CN112095150B - Growth method of zinc selenide - Google Patents
Growth method of zinc selenide Download PDFInfo
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- CN112095150B CN112095150B CN202011041984.XA CN202011041984A CN112095150B CN 112095150 B CN112095150 B CN 112095150B CN 202011041984 A CN202011041984 A CN 202011041984A CN 112095150 B CN112095150 B CN 112095150B
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/46—Sulfur-, selenium- or tellurium-containing compounds
- C30B29/48—AIIBVI compounds wherein A is Zn, Cd or Hg, and B is S, Se or Te
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B28/00—Production of homogeneous polycrystalline material with defined structure
- C30B28/12—Production of homogeneous polycrystalline material with defined structure directly from the gas state
- C30B28/14—Production of homogeneous polycrystalline material with defined structure directly from the gas state by chemical reaction of reactive gases
Abstract
The present disclosure provides a growth method of zinc selenide comprising the steps of: a. putting zinc into a crucible in a chemical vapor deposition furnace, replacing air in the deposition furnace with argon, and vacuumizing to reach a vacuum degree of 3000-10000 Pa; b. heating a deposition chamber in a chemical vapor deposition furnace to the deposition temperature of 700-800 ℃, and heating a crucible to the evaporation temperature of 650-700 ℃; c. respectively introducing gas into a crucible and a deposition chamber to perform a vapor deposition reaction of zinc selenide, introducing argon into the crucible, and introducing argon and hydrogen selenide into the deposition chamber, so that the deposition rate of the zinc selenide is 50-150 mu m/h; d. after the reaction is finished, maintaining the same pressure and gas flow as those in the deposition process, continuously heating the deposition chamber to 50-170 ℃, keeping the temperature constant for the first time, then cooling to the range of 500-650 ℃, keeping the temperature constant again, and then cooling to the room temperature to obtain the zinc selenide product. The growth method of zinc selenide provided by the disclosure can produce the polycrystalline zinc selenide material with large size, thickened size and high optical performance.
Description
Technical Field
The disclosure relates to the field of infrared materials, in particular to a growth method of zinc selenide.
Background
Chinese patent publication No. CN101759161B discloses a method for preparing zinc selenide with high optical quality, which mentions that the deposition pressure of zinc selenide is 1 × 104-5×104Pa, deposition temperature of 650-800 ℃, flow rate of hydrogen selenide of 0.5-2L/min, flow rate of argon of 5-20L/min, and molar ratio of zinc to hydrogen selenide of 0.8-1.2. The zinc selenide deposition vacuum degree value mentioned in the patent is large, the pressure is large, the zinc selenide growth rate is too large, the defects in the product are increased, including a fog layer, fog spots, impurities, bubbles and the like, meanwhile, the hydrogen selenide deposition vacuum degree value mentioned in the patent is 0.5-2L/min, the molar ratio of zinc to hydrogen selenide is 0.8-1.2, the introduction amount of a reactant is small, and the cost is very high for industrial production. In addition, because no diluent gas is added in the evaporation process of zinc, the zinc vapor in the crucible enters the deposition chamber to be mixed with hydrogen selenide for reaction, so that the zinc vapor is difficult to be fully diffused in a larger deposition chamber, the problems of smaller size and uneven thickness of the product are caused, and the requirement of a large-size zinc selenide product cannot be met. In addition, a certain growth rate needs to be ensured in the deposition process of the zinc selenide, so that a large-size thicker zinc selenide product can be grown. Finally, zinc selenide belongs to an infrared material, the product is brittle, large stress exists in the product in the deposition process, and if the stress cannot be released well, the product is easy to crack in the cooling or subsequent processing process.
The above description is merely provided as background and is not an admission that the above "background" constitutes prior art to the present disclosure.
Disclosure of Invention
In view of the problems of the background art, it is an object of the present disclosure to provide a growth method of zinc selenide, which can produce a polycrystalline zinc selenide material with large size, thickened size, and high optical performance.
