CN115057699A - Low-stress high-refractive-index film, material and preparation method - Google Patents

Low-stress high-refractive-index film, material and preparation method Download PDF

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CN115057699A
CN115057699A CN202210749238.9A CN202210749238A CN115057699A CN 115057699 A CN115057699 A CN 115057699A CN 202210749238 A CN202210749238 A CN 202210749238A CN 115057699 A CN115057699 A CN 115057699A
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low
refractive
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titanium dioxide
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高建秋
梁海亮
徐小彬
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Jiangsu Tongxin Optical Technology Co ltd
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    • 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
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    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
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    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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    • 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
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
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    • C04B2235/5436—Particle size related information expressed by the size of the particles or aggregates thereof micrometer sized, i.e. from 1 to 100 micron
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    • C04B2235/5418—Particle size related information expressed by the size of the particles or aggregates thereof
    • C04B2235/5445—Particle size related information expressed by the size of the particles or aggregates thereof submicron sized, i.e. from 0,1 to 1 micron
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
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Abstract

The invention belongs to the technical field of mixed oxides, and particularly relates to a low-stress high-refractive-index film, a low-stress high-refractive-index material and a preparation method of the low-stress high-refractive-index film. It has solved defects such as prior art fracture. The preparation method of the low-stress high-refractive-index film material comprises the following steps: s1, ball milling to prepare powder; s2, mixing and bonding; s3, standing at constant temperature and constant humidity; and S4, melting. This application advantage: the internal tensile stress performance of the material is improved, the defects that the single Ti3O5 is soft and crisp in texture and the internal stress form is compressive stress are overcome, and the problem that the Ti3O5 film is easy to crack due to the fluctuation of environmental temperature and the absorption of water in the air by the film layer in the long-term use is fundamentally solved.

