CN109507764A - A kind of optical filming material and preparation method, optical anti-reflective film - Google Patents

A kind of optical filming material and preparation method, optical anti-reflective film Download PDF

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Publication number
CN109507764A
CN109507764A CN201811424840.5A CN201811424840A CN109507764A CN 109507764 A CN109507764 A CN 109507764A CN 201811424840 A CN201811424840 A CN 201811424840A CN 109507764 A CN109507764 A CN 109507764A
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CN
China
Prior art keywords
titanium
optical
niobium pentaoxide
titanium oxide
filming material
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CN201811424840.5A
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Chinese (zh)
Inventor
秦海波
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Beijing Fuxingkai Photo-Electronic Tech Co Ltd
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Beijing Fuxingkai Photo-Electronic Tech Co Ltd
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Priority to CN201811424840.5A priority Critical patent/CN109507764A/en
Publication of CN109507764A publication Critical patent/CN109507764A/en
Pending legal-status Critical Current

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    • GPHYSICS
    • G02OPTICS
    • G02BOPTICAL ELEMENTS, SYSTEMS OR APPARATUS
    • G02B1/00Optical elements characterised by the material of which they are made; Optical coatings for optical elements
    • G02B1/10Optical coatings produced by application to, or surface treatment of, optical elements
    • G02B1/11Anti-reflection coatings
    • G02B1/113Anti-reflection coatings using inorganic layer materials only
    • G02B1/115Multilayers
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01GCOMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G33/00Compounds of niobium

Abstract

The present invention provides a kind of optical filming material and preparation method thereof, optical anti-reflective film, to solve the problems, such as that the anti-reflection membrane material such as titanium oxide easily forms that spot, intensity is not high to be also easy to produce scratch in the prior art.Optical filming material of the invention, for titanium oxide-niobium pentaoxide bi-unit composite structure or titanium oxide-titanium-niobium pentaoxide tri compound structure, pass through cofiring after the addition niobium pentaoxide in titanium oxide and/or titanium material, form titanium oxide-niobium pentaoxide or titanium oxide-titanium-niobium pentaoxide composite construction, obtain more stable membrane structure, to solve the problems, such as oxygen release during being coated with, simultaneously, intensity of the film strength that titanium oxide-niobium pentaoxide diadactic structure is formed obviously than independent titanium oxide layer is big, prepared anti-reflection film is not likely to produce scratch, longer life expectancy.

