Method for preparing patterned zinc sulfide polycrystalline material by CVD (chemical vapor deposition) method
By pretreating the deposition plate in the CVD method and optimizing the deposition chamber conditions, the problems of local defects, complex processing and low efficiency in the preparation of zinc sulfide polycrystalline materials are solved, and an efficient and resource-saving preparation process is achieved.
Patent Information
- Application Number
- CN202510110419.0
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-01-23
- Publication Date
- 2025-05-27
AI Technical Summary
When preparing zinc sulfide polycrystalline materials by the existing CVD method, there are problems such as local defects in the deposition layer, complex processing, waste of resources and low deposition efficiency.
By pretreating the deposition plate, the patterned high-surface energy deposition zone is set, and multiple deposition plates are vertically arranged in the deposition chamber to optimize the gas pressure and temperature in the deposition chamber, and the direct deposition and uniform distribution of zinc sulfide polycrystalline materials are achieved using rotating devices and reaction control methods.
It avoids the inapplicability of product caused by local defects, reduces processing steps and resource waste, improves production efficiency and deposition efficiency, and realizes the preparation of high-quality zinc sulfide polycrystalline materials.
Abstract
Description
Technical Field
[0001] The present invention relates to the field of zinc sulfide polycrystalline materials, and particularly to a method for preparing patterned zinc sulfide polycrystalline materials by chemical vapor deposition (CVD). Background Art
[0002] ZnS is a II-VI group compound, belonging to wide bandgap materials, with stable chemical properties, corrosion resistance, strong environmental adaptability, easy processing, etc. It has low optical transmission loss and good light transmission performance, and is an advanced long-wave infrared window, dome and lens material, which has important applications in infrared thermal imaging and infrared guidance technology.
[0003] In the existing CVD method for preparing polycrystalline ZnS, it is directly deposited into shapes such as integrally connected flat plates or domes, but there are the following adverse effects: First, the stress at a certain deposition site is relatively large, resulting in defects such as cracks, which may extend in the entire deposition area and expand the defects, causing the product to be unusable; Second, after the overall deposition, the required product needs to undergo processing techniques such as circular fitting and cutting. The complex processing process not only reduces production efficiency, but also generates processing stress on the product during this process, affecting the product performance; Third, a lot of scraps will be generated during the processing, causing serious waste of raw materials and being unfavorable for cost saving; Fourth, the heat distribution is uneven. The temperatures at various parts inside the deposition chamber of the deposition furnace are different due to the different distances from the deposition furnace heater, and the temperatures at various parts inside the deposition chamber are uneven; it is easy to have problems affecting the uniformity and quality of the deposition layer; Fifth, the deposition efficiency is low and the deposition distribution is uneven; the deposition plate inside the deposition chamber is horizontally arranged; however, the horizontal arrangement of the deposition plate results in a small effective deposition area in the deposition space of the same volume, thus leading to low deposition efficiency.
[0004] Therefore, how to prepare zinc sulfide polycrystalline materials by chemical vapor deposition (CVD) to avoid the product of the entire deposition layer being unusable due to a small number of local defects in the deposition layer of the entire deposition plate, and to obtain the product without undergoing processing techniques such as circular fitting and cutting on the deposited deposition layer, so as to achieve cost saving and at the same time improve production efficiency, has become a difficult problem urgently to be solved in this field. Summary of the Invention
[0005] In order to solve the above technical problems, a method for preparing patterned zinc sulfide polycrystalline materials by CVD is provided, which can avoid the product of the entire deposition layer being unusable due to a small number of local defects in the deposition layer, and can obtain the product without undergoing processing techniques such as circular fitting and cutting on the deposited deposition layer, so as to achieve cost saving and at the same time improve production efficiency.
[0006] According to the present invention, a method for preparing patterned zinc sulfide polycrystalline materials by CVD includes the following steps:
[0007] Pretreat the deposition plate, and provide a patterned high surface energy deposition area on the deposition surface of the deposition plate; Vertically arrange several deposition plates in the deposition chamber;
[0008] Exhaust air from the deposition chamber through an exhaust device, maintain the gas pressure in the deposition chamber at 3000 - 10000 Pa, and then introduce an inert gas;
[0009] Start the rotating device arranged below the deposition chamber, start the heating device of the deposition chamber, and heat the inside of the deposition chamber to a temperature of 600 - 780 °C;
[0010] Generate an atomized sulfur mixed gas through a sulfur atomization generating device, and introduce the atomized sulfur mixed gas into the deposition chamber; The atomized sulfur mixed gas includes atomized sulfur elemental liquid droplets and an inert gas;
[0011] Generate a zinc vapor mixed gas through a zinc vapor generating device, and introduce the zinc vapor mixed gas into the deposition chamber; The zinc vapor mixed gas includes zinc vapor and an inert gas;
[0012] The sulfur vapor and zinc vapor in the deposition chamber are mixed and react on the surface of the deposition plate at high temperature to obtain a zinc sulfide polycrystalline material; Preferably, the pattern of the high surface energy deposition area on the deposition surface is a pattern composed of the shapes of multiple zinc sulfide polycrystalline products.
[0013] Compared with the prior art, the beneficial effects of the present invention are as follows: By pretreating the deposition plate and providing a patterned high surface energy deposition area on the deposition surface of the deposition plate, direct deposition on the high surface energy deposition area on the deposition surface of the deposition plate is achieved, and zinc sulfide polycrystalline products are directly obtained, thereby avoiding the situation where the products of the deposition layer on the entire deposition plate cannot be used due to a small number of local defects in the deposition layer, and there is no need to subject the deposited deposition layer to processing techniques such as rounding and cutting to obtain the products, that is, the production efficiency is improved and the cost is saved;
[0014] By vertically arranging several deposition plates in the deposition chamber, the deposition of zinc sulfide on the surface of the vertical deposition plates is realized. Therefore, several deposition plates can be vertically arranged in the deposition chamber, so as to have a large effective deposition area in the deposition space of the same volume, thereby significantly improving the deposition efficiency;
[0015] Realize heating and melting of sulfur monomers and then atomizing them, and then introduce the atomized sulfur elemental liquid into the deposition chamber. The atomized sulfur monomers are instantly gasified and dispersed evenly at high temperature in the deposition chamber; Therefore, the gasified sulfur elemental enters the deposition chamber and is dispersed evenly in the deposition chamber, and problems such as blockage of the pipeline or unstable flow rate caused by solidification of sulfur monomers during transportation are avoided when sulfur monomers are gasified in advance and then enter the deposition chamber.
