal particle helps particle, the continuous film of formation, and help reducing the post-processed temperature, and improve the quality of preparation finished product.Like this, in the system film of solution process, will control the agglomeration traits of solution metal nanoparticle in dry run, otherwise volatilization along with solvent and stabilizing agent, size is easy to be agglomerated into mutually bigger particle at tens metallic particles below the nanometer, finally is to form continuous film by the particle after these bigger reunions.Big and the irregular particle in back of reuniting not only makes the post-processed temperature improve, and the compactness of film also is difficult to guarantee the quality of reduction film.Divider wall is generally used ceramic material, similar with metal nanoparticle solution, also be to be dispersed in the solvent with minimum particle, these ceramic particles of volatilization last resort by solvent form required structure, and last densification process generally will pass through (＞1000 ℃ of high temperature sinterings ^[10]).In whole process, in the sample before the sintering if the structure that has ceramic particle even, tiny, regular shape to constitute, then the finished product pottery behind the sintering is in intensity, toughness, all can there be significant advantage aspects such as the porosity than those structures that is made of bigger irregular particle, and sintering temperature also can correspondingly reduce.Therefore, the reunion of the tiny ceramic particle of control is a very crucial step in the solution evaporation process.

Therefore, exploitation is applicable to the new technology of solution film forming technology, improves into film quality, becomes very necessary work.

In another field, ultrasonic (Ultrasonic) is since being paused (Galton) discovery first 19 end of the centurys by jar (unit of capacitance), development through century more than one, be widely used in various industry and medical science, detection range, become indispensable technological means in fields such as cleaning, plastics and metal solder, metal forming and processing, chemical treatment flaw detection, hydrolocation, medical imaging, emulsification, dispersion, pulverizing.In the laboratory, use the various test vessel of ultrasonic cleaning, various solution are disperseed, to obtain more uniform solution, also right and wrong are usually used and essential treatment technology.

Along with the development of solution process masking technique, especially follow the progress of nanometer technology and inkjet technology, ultrasonicly after its birthday at the age of one hundred years old, should continue to open up new application, continue to radiate the vigour of youth.

Summary of the invention

The object of the present invention is to provide a kind of drying means and device that is used for solution film forming process, so that technology such as solution inkjet printing prepare the uneven problem of the film that occurs in the organic film process, obtain the film of central authorities and edge high conformity, and can solve in the formulations prepared from solutions process of metallic film, ceramic structure and the particle agglomeration problem occurs, make the particle of gained film and structure form uniform and smooth.

The drying means that is used for solution film forming process provided by the invention, be in film forming procedure, to introduce ultrasonic wave (Ultrasonic) technology, promptly, reach the uniformity of improving film central authorities and edge, be controlled to the particle agglomeration in the membrane process simultaneously by the evaporation process of ultrasonic concussion control solvent.

Here, said solution film forming process is meant a certain amount of solute is dissolved in coordinative solvent, make stable solution, perhaps stable within a certain period of time suspension, then by certain technological means, this solution that configures or suspension are deposited on the required substrate, and again with the solvent evaporation, dry back solute promptly forms the process of thin film on substrate.

In this solution film forming process, not only finger-type becomes thin film, comprises also that repeatedly film forming to form plural layers, perhaps forms 3-D solid structure.

Solution that uses in the solution film forming process or suspension, but wherein solute comprises the various ceramic particles of organic micromolecule compound, high molecular polymer, phosphor material, RE compound material, metal nanoparticle thermal sintering and various inorganic pigment granules etc.

Wherein said metal nanoparticle, can be made up of a kind of metal nanoparticle also can be that two or more metal nanoparticle is formed to solute in the solution.Here the average grain diameter of metal nanoparticle is below 100nm.

Also can comprise metal nano material in the wherein said ceramic particle, the average grain diameter of this metal nano material is less than 100nm.The average grain diameter of said ceramic particle and inorganic pigment granules should be at the 1 μ m order of magnitude, perhaps below the 1 μ m order of magnitude.

The solution deposition means of using in the said solution film forming process comprise inkjet printing (Ink-jet printing) technology, serigraphy (Screen printing) technology, spin coating (Spin-coating) technology etc.

Basic principle of the present invention is exactly to utilize the cavitation of ultrasonic wave in liquid, emulsification and to pulverizing, the peptizaiton of solid particle, the film sample that is in dry run is handled, improve the film thickness uniformity of organic high molecular polymer film, obtain the edge film more consistent with central authorities; The particle agglomeration of control metal or ceramic membrane or supporting construction makes the composition particle of gained sample interior finer and closely woven, performances such as the machinery of finished product and electricity after the raising post-processed; Accelerated the speed of drying and forming-film simultaneously.