Description

Low-stress high-refractive-index film, material and preparation method
Technical Field
The invention belongs to the technical field of mixed oxides, and particularly relates to a low-stress high-refractive-index film, a low-stress high-refractive-index material and a preparation method of the low-stress high-refractive-index film.
Background
Ion source assist materials, which require materials with lower stress, and higher refractive indices. At present, the traditional single Ti3O5 has the defects of soft and crisp texture and compressive stress in the form of internal stress, and is easy to crack due to the fluctuation of environmental temperature and the moisture absorption of a film layer in the air in long-term use.
Disclosure of Invention
The present invention is directed to the above-mentioned problems, and provides a low-stress high-refractive-index thin film, a material and a method for manufacturing the same.
In order to achieve the purpose, the invention adopts the following technical scheme:
the preparation method of the low-stress high-refractive-index film material comprises the following steps:
s1, ball-milling to prepare powder, namely respectively putting titanium oxide, titanium dioxide and aluminum oxide into a ceramic ball mill to prepare titanium oxide material particles, titanium dioxide material particles and aluminum oxide material particles with the mesh size of 0.1-2 microns;
s2, mixing and bonding, namely adding the titanium oxide material particles, the titanium dioxide material particles and the aluminum oxide material particles which are prepared in the step S1 into a nano material bonding agent according to a proportion to obtain a bonding mixture;
s3, standing at constant temperature and constant humidity, putting the bonding mixture obtained in the S2 into a ceramic crucible, and standing for 22-26h in an environment with 25 ℃ and 45% RH to obtain a standing mixture;
s4, melting, putting the standing mixture of S3 into a melting furnace, heating to 1600-2200 ℃ to completely melt the standing mixture, and cooling and crystallizing for 22-26h to obtain Ti 3 O 5 -Al 2 O 3 And (3) mixing the materials.
In the preparation method of the low-stress high-refractive-index thin film material, in the step S2, the ratio of titanium dioxide, titanium dioxide and aluminum oxide is 40-50%: 30% -40%: 30 to 40 percent.
In the above method for preparing a low-stress high-refractive-index thin film material, the ratio of the total amount of the titanium dioxide, titanium dioxide and aluminum oxide to the nanomaterial binder is 100:1 to 2.
The application also provides a low-stress high-refractive-index thin film material, which is prepared by the preparation method of the low-stress high-refractive-index thin film material.
The application also provides a low-stress high-refractive-index film, and the low-stress high-refractive-index film is prepared from the low-stress high-refractive-index film material.
In the low-stress high-refractive-index thin film, the low-stress high-refractive-index thin film has a light transmission range of 400nm to 7000 nm.
In the low-stress high-refractive-index thin film, the low-stress high-refractive-index thin film has a melting point of 1700 ℃.
Compared with the prior art, the application has the advantages that:
the internal tensile stress performance of the material is improved, the defects that the single Ti3O5 is soft and crisp in texture and the internal stress form is compressive stress are overcome, and the problem that the Ti3O5 film is easy to crack due to the fluctuation of environmental temperature and the absorption of water in the air by the film layer in the long-term use is fundamentally solved.
Has a high light transmission range of 400nm to 7000 nm.
Has a melting point of 1700 ℃.
Drawings
FIG. 1 shows Ti according to the present invention 3 O 5 -Al 2 O 3 And (5) picture of a real object.
FIG. 2 is a flow chart of a preparation method provided by the present invention.
Detailed Description
The following are specific embodiments of the present invention and are further described with reference to the drawings, but the present invention is not limited to these embodiments.
As shown in fig. 2, the preparation method of the low-stress high-refractive-index thin film material comprises the following steps:
and S1, ball-milling to prepare powder, namely respectively putting titanium oxide (Ti2O3), titanium dioxide (TiO2) and aluminum oxide (Al2O3) into a ceramic ball mill to prepare the powder by ball milling, and preparing titanium oxide material particles, titanium dioxide material particles and aluminum oxide material particles with the mesh size of 0.1-2 microns.
The ceramic ball mill ball-mills the above three materials into powder particles for later use.
The mesh numbers of the three powder materials are consistent, certainly, the mesh numbers can also be inconsistent, and the corresponding ball milling mesh numbers can be set according to actual requirements.
And S2, mixing and bonding, namely adding the titanium oxide material particles, the titanium dioxide material particles and the aluminum oxide material particles which are prepared in the step S1 into a nano material bonding agent according to a proportion to obtain a bonding mixture. The proportions here are titanium sesquioxide: titanium dioxide: 40-50% of aluminum oxide: 30% -40%: 30 to 40 percent.
The nano-material binding agent is commercially available, and the ratio of the total amount of the titanium dioxide, the titanium dioxide and the aluminum oxide to the nano-material binding agent is 100: 1.0-2.0. The nano material binding agent is mainly used for uniformly distributing multi-formula materials, the organic binding agent can be burnt and volatilized in a high-temperature crystal furnace without residue, and the materials also have solid-phase reaction at this time.
The adding sequence is as follows: and (3) putting the nano material binding agent into a container, then putting the titanium oxide material particles, the titanium dioxide material particles and the aluminum oxide material particles into the container, and stirring to obtain a binding mixture. The advantage of this sequence is that: can prevent titanium oxide material particles, titanium dioxide material particles and aluminum oxide material particles which are not bonded by the nano material bonding agent from being arranged at the bottom of the container.
And when the titanium dioxide material particles, the titanium dioxide material particles and the aluminum oxide material particles are placed into the container, the three materials are put into the container in an alternative placing mode, so that the uniformity of the materials is better.