[0016] It is beneficial to realize the uniform mixing of the gasified sulfur elemental and the gasified zinc elemental in the deposition chamber.
[0017] Furthermore, the method for preprocessing a deposition plate to achieve a patterned high surface energy deposition area provided on the deposition surface of the deposition plate includes the following steps:
[0018] Take a graphite template of a preset size as the deposition plate;
[0019] Coat the deposition surface of the graphite template with a low surface energy reagent, and then heat the cleaned graphite template once in a drying device under a negative pressure environment;
[0020] Then clean the graphite template after the first heating with a cleaning solution, and perform a second heating after cleaning to obtain a low surface energy deposition plate;
[0021] Connect a mask plate to the deposition surface of the obtained low surface energy deposition plate; the mask plate is provided with a patterned hollowed-out area identical to the patterned high surface energy deposition area;
[0022] Perform a high surface energy treatment on the deposition surface of the low surface energy deposition plate connected with the mask plate, and make the area of the deposition surface of the low surface energy deposition plate not covered by the mask plate achieve high surface energy, so as to obtain a deposition plate with a patterned high surface energy deposition area provided on the deposition surface.
[0023] Furthermore, the low surface energy reagent includes octadecyltrichlorosilane;
[0024] The heating temperature of the first heating is 120 - 220 °C, the heating time is 2 - 5 h, and the negative pressure environment is a pressure ≤ 0.1 Pa;
[0025] The process of cleaning the graphite template after the first heating with the cleaning solution includes successively cleaning the graphite template after the first heating with n-hexane, chloroform, and isopropanol;
[0026] The heating temperature of the second heating is 50 - 80 °C, and the heating time is 3 - 5 h;
[0027] The process of performing a high surface energy treatment on the deposition surface of the low surface energy deposition plate connected with the mask plate includes treating the exposed positions by means of oxygen plasma etching, and the treatment time is 2 - 30 min.
[0028] The beneficial effect of the previous step is to first perform a low surface energy treatment on the surface of the graphite template, and then perform a high surface energy treatment after connecting a mask plate to the deposition surface of the obtained low surface energy deposition plate, so as to obtain a patterned high surface energy deposition area on the deposition surface of the deposition plate, and the pattern of this patterned high surface energy deposition area is the same as the pattern formed by arranging the shapes of multiple products;
[0029] By cleaning the graphite template after the first heating with a cleaning solution, the excess low surface energy reagent on the deposition surface is removed, avoiding its impact on the purity of the deposited product during the subsequent deposition process;
[0030] Thus, the surface energy at different positions on the deposition surface of the deposition plate is different. The low surface energy region is already very stable, while the high surface energy region requires the coverage of ZnS molecules to reduce the overall surface energy. The ZnS molecules tending to a more stable low energy surface will be repelled by the low surface energy region and evenly distributed in the high surface energy region, forming a pre-designed ZnS polycrystalline pattern.
[0031] Furthermore, the flow rate of the sulfur-containing atomized mixed gas is 8 - 15 sccm; the flow rate of the zinc vapor-containing mixed gas is 3 - 7 sccm;
[0032] The sulfur-containing atomized mixed gas includes atomized sulfur droplets, hydrogen, and an inert gas; the volume ratio of hydrogen to atomized sulfur droplets is 1:(1 - 4); the volume ratio of the inert gas to atomized sulfur droplets is (10 - 30):1;
[0033] The zinc vapor-containing mixed gas includes an inert gas and zinc vapor with a volume ratio of (10 - 25):1;
[0034] After introducing the zinc-containing mixed gas and the sulfur-containing atomized mixed gas into the deposition chamber, the pressure in the deposition chamber is controlled at 3000 - 10000 Pa.
[0035] Furthermore, a deposition chamber exhaust hole is provided above the deposition chamber. The deposition chamber exhaust hole is connected to a discharge box. A discharge box exhaust hole is provided at a position of the discharge box far from the deposition chamber exhaust hole, and the discharge box exhaust hole is connected to an exhaust device;
[0036] After introducing the zinc-containing mixed gas and the sulfur-containing atomized mixed gas into the deposition chamber, the discharge box is connected to the deposition chamber, and the waste gas is discharged through the discharge box.
[0037] The beneficial effect of the previous step is that through the deposition chamber exhaust hole provided above the deposition chamber, the deposition chamber exhaust hole is connected to a discharge box, the discharge box exhaust hole is provided at a position of the discharge box far from the deposition chamber exhaust hole, and the discharge box exhaust hole is connected to an exhaust device; it is realized that the uniformly mixed vaporized sulfur and vaporized zinc move from the bottom to the top of the deposition chamber, and zinc sulfide is deposited on the surface of the deposition plate when passing between the deposition plates. The generated dust and slag enter the discharge box upward and are discharged through the discharge box exhaust hole, thus avoiding the problem that the dust and slag are scattered on the surface of the deposition plate, resulting in impurities in the deposited zinc sulfide, and at the same time avoiding the problem of dust and slag accumulation in the deposition furnace.
[0038] Further, the process of generating a sulfur atomized mixed gas by a sulfur atomization generating device and introducing the sulfur atomized mixed gas into a deposition chamber includes the following steps:
[0039] Put elemental sulfur into the sulfur storage pool of the sulfur atomization generating device, then evacuate the sulfur storage pool, and control the pressure of the sulfur storage pool at 3000 - 10000 Pa; heat the internal space of the sulfur storage pool and maintain the internal temperature of the sulfur storage pool at 130 - 300 °C;
[0040] When the elemental sulfur in the sulfur storage pool is in a molten state, pump the molten elemental sulfur in the sulfur storage pool through a first spraying device and spray it into the atomization device. When the molten elemental sulfur enters the atomization device, it is atomized by high-speed gas to obtain a sulfur atomized mixed gas; the flow rate of the high-speed gas is 10 - 200 m / s; the high-speed gas is a mixed gas of an inert gas and hydrogen;
[0041] The sulfur atomized mixed gas enters the deposition chamber from the atomization device; the atomized sulfur elemental droplets in the sulfur atomized mixed gas are vaporized into sulfur vapor in the deposition chamber.
