CN100437152C - Coating method of wet type anti-reflective compound film - Google Patents
Coating method of wet type anti-reflective compound film Download PDFInfo
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- CN100437152C CN100437152C CNB2004100834620A CN200410083462A CN100437152C CN 100437152 C CN100437152 C CN 100437152C CN B2004100834620 A CNB2004100834620 A CN B2004100834620A CN 200410083462 A CN200410083462 A CN 200410083462A CN 100437152 C CN100437152 C CN 100437152C
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Abstract
The present invention relates to a coating method for a wet anti-reflection compound film, which has the steps that step (1), a base material is provided and washed, step (2) film forming liquid which is formed by the mode that a compound used for forming a film is dissolved in a solvent which is easy to volatilize is provided, step (3) the film forming liquid is evenly coated on the surface of the base material at room temperature so as to ensure that after liquid on the surface of the base material is completely volatilized, the coating of a single layer film is completed without the need of heat treatment, and step (4), the step (3) is repeated according to requirements so as to complete the number of coating layers which are required. The present invention can make the film forming liquid coated and attached to the surface of the base material to directly generate an anti-reflection effect at the room temperature, can avoid damage for plastic base material because of the heat treatment, can overcome the manpower and cost consumption required in the existing film coating technology, and can form a film with uniform thickness. Besides, the film has little possibility of stripping. Therefore, the present invention is suitable for the base material with small volume, large curvature and anomalous surface shape.
Description
Technical field
The present invention relates to a kind of coating process of anti-reflection film, particularly about a kind of coating process of wet type anti-reflective compound film.
Background technology
When light wave was propagated between different medium, meeting was because of the difference of refractive index between the medium, and the phenomenon that produces refraction and reflect.In order to eliminate reflected light and to increase penetrance, can plate film in the base material both sides with suitable refractive index and thickness, the optical interference phenomenon of utilizing this film to cause reaches antireflection and anti-reflection effect.These anti-reflection films can be individual layer or the double layer design at single wavelength zero reflectivity, also can be at the multilayer design of dual wavelength or specific band zero reflectivity, need decide on special applications.
Mainly contain physical vaporous deposition (Physical Vapor Deposition is called for short the PVD method) and chemical vapour deposition technique (Chemical Vapor Deposition is called for short the CVD method) in order to the existing method that produces anti-reflection film.But these two kinds of methods still exist certain weak point.For example, the film that general PVD method forms and the adhesion of base material are relative relatively poor, easily cause demoulding.Trend towards gradually in optical module market under the situation of the optical base-substrate that volume is little, curvature is big, assembly volume is more little, curvature is big more, and then the influence of its surface effect is big more, adopts general PVD method to cause that the possibility of demoulding is also high more.And the equipment that the PVD method adopts is complicated, and the cost of purchase, Operation and maintenance equipment is higher, and this has limited being extensive use of of it.In addition, the method for evaporating that adopts in the PVD method also cools off inefficiency in a vacuum because of convection current, and the heat radiation of hot assembly material radiation might be absorbed by base material and causes the heating of base material; This heating can cause the particularly damage of plastic basis material of base material, as internal stress and warpage.
Relative PVD method, the depositing temperature of CVD method is higher, except minority can be below 600 ℃, majority all must realize 900-1000 ℃ of ability, have in addition under higher temperature, just can carry out.High temperature heats distortion and the structural variation that causes base material easily, can reduce the mechanical property of base material.In addition, the counterdiffusion mutually at high temperature of the alloying element in the rete of base material and deposition forms some fragility phase at the interface place, thereby has weakened adhesion between the two, easily causes demoulding.So the high temperature heating is the major defect of general CVD method, this makes it on using, and particularly when being applied to plastic basis material, is subjected to great restriction.
