CN109503149A - A kind of high refractive index optical filming material and preparation method, optical anti-reflective film - Google Patents
A kind of high refractive index optical filming material and preparation method, optical anti-reflective film Download PDFInfo
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- CN109503149A CN109503149A CN201811431803.7A CN201811431803A CN109503149A CN 109503149 A CN109503149 A CN 109503149A CN 201811431803 A CN201811431803 A CN 201811431803A CN 109503149 A CN109503149 A CN 109503149A
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- Prior art keywords
- optical
- filming material
- aluminum oxide
- titanium
- optical filming
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/46—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on titanium oxides or titanates
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3217—Aluminum oxide or oxide forming salts thereof, e.g. bauxite, alpha-alumina
Abstract
The present invention provides a kind of high refractive index 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-aluminum oxide bi-unit composite structure, pass through cofiring after the addition aluminum oxide in raw titanium oxide material, titanium oxide-aluminum oxide composite construction is formed, more stable membrane structure is obtained, to solve the problems, such as oxygen release during being coated with, simultaneously, intensity of the film strength that titanium oxide-aluminum oxide diadactic structure is formed obviously than independent titanium oxide layer is big, and 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 high refractive index 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 clearly beneficial to light a bit
Degree；Some are harmful lights, can reduce the clarity of imaging.In order to increase the clarity of imaging system, usually by imaging lens
Increase anti-reflection film on head or the glass of light transmission.German fraunhofer has invented plated film and first has been made within 1817
Anti-reflection film.The principle of anti-reflection film is by increasing by one layer of a quarter for being equivalent to the wavelength of reflected light on optical glass
Transparent membrane, and the two-beam that two surfaces are reflected above and below transparent membrane is made to differ half of wave-path, so that two-beam is anti-
Raw interference, to cancel out each other, to reduce reflected light, while increasing transmitted light, improves the clarity of imaging system.Existing skill
In 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 in coating process, make vacuum degree wave
Move larger, film layer easily forms spot；Another aspect titanium oxide intensity is relatively low, is coated with film layer easy shape during use
At scratch.
Summary of the invention
Easily to form spot, intensity not high in order to solve the anti-reflection membrane material such as titanium oxide in the prior art for the embodiment of the present invention
The problem of being also easy to produce scratch proposes a kind of optical filming material and preparation method thereof, and uses the optical filming material
The optical anti-reflective film being coated with.Optical filming material of the invention use in raw titanium oxide material be added aluminum oxide after cofiring,
Titanium oxide-aluminum oxide composite construction is formed, more stable membrane structure is obtained, to solve during being coated with
Oxygen discharges problem, meanwhile, the film strength that titanium oxide-aluminum oxide diadactic structure is formed is obviously than independent oxidation titanium film
The intensity of 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-aluminum oxide bi-unit composite 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-aluminum oxide bi-unit composite structure is
Titanium oxide: aluminum oxide=(75~95): (25~5).
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 aluminum oxide powder of predetermined weight ratio；
Step S2 after mixing by the titania powder and aluminum oxide 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
It is pre-sintered, and keeps the temperature 3~5 hours, 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 is coated with by optical filming material as described above
It forms.
The present invention also provides a kind of optical anti-reflective film, the anti-reflection film is prepared by optical filming material 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 aluminum oxide manufacture in titanium material, very good solution exists because of pure zirconia titanium material
The problem of spot and the intensity deficiency occurred in use process.
The additional aspect of the present invention and advantage will be set forth in part in the description, these will from the following description
Become obvious, 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 will not be explained in an idealized or overly formal meaning and unless defined as here.
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 titania-alumina binary knot
Structure, wherein the ratio of the titanium dioxide and aluminum oxide is 75:25, and the material is to be formed after two kinds of material cofirings
Graininess 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 aluminum oxide powder are (involved in present specification
To all " parts " be parts by weight)；
Step S102 after mixing by the titania powder and aluminum oxide 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 keep the temperature 5
Hour, 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 optics plating membrane material
Material is sieved, according to different requirements and the sieve of microparticle granularity selection difference sieve mesh.
The present embodiment additionally provides a kind of optical anti-reflective film, and the optical anti-reflective film is as prepared by the preparation method
The optical filming material is coated with, and 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 titania-alumina binary knot
Structure, wherein the ratio of the titanium dioxide and aluminum oxide is 85:15, and the material is to be formed after two kinds of material cofirings
Sheet 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 aluminum oxide powder；
Step S202 after mixing by the titania powder and aluminum oxide 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 microplate is put into vacuum drying oven and is sintered at 1500 DEG C by step S204, and keeps the temperature 5 hours, with furnace
The optical filming material is obtained after cooling.Further, this step can also include being sieved to sintered powder,
According to different requirements and the sieve of microplate size selection difference sieve mesh.