[0042] The beneficial effect of the previous step is that by heating the internal space of the sulfur storage pool, the melting of elemental sulfur is realized; by pumping the molten elemental sulfur in the sulfur storage pool through a first spraying device and spraying it into the atomization device, the molten liquid sulfur is dispersed and atomized by the high-speed gas introduced into the spraying device when passing through the spraying device to obtain atomized sulfur elemental droplets, and the atomized sulfur elemental droplets are small droplets that are uniformly dispersed in a foggy state; when the atomized sulfur elemental droplets enter the deposition chamber from the atomization device, they are quickly vaporized at high temperature, and the atomized sulfur elemental droplets become uniformly dispersed vaporized sulfur elemental, that is, become sulfur vapor.
[0043] Further, put elemental zinc into the crucible container of the zinc vapor generating device, introduce an inert gas to displace the air in the crucible container, and heat the inside of the crucible container. The temperature of the crucible container is 600 - 750 °C; the elemental zinc is vaporized into zinc vapor, and the zinc vapor enters the deposition chamber after being mixed with the inert gas.
[0044] The beneficial effect of the previous step is that the vaporization of elemental zinc is realized and the vaporized elemental zinc enters the deposition chamber.
[0045] Further, the deposition plate includes a first deposition plate and a second deposition plate;
[0046] One side of the first deposition plate away from the deposition surface is oppositely arranged and connected to one side of the second deposition plate away from the deposition surface to form a deposition plate group;
[0047] A number of deposition plate groups are vertically arranged in the deposition chamber;
[0048] A deposition space is formed between adjacent deposition plate groups;
[0049] The mixed gas of sulfur vapor and zinc vapor enters several deposition spaces, on the surfaces of the deposition surfaces of the deposition plate groups on both sides of the deposition spaces;
[0050] The n deposition spaces are sequentially labeled as the first deposition space, the second deposition space, the third deposition space to the mth deposition space from the middle deposition space to the deposition spaces on both sides;
[0051] m = n / 2 or (n + 1) / 2.
[0052] The beneficial effect of the previous step is that by arranging the side of the first deposition plate away from the deposition surface opposite to and connected with the side of the second deposition plate away from the deposition surface to form a deposition plate group, a deposition space is formed between adjacent deposition plate groups, so as to realize the deposition of the uniformly mixed sulfur vapor and zinc vapor on the deposition surfaces of the first deposition plate and the second deposition plate, increasing the deposition efficiency; at the same time, since the first deposition plate and the second deposition plate are arranged oppositely, only one surface of the first deposition plate and the second deposition plate deposits zinc sulfide, and the deposition efficiency will not be reduced; thus, after deposition, the first deposition plate and the second deposition plate can be separated, and then the deposited zinc sulfide can be separated from the first deposition plate and the second deposition plate without damaging the deposited zinc sulfide layer.
[0053] Further, the method for preparing the patterned zinc sulfide polycrystalline material by the CVD method further includes controlling the deposition process by adjusting one or more of the rotation rate of the deposition chamber, the flow rate of the zinc-containing mixed gas, the flow rate of the sulfur-containing atomized mixed gas, and the heating device of the deposition chamber through a reaction control method; the reaction control method includes the following steps:
[0054] Detect the temperatures of several deposition spaces; when the difference between the temperatures of several deposition spaces and the preset standard temperature is within 0 - 9 °C, there is no need to adjust the rotation rate of the deposition chamber, the zinc vapor-containing mixed gas, and the flow rate of the sulfur-containing atomized mixed gas;
[0055] When the temperatures of the first deposition space and the second deposition space are higher than the preset standard temperature within 10 - 15 °C, increase the flow rate of the sulfur-containing atomized mixed gas;
[0056] When the temperatures of the first deposition space and the second deposition space are lower than the preset standard temperature within 10 - 15 °C, reduce the flow rate of the sulfur-containing atomized mixed gas;
[0057] When the temperatures of the first deposition space and the second deposition space are higher than the preset standard temperature within 16 - 20 °C, increase the rotation rate of the deposition chamber; when the temperatures of the first deposition space and the second deposition space are lower than the preset standard temperature within 16 - 20 °C, reduce the rotation rate of the deposition chamber;
[0058] When the temperature in the third deposition space to the m-th deposition space is 10 - 20°C higher than the preset standard temperature, reduce the heating temperature of the heating device in the deposition chamber;
[0059] When the temperature in the third deposition space to the m-th deposition space is 10 - 20°C lower than the preset standard temperature, increase the heating temperature of the heating device in the deposition chamber.
[0060] The beneficial effect of the previous step is that by the reaction control method, the rotation rate of the entire deposition chamber, the flow rate of the zinc-containing mixed gas, the flow rate of the sulfur-containing atomized mixed gas, and one or more of the heating devices in the deposition chamber are adjusted to achieve uniform and high-purity zinc sulfide deposited on the surface of the deposition plate;
[0061] Specifically, by detecting the temperature in several deposition spaces and making different adjustment methods according to the different temperature differences between the temperature in different deposition spaces and the standard temperature, more accurate adjustment of different deposition spaces is realized, so as to achieve uniform deposition in each deposition space;
[0062] When the temperature difference between the temperature of several deposition spaces and the preset standard temperature is within 0 - 9°C, this temperature difference has a controllable impact on deposition and will not significantly affect the uniformity and purity of deposition, so no adjustment is required;
[0063] When the temperature difference between the temperature in the third deposition space to the m-th deposition space and the preset standard temperature is within 0 - 9°C, and the temperature in the first deposition space and the second deposition space is 10 - 15°C higher than the preset standard temperature, it is highly likely that the sulfur-containing atomized mixed gas entering the first deposition space and the second deposition space is less. Since the sulfur-containing atomized mixed gas enters the deposition chamber at a lower temperature and needs to absorb heat for the gasification of the elemental sulfur droplets after atomization, the temperature in the first deposition space and the second deposition space is 10 - 15°C higher than the preset standard temperature. Therefore, by increasing the flow rate of the sulfur-containing atomized mixed gas, it is beneficial for the sulfur-containing atomized mixed gas to diffuse into the first deposition space and the second deposition space, which is beneficial for reducing the temperature in the first deposition space and the second deposition space and does not significantly affect the uniform deposition in the third deposition space to the m-th deposition space;
[0064] When the temperature difference between the temperature in the third deposition space to the m-th deposition space and the preset standard temperature is within 0 - 9°C, and the temperature in the first deposition space and the second deposition space is 16 - 20°C higher than the preset standard temperature, the temperature difference in each deposition space is large and the temperature is unevenly distributed. Therefore, by adjusting the rotation rate of the deposition chamber, the temperature difference in each deposition space can be effectively reduced, the temperature in each deposition space can be made close to the standard temperature, and thus uniform deposition on the surface of each deposition plate can be achieved;
[0065] When the temperature in the third deposition space to the m-th deposition space is 10 - 20°C higher than the preset standard temperature, since the third deposition space to the m-th deposition space is closer to the heating device of the deposition chamber, when the temperature in the third deposition space to the m-th deposition space is relatively high, the main reason is that the heating temperature is too high. Therefore, by reducing the heating temperature of the heating device in the deposition chamber, the temperature of each deposition space is adjusted to reach the standard temperature and the temperature is uniform, so as to achieve high purity and uniform deposition of zinc sulfide on the surfaces of the deposition plates.
