CN114133226B - Optical coating substrate and using method thereof - Google Patents
Optical coating substrate and using method thereof Download PDFInfo
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- CN114133226B CN114133226B CN202111646401.0A CN202111646401A CN114133226B CN 114133226 B CN114133226 B CN 114133226B CN 202111646401 A CN202111646401 A CN 202111646401A CN 114133226 B CN114133226 B CN 114133226B
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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
- C04B35/14—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 silica
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- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
- C03C17/22—Surface treatment of glass, not in the form of fibres or filaments, by coating with other inorganic material
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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
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/24—Vacuum evaporation
- C23C14/28—Vacuum evaporation by wave energy or particle radiation
- C23C14/30—Vacuum evaporation by wave energy or particle radiation by electron bombardment
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2218/00—Methods for coating glass
- C03C2218/10—Deposition methods
- C03C2218/15—Deposition methods from the vapour phase
- C03C2218/151—Deposition methods from the vapour phase by vacuum evaporation
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- 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
- C04B2235/3224—Rare earth oxide or oxide forming salts thereof, e.g. scandium oxide
- C04B2235/3227—Lanthanum oxide or oxide-forming salts thereof
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- 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
- C04B2235/3231—Refractory metal oxides, their mixed metal oxides, or oxide-forming salts thereof
- C04B2235/3232—Titanium oxides or titanates, e.g. rutile or anatase
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- 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
- C04B2235/3231—Refractory metal oxides, their mixed metal oxides, or oxide-forming salts thereof
- C04B2235/3244—Zirconium oxides, zirconates, hafnium oxides, hafnates, or oxide-forming salts thereof
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- 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
- C04B2235/3231—Refractory metal oxides, their mixed metal oxides, or oxide-forming salts thereof
- C04B2235/3251—Niobium oxides, niobates, tantalum oxides, tantalates, or oxide-forming salts thereof
Abstract
The invention belongs to the technical field of optical coating materials, and particularly relates to an optical coating substrate and a using method thereof. The raw materials of the optical coating substrate provided by the invention comprise the following components in percentage by weight: 15-18% of silicon dioxide; 13-15% of titanium dioxide; 10-12% of zirconium dioxide; 5-8% of niobium pentoxide; 2-4% of zinc sulfide; the balance of lanthanum oxide and inevitable impurities, and the impurities account for no more than 0.03 percent of the total mass of the optical coating substrate. Compared with the prior art, the optical coating substrate provided by the invention can be widely applied to coating of various optical substrates, the prepared coating layer has a small water contact angle, can effectively prevent fogging in a damp and hot environment, has high light transmittance and a refractive index close to that of glass, does not influence the normal light transmission of the glass substrate, does not cause optical distortion, has certain wear resistance, and has a certain protection effect on the glass substrate.
Description
Technical Field
The invention belongs to the technical field of optical coating materials, and particularly relates to an optical coating substrate and a using method thereof.
Background
The optical glass is widely applied to various precision optical instruments. The coating on the surface of the optical glass is a commonly used modifying means of the optical glass, and generally, a coating material is heated to an extremely high temperature, so that the surface components of the material are evaporated in the form of atomic groups or ions and deposited on the surface of a substrate to form a coating.
The optical glass can be modified by adopting different coating materials according to different purposes. Such as increased corrosion resistance, increased wear resistance, increased light transmittance, selective transmission or filtering of light within a certain wavelength range, and the like. However, the existing coating materials can only meet the requirements of one or two aspects, and are limited by the characteristics of the materials, and the performances of different aspects are often difficult to be compatible.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides an optical coating substrate and a using method thereof.
The invention aims to form a coating layer which is wear-resistant, antifogging, high in light transmittance and close to glass in refractive index on a glass substrate so as to be applied to the surface of a substrate such as an optical lens.