Description

A kind of optical filming material and preparation method, optical anti-reflective film
Technical field
The invention belongs to optical material and thin film technique fields, and in particular to a kind of optical filming material and preparation method, Optical anti-reflective film.
Background technique
In an optical imaging system, the natural light for imaging is that can increase imaging definition beneficial to light a bit; Some are harmful lights, can reduce the clarity of imaging.In order to increase the clarity of imaging system, usually by imaging lens or Increase anti-reflection film on the glass of light transmission.German fraunhofer in 1817 has invented plated film and that first has been made is anti-reflection Film.The principle of anti-reflection film is the thin transparent by increasing a quarter for the wavelength that one layer is equivalent to reflected light on optical glass Film, and the two-beam that two surfaces are reflected above and below transparent membrane is made to differ half of wave-path, so that the anti-raw interference of two-beam, To cancel out each other, to reduce reflected light, while increasing transmitted light, improve the clarity of imaging system.In the prior art, anti-reflection Film is widely used in camera lens, eyeglass, various visual windows etc..
In the prior art, the material for being used to prepare anti-reflection film generallys use titanium oxide, and titanium oxide is a kind of high refractive index Optical filming material, application range are very extensive.But titanium oxide can discharge oxygen, make fluctuation vacuum in coating process Larger, film layer easily forms spot;Another aspect titanium oxide intensity is relatively low, and being coated with film layer, easily formation is drawn during use Trace.
Summary of the invention
The embodiment of the present invention easily forms spot, intensity not Gao Yi to solve the anti-reflection membrane material such as titanium oxide in the prior art Scratch is led to the problem of, proposes a kind of optical filming material and preparation method thereof, and plate using the optical filming material The optical anti-reflective film of system.Optical filming material of the invention uses in titanium oxide and/or titanium material after addition niobium pentaoxide Cofiring forms titanium oxide-niobium pentaoxide or titanium oxide-titanium-niobium pentaoxide composite construction, obtains more stable film knot Structure, thus solve the problems, such as oxygen release during being coated with, meanwhile, what titanium oxide-niobium pentaoxide diadactic structure was formed Intensity of the film strength obviously than independent titanium oxide layer is big, and prepared anti-reflection film is not likely to produce scratch, longer life expectancy.
To achieve the goals above, this invention takes following technical solutions.
A kind of optical filming material, the material are titanium oxide-niobium pentaoxide bi-unit composite structure or titanium oxide-titanium- Niobium pentaoxide tri compound structure.
Further, the titanium oxide includes: titanium dioxide, seven oxidation four titaniums, titanium pentoxide, titanium sesquioxide, one Titanium oxide.
Further, the weight ratio in the optical filming material in titanium oxide-niobium pentaoxide bi-unit composite structure is Titanium oxide: niobium pentaoxide=(75~95): (25~5);Titanium oxide-titanium-niobium pentaoxide in the optical filming material Weight ratio in tri compound structure is titanium oxide: titanium: niobium pentaoxide=(70~90): (10~5): (20~5).
The present invention also provides a kind of preparation methods of optical filming material, and described method includes following steps:
Step S1 weighs the titania powder and niobium pentaoxide powder of predetermined weight ratio;
Step S2 after mixing by the titania powder and niobium pentaoxide powder is granulated;
Step S3, will make obtained microparticle/microplate/microlith after material be put into Muffle furnace carried out at 1100~1250 DEG C it is pre- Sintering, and 3~5 hours are kept the temperature, pre-burning microparticle/microplate/microlith is obtained after furnace cooling;
Pre-burning microparticle/microplate/the microlith is put into vacuum drying oven and is sintered at 1400~1600 DEG C by step S4, And 3~6 hours are kept the temperature, the optical filming material is obtained after furnace cooling.
Further, the step S4 further include: be sieved to the optical filming material after furnace cooling.
The present invention also provides a kind of optical anti-reflective film, the anti-reflection film be coated with by optical filming material as described above and At.
The present invention also provides a kind of optical anti-reflective film, the anti-reflection film is by optical filming material preparation side as described above Optical filming material prepared by method is coated with.
As can be seen from the technical scheme provided by the above-mentioned embodiment of the present invention, the embodiment of the present invention in titanium oxide and/or Introduce the optical filming material of suitable niobium pentaoxide manufacture in titanium material, very good solution makes because of pure zirconia titanium material With the problem of spot and the intensity deficiency occurred in the process.
The additional aspect of the present invention and advantage will be set forth in part in the description, these will become from the following description Obviously, or practice through the invention is recognized.
Specific embodiment
Those skilled in the art of the present technique are appreciated that unless expressly stated, singular " one " used herein, " one It is a ", " described " and "the" may also comprise plural form.It is to be further understood that being arranged used in specification of the invention Diction " comprising " refer to that there are the feature, integer, step, operation, element and/or component, but it is not excluded that in the presence of or addition Other one or more features, integer, step, operation, element, component and/or their group.It should be understood that used herein Wording "and/or" includes one or more associated any cells for listing item and all combinations.
Those skilled in the art of the present technique are appreciated that unless otherwise defined, all terms used herein (including technology Term and scientific term) there is meaning identical with the general understanding of those of ordinary skill in fields of the present invention.Also answer It should be appreciated that those terms such as defined in the general dictionary should be understood that have in the context of the prior art The consistent meaning of meaning, and unless defined as here, it will not be explained in an idealized or overly formal meaning.
Below by taking several specific embodiments as an example, explanation that the present invention will be further explained, and each embodiment is not Constitute the restriction to the embodiment of the present invention.
Embodiment 1
