CN117604453A - Quartz coating process for producing quartz substrate with high infrared reflectivity - Google Patents
Quartz coating process for producing quartz substrate with high infrared reflectivity Download PDFInfo
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- CN117604453A CN117604453A CN202311681079.4A CN202311681079A CN117604453A CN 117604453 A CN117604453 A CN 117604453A CN 202311681079 A CN202311681079 A CN 202311681079A CN 117604453 A CN117604453 A CN 117604453A
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 139
- 239000010453 quartz Substances 0.000 title claims abstract description 95
- 239000000758 substrate Substances 0.000 title claims abstract description 76
- 238000000576 coating method Methods 0.000 title claims abstract description 56
- 238000002310 reflectometry Methods 0.000 title claims abstract description 35
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 40
- 239000011248 coating agent Substances 0.000 claims abstract description 37
- 229910052581 Si3N4 Inorganic materials 0.000 claims abstract description 33
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 claims abstract description 33
- 229910052709 silver Inorganic materials 0.000 claims abstract description 24
- 239000004332 silver Substances 0.000 claims abstract description 24
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 23
- 239000010703 silicon Substances 0.000 claims abstract description 23
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 23
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 22
- 239000000463 material Substances 0.000 claims abstract description 20
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 20
- 238000004140 cleaning Methods 0.000 claims abstract description 6
- 238000001771 vacuum deposition Methods 0.000 claims abstract description 4
- 235000012239 silicon dioxide Nutrition 0.000 claims description 107
- 239000010410 layer Substances 0.000 claims description 52
- 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 description 50
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 46
- 229910052786 argon Inorganic materials 0.000 claims description 23
- 238000000034 method Methods 0.000 claims description 22
- 239000000377 silicon dioxide Substances 0.000 claims description 22
- 238000004544 sputter deposition Methods 0.000 claims description 18
- 238000000137 annealing Methods 0.000 claims description 13
- 238000010438 heat treatment Methods 0.000 claims description 13
- 239000002994 raw material Substances 0.000 claims description 13
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 12
- 239000001301 oxygen Substances 0.000 claims description 12
- 229910052760 oxygen Inorganic materials 0.000 claims description 12
- 239000007789 gas Substances 0.000 claims description 9
- 238000001816 cooling Methods 0.000 claims description 8
- 125000004122 cyclic group Chemical group 0.000 claims description 7
- 238000004381 surface treatment Methods 0.000 claims description 7
- 239000013077 target material Substances 0.000 claims description 7
- 238000000151 deposition Methods 0.000 claims description 6
- 230000008021 deposition Effects 0.000 claims description 6
- 239000002344 surface layer Substances 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 4
- 238000010849 ion bombardment Methods 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 239000012495 reaction gas Substances 0.000 claims description 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 abstract description 20
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 abstract description 4
- 238000002844 melting Methods 0.000 abstract description 4
- 230000008018 melting Effects 0.000 abstract description 4
- 239000002245 particle Substances 0.000 abstract description 4
- 239000000126 substance Substances 0.000 abstract description 4
- 230000000052 comparative effect Effects 0.000 description 7
- 238000007747 plating Methods 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 239000007888 film coating Substances 0.000 description 3
- 238000009501 film coating Methods 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 239000011856 silicon-based particle Substances 0.000 description 3
- 239000000853 adhesive Substances 0.000 description 2
- 230000001070 adhesive effect Effects 0.000 description 2
- 239000002390 adhesive tape Substances 0.000 description 2
- CXOWYMLTGOFURZ-UHFFFAOYSA-N azanylidynechromium Chemical compound [Cr]#N CXOWYMLTGOFURZ-UHFFFAOYSA-N 0.000 description 2
- 239000011247 coating layer Substances 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 239000010408 film Substances 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 239000013076 target substance Substances 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 230000003679 aging effect Effects 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 230000003373 anti-fouling effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000005693 optoelectronics Effects 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