Except that PVD method and CVD method, also can be used for forming anti-reflection film based on the wet type coating method of sol-gel technique (Sol-Gel).Sol-gel technique is meant that metal organic or inorganic compound solidifies through solution, colloidal sol, gel, forms the method for oxide or other compound solid again through thermal treatment.Its general film forming procedure is: solution or colloidal sol are formed liquid film by infusion process on base material, subsequently base material is vertically erected, be transformed into amorphous state or polycrystalline attitude coating by thermal treatment after gelation.Adopt this method still to need through bakingout process, i.e. baking, therefore the ability film-forming is not suitable for plastic basis material yet.And base material is mentioned from solution or colloidal sol and is used for toasting dry process, because solution or the downward sedimentation of colloidal sol meeting, thereby cause the thickness of base material lower portion film to increase.Special under the bigger situation of base material area, differing greatly of base material upper and lower sides thickness consequently is difficult to form the uniform film of thickness.
Therefore, be necessary to provide a kind of anti-reflection film coating process of improvement, the device that its needs are succinct, cheap at room temperature can be implemented, and the film thickness that forms is even, is difficult for demoulding.
Summary of the invention
Fundamental purpose of the present invention is to provide a kind of coating process of wet type anti-reflective compound film, and this method need not can be implemented at normal temperatures in thermal treatment, thereby applicable to the coating of the various base materials that comprise plastic basis material.
Another object of the present invention is to provide a kind of coating process of wet type anti-reflective compound film, the film thickness that this method of mat forms is even, is difficult for demoulding, and is little applicable to volume, curvature is big, the irregular base material of surface configuration.
A further object of the present invention is to provide a kind of coating process of wet type anti-reflective compound film, this method only needs succinct, cheap device to implement, a large amount of manpowers and the board cost of having avoided existing coating technique to expend, thus can significantly reduce cost.
For achieving the above object, the coating process of wet type anti-reflective compound film of the present invention comprises the following steps: that (1) provides and clean a base material; (2) provide a film forming liquid, this film forming liquid is formed by being dissolved in the easy volatile solvent in order to film forming compound; (3) at room temperature base material is soaked into certain hour in the film forming liquid; (4) make base material break away from film forming liquid with certain speed, this speed control is the i.e. volatilization fully of moment solution that base material leaves film forming liquid liquid level, promptly finish single thin film coating and need not thermal treatment; And (5) repeating step (3) and (4) on demand, to finish the required coating number of plies.
In the coating process of above-mentioned wet type anti-reflective compound film, be inorganic oxide, nitride, sulfide, selenide or fluoride in order to film forming compound in this film forming liquid.Step wherein (4) can realize by the dip coated method, is about to base material and is soaked into certain hour in the film forming liquid, and the mode by mode that lifts or the sedimentation of film forming liquid liquid level makes base material break away from film forming liquid subsequently.When employing lifted mode, this base material can be positioned in the fixable basket support, and the motor that utilizes the constant speed lifting is soaked in the film forming liquid constant speed with this base material basket constant speed again and mentions.Wherein, with this base material basket speed control that constant speed is mentioned from film forming liquid be the i.e. volatilization fully of moment solution that base material leaves film forming liquid liquid level.
Compared with prior art, the present invention at room temperature is attached to the coating of film forming liquid and directly produces anti-reflection effect on the substrate surface, can avoid thermal treatment that the damage of plastic basis material is reached manpower and the cost that existing coating technique need expend, and the film thickness that forms is even, be difficult for demoulding, little applicable to volume, curvature is big, the irregular base material of surface configuration.
The present invention is further illustrated below in conjunction with accompanying drawing and embodiment.
Description of drawings
Fig. 1 is a coating flow synoptic diagram of the present invention.
Fig. 2 is soaked in the film forming liquid of fixed concentration the graph of a relation of its reflectivity of the film that is obtained and wavelength for adopting coating process of the present invention that plastic basis material is soaked frequency with difference.
Fig. 3 is soaked in glass baseplate in the film forming liquid of variable concentrations with fixing soak time for adopting coating process of the present invention, the graph of a relation of its reflectivity of the film that is obtained and wavelength, and the comparison diagram of its reflectivity of the film that is obtained and uncoated glass baseplate reflectivity.
