CN115142137A - Novel optical coating material and preparation method thereof - Google Patents
Novel optical coating material and preparation method thereof Download PDFInfo
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- CN115142137A CN115142137A CN202111530782.6A CN202111530782A CN115142137A CN 115142137 A CN115142137 A CN 115142137A CN 202111530782 A CN202111530782 A CN 202111530782A CN 115142137 A CN115142137 A CN 115142137A
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- 239000000463 material Substances 0.000 title claims abstract description 103
- 238000000576 coating method Methods 0.000 title claims abstract description 50
- 230000003287 optical effect Effects 0.000 title claims abstract description 46
- 239000011248 coating agent Substances 0.000 title claims abstract description 43
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 238000005245 sintering Methods 0.000 claims abstract description 37
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 33
- 239000002994 raw material Substances 0.000 claims abstract description 26
- 238000001816 cooling Methods 0.000 claims abstract description 25
- 239000010936 titanium Substances 0.000 claims abstract description 20
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 20
- 229910052751 metal Inorganic materials 0.000 claims abstract description 19
- 239000002184 metal Substances 0.000 claims abstract description 19
- 238000002156 mixing Methods 0.000 claims abstract description 18
- 238000002844 melting Methods 0.000 claims abstract description 16
- 230000008018 melting Effects 0.000 claims abstract description 16
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims abstract description 16
- BPUBBGLMJRNUCC-UHFFFAOYSA-N oxygen(2-);tantalum(5+) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Ta+5].[Ta+5] BPUBBGLMJRNUCC-UHFFFAOYSA-N 0.000 claims abstract description 16
- PBCFLUZVCVVTBY-UHFFFAOYSA-N tantalum pentoxide Inorganic materials O=[Ta](=O)O[Ta](=O)=O PBCFLUZVCVVTBY-UHFFFAOYSA-N 0.000 claims abstract description 16
- 238000002425 crystallisation Methods 0.000 claims abstract description 6
- 230000008025 crystallization Effects 0.000 claims abstract description 6
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 31
- 239000013078 crystal Substances 0.000 claims description 15
- 239000004408 titanium dioxide Substances 0.000 claims description 15
- 238000000034 method Methods 0.000 claims description 11
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 10
- 238000005086 pumping Methods 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 6
- 229910052786 argon Inorganic materials 0.000 claims description 5
- 238000011049 filling Methods 0.000 claims description 4
- 238000005303 weighing Methods 0.000 claims description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims 2
- MRELNEQAGSRDBK-UHFFFAOYSA-N lanthanum(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[La+3].[La+3] MRELNEQAGSRDBK-UHFFFAOYSA-N 0.000 claims 1
- ORUIBWPALBXDOA-UHFFFAOYSA-L magnesium fluoride Chemical compound [F-].[F-].[Mg+2] ORUIBWPALBXDOA-UHFFFAOYSA-L 0.000 claims 1
- 229910001635 magnesium fluoride Inorganic materials 0.000 claims 1
- ZKATWMILCYLAPD-UHFFFAOYSA-N niobium pentoxide Inorganic materials O=[Nb](=O)O[Nb](=O)=O ZKATWMILCYLAPD-UHFFFAOYSA-N 0.000 claims 1
- URLJKFSTXLNXLG-UHFFFAOYSA-N niobium(5+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Nb+5].[Nb+5] URLJKFSTXLNXLG-UHFFFAOYSA-N 0.000 claims 1
- 235000012239 silicon dioxide Nutrition 0.000 claims 1
- 239000000377 silicon dioxide Substances 0.000 claims 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract description 14
- 239000001301 oxygen Substances 0.000 abstract description 14
- 229910052760 oxygen Inorganic materials 0.000 abstract description 14
- AZCUJQOIQYJWQJ-UHFFFAOYSA-N oxygen(2-) titanium(4+) trihydrate Chemical compound [O-2].[O-2].[Ti+4].O.O.O AZCUJQOIQYJWQJ-UHFFFAOYSA-N 0.000 abstract description 14
- 230000001276 controlling effect Effects 0.000 description 10
- 239000000758 substrate Substances 0.000 description 7
- 239000002245 particle Substances 0.000 description 4
- 239000002131 composite material Substances 0.000 description 3
- 239000003337 fertilizer Substances 0.000 description 3
- 239000011521 glass Substances 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000005304 optical glass Substances 0.000 description 2
- 230000001681 protective effect Effects 0.000 description 2
- 238000004611 spectroscopical analysis Methods 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000003990 capacitor Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000004973 liquid crystal related substance Substances 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 238000010791 quenching Methods 0.000 description 1
- 230000000171 quenching effect Effects 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/52—Alloys
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C14/00—Alloys based on titanium
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B11/00—Single-crystal growth by normal freezing or freezing under temperature gradient, e.g. Bridgman-Stockbarger method
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B28/00—Production of homogeneous polycrystalline material with defined structure
- C30B28/04—Production of homogeneous polycrystalline material with defined structure from liquids