[0066] Furthermore, a first connecting member is provided on one side of the first deposition plate away from the deposition surface, and a second connecting member is provided on one side of the second deposition plate away from the deposition surface; the first connecting member and the second connecting member are connected by a mortise and tenon structure.
[0067] The beneficial effect of the previous step is that one side of the first deposition plate away from the deposition surface and one side of the second deposition plate away from the deposition surface are arranged opposite to each other and connected to form a deposition plate group; depositions are carried out on both deposition surfaces of multiple deposition plate groups, improving the deposition efficiency. At the same time, only one surface of the first deposition plate and the second deposition plate is deposited with zinc sulfide, so that after deposition, the first deposition plate and the second deposition plate can be separated, and then the deposited zinc sulfide can be detached from the first deposition plate and the second deposition plate without damaging the deposited zinc sulfide layer.
[0068] Furthermore, zinc sulfide polycrystalline materials are prepared by a CVD zinc sulfide polycrystalline material preparation device, and the CVD zinc sulfide polycrystalline material preparation device includes a deposition furnace main body, a sulfur atomization generating device, and an exhaust device;
[0069] The deposition furnace main body is provided with a deposition furnace inner cavity; a zinc vapor generating device is provided at the bottom inside the deposition furnace inner cavity;
[0070] Above the zinc vapor generating device, a rotating table device is arranged, and the rotating device is rotationally connected with a deposition chamber; a discharge box is arranged above the deposition chamber;
[0071] The zinc vapor generating device includes a crucible container and a crucible support, and the crucible container is provided with a detachably connected crucible cover body, a crucible air inlet, and a crucible air outlet;
[0072] The crucible air inlet is connected to an inert storage source; the crucible air outlet is communicated with the deposition chamber through a first air inlet pipe;
[0073] The sulfur atomization generating device comprises a sulfur storage tank and an atomizing device; the sulfur storage tank is provided with a heating device and a liquid outlet of the sulfur storage tank; the liquid outlet of the sulfur storage tank is connected to a pump body through a liquid infusion pipe; the pump body is connected to a first injection device through a liquid infusion pipe, and the first injection device is connected to an atomizing device; the atomizing device is connected to a deposition chamber through a second air inlet pipe; the first injection device is provided with a first inlet and a second inlet, the first inlet is connected to the sulfur storage tank through a liquid infusion pipe and a pump body, and the second inlet is connected to a high-speed gas storage tank;
[0074] Preferably, the exhaust hole of the deposition chamber is connected to a discharge box, and the discharge box is provided with a discharge box exhaust hole at a position away from the exhaust hole of the deposition chamber, and the discharge box exhaust hole is connected to an exhaust device.
[0075] Compared with the prior art, the present invention has the following beneficial effects: the deposition furnace body is provided with a deposition furnace inner cavity; the bottom of the deposition furnace inner cavity is provided with a zinc vapor generating device, so that zinc element is vaporized and enters the deposition chamber;
[0076] A rotating table device is arranged above the zinc vapor generating device, and the rotating device is rotatably connected to the deposition chamber, which effectively avoids uneven deposition thickness caused by different deposition temperatures at different positions in the deposition chamber;
[0077] A discharge box is arranged above the deposition chamber, the discharge box is connected to the discharge box through the discharge hole of the deposition chamber, the discharge box is provided with a discharge box exhaust hole at a position away from the discharge hole of the deposition chamber, and the discharge box exhaust hole is connected to the exhaust device, so that the uniformly mixed vaporized sulfur element and vaporized zinc element move from the bottom to the top from the bottom of the deposition chamber, and zinc sulfide is deposited on the surface of the deposition plate when passing between the deposition plates, and the generated ash and slag enter the discharge box upward and are discharged from the discharge box exhaust hole, thereby avoiding the ash and slag being dispersed on the surface of the deposition plate to cause the deposited zinc sulfide to contain impurities, and at the same time avoiding the problem of ash and slag accumulation in the deposition furnace;
[0078] The first injection device is provided with a first inlet and a second inlet, the first inlet is connected to the sulfur storage tank through an infusion tube and a pump body, and the second inlet is connected to a high-speed gas storage tank, so that the molten sulfur in the sulfur storage tank is vaporized and enters the atomizing device, and then the atomized sulfur liquid enters the deposition chamber, and the atomized sulfur monomer is instantly vaporized and dispersed evenly under the high temperature in the deposition chamber, so that the sulfur vapor and the zinc vapor are evenly dispersed in the deposition chamber, and the problem of sulfur monomer solidification during transportation leading to pipeline blockage or unstable flow is avoided when the sulfur monomer is vaporized in advance and then enters the deposition chamber; thereby, the zinc sulfide deposited on the surface of the deposition plate is uniform and high in purity.
[0079] Furthermore, the rotating table device includes a rotating table connecting part, a rotating shaft, a transmission mechanism, and a power device;
[0080] The rotary table connecting part is connected to the crucible cover or the deposition furnace body;
[0081] The rotating shaft is rotatably connected to the rotary table connecting part; one end of the rotating shaft is connected to the deposition chamber, and the other end of the rotating shaft is in transmission connection with the transmission mechanism;
[0082] The transmission mechanism is in transmission connection with the power device, and the power device is arranged outside the deposition furnace body;
[0083] Preferably, the transmission mechanism includes a first bevel gear, a second bevel gear, and a first transmission shaft; the first bevel gear is connected to the rotating shaft, and the first bevel gear meshes with the second bevel gear; the second bevel gear is connected to the first transmission shaft, the first transmission shaft is rotatably connected to the deposition furnace body through a bearing, and the first transmission shaft is in transmission connection with the power device.
[0084] The beneficial effect of the previous step is to realize the rotation of the rotary table, thereby driving the rotation of the deposition chamber.
