CN112813411A - Preparation method of thick infrared optical material - Google Patents
Preparation method of thick infrared optical material Download PDFInfo
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- CN112813411A CN112813411A CN202011583651.XA CN202011583651A CN112813411A CN 112813411 A CN112813411 A CN 112813411A CN 202011583651 A CN202011583651 A CN 202011583651A CN 112813411 A CN112813411 A CN 112813411A
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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
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
- C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
- C23C16/305—Sulfides, selenides, or tellurides
- C23C16/306—AII BVI compounds, where A is Zn, Cd or Hg and B is S, Se or Te
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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
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
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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
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/56—After-treatment
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Abstract
The present disclosure provides a method for preparing a thick-sized infrared optical material. Which comprises the following steps: (S1): grinding and polishing an infrared optical material obtained by a chemical vapor deposition method as a substrate; (S2): carrying out plasma cleaning on the substrate; (S3): placing the substrate in a deposition chamber of a chemical vapor deposition furnace, and filling a crucible in the chemical vapor deposition furnace with reaction solids; (S4): vacuumizing the chemical vapor deposition furnace; (S5): slowly raising the temperature of the deposition chamber to 600-850 ℃; slowly raising the temperature of the crucible to 500-800 ℃; (S6): respectively taking the vapor of the reaction solid and the reaction gas as raw materials, and taking argon as the vapor of the reaction solid and the carrier gas of the reaction gas to be introduced into the deposition chamber; (S7): after the reaction solid in the crucible is evaporated, stopping introducing the reaction gas into the deposition chamber, and cooling the deposition chamber and the crucible; (S8): grinding and polishing, then placing in a hot isostatic pressing furnace, and carrying out constant-temperature and constant-pressure treatment for 40-250 h; (S9): and (5) cooling and depressurizing, and then discharging from the furnace.
Description
Technical Field
The disclosure relates to the technical field of chemical industry, in particular to a preparation method of a thick-size infrared optical material.
Background
Zinc sulfide (ZnS) is an infrared optical material which has the only transmission waveband covering visible light to long-wave infrared full waveband except diamond, has stronger spectral adaptability, high mechanical strength, good moisture resistance, good thermal shock resistance, stable chemical property and moderate linear expansion coefficient, is closer to a plurality of metals or alloys, and is considered as a better infrared optical material at present.
The main method for preparing ZnS at present is a chemical vapor deposition method (CVD method), which uses a chemical vapor deposition device (vacuum furnace), wherein the vacuum furnace is provided with a crucible and a deposition chamber from bottom to top, the crucible is used for containing zinc materials, and the deposition chamber is used for carrying out chemical reaction on reactants; with solid zinc and H2S gas is used as a raw material, argon (Ar) is used as a carrier gas, the equipment is vacuumized through a vacuum pump, and the deposition pressure in the equipment is controlled to be 3000-10000 Pa. Evaporating the solid Zn in the crucible into Zn vapor in the temperature range of 500-800 ℃, carrying the Zn vapor into the deposition chamber by argon, and carrying the Zn vapor into the deposition chamber by the argon2The S gas is subjected to chemical reaction at the temperature range of 600-850 ℃ to obtain ZnS, the molar ratio of the zinc to the hydrogen sulfide is controlled to be 1: 1-1.5: 1, and ZnS molecules are deposited on the graphite substrate and continuously grow.
In the process, as the solid zinc raw material is put in a crucible in a vacuum furnace, when the zinc material is evaporated to be dry, the deposition is finished, and the deposition growth cannot be continued, the zinc material loading in the furnace is limited by the volume of the crucible, and a zinc sulfide product with thicker size cannot grow; furthermore, the thicker the zinc sulphide product to be obtained, the longer the time required for deposition, which will be a great challenge for the stability of the operation of the whole deposition system equipment, and in case of failure of one of the critical system equipment, the product will not continue to grow and deposition has to be stopped.