And S3, standing at constant temperature and constant humidity, putting the bonding mixture obtained in the S2 into a ceramic crucible, and standing for 22-26h in an environment with 25 ℃ and 45% RH to obtain a standing mixture.
S4, melting, putting the standing mixture of S3 into a melting furnace, heating to 1600-2200 ℃ to completely melt the standing mixture, and cooling and crystallizing for 22-26h to obtain Ti 3 O 5 -Al 2 O 3 And (3) mixing the materials.
This example gives Ti 3 O 5 -Al 2 O 3 The hybrid material, which allows the material to have very good ductility, i.e. tensile stress properties, in end-use applications, solves the cracking problem.
Figure BDA0003717696690000041
From the above test data, it can be seen that the present application has very good refractive index and produces tensile stress in both the heated and unheated state, which provides a high resistance to cracking for the end use of the material.
FIG. 1 is Ti 3 O 5 -Al 2 O 3 And (5) a mixed material object diagram.
Example one
The preparation method comprises the following steps:
s1, ball-milling to prepare powder, namely respectively putting titanium oxide, titanium dioxide and aluminum oxide into a ceramic ball mill to prepare powder by ball milling, and preparing titanium oxide material particles, titanium dioxide material particles and aluminum oxide material particles with the mesh size of 0.1 micrometer;
s2, mixing and bonding, namely adding the titanium oxide material particles, the titanium dioxide material particles and the aluminum oxide material particles which are prepared in the step S1 into a nano material bonding agent according to a proportion to obtain a bonding mixture; the proportion is titanium sesquioxide: titanium dioxide: aluminum oxide 40%: 30%: 30 percent.
S3, standing at constant temperature and constant humidity, putting the bonding mixture obtained in the S2 into a ceramic crucible, and standing for 22 hours in an environment with 25 ℃ and 45% RH to obtain a standing mixture;
s4, melting, namely putting the standing mixture of S3 into a melting furnace, heating to 1600 ℃ to completely melt the standing mixture, and cooling and crystallizing for 22 hours to obtain Ti 3 O 5 -Al 2 O 3 And (3) mixing the materials.
This example gives Ti 3 O 5 -Al 2 O 3 The hybrid material, which allows the material to have very good ductility, i.e. tensile stress properties, in end-use applications, solves the cracking problem.
Figure BDA0003717696690000051
From the above test data, it can be seen that the present application has very good refractive index and produces tensile stress in both the heated and unheated state, which provides a high resistance to cracking for the end use of the material.
Example two
The preparation method comprises the following steps:
s1, ball-milling to prepare powder, namely respectively putting titanium oxide, titanium dioxide and aluminum oxide into a ceramic ball mill to prepare titanium oxide material particles, titanium dioxide material particles and aluminum oxide material particles with the mesh size of 0.85 micrometer;
s2, mixing and bonding, namely adding the titanium oxide material particles, the titanium dioxide material particles and the aluminum oxide material particles which are prepared in the step S1 into a nano material bonding agent according to a proportion to obtain a bonding mixture; the proportion of titanium sesquioxide: titanium dioxide: 45% of aluminum oxide: 35%: 35 percent.
S3, standing at constant temperature and constant humidity, putting the bonding mixture obtained in the S2 into a ceramic crucible, and standing for 24 hours in an environment with 25 ℃ and 45% RH to obtain a standing mixture;
s4, melting, putting the standing mixture of S3 into a melting furnace, heating to 1900 ℃ to completely melt the standing mixture, and cooling and crystallizing for 24 hours to obtain Ti 3 O 5 -Al 2 O 3 And (3) mixing the materials.
This example gives Ti 3 O 5 -Al 2 O 3 The hybrid material, which allows the material to have very good ductility, i.e. tensile stress properties, in end-use applications, solves the cracking problem.
Figure BDA0003717696690000061
EXAMPLE III
The preparation method comprises the following steps:
s1, ball-milling to prepare powder, namely respectively putting titanium oxide, titanium dioxide and aluminum oxide into a ceramic ball mill to prepare powder by ball milling, and preparing titanium oxide material particles, titanium dioxide material particles and aluminum oxide material particles with the mesh size of 2 microns;
s2, mixing and bonding, namely adding the titanium oxide material particles, the titanium dioxide material particles and the aluminum oxide material particles which are prepared in the step S1 into a nano material bonding agent according to a proportion to obtain a bonding mixture; the proportion of titanium sesquioxide: titanium dioxide: 50% of aluminum oxide: 40%: 40 percent.
S3, standing at constant temperature and constant humidity, putting the bonding mixture obtained in the S2 into a ceramic crucible, and standing for 26 hours in an environment with 25 ℃ and 45% RH to obtain a standing mixture;
s4, melting, putting the standing mixture of S3 into a melting furnace, heating to 2200 ℃ to completely melt the standing mixture, and cooling and crystallizing for 26 hours to obtain Ti 3 O 5 -Al 2 O 3 And (3) mixing the materials.
This example gives Ti 3 O 5 -Al 2 O 3 The hybrid material, which allows the material to have very good ductility, i.e. tensile stress properties, in end-use applications, solves the cracking problem.
Figure BDA0003717696690000071
Example four
The embodiment provides a low-stress high-refractive-index thin film material, which is prepared by the preparation method of the low-stress high-refractive-index thin film material in the first embodiment.
EXAMPLE five
This example provides a low stress high refractive index thin film made from the low stress high refractive index thin film material of example two.
The low-stress high-refractive-index thin film has the following advantages:
light transmission range of the film: 400nm to 7000 nm;
melting point: 1700 ℃;
weather resistance: MIL-C-675B/C;
density g/cm3: 4.5
The material type is as follows: a Ti-Al mixed oxide.
IAD: ion Assist position, Ion Source assistance.
The specific embodiments described herein are merely illustrative of the spirit of the invention. Various modifications or additions may be made to the described embodiments or alternatives may be employed by those skilled in the art without departing from the spirit or ambit of the invention as defined in the appended claims.