Classifications
-
- 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
- C23C14/10—Glass or silica
-
- 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
- C23C14/0641—Nitrides
- C23C14/0652—Silicon nitride
-
- 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
- C23C14/0688—Cermets, e.g. mixtures of metal and one or more of carbides, nitrides, oxides or borides
-
- 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
- C23C14/34—Sputtering
- C23C14/3464—Sputtering using more than one target
-
- 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
- C23C14/54—Controlling or regulating the coating process
- C23C14/542—Controlling the film thickness or evaporation rate
-
- 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
- C23C14/58—After-treatment
- C23C14/5806—Thermal treatment
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Physical Vapour Deposition (AREA)
- Surface Treatment Of Glass (AREA)
Abstract
The invention discloses a quartz coating process for producing an infrared high-reflectivity quartz substrate, and belongs to the technical field of quartz substrate coating. The invention relates to a quartz coating process for producing an infrared high-reflectivity quartz substrate, which comprises the following steps of: step one: cleaning quartz substrate, removing surface dirt, preparing vacuum coating equipment, vacuumizing the coating equipment to make vacuum degree reach 8×10 ‑4 ～10×10 ‑4 Pa. The invention solves the problems of the prior artThe quartz coating process for producing the quartz substrate with high infrared reflectivity adopts silicon, nitrogen, silver and aluminum as coating materials, has the infrared reflectivity of more than 90 percent, and simultaneously utilizes the characteristic of low melting point of silicon to react with nitrogen to generate silicon nitride, and the silicon nitride fuses silver and aluminum particles to jointly form a silicon nitride layer, so that the reflectivity is ensured, and the strength and chemical stability of the whole film layer are improved.
Description
Technical Field
The invention relates to the technical field of quartz substrate coating, in particular to a quartz coating process for producing an infrared high-reflectivity quartz substrate.
Background
Quartz has the characteristics of transparency, high refractive index, low scattering loss and the like, and is widely applied to the fields of optical devices, optoelectronics devices and crystals.
Chinese patent publication No. CN115341183B discloses a high-precision quartz substrate coating film and its production process, wherein the coating film is provided in a double-layer structure, and is a chromium nitride coating layer on the surface layer and a release composite coating layer on the bottom layer respectively. The quartz substrate processed by the method protects the quartz substrate through the chromium nitride layer when the quartz substrate is finally used, but when the quartz substrate is applied to infrared quartz, the quartz substrate has the problem of low infrared reflectivity.
Disclosure of Invention
The invention aims to provide a quartz coating process for producing a quartz substrate with high infrared reflectivity, which solves the problems in the background technology by adopting silicon, nitrogen, silver and aluminum as coating materials and adopting silver and aluminum as metal coating materials, wherein the infrared reflectivity is as high as more than 90 percent.
In order to achieve the above purpose, the present invention provides the following technical solutions: a quartz coating process for producing a quartz substrate with high infrared reflectivity comprises the following steps:
step one: cleaning quartz substrate, removing surface dirt, preparing vacuum coating equipment, vacuumizing the coating equipment to make vacuum degree reach 8×10 -4 ～10×10 -4 Pa；
Step two: starting a coating device, heating the quartz substrate at 150-200 ℃ for 5-10min, and injecting argon into a vacuum chamber for partial pressure after heating, wherein the pressure is controlled at 0.75Pa;
step three: argon is used as sputtering gas in the coating equipment, silicon is used as a target material, oxygen is introduced as reaction gas, and a silicon dioxide film layer is formed on the quartz substrate;
step four: argon is used as sputtering gas, a silicon nitride film material is used as a target material, and a silicon nitride film is plated on the silicon dioxide film in a sputtering gas mode;
step five: after coating, annealing the substrate and the film surface at 700-800 ℃, wherein the annealing process adopts stepped heating and stepped cooling, and the quartz substrate is taken out after annealing is completed;
step six: and carrying out surface treatment on the quartz substrate.
