CVD (Chemical Vapor Deposition) equipment for preparing zinc sulfide and preparation method

Abstract

The CVD equipment comprises a deposition chamber and further comprises a sulfur melting pool, an atomization device and a conveying device, the atomization device is connected with the deposition chamber and comprises a spraying part, the spraying part is provided with a first inner cavity, a second inner cavity and a crushing part which are isolated from one another, and the first inner cavity and the second inner cavity communicate with the crushing part; the sulfur melting tank is communicated with the first inner cavity through a conveying device and a third pipeline, the second inner cavity is communicated with the first pipeline, and the crushing part is communicated with the deposition chamber. The method has the beneficial effects that the quality of zinc sulfide products can be improved, and zinc sulfide is safely and efficiently prepared.

Description

Technical Field

[0001] The present invention relates to the technical field of material preparation, in particular to the field of zinc sulfide material preparation, and specifically refers to a CVD device and a preparation method for zinc sulfide. Background Art

[0002] Zinc sulfide is a typical II-VI compound and a wide bandgap material. It has the characteristics of stable chemical properties, strong environmental adaptability, easy processing, low light transmission loss, and strong light transmittance. It is widely used in the field of infrared optics. Common zinc sulfide preparation methods include hot pressing, physical vapor deposition, chemical vapor deposition (CVD), etc. Among them, the zinc sulfide product prepared by CVD has the advantages of high purity, dense material, flexible shape, and high transmittance. It is the most common zinc sulfide preparation method currently used.

[0003] In the prior art, when zinc sulfide is prepared by CVD method, hydrogen sulfide and zinc are usually used as raw materials. However, in the preparation process of zinc sulfide, the hydrogen ions in hydrogen sulfide are very easy to react with zinc to form Zn-H complex. The Zn-H complex is deposited in zinc sulfide, which will cause the zinc sulfide material to have an obvious absorption peak at 6um. At the same time, the presence of Zn-H complex will cause zinc sulfide lattice distortion, reduce the symmetry of lattice vibration, and increase the thermal radiation of standard zinc sulfide material itself with the increase of temperature. These problems will cause the transmittance of zinc sulfide material to infrared signal to decrease significantly, affecting the normal operation of infrared signal receiving equipment.

[0004] In addition, hydrogen sulfide, as a raw material, is highly toxic and poses a high safety hazard in every link including transportation, storage, use, and waste disposal. Once hydrogen sulfide leakage occurs, it will cause great harm to personnel and the environment, which undoubtedly increases the safety risk in the zinc sulfide preparation process. Summary of the invention

[0005] In view of the deficiencies in the prior art, the present invention provides a CVD device and a preparation method for preparing zinc sulfide by using sulfur as a raw material for preparing zinc sulfide, which can improve the quality of zinc sulfide products and is safe and efficient.

[0006] The present invention is achieved through the following technical scheme, which provides a CVD device for preparing zinc sulfide, including a deposition chamber, a molten sulfur pool, an atomizing device, and a conveying device. The atomizing device is connected to the deposition chamber, and the atomizing device includes an injection component. The injection component is provided with a first inner cavity, a second inner cavity and a crushing part which are isolated from each other. The first inner cavity and the second inner cavity are both connected to the crushing part. The molten sulfur pool is connected to the first inner cavity through the conveying device and the second pipeline, the second inner cavity is connected to the first pipeline, and the crushing part is connected to the deposition chamber.

[0007] Compared with the prior art, the beneficial effect of the present invention is that: through the molten sulfur pool, sulfur can be heated from solid to liquid, and the liquid sulfur melt is transported to the atomizing device through the conveying device, and then the liquid sulfur melt is broken into uniformly dispersed atomized droplets through the atomizing device and sprayed into the deposition chamber. After the atomized droplets of the sulfur melt enter the deposition chamber, they are rapidly gasified into sulfur vapor in the high temperature environment in the deposition chamber and react with zinc vapor to form a finished zinc sulfide product, thereby realizing the preparation of zinc sulfide using sulfur as a raw material. Compared with the prior art, since sulfur is used to replace hydrogen sulfide as a raw material for preparing zinc sulfide, the generation of Zn-H complexes in the preparation process of zinc sulfide is completely avoided, thereby improving the product quality of the finished zinc sulfide, and at the same time avoiding the safety hazards to personnel and the environment due to the severe toxicity of hydrogen sulfide when preparing zinc sulfide.

