Automatic hydrogen sulfide supply device

Abstract

An automatic hydrogen sulfide gas supply device is suitable for supplying hydrogen sulfide gas to CVD grown zinc sulfide blocks. The automatic hydrogen sulfide gas supply device comprises a basic steel cylinder module, a standby steel cylinder module, an anti-explosion heating fan, a hydrogen sulfide gas supply main line and a control cabinet. The basic steel cylinder module comprises n panel groups, n is greater than or equal to 2, the standby steel cylinder module comprises one panel group, the one panel group is defined as the (n + 1) th panel group, each panel group comprises m panels, m is greater than or equal to 2, each panel comprises a hydrogen sulfide steel cylinder, the hydrogen sulfide steel cylinder is filled with hydrogen sulfide liquefied gas, and m is greater than or equal to 2. Each panel group is used for supplying hydrogen sulfide gas formed by vaporization of liquefied hydrogen sulfide of the hydrogen sulfide steel cylinders to the hydrogen sulfide gas supply main line at the same time by all panels of the panel group when gas supply is executed, and the anti-explosion heating fan is used for heating and controlling the temperature of the hydrogen sulfide steel cylinders of all the panel groups; and the control cabinet is connected to the hydrogen sulfide gas supply main line and is in communication connection with and controls the basic steel cylinder module, the standby steel cylinder module and the anti-explosion heating fan.

Description

Technical Field

[0001] The present disclosure relates to the field of chemical vapor deposition (CVD) growth of zinc sulfide (ZnS), and more specifically to an automatic hydrogen sulfide gas supply device. Background Art

[0002] With the continuous advancement of science and technology, the application prospects of zinc sulfide in various fields are also constantly expanding, especially in the field of optoelectronic materials. Zinc sulfide has a wide transmission band (0.35-13μm), and has good transmittance in visible light, near infrared, medium-wave infrared and long-wave infrared. It has excellent optical and mechanical properties and is currently an important long-wave infrared window material and full-band optoelectronic window material.

[0003] High-quality zinc sulfide is usually prepared by chemical vapor deposition, using high-purity zinc and high-purity highly toxic H2S (hydrogen sulfide) gas as raw materials, and high-purity inert gas Ar gas as carrier gas. Zn is evaporated into Zn vapor in the temperature range of 550-750°C, and is carried into the deposition chamber by Ar gas. It reacts with H2S gas also carried into the deposition chamber by Ar gas in the temperature range of 600-850°C to obtain CVD-ZnS product. The chemical equation is Zn+H2S=ZnS+H2, CVD The preparation of CVD-ZnS by this method requires a stable and uninterrupted gas supply device to continuously supply H2S gas to the deposition chamber to ensure stable and continuous crystal growth (depending on the size of the CVD-grown zinc sulfide block and the production capacity of the deposition chamber, the entire duration from the start of gas supply to the end of CVD-grown zinc sulfide block is as long as dozens of days), so that the molar ratio of hydrogen sulfide to zinc reacts according to 1:1. During the crystal growth process, the H2S flow rate fluctuates or even stops, which will cause zinc sulfide crystals to have quality defects such as material points and fog layers, and the optical properties will decrease. In addition, the saturated vapor of hydrogen sulfide gas is greatly affected by the ambient temperature. The saturated vapor pressure at 35°C is twice that of the saturated vapor at 5°C. The lower the ambient temperature, the lower the saturated vapor pressure, and the more unstable the gas supply. When in use, the liquid hydrogen sulfide in the zinc sulfide cylinder absorbs a lot of heat when it vaporizes, and ice forms at the bottom of the hydrogen sulfide cylinder, further reducing the temperature in the zinc sulfide cylinder and reducing the saturated vapor pressure of hydrogen sulfide. The currently adopted technical solution is to connect the gas pipeline through a hydrogen sulfide cylinder, manually open the hydrogen sulfide cylinder and the gas valve, and promptly replace an empty hydrogen sulfide cylinder in the continuous gas supply with a full cylinder. Before replacing the empty hydrogen sulfide cylinder, it is necessary to manually close the corresponding gas valve and manually replace the residual highly toxic hydrogen sulfide gas in the gas pipeline. The residual highly toxic hydrogen sulfide gas is not completely replaced, hydrogen sulfide gas leaks, and people are poisoned. Manual operation is complicated and time is limited. Relying on manpower is full of uncertainties and cannot ensure the stable and continuous output of hydrogen sulfide gas during the CVD-ZnS crystal growth process. Summary of the invention

[0004] In view of the problems existing in the background technology, an object of the present disclosure is to provide a hydrogen sulfide automatic gas supply device, which can stably and continuously operate the hydrogen sulfide gas supply automatically during the entire duration from the start of gas supply to the end of CVD growth of zinc sulfide blocks.