Disclosure of Invention
In view of the problems in the background art, the present disclosure is directed to a method for manufacturing a thick-sized infrared optical material, which can manufacture a thick-sized infrared optical material, and the manufactured thick-sized infrared optical material has good quality, and can eliminate the defect of secondary deposition at the interface.
In order to achieve the above object, the present disclosure provides a method for preparing a thick-sized infrared optical material, comprising the steps of: (S1): taking an infrared optical material obtained by a chemical vapor deposition method as a substrate, and grinding and polishing the substrate; (S2): carrying out plasma cleaning on the substrate; (S3): placing the substrate in a deposition chamber of a chemical vapor deposition furnace, and filling a high-purity reaction solid into a crucible in the chemical vapor deposition furnace; (S4): vacuumizing the chemical vapor deposition furnace; (S5): slowly raising the temperature of the deposition chamber to 600-850 ℃; slowly raising the temperature of the crucible to 500-800 ℃, wherein the reaction solid in the crucible is converted into steam; (S6): respectively taking the steam and the reaction gas of the reaction solid as raw materials, taking argon as the steam of the reaction solid and the carrier gas of the reaction gas, and introducing the steam and the carrier gas into a deposition chamber, wherein the ratio range of the flow of the argon carrying the reaction gas to the flow of the reaction gas is 10-25; the ratio of the flow of the argon carrying the steam to the flow of the steam is 3-10; the molar ratio of the vapor of the reaction solid to the reaction gas is 1.0-1.5 during the deposition process; (S7): after the reaction solid in the crucible is evaporated, stopping introducing the reaction gas into the deposition chamber, and cooling the deposition chamber and the crucible to obtain thick plates; (S8): grinding and polishing the thick plate, and then placing the thick plate in a hot isostatic pressing furnace for hot isostatic pressing treatment, wherein the constant-temperature and constant-pressure treatment time is 40-250 h; (S9): and after the treatment is finished, cooling and depressurizing the hot isostatic pressing furnace, and then discharging the hot isostatic pressing furnace to finally obtain the thick infrared optical material.
In one embodiment, the reactant gas is hydrogen sulfide and the reactant solid is zinc.
In one embodiment, in the step (S1), the substrate has a thickness of 10-30mm, and the roughness of the ground and polished substrate is less than ra 12.5.
In one embodiment, in the step (S5), the temperature rise rate of the deposition chamber is 0.2 deg.C-1.5 deg.C/min; the temperature rise rate of the crucible is 0.5-3 ℃/min.
In one embodiment, in step (S7), the thickness of the resulting thick-sized board is 30-60 mm.
In one embodiment, in step (S9), the thickness of the thick-sized infrared optical material is 30-60 mm.
In one embodiment, in the step (S6), during the deposition process, the reaction solid vapor carried by the argon gas and the reaction gas carried by the argon gas are chemically reacted in the deposition chamber to generate the product, and the deposition rate of the product is controlled to be 20-100 μm/h.
The beneficial effects of this disclosure are as follows: according to the preparation method of the thick-size infrared optical material, secondary deposition is carried out on a product subjected to primary chemical vapor deposition to obtain a thick-size plate material which is thicker than the product subjected to primary chemical vapor deposition, and then the thick-size plate material subjected to secondary chemical vapor deposition is subjected to heat equal-pressure treatment, so that the internal defects of the thick-size plate material can be effectively eliminated.
Detailed Description
The preparation method of the thick-size infrared optical material adopts the existing chemical vapor deposition furnace and hot isostatic pressing furnace for preparation, and comprises the following steps:
(S1): the infrared optical material obtained by a chemical vapor deposition method is used as a substrate, and the substrate is ground and polished. In this step, the substrate is a product directly obtained through one chemical vapor deposition, and the thickness of the obtained substrate is 10mm to 30mm due to the limitations of equipment and processes. The roughness of the ground and polished substrate is less than Ra12.5.
