CN105289946A - Method and equipment for preparing compact thin film by electrostatic spraying method - Google Patents
Method and equipment for preparing compact thin film by electrostatic spraying method Download PDFInfo
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- CN105289946A CN105289946A CN201510829620.0A CN201510829620A CN105289946A CN 105289946 A CN105289946 A CN 105289946A CN 201510829620 A CN201510829620 A CN 201510829620A CN 105289946 A CN105289946 A CN 105289946A
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Abstract
The invention provides a method for preparing a compact thin film by an electrostatic spraying method. The method comprises the following steps that at least two spray nozzles are adopted for spraying at least two kinds of precursors to the same substrate or collecting device; after meeting on the substrate or in the collecting process, the precursors carry out a chemical reaction so as to generate a thin film. According to the method, the spray nozzles simultaneously spray the precursors to the substrate or collecting device, or sequentially spray the precursors to the substrate or collecting device; the distance between the spray nozzles is adjustable; relative positions of the spray nozzles and the substrate or collecting device are adjustable. The method disclosed by the invention is low in cost, simple to operate, and high in repeatability; the thin film prepared by the method disclosed by the invention is not liable to crack.
Description
Technical field
The invention belongs to film fabrication techniques field in micro-nano opto-electronic device, particularly a kind of standby without cracking and the method and apparatus of the film of densification based on two shower nozzle or many shower nozzles electrostatic spraying legal system.
Background technology
Liquid phase method is the common technique preparing the films such as silica, have with low cost, easy and simple to handle, can be used for the outstanding advantages such as flexible substrates, flourish along with fields such as solar cell and flexible wearable equipment, liquid phase method film preparation is subject to more and more higher attention in recent years, has been widely used in the every field such as the preparation of electronics, optics, electromagnetism, calorifics, chemistry and composite at present.
In the process using Liquid preparation methods film, czochralski method and spin-coating method are two kinds of common plated film means.Liquid preparation methods silicon oxide film common at present utilizes sol-gal process first to generate silica sol, and recycling spin-coating method, dip-coating method, single spraying head electrostatic spraying method etc. generate silica membrane at substrate surface.Concrete method: at a certain temperature, utilizes silica precursor solution: ethyl orthosilicate (TEOS) and another kind of reactant deionized water are hydrolyzed polycondensation reaction in solvent absolute ethyl alcohol, use acid or alkali as catalyst simultaneously.After silicon dioxide gel generates, after sealing and standing a period of time, be coated with silicon oxide film with different coating methods at substrate surface, and do some Post isothermal treatment by organic matter and water volatilization, thus pure silicon oxide film, but film problem easy to crack can be there is.Trace it to its cause, because czochralski method and spin-coating method are all before film coated, precursor reactant have already been mades chemical reaction and generates certain liquid phase, molecule or other micro-nano structures of reaction of formation thing in the liquid phase can be caused like this, the size of these molecules or other micro-nano structures usually in tens nanometers to several micron dimension, molecular atoms particle compared to precursor reactant itself wants large several order of magnitude, thus be difficult in the film link together preferably, extremely be unfavorable for finally obtaining dense film, the film generated also easily ftractures.
Summary of the invention
The object of the present invention is to provide a kind of low cost, simple to operate, repeatable strong, energy-conserving and environment-protective, can large area prepare film based on two shower nozzle or many shower nozzles electrostatic spraying legal system for the new method of film and equipment, the film of preparation is not easy to crack.
In order to solve the problems of the technologies described above, the invention provides a kind of electrostatic spraying legal system that adopts for the method for film, adopt at least two shower nozzles to spray at least two kinds of precursor in same substrate or gathering-device, described precursor carries out chemical reaction film former after meeting in substrate or collection process.