The present embodiment additionally provides a kind of optical anti-reflective film, and the optical anti-reflective film is as prepared by the preparation method
The optical filming material is coated with, and 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 titania-alumina binary knot
Structure, wherein the ratio of the titanium dioxide and aluminum oxide is 95:5, and the material is to be formed after two kinds of material cofirings
Microlith 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 aluminum oxide powder；
Step S302 after mixing by the titania powder and aluminum oxide 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
It is sieved, 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, and the optical anti-reflective film is as prepared by the preparation method
The optical filming material is coated with, and 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 aluminum oxide.
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 aluminum oxide powder；
Step S402 aoxidizes four titanium powders and aluminum oxide 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 keep the temperature 4
Hour, 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 optics plating membrane material
Material is sieved, and the sieve of different sieve meshes is selected according to different requirements and starting powder condition.
The present embodiment additionally provides a kind of optical anti-reflective film, and the optical anti-reflective film is as prepared by the preparation method
The optical filming material is coated with, and 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 aluminum oxide.
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 aluminum oxide powder；
Step S502 after mixing by the titanium pentoxide powder and aluminum oxide 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
It is sieved, according to different requirements and the sieve of microplate size selection difference sieve mesh.
The present embodiment additionally provides a kind of optical anti-reflective film, and the optical anti-reflective film is as prepared by the preparation method
The optical filming material is coated with, and 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 aluminum oxide.
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 aluminum oxide powder；
Step S602 after mixing by the titanium sesquioxide powder and aluminum oxide 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
It is sieved, 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, and the optical anti-reflective film is as prepared by the preparation method
The optical filming material is coated with, and 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 aluminum oxide.
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 aluminum oxide powder；
Step S702 after mixing by the titanium monoxide powder and aluminum oxide 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
It is sieved, according to different requirements and the sieve of microplate size selection difference sieve mesh.
The present embodiment additionally provides a kind of optical anti-reflective film, and the optical anti-reflective film is as prepared by the preparation method
The optical filming material is coated with, and 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 7 is tested, as a result such as 1 institute of table
Show.
Table 1
By above-mentioned several experiments, the optics of suitable aluminum oxide 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 protection scope of the present invention be not limited to
This, anyone skilled in the art in the technical scope disclosed by the present invention, the variation that can readily occur in or replaces
It changes, should be covered by the protection scope of the present invention.Therefore, protection scope of the present invention should be with the protection of claim
Subject to range.It should be pointed out that for those skilled in the art, not departing from principle of the present invention
Under the premise of, 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-aluminum oxide bi-unit composite 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-three in the optical filming material
Weight ratio in Al 2 O bi-unit composite structure is titanium oxide: aluminum oxide=(75~95): (25~5).
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 aluminum oxide powder of predetermined weight ratio；
Step S2 after mixing by the titania powder and aluminum oxide 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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| CN201811431803.7A CN109503149A (en) | 2018-11-27 | 2018-11-27 | A kind of high refractive index optical filming material and preparation method, optical anti-reflective film |
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| CN201811431803.7A CN109503149A (en) | 2018-11-27 | 2018-11-27 | A kind of high refractive index optical filming material and preparation method, optical anti-reflective film |
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Cited By (4)
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|---|---|---|---|---|
| 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 |
| CN114133226A (en) * | 2021-12-30 | 2022-03-04 | 苏州晶生新材料有限公司 | Optical coating substrate and using method thereof |
| CN115057699A (en) * | 2022-06-28 | 2022-09-16 | 江苏瞳芯光学科技有限公司 | Low-stress high-refractive-index film, material and preparation method |
| CN116751050A (en) * | 2023-05-31 | 2023-09-15 | 有研资源环境技术研究院(北京)有限公司 | Coating material for antireflection film, preparation method and application thereof |
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| CN115057699A (en) * | 2022-06-28 | 2022-09-16 | 江苏瞳芯光学科技有限公司 | Low-stress high-refractive-index film, material and preparation method |
| CN116751050A (en) * | 2023-05-31 | 2023-09-15 | 有研资源环境技术研究院(北京)有限公司 | Coating material for antireflection film, preparation method and application thereof |
| CN116751050B (en) * | 2023-05-31 | 2024-01-02 | 有研资源环境技术研究院(北京)有限公司 | Coating material for antireflection film, preparation method and application thereof |
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