[0085] Further, a plurality of deposition plates are provided at the bottom of the deposition chamber; the deposition plates include a first deposition plate and a second deposition plate;
[0086] The first deposition plate and the second deposition plate are oppositely arranged and connected to form a deposition plate group; a plurality of deposition plate groups are vertically arranged in the deposition chamber; a first connecting member is provided on the connecting surface of the first deposition plate and the second deposition plate, and a second connecting member is provided on the connecting surface of the second deposition plate and the first deposition plate; the first connecting member and the second connecting member are connected by a mortise and tenon structure;
[0087] A deposition space is formed between adjacent deposition plate groups;
[0088] The mixed gas of sulfur vapor and zinc vapor enters a plurality of deposition spaces and is on the surfaces of the deposition plate groups on both sides of the deposition space;
[0089] and / or
[0090] The inner cavity of the deposition furnace is a vertical semi-circular structure;
[0091] A water cooling device is provided on the outside of the deposition furnace body; a plurality of graphite heating elements are provided on the inner side wall and the bottom of the deposition furnace body;
[0092] Preferably, a temperature sensing device is provided in the deposition space, and the temperature sensing device is electrically connected to a temperature display arranged outside the deposition furnace body through an electric wire.
[0093] The beneficial effect of adopting the previous step is that several deposition plate groups are vertically arranged in the deposition chamber; a deposition space is formed between adjacent deposition plate groups, so as to realize the deposition of the uniformly mixed sulfur vapor and zinc vapor on the deposition surfaces of the first deposition plate and the second deposition plate, increasing the deposition efficiency; at the same time, since the first deposition plate and the second deposition plate are oppositely arranged and connected to form a deposition plate group, only one surface of the first deposition plate and the second deposition plate deposits zinc sulfide, and the deposition efficiency will not be reduced; thus, after deposition, the first deposition plate and the second deposition plate can be separated, and further, the deposited zinc sulfide can be detached from the first deposition plate and the second deposition plate without damaging the deposited zinc sulfide layer.
[0094] Since the inner cavity of the deposition furnace is of a vertical semi-circular structure, it helps to optimize the heat transfer path, reduce the heat transfer distance in the furnace body, and improve the heat transfer efficiency; especially in the high-temperature deposition process, this design can more effectively transfer heat to the sediment and promote the deposition reaction.
[0095] In a high-temperature deposition furnace, radiation heat transfer is the main heat transfer method; the semi-circular furnace body can make better use of the characteristics of radiation heat transfer, and improve the radiation heat transfer efficiency through multiple reflections and scatterings between the furnace wall and the sediment. Specific Embodiments
[0096] To better understand the technical solution of the present invention, the present invention will be further described below in conjunction with specific embodiments.
[0097] Embodiment 1:
[0098] This embodiment provides a method for preparing a patterned zinc sulfide polycrystalline material by CVD method, including the following steps:
[0099] Pretreat the deposition plate, and provide a patterned high surface energy deposition area on the deposition surface of the deposition plate; specifically including the following steps:
[0100] Take a graphite template of a preset size as the deposition plate;
[0101] Coat the deposition surface of the graphite template with a low surface energy reagent, and then heat the cleaned graphite template once in a drying device under a negative pressure environment;
[0102] Then successively clean the once-heated graphite template with n-hexane, chloroform, and isopropanol, and perform secondary heating after cleaning to obtain a low surface energy deposition plate;
[0103] Connect a mask plate to the deposition surface of the obtained low surface energy deposition plate; the mask plate is provided with a patterned hollow area identical to the patterned high surface energy deposition area;
[0104] Perform a high surface energy treatment on the deposition surface of a low surface energy deposition plate connected with a mask plate, to achieve high surface energy for the area of the deposition surface of the low surface energy deposition plate that is not covered by the mask plate, and obtain a deposition plate with a patterned high surface energy deposition area provided on the deposition surface;
[0105] The low surface energy reagent includes octadecyltrichlorosilane;
[0106] The heating temperature of the primary heating is 170 °C, the heating time is 3.5 h, and the pressure of the negative pressure environment is 0.090 Pa;
[0107] The heating temperature of the secondary heating is 65 °C, and the heating time is 4 h;
[0108] The process of performing a high surface energy treatment on the deposition surface of a low surface energy deposition plate connected with a mask plate includes treating the exposed position by oxygen plasma etching, and the treatment time is 16 min.
[0109] A plurality of deposition plates are vertically arranged in the deposition chamber; specifically, the deposition plates include a first deposition plate and a second deposition plate;
[0110] One side of the first deposition plate away from the deposition surface is arranged opposite to and connected with one side of the second deposition plate away from the deposition surface to form a deposition plate group; a first connecting piece is provided on one side of the first deposition plate away from the deposition surface, and a second connecting piece is provided on one side of the second deposition plate away from the deposition surface; the first connecting piece and the second connecting piece are connected by a mortise and tenon structure;
[0111] A plurality of deposition plate groups are vertically arranged in the deposition chamber; a deposition space is formed between adjacent deposition plate groups;
[0112] The mixed gas of sulfur vapor and zinc vapor enters a plurality of deposition spaces, on the surfaces of the deposition surfaces of the deposition plate groups on both sides of the deposition space;
[0113] The n deposition spaces are sequentially marked as the first deposition space, the second deposition space, the third deposition space to the m deposition space from the middle deposition space to the deposition spaces on both sides;
[0114] m = n / 2 or (n + 1) / 2.
[0115] Exhaust air from the deposition chamber through an exhaust device to maintain the gas pressure in the deposition chamber at 6500 Pa, and then introduce an inert gas;
[0116] Start the rotating device arranged below the deposition chamber, start the heating device of the deposition chamber, and heat the inside of the deposition chamber to a temperature of 690 °C;
[0117] Generate an atomized sulfur mixed gas through a sulfur atomization generating device, and introduce the atomized sulfur mixed gas into the deposition chamber;
[0118] A zinc vapor generating device is used to generate a zinc vapor-containing mixed gas, and the zinc vapor-containing mixed gas is introduced into a deposition chamber;
[0119] The flow rate of the sulfur atomized mixed gas is 11 slm; the flow rate of the zinc vapor-containing mixed gas is 5 slm;
[0120] The sulfur atomized mixed gas includes atomized sulfur droplets, hydrogen, and an inert gas; the volume ratio of hydrogen to atomized sulfur droplets is 1:2.5; the volume ratio of the inert gas to atomized sulfur droplets is 20:1;
[0121] The zinc vapor-containing mixed gas includes an inert gas and zinc vapor with a volume ratio of 18:1;
[0122] After introducing the zinc-containing mixed gas and the sulfur atomized mixed gas into the deposition chamber, the pressure in the deposition chamber is controlled at 6500 Pa; the inert gas is argon.