The step of the drying means that the present invention proposes is as follows: the required solution of deposit film forming on the good substrate of surface treatment; the substrate that (guarantees solvent the least possible evaporation in transfer process) then rapidly and will be loaded with required solution is transferred to (as shown in Figure 1) in the Vltrasonic device; place substrate; carry out protective atmosphere, beginning is dry, opens ultrasonic generator; select suitable frequency and intensity; with the drying effect that obtains, treat the solution example drying and moulding after, this phase process process can finish.Can in device shown in Figure 1, continue further to handle or transfer to carry out complicated more processing in other Special Equipments.

In the said method, ultrasonic frequency range is controlled at 18MHz between the 100MHz, and ultrasonic power bracket is controlled at 100W between the 105W, and ultrasonic time is determined by the film forming requirement, was generally 10-60 minute.

In the said method, used Vltrasonic device is made up of the transmitting medium and the protective device that are used to conduct ultrasonic concussion and energy between ultrasonic generator, film forming sample substrate, ultrasonic generator and the film forming sample substrate; Wherein closely contact with ultrasonic generator below the transmitting medium, closely contact with the film forming sample substrate above, be beneficial to ultrasonic transmission; The film forming solution sample of carrying processing to be dried on the film forming sample substrate; Protective device is covered on the film forming sample substrate, is used for protection and avoids external environment influence in ultrasonic processing procedure.Structure principle chart is seen shown in Figure 1.

Description of drawings

Fig. 1 is a Vltrasonic device structure principle chart of the present invention.

Fig. 2 is the ultrasonic dry AFM vertical view (a) of handling back drop sample and this sample thickness profile figure (b) along the A-B line.

Fig. 3 handles the AFM vertical view (a) of back drop sample and this sample thickness profile figure (b) along the A-B line for air dry.

Fig. 4 is the optical microscope photograph (50X) of ultrasonic processing sample.

Fig. 5 is the AFM photo (a) and the granularmetric analysis diagram (b) of Au film.

Fig. 6 is the optical microscope photograph (50X) of air dry sample.

Number in the figure: 1-1 is a ultrasonic generator, and 1-2 is a transmitting medium, and 1-3 is the film forming sample substrate, and 1-4 is a solution example, and 1-5 is a protective device.

The specific embodiment

Below with reference to accompanying drawing content of the present invention is described in further details.

Fig. 1 is a schematic diagram of device of the present invention.

1-1 is a ultrasonic generator among Fig. 1, and this generator may be provided in the required high-power ultrasonic of membrane process, and power requirement should be in watt level or higher, and its power should be regulated, and it will be desirable selection that supersonic frequency can be regulated.General supersonic frequency be 18KHz between the 100KHz, the ultrasonic power scope is 10 ⁰W to 10 ⁵W.

1-2 is the medium that can conduct ultrasonic concussion and energy between ultrasonic generator and the film forming sample substrate 1-3 among Fig. 1, and this medium both closely contacted with ultrasonic generating means, and accompanying with becoming membrane sample again substrate closely contacts, and is beneficial to ultrasonic conduction.

1-3 is the substrate of carrying solution film forming sample among Fig. 1, and substrate can be various materials, and the most common is glass or ITO (tin indium oxide) glass, also can be other rigid substrates such as silicon chip, perhaps is flexible base, board; Substrate will closely contact with the transmitting medium shown in the 1-2 so that ultrasonic energy successfully be transmitted to substrate, and then be transmitted to pending drop again, make ultrasonic energy have to intervene suitably and handle film forming procedure; Substrate keep horizontal state with when the ultrasonic conducting medium contacts closely, to guarantee that film forming procedure is unlikely because the factor of gravity causes the film morphology of inclination, influences the uniformity of film forming;

Substrate among Fig. 1 shown in the 1-3 can expand to the substrate of being not only carrying solution film forming sample, also can comprise the device that carries this substrate, this device can make things convenient for the placement of sample substrate, can satisfy the requirement that keeps the substrate level, can conduct ultrasonic energy smoothly, the mode of placing substrate also helps ultrasonic concussion, and the drop on the substrate is applied effect; This device also can comprise temperature control and wait other equipment, better to be controlled to film quality;

1-4 is solution example to be dried on the substrate among Fig. 1, and after the solvent evaporation, solute is promptly stayed the required film of formation on the substrate, and follow-up operation is not got rid of certainly, but does not belong to this scope of invention.Sample can be the solution of organic molecule, polymer, also can be to be dispersed with nano metal, and the perhaps outstanding turbid emulsion of ceramic particle etc., the solution of all suitable solution film forming process all allows;

1-5 is the protective device of sample drying processing procedure among Fig. 1, can protect the influence of avoiding external environment condition in ultrasonic processing procedure, and should help the evaporation of solvent, regulates; If can observe pending sample treatment process then be better choice.