The raw materials of the optical coating base material provided by the invention comprise the following components in percentage by weight:
15 to 18 percent of silicon dioxide
13 to 15 percent of titanium dioxide
Zirconium dioxide 10-12%
Niobium pentoxide 5-8%
2 to 4 percent of zinc sulfide
The balance of lanthanum oxide and inevitable impurities, wherein the impurities account for no more than 0.03 percent of the total mass of the optical coating substrate;
the optical coating base material is powder prepared by mixing, grinding, briquetting, sintering, crushing and screening the raw materials.
Further, the raw materials are ground by a wet method, a certain amount of ethanol is added in the grinding process, and the weight ratio of the ethanol to the raw materials is 0.15-0.3.
Further, the raw material is ground and then transferred into a die, and the raw material in the die is pressed into blocks by using a press, wherein the pressure is 30-45MPa.
Further, sintering the raw materials pressed into blocks at high temperature, wherein the sintering comprises two stages of pre-sintering and re-sintering; the pre-sintering is to place the raw materials pressed into blocks in a muffle furnace and pre-sinter the raw materials at 900-1250 ℃; the re-sintering is to place the pre-sintered raw material in a vacuum smelting furnace and re-sinter the raw material at 1550-1800 ℃.
Further, the temperature setting of the pre-sintering stage is as follows:
the first step is as follows: 5 ℃/min, raising the temperature from room temperature to 120 ℃;
the second step: preserving the heat for 3 hours;
the third step: heating from 120 ℃ to the pre-sintering temperature at 10 ℃/min;
the fourth step: preserving the heat for 5-7h at the pre-sintering temperature;
the fifth step: cooling to room temperature along with the furnace.
Further, the temperature setting in the re-sintering stage is as follows:
the first step is as follows: heating to the re-sintering temperature from room temperature at 10 deg.c/min;
the second step: preserving the heat for 12-15h at the re-sintering temperature;
the third step: cooling to room temperature along with the furnace.
Further, crushing and screening the raw material blocks obtained by sintering to obtain powder with the particle size of 0.2-1.5, namely the optical coating substrate.
The invention further provides a using method of the optical coating substrate, a vapor deposition device is used for coating, and the method comprises the following steps:
(S1) putting the optical coating base material into an electron beam evaporator of a vapor deposition device, and fixing a substrate to be coated in a deposition cavity of the vapor deposition device;
(S2) vacuumizing the deposition cavity to reduce the pressure to be within the range of 0.1-2Pa;
(S3) preheating a substrate to be plated to 250-280 ℃;
and (S4) heating the optical coating substrate in the electron beam evaporator to 2250-2300 ℃, and then opening a channel between the electron beam evaporator and the deposition chamber to enable the optical coating substrate to enter the deposition chamber through vapor, thereby depositing and forming a coating on the substrate to be coated.
Further, the substrate to be plated is glass or quartz, and the substrate to be plated is kept clean and dry before use.
Further, the substrate to be plated is pretreated before use as follows: and immersing the substrate to be plated into deionized water for ultrasonic cleaning for 3-10min, then immersing the substrate into acetone for ultrasonic cleaning for 3-10min, and drying to obtain a clean and dry substrate to be plated.
Has the beneficial effects that: compared with the prior art, the optical coating substrate provided by the invention can be widely applied to coating of various optical substrates, the prepared coating layer has a small water contact angle, can effectively prevent fogging in a damp and hot environment, has high light transmittance and a refractive index close to that of glass, does not influence the normal light transmission of the glass substrate, does not cause optical distortion, has certain wear resistance, and has a certain protection effect on the glass substrate.
Detailed Description
The invention is further illustrated by the following specific examples, which are illustrative and intended to illustrate the problem and explain the invention, but not limiting.
Example 1
The embodiment provides an optical coating substrate and a using method thereof.