- C30B28/06—Production of homogeneous polycrystalline material with defined structure from liquids by normal freezing or freezing under temperature gradient
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/16—Oxides
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Crystallography & Structural Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Mechanical Engineering (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention relates to the field of C30B29/00, in particular to a novel optical coating material and a preparation method thereof, wherein a titanium-based material and a metal improved material are used as raw materials, and the novel optical coating material is prepared by the steps of raw material mixing, high-temperature sintering, vacuum melting and cooling crystallization, and the novel optical coating material with high refractive index, high oxygen loss and high quality is provided. By adopting the aluminum oxide and the tantalum pentoxide with specific mass, on the premise of not influencing the high refractive index of the titanium pentoxide through vacuum melting and temperature-controlled crystallization, the problem that a film layer of the coating material falls off under extreme conditions is fundamentally solved, the problem that the product quality is seriously influenced due to the fact that the film layer is uneven because of splashing caused by oxygen release in the coating process due to high oxygen content is effectively avoided, and the application of the novel optical coating material in the fields of aerospace and the like in a large range is expanded.
Description
Technical Field
The invention relates to the field of C30B29/00, in particular to a novel optical coating material and a preparation method thereof.
Background
Lenses on lenses in the fields of vehicles, security, cameras and the like are key optical devices for determining the image pickup quality of the lenses. The optical glass substrate material is widely applied at the earlier stage, but the optical glass substrate material needs to be mechanically processed into a lens, so that the problems of high processing cost and poor product batch stability exist. With the rapid development of plastic technology, the performance of the plastic substrate in transmittance and the like is close to that of a glass substrate, and compared with the glass substrate, the plastic substrate can be formed at one step according to the required shape, and is simple to process and low in cost, so that at present, the plastic substrate material is more and more substituted for a glass lens material to form a mainstream of a lens material.
The titanium oxide with high refractive index has stable performance and is widely applied to the fields of optical filters, cold light source coatings, antireflection films, multilayer films and the like. In particular, the titanium pentoxide material is gradually used in the fields of optical antireflection films, absorption films, protective films, insulating films for liquid crystal displays, protective films for semiconductor elements, insulating films for capacitors, antireflection films for solar cells, exhaust devices, and the like.
Chinese patent CN101280456A discloses a method for growing a trititanium pentoxide crystal by a Bridgman method, but the method has the problems of slow crystal growth, difficult crystal processing, low yield and the like. The Chinese patent CN103806100A adopts a vertical temperature gradient method to improve the preparation method of the titanium pentoxide, so that the crystal growth rate of the titanium pentoxide is greatly improved, the production efficiency is improved, and the production cost is reduced; however, with the continuous development of optical coated lenses, higher requirements are put forward on the coated materials, and how to solve the problem of film layer falling of the optical coated materials under the extreme conditions of quenching, ultralow temperature, ultrahigh temperature and the like is an important factor for limiting the development of the optical coated materials and the optical lenses.
Therefore, the formula of the titanium pentoxide is optimized, the novel optical coating material is provided, the problem of film falling of the coating material under extreme conditions is fundamentally solved, and the optical coating material has important research significance and practical application value.
Disclosure of Invention
In order to solve the above problems, the present invention provides a novel optical coating material, which comprises at least the following raw materials in parts by weight: 80-109 parts of titanium-based material and 0-10 parts of metal modified material.
As a preferred technical scheme, the titanium-based material comprises 80-99 parts of titanium dioxide and 0-10 parts of titanium powder, and preferably, the mass ratio of the titanium dioxide to the titanium powder is (90-99): (4-8), the purity of the novel optical coating material is high, the oxygen loss of the titanium pentoxide is improved, and the serious product quality problem caused by splashing of the material in the coating process is avoided.
The purity of the titanium powder is 99.99 percent and is purchased from Shanghai Xian Xin New Material science and technology Co., ltd; the purity of the titanium dioxide is 99.99 percent, and the titanium dioxide is purchased from composite fertilizer Zhonghang nanotechnology development Co.