[0123] The process of generating a sulfur atomized mixed gas through a sulfur atomization generating device and introducing the sulfur atomized mixed gas into the deposition chamber includes the following steps:
[0124] Put sulfur into the sulfur storage pool of the sulfur atomization generating device, then evacuate the sulfur storage pool, and control the pressure in the sulfur storage pool at 6500 Pa; heat the internal space of the sulfur storage pool and maintain the internal temperature of the sulfur storage pool at 210 °C;
[0125] When the sulfur in the sulfur storage pool is in a molten state, the molten sulfur in the sulfur storage pool is pumped through a first spraying device and sprayed into an atomization device by a pump body. When the molten sulfur enters the atomization device, it is atomized by high-speed gas to obtain a sulfur atomized mixed gas; the flow rate of the high-speed gas is 105 m / s; the high-speed gas is a mixed gas of an inert gas and hydrogen;
[0126] The sulfur atomized mixed gas enters the deposition chamber from the atomization device; the atomized sulfur droplets in the sulfur atomized mixed gas are vaporized into sulfur vapor in the deposition chamber.
[0127] The specific process of generating a zinc vapor-containing mixed gas through a zinc vapor generating device and introducing the zinc vapor-containing mixed gas into the deposition chamber includes: putting zinc into the crucible container of the zinc vapor generating device, introducing an inert gas to displace the air in the crucible container, heating the inside of the crucible container, and the temperature of the crucible container is 675 °C; the zinc is vaporized into zinc vapor, and after mixing with the inert gas, it enters the deposition chamber.
[0128] An exhaust hole is provided above the deposition chamber. The exhaust hole of the deposition chamber is connected to a discharge box. A discharge box exhaust hole is provided at a position of the discharge box far from the exhaust hole of the deposition chamber, and the discharge box exhaust hole is connected to an exhaust device;
[0129] After introducing a zinc-containing mixed gas and an atomized sulfur-containing mixed gas into the deposition chamber, the discharge box is connected to the deposition chamber, and the waste gas is discharged through the discharge box.
[0130] The sulfur vapor and zinc vapor in the deposition chamber are mixed at high temperature and react on the surface of the deposition plate to obtain a zinc sulfide polycrystalline material.
[0131] Example 2:
[0132] The same content as in Example 1 will not be elaborated here; the different solutions in this example from Example 1 are as follows:
[0133] This example provides a method for preparing a patterned zinc sulfide polycrystalline material by CVD method, which further includes the following steps:
[0134] By a reaction control method, adjust one or more of the rotation rate of the deposition chamber, the flow rate of the zinc-containing mixed gas, the flow rate of the atomized sulfur-containing mixed gas, and the heating device of the deposition chamber to control the deposition process; the reaction control method includes the following steps:
[0135] Detect the temperatures of several deposition spaces; when the temperature difference between the temperatures of several deposition spaces and the preset standard temperature is within 0 - 9 °C, there is no need to adjust the rotation rate of the deposition chamber, the zinc vapor-containing mixed gas, and the flow rate of the atomized sulfur-containing mixed gas;
[0136] When the temperatures of the first deposition space and the second deposition space are higher than the preset standard temperature within 10 - 15 °C, increase the flow rate of the atomized sulfur-containing mixed gas;
[0137] When the temperatures of the first deposition space and the second deposition space are lower than the preset standard temperature within 10 - 15 °C, reduce the flow rate of the atomized sulfur-containing mixed gas;
[0138] When the temperatures of the first deposition space and the second deposition space are higher than the preset standard temperature within 16 - 20 °C, increase the rotation rate of the deposition chamber; when the temperatures of the first deposition space and the second deposition space are lower than the preset standard temperature within 16 - 20 °C, reduce the rotation rate of the deposition chamber;
[0139] When the temperatures of the third deposition space to the m-th deposition space are higher than the preset standard temperature within 10 - 20 °C, reduce the heating temperature of the heating device of the deposition chamber;
[0140] When the temperatures of the third deposition space to the m-th deposition space are lower than the preset standard temperature within 10 - 20 °C, increase the heating temperature of the heating device of the deposition chamber.
[0141] The heating temperature of the primary heating is 210 °C, the heating time is 2.5 h, and the pressure of the negative pressure environment is 0.095 Pa;
[0142] The heating temperature of the secondary heating is 60 °C, and the heating time is 4.5 h;
[0143] The process of performing high-surface-energy treatment on the deposition surface of the low-surface-energy deposition plate connected with the mask plate includes treating the exposed positions by means of oxygen plasma etching, and the treatment time is 25 min.
[0144] Turn on the rotating device arranged below the deposition chamber, turn on the heating device of the deposition chamber, and heat the inside of the deposition chamber to a temperature of 620 °C;
[0145] The flow rate of the sulfur-containing atomized mixed gas is 9 slm; the flow rate of the zinc-vapor-containing mixed gas is 4 slm;
[0146] The sulfur-containing atomized mixed gas includes atomized sulfur elemental droplets, hydrogen, and inert gas; the volume ratio of hydrogen to atomized sulfur elemental droplets is 1:2; the volume ratio of inert gas to atomized sulfur elemental droplets is 15:1;
[0147] The zinc-vapor-containing mixed gas includes an inert gas and zinc vapor with a volume ratio of 15:1;
[0148] After introducing the zinc-containing mixed gas and the sulfur-containing atomized mixed gas into the deposition chamber, control the pressure in the deposition chamber at 4000 Pa.
[0149] Put sulfur into the sulfur storage pool of the sulfur atomization generating device, then perform vacuum pumping on the sulfur storage pool, and control the pressure in the sulfur storage pool at 8000 Pa; heat the internal space of the sulfur storage pool, and maintain the internal temperature of the sulfur storage pool at 280 °C;
[0150] The flow rate of the high-speed gas is 180 m / s; the high-speed gas is a mixed gas of inert gas and hydrogen;
[0151] Put zinc into the crucible container of the zinc vapor generating device, introduce inert gas to displace the air in the crucible container, and after heating the inside of the crucible container, the temperature of the crucible container is 730 °C; the zinc is vaporized into zinc vapor, and after the zinc vapor is mixed with the inert gas, it enters the deposition chamber.