(S2): the substrate is plasma cleaned, and impurities on the surface of the substrate can be effectively removed.
(S3): the substrate is placed in a deposition chamber of a chemical vapor deposition furnace and a crucible in the chemical vapor deposition furnace is filled with a high purity reaction solid. Specifically, the purity of the high purity reaction solid was 99.999%. In one embodiment, the reaction solid is a high purity zinc ingot.
(S4): vacuumizing the chemical vapor deposition furnace, detecting leakage, and controlling the pressure value in the deposition chamber to 3000-10000 Pa.
(S5): slowly raising the temperature of the deposition chamber to 600-850 ℃, wherein the temperature raising rate is 0.2-1.5 ℃/min; the temperature of the crucible is slowly raised to 800 ℃ below zero at a heating rate of 0.5-3 ℃/min, wherein when the temperature of the crucible is raised to 800 ℃ below zero at 500 ℃, the reaction solid in the crucible is converted into vapor. In one embodiment, the crucible is a graphite crucible.
(S6): respectively taking the vapor of the reaction solid and the reaction gas as raw materials, taking argon as the carrier gas of the vapor of the reaction solid and the carrier gas of the reaction gas, and introducing the raw materials into a deposition chamber, wherein the ratio range of the flow of the argon carrying the reaction gas to the flow of the reaction gas is 10-25; the ratio of the flow of argon carrying the vapor of the reaction solid to the vapor flow is in the range of 3-10; in the deposition process, the mol ratio of the vapor of the reaction solid to the reaction gas is 1.0-1.5, the vapor of the reaction solid carried by the argon gas and the reaction gas carried by the argon gas generate chemical reaction in the deposition chamber to generate a product, and the deposition rate of the product is controlled to be 20-100 mu m/h. In one embodiment, the reactant gas is hydrogen sulfide and the reactant solid is zinc. Thus, the ratio of the flow of argon carrying hydrogen sulfide to the flow of hydrogen sulfide is Ar: H210-25% of S; the ratio of the flow of the argon carrying the zinc vapor to the flow of the zinc vapor is Ar, Zn, 3-10; molar ratio of zinc vapour to hydrogen sulphide Zn: H2And S is 1.0-1.5. The purity of the introduced argon is 99.999 percent, the purity of the zinc ingot is 99.999 percent, and the purity of the hydrogen sulfide is 99.999 percent.
(S7): and stopping introducing the reaction gas into the deposition chamber after the evaporation of the raw materials in the crucible is finished, and cooling the deposition chamber and the crucible to obtain the thick-size plate. The thickness of the obtained thick-size plate is 30-60 mm. That is, the thickness of the thick-sized slab is equal to the sum of the thickness of the newly deposited reactant and the thickness of the substrate in the step (S1), and thus, a thick-sized slab, which cannot be obtained by one chemical vapor deposition, is obtained by the second deposition.
(S8): and grinding and polishing the thick plate, and then placing the thick plate in a hot isostatic pressing furnace for hot isostatic pressing treatment, wherein the constant-temperature and constant-pressure treatment time is 40-250 h. The treatment temperature of the hot isostatic pressing treatment is 800-1100 ℃, and the pressure is 100-150 MPa. The hot isostatic pressing technology can enable all surfaces of the plate to be subjected to the pressure of gas in a balanced manner in all directions at high temperature, and can effectively reduce or eliminate the defects of micropores, delamination and the like at the interface boundary of primary deposition and secondary deposition of the plate, so that the thick infrared optical material with good compactness and high consistency is obtained.
(S9): and after the treatment is finished, cooling and depressurizing the hot isostatic pressing furnace, and then discharging the hot isostatic pressing furnace to finally obtain the thick infrared optical material. Specifically, the thickness of the obtained thick-size infrared optical material is 30-60 mm.