[0008] In addition, through the atomization device, the sulfur element can be transported into the deposition chamber in an atomized state. Compared with the gaseous state, the influence of environmental factors such as airflow and temperature on the sulfur element can be reduced, and the injection distance and distribution range of the sulfur element in the deposition chamber can be effectively improved, so that the vaporized sulfur element can be more comprehensively and evenly covered on the surface of the deposition plate, thereby improving the deposition efficiency and the uniformity of the deposition layer, and further improving the product quality of zinc sulfide.

[0009] Preferably, the second inner cavity is located outside the first inner cavity and surrounds the first inner cavity, the second inner cavity is concentrically arranged with the first inner cavity, a transition portion is provided on the side of the first inner cavity close to the crushing portion, the diameter of the transition portion of the first inner cavity gradually decreases from the side away from the crushing portion to the side close to the crushing portion, the diameter of the crushing portion is larger than the minimum diameter of the transition portion of the first inner cavity, and the injection component is provided with a trumpet-shaped discharge port.

[0010] The beneficial effect of adopting the above-mentioned preferred technical scheme is that: since the diameter of the transition part of the first inner cavity gradually decreases from the side far away from the crushing part to the side close to the crushing part, and the diameter of the crushing part is larger than the minimum diameter of the transition part of the first inner cavity, when the sulfur melt passes through the transition part of the first inner cavity, the flow rate of the sulfur melt will gradually increase. When the sulfur melt enters the crushing part, since the space of the crushing part suddenly becomes larger than the transition part of the first inner cavity, the flow rate of the sulfur melt will drop rapidly, so that the ejection medium can fully break the sulfur melt into atomized droplets in the crushing part. By setting the discharge port of the injection component as a trumpet-mouth structure, the atomized sulfur melt droplets can be evenly distributed in the deposition chamber, and at the same time, the speed of the atomized droplets can be reduced, and the occurrence of the atomized droplets re-aggregating into large droplets can be reduced, further improving the uniformity of the distribution of the sulfur melt droplets in the deposition chamber, and also making the atomized droplets easier to gasify.

[0011] Preferably, the atomization device also includes a control component connected to the injection component, the control component includes a first connecting part and a first sealing part, the first sealing part is located in the first inner cavity, the first inner cavity is provided with a first stop part, the first sealing part and the first stop part are both conical, the maximum diameter of the first sealing part is greater than the minimum diameter of the first stop part, and the first stop part is located at the connection between the first inner cavity and the crushing part.

[0012] The beneficial effect of adopting the above-mentioned preferred technical solution is that: since the first sealing part and the first stop part are both conical, and the maximum diameter of the first sealing part is greater than the minimum diameter of the first stop part, when the first sealing part is in contact with the first stop part, the first inner cavity and the crushing part can be isolated from each other to prevent the sulfur melt from leaking from the first inner cavity into the deposition chamber when the atomization device is shut down. The first connecting part can drive the first sealing part to move along the axial direction of the first inner cavity, thereby controlling the on-off state of the first inner cavity and the crushing part.

[0013] Preferably, a third inner cavity is provided inside the first connecting portion, an air hole is provided in the first sealing portion and the air hole is communicated with the third inner cavity, and compressed gas flows in the third inner cavity.

[0014] The beneficial effect of adopting the above-mentioned preferred technical solution is that when the compressed gas in the third inner cavity is sprayed toward the first stop part through the air holes on the first sealing component, it can provide a thrust for the first sealing component to move away from the first stop part, thereby preventing the first sealing component from being adsorbed on the first stop part and unable to be separated due to the vacuum generated during the cooling or sealing of the sulfur melt.

[0015] Preferably, the first inner cavity is provided with a first plating layer, and preferably, the first plating layer is a gold plating layer.

[0016] The beneficial effect of adopting the above preferred technical solution is that the first coating layer can effectively prevent the metal on the inner wall of the first inner cavity from being corroded by high-temperature sulfur and entering the deposition chamber with the sulfur melt to become an impurity, thereby affecting the purity of the zinc sulfide product.