Combine by the protective device shown in the 1-5 among the substrate shown in the 1-3 among Fig. 1 and substrate expanding unit and Fig. 1; also can provide ask for something not high subsequent processes for the film forming sample; annealing process such as various atmosphere; as long as device can bear its annealing temperature; but do not impose this ability, the annealing of requirements at the higher level and temperature or other processing procedures can be transferred in the more special device and carry out.

Provide two embodiment and the corresponding Comparative Examples of using said method and device below, but the present invention is not limited to this two embodiment.

Embodiment 1

The material that uses in the present embodiment is the polymer ink sample, viscosity 4.5cps, spent glycol ether acetic acid esters dilution in 1: 1 by volume during use.

Substrate adopts glass substrate, and processing mode is as follows: glass substrate is added the ultrasonic processing of washing agent 10min with deionized water, rinse well with deionized water then, and again at deionized water for ultrasonic 10min, twice, preserve stand-by.

Solution deposition adopts the mode of inkjet printing (IJP) to prepare.Shower nozzle diameter 50 μ m adopt the work of piezoelectricity pattern.

Drying mode adopts the method for being set forth among the present invention, and drop dot matrix ejection back is transferred to substrate in the device shown in Figure 1 at once, opens ultrasonic generator, carries out drying and handles.The supersonic frequency that is adopted is 59KHz, and the power of selecting for use is 160W, processing time 30min.

After finishing, drying observes the pattern and the sectional thickness distribution of drop film forming with scanning probe microscopy.The result as shown in Figure 2.

Diameter is about 180 μ m after the droplet drying film forming that sprays among this embodiment.Fig. 2 (a) is that the AFM (AFM) behind droplet drying is observed photo in the ejection dot matrix, about liquid-drop diameter 180 μ m, we select scanner scans to 100 * 100 μ m of 125 μ m for use, coverage has contained the overwhelming majority of drop, Fig. 2 (b) is along the profile of A-B line among Fig. 2 (a), scope has covered the about more than 70% of diameter, from profile as can be seen, central authorities are thin, and the typical case that the edge is thick " coffee ring " (shown in the Comparative Examples of Fig. 2, Fig. 3) phenomenon improves.

Comparative Examples 1

The material that uses in this Comparative Examples is the polymer ink sample, viscosity 4.5cps, spent glycol ether acetic acid esters dilution in 1: 1 by volume during use.

Substrate adopts glass substrate, and processing mode is as follows: glass substrate is added the ultrasonic processing of washing agent 10min with deionized water, rinse well with deionized water then, and again at deionized water for ultrasonic 10min, twice, preserve stand-by.

Solution deposition adopts the mode of inkjet printing (IJP) to prepare.Shower nozzle diameter 50 μ m adopt the work of piezoelectricity pattern.

Drying mode adopts conventional air drying, and drop sprays on substrate all, at normal temperatures air dry.

After finishing, drying observes the pattern and the sectional thickness distribution of drop film forming with scanning probe microscopy.The result as shown in Figure 3.

Less from the drop of shower nozzle ejection in this example, diameter is about 110 μ m after the droplet drying film forming.Fig. 3 (a) is that the AFM (AFM) of a drop in the dot matrix is observed photo, about liquid-drop diameter 110 μ m, we select scanner scans to 100 * 100 μ m of 125 μ m for use, Fig. 3 (b) be among Fig. 3 (a) along the profile of A-B line, the last 70% that the section scope of Fig. 3 (b) has covered diameter.

As can be seen, the polymer ink after the air dry, the difference in thickness at film forming back edge and center are very tangible from profile, and difference in thickness presents typical coffee ring phenomenon about 180nm.Comparative example 1 observation data, the sample of crossing through ultrasonic aid in treatment is becoming to have shown the relative uniformity preferably with the edge of central authorities on the film uniformity that coffee ring phenomenon has obtained bigger improvement.

Embodiment 2

Used material is the nano particle of Au in the present embodiment, and Au is not more than the evengranular of 25nm with diameter and is dispersed in the solvent deionized water, and the concentration of Au is 10 ^-3The magnitude of mol/L keeps stable in order to make system, unlikelyly promptly reunites in solution, all is surrounded by one deck stabilizing agent around each Au particle, makes whole solution keep stablizing and clear state under the storage situation usually.