Claims (7)

1. The preparation method of the low-stress high-refractive-index thin film material is characterized by comprising the following steps of:
s1, ball-milling to prepare powder, namely respectively putting titanium oxide, titanium dioxide and aluminum oxide into a ceramic ball mill to prepare titanium oxide material particles, titanium dioxide material particles and aluminum oxide material particles with the mesh size of 0.1-2 microns;
s2, mixing and bonding, namely adding the titanium trioxide material particles, the titanium dioxide material particles and the aluminum trioxide material particles prepared in the step S1 into a nano material bonding agent according to a proportion to obtain a bonding mixture;
s3, standing at constant temperature and constant humidity, putting the bonding mixture obtained in the S2 into a ceramic crucible, and standing for 22-26h in an environment with 25 ℃ and 45% RH to obtain a standing mixture;
s4, melting, putting the S3 standing mixture into a melting furnace, heating to 1600-2200 ℃ to completely melt the standing mixture, and cooling and crystallizing for 22-26h to obtain Ti 3 O 5 -Al 2 O 3 And (3) mixing the materials.
2. The method for preparing a low-stress high-refractive-index thin film material according to claim 1, wherein in the step S2, the ratio of titanium dioxide to aluminum oxide is 40-50%: 30% -40%: 30 to 40 percent.
3. The method according to claim 1, wherein in step S2, the ratio of the total amount of titanium dioxide, titanium dioxide and aluminum oxide to the nanomaterial binder is 100:1 to 2.
4. The low-stress high-refractive-index thin film material is characterized by being prepared by the preparation method of the low-stress high-refractive-index thin film material according to any one of claims 1 to 3.
5. The low-stress high-refractive-index thin film is characterized in that the low-stress high-refractive-index thin film is prepared from the low-stress high-refractive-index thin film material in claim 4.
6. The low stress high refractive index film according to claim 5, wherein the low stress high refractive index film has a film light transmission range of 400nm to 7000 nm.
7. The low stress high refractive index film of claim 5, wherein said low stress high refractive index film has a melting point of 1700 ℃.
CN202210749238.9A 2022-06-28 2022-06-28 Low-stress high-refractive-index film, material and preparation method Pending CN115057699A (en)

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Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2007047530A (en) * 2005-08-11 2007-02-22 Seiko Epson Corp Optical multilayer film filter and its manufacturing method
JP2009132989A (en) * 2007-11-09 2009-06-18 Epson Toyocom Corp Method for forming optical thin film, and optical element provided with the optical thin film
CN103806099A (en) * 2014-01-20 2014-05-21 福州阿石创光电子材料有限公司 Method for preparing titanium oxide crystal
CN103806100A (en) * 2014-02-12 2014-05-21 常州瞻驰光电科技有限公司 Vertical temperature gradient growing method of trititanium pentoxide polycrystal
US20180244565A1 (en) * 2017-02-28 2018-08-30 Corning Incorporated Scratch resistant films and methods of making the same
CN109503149A (en) * 2018-11-27 2019-03-22 北京富兴凯永兴光电技术有限公司 A kind of high refractive index optical filming material and preparation method, optical anti-reflective film
CN113200566A (en) * 2021-04-15 2021-08-03 有研资源环境技术研究院(北京)有限公司 Pre-melted high-refractive-index optical coating material and preparation method and application thereof

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2007047530A (en) * 2005-08-11 2007-02-22 Seiko Epson Corp Optical multilayer film filter and its manufacturing method
JP2009132989A (en) * 2007-11-09 2009-06-18 Epson Toyocom Corp Method for forming optical thin film, and optical element provided with the optical thin film
CN103806099A (en) * 2014-01-20 2014-05-21 福州阿石创光电子材料有限公司 Method for preparing titanium oxide crystal
CN103806100A (en) * 2014-02-12 2014-05-21 常州瞻驰光电科技有限公司 Vertical temperature gradient growing method of trititanium pentoxide polycrystal
US20180244565A1 (en) * 2017-02-28 2018-08-30 Corning Incorporated Scratch resistant films and methods of making the same
CN109503149A (en) * 2018-11-27 2019-03-22 北京富兴凯永兴光电技术有限公司 A kind of high refractive index optical filming material and preparation method, optical anti-reflective film
CN113200566A (en) * 2021-04-15 2021-08-03 有研资源环境技术研究院(北京)有限公司 Pre-melted high-refractive-index optical coating material and preparation method and application thereof

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