[0017] Preferably, the atomization device also includes a recovery component connected to the deposition chamber, the recovery component is connected to the injection component, the injection component is connected to the deposition chamber through the recovery component, the recovery component is connected to the molten sulfur pool through a second pipe, and the second pipe is connected to a second switch component.

[0018] The beneficial effect of adopting the above-mentioned preferred technical solution is that: through the recovery component, droplets with larger particle sizes in the atomized sulfur melt can be separated out, which is conducive to the uniform distribution of the atomized sulfur melt in the deposition chamber, and the separated sulfur melt can also be returned to the molten sulfur pool through the second pipeline for reuse.

[0019] Preferably, a vacuum device is further included, wherein the vacuum device is connected to the molten sulfur pool via a fourth pipe, the molten sulfur pool is connected to the first inner cavity via a fifth pipe, and the fifth pipe is connected to a fifth switch component.

[0020] The beneficial effect of adopting the above-mentioned preferred technical solution is that: through the vacuum device, a vacuum negative pressure can be formed in the molten sulfur pool, and the gas in the molten sulfur pool can be extracted to prevent impurities in the gas in the molten sulfur pool from entering the deposition chamber with the sulfur melt, affecting the purity of the zinc sulfide product, thereby improving the product quality of zinc sulfide. In addition, through the vacuum device, after the preparation of zinc sulfide is completed, the sulfur melt remaining in the first inner cavity can be drawn back into the molten sulfur pool to prevent the cooled sulfur melt from clogging the first inner cavity.

[0021] Preferably, the first pipeline is connected to a first detection component, a first adjustment component, and a first switch component, the third pipeline is connected to a second detection component, a second adjustment component, and a third switch component, the deposition chamber is connected to a sixth pipeline, and the sixth pipeline is connected to a third detection component, a third adjustment component, and a sixth switch component.

[0022] Preferably, the deposition chamber is connected to a fourth detection component.

[0023] The beneficial effect of adopting the above preferred technical solution is that: the real-time flow of the injection medium and the sulfur melt can be monitored by the first detection component and the second detection component, and the flow of the sulfur melt and the injection medium can be accurately adjusted by adjusting the first adjustment component, the second adjustment component, and the third adjustment component based on the first detection component and the second detection component to make them meet the specified flow size, thereby achieving the best atomization effect of the sulfur melt;

[0024] Through the fourth detection component, the content of sulfur vapor and zinc vapor in the deposition chamber can be detected in real time. When the content of sulfur vapor or zinc vapor does not conform to the set range, the first adjustment component, the second adjustment component or the third adjustment component is automatically adjusted, so that the content of sulfur vapor or zinc vapor in the deposition chamber can always be within the set range.

[0025] Preferably, the raw material contained in the molten sulfur pool is elemental sulfur, and the molten sulfur pool is connected to a heating device.

[0026] The present invention also provides a method for preparing zinc sulfide, comprising the following steps:

[0027] Firstly, through simulation software simulation, according to the set particle size requirements of the atomized sulfur melt droplets, the flow rate of the sulfur melt in the first inner cavity and the flow rate of the ejection medium in the second inner cavity are determined;

[0028] After that, sulfur with a purity of 99.999% is placed in the molten sulfur pool and heated. At the same time, a vacuum device is used to form a vacuum negative pressure inside the molten sulfur pool.

[0029] Afterwards, when the sulfur element is heated from a solid state to a liquid state, the sulfur melt in the molten sulfur pool is transported to the first inner cavity of the injection component through the conveying device. At the same time, the ejection medium enters the second inner cavity of the injection component through the first pipe. The sulfur melt and the ejection medium are mixed in the crushing part of the injection component. The high-speed ejection medium breaks the liquid sulfur melt into tiny droplets. The atomized sulfur melt enters the recovery component together with the ejection medium. The sulfur melt droplets with larger particle sizes after crushing are recovered to the molten sulfur pool through the recovery component, and the rest of the atomized sulfur melt is ejected into the deposition chamber. During the atomization process of the sulfur melt, the flow rates of the ejection medium and the sulfur melt are monitored in real time by the first detection component and the second detection component, and the flow rates of the ejection medium and the sulfur melt are accurately adjusted by the first adjustment component and the second adjustment component.