[0152] Example 3:
[0153] The same content as in Example 1 will not be elaborated here; the different solutions of this example from Example 1 are as follows:
[0154] This example provides a method for preparing a patterned zinc sulfide polycrystalline material by CVD method, and further includes the following steps:
[0155] By means of a reaction control method, adjust one or more of the deposition chamber rotation rate, the flow rate of the zinc-containing mixed gas, the flow rate of the atomized sulfur-containing mixed gas, and the heating device of the deposition chamber to control the deposition process; the reaction control method includes the following steps:
[0156] Detect the temperatures of a number of deposition spaces; when the temperature difference between the temperatures of the number of deposition spaces and the preset standard temperature is within 0-9°C, there is no need to adjust the deposition chamber rotation rate, the zinc vapor-containing mixed gas, or the flow rate of the atomized sulfur-containing mixed gas;
[0157] When the temperatures of the first deposition space and the second deposition space are higher than the preset standard temperature by 10-15°C, increase the flow rate of the atomized sulfur-containing mixed gas;
[0158] When the temperatures of the first deposition space and the second deposition space are lower than the preset standard temperature by 10-15°C, reduce the flow rate of the atomized sulfur-containing mixed gas;
[0159] When the temperatures of the first deposition space and the second deposition space are higher than the preset standard temperature by 16-20°C, increase the deposition chamber rotation rate; when the temperatures of the first deposition space and the second deposition space are lower than the preset standard temperature by 16-20°C, reduce the deposition chamber rotation rate;
[0160] When the temperatures of the third deposition space to the mth deposition space are higher than the preset standard temperature by 10-20°C, reduce the heating temperature of the heating device of the deposition chamber;
[0161] When the temperatures of the third deposition space to the mth deposition space are lower than the preset standard temperature by 10-20°C, increase the heating temperature of the heating device of the deposition chamber.
[0162] The heating temperature of the primary heating is 130°C, the heating time is 4.8 h, and the pressure of the negative pressure environment is 0.085 Pa;
[0163] The heating temperature of the secondary heating is 70°C, and the heating time is 3.2 h;
[0164] The process of performing a high surface energy treatment on the deposition surface of the low surface energy deposition plate connected with the mask plate includes treating the exposed positions by means of oxygen plasma etching, and the treatment time is 10 min.
[0165] Turn on the rotating device provided below the deposition chamber, turn on the heating device of the deposition chamber, and heat the inside of the deposition chamber to a temperature of 770°C;
[0166] The flow rate of the atomized sulfur-containing mixed gas is 14 s lm; the flow rate of the zinc vapor-containing mixed gas is 6.5 s lm;
[0167] The sulfur atomized mixed gas includes atomized sulfur elemental droplets, hydrogen, and inert gas; the volume ratio of hydrogen to atomized sulfur elemental droplets is 1:3.5; the volume ratio of inert gas to atomized sulfur elemental droplets is 28:1;
[0168] The zinc vapor mixed gas includes an inert gas and zinc vapor with a volume ratio of 22:1;
[0169] After introducing the zinc-containing mixed gas and the sulfur atomized mixed gas into the deposition chamber, the pressure in the deposition chamber is controlled at 9000 Pa.
[0170] Put sulfur elemental into the sulfur storage pool of the sulfur atomization device, then evacuate the sulfur storage pool, and control the pressure in the sulfur storage pool at 5000 Pa; heat the internal space of the sulfur storage pool to maintain the internal temperature of the sulfur storage pool at 150 °C;
[0171] The high-speed gas flow rate is 50 m / s; the high-speed gas is a mixed gas of inert gas and hydrogen;
[0172] Put zinc elemental into the crucible container of the zinc vapor generation device, introduce inert gas to displace the air in the crucible container, and after heating the inside of the crucible container, the temperature of the crucible container is 630 °C; the zinc elemental is vaporized into zinc vapor, and after the zinc vapor is mixed with the inert gas, it enters the deposition chamber.
[0173] The above description is only the preferred embodiment of the present application and the explanation of the applied technical principles. Those skilled in the art should understand that the scope of the invention involved in the present application is not limited to the technical solution formed by the specific combination of the above technical features, but should also cover other technical solutions formed by any combination of the above technical features or their equivalent features without departing from the inventive concept. For example, the technical solutions formed by mutually replacing the above features with the (but not limited to) technical features with similar functions disclosed in the present application.
Claims
1. A method for preparing patterned zinc sulfide polycrystalline material by CVD method, characterized in that: The following steps are involved: The deposition plate is pre-treated, and a patterned high surface energy deposition area is provided on the deposition surface of the deposition plate; a plurality of deposition plates are vertically arranged in the deposition chamber; Exhaust air from the deposition chamber through an exhaust device to maintain the gas pressure in the deposition chamber at 3000-10000 Pa, and then introduce inert gas; Turn on the rotating device provided under the deposition chamber, turn on the heating device of the deposition chamber, and heat the deposition chamber to a temperature of 600-780°C; A sulfur atomization generating device is used to generate a mixed gas containing atomized sulfur, and the mixed gas containing atomized sulfur is introduced into a deposition chamber; the mixed gas containing atomized sulfur includes atomized sulfur elemental liquid droplets and an inert gas; Generating a zinc vapor mixed gas by a zinc vapor generating device, and passing the zinc vapor mixed gas into a deposition chamber; the zinc vapor mixed gas comprises zinc vapor and an inert gas; The sulfur vapor and zinc vapor in the deposition chamber are mixed at high temperature and react on the surface of the deposition plate to obtain zinc sulfide polycrystalline material.
2. The method for preparing patterned zinc sulfide polycrystalline material by CVD method according to claim 1, characterized in that: The method of pre-treating a deposition plate to provide a patterned high surface energy deposition area on a deposition surface of the deposition plate comprises the following steps: A graphite template of a preset size is used as a deposition plate; The deposition surface of the graphite template is coated with a low surface energy reagent, and then the cleaned graphite template is heated once in a drying device under a negative pressure environment; Then, the graphite template after the primary heating is cleaned with a cleaning liquid, and then heated again after cleaning to obtain a low surface energy deposition plate; Connecting the obtained deposition surface of the low surface energy deposition plate to a mask plate; the mask plate is provided with a patterned hollow area that is the same as the patterned high surface energy deposition area; The deposition surface of a low surface energy deposition plate connected to a mask is subjected to high surface energy treatment, and the area of the deposition surface of the low surface energy deposition plate not covered by the mask is subjected to high surface energy treatment, thereby obtaining a deposition plate having a patterned high surface energy deposition area on the deposition surface.
