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CN218203044U - Gas inlet device for preparing zinc sulfide and zinc selenide optical material by chemical vapor deposition - Google Patents

Gas inlet device for preparing zinc sulfide and zinc selenide optical material by chemical vapor deposition Download PDF

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Publication number
CN218203044U
CN218203044U CN202222497464.0U CN202222497464U CN218203044U CN 218203044 U CN218203044 U CN 218203044U CN 202222497464 U CN202222497464 U CN 202222497464U CN 218203044 U CN218203044 U CN 218203044U
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raw materials
raw material
gas
base plate
air cock
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张树玉
甄西合
刘伟
邰超
朱逢锐
熊加丽
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Henan Liuxi Technology Co ltd
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Jiangsu Liuxi Optical Technology Co ltd
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Abstract

The utility model discloses a chemical vapor deposition preparation zinc sulfide, zinc selenide optical material's air inlet unit, including base plate and first raw materials air cock and the second raw materials air cock of setting on the base plate, first raw materials year gas pocket has been seted up on the base plate side surface, terminal surface through connection under first raw materials year gas pocket and the base plate, the end of giving vent to anger of first raw materials air cock and second raw materials air cock all is located base plate up end one side, the inlet end is located terminal surface one side under the base plate, first raw materials year gas pocket and first raw materials air cock cooperation supply mixed gas, be provided with outer sleeve pipe on the second raw materials air cock surface, be provided with the air cavity between outer sleeve pipe and the second raw materials air cock, be provided with the second raw materials carrier gas pipe who link up the air cavity on the outer sleeve pipe, outer sleeve pipe is located second raw materials air cock end one side of giving vent to anger and is provided with the venthole on the surface. The utility model discloses the reaction gas flow pattern is stable among the deposition process, can adapt to long-term continuous deposition growth, satisfies the crystal growth demand of high quality, high thickness.