Preferably, described shower nozzle basad or gathering-device sprays precursor or described shower nozzle simultaneously and successively basad or gathering-device sprays precursor.Namely such as shower nozzle A moves away after substrate surface sprays a kind of precursor reactant, and another kind of precursor reactant is sprayed in the place that shower nozzle B sprayed at shower nozzle A again; Shower nozzle A and shower nozzle B also relative the fixing in position can spray precursor reactant simultaneously, and select motion path to spray, the region that shower nozzle A and shower nozzle B is sprayed is overlapping, film former after the precursor reactant chemical reaction of overlay region.Relative motion mode between shower nozzle and substrate or gathering-device can be the tracks such as straight line, circle, spiral, rectangle.
Preferably, spray the position of mobile shower nozzle in the process of precursor at shower nozzle, make film that substrate or gathering-device deposit even.
Preferably, spray the position of mobile substrate or gathering-device in the process of precursor at shower nozzle, make film that substrate or gathering-device deposit even.
Preferably, the relative position of shower nozzle and substrate or gathering-device is adjustable, even by the film regulating relative position to make substrate or gathering-device deposit.
Preferably, the spacing between shower nozzle is adjustable, by the film regulating the spacing between shower nozzle can generate diverse microcosmic structure or different component ratio.
Preferably, two shower nozzles ethyl orthosilicate and deionized water is respectively adopted.
The present invention also proposes a kind of electrostatic spraying legal system that adopts for the equipment of film, and comprising can the mechanical platform of three-dimensional movement; At least two electrostatic spraying shower nozzles are fixed on mechanical platform, and described shower nozzle is moving under the drive of mechanical platform; Described shower nozzle is used for the precursor prepared needed for film that splendid attire is different respectively.
Further, the position between shower nozzle and the movement locus of shower nozzle can adjust.
The present invention compared with prior art, its remarkable advantage is, (1) sprayed in different precursor to substrate or gathering-device by two shower nozzles or multiple shower nozzle and carry out reacting the film required for generating, can effectively control point of response and time, avoid in common sol-gel process to react and to have produced in precursor thus the film generated problem easy to crack; (2) the present invention is simple to operate, repeatability is strong; (2) can carry out under room temperature or different temperatures; (3) large-scale industrial production is applicable to; (4) can at flexible substrate material surface coating; (5) cost is low; (6) the different nanostructureds etc. of commaterial can be prepared without the need to HTHP.
Accompanying drawing explanation
Fig. 1 the present invention is based on the principle schematic of electrostatic spraying legal system for silicon oxide film.
Fig. 2 is that the present invention adopts two static nozzles to prepare the schematic diagram of silicon oxide film.
Fig. 3 is that the present invention adopts multiple static nozzle to prepare the schematic diagram of silicon oxide film.
Respectively based on the scanning electron microscope (SEM) photograph of the standby silicon oxide film of the electrostatic spraying legal system of the electrostatic spraying method of dip-coating method, spin-coating method, single spraying head, of the present invention pair of shower nozzle in Fig. 4 test, four scanning electron microscope (SEM) photographs a, b, c, d respectively in corresponding diagram.
Detailed description of the invention
Easy understand, according to technical scheme of the present invention, when not changing connotation of the present invention, one of ordinary skill in the art can imagine that the present invention adopts electrostatic spraying legal system for the numerous embodiments of the method and apparatus of dense film.Therefore, following detailed description of the invention and accompanying drawing are only the exemplary illustrations to technical scheme of the present invention, and should not be considered as of the present invention all or the restriction be considered as technical solution of the present invention or restriction.