[0030] When the atomized sulfur melt enters the deposition chamber, the temperature in the deposition chamber is controlled at 600-750°C, and the pressure is controlled at 3000-8000 Pa. The atomized sulfur melt entering the deposition chamber is rapidly evaporated into sulfur vapor. At the same time, zinc vapor enters the deposition chamber through the sixth pipeline. The content of sulfur vapor and zinc vapor in the deposition chamber is detected in real time by the fourth detection component, and the detection signal is fed back to the control system. The control system compares the detection result with the set content of sulfur vapor and zinc vapor. When the content of sulfur or zinc in the deposition chamber does not meet the requirements, the first adjustment component, the second adjustment component or the third adjustment component is automatically adjusted until the detection result of the fourth detection component meets the requirements, and the zinc vapor reacts with the sulfur vapor in the deposition chamber and generates zinc sulfide on the deposition plate.

[0031] When the preparation of zinc sulfide is completed, the first switch component, the third switch component, and the sixth switch component are closed, and the second switch component and the fifth switch component are opened. The control component isolates the first inner cavity of the injection component from the crushing part, and the vacuum device draws the remaining molten sulfur in the first inner cavity and the recovery component back into the molten sulfur pool to prevent the molten sulfur after shutdown and cooling from clogging the first inner cavity, the recovery component and the pipeline. BRIEF DESCRIPTION OF THE DRAWINGS

[0032] Figure 1 It is the schematic diagram of the device of the present invention;

[0033] Figure 2 It is a schematic diagram of the structure of the injection component and the control component in the present invention.

[0034] As shown in the figure:

[0035] 1. deposition chamber, 2. molten sulfur pool, 3. atomizing device, 4. conveying device, 5. vacuum device, 6. first pipeline, 7. first switch component, 8. first detection component, 9. first regulating component, 10. second pipeline, 11. second switch component, 12. third pipeline, 13. second regulating component, 14. second detection component, 15. third switch component, 16. fourth pipeline, 17. fourth switch component, 18. fifth pipeline, 19. fifth switch component, 20. sixth pipeline, 21. sixth switch component, 22. third detection component, 23. third regulating component, 24. fourth detection component;

[0036] 301, injection component, 302, recovery component, 303, control component;

[0037] 3011, first inner cavity, 3012, second inner cavity, 3013, crushing part, 3014, first stopping part;

[0038] 3031. A first connecting portion. 3032. A first sealing portion. DETAILED DESCRIPTION

[0039] The technical solutions in the embodiments of the present invention are described clearly and completely below. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0040] Embodiment 1:

[0041] like Figure 1-2The CVD equipment for preparing zinc sulfide shown in the figure includes a deposition chamber 1, a molten sulfur pool 2, an atomizing device 3, a conveying device 4, and a vacuum device 5. The atomizing device 3 is connected to the deposition chamber 1. The atomizing device 3 includes an injection component 301, a recovery component 302, and a control component 303. The injection component 301 is provided with a first inner cavity 3011 and a second inner cavity 3012 that are isolated from each other. The second inner cavity 3012 is located outside the first inner cavity 3011 and surrounds the first inner cavity 3011. The first inner cavity 3011 and the second inner cavity 3012 are connected to each other. The inner cavity 3012 is arranged concentrically, and a transition portion is provided on the side of the first inner cavity 3011 close to the crushing portion 3013. The diameter of the transition portion of the first inner cavity 3011 gradually decreases from the side away from the crushing portion 3013 to the side close to the crushing portion 3013. The diameter of the crushing portion 3013 is larger than the minimum diameter of the transition portion of the first inner cavity 3011. The injection component 301 is provided with a trumpet-shaped discharge port. The first inner cavity 3011 is connected to the molten sulfur pool 2 through the conveying device 4. The second inner cavity 3012 is connected to the first inner cavity 3011 through which the injection medium flows. The first pipe 6 is connected to the atomizing device 3, and the first pipe 6 is connected to the atomizing device 3. In this embodiment, preferably, the injection medium is argon gas, and the flow rate of the injection medium is 10-200m / s. The injection component 301 is also provided with a crushing part 3013. The first inner cavity 3011 and the second inner cavity 3012 are both connected to the crushing part 3013. The high-speed injection medium crushes the low-speed sulfur melt into fine droplets in the crushing part 3013. The sulfur melt can be atomized and injected into the deposition chamber 1 by the injection component 301. The first pipe 6 is connected to the first switch part 3013 from near to far from the atomizing device 3. Part 7, first detection component 8, first adjustment component 9, in this embodiment, preferably, the first switch component 7, the first detection component 8, and the first adjustment component 9 are respectively a high-temperature electric gate valve, a gas flow meter, and an electric regulating valve. The inner wall of the first inner cavity 3011 is provided with a first coating. In this embodiment, preferably, the first coating is a gold coating. The first coating can prevent the high-temperature molten sulfur from corroding the inner wall metal of the first inner cavity 3011, thereby preventing the atomized molten sulfur entering the deposition chamber 1 from being mixed with metal impurities;