In order to provide a novel optical coating material meeting the use requirement under extreme conditions under the condition of ensuring high refractive index of the titanium pentoxide, the metal modified material is a combination of the aluminum oxide and the tantalum pentoxide, and the applicant finds that when the mass ratio of the aluminum oxide to the tantalum pentoxide is (0.5-5): (0-5), especially when the mass ratio of the aluminum oxide to the tantalum pentoxide is (0.5-2): (0.8-1.5), on the premise of not influencing the high refractive index of the titanium pentoxide, the problem that a film layer of the coating material falls off under extreme conditions is fundamentally solved, which is probably because the introduction of aluminum oxide and tantalum pentoxide with specific mass ratio plays a certain role in regulating and controlling the growth of the titanium pentoxide crystal, and in the actual coating process, the film layer with high uniformity and low stress is easier to form.
The invention provides a preparation method of the novel optical coating material, which takes the titanium-based material and the metal modified material as raw materials, and the novel optical coating material is prepared through the steps of raw material mixing, high-temperature sintering, vacuum melting, cooling and crystallization.
As a preferable technical scheme, the preparation method of the novel optical coating material specifically comprises the following steps:
(1) Mixing raw materials: accurately weighing the titanium-based material and the metal modified material according to the parts by weight, then placing the materials in a mixing device for mixing for 25-30min, and then placing the materials in a crucible for compacting;
(2) And (3) high-temperature sintering: putting the crucible into a high-temperature sintering furnace for high-temperature sintering;
(3) Vacuum melting: and starting a vacuum pumping system, controlling the conditions in the high-temperature sintering furnace to melt the raw materials after the vacuum degree of the high-temperature sintering furnace reaches a certain value.
(4) Cooling and crystallizing: and controlling the cooling rate, slowly cooling, and taking out the crystal after the crystal growth is finished.
As a preferable technical scheme, the step (2) of high-temperature sintering specifically comprises the steps of loading the crucible into a high-temperature sintering furnace, raising the temperature to 500-700 ℃ under the aerobic condition, and maintaining the temperature for 1-3 hours, so that organic impurities in the raw materials can be fully degraded.
As a preferred technical solution, the vacuum melting in step (3) comprises the following specific steps: starting a vacuum-pumping system to ensure that the vacuum degree of the high-temperature sintering furnace reaches 10 -3 -10 -4 Pa, when the temperature in the furnace reaches 1400-1700 ℃, filling argon, continuously heating to 1800-1900 ℃, and preserving the heat for 3-6 hours at the temperature; the vacuum degree of the high-temperature sintering furnace is controlled to be 10 -3 -10 -4 Pa, when the temperature in the furnace reaches 1400-1700 ℃, argon is flushed, and the novel optical coating material with higher quality is prepared under the condition of fully ensuring no oxygen, so that the prepared titanium pentoxide has obviously reduced oxygen loss, and the problem that the product quality is seriously affected due to uneven film caused by splashing of the high oxygen content in the coating process due to the release of oxygen is effectively avoided. The raw materials are fully melted and uniformly mixed by continuously heating to 1800-1900 ℃ and preserving heat for 3-6 hours at the temperature.
As a preferable technical scheme, the cooling rate in the step (4) is 15-30 ℃/h, and in the research process, the introduction of aluminum oxide and tantalum pentoxide can promote the generation of multivalent titanium to a certain extent, so that the phase purity of the material is affected.
Has the advantages that:
1. the invention takes titanium-based material and metal improved material as raw materials, and prepares the novel optical coating material through the steps of raw material mixing, high-temperature sintering, vacuum melting and cooling crystallization, and provides the novel optical coating material with high refractive index, high oxygen loss and high quality.
2. Controlling the mass ratio of titanium dioxide to titanium powder to be (90-99): (4-8), the purity of the novel optical coating material is high, the oxygen loss of the titanium pentoxide is improved, and the serious product quality problem caused by splashing of the material in the coating process is avoided.
3. Controlling the mass ratio of aluminum oxide to tantalum pentoxide to be (0.5-2): (0.8-1.5), on the premise of not influencing the high refractive index of the titanium pentoxide, the problem of film layer falling of the coating material under extreme conditions is fundamentally solved, and the wide-range application of the novel optical coating material in the fields of aerospace and the like is expanded.
4. Through the vacuum melting step, the novel optical coating material with higher quality is prepared under the condition of fully ensuring no oxygen, so that the prepared trititanium pentoxide has obviously reduced oxygen loss amount, and the problem that the film layer is uneven and further the product quality is seriously influenced due to splashing caused by the release of oxygen in the coating process due to higher oxygen content is effectively avoided.