The raw materials of the optical coating base material comprise the following components in percentage by weight:
silicon dioxide 15%
13 percent of titanium dioxide
Zirconium dioxide 10%
Niobium pentoxide 5%
2 percent of zinc sulfide
The balance of lanthanum oxide and inevitable impurities, wherein the impurities account for no more than 0.03 percent of the total mass of the optical coating substrate;
the optical coating substrate is powder prepared by mixing, grinding, briquetting, sintering, crushing and screening the raw materials.
In this example, the raw materials were ground by a wet method, and a certain amount of ethanol was added during the grinding, with the weight ratio of ethanol to raw materials being 0.15.
In this example, the raw material was ground and transferred to a mold, and the raw material in the mold was pressed into a block shape by a press at a pressure of 45MPa.
In the embodiment, the raw materials pressed into blocks are sintered at high temperature, and the sintering comprises two stages of pre-sintering and re-sintering; the pre-sintering is to place the raw materials pressed into blocks in a muffle furnace and pre-sinter the raw materials at 900 ℃; the re-sintering is to place the pre-sintered raw material in a vacuum melting furnace and re-sinter the raw material at 1550 ℃.
In this embodiment, the temperature at the pre-sintering stage is set as follows:
the first step is as follows: 5 ℃/min, raising the temperature from room temperature to 120 ℃;
the second step is that: preserving the heat for 3 hours;
the third step: 10 ℃/min is increased from 120 ℃ to the pre-sintering temperature;
the fourth step: preserving the heat for 7 hours at the pre-sintering temperature;
the fifth step: cooling to room temperature along with the furnace.
In this example, the temperature at the re-sintering stage was set as follows:
the first step is as follows: heating to the re-sintering temperature from room temperature at 10 deg.c/min;
the second step is that: preserving the heat for 15 hours at the re-sintering temperature;
the third step: cooling to room temperature along with the furnace.
In this embodiment, the raw material block obtained by sintering is crushed and sieved to obtain powder with a particle size in the range of 0.2 to 1.5, which is the optical coating substrate.
The application method of the optical coating substrate uses a vapor deposition device for coating, and comprises the following steps:
(S1) putting the optical coating base material into an electron beam evaporator of a vapor deposition device, and fixing a substrate to be coated in a deposition cavity of the vapor deposition device;
(S2) vacuumizing the deposition cavity to reduce the pressure to 0.1-2Pa;
(S3) preheating a substrate to be plated to 250 ℃;
and (S4) heating the optical coating substrate in the electron beam evaporator to 2250 ℃, and then opening a channel between the electron beam evaporator and the deposition chamber to enable the optical coating substrate to enter the deposition chamber through vapor, thereby depositing and forming a coating on the substrate to be coated.
In the embodiment, the substrate to be plated is glass, and the substrate to be plated is kept clean and dry before use, specifically, the substrate to be plated is firstly immersed in deionized water for ultrasonic cleaning for 3min, then immersed in acetone for ultrasonic cleaning for 3min, and dried to obtain a clean and dry substrate to be plated.
Example 2
The embodiment provides an optical coating substrate and a using method thereof.
The raw materials of the optical coating substrate comprise the following components in percentage by weight:
18 percent of silicon dioxide
Titanium dioxide 15%
Zirconium dioxide 12%
Niobium pentoxide 8%
4 percent of zinc sulfide
The balance of lanthanum oxide and inevitable impurities, wherein the impurities account for no more than 0.03 percent of the total mass of the optical coating substrate;
the optical coating substrate is powder prepared by mixing, grinding, briquetting, sintering, crushing and screening the raw materials.
In this embodiment, the raw materials are ground by a wet method, a certain amount of ethanol is added during the grinding process, and the weight ratio of the ethanol to the raw materials is 0.3.
In this example, the raw material was ground and transferred to a mold, and the raw material in the mold was pressed into a block shape by a press at a pressure of 30MPa.
In the embodiment, the raw materials pressed into blocks are sintered at high temperature, and the sintering comprises two stages of pre-sintering and re-sintering; the pre-sintering is to place the raw materials pressed into blocks in a muffle furnace and pre-sinter the raw materials at 1250 ℃; the re-sintering is to place the pre-sintered raw material in a vacuum melting furnace and re-sinter at 1800 ℃.
