CN1332799C - Transparent, heat insulated nano multilayer film solidified by ultraviolet radiation - Google Patents
Transparent, heat insulated nano multilayer film solidified by ultraviolet radiation Download PDFInfo
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- CN1332799C CN1332799C CNB2004100170244A CN200410017024A CN1332799C CN 1332799 C CN1332799 C CN 1332799C CN B2004100170244 A CNB2004100170244 A CN B2004100170244A CN 200410017024 A CN200410017024 A CN 200410017024A CN 1332799 C CN1332799 C CN 1332799C
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Abstract
The present invention relates to a transparent and heat insulated nanometer multilayer film used for ultraviolet curing, which is used for the technical field of nanometer optics thin film materials. The present invention adopts a DMD structure. Dielectric alternates with a metal layer which is between two layers of dielectric, wherein the metal of the metal layer is silver which has a layer thickness of 14 to 18 nm, the material of the dielectric is TiO2, the dielectric has a layer thickness of 25 to 36 nm. The present invention can ensure that the good transmissivity of ultraviolet light is maintained, harmful heat of an ultraviolet curing furnace is isolated by reflection. The transparent and heat insulated nanometer multilayer film which is coated on quartz glass for ultraviolet light is positioned between the ultraviolet light and a product to be solidified, and is used for the heat insulation of an ultraviolet curing furnace. The present invention can be used for the replenishment of water cooling and air cooling, and can be used singly to overcome the solidification quality problem caused by temperature rise in an ultraviolet curing process, and ensure the quality stability of solidified products.
Description
Technical field
What the present invention relates to is a kind of nanometer multilayer functional membrane that is used for nanocomposite optical thin-film material technical field, particularly a kind of heat insulation transparent multilayer film of ultra-violet curing that is used for.
Background technology
Ultra-violet curing is as the extensive use in press and liquid crystal display manufacturing of a kind of important operation.Ultra-violet curing promptly utilizes UV (Ultra Violet i.e. ultraviolet ray) irradiation energy to make the glazing process of radical polymerization type esters of acrylic acid paint solidification film forming.Ultraviolet curing has the characteristics of quick curing and low-temperature setting, helps to improve the quality of products, and keeps solid colour, shortens printing time, and air conservation reduces fire hazard and improves operating environment.Solved the adhesion that solvent-borne type glazing paint Yin Wendu, humidity variation cause.Ultraviolet curing lamp mercury lamp generally commonly used and metal halide lamp, industrial production belongs to long wavelength ultraviolet lamp with uviol lamp, and (350nm～450nm), main peak is 365nm.But because problem such as ultraviolet light source can produce a large amount of heats, change 60% general power into infra-red radiation as ultraviolet high-pressure mercury lamps in the use of reality, the surface of the light tube temperature can be raised to 700-800 ℃.The infra-red radiation that comes from the UV fluorescent tube is to produce overheated basic reason, and temperature is too high to be one of critical limitation factor that influences solidification process.Overheated for fear of material, adopt high power lamp and multi-lamp syste in the ultraviolet light polymerization device, generally to take multiple measure to cool off fluorescent tube, reflection lampshade and base material.Way now commonly used has two kinds, one, air cooling, and this method is to use maximum methods now, cost is lower, but air-cooledly causes drift easily; Two, water cooling installs water jacket additional outside fluorescent tube, this method is effective, but cost is higher, and the leakage of water also may take place.
Find by retrieval: United States Patent (USP) U.S.Pat.No.4,563,589, this patent adopts air-cooled in handling the ultra-violet curing cooling, and what saturating ultraviolet window adopted is the quartz glass disc of no plated film.
If add plating multilayer functional membrane in a saturating ultraviolet glass pane side close with ultraviolet source, realize ultraviolet and the reflective infrared heat, so just realized cooling once more.Though as the liquid crystal uv oven air cooling system is arranged, the temperature of uv oven can be up to 80 ℃ sometimes, so very easily cause the protection paster Yin Gaowen heating of liquid crystal and stick together.The heat insulation nano multilayer film that has for this reason prepared saturating ultraviolet at the heat-insulating problem design of the uv oven of liquid crystal display.
Summary of the invention
The objective of the invention is at the deficiencies in the prior art and defective, a kind of transparent heat-insulated nano-multilayer film that is used for ultra-violet curing is provided, make it can guarantee good ultraviolet permeability, simultaneously harmful reflect heat of uv oven is isolated, be plated on the ultraviolet quartz glass, place ultraviolet source and wait to solidify to be used for the heat insulation of uv oven between the part.Can be used as water-cooled or air-cooled replenishing, also can use separately,, guarantee the cured article quality of stability to overcome the curing quality problems that cause because of temperature rise in the ultra-violet curing process.