5. Through controlling the cooling rate in cooling crystallization, on one hand, the reduction of phase purity caused by self-impurity removal can be avoided due to the fact that cooling is fast, the production promotion effect of aluminum oxide and tantalum pentoxide on polyvalent titanium impurities is weakened, the quality of the novel optical coating material is improved, the quality of a film layer is further improved, and the large-scale application of the film layer in the fields of aerospace and the like is expanded.
Detailed Description
Example 1
In one aspect, embodiment 1 of the present invention provides a novel optical coating material, which at least comprises the following raw materials in parts by weight: 39.2kg of titanium-based material and 0.8kg of metal modified material.
The titanium-based material comprises titanium dioxide and titanium powder; the mass ratio of the titanium dioxide to the titanium powder is 93:5.
the purity of the titanium powder is 99.99 percent, and the titanium powder is purchased from Shanghai Xian Xin New Material science and technology company Limited; the purity of the titanium dioxide is 99.99 percent and the titanium dioxide is purchased from composite fertilizer Zhonghang nanotechnology development Limited company.
The metal improvement material is a combination of aluminum oxide and tantalum pentoxide, and the mass ratio of the aluminum oxide to the tantalum pentoxide is 1:1.
in another aspect, embodiment 1 of the present invention provides a method for preparing a novel optical coating material, which comprises the steps of mixing raw materials, sintering at a high temperature, melting in vacuum, cooling, and crystallizing, wherein a titanium-based material and a metal modified material are used as raw materials.
The preparation method of the novel optical coating material specifically comprises the following steps:
(1) Mixing raw materials: accurately weighing the titanium-based material and the metal improved material according to the parts by weight, then placing the materials in a mixing device for mixing for 30min, and then placing the materials in a crucible for compacting;
(2) And (3) high-temperature sintering: putting the crucible into a high-temperature sintering furnace for high-temperature sintering;
(3) Vacuum melting: and starting a vacuum pumping system, controlling the conditions in the high-temperature sintering furnace to melt the raw materials after the vacuum degree of the high-temperature sintering furnace reaches a certain value.
(4) Cooling and crystallizing: and controlling the cooling rate, slowly cooling, and taking out the crystal after the crystal growth is finished.
And (3) the step (2) of high-temperature sintering specifically comprises the steps of putting the crucible into a high-temperature sintering furnace, heating to 600 ℃ under an aerobic condition, and maintaining the temperature for 2 hours.
The vacuum melting in the step (3) comprises the following specific steps: starting a vacuum-pumping system to ensure that the vacuum degree of the high-temperature sintering furnace reaches 10 -3 Pa, when the temperature in the furnace reaches 1500 ℃, filling argon, continuing to heat to 1850 ℃, and preserving the temperature for 4 hours at the temperature.
And (3) in the step (4), the cooling rate is 20 ℃/h, the prepared crystal is crushed and sieved to obtain 28kg of particles with the particle size of 1-3mm, and the titanium-oxygen ratio of the titanium pentoxide is 1.13 through EDS (electron-dispersive spectroscopy) analysis.
Example 2
In one aspect, embodiment 2 of the present invention provides a novel optical coating material, which at least comprises the following raw materials in parts by weight: 29.4kg of titanium-based material and 0.6kg of metal modified material.
The titanium-based material comprises titanium dioxide and titanium powder; the mass ratio of the titanium dioxide to the titanium powder is 93:5.
the purity of the titanium powder is 99.99 percent and is purchased from Shanghai Xian Xin New Material science and technology Co., ltd; the purity of the titanium dioxide is 99.99 percent, and the titanium dioxide is purchased from composite fertilizer Zhonghang nanotechnology development Co.
The metal improvement material is a combination of aluminum oxide and tantalum pentoxide, and the mass ratio of the aluminum oxide to the tantalum pentoxide is 1.2:1.
in another aspect, embodiment 1 of the present invention provides a method for preparing a novel optical coating material, which comprises the steps of mixing raw materials, sintering at a high temperature, melting in vacuum, cooling, and crystallizing, wherein a titanium-based material and a metal modified material are used as raw materials.
The preparation method of the novel optical coating material specifically comprises the following steps:
(1) Mixing raw materials: accurately weighing the titanium-based material and the metal improved material according to the parts by weight, then placing the materials in a mixing device for mixing for 30min, and then placing the materials in a crucible for compacting;
(2) And (3) high-temperature sintering: putting the crucible into a high-temperature sintering furnace for high-temperature sintering;
(3) Vacuum melting: and starting a vacuum pumping system, controlling the conditions in the high-temperature sintering furnace to melt the raw materials after the vacuum degree of the high-temperature sintering furnace reaches a certain value.