According to the preparation method of the thick-size infrared optical material, secondary deposition is directly carried out on a product subjected to primary chemical vapor deposition to obtain a thick-size plate material which is thicker than the product subjected to primary chemical vapor deposition, then the thick-size plate material subjected to secondary chemical vapor deposition is subjected to heat equal pressurization treatment, and the internal defects of the thick-size plate material can be effectively eliminated.
The thick multispectral zinc sulfide material is prepared by using reaction gas as high-purity hydrogen sulfide and reaction solid as high-purity zinc ingot according to the preparation method of the thick infrared optical material disclosed by the invention.
In example 1, a primary zinc sulfide flat plate (a primary deposited zinc sulfide substrate) was cut, ground, and polished to obtain a flat plate having a roughness of ra0.4 and a specification of 250 × 250 × 20mm, and after plasma cleaning, the flat plate was mounted in a graphite depositor of a chemical vapor deposition furnace, a high-purity 5N zinc material was charged into a crucible, about 200KG was charged into the furnace, the deposition furnace was evacuated and pressure-maintained, leak detection was performed, after the furnace pressure rise rate was acceptable, a high-purity 5N argon gas was introduced, temperature programming was started, the vacuum pressure in the furnace was maintained at 6000Pa, the crucible temperature rise rate was 0.5 ℃/min, and the target temperature was raised to 630 ℃. The heating rate of the deposition chamber is 0.7 ℃/min, the target temperature is raised to 680 ℃, the flow of high-purity argon for carrying zinc vapor is introduced into the crucible for 30L/min, the evaporation rate of zinc is controlled to be about 3L/min, and the flow ratio of argon to zinc vapor is Ar: zn is 10; the flow rate of high-purity argon for diluting hydrogen sulfide is 30L/min, the flow rate of hydrogen sulfide is 2.7L/min, and the flow ratio Ar of argon to hydrogen sulfide is as follows: h2S is 11.1, after the deposition chamber reaches the deposition temperature, hydrogen sulfide and zinc vapor are introduced to start depositionAfter the zinc in the crucible is evaporated, the deposition is finished, the crucible and the deposition chamber are cooled to room temperature, a small amount of hydrogen sulfide is introduced in the cooling process (so that the zinc vapor in the deposition chamber is consumed), the crucible cooling rate is 0.35 ℃/min, the deposition chamber cooling rate is 0.3 ℃/min, and secondary deposition thick-size zinc sulfide plates with the thickness of more than 40mm can be obtained after the plates are taken out of the furnace. Grinding and polishing the zinc sulfide plate material subjected to secondary deposition to obtain a zinc sulfide plate material with the roughness of Ra12.5 and the size of 240 multiplied by 40 mm; mounting the sheet in a hot isostatic pressing furnace; heating and pressurizing the hot isostatic pressing furnace; the target temperature is reached to 850 ℃, and the pressure is 140 MPa; keeping the temperature and the pressure constant for 120 hours; and cooling and extruding the mixture out of the furnace to obtain a multispectral zinc sulfide flat plate with the thickness of 40 mm. The zinc sulfide flat plate formed by the method has the thickness of 40mm, has stronger spectrum adaptability and meets the requirements of the thickness and the performance of the product.