In this example, the temperature at the pre-sintering stage is set as follows:
the first step is as follows: 5 ℃/min, raising the temperature from room temperature to 120 ℃;
the second step is that: preserving the heat for 3 hours;
the third step: heating from 120 ℃ to the pre-sintering temperature at 10 ℃/min;
the fourth step: preserving the heat for 5 hours at the pre-sintering temperature;
the fifth step: cooling to room temperature along with the furnace.
In this example, the temperature at the re-sintering stage was set as follows:
the first step is as follows: heating to the re-sintering temperature from room temperature at 10 deg.c/min;
the second step: preserving the heat for 12 hours at the re-sintering temperature;
the third step: cooling to room temperature along with the furnace.
In this embodiment, the raw material block obtained by sintering is crushed and sieved to obtain powder with a particle size in the range of 0.2 to 1.5, that is, the optical coating substrate.
The application method of the optical coating substrate uses a vapor deposition device for coating, and comprises the following steps:
(S1) putting the optical coating base material into an electron beam evaporator of a vapor deposition device, and fixing a substrate to be coated in a deposition cavity of the vapor deposition device;
(S2) vacuumizing the deposition cavity to reduce the pressure to be within the range of 0.1-2Pa;
(S3) preheating a substrate to be plated to 280 ℃;
and (S4) heating the optical coating base material in the electron beam evaporator to 2300 ℃, and then opening a channel between the electron beam evaporator and the deposition cavity to enable the optical coating base material to enter the deposition cavity through steam, so that a coating is deposited on the substrate to be coated.
In the embodiment, the substrate to be plated is glass, and the substrate to be plated is kept clean and dry before use, specifically, the substrate to be plated is firstly immersed in deionized water for ultrasonic cleaning for 10min, then immersed in acetone for ultrasonic cleaning for 10min, and dried to obtain a clean and dry substrate to be plated.
Example 3
The embodiment provides an optical coating substrate and a using method thereof.
The raw materials of the optical coating substrate comprise the following components in percentage by weight:
silicon dioxide 16%
14 percent of titanium dioxide
Zirconium dioxide 11%
Niobium pentoxide 7%
3 percent of zinc sulfide
The balance of lanthanum oxide and inevitable impurities, wherein the impurities account for no more than 0.03 percent of the total mass of the optical coating substrate;
the optical coating substrate is powder prepared by mixing, grinding, briquetting, sintering, crushing and screening the raw materials.
In the embodiment, the raw materials are ground by a wet method, a certain amount of ethanol is added in the grinding process, and the weight ratio of the ethanol to the raw materials is 0.22.
In this example, the raw material was ground and transferred to a mold, and the raw material in the mold was pressed into a block shape by a press at a pressure of 40MPa.
In the embodiment, the raw materials pressed into blocks are sintered at high temperature, and the sintering comprises two stages of pre-sintering and re-sintering; the pre-sintering is to place the raw materials pressed into blocks in a muffle furnace and perform pre-sintering at 1200 ℃; and the step of re-sintering is to place the pre-sintered raw materials in a vacuum melting furnace and re-sinter the materials at 1750 ℃.
In this embodiment, the temperature at the pre-sintering stage is set as follows:
the first step is as follows: 5 ℃/min, raising the temperature from room temperature to 120 ℃;
the second step is that: preserving the heat for 3 hours;
the third step: 10 ℃/min is increased from 120 ℃ to the pre-sintering temperature;
the fourth step: preserving the heat for 6 hours at the pre-sintering temperature;
the fifth step: cooling to room temperature along with the furnace.
In this example, the temperature at the re-sintering stage was set as follows:
the first step is as follows: heating to the re-sintering temperature from room temperature at 10 deg.c/min;
the second step is that: preserving the heat for 13 hours at the re-sintering temperature;
the third step: cooling to room temperature along with the furnace.