[0042] The control component 303 is connected to the injection component 301, and the control component 303 includes a first connection part 3031 and a first sealing part 3032. The first sealing part 3032 is located in the first inner cavity 3011, and the first connection part 3031 is connected to the first sealing part 3032. A first stopper 3014 is provided at the junction of the first inner cavity 3011 and the crushing part 3013. The first sealing part 3032 and the first stopper 3014 are both conical. The maximum diameter of the first sealing part 3032 is greater than the minimum diameter of the first stopper 3014. After the first stopper 3014 is fitted, the first inner cavity 3011 and the crushing portion 3013 can be isolated from each other. The first connecting portion 3031 can drive the first sealing portion 3032 to move forward and backward along the axial direction of the first inner cavity 3011, thereby controlling the connection state between the first inner cavity 3011 and the crushing portion 3013. A third inner cavity is provided inside the first connecting portion 3031. The first sealing portion 3032 is provided with an air hole, and the air hole is connected to the third inner cavity. The third inner cavity is connected to a compressed gas pipeline, and a switch valve is provided on the compressed gas pipeline.

[0043] The recovery component 302 includes an air inlet, an air outlet, a recovery port, and a folding baffle. The air inlet of the recovery component 302 is connected to the crushing part 3013 of the injection component 301, and the air outlet is connected to the deposition chamber 1. In the air flow path from the air inlet to the air outlet, a plurality of folding baffles are sequentially arranged according to the direction of the air flow. The recovery port of the recovery component 302 is located at the bottom of the recovery component 302. The recovery port is connected to the molten sulfur pool 2 through the second pipeline 10. When the atomized sulfur melt enters the recovery component 302 from the injection component 301, the sulfur melt It collides with several folding baffles in sequence. When the airflow collides with the folding baffles, a sudden turn will occur. In this process, the droplets tend to leave the airflow due to inertia. The larger the droplet size, the greater the inertia force. Therefore, the folding baffle can separate the large-size droplets in the atomized sulfur melt. The separated large-size droplets return to the molten sulfur pool 2 through the second pipe 10. A second switch component 11 is provided on the second pipe 10. In this embodiment, preferably, the second switch component 11 is a high-temperature electric gate valve;

[0044] The molten sulfur pool 2 is located at one side of the deposition chamber 1. The molten sulfur pool 2 contains sulfur. The molten sulfur pool 2 is connected to a heating device, and the sulfur in the molten sulfur pool 2 can be heated from a solid state to a liquid state through the heating device. The conveying device 4 is connected to the molten sulfur pool 2. The conveying device 4 is connected to the first inner cavity 3011 of the atomizing device 3 through a third pipeline 12. On the third pipeline 12, a second regulating component 13, a second detecting component 14, and a third switching component 15 are sequentially connected from near to far from the conveying device 4. In this embodiment, preferably, the second regulating component 13, the second detecting component 14, and the third switching component 15 are respectively an electric regulating valve, a liquid flow meter, and an electric gate valve;