Embodiment
Relevant detailed description of the present invention and technology contents, existing as follows with regard to accompanying drawings:
See also first figure, the coating process of wet type anti-reflective compound film of the present invention comprises the following steps: at first, shown in step S10, provides and clean a base material, as an optical base-substrate (plastics, glass mirror etc.); Then, shown in step S20, provide a film forming liquid, this film forming liquid is formed by being dissolved in the easy volatile solvent in order to film forming compound; Then, shown in step S30, at room temperature film forming liquid is evenly coated substrate surface, the liquid of confirming substrate surface is at room temperature fully after the volatilization, promptly finishes the coating of single thin film and thermal treatment such as need not toast; At last, shown in step S40, repeating step S30 to finish the required coating number of plies, so far promptly finishes the whole coating process of base film on demand.
Wherein, among the step S10, the cleaning of base material can realize by methods such as chemical cleaning method, ultrasonic cleaning process, ion blast techniques, with the dirt of removing substrate surface, and then obtain superior in quality film.Angle considers that optimal way is a chemical cleaning method from reducing cost.
Among the step S20, be inorganic oxide, nitride, sulfide, selenide or fluoride in order to film forming compound in the film forming liquid.The preferred embodiment of the present invention is a solid-state fluoride, and it is Bi, Ca, Ce, Na, Pb, Li, Mg, Nd, Ba or the Th that fluoridizes.Volatile solvent is a volatile at normal temperatures solvent known in the art in this film forming liquid, as supercritical CO
2
Among the step S30, the better embodiment of at room temperature film forming liquid evenly being coated substrate surface can realize by the dip coated method, that is, base material is soaked into certain hour in the film forming liquid, the mode by mode that lifts or the sedimentation of film forming liquid liquid level makes base material break away from film forming liquid subsequently.This dip coated method is the easiest, can carry out large-area coating film, also is suitable for various curved surfaces, shaped face.Film thickness is controlled by the settling velocity of pull rate or liquid level.In addition, the coefficient of viscosity of solution is high more, and film is thick more.
When employing lifted mode, this base material can be positioned in the fixable basket support, and the motor that utilizes the constant speed lifting is soaked in the film forming liquid constant speed with this base material basket constant speed again and mentions.Wherein, the rising or falling speed of motor adopts constant speed, and this rising or falling speed is decided at that time base material material, surfaceness, base material molding condition, surface area size, surface curvature.Big as the substrate surface roughness, be that irregular shape, surface area are bigger, should reduce the rising or falling speed of motor.The principle of speed control is the i.e. volatilization fully of moment solution that base material leaves liquid level, can avoid solution to dry in the shade naturally so phenomenon that the residual water stain phenomenon in back and uneven film thickness spare.
Mainly the acting as fixing substrate and can not drop in lifting process of the basket support of above-mentioned placement base material, its design must meet fixing substrate, avoid soaking the principle of back substrate surface thickness inequality.Therefore, the design of base material basket must cooperate base material to be soaked into angle, the direction of film forming liquid liquid level, and is not to be completely fixed.Base material is soaked into the angle and direction of liquid level to be decided by material, surfaceness, base material molding condition, surface area size, the surface curvature of base material.
Base material is mentioned after being soaked into film forming liquid, and the liquid of confirming substrate surface can be soaked into the base material basket in the film forming liquid at room temperature fully after the volatilization on demand again.So repeat to soak repeatedly, shown in step S40, reach desired anti-reflection effect until substrate surface.Wherein, the base material number of times that repeats to soak or to soak frequency relevant with material, surfaceness, base material molding condition, surface area size, the surface curvature of base material itself; Relevant with film forming liquid concentration, solute com-pounds, solvent composition; Relevant with the antireflection wave band of demand; Also relevant with the time length in base material is immersed in film forming liquid.Big as the substrate surface roughness, be irregular shape, surface area greatly, surface curvature is bigger, should increase the number of times that repeats to soak; Under the condition of fixedly solute com-pounds, solvent composition, film forming liquid concentration is high more, and the number of times that then repeats to soak should be few more; Under the situation of the antireflection wave band broad of demand, the number of times that repeats to soak should increase; Longer as the time that base material is immersed in the film forming liquid, the number of times that then repeats to soak should reduce.