Description

Gas inlet device for preparing zinc sulfide and zinc selenide optical material by chemical vapor deposition
Technical Field
The utility model relates to a chemical vapor deposition technical field, concretely relates to chemical vapor deposition prepares zinc sulfide, zinc selenide optical material's air inlet unit.
Background
Zinc sulfide (ZnS) and zinc selenide (ZnSe) are two important infrared optical materials, have the characteristics of wide spectral transmission, small absorption coefficient, high purity, moderate thermal expansion coefficient and the like, and are widely applied to the field of infrared thermal imaging and the field of CO2 lasers. The chemical vapor deposition technology is the mainstream technology for preparing ZnS and ZnSe materials at present. The technical scheme is as follows: the bottom of the deposition furnace is a crucible for containing raw material Zn, the upper part of the deposition furnace is a deposition chamber formed by splicing graphite plates, the crucible and the deposition chamber are respectively heated to set temperatures, then carrier gas Ar is introduced to the surface of molten Zn, zn vapor carried by the carrier gas Ar enters the deposition chamber through an air inlet device, and meanwhile H 2 S(H 2 Se) gas is diluted by Ar and then is conveyed to a deposition chamber through a gas inlet device, H 2 S(H 2 Se) and Zn react on a graphite plate to generate solid ZnS (ZnSe), and after a period of depositionFinally, the bulk polycrystalline ZnS (ZnSe) material with a certain thickness can be obtained.
Preparation of ZnS and ZnSe materials, zn vapor and H by chemical vapor deposition 2 S(H 2 Se) gas inlet device is the core of a deposition system, particularly, the nozzle structures and the distribution of two raw material gases can directly influence the reasonability of the flow pattern of reaction gas in a deposition chamber, further influence the material to improve the quality of the material, and the cycle of preparing ZnS and ZnSe materials by deposition is longer, if the nozzle structures and the distribution are unreasonable, a large amount of ZnS (ZnSe) materials can be deposited and attached on the nozzle, so that the nozzle structures have unrepeatable irregular deformation, the flow rate and the flow pattern of the raw material gases are influenced, the thickness uniformity of the ZnS (ZnSe) materials deposited on a graphite substrate in the deposition chamber in the long-time deposition process is poorer, the performance can be different, layering can be generated in serious conditions, the stability of the deposition process and the repeatability can not be ensured, and even the deposition process can not be carried out, and the deposition process can be forced to stop. With the development of the infrared market, the demand for large-size and high-quality ZnS (ZnSe) materials is more and more urgent, and those skilled in the relevant art also design and develop various gas inlet schemes to improve the stability of the deposition process, but it is still very difficult to prepare high-quality ZnS (ZnSe) materials with a thickness of more than 40mm and high optical uniformity.
Disclosure of Invention
The utility model aims to solve the technical problem and provide a chemical vapor deposition preparation zinc sulfide, zinc selenide optical material's air inlet unit, the reaction gas flow pattern is stable among the deposition process, can adapt to long-term continuous deposition growth, satisfies the crystal growth demand of high quality, high thickness.
In order to solve the technical problem, the utility model provides a chemical vapor deposition prepares air inlet unit of zinc sulfide, zinc selenide optical material, including base plate and first raw materials air cock and the second raw materials air cock of setting on the base plate, the lower terminal surface of base plate is used for being connected with the crucible, the up end of base plate is used for being connected with the deposit room, first raw materials year gas pocket has been seted up on the base plate side surface, terminal surface through connection under the base plate that first raw materials year gas pocket and crucible correspond, the end of giving vent to anger of first raw materials air cock and second raw materials air cock all is located base plate up end one side, the inlet end is located terminal surface one side under the base plate, first raw materials year gas pocket and the cooperation of first raw materials air cock supply mixed gas, be provided with outer sleeve pipe on the second raw materials air cock surface, be provided with the air cavity between outer sleeve pipe and the second raw materials air cock, be provided with the second raw materials year gas pipe that link up the air cavity on the outer sleeve pipe, outer sleeve pipe is located second raw materials air cock and is provided with the venthole on the surface of giving vent end one side, be provided with the distribution dish in the first raw materials air cock, be provided with a plurality of distribution dish, be provided with a plurality of through-hole on the distribution dish.
Furthermore, the second raw material air nozzles are arranged on the central line of the deposition chamber, and the first raw material air nozzles are distributed on two sides of the second raw material air nozzles in two rows and at equal intervals.
Furthermore, the height of the air outlet end of the second raw material air nozzle is greater than that of the air outlet end of the first raw material air nozzle, and the height difference between the air outlet end of the second raw material air nozzle and the air outlet end of the first raw material air nozzle is not less than 30mm.
Further, the through-hole is tangent with the internal surface of first raw materials air cock, and 3 are no less than to the quantity of through-hole, and the diameter of through-hole is 1 with the inner wall diameter ratio of first raw materials air cock: 2-8.
Further, the base plate and the first raw material nozzle are made of graphite.
Furthermore, the second raw material air nozzle and the outer sleeve are made of metal.
Further, outer sleeve pipe and second raw materials air cock between through welded connection, the venthole is the annular structure.
Furthermore, pass through threaded connection between outer sleeve pipe and the second raw materials air cock, be provided with the spacing ring on the second raw materials air cock, outer sleeve pipe bottom sets up with the spacing ring butt, still be provided with the sealing member between outer sleeve pipe bottom and the spacing ring.
Further, the flow rate ratio of the second raw material gas nozzles to the first raw material gas nozzles is 1.5-2:1.
the utility model has the advantages that:
1. in the deposition process, the periphery of the second raw material air nozzle is provided with protective gas sprayed out through the air outlet, and under the scouring and isolation protection of the protective gas, the upper end face of the second raw material air nozzle can be ensured not to be attached by solid materials, so that the flow rate of the second raw material air nozzle is always kept consistent in the long-time continuous deposition growth process, and the process is stable and repeatable.
