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 PDFInfo
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- 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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- titanium
- optical
- niobium pentaoxide
- titanium oxide
- filming material
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- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B1/00—Optical elements characterised by the material of which they are made; Optical coatings for optical elements
- G02B1/10—Optical coatings produced by application to, or surface treatment of, optical elements
- G02B1/11—Anti-reflection coatings
- G02B1/113—Anti-reflection coatings using inorganic layer materials only
- G02B1/115—Multilayers
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G33/00—Compounds of niobium
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- Inorganic Chemistry (AREA)
- Organic Chemistry (AREA)
- Physics & Mathematics (AREA)
- General Physics & Mathematics (AREA)
- Optics & Photonics (AREA)
- Optical Elements Other Than Lenses (AREA)
- Compositions Of Oxide Ceramics (AREA)
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
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.
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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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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 |
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