A kind of optical filming material is present embodiments provided, the material is titanium dioxide-niobium pentaoxide diadactic structure, Wherein, the ratio of the titanium dioxide and niobium pentaoxide is 75:25, and the material is the particle formed after two kinds of material cofirings Shape diadactic structure material.
The present embodiment additionally provides a kind of preparation method of optical filming material, and described method includes following steps:
Step S101, weighs 75 parts of titania powders and 25 parts of niobium pentaoxide powder are (involved in present specification To all " parts " be parts by weight);
Step S102 after mixing by the titania powder and niobium pentaoxide powder is granulated to obtain micro- Particle;
Step S103, will make the microparticle that is formed after material and be put into Muffle furnace and be pre-sintered at 1250 DEG C, and it is small to keep the temperature 5 When, pre-burning microparticle is obtained after furnace cooling;
The pre-burning microparticle is put into vacuum drying oven and is sintered at 1600 DEG C by step S104, and keeps the temperature 6 hours, with The optical filming material is obtained after furnace is cooling.Further, this step can also include, to sintered optical filming material It is sieved, the sieve of different sieve meshes is selected according to different requirements and microparticle granularity condition.
The present embodiment additionally provides a kind of optical anti-reflective film, optical anti-reflective film institute as prepared by the preparation method It states optical filming material to be coated with, is coated with parameter are as follows: 50 DEG C of substrate temperature, evaporation rate is
Embodiment 2
A kind of optical filming material is present embodiments provided, the material is titanium dioxide-niobium pentaoxide diadactic structure, Wherein, the ratio of the titanium dioxide and niobium pentaoxide is 85:15, and the material is the sheet formed after two kinds of material cofirings Diadactic structure material.
The present embodiment additionally provides a kind of preparation method of optical filming material, and described method includes following steps:
Step S201 weighs 85 parts of titania powders and 15 parts of niobium pentaoxide powder;
Step S202 after mixing by the titania powder and niobium pentaoxide powder is granulated to obtain micro- Piece;
Step S203, will make the microplate that is formed after material and be put into Muffle furnace and be pre-sintered at 1200 DEG C, and it is small to keep the temperature 4 When, pre-burning microplate is obtained after furnace cooling;
The pre-burning powder is put into vacuum drying oven and is sintered at 1500 DEG C by step S204, and keeps the temperature 5 hours, cold with furnace But the optical filming material is obtained afterwards.Further, this step can also include carrying out to sintered optical filming material Sieving, the sieve of different sieve meshes is selected according to different requirements and microplate size condition.
The present embodiment additionally provides a kind of optical anti-reflective film, optical anti-reflective film institute as prepared by the preparation method It states optical filming material to be coated with, is coated with parameter are as follows: 50 DEG C of substrate temperature, evaporation rate is
Embodiment 3
A kind of optical filming material is present embodiments provided, the material is titanium dioxide-niobium pentaoxide diadactic structure, Wherein, the ratio of the titanium dioxide and niobium pentaoxide is 95:5, and the material is the microlith formed after two kinds of material cofirings Shape diadactic structure material.
The present embodiment additionally provides a kind of preparation method of optical filming material, and described method includes following steps:
Step S301 weighs 95 parts of titania powders and 5 parts of niobium pentaoxide powder;
Step S302 after mixing by the titania powder and niobium pentaoxide powder is granulated to obtain micro- Block;
Step S303, will make the microlith that is formed after material and be put into Muffle furnace and be pre-sintered at 1100 DEG C, and it is small to keep the temperature 3 When, pre-burning microlith is obtained after furnace cooling;
The pre-burning microlith is put into vacuum drying oven and is sintered at 1400 DEG C by step S304, and keeps the temperature 3 hours, with furnace The optical filming material is obtained after cooling.Further, this step can also include, to sintered optical filming material into Row sieving, according to different requirements and the sieve of microlith size selection difference sieve mesh.
The present embodiment additionally provides a kind of optical anti-reflective film, optical anti-reflective film institute as prepared by the preparation method It states optical filming material to be coated with, is coated with parameter are as follows: 50 DEG C of substrate temperature, evaporation rate is
Embodiment 4
Present embodiments provide a kind of optical filming material, the material and preparation method and 1 component ratio phase of embodiment Together, the difference is that used binary mixture is seven four titaniums of oxidation and niobium pentaoxide.
The present embodiment additionally provides a kind of preparation method of optical filming material, and described method includes following steps:
Step S401 weighs 75 part of seven four titanium powder of oxidation and 25 parts of niobium pentaoxide powder;
Step S402 aoxidizes four titanium powders and niobium pentaoxide powder after mixing for described seven, is granulated to obtain Microparticle;
Step S403, will make the microparticle that is formed after material and be put into Muffle furnace and be pre-sintered at 1200 DEG C, and it is small to keep the temperature 4 When, pre-burning microparticle is obtained after furnace cooling;
The pre-burning microparticle is put into vacuum drying oven and is sintered at 1600 DEG C by step S404, and keeps the temperature 5 hours, with The optical filming material is obtained after furnace is cooling.Further, this step can also include, to sintered optical filming material It is sieved, the sieve of different sieve meshes is selected according to different requirements and microparticle granularity condition.
The present embodiment additionally provides a kind of optical anti-reflective film, optical anti-reflective film institute as prepared by the preparation method It states optical filming material to be coated with, is coated with parameter are as follows: 50 DEG C of substrate temperature, evaporation rate is
Embodiment 5
Present embodiments provide a kind of optical filming material, the material and preparation method and 2 component ratio phase of embodiment Together, the difference is that used binary mixture is titanium pentoxide and niobium pentaoxide.
The present embodiment additionally provides a kind of preparation method of optical filming material, and described method includes following steps:
Step S501 weighs 85 parts of titanium pentoxide powder and 15 parts of niobium pentaoxide powder;
Step S502 after mixing by the titanium pentoxide powder and niobium pentaoxide powder is granulated to obtain Microplate;
