CN104557039B - Intermediate-refraction index evaporation coating material, as well as preparation technique and application thereof - Google Patents
Intermediate-refraction index evaporation coating material, as well as preparation technique and application thereof Download PDFInfo
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- CN104557039B CN104557039B CN201410815306.2A CN201410815306A CN104557039B CN 104557039 B CN104557039 B CN 104557039B CN 201410815306 A CN201410815306 A CN 201410815306A CN 104557039 B CN104557039 B CN 104557039B
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Abstract
The invention provides an intermediate-refraction index evaporation coating material, as well as a preparation technique and application thereof. The material comprises lanthanum oxide, aluminium oxide, silicon dioxide and an 8% polyvinyl alcohol solution with the mass ratio of 30:20:1:13. The preparation technique comprises the steps of mixing reaction, pressure molding, high-temperature sintering and the like. According to the preparation technique which adopts the evaporation coating material to prepare an evaporation coating film, a vacuum evaporation coating machine in the type of Nanguang ZZS600 is selected, a series of coating parameters are set up for carrying out evaporation coating on the evaporation coating material to obtain a single-layer film. The evaporation coating material, the preparation technique and application thereof have the advantages that the specific single-layer film with the refraction index of 1.75 can be prepared, the evaporation coating material has good stability, is stable in use for preparing multi-layer films, and is an ideal intermediate-refraction index evaporation coating material.
Description
Technical field
The present invention relates to a kind of middle refractive index structural evaporation coating film material and its preparation technology, and refractive index evaporation plating in utilizing
The technique that membrane material prepares monofilm.
Background technology
Initial anti-reflection film, it is mainly plates monolayer low refractive index film on optical substrate material, using the low refraction of material
The effect that rate is anti-reflection enables the transmitance of base material to be lifted, and this thin film can be such that the transmitance of base material carries from 96%
Rise to 98.5% or so.
The process of contemporary optics eyeglass, puts forward higher requirement to anti-reflection effect, the preparation of anti-reflection film, by original list
One refractive index, basic, normal, high various refractive indexs till now are used alternatingly, and using the effect of optical interference, the reflection of substrate light are subtracted
As little as minimum, its increasingly perfect technique, the making to optical filming material is put forward higher requirement.
The content of the invention
One of the technical problem to be solved in the present invention, is to provide a kind of middle refractive index structural evaporation coating film material.
The present invention is realized in one of above-mentioned technical problem：A kind of middle refractive index structural evaporation coating film material, including quality
Than for 30：20：1 lanthana, aluminium sesquioxide and silicon dioxide.
Further, also including 8% polyvinyl alcohol water solution, and the polyvinyl alcohol water solution of mass ratio 8%：Silicon dioxide=
13：1.
The two of the technical problem to be solved in the present invention, are to provide a kind of system of described middle refractive index structural evaporation coating film material
Standby technique.
The present invention is realized in the twos' of above-mentioned technical problem：A kind of system of described middle refractive index structural evaporation coating film material
Standby technique, its operational approach is as follows：
(1) batch mixing reaction：It is 30 by mass ratio：20：1：13 lanthana, aluminium sesquioxide, silicon dioxide and 8% poly- second
Enol aqueous solution is uniform, is placed in closed reactor and reacts at least 8h, obtains reactant；
(2) it is compressing：Reactant is pressed using dry powder prilling machine, then screen cloth sieves；
(3) high temperature sintering：From 1700 DEG C of Si-Mo rod high temperature atmosphere sintering furnaces and alumina crucible to after (2) are processed
Reactant carry out high temperature sintering, obtain final product product；Wherein, the temperature curve of high temperature sintering is as follows：
0-1000 DEG C, heating rate is 1.5-3 DEG C/min；
1000-1500 DEG C, 0.7-1.5 DEG C of heating rate/min；
1500 DEG C, it is incubated 4-6h；
Power-off, Temperature fall.
The three of the technical problem to be solved in the present invention, are to provide a kind of described middle refractive index structural evaporation coating film material to prepare
The technique of monofilm.