In example 2, a primary zinc sulfide flat plate was cut, ground, and polished to obtain a substrate having a roughness of ra0.4 and a specification of 250 × 250 × 25mm, and after plasma cleaning, the substrate was put into a graphite depositor installed in a chemical vapor deposition furnace, a high-purity 5N zinc material of about 200KG was charged into a crucible, the furnace was closed, vacuum-pumping and pressure-maintaining were performed, leak-checking was performed, after the furnace pressure rise rate was qualified, high-purity 5N argon gas was introduced, programmed temperature rise was started, a vacuum pressure of 6000Pa was maintained, a crucible temperature rise rate of 0.5 ℃/min was maintained, and a target temperature was raised to 650 ℃. The heating rate of the deposition chamber is 0.7 ℃/min, the target temperature is increased to 690 ℃, the flow of high-purity argon carrying zinc vapor in the crucible is 30L/min, the evaporation rate of zinc is controlled to be about 3.5L/min, and the flow ratio Ar: zn 8.5, a high purity argon flow for hydrogen sulfide dilution of 30L/min, a hydrogen sulfide flow of 3L/min, Ar: h2After the deposition temperature is reached, introducing hydrogen sulfide and zinc vapor to start deposition, finishing the evaporation of the zinc in the crucible, finishing the deposition, cooling the crucible and the deposition chamber to room temperature, and introducing a small amount of hydrogen sulfide in the process; the temperature reduction rate of the crucible is 0.35 ℃/min, the temperature reduction rate of the deposition chamber is 0.3 ℃/min, and secondary deposition thick-size zinc sulfide plates with the thickness of more than 45mm can be obtained after the zinc sulfide plates are taken out of the furnace. Grinding and polishing the secondarily deposited thick-size zinc sulfide plate to obtain a thick-size zinc sulfide plate with the roughness of Ra12.5 and the size of 240 mm multiplied by 45 mm; mounting the sheet in a hot isostatic pressing furnacePerforming the following steps; heating and pressurizing the hot isostatic pressing furnace; the target temperature is reached to 850 ℃, and the pressure is 140 MPa; keeping the temperature and the pressure constant for 150 hours; and cooling, depressurizing and discharging to obtain the multispectral zinc sulfide flat plate with the thickness of 45 mm. The zinc sulfide flat plate formed by the method has the thickness of 45mm, has stronger spectrum adaptability and meets the requirements of the thickness and the performance of the product.
In example 3, a primary zinc sulfide flat plate was cut, ground, and polished to obtain a substrate having a roughness of ra0.4 and a specification of 220 × 220 × 30mm, and after plasma cleaning, the substrate was put into a graphite deposition apparatus installed in a chemical vapor deposition furnace, a high-purity 5N zinc material, about 200KG, and the furnace was closed, and after vacuum pumping, pressure maintaining, leak detection, and the furnace pressure rise rate was qualified, high-purity 5N argon gas was introduced, programmed temperature rise was started, the vacuum pressure of 6000Pa was maintained, the crucible temperature rise rate was 0.5 ℃/min, and the target temperature was raised to 650 ℃. The heating rate of the deposition chamber is 0.7 ℃/min, the target temperature is increased to 690 ℃, the flow of high-purity argon carrying zinc vapor in the crucible is 30L/min, the evaporation rate of zinc is controlled to be about 3.3L/min, and the flow ratio Ar: zn 9, a high purity argon gas flow for hydrogen sulfide dilution of 30L/min, a hydrogen sulfide flow of 3L/min, Ar: h2And S is 10: 1, after the deposition temperature is reached, introducing hydrogen sulfide to start deposition, completely evaporating zinc in a crucible, completing deposition, cooling the crucible and a deposition chamber to room temperature, and introducing a small amount of hydrogen sulfide in the process; the temperature reduction rate of the crucible is 0.35 ℃/min, the temperature reduction rate of the deposition chamber is 0.3 ℃/min, and secondary deposition thick-size zinc sulfide plates with the thickness of more than 50mm can be obtained after the zinc sulfide plates are taken out of the furnace. Grinding and polishing the secondarily deposited thick-size zinc sulfide plate to obtain a thick-size zinc sulfide plate with the roughness of Ra12.5 and the size of 200 multiplied by 50 mm; mounting the sheet in a hot isostatic pressing furnace; heating and pressurizing the hot isostatic pressing furnace; the target temperature is reached to 850 ℃, and the pressure is 140 MPa; keeping the temperature and the pressure constant for 180 hours; and cooling and extruding the mixture out of the furnace to obtain a multispectral zinc sulfide flat plate with the thickness of 50 mm. The zinc sulfide flat plate formed by the method has the thickness of 50mm, has stronger spectrum adaptability and meets the requirements of the thickness and the performance of the product.