In one embodiment, the disclosed growth method of zinc selenide comprises the steps of:
a. putting zinc into a crucible in a chemical vapor deposition furnace, replacing air in the deposition furnace with argon, vacuumizing, and maintaining the vacuum degree in the furnace to be 3000-10000 Pa;
b. heating a chemical vapor deposition furnace, heating a deposition chamber in the chemical vapor deposition furnace to the deposition temperature of 700-800 ℃, and heating a crucible to the evaporation temperature of 650-700 ℃;
c. respectively introducing gas into a crucible and a deposition chamber to perform a vapor deposition reaction of zinc selenide, introducing argon into the crucible, and introducing argon and hydrogen selenide into the deposition chamber, so that the deposition rate of the zinc selenide is 50-150 mu m/h;
d. after the reaction is finished, maintaining the same pressure and gas flow as those in the deposition process, continuously heating the deposition chamber to 50-170 ℃, keeping the temperature constant for the first time, then cooling to the range of 500-650 ℃, keeping the temperature constant again, and then cooling to the room temperature to obtain the zinc selenide product.
The beneficial effects of this disclosure are as follows:
the growth method of the zinc selenide can solve the size problem of a growing product, improve the growth rate of the product, reduce the production cost, effectively eliminate the stress in the product, improve the utilization rate of the product and be suitable for producing the polycrystalline zinc selenide material with large size, thickened size and high optical performance.
Detailed Description
It is to be understood that the disclosed embodiments are merely exemplary of the disclosure that may be embodied in various forms, and that specific details of the disclosure are not to be interpreted as limiting, but merely as a basis for the claims and as a representative basis for teaching one skilled in the art to variously employ the disclosure.
In the description of the present disclosure, terms and terms not specifically described are common general knowledge of those skilled in the art, and methods not specifically described are conventional methods known to those skilled in the art.
In the description of the present disclosure, the chemical vapor deposition furnace is a chemical vapor deposition apparatus known in the art, and the structure thereof includes a crucible, a deposition chamber for depositing a product, a vacuum system for maintaining a vacuum degree of the chemical vapor deposition furnace, and a gas supply system for supplying gas into the chemical vapor deposition furnace, wherein the gas supply system can supply gas into the crucible and/or the deposition chamber.
The following describes the growth method of zinc selenide provided by the present disclosure in detail.
The growth method of the zinc selenide mainly comprises four steps of vacuumizing, temperature programming, chemical vapor deposition and stress relief.
In one embodiment, the disclosed growth method of zinc selenide comprises the steps of:
a. putting zinc into a crucible in a chemical vapor deposition furnace, replacing air in the deposition furnace with argon, and vacuumizing to reach a vacuum degree of 3000-10000 Pa;
b. heating a chemical vapor deposition furnace, heating a deposition chamber in the chemical vapor deposition furnace to the deposition temperature of 700-800 ℃, and heating a crucible to the evaporation temperature of 650-700 ℃;
c. respectively introducing gas into a crucible and a deposition chamber to perform a vapor deposition reaction of zinc selenide, introducing argon into the crucible, and introducing argon and hydrogen selenide into the deposition chamber, so that the deposition rate of the zinc selenide is 50-150 mu m/h;
d. after the reaction is finished, maintaining the same pressure and gas flow as those in the deposition process, continuously heating the deposition chamber to 50-170 ℃, keeping the temperature constant for the first time, then cooling to the range of 500-650 ℃, keeping the temperature constant again, and then cooling to the room temperature to obtain the zinc selenide product.
In one embodiment, step a is vacuuming, step b is temperature programming, step c is chemical vapor deposition, and step d is stress relief.
In one embodiment, in step a, the zinc is a high-purity zinc ingot, preferably, the purity of the zinc is greater than or equal to 99.999%, so that the purity of the zinc selenide product can be ensured.
In one embodiment, the crucible is made of high purity isostatic graphite.
In one embodiment, in step b, the temperature rise rate of the deposition chamber is 0.3 ℃/min to 1 ℃/min.
In one embodiment, in step b, the temperature rise rate of the crucible is 0.2 ℃/min to 0.8 ℃/min.