Preferably, in the third step, the argon flow is set to be 25-35 sccm, the pressure in the equipment is 0.4-1.0 pa, and the ratio of the argon to the oxygen is 1:3.
Preferably, the silicon dioxide film layer in the third step is formed by four-cycle deposition, and the thickness of the single-cycle coating film is 1 μm.
Preferably, the silicon nitride film layer material comprises the following raw materials in parts by weight: 24-28 parts of silicon, 12-18 parts of nitrogen, 7-12 parts of silver and 2-4 parts of aluminum.
Preferably, in the fourth step, the argon flow is set to be 30-37 sccm, the pressure in the equipment is 0.6-0.8 pa, and the ratio of the argon to the nitrogen is 4:1.
Preferably, the third step and the fourth step are both performed with a pre-sputtering step before the main sputtering, and the pre-sputtering removes the target oxide film and other non-target substances by an ion bombardment method.
Preferably, in the fourth step, the silicon nitride film layer is divided into two layers, each silicon nitride film layer is formed by four times of cyclic deposition, and the thickness of the single-cycle coating film is 2 μm.
Preferably, the temperature of the step-type heating in the annealing process is 300 ℃, 400 ℃, 500 ℃, 600 ℃, 700 ℃,800 ℃, and the temperature is kept for 10min, 9min, 8min, 7min, 6min and 5min respectively, the temperature of the step-type cooling is 700 ℃, 600 ℃, 500 ℃, 400 ℃, 300 ℃, 200 ℃, 150 ℃, 100 ℃, 50 ℃, and the temperature is kept for 10min, 15min and 15min respectively.
Preferably, the surface treatment in the sixth step includes the following steps:
preparing lanthanum oxide solution, immersing the cooled quartz substrate into the lanthanum oxide solution to fully absorb lanthanum oxide in the solution, taking the quartz substrate out of the solution, and drying to form a lanthanum oxide film layer on the surface layer of the quartz substrate.
Preferably, the lanthanum oxide solution is prepared by mixing lanthanum oxide with ethanol, and the mass ratio of the lanthanum oxide to the ethanol is 1:3.
Compared with the prior art, the invention has the beneficial effects that:
a layer of silicon dioxide film is firstly plated on the surface of the quartz substrate, the silicon dioxide can improve the infrared reflectivity of the quartz substrate, and meanwhile, the silicon dioxide improves the adhesive force of the surface layer of the quartz substrate, so that a good foundation is improved for subsequent film plating; on the second layer film, silicon, nitrogen, silver and aluminum are adopted as coating materials, silver and aluminum are adopted as metal coating materials, the infrared reflectivity is up to more than 90%, meanwhile, the characteristic of low melting point of silicon is utilized to react with nitrogen to generate silicon nitride, the silicon nitride fuses silver and aluminum particles to form a silicon nitride layer together, and the strength and chemical stability of the whole film layer are improved while the reflectivity is ensured; and a third wrapping film layer is formed by lanthanum oxide, and wrapping is performed outside the quartz substrate and the coating, so that the connection firmness of the coating and the quartz substrate is improved, and the coating can be prevented from falling off.