Step S503, will make the microplate that is formed after material and be put into Muffle furnace and be pre-sintered at 1150 DEG C, and it is small to keep the temperature 5 When, pre-burning microplate is obtained after furnace cooling;
The pre-burning microplate is put into vacuum drying oven and is sintered at 1500 DEG C by step S504, and keeps the temperature 6 hours, with furnace The optical filming material is obtained after cooling.Further, this step can also include, to sintered optical filming material into Row sieving, the sieve of different sieve meshes is selected according to different requirements and microplate size condition.
The present embodiment additionally provides a kind of optical anti-reflective film, optical anti-reflective film institute as prepared by the preparation method It states optical filming material to be coated with, is coated with parameter are as follows: 50 DEG C of substrate temperature, evaporation rate is
Embodiment 6
Present embodiments provide a kind of optical filming material, the material and preparation method and 3 component ratio phase of embodiment Together, the difference is that used binary mixture is titanium sesquioxide and niobium pentaoxide.
The present embodiment additionally provides a kind of preparation method of optical filming material, and described method includes following steps:
Step S601 weighs 95 parts of titanium sesquioxide powder and 5 parts of niobium pentaoxide powder;
Step S602 after mixing by the titanium sesquioxide powder and niobium pentaoxide powder is granulated to obtain Microlith;
Step S603, will make the microlith that is formed after material and be put into Muffle furnace and be pre-sintered at 1050 DEG C, and it is small to keep the temperature 4 When, pre-burning microlith is obtained after furnace cooling;
The pre-burning microlith is put into vacuum drying oven and is sintered at 1450 DEG C by step S604, and keeps the temperature 4 hours, with furnace The optical filming material is obtained after cooling.Further, this step can also include, to sintered optical filming material into Row sieving, the sieve of different sieve meshes is selected according to different requirements and microlith size condition.
The present embodiment additionally provides a kind of optical anti-reflective film, optical anti-reflective film institute as prepared by the preparation method It states optical filming material to be coated with, is coated with parameter are as follows: 50 DEG C of substrate temperature, evaporation rate is
Embodiment 7
Present embodiments provide a kind of optical filming material, the material and preparation method and 2 component ratio phase of embodiment Together, the difference is that used binary mixture is titanium monoxide and niobium pentaoxide.
The present embodiment additionally provides a kind of preparation method of optical filming material, and described method includes following steps:
Step S701 weighs 85 parts of titanium monoxide powder and 15 parts of niobium pentaoxide powder;
Step S702 after mixing by the titanium monoxide powder and niobium pentaoxide powder is granulated to obtain micro- Piece;
Step S703, will make the microplate that is formed after material and be put into Muffle furnace and be pre-sintered at 1150 DEG C, and it is small to keep the temperature 5 When, pre-burning microplate is obtained after furnace cooling;
The pre-burning microplate is put into vacuum drying oven and is sintered at 1550 DEG C by step S704, and keeps the temperature 5 hours, with furnace The optical filming material is obtained after cooling.Further, this step can also include, to sintered optical filming material into Row sieving, the sieve of different sieve meshes is selected according to different requirements and microplate size condition.
The present embodiment additionally provides a kind of optical anti-reflective film, optical anti-reflective film institute as prepared by the preparation method It states optical filming material to be coated with, is coated with parameter are as follows: 50 DEG C of substrate temperature, evaporation rate is
Embodiment 8
A kind of optical filming material is present embodiments provided, the material is titanium dioxide-titanium valve-niobium pentaoxide ternary Structure, wherein the titanium dioxide, titanium valve, niobium pentaoxide ratio be 75:5:20, the material be three kinds of material cofirings The graininess ternary structural material formed afterwards.
The present embodiment additionally provides a kind of preparation method of optical filming material, and described method includes following steps:
Step S801 weighs 75 parts of titania powders, 5 parts of titanium powders, 20 parts of niobium pentaoxide powder;
Step S802 after mixing by the titania powder, titanium valve powder and niobium pentaoxide powder is made Grain obtains microparticle;
Step S803, will make the particle that is formed after material and be put into Muffle furnace and be pre-sintered at 1100 DEG C, and it is small to keep the temperature 4 When, pre-burning particle is obtained after furnace cooling;
The pre-burning particle is put into vacuum drying oven and is sintered at 1500 DEG C by step S804, and keeps the temperature 6 hours, with furnace The optical filming material is obtained after cooling.Further, this step can also include, to sintered optical filming material into Row sieving, the sieve of different sieve meshes is selected according to different requirements and grain graininess condition.
The present embodiment additionally provides a kind of optical anti-reflective film, optical anti-reflective film institute as prepared by the preparation method It states optical filming material to be coated with, is coated with parameter are as follows: 50 DEG C of substrate temperature, evaporation rate is
The optical anti-reflective film being coated with to the optical filming material in above-mentioned implementation 1 to 8 is tested, as a result such as 1 institute of table Show.
Table 1
By above-mentioned several experiments, the optics of suitable niobium pentaoxide manufacture is introduced in titanium oxide and/or titanium material Coating Materials, very good solution is because of the pure zirconia titanium material spot occurred in use and the problem of intensity deficiency.
The foregoing is only a preferred embodiment of the present invention, but scope of protection of the present invention is not limited thereto, In the technical scope disclosed by the present invention, any changes or substitutions that can be easily thought of by anyone skilled in the art, It should be covered by the protection scope of the present invention.Therefore, protection scope of the present invention should be with scope of protection of the claims Subject to.It should be pointed out that for those skilled in the art, in the premise for not departing from principle of the present invention Under, several improvements and modifications can also be made, these modifications and embellishments should also be considered as the scope of protection of the present invention.