[0045] The vacuum device 5 is connected to the molten sulfur pool 2 through a fourth pipe 16, and a fourth switch component 17 is connected to the fourth pipe 16. In this embodiment, preferably, the fourth switch component 17 is an electric gate valve. The molten sulfur pool 2 is also connected to the first inner cavity 3011 of the injection component 301 through a fifth pipe 18, and a fifth switch component 19 is connected to the fifth pipe 18. The fifth pipe 18 is connected to the third pipe 12 or the fifth pipe 18 is directly connected to the first inner cavity 3011. When the fifth pipe 18 is connected to the third pipe 12, the connection between the fifth pipe 18 and the third pipe 12 is located between the third switch component 15 and the first inner cavity 3011. When the control component 303 isolates the first inner cavity 3011 from the crushing part 3013, the fifth pipe 18 can be used to draw the remaining sulfur melt in the first inner cavity 3011 back into the molten sulfur pool 2 through the vacuum device 5;

[0046] The deposition chamber 1 is also connected to a sixth pipeline 20, which is used for the circulation of zinc vapor. A sixth switch component 21, a third detection component 22, and a third adjustment component 23 are connected to the sixth pipeline 20 in sequence from near to far from the deposition chamber 1. In the present embodiment, the sixth switch component 21, the third detection component 22, and the third adjustment component 23 are respectively an electric gate valve, a gas flow meter, and an electric control valve. A fourth detection component 24 is connected to the deposition chamber 1. In the present embodiment, preferably, the fourth detection component 24 is an infrared gas detector. Through the fourth detection component 24, the content of the gas entering the deposition chamber 1 can be detected in real time.

[0047] This embodiment also provides a method for preparing zinc sulfide using the above-mentioned CVD equipment for preparing zinc sulfide:

[0048] First, through simulation software simulation, according to the set particle size requirements of the sulfur melt droplets after atomization, the flow rate of the sulfur melt in the first inner cavity 3011 and the flow rate of the injection medium in the second inner cavity 3012 are determined;

[0049] Afterwards, sulfur with a purity of 99.999% is placed in the molten sulfur pool 2, and the temperature in the molten sulfur pool 2 is controlled within the range of 130-300° C. by a heating device. At the same time, a vacuum device 5 is used to form a vacuum negative pressure inside the molten sulfur pool 2, and the vacuum degree is controlled within the range of 3000-10000 Pa to prevent gas impurities in the molten sulfur pool 2 from entering the deposition chamber 1 and affecting the purity of the zinc sulfide product.

[0050] Afterwards, when the sulfur element is heated from a solid state to a liquid state, the sulfur melt in the molten sulfur pool 2 is transported to the first inner cavity 3011 of the injection component 301 through the conveying device 4. At the same time, the ejection medium enters the second inner cavity 3012 of the injection component 301 through the first pipe 6. The sulfur melt and the ejection medium are mixed in the crushing part 3013 of the injection component 301. The high-speed ejection medium breaks the liquid sulfur melt into tiny droplets. The atomized sulfur melt enters the recovery component 302 together with the ejection medium. The sulfur melt droplets with larger particle sizes after crushing are recovered to the molten sulfur pool 2 through the recovery component 302. The rest of the atomized sulfur melt is ejected into the deposition chamber 1. During the atomization process of the sulfur melt, the flow rates of the ejection medium and the sulfur melt are monitored in real time by the first detection component 8 and the second detection component 14, and the flow rates of the ejection medium and the sulfur melt are accurately adjusted by the first adjustment component 9 and the second adjustment component 13.

[0051] When the atomized sulfur melt enters the deposition chamber 1, the temperature in the deposition chamber 1 is controlled at 600-750°C, and the pressure is controlled at 3000-8000 Pa. The atomized sulfur melt entering the deposition chamber 1 is rapidly evaporated into sulfur vapor. At the same time, zinc vapor enters the deposition chamber 1 through the sixth pipe 20. The content of sulfur vapor and zinc vapor in the deposition chamber 1 is detected in real time by the fourth detection component 24, and the detection signal is fed back to the control system. The control system compares the detection result with the set content of sulfur vapor and zinc vapor. When the sulfur or zinc content in the deposition chamber 1 does not meet the requirements, the first adjustment component 9, the second adjustment component 13 or the third adjustment component 23 are automatically adjusted until the detection result of the fourth detection component 24 meets the requirements, and the zinc vapor reacts with the sulfur vapor in the deposition chamber 1 and generates zinc sulfide on the deposition plate.