Drawings
FIG. 1 is a flow chart of a quartz coating process of the invention.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
In order to solve the existing problems, referring to fig. 1, the present embodiment provides the following technical solutions: a quartz coating process for producing a quartz substrate with high infrared reflectivity comprises the following steps:
step one: cleaning quartz substrate to remove dirt on surface, cleaning quartz substrate dust with water, boiling with 10% NaOH solution for several minutes, cleaning with pure water and ultrasonic wave, taking out, drying with high-purity nitrogen for standby or baking in 100 deg.C oven for half an hour, preparing vacuum coating equipment, vacuumizing the coating equipment to make vacuum degree reach 8×10 -4 ～10×10 - 4 Pa；
Step two: starting a coating device, heating the quartz substrate at 150-200 ℃ for 5-10min, and injecting argon into a vacuum chamber for partial pressure after heating, wherein the pressure is controlled at 0.75Pa;
step three: argon is used as sputtering gas in the film plating equipment, silicon is used as a target, oxygen is introduced as reaction gas, a silicon dioxide film layer is formed on a quartz substrate, the argon flow is set to be 25-35 sccm, the pressure in the equipment is 0.4-1.0 pa, the ratio of the argon to the oxygen is 3:1, positive ions formed after ionization of the argon bombard the surface of the target at a high speed, so that target particles are sputtered to react with the oxygen and reach the surface of the substrate to form the silicon dioxide film layer, the silicon dioxide film layer is formed by four-time cyclic deposition, and the thickness of a single-cycle film plating is 1 mu m;
step four: using argon as sputtering gas, adopting a silicon nitride film material as a target material, plating a layer of silicon nitride film on the silicon dioxide film by using the sputtering gas, wherein positive ions formed after ionization of the argon bombard the surface of the target material at a high speed, so that silver and aluminum of the target material are sputtered by silicon particles, the melting point of the silicon particles is lowest, firstly, the silicon particles react with nitrogen to generate silicon nitride, the silver and the aluminum are fused, a layer of mixed film is formed on the silicon dioxide film together, the silver and the aluminum are distributed in the silicon nitride material, the silicon nitride material has good reflectivity for infrared rays, the clamping of the silver and the aluminum metal material is realized, the reflectivity is improved, meanwhile, the silicon nitride can improve the chemical stability and the hardness of the silver and the aluminum, the argon flow is set to be 30-37 sccm, the pressure in equipment is 0.6-0.8 pa, the proportion of the argon and the nitrogen is 4:1, the silicon nitride film is divided into two layers, each layer of silicon nitride film is formed by four times of cyclic deposition, and the thickness of a single cyclic coating film is 2 mu m;
the silicon nitride film layer material comprises the following raw materials in parts by weight: 24-28 parts of silicon, 12-18 parts of nitrogen, 7-12 parts of silver and 2-4 parts of aluminum;
and step three and step four, before formal sputtering, performing a pre-sputtering step, wherein the pre-sputtering removes the target oxide film and other non-target substances by an ion bombardment method.
Step five: after coating, annealing the substrate and the film surface, wherein the annealing temperature is 700-800 ℃, the annealing process adopts stepped heating and stepped cooling, the quartz substrate is taken out after annealing, the stepped heating temperature in the annealing process is 300 ℃, 400 ℃, 500 ℃, 600 ℃, 700 ℃,800 ℃, 10min, 9min, 8min, 7min, 6min and 5min respectively, the stepped cooling temperature is 700 ℃, 600 ℃, 500 ℃, 400 ℃, 300 ℃, 200 ℃, 150 ℃, 100 ℃, 50 ℃, 10min, 15min and 15min respectively, and the gradient cooling is carried out in a manner of relatively directly closing heating and naturally cooling, so that the aging effect is better, and the firmness of the film can be obviously improved;
step six: surface treatment is carried out on the quartz substrate, wherein the surface treatment comprises the following steps:
preparing a lanthanum oxide solution, immersing the cooled quartz substrate into the lanthanum oxide solution to fully absorb lanthanum oxide in the solution, taking the quartz substrate out of the solution, drying the solution to form a lanthanum oxide film layer on the surface layer of the quartz substrate, wherein the lanthanum oxide solution is prepared by mixing lanthanum oxide with ethanol, the mass ratio of the lanthanum oxide to the ethanol is 1:3, and the lanthanum oxide layer is added to improve the anti-fouling and wear-resisting capabilities of the quartz substrate, wrap the whole quartz substrate and the film coating layer, and improve the compactness of the film coating.