2. In the deposition process, through the setting of distribution disc, it is porous injection to give vent to anger, has higher air velocity, can play the purpose of "scouring" to first raw materials air cock up end, prevents that gas diffusion to first raw materials air cock up end, reaches the purpose that can not deposit solid-state material on the up end, and in long-time continuous deposition growth process, the velocity of flow of first raw materials gas remains unanimous throughout, and the process is stable repeatedly.
3. Utilize the utility model provides an air inlet unit, in the long-time continuous deposition process, two kinds of air cock up end do not have the solid material deposit, and the air velocity keeps unanimous, and the reaction gas flow pattern is unchangeable, and the process is stable controllable, is suitable for the production of big thickness, high quality ZnS (ZnSe) material very much.
Drawings
FIG. 1 is a schematic view of the overall structure of the present invention;
fig. 2 is a schematic view of the bottom structure of the base plate of the present invention;
fig. 3 is a schematic structural view of a second raw material gas nozzle part of the present invention;
fig. 4 is a schematic structural view of a first raw material gas nozzle part of the present invention;
fig. 5 is a schematic structural view of the present invention in use;
fig. 6 is a schematic structural diagram of a first raw material gas nozzle portion in an embodiment of the present invention.
Detailed Description
The present invention is further described with reference to the following drawings and specific embodiments so that those skilled in the art can better understand the present invention and can implement the present invention, but the embodiments are not to be construed as limiting the present invention.
Referring to fig. 1 to 5, an embodiment of an air inlet device for preparing optical material of zinc sulfide and zinc selenide by chemical vapor deposition of the present invention is used for preparing optical material of ZnS, comprising a substrate 1 and six first raw material air nozzles 2 and two second raw material air nozzles 3 disposed on the substrate, wherein the first raw material air nozzles are Zn steam air nozzles, the graphite material and the second raw material air nozzles are H steam air nozzles 2 S air cock, metal material, the end of giving vent to anger of first raw materials air cock and second raw materials air cock all is located base plate up end one side, the end of admitting air is located base plate down end one side, the lower terminal surface of base plate is used for being connected with crucible 4, the quantity of crucible is 2 at least, the up end of base plate is used for being connected with deposit room 5, deposit room cross-section is the rectangle structure, enclose by 2 narrow graphite slabs and 2 wide graphite slabs, the size of narrow slab is 220mm 1200mm, the size of wide slab is 4000mm 120mm, two H is 0mm 2 The S gas nozzles are arranged on the central line of the deposition chamber, the six Zn steam gas nozzles are divided into 2 rows, 3 gas nozzles are arranged in each row, the six Zn steam gas nozzles are distributed on two sides of the central line at equal intervals, and the two rows respectively correspond to the two crucibles; h 2 The upper end surface of the S air nozzle is 30mm higher than that of the Zn steam air nozzle; h 2 S gas in H 2 The air flow speed in the S air nozzle is 1.5 times of that of Zn steam.
The side surface of the substrate is also provided with a first raw material gas carrying hole 6 which is communicated with the lower end surface of the substrate corresponding to the crucible, namely, carrier gas can be introduced into the crucible through the first raw material gas carrying hole, zn steam in the crucible is carried by the carrier gas and is sprayed out to the deposition chamber from the Zn steam nozzle, and the number of the first raw material gas carrying holes can be one or a plurality.
Be provided with outer sleeve pipe 7 on the second raw materials air cock surface, outer sleeve pipe is the metal material, with second raw materials air cock welded connection, be provided with air cavity 8 between outer sleeve pipe and the second raw materials air cock, be provided with the second raw materials carrier gas pipe 9 that link up the air cavity on the outer sleeve pipe, outer sleeve pipe is located second raw materials air cock and gives vent to anger and is provided with venthole 10 on the surface of end one side, the venthole is the loop configuration, it is even to give vent to anger, the carrier gas here can be Ar gas, the carrier gas passes through second raw materials carrier gas pipe and gets into the air cavity, then upwards spout from the venthole at air cavity top, under the washing of Ar gas, isolation protection, can guarantee that second raw materials air cock up end does not have solid material to adhere to, the high position of venthole and the end height uniformity of giving vent to anger of second raw materials air cock, be in on the coplanar.
A distribution disc 11 is arranged in the first raw material nozzle, and a plurality of through holes 12 are formed in the distribution disc. The through-hole is tangent with the internal surface of first raw materials air cock, and 3 are no less than to the quantity of through-hole, and the diameter of through-hole is 1 with the inner wall diameter ratio of first raw materials air cock: 5, the porous design can improve the flow velocity of the airflow.
And depositing ZnS by adopting a chemical vapor deposition method, wherein the temperature of a deposition chamber is 670 ℃, the pressure is 7000Pa, the deposition chamber is cooled to the room temperature according to 100 ℃/day after 23 days of deposition, the deposition rate is 2 mm/day, the prepared ZnS blank has the maximum thickness of 46mm, and a ZnS optical window with the maximum size of 350 x 500 x 40mm can be obtained after optical processing.
In another embodiment, the graphite deposition system of the present invention is used for preparing ZnSe material:
the difference from the above example is that the narrow plate has a size of 500mm 2000mm, the wide plate has a size of 1000mm 2000mm, and the second raw material air nozzle has a size of H 2 Se nozzle, H 2 4 Se gas nozzles and 2 Zn steam gas nozzles, 5 in each row, H 2 The upper end surface of the Se gas nozzle is 50mm higher than that of the Zn steam gas nozzle; h 2 Se gas in H 2 The gas flow rate in the Se nozzle is 2 times that of the Zn vapor.
Depositing ZnSe by chemical vapor deposition at 750 deg.c and 4000Pa in a deposition chamber, cooling the deposition chamber to room temperature at 120 deg.c/day after 40 days of deposition, depositing at 1.5 mm/day to prepare ZnS blank with maximum thickness of 60mm, and optical processing to obtain ZnSe optical window with maximum size of 650 x 1000 x 50mm.
In one embodiment, referring to FIG. 6, the outer sleeve and the second material nozzle may be connected by a screw thread. When being threaded connection, be provided with spacing ring 13 on the second raw materials air cock, outer sleeve pipe bottom sets up with the spacing ring butt, still is provided with unsmooth seal groove between outer sleeve pipe bottom and the spacing ring, the clean maintenance of convenient to detach.
The above embodiments are only used to illustrate the technical solution of the present invention, and not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, those skilled in the art will understand that: the technical solutions described in the foregoing embodiments may be modified or some technical features may be equivalently replaced; such modifications and substitutions do not depart from the spirit and scope of the present invention in its corresponding aspects.