3. The method for preparing patterned zinc sulfide polycrystalline material by CVD method according to claim 2, characterized in that: The low surface energy agent includes octadecyltrichlorosilane; The heating temperature of the primary heating is 120-220°C, the heating time is 2-5h, and the negative pressure environment has a pressure of ≤0.1Pa; The cleaning process of the cleaning liquid cleaning the graphite template after the first heating includes cleaning the graphite template after the first heating with n-hexane, chloroform and isopropanol in sequence; The secondary heating temperature is 50-80°C and the heating time is 3-5h; The process of performing high surface energy treatment on the deposition surface of the low surface energy deposition plate connected to the mask plate includes treating the exposed position by an oxygen plasma etching method, and the treatment time is 2-30 minutes.
4. The method for preparing patterned zinc sulfide polycrystalline material by CVD method according to claim 3, characterized in that: The flow rate of the mixed gas containing atomized sulfur is 8-15 slm; the flow rate of the mixed gas containing zinc vapor is 3-7 slm; The atomized sulfur-containing mixed gas includes atomized sulfur elemental liquid droplets, hydrogen, and an inert gas; the volume ratio of the hydrogen to the atomized sulfur elemental liquid droplets is 1:(1-4); the volume ratio of the inert gas to the atomized sulfur elemental liquid droplets is (10-30):1; The zinc vapor mixed gas comprises an inert gas and zinc vapor in a volume ratio of (10-25):1; After the zinc-containing mixed gas and the atomized sulfur-containing mixed gas are introduced into the deposition chamber, the pressure of the deposition chamber is controlled at 3000-10000Pa.
5. The method for preparing patterned zinc sulfide polycrystalline material by CVD method according to claim 4, characterized in that: A deposition chamber exhaust hole is provided above the deposition chamber, the deposition chamber exhaust hole is connected to a discharge box, the discharge box is provided with a discharge box exhaust hole at a position away from the deposition chamber exhaust hole, and the discharge box exhaust hole is connected to an exhaust device; After the zinc-containing mixed gas and the atomized sulfur-containing mixed gas are introduced into the deposition chamber, the discharge box is connected with the deposition chamber, and the waste gas is discharged through the discharge box.
6. The method for preparing patterned zinc sulfide polycrystalline material by CVD method according to claim 1, characterized in that: The process of generating a mixed gas containing atomized sulfur by a sulfur atomization generating device and passing the mixed gas containing atomized sulfur into a deposition chamber comprises the following steps: Put the sulfur into the sulfur storage tank of the sulfur atomization generating device, then evacuate the sulfur storage tank, and control the pressure of the sulfur storage tank at 3000-10000Pa; heat the internal space of the sulfur storage tank, and maintain the internal temperature of the sulfur storage tank at 130-300℃; When the sulfur in the sulfur storage tank is in a molten state, the molten sulfur in the sulfur storage tank is injected into the atomizing device through the pump body through the first injection device, and the molten sulfur is atomized by high-speed gas when entering the atomizing device to obtain a mixed gas containing atomized sulfur; the flow rate of the high-speed gas is 10-200m / s; the high-speed gas is a mixed gas of inert gas and hydrogen; The mixed gas containing atomized sulfur enters the deposition chamber from the atomizing device; the atomized sulfur element droplets in the mixed gas containing atomized sulfur are gasified into sulfur vapor in the deposition chamber.
7. The method for preparing patterned zinc sulfide polycrystalline material by CVD method according to claim 1, characterized in that: The process of generating a zinc vapor mixed gas by a zinc vapor generating device and passing the zinc vapor mixed gas into a deposition chamber comprises the following steps: Zinc is placed in a crucible container of a zinc vapor generating device, and an inert gas is introduced to replace the air in the crucible container. The inside of the crucible container is heated to a temperature of 600-750°C; the zinc is vaporized into zinc vapor, which is mixed with the inert gas and enters the deposition chamber.
8. The method for preparing patterned zinc sulfide polycrystalline material by CVD method according to claim 1, characterized in that: The deposition plate comprises a first deposition plate and a second deposition plate; A side of the first deposition plate away from the deposition surface and a side of the second deposition plate away from the deposition surface are arranged opposite to each other and connected to form a deposition plate group; A plurality of deposition plate groups are vertically arranged in the deposition chamber; A deposition space is formed between adjacent deposition plate groups; The sulfur vapor and zinc vapor mixed gas enters a plurality of deposition spaces and deposits on the surfaces of the deposition plate groups on both sides of the deposition spaces; The n deposition spaces are labeled as a first deposition space, a second deposition space, a third deposition space to an mth deposition space in sequence from the middle deposition space to the deposition spaces on both sides; m=n / 2 or (n+1) / 2.
9. The method for preparing patterned zinc sulfide polycrystalline material by CVD method according to claim 8, characterized in that: The method further includes adjusting one or more of the rotation rate of the deposition chamber, the flow rate of the zinc-containing mixed gas, the flow rate of the atomized sulfur-containing mixed gas, and the heating device of the deposition chamber by a reaction control method to control the deposition process; the reaction control method includes the following steps: The temperature of several deposition spaces is detected; when the temperature difference between several deposition spaces and the preset standard temperature is within 0-9°C, there is no need to adjust the rotation rate of the deposition chamber, the flow rate of the zinc vapor mixed gas, and the flow rate of the atomized sulfur mixed gas; When the temperature of the first deposition space and the second deposition space is higher than the preset standard temperature within 10-15°C, the flow rate of the mixed gas containing atomized sulfur is increased; When the temperature of the first deposition space and the second deposition space is lower than the preset standard temperature within 10-15°C, the flow rate of the mixed gas containing atomized sulfur is reduced; When the temperature of the first deposition space and the second deposition space is higher than the preset standard temperature within 16-20°C, the rotation rate of the deposition chamber is increased; when the temperature of the first deposition space and the second deposition space is lower than the preset standard temperature within 16-20°C, the rotation rate of the deposition chamber is reduced; When the temperature of the third deposition space to the mth deposition space is higher than the preset standard temperature within 10-20° C., reducing the heating temperature of the heating device of the deposition chamber; When the temperature of the third deposition space to the mth deposition space is lower than the preset standard temperature within 10-20° C., the heating temperature of the heating device of the deposition chamber is increased.
10. The method for preparing patterned zinc sulfide polycrystal by CVD method according to claim 9, characterized in that: A first connecting member is provided on a side of the first deposition plate away from the deposition surface, and a second connecting member is provided on a side of the second deposition plate away from the deposition surface; the first connecting member and the second connecting member are connected by a mortise and tenon structure.