In this embodiment, the raw material block obtained by sintering is crushed and sieved to obtain powder with a particle size in the range of 0.2 to 1.5, which is the optical coating substrate.
The application method of the optical coating substrate uses a vapor deposition device for coating, and comprises the following steps:
(S1) putting the optical coating substrate into an electron beam evaporator of a vapor deposition device, and fixing a substrate to be coated in a deposition cavity of the vapor deposition device;
(S2) vacuumizing the deposition cavity to reduce the pressure to be within the range of 0.1-2Pa;
(S3) preheating a substrate to be plated to 270 ℃;
and (S4) heating the optical coating base material in the electron beam evaporator to 2280 ℃, and then opening a channel between the electron beam evaporator and the deposition cavity to enable the optical coating base material to enter the deposition cavity through steam, thereby depositing and forming a coating on the substrate to be coated.
In the embodiment, the substrate to be plated is glass, and the substrate to be plated is kept clean and dry before use, specifically, the substrate to be plated is firstly immersed in deionized water for ultrasonic cleaning for 5min, then immersed in acetone for ultrasonic cleaning for 5min, and dried to obtain a clean and dry substrate to be plated.
Example 4
The embodiment provides an optical coating substrate and a using method thereof.
The raw materials of the optical coating substrate comprise the following components in percentage by weight:
silicon dioxide 16%
Titanium dioxide 15%
Zirconium dioxide 10%
Niobium pentoxide 7%
3 percent of zinc sulfide
The balance of lanthanum oxide and inevitable impurities, wherein the impurities account for no more than 0.03 percent of the total mass of the optical coating substrate;
the optical coating substrate is powder prepared by mixing, grinding, briquetting, sintering, crushing and screening the raw materials.
In the embodiment, the raw materials are ground by a wet method, a certain amount of ethanol is added in the grinding process, and the weight ratio of the ethanol to the raw materials is 0.25.
In this example, the raw material was ground and transferred to a mold, and the raw material in the mold was pressed into a block shape by a press at a pressure of 35MPa.
In the embodiment, the raw materials pressed into blocks are sintered at high temperature, and the sintering comprises two stages of pre-sintering and re-sintering; the pre-sintering is to place the raw materials pressed into blocks in a muffle furnace and pre-sinter the raw materials at 1000 ℃; the re-sintering is to place the pre-sintered raw material in a vacuum melting furnace and re-sinter the raw material at 1600 ℃.
In this embodiment, the temperature at the pre-sintering stage is set as follows:
the first step is as follows: 5 ℃/min, raising the temperature from room temperature to 120 ℃;
the second step: preserving the heat for 3 hours;
the third step: 10 ℃/min is increased from 120 ℃ to the pre-sintering temperature;
the fourth step: preserving the heat for 6 hours at the pre-sintering temperature;
the fifth step: cooling to room temperature along with the furnace.
In this example, the temperature at the re-sintering stage was set as follows:
the first step is as follows: heating to the re-sintering temperature from room temperature at 10 deg.c/min;
the second step is that: preserving the heat for 13 hours at the re-sintering temperature;
the third step: cooling to room temperature along with the furnace.
In this embodiment, the raw material block obtained by sintering is crushed and sieved to obtain powder with a particle size in the range of 0.2 to 1.5, which is the optical coating substrate.
The application method of the optical coating substrate uses a vapor deposition device for coating, and comprises the following steps:
(S1) putting the optical coating substrate into an electron beam evaporator of a vapor deposition device, and fixing a substrate to be coated in a deposition cavity of the vapor deposition device;
(S2) vacuumizing the deposition cavity to reduce the pressure to be within the range of 0.1-2Pa;
(S3) preheating a substrate to be plated to 250 ℃;
and (S4) heating the optical coating base material in the electron beam evaporator to 2300 ℃, and then opening a channel between the electron beam evaporator and the deposition cavity to enable the optical coating base material to enter the deposition cavity through steam, so that a coating is deposited on the substrate to be coated.