Second figure is depicted as and adopts above-mentioned dip coated method that plastic basis material is soaked in the film forming liquid of fixed concentration with difference immersion frequency, the graph of a relation of its reflectivity of the film that is obtained (representing with number percent) and wavelength (so that how rice nm represents).As known in the figure, in film forming liquid concentration fixed, each soak time is under 10 seconds the situation, in visible light wave range (400-760nm), each reflectance curve (joining curve A, curve B, curve C respectively) of once immersion (10 seconds), secondary immersion (10+10 second), three immersion (10+10+10 second) plastic basis material gained totally tapers off trend.That is, the film mass reflex rate of three immersion gained is starkly lower than once to soak with secondary soaks, and also, the film anti-reflection effect of three immersion gained is best, and its reflectivity is positioned within the scope of 1%-2% in visible light wave range substantially.
The 3rd figure is depicted as and adopts above-mentioned dip coated method that glass baseplate is soaked in the film forming liquid of variable concentrations with fixing soak time, the graph of a relation of its reflectivity of the film that is obtained (representing) and wavelength (so that how rice nm represents), and the comparison diagram of its reflectivity of the film that is obtained and uncoated blank glass reflectivity with number percent.As known in the figure, before coating, the reflectivity of blank glass nitre material in visible light wave range is approximately 4% (ginseng curve D).Behind the coating film forming liquid, its reflectivity obviously reduces (ginseng curve E, F, G).Identical in soak time, under the identical situation of film forming liquor composition, relatively reflectance curve E (0.8 not ear concentration) and curve F (0.5 not ear concentration) as can be known, when solution concentration is higher, the mass reflex rate of gained film is lower, and promptly overall anti-reflection effect is better in visible light wave range.Especially, in a certain visible light wave range (400-500nm), promptly near the near ultraviolet band district, the refractive index of the curve F that concentration is lower will be lower than curve E on the contrary.Therefore, the selection of film forming liquid actual concentrations also should be decided according to required antireflection wave band, is not to be absolute.Curve G (0.5 not ear concentration) is different with the solution compolision of curve E, F, but soak time is identical.F compares with curve, and the mass reflex rate of curve G is obviously lower, and promptly the overall anti-reflection effect of gained film is better in visible light wave range.This explanation, except that the concentration of film forming liquid, the composition of film forming liquid also directly affects the anti-reflection effect of gained film.
Except that above-mentioned dip coated method, the present invention is volatilized after also can using other similar mode to allow film forming liquid be attached to substrate surface, to reach antireflecting effect equally.These modes comprise method of spin coating, splash rubbing method, embrocate rubbing method etc.
Method of spin coating is to adopt the adjustable high speed rotating instrument of rotating speed to drive base material to make steady high-speed rotation in surface level, film forming liquid drips on the base material from the top, the centrifugal force that utilizes the instrument rotation to be produced is uniformly distributed in substrate surface by film forming liquid, and forms required anti-reflection effect by control film forming liquor concentration, solution compolision, solution amount and rotational speed.The film forming liquor is promptly realized plated film after at room temperature volatilizing fast.This method is simpler, and the film of coating is more even, and film thickness is regulated control by the coefficient of viscosity of rotating speed and film forming liquid.Rotating speed is high more, and coefficient of viscosity is more little, and film is thin more.This method is very high to the utilization factor of film forming liquid, only needs a small amount of (several milliliters) film forming liquid of preparation to be coated with, but can only be used to be coated with the less circular base material of size.
Adopt above-mentioned method of spin coating, because film forming liquid at room temperature can volatilize fast, therefore, the gained film is more even, has effectively overcome the thickness inequality that existing rotary plating method is produced, defectives such as necessary force drying.
The splash rubbing method is similar to spray paint, and after placing base material, instrument that can the utilization activity as shower nozzle, cooperates the base material profile that film forming liquid evenly is sprayed on substrate surface, utilizes the levelling effect of liquid to form one deck homogeneous film.Required anti-reflection effect can be by control film forming liquor concentration, solution compolision, solution amount, and the conjugate solutions evaporation rate is reached again.This method is to the utilization factor height of film forming liquid, can large-area coating film, and also can be to the irregular surface plated film.Film thickness is by controls such as spray volume and solution coefficient of viscosity, solutes contents, but the difficult control of the homogeneity of film.