The present invention is realized in the threes' of above-mentioned technical problem：It is prepared by a kind of described middle refractive index structural evaporation coating film material
The technique of evaporation coating, from southern light ZZS600 type vacuum evaporating coating machines, is carried out to the middle refractive index structural evaporation coating film material
Evaporation coating is to obtain monofilm, and filming parameter is as follows：
From substrate：80 × 80 × 0.3mm of corning glass
Plated film initial depression：3.0×10-3pa
Oxygenation flow：4sccm
DP temperature：260℃
Heating-up temperature：300℃
Evaporation rate：2A/s
Spot size：X=20%, y=20%
Film thickness：500nm.
Preferably, the refractive index of the monofilm is 1.75.
It is an advantage of the current invention that：The monofilm that specific refractive index is 1.75, middle refractive index evaporation coating can be prepared
Material has good stability, and it is stable used in the preparation of multilayer film, is a kind of preferably middle refractive index evaporation coating
Material.
Specific embodiment
A kind of middle refractive index structural evaporation coating film material, including mass ratio is 30：20：1：13 lanthana, aluminium sesquioxide, two
Silicon oxide and 8% polyvinyl alcohol water solution.The refractive index of monofilm is by obtained in the middle refractive index structural evaporation coating film material
1.75。
Wherein, lanthana La2O3：Purity more than 99.9%, 10-30 μm of meso-position radius.
Aluminium sesquioxide Al2O3：Purity more than 99.99%, 0.5-1.5 μm of meso-position radius.
Silicon dioxide SiO2：Purity more than 99.95,3-8 μm of meso-position radius.
The preparation technology of the middle refractive index structural evaporation coating film material, its operational approach is as follows：
(1) batch mixing reaction：It is 30 by mass ratio：20：1：13 lanthana, aluminium sesquioxide, silicon dioxide and 8% poly- second
Enol aqueous solution is uniform, is placed in closed reactor and reacts at least 8h, obtains reactant；Lanthana can occur with moisture
Violent exothermic reaction.
(2) it is compressing：Reactant is pressed using dry powder prilling machine, and the reactant granular size of molding
For 1.5-3.5mm, then screen cloth sieves；
(3) high temperature sintering：From 1700 DEG C of Si-Mo rod high temperature atmosphere sintering furnaces and alumina crucible, (selection of container, can
Reactant is set to pollute from other materials or react, it is ensured that the product purity after sintering, is that the product stability of later stage plated film is carried
For ensureing) high temperature sintering is carried out to the reactant after (2) are processed, obtain middle refractive index structural evaporation coating film material.Wherein, high temperature
The temperature curve of sintering is as follows：
0-1000 DEG C, heating rate is 1.5-3 DEG C/min；
1000-1500 DEG C, 0.7-1.5 DEG C of heating rate/min；
1500 DEG C, insulation 4-6h (each material fills gap each other, and covalent bond, ionic bond rupture and combine again in structure,
Form stable product)；
Power-off, Temperature fall.
From southern light ZZS600 type vacuum evaporating coating machines, plated film is carried out to the middle refractive index structural evaporation coating film material of the present invention
Verification, refractive index verification is carried out from Japanese Shimadzu UV2550 spectrophotometer to obtained monofilm.
Wherein, filming parameter is as follows：
Type：Southern light ZZS600 type vacuum evaporating coating machines
From substrate：80 × 80 × 0.3mm of corning glass
Plated film initial depression：3.0×10-3pa
Oxygenation flow：4sccm
DP temperature：260℃
Heating-up temperature：300℃
Evaporation rate：2A/s
Spot size：X=20%, y=20%
Film thickness：500nm.
With the obtained monofilm of Shimadzu UV2550 spectrophotometer test, Essential Macleod softwares are simulated described
The refractive index of monofilm is 1.75, and stable refractive index value can be reached under the conditions of above-mentioned filming parameter, therefore the present invention
Middle refractive index structural evaporation coating film material be applied to the use of current optical monolayer film and multilayer film.