The key point of the step c is to control the deposition rate of zinc selenide to be 50-150 μm/h.
In the step c, the argon is introduced into the crucible to carry the zinc vapor, so that the zinc vapor is pushed into the deposition chamber, and the zinc vapor evaporated from the crucible is diffused in the deposition chamber in a small area, so that the zinc selenide product with large size and uniform thickness cannot be obtained.
In step c, the deposition time of zinc selenide is not particularly limited as long as the deposition chamber can accommodate the final deposited zinc selenide product.
In step c, it is necessary to control the evaporation rate of zinc in the crucible according to the size of the crucible and its temperature.
In one embodiment, in step c, the deposition rate of zinc selenide can be achieved by controlling the flow rate of argon gas introduced into the crucible, the temperature of the crucible, the ratio of the flow rate of argon gas introduced into the crucible to the evaporation rate of zinc vapor in the crucible, the flow rate of argon gas in the mixed gas of argon gas and hydrogen selenide introduced into the deposition chamber, the ratio of the flow rate of argon gas introduced into the deposition chamber to the flow rate of hydrogen selenide, the ratio of the flow rate of hydrogen selenide introduced into the deposition chamber to the flow rate of zinc vapor entering the deposition chamber from the crucible, and the vacuum degree of the chemical vapor deposition furnace.
In one embodiment, in step c, the amount of argon gas introduced into the crucible is between 12L/min and 60L/min.
In one embodiment, in step c, the ratio of the amount of argon introduced into the crucible to the evaporation rate of zinc vapor in the crucible is 3:1 to 15:1, wherein the flow rate is L/min and the evaporation rate of zinc vapor is L/min.
In one embodiment, in step c, the ratio of the argon flow to the hydrogen selenide flow introduced into the deposition chamber is 5:1-20:1, wherein the argon flow unit and the hydrogen selenide flow unit are both L/min.
In one embodiment, in step c, the ratio of the flow rate of hydrogen selenide introduced into the deposition chamber to the flow rate of zinc vapor entering the deposition chamber from the crucible is 1:1-1.3:1, wherein both the flow rate unit of hydrogen selenide and the flow rate unit of zinc vapor are L/min, and excess hydrogen selenide increases the reaction rate.
In one embodiment, in step c, the flow rate of hydrogen selenide into the deposition chamber is 8-12L/min.
In one embodiment, in step c, the flow rate of zinc vapor from the crucible into the deposition chamber is 6-12L/min.
In step d, the determination of the constant temperature time needs to be determined according to the thickness of the deposited zinc selenide product, the thicker the zinc selenide product is, the longer the required constant temperature time is, and the smaller the temperature rise rate at this stage is.
In one embodiment, in the step d, the first constant temperature time is 8h-72h, and the second constant temperature time is 10h-48 h.
The disclosure is further illustrated with reference to the following examples. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present disclosure.
In the following examples and comparative examples, reagents, materials and instruments used were commercially available or prepared by methods known in the art, unless otherwise specified.
Example 1
In a chemical vapor deposition furnace, a deposition chamber with the length of 600mm, the width of 300mm and the height of 1100mm is adopted, zinc ingots with the purity of 99.999 percent are filled into a crucible, the crucible is vacuumized, the vacuum degree is 3000Pa, and leakage detection is carried out. And starting temperature programming after the crucible is qualified, wherein the temperature rise rate of the crucible is 0.3 ℃/min, the temperature rise rate of the deposition chamber is 0.5 ℃/min, the temperature of the crucible is raised to 650 ℃, and the temperature of the deposition chamber is raised to 700 ℃. Then introducing gas into the crucible and the deposition chamber respectively, wherein the flow of argon introduced into the crucible is 30L/min, and the evaporation rate of zinc vapor is 5L/min; the flow rate of the hydrogen selenide led into the deposition chamber is 5.5L/min, the flow rate of the argon gas led into the deposition chamber and mixed with the hydrogen selenide is 55L/min, the deposition rate is controlled to be 80 mu m/h, and the zinc selenide is deposited. After the deposition is finished, maintaining the same pressure and gas flow as those in the deposition process, heating the deposition chamber to 750 ℃ at the heating rate of 0.2 ℃/min, and keeping the temperature for 8 hours; then cooling the deposition chamber to 500 ℃ at the cooling rate of 0.2 ℃/min, keeping the temperature for 10h, then cooling to room temperature at the cooling rate of 0.5 ℃/min, and discharging to obtain the zinc selenide product.