In the embodiment, the substrate to be plated is glass, and the substrate to be plated is kept clean and dry before use, specifically, the substrate to be plated is firstly immersed in deionized water for ultrasonic cleaning for 8min, then immersed in acetone for ultrasonic cleaning for 8min, and dried to obtain a clean and dry substrate to be plated.
Example 5
The embodiment provides an optical coating substrate and a using method thereof.
The raw materials of the optical coating substrate comprise the following components in percentage by weight:
18 percent of silicon dioxide
13 percent of titanium dioxide
Zirconium dioxide 10%
Niobium pentoxide 6%
4 percent of zinc sulfide
The balance of lanthanum oxide and inevitable impurities, wherein the impurities account for no more than 0.03 percent of the total mass of the optical coating substrate;
the optical coating substrate is powder prepared by mixing, grinding, briquetting, sintering, crushing and screening the raw materials.
In this example, the raw materials were ground by a wet method, and a certain amount of ethanol was added during the grinding, with the weight ratio of ethanol to raw materials being 0.2.
In this example, the raw material was ground and transferred to a mold, and the raw material in the mold was pressed into a block shape by a press at a pressure of 45MPa.
In the embodiment, the raw materials pressed into blocks are sintered at high temperature, and the sintering comprises two stages of pre-sintering and re-sintering; the pre-sintering is to place the raw materials pressed into blocks in a muffle furnace and perform pre-sintering at 1100 ℃; the re-sintering is to place the pre-sintered raw material in a vacuum melting furnace and re-sinter at 1800 ℃.
In this embodiment, the temperature at the pre-sintering stage is set as follows:
the first step is as follows: 5 ℃/min, raising the temperature from room temperature to 120 ℃;
the second step is that: preserving the heat for 3 hours;
the third step: heating from 120 ℃ to the pre-sintering temperature at 10 ℃/min;
the fourth step: preserving the heat for 6 hours at the pre-sintering temperature;
the fifth step: cooling to room temperature along with the furnace.
In this example, the temperature at the re-sintering stage was set as follows:
the first step is as follows: heating to the re-sintering temperature from room temperature at 10 ℃/min;
the second step is that: preserving the heat for 13 hours at the re-sintering temperature;
the third step: cooling to room temperature along with the furnace.
In this embodiment, the raw material block obtained by sintering is crushed and sieved to obtain powder with a particle size in the range of 0.2 to 1.5, that is, the optical coating substrate.
The application method of the optical coating substrate uses a vapor deposition device for coating, and comprises the following steps:
(S1) putting the optical coating base material into an electron beam evaporator of a vapor deposition device, and fixing a substrate to be coated in a deposition cavity of the vapor deposition device;
(S2) vacuumizing the deposition cavity to reduce the pressure to be within the range of 0.1-2Pa;
(S3) preheating a substrate to be plated to 280 ℃;
and (S4) heating the optical coating base material in the electron beam evaporator to 2250 ℃, then opening a channel between the electron beam evaporator and the deposition chamber, and allowing the optical coating base material to enter the deposition chamber through vapor, thereby depositing and forming a coating on the substrate to be coated.
In the embodiment, the substrate to be plated is glass, and the substrate to be plated is kept clean and dry before use, specifically, the substrate to be plated is firstly immersed in deionized water for ultrasonic cleaning for 8min, then immersed in acetone for ultrasonic cleaning for 8min, and dried to obtain a clean and dry substrate to be plated.
The parameters of the coatings obtained in examples 1 to 5 are shown in table 1.
TABLE 1
| Sample examples | Film thickness (nm) | Film transmittance (%) | Refractive index | Water contact Angle (°) |
| Example 1 | 279 | 99.2 | 1.65 | 11 |
| Example 2 | 268 | 99.4 | 1.71 | 7 |
| Example 3 | 272 | 99.1 | 1.70 | 9 |
| Example 4 | 275 | 99.1 | 1.64 | 8 |
| Example 5 | 269 | 99.4 | 1.67 | 12 |
Note: the light transmittance and refractive index of the film were measured under 500nm light source.