At present high permeability optical monolayer film is mainly used in the optics such as optical microscope, projector, photographing unit, video camera
The use of electronics field, especially Powerful Light Microscope and associated components to multi-layered antireflection coating have it is very high will
Ask, the middle refractive index structural evaporation coating film material of the present invention is not only well combined with low-refraction Coating Materials MgF2, SiO2 etc.,
It is well combined with the high index of refraction Coating Materials such as zirconium oxide, lanthanium titanate, it is stable used in the preparation of multilayer film, it is a kind of preferable
Middle refractive index structural evaporation coating film material.
The present invention is mutually filled out using each single property of lanthana, aluminium sesquioxide, silicon dioxide, material microscopic gaps
Fill, be configured to the middle refractive index structural evaporation coating film material of the mutual supplement with each other's advantages of perfect performance, its good stability makes for later stage plated film
With laying the first stone, it can provide the monofilm that specific refractive index is 1.75, also be the evaporation of the more excellent properties of post-production
Coating Materials provides Process ba- sis.
Claims (2)
1. a kind of middle refractive index structural evaporation coating film material, it is characterised in that：It is 30 including mass ratio：20：1 lanthana, three oxidations
Two aluminum and silicon dioxide；Also include 8% polyvinyl alcohol water solution, and the polyvinyl alcohol water solution of mass ratio 8%：Silicon dioxide=
13：1；
The meso-position radius of the silicon dioxide are 3-8 μm.
2. it is a kind of it is as claimed in claim 1 in refractive index structural evaporation coating film material preparation technology, it is characterised in that：Its operation side
Method is as follows：
(1) batch mixing reaction：It is 30 by mass ratio：20：1：13 lanthana, aluminium sesquioxide, silicon dioxide and 8% polyvinyl alcohol
Aqueous solution is uniform, is placed in closed reactor and reacts at least 8h, obtains reactant, and the reaction is that lanthana and water are sent out
Raw exothermic reaction；
(2) it is compressing：Reactant is pressed using dry powder prilling machine, then screen cloth sieves；
(3) high temperature sintering：From 1700 DEG C of Si-Mo rod high temperature atmosphere sintering furnaces and alumina crucible to anti-after (2) are processed
Answer thing to carry out high temperature sintering, obtain final product product；Wherein, the temperature curve of high temperature sintering is as follows：
0-1000 DEG C, heating rate is 1.5-3 DEG C/min；
1000-1500 DEG C, 0.7-1.5 DEG C of heating rate/min；
1500 DEG C, it is incubated 4-6h；
Power-off, Temperature fall.
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| CN106019417A (en) * | 2016-08-08 | 2016-10-12 | 北京富兴凯永兴光电技术有限公司 | Low-refractive-index optical coating material |
| CN110713382A (en) * | 2019-10-24 | 2020-01-21 | 福建阿石创新材料股份有限公司 | Coating material and preparation method and application thereof |
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| DE4219817A1 (en) * | 1992-06-17 | 1993-12-23 | Merck Patent Gmbh | Evaporation material for the production of medium refractive optical layers |
| CN100532629C (en) * | 2007-07-09 | 2009-08-26 | 昆山光铭光电子元件有限公司 | Method for preparing premelting lanthanum titanate crystalloid steam plating material |
| CN100549216C (en) * | 2008-05-28 | 2009-10-14 | 昆山光铭光电子元件有限公司 | Crystal qualitative SiO 2-Al 2O 3The preparation method of mixed oxide deposition material |
| CN101363920B (en) * | 2008-09-18 | 2010-06-02 | 北京有色金属研究总院 | Vaporizing material for medium refractive index optical film and manufacturing method thereof |
| DE102009034532A1 (en) * | 2009-07-23 | 2011-02-03 | Msg Lithoglas Ag | Process for producing a structured coating on a substrate, coated substrate and semifinished product with a coated substrate |
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