Example 2
In a chemical vapor deposition furnace, a deposition chamber with the length of 500mm, the width of 400mm and the height of 1200mm is adopted, zinc ingots with the purity of 99.999 percent are filled into a crucible, the crucible is vacuumized, the vacuum degree is 5800Pa, and leakage detection is carried out. And starting temperature programming after the temperature of the crucible is qualified, wherein the temperature rising rate of the crucible is 0.5 ℃/min, the temperature rising rate of the deposition chamber is 0.8 ℃/min, the temperature of the crucible is raised to 680 ℃, and the temperature of the deposition chamber is raised to 750 ℃. Then introducing gas into the crucible and the deposition chamber respectively, wherein the flow of the argon introduced into the crucible is 50L/min, and the evaporation rate of zinc vapor is 7L/min; the flow rate of the hydrogen selenide led into the deposition chamber is 9L/min, the flow rate of the argon gas led into the deposition chamber and mixed with the hydrogen selenide is 100L/min, the deposition rate is controlled at 110 mu m/h, and the zinc selenide is deposited. After the deposition is finished, maintaining the same pressure and gas flow as those in the deposition process, heating the deposition chamber to 780 ℃ at the heating rate of 0.1 ℃/min, and keeping the temperature for 16 hours; and then cooling the deposition chamber to 650 ℃ at the cooling rate of 0.2 ℃/min, keeping the temperature for 14h, then cooling to room temperature at the cooling rate of 0.5 ℃/min, and discharging to obtain a zinc selenide product.
Example 3
In a chemical vapor deposition furnace, a deposition chamber with the length of 650mm, the width of 250mm and the height of 800mm is adopted, zinc ingots with the purity of 99.999 percent are filled into a crucible, the crucible is vacuumized, the vacancy is 10000Pa, and leakage detection is carried out. And starting temperature programming after the temperature of the crucible is qualified, wherein the temperature rising rate of the crucible is 0.8 ℃/min, the temperature rising rate of the deposition chamber is 1 ℃/min, the temperature of the crucible is raised to 700 ℃, and the temperature of the deposition chamber is raised to 800 ℃. Then introducing gas into the crucible and the deposition chamber respectively, wherein the flow of the argon introduced into the crucible is 80L/min, and the evaporation rate of zinc vapor is 8L/min; the flow rate of the hydrogen selenide led into the deposition chamber is 10L/min, the flow rate of the argon gas led into the deposition chamber and mixed with the hydrogen selenide is 150L/min, the deposition rate is controlled at 150 mu m/h, and the zinc selenide is deposited. After the deposition is finished, maintaining the same pressure and gas flow as those in the deposition process, heating the deposition chamber to 850 ℃ at the heating rate of 0.1 ℃/min, and keeping the temperature for 20 hours; then cooling the deposition chamber to 500 ℃ at the cooling rate of 0.1 ℃/min, keeping the temperature for 20h, then cooling to room temperature at the cooling rate of 0.5 ℃/min, and discharging to obtain the zinc selenide product.