The above embodiments are exemplary only, and are intended to illustrate the technical concept and features of the present invention so that those skilled in the art can understand the contents of the present invention and implement the present invention, and not to limit the scope of the present invention. All equivalent changes and modifications made according to the spirit of the present invention should be covered in the protection scope of the present invention.
Claims (6)
1. An optical coating substrate characterized by:
the raw materials of the optical coating base material comprise the following components in percentage by weight:
silicon dioxide 15-18%
13 to 15 percent of titanium dioxide
Zirconium dioxide 10-12%
Niobium pentoxide 5-8%
2 to 4 percent of zinc sulfide
The balance of lanthanum oxide and inevitable impurities, wherein the impurities account for no more than 0.03 percent of the total mass of the optical coating substrate;
the optical coating substrate is powder prepared by mixing, grinding, briquetting, sintering, crushing and screening the raw materials;
sintering the raw materials pressed into blocks at high temperature, wherein the sintering comprises two stages of pre-sintering and re-sintering; the pre-sintering is to place the raw materials pressed into blocks in a muffle furnace and pre-sinter the raw materials at 900-1250 ℃; the step of re-sintering is to place the pre-sintered raw material in a vacuum smelting furnace and re-sinter the raw material at 1550-1800 ℃;
the temperature settings in the pre-sintering stage were as follows:
the first step is as follows: 5 ℃/min, raising the temperature from room temperature to 120 ℃;
the second step is that: preserving the heat for 3 hours;
the third step: 10 ℃/min is increased from 120 ℃ to the pre-sintering temperature;
the fourth step: preserving the heat for 5-7h at the pre-sintering temperature;
the fifth step: cooling to room temperature along with the furnace;
the temperature settings in the re-sintering phase were as follows:
the first step is as follows: heating to the re-sintering temperature from room temperature at 10 ℃/min;
the second step is that: preserving the heat for 12-15h at the re-sintering temperature;
the third step: cooling to room temperature along with the furnace;
the optical coating substrate can be coated by using a vapor deposition device, and the method comprises the following steps:
(S1) putting the optical coating substrate into an electron beam evaporator of a vapor deposition device, and fixing a substrate to be coated in a deposition cavity of the vapor deposition device;
(S2) vacuumizing the deposition cavity to reduce the pressure to be within the range of 0.1-2Pa;
(S3) preheating a substrate to be plated to 250-280 ℃;
and (S4) heating the optical coating substrate in the electron beam evaporator to 2250-2300 ℃, and then opening a channel between the electron beam evaporator and the deposition chamber to enable the optical coating substrate to enter the deposition chamber through vapor, thereby depositing and forming a coating on the substrate to be coated.
2. An optically coated substrate according to claim 1, wherein: the raw materials are ground by a wet method, a certain amount of ethanol is added in the grinding process, and the weight ratio of the ethanol to the raw materials is 0.15-0.3.
3. An optically coated substrate according to claim 2, wherein: the raw materials are ground and then transferred into a die, and the raw materials in the die are pressed into blocks by a press, wherein the pressure is 30-45MPa.
4. An optically coated substrate according to claim 1, wherein: and crushing and screening the raw material blocks obtained by sintering to obtain powder with the particle size of 0.2-1.5, namely the optical coating substrate.
5. The optically coated substrate according to claim 1, wherein: the substrate to be plated is glass or quartz, and the substrate to be plated is kept clean and dry before use.
6. An optically coated substrate according to claim 5, wherein: the substrate to be plated is subjected to the following pretreatment before use: and immersing the substrate to be plated in deionized water for ultrasonic cleaning for 3-10min, then immersing in acetone for ultrasonic cleaning for 3-10min, and drying to obtain a clean and dry substrate to be plated.
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