Claims (7)

1. a kind of optical filming material, which is characterized in that the material is titanium oxide-niobium pentaoxide bi-unit composite structure or oxygen Change titanium-titanium-niobium pentaoxide tri compound structure.
2. optical filming material according to claim 1, which is characterized in that the titanium oxide includes: titanium dioxide, seven oxygen Change four titaniums, titanium pentoxide, titanium sesquioxide, titanium monoxide.
3. optical filming material according to claim 1, which is characterized in that titanium oxide-five in the optical filming material Aoxidizing the weight ratio in two niobium bi-unit composite structures is titanium oxide: niobium pentaoxide=(75~95): (25~5);The optics The weight ratio in titanium oxide-titanium-niobium pentaoxide tri compound structure in Coating Materials is titanium oxide: titanium: niobium pentaoxide =(70~90): (10~5): (20~5).
4. a kind of preparation method of optical filming material, which is characterized in that described method includes following steps:
Step S1 weighs the titania powder and/or titanium powder and niobium pentaoxide powder of predetermined weight ratio;
Step S2 after mixing by the titania powder and/or titanium powder and niobium pentaoxide powder is granulated;
Step S3 will make the microparticle/microplate/microlith obtained after material and be put into Muffle furnace in 1100~1250 DEG C of progress pre-burnings Knot, and 3~5 hours are kept the temperature, pre-burning microparticle/microplate/microlith is obtained after furnace cooling;
Pre-burning microparticle/microplate/the microlith is put into vacuum drying oven and is sintered at 1400~1600 DEG C, and protected by step S4 Temperature 3~6 hours, obtains the optical filming material after furnace cooling.
5. the preparation method of optical filming material according to claim 4, which is characterized in that the step S4 further include: It is sieved to the optical filming material after furnace cooling.
6. a kind of optical anti-reflective film, which is characterized in that the anti-reflection film is by the described in any item optical coatings of claims 1 to 3 Material is coated with.
7. a kind of optical anti-reflective film, which is characterized in that the anti-reflection film is by optical filming material system described in claim 4 or 5 Optical filming material prepared by Preparation Method is coated with.
CN201811424840.5A 2018-11-27 2018-11-27 A kind of optical filming material and preparation method, optical anti-reflective film Pending CN109507764A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110456427A (en) * 2019-08-15 2019-11-15 北京富兴凯永兴光电技术有限公司 Low-refraction optical filming material and its application
CN112552045A (en) * 2020-12-28 2021-03-26 海宁拓材科技股份有限公司 Low-valence zirconia optical coating material and preparation method thereof