Example 4
In a chemical vapor deposition furnace, a deposition chamber with the length of 550mm, the width of 40mm and the height of 800mm is adopted, zinc ingots with the purity of 99.999 percent are filled into a crucible, the crucible is vacuumized, the vacuum degree is 8000Pa, and leakage detection is carried out. And starting temperature programming after the temperature of the crucible is qualified, wherein the temperature rising rate of the crucible is 0.8 ℃/min, the temperature rising rate of the deposition chamber is 1 ℃/min, the temperature of the crucible is raised to 700 ℃, and the temperature of the deposition chamber is raised to 750 ℃. Then introducing gas into the crucible and the deposition chamber respectively, wherein the flow of the argon introduced into the crucible is 80L/min, and the evaporation rate of zinc vapor is 8L/min; the flow rate of the hydrogen selenide led into the deposition chamber is 10L/min, the flow rate of the argon gas led into the deposition chamber and mixed with the hydrogen selenide is 150L/min, the deposition rate is controlled at 100 mu m/h, and the zinc selenide is deposited. After the deposition is finished, maintaining the same pressure and gas flow as those in the deposition process, heating the deposition chamber to 820 ℃ at the heating rate of 0.1 ℃/min, and keeping the temperature for 20 hours; then cooling the deposition chamber to 500 ℃ at the cooling rate of 0.1 ℃/min, keeping the temperature for 20h, then cooling to room temperature at the cooling rate of 0.5 ℃/min, and discharging to obtain the zinc selenide product.
Comparative example 1
In a chemical vapor deposition furnace, a deposition chamber with the length of 550mm, the width of 400mm and the height of 1000mm is adopted, zinc ingots with the purity of 99.999 percent are filled into a crucible, the crucible is vacuumized, the vacuum degree is 10000Pa, and leakage detection is carried out. And starting temperature programming after the temperature of the crucible is qualified, wherein the temperature rising rate of the crucible is 0.8 ℃/min, the temperature rising rate of the deposition chamber is 1 ℃/min, the temperature of the crucible is raised to 700 ℃, and the temperature of the deposition chamber is raised to 750 ℃. Then introducing gas into the crucible and the deposition chamber respectively, wherein the flow of the argon introduced into the crucible is 80L/min, and the evaporation rate of the zinc vapor is 18L/min; the flow rate of the hydrogen selenide led into the deposition chamber is 23.4L/min, the flow rate of the argon gas led into the deposition chamber and mixed with the hydrogen selenide is 240L/min, the deposition rate of the zinc selenide is 212 mu m/h, and the zinc selenide is deposited. After the deposition is finished, maintaining the same pressure and gas flow as those in the deposition process, heating the deposition chamber to 850 ℃ at the heating rate of 0.1 ℃/min, and keeping the temperature for 20 hours; then cooling the deposition chamber to 500 ℃ at the cooling rate of 0.1 ℃/min, keeping the temperature for 20h, then cooling to room temperature at the cooling rate of 0.5 ℃/min, and discharging to obtain the zinc selenide product.
Comparative example 2
In a chemical vapor deposition furnace, a deposition chamber with the length of a deposition chamber of 400mm, the width of 400mm and the height of 1200mm is adopted, zinc ingots with the purity of 99.999 percent are filled in a crucible, the crucible is vacuumized, the vacuum degree is 15000Pa, and leakage detection is carried out. And starting temperature programming after the temperature of the crucible is qualified, wherein the temperature rising rate of the crucible is 0.5 ℃/min, the temperature rising rate of the deposition chamber is 0.8 ℃/min, the temperature of the crucible is raised to 680 ℃, and the temperature of the deposition chamber is raised to 750 ℃. Then introducing gas into the crucible and the deposition chamber respectively, wherein the flow of the argon introduced into the crucible is 50L/min, and the evaporation rate of zinc vapor is 7L/min; the flow rate of the hydrogen selenide led into the deposition chamber is 9L/min, the flow rate of the argon gas led into the deposition chamber and mixed with the hydrogen selenide is 100L/min, the deposition rate of the zinc selenide is controlled to be 180 mu m/h, and the zinc selenide is deposited. After the deposition is finished, maintaining the same pressure and gas flow as those in the deposition process, heating the deposition chamber to 780 ℃ at the heating rate of 0.1 ℃/min, and keeping the temperature for 16 hours; and then cooling the deposition chamber to 650 ℃ at the cooling rate of 0.2 ℃/min, keeping the temperature for 14h, then cooling to room temperature at the cooling rate of 0.5 ℃/min, and discharging to obtain a zinc selenide product.