When the present invention adopts two shower nozzle or many shower nozzles electrostatic spraying method to carry out plated film; different precursor reactant is imported respectively by two shower nozzle or many shower nozzles; the chemical reaction of different precursor reactant is allowed to carry out in substrate or gathering-device; so just efficiently avoid the generation of molecule or structure in precursor, easily obtain the high-quality fine and close film without cracking.Electrostatic spraying is that a kind of hydrostatic(al) principle of dynamics that utilizes makes liquid dispersion produce the method for fine drop spraying, and the leaking medium model that J.R.Melcher and G.I.Taylor etc. propose has detailed explanation to its basic physical process.The method is used widely in fields such as mcroorganism molecular mass instrument, industry spraying, close-weave, nano-fabrication technique.The pattern of electrostatic spraying generally can be divided into drop pattern (dropletmode), one-jet pattern (single-jetmode) and many jet models (multi-jetmode).Along with voltage increases, drop becomes one-jet and finally becomes many jets, in the process of masking, adopts many jets.The height of shower nozzle distance substrate can affect the distribution of fine drop, distance hour, the tightly packed formation film of film particles; Apart from time large, it is very wide in range that film particles distributes, and spacing is very large.The flow of injecting fluid can affect the distribution of film particle, and flow is larger, and the distribution of particles of substrate surface is tightr.Injecting time is more of a specified duration, and film is thicker, if the time is excessively of a specified duration, likely there will be cracking phenomena, controllable thickness scope: tens nanometers-several microns.
General principle of the present invention as shown in Figure 1, comprise at least two shower nozzles 2, different precursor reactants 1 is placed in different shower nozzles 2 respectively, be that different shower nozzles 2 powers up by high-voltage DC power supply 3, thus by shower nozzle 2, precursor reactant 1 is sprayed with the form of taper injection stream 4, and be injected in and be placed in the substrate 5 of heating platform 6, spray film former after different precursor reactant generation chemical reactions on substrate 5.Heating platform 6 one end ground connection 7.
Embodiment
When using multiple shower nozzle to prepare required film, as shown in Figure 2, build XY precision optical machinery platform, can be three-dimensional mobile arbitrarily; Fixing multiple electrostatic spraying shower nozzle is on mechanical platform, the shower nozzle other end has liquid injection pipe and the wire for transferring high voltage electricity, high-tension electricity applies high-magnitude DC electrostatic to the precursor reactant liquid of injection, make the liquid droplet charged from shower nozzle drippage, when after same sex electric charge on the molecular band in drop, mutual repulsion can be started, after electrostatic force is greater than Surface Tension of Liquid Drops, finally split into countless tiny drops, thus eject the many jets of formation.Relative position between multiple shower nozzle needs to determine according to plated film, and distance is different, can form different membrane structures at substrate surface, as the film etc. of the network structure that the film of smooth densification, particle are piled up in order; Mechanical platform drives the opposed substrate motion simultaneously of multiple shower nozzle according to the distance of setting, ejects the precursor of given flow to substrate simultaneously simultaneously, thus be coated with film with high-pressure electrostatic from multiple shower nozzle in substrate.
Composition graphs 3, uses the electrostatic spraying legal system of of the present invention pair of shower nozzle for silicon oxide film.Whole experiment is carried out in hundred-grade super-clean.First building three-dimensional mobile platform, keeping and the setting that corresponding program completes set distance is inputted to platform courses end; Two shower nozzles are fixed on platform, make spacing be 3cm; By the skinny device needed for experimental provision as high-voltage DC power supply, syringe pump, heating platform etc. put into respective position accordingly, connect corresponding power line; The configuration of solution: proportionally, appropriate ethanol solution is injected at a clean glass reagent bottle, measure corresponding ethyl orthosilicate again to inject wherein, certain absolute ethyl alcohol is injected in the glass reagent bottle of another cleaning, measure corresponding reactant deionized water and catalyst adds wherein, separately fully mixing; Regulating parameter: injection flow, voltage, the shower nozzle distance height of bottom, plated film time, shower nozzle translational speed and the parameter such as track, substrate heating-up temperature.Concrete parameter is as follows: the liquid injection flow of two shower nozzles is 60ul/m; Voltage is 12KV; The height of shower nozzle distance bottom is 6cm; The plated film time is 5min.Because the liquid in two shower nozzles is two reactant TEOS for hydrolysis condensation reaction and deionized water respectively, react so utilize two shower nozzles to realize the substrate surface sprayed heating.Also respectively based on the electrostatic spraying method of dip-coating method, spin-coating method, single spraying head in test.The scanning electron microscope (SEM) photograph of the silicon oxide film that aforementioned four kinds of methods obtain is respectively as shown in a, b, c, d in Fig. 4.Obviously can be found out that by Fig. 4 the smooth densification of silicon oxide film that the two shower nozzle electrostatic spraying legal system of the present invention is standby does not have crackle or cracking, is better than additive method.Use the present invention when preparing silicon oxide film, the temperature that can change substrate to obtain the silica of different structure, as square particle, wire, bar-shaped, tree-shaped.