From the three embodiments, the preparation method of the thick infrared optical material disclosed by the invention can be used for effectively preparing the thick and high-quality multispectral zinc sulfide material by combining the secondary chemical vapor deposition method and the hot isostatic pressing technology, so that the limitation of chemical vapor deposition equipment on the thickness of a deposited product is avoided, and the production efficiency is improved.
Claims (7)
1. A preparation method of a thick-size infrared optical material is characterized by comprising the following steps:
(S1): taking an infrared optical material obtained by a chemical vapor deposition method as a substrate, and grinding and polishing the substrate;
(S2): carrying out plasma cleaning on the substrate;
(S3): placing the substrate in a deposition chamber of a chemical vapor deposition furnace, and filling a high-purity reaction solid into a crucible in the chemical vapor deposition furnace;
(S4): vacuumizing the chemical vapor deposition furnace;
(S5): slowly raising the temperature of the deposition chamber to 600-850 ℃; slowly raising the temperature of the crucible to 500-800 ℃, wherein the reaction solid in the crucible is converted into steam;
(S6): respectively taking the steam and the reaction gas of the reaction solid as raw materials, taking argon as the steam of the reaction solid and the carrier gas of the reaction gas, and introducing the steam and the carrier gas into a deposition chamber, wherein the ratio range of the flow of the argon carrying the reaction gas to the flow of the reaction gas is 10-25; the ratio of the flow of the argon carrying the steam to the flow of the steam is 3-10; the molar ratio of the vapor of the reaction solid to the reaction gas is 1.0-1.5 during the deposition process;
(S7): after the reaction solid in the crucible is evaporated, stopping introducing the reaction gas into the deposition chamber, and cooling the deposition chamber and the crucible to obtain thick plates;
(S8): grinding and polishing the thick plate, and then placing the thick plate in a hot isostatic pressing furnace for hot isostatic pressing treatment, wherein the constant-temperature and constant-pressure treatment time is 40-250 h;
(S9): and after the treatment is finished, cooling and depressurizing the hot isostatic pressing furnace, and then discharging the hot isostatic pressing furnace to finally obtain the thick infrared optical material.
2. The method of claim 1, wherein the reactive gas is hydrogen sulfide and the reactive solid is zinc.
3. The method for preparing a thick size infrared optical material as set forth in claim 1, wherein in the step (S1), the thickness of the substrate is 10-30mm, and the roughness of the ground and polished substrate is less than ra12.5.
4. The method for preparing a thick-sized infrared optical material as claimed in claim 1, wherein, in the step (S5), the temperature rising rate of the deposition chamber is 0.2 ℃ to 1.5 ℃/min; the temperature rise rate of the crucible is 0.5-3 ℃/min.
5. The method for preparing a thick-sized infrared optical material as set forth in claim 3, wherein in the step (S7), the thickness of the resulting thick-sized board is 30-60 mm.
6. The method for preparing a thick-sized infrared optical material as set forth in claim 5, wherein in the step (S9), the thickness of the thick-sized infrared optical material is 30 to 60 mm.
7. The method for preparing a thick-sized infrared optical material as claimed in claim 1, wherein in the step (S6), the reaction solid vapor carried by argon gas and the reaction gas carried by argon gas are chemically reacted in the deposition chamber during the deposition process to generate the product, and the deposition rate of the product is controlled to be 20-100 μm/h.
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| CN115465840A (en) * | 2022-09-30 | 2022-12-13 | 先导薄膜材料（广东）有限公司 | High-purity metal sulfide and preparation method and application thereof |
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| CN115465840A (en) * | 2022-09-30 | 2022-12-13 | 先导薄膜材料（广东）有限公司 | High-purity metal sulfide and preparation method and application thereof |
| CN115465840B (en) * | 2022-09-30 | 2024-01-23 | 先导薄膜材料（广东）有限公司 | High-purity metal sulfide and preparation method and application thereof |
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