The present invention is achieved by the following technical solutions, multilayer film of the present invention adopts DMD (dielectrjc/metal/dielectric) sandwich structure, dielectric and metal level replace, in the middle of the two-layer dielectric is metal level, metal is an argent, metallic silver layer thickness is 14～18nm, and dielectric substance is TiO
2, bed thickness 25～36nm.Utilize the transmission theorem of inducing of metal film to realize disappearing anti-anti-reflection.The selection of layers of material is mainly carried out through reaching high infrared external reflection around ultraviolet.The present invention will (ultraviolet light 350～450nm) in has the transmitance of excellence, and the design and the application extension of Metal Substrate composite multilayer membrane arrived the ultra-violet (UV) band to using wave-length coverage when guaranteeing good heat reflection effect.Because the ultraviolet band energy is higher, most of optical materials have the certain absorption effect to it, and therefore to be different from the traditional sense with visible light be the transparent heat mirror of anti-reflection object to the rete coupling of seeking high transmissivity at ultraviolet band.The tradition thermal isolation film is ended ultraviolet band, and is opaque.
The dielectric constant of metal material is a plural number, and its real part has reflected the chromatic dispersion of metal pair light.The dielectric constant that wants to make metal is suitable in broadband very, consider when considering its free electron that bound electron is to the contribution of dielectric function, especially at visible and ultraviolet band around its atomic nucleus.The intrinsic of Ag film absorbs limit at 310nm, and ultraviolet band λ＞310nm that ultra-violet curing uses, this just guaranteed the Ag film this wave band the low absorbability of height reflection, realizing disappearing anti-anti-reflection providing for whole rete near ultraviolet may.And its good properties of infrared reflection early has application in traditional transparent heat-insulated film.Except Ag, absorb less common metal thin-film material at the long wave ultraviolet band and also have Al, the ultraviolet reflectance of Al is best, but the infrared external reflection of Al film particularly 1000～2000nm wave band is relatively poor.So the present invention takes all factors into consideration its ultraviolet and infrared character, select Ag as the core metal layer.
The dielectric substance that is suitable for the DMD of ultraviolet must possess following two conditions: a) using ultraviolet band transparent; B) at this wave band higher refractive index is arranged.The high refraction of ultraviolet commonly used dielectric substance is ZrO
2, its clear area be (300～1200nm), TiO
2Clear area (350～1200nm).ZrO
2The refractive index instability of coating materials.The ultraviolet peak value of most commercial uv cure systems is at the 365nm place, so from the angle TiO of saturating ultraviolet
2Can meet the demands.TiO
2Forbidden band broad, its intrinsic absorb limit at the 350nm place, so long wavelength's near ultraviolet is not enough to excite its electron production band-to-band transition.In 365nm characteristic wave strong point n is arranged
D=2.43 high index of refraction.This just induces transmission that possibility is provided for being implemented in the ultra-violet (UV) band.And employing vacuum evaporation TiO
2Have preferably with the Ag film that the interface combines, use TiO so determine the dielectric coating materials
2
The infrared external reflection of D/M/D multilayer film mainly relies on the thickness of core metal layer to control, but metal level can not be too thick, otherwise, can produce absorption to ultraviolet, make medium induce metal level to produce best transmission simultaneously at the feature ultraviolet band.Traditional transparent heat mirror designs at visible light anti-reflection often, considers the higher limit of its thickness from the angle of metal film Kelvin effect
d
sBe skin depth.With λ=365 nm according to d
s=λ/4 π k
MBring the d that relevant parameter calculates into
sValue is 18.9nm, d
Ag≤ 77.1nm.Obviously, such critical film thickness is irrational.Therefore, it is anti-anti-reflection to realize disappearing at ultraviolet band, and the skin depth of metal level has lost its original meaning.The present invention calculates when using for reference the traditional design computational methods, take all factors into consideration the ultraviolet optics characteristic of metal and dielectric substance and in conjunction with analysis of experiments, according to correlation theory and with λ=365nm is characteristic wavelength, pass through computerized optimization then, determine the optimum thickness of each rete, do further checking by test at last.Determine the TiO of the compound 25～36nm of Ag layer of 14～18nm ranges of thicknesses
2The multilayer film that forms has the saturating preferably anti-infrared characteristic of ultraviolet.Dielectric layer thickness can be symmetrically distributed in the both sides of silverskin or bottom than the thick 2～4nm of top layer.
Ultraviolet heat insulation nano multilayer film of the present invention adopts the method preparation of vacuum evaporation, and substrate glass adopts the quartz glass of ultraviolet.DMD nano-multilayer film of the present invention can be used as the ultraviolet curing equipment window material, is plated in the glass window of ultraviolet source, realizes the secondary cooling of ultra-violet curing, and harmful reflect heat that ultraviolet source sends is isolated.By experimental test, the excellent in optical properties of multilayer film of the present invention, the transmissivity of ultraviolet main peak reaches 81%, and transmissivity reaches 84% near the 384nm, and infrared anti-rate has just surpassed 90% at the 1600nm wave band.
The specific embodiment
Provide following examples to come the present invention is done further statement in conjunction with content of the present invention:
Embodiment 1:
Nano-multilayer film: 25nmTiO
2/ 14nmAg/25nmTiO
2/ G
The rete design: utilizing and induce the transmission correlation theory, is characteristic wavelength with λ=365nm, and actual measurement Ag and TiO
2The optical constant of film is calculated the thickness of each rete of primary election, and carries out the plated film test.Specifically determine the optimum thickness of rete then by computer optimization according to the test feedback.