Claims (10)
1. one kind adopts electrostatic spraying legal system for the method for film, it is characterized in that, adopt at least two shower nozzles to spray at least two kinds of precursor in same substrate or gathering-device, described precursor carries out chemical reaction film former after meeting in substrate or collection process.
2. prepare the method for film according to claim 1, it is characterized in that, described shower nozzle basad or gathering-device sprays precursor simultaneously.
3. prepare the method for film according to claim 1, it is characterized in that, described shower nozzle successively basad or gathering-device sprays precursor.
4. prepare the method for film according to claim 1, it is characterized in that, spray the position of mobile shower nozzle in the process of precursor at shower nozzle.
5. prepare the method for film according to claim 1, it is characterized in that, spray the position of mobile substrate or gathering-device in the process of precursor at shower nozzle.
6. prepare the method for film according to claim 1, it is characterized in that, the relative position of shower nozzle and substrate or gathering-device is adjustable.
7. prepare the method for film according to claim 1, it is characterized in that, the spacing between shower nozzle is adjustable.
8. prepare the method for film according to claim 1, it is characterized in that, adopt two shower nozzles ethyl orthosilicate and deionized water respectively.
9. adopt electrostatic spraying legal system for an equipment for film, it is characterized in that, comprising can the mechanical platform of three-dimensional movement; At least two electrostatic spraying shower nozzles are fixed on mechanical platform, and described shower nozzle is moving under the drive of mechanical platform; Described shower nozzle is used for the precursor prepared needed for film that splendid attire is different respectively.
10. adopt electrostatic spraying legal system for the equipment of film according to claim 9, it is characterized in that, the position between shower nozzle and the movement locus of shower nozzle can adjust.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106218223A (en) * | 2016-07-26 | 2016-12-14 | 珠海纳金科技有限公司 | A kind of method and apparatus of on-demand electrostatic spraying |
| CN107716182A (en) * | 2017-11-17 | 2018-02-23 | 中国计量大学 | Viscose spray equipment |
| CN109860507A (en) * | 2018-12-03 | 2019-06-07 | 中国计量大学 | A kind of foam conductive net/silica preparation facilities and control method |
| CN111432937A (en) * | 2017-11-30 | 2020-07-17 | 艾仕得涂料系统有限责任公司 | System for applying a coating composition using a high transfer efficiency applicator, coating and corresponding method |
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| CN103469179A (en) * | 2013-10-07 | 2013-12-25 | 复旦大学 | Method for preparing inorganic gradient thin film based on solution in vacuum environment |
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| CN106218223A (en) * | 2016-07-26 | 2016-12-14 | 珠海纳金科技有限公司 | A kind of method and apparatus of on-demand electrostatic spraying |
| CN106218223B (en) * | 2016-07-26 | 2018-06-22 | 珠海纳金科技有限公司 | A kind of method and apparatus of on-demand electrostatic spraying |
| CN107716182A (en) * | 2017-11-17 | 2018-02-23 | 中国计量大学 | Viscose spray equipment |
| CN111432937A (en) * | 2017-11-30 | 2020-07-17 | 艾仕得涂料系统有限责任公司 | System for applying a coating composition using a high transfer efficiency applicator, coating and corresponding method |
| CN109860507A (en) * | 2018-12-03 | 2019-06-07 | 中国计量大学 | A kind of foam conductive net/silica preparation facilities and control method |
| CN109860507B (en) * | 2018-12-03 | 2022-01-28 | 中国计量大学 | Foam conductive net/silicon dioxide preparation device and control method |
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