Embodiment one:
the silicon dioxide film layer comprises the following raw materials in parts by weight: 12 parts of silicon and 8 parts of oxygen;
the silicon nitride film layer material comprises the following raw materials in parts by weight: 24 parts of silicon, 12 parts of nitrogen, 12 parts of silver and 2 parts of aluminum;
the quartz substrate is coated by adopting the method.
Embodiment two:
the silicon dioxide film layer comprises the following raw materials in parts by weight: 12 parts of silicon and 8 parts of oxygen;
the silicon nitride film layer material comprises the following raw materials in parts by weight: 30 parts of silicon, 12 parts of nitrogen, 12 parts of silver and 2 parts of aluminum;
the quartz substrate is coated by adopting the method.
Embodiment III:
the silicon dioxide film layer comprises the following raw materials in parts by weight: 12 parts of silicon and 8 parts of oxygen;
the silicon nitride film layer material comprises the following raw materials in parts by weight: 24 parts of silicon, 12 parts of nitrogen, 7 parts of silver and 2 parts of aluminum;
the quartz substrate is coated by adopting the method.
Comparative example one:
the silicon dioxide film layer comprises the following raw materials in parts by weight: 12 parts of silicon and 8 parts of oxygen;
the silicon nitride film layer material comprises the following raw materials in parts by weight: 24 parts of silicon, 12 parts of nitrogen and 2 parts of aluminum;
the quartz substrate is coated by adopting the method.
Comparative example two:
the silicon dioxide film layer comprises the following raw materials in parts by weight: 12 parts of silicon and 8 parts of oxygen;
the silicon nitride film layer material comprises the following raw materials in parts by weight: 24 parts of silicon, 12 parts of nitrogen, 7 parts of silver and 2 parts of aluminum;
the quartz substrate is coated by the method, but the step six is not performed, and the surface treatment of the quartz substrate is omitted.
Examples and comparative examples were tested: respectively preparing the film structures of the examples and the comparative examples, randomly selecting 10 x 10cm film area for detection, and observing the film coating quality of the intercepted samples;
as can be seen from the table, the film body processed in the embodiment has no difference in appearance quality, hardness, reflectivity and film falling-off condition, wherein the addition amount of silver in the third embodiment is reduced, the reflectivity of infrared light above 800nm is lower, and in the first comparative example, because no silver is added, the reflectivity of infrared light is lower, in a scratch experiment, 5 x 5 square grids are marked on a detection film layer by adopting a square grid method, the angle between the cuts is 30-40 degrees, an ISO adhesive tape is firmly adhered to square grid paper, after the adhesive tape is torn off, the film layer falls off in the second comparative example, the lanthanum oxide film layer is not plated in the second comparative example, and the film layer is poor in firmness.
To sum up: according to the quartz coating process for producing the quartz substrate with high infrared reflectivity, a layer of silicon dioxide film is coated on the surface of the quartz substrate, the infrared reflectivity of the quartz substrate can be improved by silicon dioxide, meanwhile, the adhesive force of the surface layer of the quartz substrate is improved by silicon dioxide, and a good foundation is improved for subsequent coating; on the second layer film, silicon, nitrogen, silver and aluminum are adopted as coating materials, silver and aluminum are adopted as metal coating materials, the infrared reflectivity is up to more than 90%, meanwhile, the characteristic of low melting point of silicon is utilized to react with nitrogen to generate silicon nitride, the silicon nitride fuses silver and aluminum particles to form a silicon nitride layer together, and the strength and chemical stability of the whole film layer are improved while the reflectivity is ensured; and a third wrapping film layer is formed by lanthanum oxide, and wrapping is performed outside the quartz substrate and the coating, so that the connection firmness of the coating and the quartz substrate is improved, and the coating can be prevented from falling off.
It is noted that relational terms such as first and second, and the like are used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Moreover, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus.