Embrocating rubbing method is after placing base material, utilize active tool,, film forming liquid is evenly embrocated in substrate surface as anilox roll, and by control film forming liquor concentration, solution compolision, solution amount, the conjugate solutions evaporation rate is reached required anti-reflection effect again.
Wet type rubbing method of the present invention at room temperature can be implemented, and chemical substance directly forms the compound film of tool anti-reflection effect attached to substrate surface behind the solution evaporation, and thermal treatment such as need not toast.Therefore, the present invention is applicable to various base materials, be not suitable for the irregular base material that easily causes the plated film inequality of heat treated material, surface configuration, be not suitable for swinging in the stereo structure base material of plated film in the board as plastics or other, and surface energy instability, the easy base material of demoulding.
The present invention is directly at substrate surface coating chemical agent, omitted many complicated and steps of easily makeing mistakes compared to existing coating technique, volume production stability and yield so can significantly promote.Even with the anti-reflection film thickness that the method makes, behind environmental testing, confirm to pass through tests such as thermal shock, constant temperature, constant humidity, even substrate body is actively little, also be difficult for having the puzzlement of demoulding.
In addition, except the cleaned base material surface, the present invention does not need base material is carried out other particular processing.Required device is succinct, cheap, compares existing coating technique and has saved board expense and human cost significantly.
Claims (7)
1, a kind of coating process of wet type anti-reflective compound film comprises the following steps:
(1) provides and cleans a base material;
(2) provide a film forming liquid, this film forming liquid is formed by being dissolved in the easy volatile solvent in order to film forming compound;
(3) at room temperature base material is soaked into certain hour in the film forming liquid;
(4) make base material break away from film forming liquid with certain speed, this speed control is the i.e. volatilization fully of moment solution that base material leaves film forming liquid liquid level, promptly this finish single thin film coating and need not thermal treatment; And
(5) repeating step (3) and (4) on demand are to finish the required coating number of plies.
2, the coating process of wet type anti-reflective compound film as claimed in claim 1 is characterized in that in the described film forming liquid in order to film forming compound being solid-state fluoride.
3, the coating process of wet type anti-reflective compound film as claimed in claim 1 is characterized in that described step (4) makes base material break away from film forming liquid by the mode of mode that lifts or the sedimentation of film forming liquid liquid level.
4, the coating process of wet type anti-reflective compound film as claimed in claim 3 is characterized in that described base material is positioned in the fixable basket support, and the motor that utilizes the constant speed lifting is soaked in the film forming liquid constant speed with this basket support constant speed again and mentions.
5, the coating process of wet type anti-reflective compound film as claimed in claim 1 is characterized in that, each coating layer uses identical film forming liquid.
6, the coating process of wet type anti-reflective compound film as claimed in claim 1 is characterized in that described base material is an optical base-substrate.
7, the coating process of wet type anti-reflective compound film as claimed in claim 6 is characterized in that described optical base-substrate is glass lens or glass mirror.
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| CNB2004100834620A CN100437152C (en) | 2004-09-30 | 2004-09-30 | Coating method of wet type anti-reflective compound film |
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| CNB2004100834620A CN100437152C (en) | 2004-09-30 | 2004-09-30 | Coating method of wet type anti-reflective compound film |
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| CN100437152C true CN100437152C (en) | 2008-11-26 |
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| CN102381067B (en) * | 2011-08-30 | 2014-02-19 | 福州华映视讯有限公司 | Method for manufacturing cavity and method for manufacturing optical film by using cavity |
| CN103257378B (en) * | 2012-02-21 | 2014-11-26 | 江苏华天通科技有限公司 | Method of manufacturing coated CR39 resin lens |
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| CN1340001A (en) * | 1999-12-28 | 2002-03-13 | Tdk株式会社 | Functional film and method for preparation thereof |
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Patent Citations (11)
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|---|---|---|---|---|
| CN88102016A (en) * | 1987-04-10 | 1988-11-23 | 东芝株式会社 | Method for forming film on outer surface of display screen of cathode ray tube |
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| JP2001261865A (en) * | 2000-03-14 | 2001-09-26 | Nippon Sheet Glass Co Ltd | Resin substrate having antireflection coating, its preparation process, and display member |
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