Substrate adopts glass substrate in the test, and processing mode is as follows: washing agent adds the deionized water ultrasonic wave and cleans 15min, rinses back deionized water ultrasonic cleaning 10min well with deionized water then, and twice, use absolute ethyl alcohol ultrasonic cleaning twice at last again, standby.

Mainly be in order to verify ultrasonic drying and forming-film technology control action for the nanoparticle agglomerates effect in metal nano suspension film forming procedure in the experiment.The thin particle that keeps trying one's best can make the easier formation metallic film of metallic particles.Suspension deposition process on substrate does not use ink-jet print system in the present embodiment, but adopt more simple mode: the disposable syringe of usefulness 1ml careful drips of solution on glass substrate, make every effort to each drop volume size unanimity, though ratio method is very simple mutually with ink-jet print system, the principle of drying and forming-film and process are similar.

Drying mode adopts the method for being set forth among the present invention, and drop drips good back to be transferred to substrate in as shown in Figure 1 the device at once, opens ultrasonic generator, carries out drying processing.The supersonic frequency that is adopted is 99KHz, and the power of selecting for use is 30W, processing time 20min.

After finishing, drying observes the surface topography and the surface uniformity of drop film forming with light microscope and scanning probe microscopy.Result such as Fig. 4, shown in Figure 5.

Fig. 4 is respectively the light microscope droplet drying film forming photo under 50 times of object lens, can only observe large-area Au film and exist under 50 times of object lens, and the centre is being mingled with hole not of uniform size, but does not observe the existence of Au particle; Fig. 5 is with the observed image of golden film and the roughly analysis of granularity in the scope of 5 * 5 μ m of AFM (AFM), middle the relatively large of light tone is residual organic stabilizer, from two kinds of charts, can see, the gold film in the gold reunion after particle size distribution more even, particle diameter is about 110nm (0.10 μ m), and the reunion of particle has obtained control preferably.

Comparative Examples 2

Used material is the nano particle of Au in the present embodiment, and Au is not more than the evengranular of 25nm with diameter and is dispersed in the solvent deionized water, and the concentration of Au is 10 ^-3The magnitude of mol/L keeps stable in order to make system, unlikelyly promptly reunites in solution, all is surrounded by one deck stabilizing agent around each Au particle, makes whole solution keep stablizing and clear state under the storage situation usually.

Substrate adopts glass substrate in the test, and processing mode is as follows: washing agent adds the deionized water ultrasonic wave and cleans 15min, rinses back deionized water ultrasonic cleaning 10min well with deionized water then, and twice, use absolute ethyl alcohol ultrasonic cleaning twice at last again, standby.

Mainly be in order to verify ultrasonic drying and forming-film technology control action for the nanoparticle agglomerates effect in metal nano suspension film forming procedure in the experiment.The thin particle that keeps trying one's best can make the easier formation metallic film of metallic particles.Suspension deposition process on substrate does not use ink-jet print system in the present embodiment, but adopt more simple mode: the disposable syringe of usefulness 1ml careful drips of solution on glass substrate, make every effort to each drop volume size unanimity, though ratio method is very simple mutually with ink-jet print system, the principle of drying and forming-film and process are similar.

Dry run and embodiment 2 compare, and adopt the normal temperature air dry.

With the pattern after the observation by light microscope drop film forming, the result as shown in Figure 6 after drying was finished.

Fig. 6 is that 50 times object lens are taken down, and scale label is 10 μ m among the figure.From photo, can see, be studded with not of uniform size among the figure, particle in irregular shape, particle diameter is between 1-10 μ m, as seen bigger agglomerated particle has taken place in the natural air drying film forming procedure, the result has caused isolated one by one big metallic particles, and does not have to form comparatively continuous Au film.Situation shown in this and the embodiment 2 differs greatly, and ultrasonic drying aid technology is to the solution process preparation of Au film, at the control particle agglomeration, keeps after the nano particle film forming still playing a good role having aspect the more tiny particle.

1.Yiliang?Wu，Yuning?Li，Beng?S.Ong， ^*Ping?Liu，Sandra?Gardner，and?Brian?Chiang.Adv.Mater.17，184(2005).

2.Dino?A.Pardo，Ghassan?E.Jabbour ^*and?Nasser?Peyghambarian，Adv.Mater.12，1249(2000).

3. yellow spring brightness, Li Fuyou, yellow dimension. electroluminescent organic material and device introduction. Shanghai: publishing house of Fudan University, 2005, p59.