Although embodiments of the present invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made therein without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (10)
1. The quartz coating process for producing the quartz substrate with high infrared reflectivity is characterized by comprising the following steps of:
step one: cleaning quartz substrate, removing surface dirt, preparing vacuum coating equipment, vacuumizing the coating equipment to make vacuum degree reach 8×10 -4 ～10×10 -4 Pa；
Step two: starting a coating device, heating the quartz substrate at 150-200 ℃ for 5-10min, and injecting argon into a vacuum chamber for partial pressure after heating, wherein the pressure is controlled at 0.75Pa;
step three: argon is used as sputtering gas in the coating equipment, silicon is used as a target material, oxygen is introduced as reaction gas, and a silicon dioxide film layer is formed on the quartz substrate;
step four: argon is used as sputtering gas, a silicon nitride film material is used as a target material, and a silicon nitride film is plated on the silicon dioxide film in a sputtering gas mode;
step five: after coating, annealing the substrate and the film surface at 700-800 ℃, wherein the annealing process adopts stepped heating and stepped cooling, and the quartz substrate is taken out after annealing is completed;
step six: and carrying out surface treatment on the quartz substrate.
2. The quartz coating process for producing an infrared high-reflectivity quartz substrate according to claim 1, wherein: in the third step, the argon flow is set to be 25-35 sccm, the pressure in the equipment is 0.4-1.0 pa, and the ratio of the argon to the oxygen is 1:3.
3. The quartz coating process for producing an infrared high-reflectivity quartz substrate according to claim 1, wherein: the silicon dioxide film layer in the third step is formed by four times of cyclic deposition, and the thickness of the single-cycle coating film is 1 mu m.
4. The process for coating a quartz substrate for producing an infrared high-reflectivity quartz according to claim 3, wherein: the silicon nitride film layer material comprises the following raw materials in parts by weight: 24-28 parts of silicon, 12-18 parts of nitrogen, 7-12 parts of silver and 2-4 parts of aluminum.
5. The quartz coating process for producing an infrared high-reflectivity quartz substrate according to claim 1, wherein: in the fourth step, the argon flow is set to be 30-37 sccm, the pressure in the equipment is 0.6-0.8 pa, and the ratio of the argon to the nitrogen is 4:1.
6. The quartz coating process for producing an infrared high-reflectivity quartz substrate according to claim 1, wherein: and step three and step four, before formal sputtering, performing a pre-sputtering step, wherein the pre-sputtering removes the target oxide film by an ion bombardment method.
7. The quartz coating process for producing an infrared high-reflectivity quartz substrate according to claim 1, wherein: in the fourth step, the silicon nitride film layer is divided into two layers, each silicon nitride film layer is formed by four times of cyclic deposition, and the thickness of the single cyclic coating film is 2 mu m.
8. The process for coating a quartz substrate for producing an infrared high-reflectivity quartz according to claim 7, wherein: the temperature of the step-type heating in the annealing process is 300 ℃, 400 ℃, 500 ℃, 600 ℃, 700 ℃,800 ℃, and the temperature is respectively kept for 10min, 9min, 8min, 7min, 6min and 5min, the temperature of the step-type cooling is respectively 700 ℃, 600 ℃, 500 ℃, 400 ℃, 300 ℃, 200 ℃, 150 ℃, 100 ℃, 50 ℃, and the temperature is respectively kept for 10min, 15min and 15min.
9. The quartz coating process for producing an infrared high-reflectivity quartz substrate according to claim 1, wherein: the surface treatment in the step six comprises the following steps:
preparing lanthanum oxide solution, immersing the cooled quartz substrate into the lanthanum oxide solution to fully absorb lanthanum oxide in the solution, taking the quartz substrate out of the solution, and drying to form a lanthanum oxide film layer on the surface layer of the quartz substrate.
10. The quartz coating process for producing an infrared high-reflectivity quartz substrate according to claim 9, wherein: the lanthanum oxide solution is prepared by mixing lanthanum oxide with ethanol, and the mass ratio of the lanthanum oxide to the ethanol is 1:3.
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