(4) Cooling and crystallizing: and controlling the cooling rate, slowly cooling, and taking out the crystal after the crystal growth is finished.
And (3) the step (2) of high-temperature sintering specifically comprises the steps of putting the crucible into a high-temperature sintering furnace, heating to 600 ℃ under an aerobic condition, and maintaining the temperature for 2 hours.
The vacuum melting in the step (3) comprises the following specific steps: starting a vacuum-pumping system to make the vacuum degree of the high-temperature sintering furnace reach 10 -3 Pa, when the temperature in the furnace reaches 1500 ℃, filling argon, continuing to heat to 1850 ℃, and preserving the temperature for 4 hours at the temperature.
And (3) in the step (4), the cooling rate is 22 ℃/h, 20kg of particles with the particle size of 1-3mm are obtained after the prepared crystals are crushed and screened, and the titanium-oxygen ratio of the titanium pentoxide is 1.14 through EDS (electron-dispersive spectroscopy) analysis.
Claims (10)
1. The novel optical coating material is characterized by comprising the following preparation raw materials in parts by weight: 80-109 parts of titanium-based material and 0-10 parts of metal modified material.
2. The novel optical coating material as claimed in claim 1, wherein the titanium-based material comprises 80-99 parts of titanium dioxide and 0-10 parts of titanium powder.
3. The novel optical coating material according to claim 2, wherein the mass ratio of the titanium dioxide to the titanium powder is (90-99): (4-8).
4. The novel optical coating material according to claim 1, wherein the metal modified material is at least one selected from the group consisting of aluminum oxide, tantalum pentoxide, magnesium fluoride, lanthanum trioxide, silicon dioxide, and niobium pentoxide.
5. The novel optical coating material according to claim 4, wherein the metal modified material is a combination of aluminum oxide and tantalum pentoxide, and the mass ratio of the aluminum oxide to the tantalum pentoxide is (0.5-5): (0-5).
6. The novel optical coating material according to claim 5, wherein the mass ratio of the aluminum oxide to the tantalum pentoxide is (0.5-2): (0.8-1.5).
7. The preparation method of a novel optical coating material according to any one of claims 1 to 6, wherein the novel optical coating material is prepared by using a titanium-based material and a metal modified material as raw materials and performing the steps of raw material mixing, high-temperature sintering, vacuum melting and cooling crystallization.
8. The method for preparing a novel optical coating material according to claim 7, comprising the following steps:
(1) Mixing raw materials: accurately weighing the titanium-based material and the metal modified material according to the parts by weight, then placing the materials in a mixing device for mixing for 25-30min, and then placing the materials in a crucible for compacting;
(2) And (3) high-temperature sintering: putting the crucible into a high-temperature sintering furnace for high-temperature sintering;
(3) Vacuum melting: starting a vacuum pumping system, controlling the conditions in the high-temperature sintering furnace to melt the raw materials after the vacuum degree of the high-temperature sintering furnace reaches a certain value;
(4) Cooling and crystallizing: and controlling the cooling rate, slowly cooling, and taking out the crystal after the crystal growth is finished.
9. The method for preparing a novel optical coating material according to claim 8, wherein the step (3) of vacuum melting comprises the following specific steps: starting a vacuum-pumping system to ensure that the vacuum degree of the high-temperature sintering furnace reaches 10 -3 -10 -4 Pa, when the temperature in the furnace reaches 1400-1700 ℃, filling argon, continuously heating to 1800-1900 ℃, and heating at the temperatureKeeping the temperature for 3-6 hours.
10. The method for preparing a novel optical coating material according to claim 8, wherein the cooling rate in step (4) is 15-30 ℃/h.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115893864A (en) * | 2022-10-28 | 2023-04-04 | 苏州晶生新材料有限公司 | Antistatic wear-resistant coating substrate and coating method |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101280456A (en) * | 2007-12-28 | 2008-10-08 | 上海晶生实业有限公司 | Growing method by Ti3O5 by bridgman method |
| CN103413776A (en) * | 2013-07-09 | 2013-11-27 | 中国科学院物理研究所 | Composite substrate with isolation layer and manufacturing method thereof |
| 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 |
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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 |
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| CN115893864A (en) * | 2022-10-28 | 2023-04-04 | 苏州晶生新材料有限公司 | Antistatic wear-resistant coating substrate and coating method |
| CN115893864B (en) * | 2022-10-28 | 2023-11-14 | 苏州晶生新材料有限公司 | Antistatic wear-resistant coating substrate and coating method |
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