4.Y?Yang，S?C?Chang，J?Bharathan，J.J?Liu，J.Mater.Sci：Mater.in?Electro.11，89(2000).

5.H.kiguchi，S.Katagami，Yamada，S.Miyashita，H.Aruga，A.Mori，T.Shimoda，T.Nakamura，H.Miymaoto?and?Y.Takeuchi，Tech?Digest?of?Asia?Display/IDW01，1745(2001).

6.H.Sirringhaus，T.Kawase，R.H.Friend，T.Shimoda，M.Inbasekaran，W.Wu?and?E.P.Woo，Science?290，2123(2000).

7.T.Kawase，H.Sirringhaus，R.H.Friend?and?T.Shimoda，Tech?Digest?of?IEDM，623(2000).

8.Takeo?Kawase，Christopher?Newsome，Satoshi?Inoue，Takayuki?Saeki，Hideyuki?Kawai，Sadao?Kanbe，Tatsuya?Shimoda，Henning?Sirringhaus，Devin?Mackenzie，Seamus?Burns?andRichard?Friend，Tech?Digest?of?SID02，1017(2002).

9.M.Furusawa，T.Hashimoto，M.Ishida，T.Shimoda，H.Hasei，T.Horai，H.Kiguchi，H.Aruga，M.Oda，N.Saito，H.Iwashige，N.Abe，S.Fukuda?and?K.Betsui，Tech?Digest?ofSID02，753(2002).

10.Xinglong?Zhao，Julian?R.G.Evans，and?Moban?J.Edirisinghe，J.Am.Ceram.Soc.85，2113(2002).

11.K.Morii?and?T.Shimoda，Journal?of?The?Surface?Science?Society?of?Japan(in?Japanese)24，28(2003).

12.T.R.Hebner，C.C.Wu，D.Marcy，M.H.Lu，and?J.C.Sturm，Appl.Phys.Lett.72，519(1998).

Claims (10)

1, a kind of solution film forming process ultrasonic auxiliary drying method that is used for; it is characterized in that concrete steps are as follows: the required solution of deposit film forming on the good substrate of surface treatment; the substrate that will be loaded with required solution is then transferred in the Vltrasonic device; place substrate; carry out protective atmosphere, beginning is dry, opens ultrasonic generator; the control supersonic frequency is 18MHz-100MHz, and ultrasonic power is 10 ⁰W-10 ⁵W.

2, method according to claim 1, it is characterized in that described solution film forming process is as follows: solute is dissolved in the coordinative solvent, make stable solution, perhaps stable within a certain period of time suspension, then this solution that configures or suspension are deposited on the substrate, with the solvent evaporation, dry back solute promptly forms thin film on substrate again.

3, method according to claim 2 is characterized in that the film forming procedure of described solution, comprises that repeatedly film forming to form plural layers, perhaps forms 3-D solid structure.

4, method according to claim 2, it is characterized in that the solution or the suspension that use in the solution film forming process, but wherein solute comprises the various ceramic particles and the various inorganic pigment granules of organic micromolecule compound, high molecular polymer, phosphor material, RE compound material, metal nanoparticle thermal sintering.

5, method according to claim 4, the average grain diameter that it is characterized in that said metal nanoparticle is below 100nm.

6, method according to claim 4; it is characterized in that including metal nano in the said ceramic particle; the average grain diameter of this metal nano material is less than 100nm, and the average grain diameter of ceramic particle or inorganic pigment granules is the 1 μ m order of magnitude, or below it.

7, method according to claim 1, it is characterized in that described on substrate the method for deposit solution be inkjet printing, serigraphy or spin coating.

8, a kind of device that is used for the ultrasonic drying aid of solution film forming process is characterized in that being made up of the transmitting medium and the protective device that are used to conduct ultrasonic concussion and energy between ultrasonic generator, film forming sample substrate, ultrasonic generator and the film forming sample substrate; Wherein closely contact with ultrasonic generator below the transmitting medium, closely contact with the film forming sample substrate above, be beneficial to ultrasonic transmission; The film forming solution sample of carrying processing to be dried on the film forming sample substrate; Protective device is covered on the film forming sample substrate.

9, device according to claim 8 is characterized in that the ultrasonic generator frequency is 18MHz-100MHz, and ultrasonic power is 10 ⁰W-10 ⁵W, adjustable.

10, device according to claim 9 is characterized in that described film forming sample substrate also comprises the device that carries this substrate, and this device can make things convenient for sample substrate to place, and can keep the substrate level, can conduct ultrasonic energy smoothly, helps ultrasonic concussion.

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