Comparative example 3
In a chemical vapor deposition furnace, a deposition chamber with the length of 600mm, the width of 300mm and the height of 1100mm is adopted, zinc ingots with the purity of 99.999 percent are filled into a crucible, the crucible is vacuumized, the vacuum degree is 3000Pa, and leakage detection is carried out. And starting temperature programming after the crucible is qualified, wherein the temperature rise rate of the crucible is 0.3 ℃/min, the temperature rise rate of the deposition chamber is 0.5 ℃/min, the temperature of the crucible is raised to 650 ℃, and the temperature of the deposition chamber is raised to 700 ℃. Then introducing gas into the crucible and the deposition chamber respectively, wherein the flow of argon introduced into the crucible is 30L/min, and the evaporation rate of zinc vapor is 5L/min; and (3) the flow of the hydrogen selenide introduced into the deposition chamber is 5.5L/min, the flow of the argon gas introduced into the deposition chamber and mixed with the hydrogen selenide is 55L/min, the deposition of the zinc selenide is started, after the deposition is finished, the temperature is reduced to the room temperature by adopting 0.5 ℃/min, and the zinc selenide product is obtained after the zinc selenide is discharged from the furnace.
The results of the zinc selenide products of examples 1-4 and comparative examples 1-3 are shown in table 1.
TABLE 1
It can be seen from the results of the zinc selenide products of examples 1-3 that large-sized, thickened zinc selenide products can be grown in correspondingly sized deposition chambers using the zinc selenide growth methods provided by the present disclosure.
In the comparative example 1, the growth rate of the zinc selenide is too high and reaches 212 mu m/h, and the obtained zinc selenide product has a fog layer and serious fog spots, has many defects, has low product performance and cannot meet the use requirement. In comparative example 2, the growth rate of zinc selenide is too high, 180 μm/h and the vacuum degree value is large, and the obtained zinc selenide product has the same quality of serious fog spots and many defects, and cannot be used. In comparative example 3, there was no stress relief step to relieve the large stress present during deposition, and the resulting zinc selenide product cracked severely, thus failing to form zinc selenide of larger size. In addition, the zinc selenide products obtained in the comparative examples 1 to 3 have the phenomenon of product cracking.
Researchers in the disclosure further find that, by using the growth method of zinc selenide in the disclosure, zinc selenide can be deposited in a deposition chamber with a length of 200-.
Claims (9)
1. A growth method of zinc selenide is characterized by comprising the following steps:
a. putting zinc into a crucible in a chemical vapor deposition furnace, replacing air in the deposition furnace with argon, and vacuumizing to reach a vacuum degree of 3000-10000 Pa;
b. heating a chemical vapor deposition furnace, heating a deposition chamber in the chemical vapor deposition furnace to the deposition temperature of 700-800 ℃, and heating a crucible to the evaporation temperature of 650-700 ℃;
c. respectively introducing gas into a crucible and a deposition chamber to perform a vapor deposition reaction of zinc selenide, introducing argon into the crucible, wherein the flow of the argon introduced into the crucible is 12L/min-60L/min, and introducing the argon and hydrogen selenide into the deposition chamber to ensure that the deposition rate of the zinc selenide is 50-150 mu m/h;
d. after the reaction is finished, maintaining the same pressure and gas flow as those in the deposition process, continuously heating the deposition chamber to 50-170 ℃, keeping the temperature constant for the first time, then cooling to the range of 500-650 ℃, keeping the temperature constant again, and then cooling to room temperature to obtain the zinc selenide product, wherein the diameter of the zinc selenide product is 500mm, and the thickness of the zinc selenide product is 20-40 mm.
2. The growth method of zinc selenide according to claim 1,
in the step a, the purity of zinc is more than or equal to 99.999 percent; and/or
The crucible is made of isostatic pressing graphite.