[0052] When the preparation of zinc sulfide is completed, the first switch component 7, the third switch component 15, and the sixth switch component 21 are closed, the second switch component 11 and the fifth switch component 19 are opened, and the fourth switch component 17 remains opened. The control component 303 isolates the first inner cavity 3011 of the injection component 301 from the crushing part 3013, and the vacuum device 5 draws the remaining molten sulfur in the first inner cavity 3011 and the recovery component 302 back into the molten sulfur pool 2 to prevent the molten sulfur after shutdown and cooling from clogging the first inner cavity 3011, the recovery component 302 and the pipeline.

[0053] The above embodiments are only used to illustrate the technical solutions of the present invention, rather than to limit them; based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention. Although the present invention has been described in detail with reference to the above embodiments, ordinary technicians in this field should understand that they can still modify the technical solutions recorded in the above embodiments, or replace some of the technical features therein by equivalents; and these modifications or replacements do not make the essence of the corresponding technical solutions deviate from the spirit and scope of the technical solutions of the embodiments of the present invention.

Claims

1. A CVD apparatus for preparing zinc sulfide, comprising a deposition chamber (1), characterized in that: The invention also comprises a molten sulfur pool (2), an atomizing device (3), and a conveying device (4), wherein the atomizing device (3) is connected to the deposition chamber (1), the atomizing device (3) comprises an injection component (301), the injection component (301) is provided with a first inner cavity (3011), a second inner cavity (3012), and a crushing part (3013) which are isolated from each other, the first inner cavity (3011) and the second inner cavity (3012) are both connected to the crushing part (3013), the molten sulfur pool (2) is connected to the first inner cavity (3011) through the conveying device (4) and a third pipeline (12), the second inner cavity (3012) is connected to the first pipeline (6), and the crushing part (3013) is connected to the deposition chamber (1).

2. A CVD device for preparing zinc sulfide according to claim 1, characterized in that: The second inner cavity (3012) is located outside the first inner cavity (3011) and surrounds the first inner cavity (3011); the second inner cavity (3012) is concentrically arranged with the first inner cavity (3011); a transition portion is provided on the side of the first inner cavity (3011) close to the crushing portion (3013); the diameter of the transition portion of the first inner cavity (3011) gradually decreases from the side far from the crushing portion (3013) to the side close to the crushing portion (3013); the diameter of the crushing portion (3013) is larger than the minimum diameter of the transition portion of the first inner cavity (3011); and the injection component (301) is provided with a trumpet-shaped discharge port.

3. A CVD device for preparing zinc sulfide according to claim 1, characterized in that: The atomizing device (3) further comprises a control component (303) connected to the spraying component (301), wherein the control component (303) comprises a first connecting portion (3031) and a first sealing portion (3032), wherein the first sealing portion (3032) is located in the first inner cavity (3011), and the first inner cavity (3011) is provided with a first stop portion (3014), wherein the first sealing portion (3032) and the first stop portion (3014) are both conical, wherein the maximum diameter of the first sealing portion (3032) is greater than the minimum diameter of the first stop portion (3014), and the first stop portion (3014) is located at the connection between the first inner cavity (3011) and the crushing portion (3013).

4. A CVD device for preparing zinc sulfide according to claim 3, characterized in that: A third inner cavity is provided inside the first connecting portion (3031), an air hole is provided in the first sealing portion (3032) and the air hole is communicated with the third inner cavity, and compressed gas flows in the third inner cavity.

5. A CVD device for preparing zinc sulfide according to claim 1, characterized in that: The first inner cavity (3011) is provided with a first coating, and preferably, the first coating is a gold coating.

6. A CVD device for preparing zinc sulfide according to claim 1, characterized in that: The atomizing device (3) further comprises a recovery component (302) connected to the deposition chamber (1), the recovery component (302) being connected to the injection component (301), the injection component (301) being connected to the deposition chamber (1) via the recovery component (302), the recovery component (302) being connected to the molten sulfur pool (2) via a second pipe (10), and the second pipe (10) being connected to a second switch component (11).