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CN102365385A (en) * 2009-03-27 2012-02-29 吉坤日矿日石金属株式会社 Ti-Nb oxide sintered body sputtering target, Ti-Nb oxide thin film, and method for producing the thin film
CN102931285A (en) * 2012-11-20 2013-02-13 蚌埠玻璃工业设计研究院 Method for preparing niobium-doped titanium dioxide transparent conducting film
CN105112850A (en) * 2015-09-09 2015-12-02 福建阿石创新材料股份有限公司 Preparation method for titanium monoxide for optical evaporation
CN105924168A (en) * 2016-05-09 2016-09-07 中科院微电子研究所昆山分所 Preparation method of TiO2-doped ZnNb2O6 ceramic target material

Patent Citations (4)

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Publication number Priority date Publication date Assignee Title
CN102365385A (en) * 2009-03-27 2012-02-29 吉坤日矿日石金属株式会社 Ti-Nb oxide sintered body sputtering target, Ti-Nb oxide thin film, and method for producing the thin film
CN102931285A (en) * 2012-11-20 2013-02-13 蚌埠玻璃工业设计研究院 Method for preparing niobium-doped titanium dioxide transparent conducting film
CN105112850A (en) * 2015-09-09 2015-12-02 福建阿石创新材料股份有限公司 Preparation method for titanium monoxide for optical evaporation
CN105924168A (en) * 2016-05-09 2016-09-07 中科院微电子研究所昆山分所 Preparation method of TiO2-doped ZnNb2O6 ceramic target material

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110456427A (en) * 2019-08-15 2019-11-15 北京富兴凯永兴光电技术有限公司 Low-refraction optical filming material and its application
CN112552045A (en) * 2020-12-28 2021-03-26 海宁拓材科技股份有限公司 Low-valence zirconia optical coating material and preparation method thereof

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Application publication date: 20190322