3. The method for growing zinc selenide according to claim 1, wherein in the step c, the deposition rate of zinc selenide is realized by controlling the flow rate of argon gas introduced into the crucible, the temperature of the crucible, the ratio of the flow rate of argon gas introduced into the crucible to the evaporation rate of zinc vapor in the crucible, the flow rate of argon gas in the mixed gas of argon gas and hydrogen selenide introduced into the deposition chamber, the ratio of the flow rate of argon gas introduced into the deposition chamber to the flow rate of hydrogen selenide, the ratio of the flow rate of hydrogen selenide introduced into the deposition chamber to the flow rate of zinc vapor entering the deposition chamber from the crucible, and the vacuum degree of the chemical vapor deposition furnace.
4. The growth method of zinc selenide according to claim 1,
in the step b, the temperature rise rate of the deposition chamber is 0.3 ℃/min-1 ℃/min; and/or
In the step b, the temperature rise rate of the crucible is 0.2-0.8 ℃/min.
5. The growing method of zinc selenide according to claim 3, wherein in the step c, the ratio of the flow rate of argon gas introduced into the crucible to the evaporation rate of zinc vapor in the crucible is 3:1-15:1, wherein the flow rate is L/min, and the evaporation rate of zinc vapor is L/min.
6. The growing method of zinc selenide according to claim 3, wherein in the step c, the ratio of the argon gas flow to the hydrogen selenide flow which are introduced into the deposition chamber is 5:1-20:1, wherein the argon gas flow unit and the hydrogen selenide flow unit are both L/min.
7. The growing method of zinc selenide according to claim 3, wherein in the step c, the ratio of the flow rate of hydrogen selenide introduced into the deposition chamber to the flow rate of zinc vapor entering the deposition chamber from the crucible is 1:1-1.3:1, wherein the flow rate unit of hydrogen selenide and the flow rate unit of zinc vapor are both L/min.
8. The growing method of zinc selenide according to claim 3, wherein, in the step c,
the flow of hydrogen selenide introduced into the deposition chamber is 8-12L/min; and/or
The flow rate of zinc vapor entering the deposition chamber from the crucible is 6-12L/min.
9. The growing method of zinc selenide according to claim 1, wherein in the step d, the first constant temperature time is 8-72 h, and the second constant temperature time is 10-48 h.
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| CN112795897B (en) * | 2020-12-25 | 2022-12-02 | 安徽中飞科技有限公司 | Preparation method of polycrystalline zinc selenide |
| CN112813411B (en) * | 2020-12-28 | 2022-07-08 | 安徽中飞科技有限公司 | Preparation method of thick infrared optical material |
| CN114016129B (en) * | 2021-10-09 | 2023-03-24 | 山东有研国晶辉新材料有限公司 | Novel zinc selenide growth method |
| CN114380599A (en) * | 2022-01-26 | 2022-04-22 | 中国工程物理研究院化工材料研究所 | Preparation method of transition metal ion doped zinc selenide laser transparent ceramic |
| CN115961349A (en) * | 2022-12-29 | 2023-04-14 | 安徽光智科技有限公司 | Growth method of high-uniformity zinc sulfide polycrystalline infrared material |
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| CN101759161A (en) * | 2008-12-25 | 2010-06-30 | 北京有色金属研究总院 | Preparation method of zinc selenide with high optical quality |
| CN102168309A (en) * | 2011-04-07 | 2011-08-31 | 合肥工业大学 | Method for preparing p-type IIB-VIA family quasi-one-dimensional semiconductor nano material by chemical vapor-deposition in-situ doping |
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2020
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0132618A1 (en) * | 1983-06-29 | 1985-02-13 | Sumitomo Electric Industries Limited | Process for preparing ZnSe single crystal |
| CN101759161A (en) * | 2008-12-25 | 2010-06-30 | 北京有色金属研究总院 | Preparation method of zinc selenide with high optical quality |
| CN101649449A (en) * | 2009-09-17 | 2010-02-17 | 北京中材人工晶体研究院有限公司 | Preparation method and preparation mould of ZnS/ZnSe composite infrared transmission material |
| CN102168309A (en) * | 2011-04-07 | 2011-08-31 | 合肥工业大学 | Method for preparing p-type IIB-VIA family quasi-one-dimensional semiconductor nano material by chemical vapor-deposition in-situ doping |
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