7. A CVD device for preparing zinc sulfide according to claim 1, characterized in that: It also includes a vacuum device (5), which is connected to the molten sulfur pool (2) through a fourth pipe (16), and the molten sulfur pool (2) is connected to the first inner cavity (3011) through a fifth pipe (18), and the fifth pipe (18) is connected to a fifth switch component (19).

8. A CVD device for preparing zinc sulfide according to claim 1, characterized in that: The first pipeline (6) is connected to a first detection component (8), a first adjustment component (9), and a first switch component (7); the third pipeline is connected to a second detection component (14), a second adjustment component (13), and a third switch component (15); the deposition chamber (1) is connected to a sixth pipeline (20); the sixth pipeline (20) is connected to a third detection component (22), a third adjustment component (23), and a sixth switch component (21); and the deposition chamber (1) is connected to a fourth detection component (24).

9. A CVD device for preparing zinc sulfide according to claim 1, characterized in that: The raw material contained in the molten sulfur pool (2) is sulfur element, and the molten sulfur pool (2) is connected to a heating device.

10. A method for preparing zinc sulfide, for preparing zinc sulfide by using the CVD equipment for preparing zinc sulfide according to any one of claims 1 to 9, characterized in that: First, through simulation software, according to the set particle size requirements of the sulfur melt droplets after atomization, the flow rate of the sulfur melt in the first inner cavity (3011) and the flow rate of the injection medium in the second inner cavity (3012) are determined; Then, sulfur with a purity of 99.999% is placed in a molten sulfur pool (2) and heated, and at the same time, a vacuum device (5) is used to form a vacuum negative pressure inside the molten sulfur pool (2); Afterwards, when the sulfur element is heated from a solid state to a liquid state, the sulfur melt in the molten sulfur pool (2) is transported to the first inner cavity (3011) of the injection component (301) through the transport device (4). At the same time, the injection medium enters the second inner cavity (3012) of the injection component (301) through the first pipe (6). The sulfur melt and the injection medium are mixed in the crushing part (3013) of the injection component (301). The high-speed injection medium crushes the liquid sulfur melt into tiny droplets. The atomized sulfur melt The molten sulfur enters the recovery component (302) together with the ejection medium, and the molten sulfur droplets with larger particle sizes after being crushed are recovered into the molten sulfur pool (2) through the recovery component (302), and the remaining atomized molten sulfur is sprayed into the deposition chamber (1). During the atomization process of the molten sulfur, the flow rates of the ejection medium and the molten sulfur are monitored in real time by the first detection component (8) and the second detection component (14), and the flow rates of the ejection medium and the molten sulfur are accurately adjusted by the first adjustment component (9) and the second adjustment component (13); When the atomized sulfur melt enters the deposition chamber (1), the temperature in the deposition chamber (1) is controlled at 600-750°C and the pressure is controlled at 3000-8000 Pa. The atomized sulfur melt entering the deposition chamber (1) is rapidly evaporated into sulfur vapor. At the same time, zinc vapor enters the deposition chamber (1) through the sixth pipe (20). The content of sulfur vapor and zinc vapor in the deposition chamber (1) is detected in real time by the fourth detection component (24), and the detection signal is fed back to the control system. The control system compares the detection result with the set content of sulfur vapor and zinc vapor. When the content of sulfur or zinc in the deposition chamber (1) does not meet the requirements, the first adjustment component (9), the second adjustment component (13) or the third adjustment component (23) automatically adjusts until the detection result of the fourth detection component (24) meets the requirements. The zinc vapor reacts with the sulfur vapor in the deposition chamber (1) and generates zinc sulfide on the deposition plate. When the preparation of zinc sulfide is completed, the first switch component (7), the third switch component (15), and the sixth switch component (21) are closed, and the second switch component (11) and the fifth switch component (19) are opened. The control component (303) isolates the first inner cavity (3011) of the injection component (301) from the crushing part (3013), and the vacuum device (5) draws the remaining molten sulfur in the first inner cavity (3011) and the recovery component (302) back into the molten sulfur pool (2) to prevent the molten sulfur after shutdown and cooling from clogging the first inner cavity (3011), the recovery component (302) and the pipeline.

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