Its preparation process is as follows: substrate is quartz crystal polishing section 35mm * 20mm * 1mm and Si (111) sheet.Adopt chemistry and ultrasonic wave to clean.Base reservoir temperature is 45 ℃.Vacuum: background vacuum 1 * 10
-2Pa behind ion beam bombardment substrate 15min, is evacuated to 1 * 10 with vacuum again
-3Pa.Raw material and heating source: Ag: purity is 99.9% particle, the heating of molybdenum boat resistance wire; TiO
2: purity is 99.9% particle, the heating of cold-crucible electron gun.Sedimentation rate is 0.3nm/s.
THICKNESS CONTROL: thickness is monitored in real time by quartz oscillation film thickness monitoring instrument in the film preparation process, and accurately measures its thickness with ellipsometer test.
Be somebody's turn to do the optical property index of how transparent heat-insulated nano-multilayer film:
| Membrane structure | Transmissivity T@365nm/% | Transmissivity T@465nm/% | Reflectivity R@1600nm/% |
| 25nmTiO 2/14nmAg /25nmTiO 2 | 78.9 | 80.1 | 81.0 |
Embodiment 2
Nano-multilayer film: 29nmTiO
2/ 15nmAg/33nmTiO
2/ G, preparation technology is with embodiment 1.The optical property index of this nano-multilayer film:
| Membrane structure | Transmissivity T@365nm/% | Transmissivity T@465nm/% | Reflectivity R@1600nm/% |
| 29nmTiO 2/15nmAg /33nmTiO 2 | 81.0 | 80.2 | 82.0 |
Embodiment 3:
Nano-multilayer film: 33nmTiO
2/ 18nmAg/36nmTiO
2/ G, preparation technology are with the optical property index of embodiment 1 this nano-multilayer film:
| Membrane structure | Transmissivity T@365nm/% | Transmissivity T@465nm/% | Reflectivity R@1600nm/% |
| 33nmTiO 2/18nmAg /36nmTiO 2 | 79.8 | 80.3 | 93.0 |
Claims (4)
1, a kind of transparent heat-insulated nano-multilayer film that is used for ultra-violet curing is characterized in that, adopts the DMD sandwich structure, dielectric and metal level replace, and are metal levels in the middle of the two-layer dielectric, and metal is an argent, metallic silver layer thickness is 14～18nm, and dielectric substance is TiO
2, bed thickness 25～36nm.
2, the transparent heat-insulated nano-multilayer film that is used for ultra-violet curing according to claim 1 is characterized in that dielectric layer thickness is symmetrically distributed in the both sides of silverskin, and perhaps bottom is than the thick 2～4nm of top layer.
3, the transparent heat-insulated nano-multilayer film that is used for ultra-violet curing according to claim 1 is characterized in that, the intrinsic of silverskin absorbs limit at 310nm, ultraviolet band λ＞310nm that ultra-violet curing uses, and silverskin has the low absorbability of high reflection at this wave band.
4, the transparent heat-insulated nano-multilayer film that is used for ultra-violet curing according to claim 1 is characterized in that TiO
2The forbidden band is wide, and its intrinsic absorbs limit at the 350nm place, in 365nm characteristic wave strong point n is arranged
D=2.43 high index of refraction.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2004100170244A CN1332799C (en) | 2004-03-18 | 2004-03-18 | Transparent, heat insulated nano multilayer film solidified by ultraviolet radiation |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2004100170244A CN1332799C (en) | 2004-03-18 | 2004-03-18 | Transparent, heat insulated nano multilayer film solidified by ultraviolet radiation |
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| Publication Number | Publication Date |
|---|---|
| CN1562603A CN1562603A (en) | 2005-01-12 |
| CN1332799C true CN1332799C (en) | 2007-08-22 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB2004100170244A Expired - Fee Related CN1332799C (en) | 2004-03-18 | 2004-03-18 | Transparent, heat insulated nano multilayer film solidified by ultraviolet radiation |
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Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112028499B (en) * | 2020-08-21 | 2023-01-24 | 河南理工大学 | Amorphous transparent conductive composite film with CuAg alloy as buffer layer and capable of being prepared at room temperature, and preparation method and application thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4563589A (en) * | 1984-01-09 | 1986-01-07 | Scheffer Herbert D | Ultraviolet curing lamp device |
| CN1417148A (en) * | 2001-10-29 | 2003-05-14 | 李宏强 | Infrared radiation-isolating film material for building glass |
-
2004
- 2004-03-18 CN CNB2004100170244A patent/CN1332799C/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4563589A (en) * | 1984-01-09 | 1986-01-07 | Scheffer Herbert D | Ultraviolet curing lamp device |
| CN1417148A (en) * | 2001-10-29 | 2003-05-14 | 李宏强 | Infrared radiation-isolating film material for building glass |
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| Publication number | Publication date |
|---|---|
| CN1562603A (en) | 2005-01-12 |
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