Claims (10)

1. The utility model provides a chemical vapor deposition prepares air inlet unit of zinc sulfide, zinc selenide optical material, a serial communication port, including the base plate and set up first raw materials air cock and the second raw materials air cock on the base plate, the lower terminal surface of base plate is used for being connected with the crucible, the up end of base plate is used for being connected with the deposit room, first raw materials year gas pocket has been seted up on the base plate side surface, terminal surface through connection under the base plate that first raw materials year gas pocket and crucible correspond, the end of giving vent to anger of first raw materials air cock and second raw materials air cock all is located base plate up end one side, the end is located terminal surface one side under the base plate, first raw materials year gas pocket and the cooperation of first raw materials air cock supply gas mixture, be provided with outer sleeve pipe on the second raw materials air cock surface, be provided with the air cavity between outer sleeve pipe and the second raw materials air cock, be provided with the second raw materials year gas pipe that the air cavity link up on the outer sleeve pipe, outer sleeve pipe is located second raw materials air cock and gives vent to anger on the surface and is provided with the venthole, be provided with the distribution dish in the first raw materials air cock, be provided with a plurality of through-holes on the distribution dish.
2. The apparatus according to claim 1, wherein the second raw material nozzles are disposed on a center line of the deposition chamber, and the first raw material nozzles are arranged in two rows and are equidistantly distributed on two sides of the second raw material nozzles.
3. The apparatus according to claim 1, wherein the height of the gas outlet end of the second raw material gas nozzle is greater than that of the first raw material gas nozzle, and the height difference between the gas outlet end of the second raw material gas nozzle and the gas outlet end of the first raw material gas nozzle is not less than 30mm.
4. The gas inlet device for preparing the zinc sulfide and zinc selenide optical material by chemical vapor deposition as claimed in claim 1, wherein the through holes are tangential to the inner surface of the first raw material gas nozzle, and the number of the through holes is not less than 3.
5. The gas inlet device for preparing optical material of zinc sulfide and zinc selenide by chemical vapor deposition according to claim 4, wherein the ratio of the diameter of the through hole to the diameter of the inner wall of the first raw material nozzle is 1:2-8.
6. The gas inlet device for preparing optical material of zinc sulfide and zinc selenide by chemical vapor deposition according to claim 1, wherein the substrate and the first raw material nozzle are made of graphite.
7. The gas inlet device for preparing optical material of zinc sulfide and zinc selenide by chemical vapor deposition according to claim 1, wherein the second raw material gas nozzle and the outer sleeve are made of metal.
8. The gas inlet device for preparing optical material of zinc sulfide and zinc selenide by chemical vapor deposition according to claim 7, wherein the outer sleeve is connected with the second raw material nozzle by welding, and the gas outlet hole is of an annular structure.
9. The gas inlet device for preparing optical material of zinc sulfide and zinc selenide by chemical vapor deposition according to claim 7, wherein the outer sleeve is connected with the second raw material gas nozzle through a screw thread, a limit ring is arranged on the second raw material gas nozzle, the bottom of the outer sleeve is abutted against the limit ring, and a sealing element is further arranged between the bottom of the outer sleeve and the limit ring.
10. The gas inlet device for preparing zinc sulfide and zinc selenide optical materials by chemical vapor deposition as claimed in claim 1, wherein the flow rate ratio of the second raw material gas nozzle to the first raw material gas nozzle is 1.5-2:1.
CN202222497464.0U 2022-08-29 2022-09-21 Gas inlet device for preparing zinc sulfide and zinc selenide optical material by chemical vapor deposition Active CN218203044U (en)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
CN202222274997 2022-08-29
CN2022222749972 2022-08-29

Publications (1)

Publication Number Publication Date
CN218203044U true CN218203044U (en) 2023-01-03

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Application Number Title Priority Date Filing Date
CN202222497464.0U Active CN218203044U (en) 2022-08-29 2022-09-21 Gas inlet device for preparing zinc sulfide and zinc selenide optical material by chemical vapor deposition

Country Status (1)

Country Link
CN (1) CN218203044U (en)

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Effective date of registration: 20240401

Address after: No. 109, Light Industry Park, Chengguan Town, Shangcheng County, Xinyang City, Henan Province, 465350

Patentee after: Henan Liuxi Technology Co.,Ltd.

Country or region after: China

Address before: Room 126C, building a, emerging industry education center, Zhangjiagang Free Trade Zone, Suzhou, Jiangsu 215600

Patentee before: Jiangsu Liuxi Optical Technology Co.,Ltd.

Country or region before: China

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