[0005] Another object of the present disclosure is to provide an automatic hydrogen sulfide gas supply device, which avoids the occurrence of an empty hydrogen sulfide cylinder that is used up during the entire duration from the start of gas supply to the end of CVD growth of zinc sulfide blocks.

[0006] Another object of the present disclosure is to provide an automatic hydrogen sulfide gas supply device, which can reduce the impact of switching on the stability of gas supply.

[0007] Another object of the present disclosure is to provide an automatic hydrogen sulfide gas supply device, which can ensure the reliability of gas supply during the entire duration from the start of gas supply to the end of CVD growth of zinc sulfide blocks.

[0008] Thus, a hydrogen sulfide automatic gas supply device is suitable for supplying hydrogen sulfide gas to a CVD-grown zinc sulfide block. The hydrogen sulfide automatic gas supply device includes a basic cylinder module, a spare cylinder module, an explosion-proof heating fan, a hydrogen sulfide gas supply main line, and a control cabinet; the basic cylinder module includes n panel groups, n≥2, the spare cylinder module includes 1 panel group, the 1 panel group is defined as the n+1th panel group, each panel group includes m panels, m≥2, each panel includes a hydrogen sulfide cylinder, and the hydrogen sulfide cylinder is filled with The panel group is equipped with liquefied hydrogen sulfide gas. When the gas supply is executed, all panels of the panel group simultaneously supply the hydrogen sulfide gas formed by vaporizing the liquefied hydrogen sulfide in the hydrogen sulfide cylinder to the hydrogen sulfide gas supply main line. The explosion-proof heating fan is used to heat and control the temperature of the hydrogen sulfide cylinders of all panel groups. The control cabinet is connected to the hydrogen sulfide gas supply main line to receive the hydrogen sulfide gas and communicate with and control the basic cylinder module, the spare cylinder module, and the explosion-proof heating fan. The n panel groups of the basic cylinder module and the spare The panel group of the cylinder module is controlled by the control cabinet as follows: after the hydrogen sulfide gas supply is started, the n panel groups of the basic cylinder module are switched from the 1st panel group to the nth panel group in sequence to supply hydrogen sulfide gas for the first cycle of gas supply. When the first cycle of gas supply reaches the point where the nth panel group is switched, it is determined whether to switch to the n panel groups of the basic cylinder module for the next cycle from the 1st panel group to the nth panel group in sequence to supply hydrogen sulfide gas or to switch to the panel group in the spare cylinder module for gas supply. When the panel group in the spare cylinder module cannot supply gas, it is switched to the n panel groups of the basic cylinder module from the 1st panel group to the nth panel group in sequence to supply hydrogen sulfide gas, and so on, until the gas supply provided by the n panel groups of the basic cylinder module and the panel group in the spare cylinder module completes the CVD growth of zinc sulfide blocks.

[0009] The beneficial effects of the present disclosure are as follows.

[0010] In the hydrogen sulfide automatic gas supply device according to the present disclosure, the hydrogen sulfide cylinders of all panels together with the entire gas supply pipeline only need to be prepared before the gas supply starts, and then the hydrogen sulfide gas supply main line can be automatically and continuously supplied with hydrogen sulfide gas through the communication control between the control cabinet and the n panel groups of the basic cylinder module and the panel groups of the spare cylinder module, until the gas supply provided by the n panel groups of the basic cylinder module and the panel groups in the spare cylinder module completes the CVD growth of zinc sulfide blocks. In this way, no manual operation is required during the entire duration from the start of gas supply to the end of CVD growth of zinc sulfide blocks, eliminating the uncertainty caused by human factors in the background technology, and realizing the stable and continuous automatic operation of hydrogen sulfide gas supply during the entire duration from the start of gas supply to the end of CVD growth of zinc sulfide blocks, thereby being able to achieve stable and continuous CVD growth of zinc sulfide blocks (i.e., CVD growth of zinc sulfide blocks in the deposition chamber).

[0011] In the hydrogen sulfide automatic gas supply device according to the present disclosure, the switching of the n panel groups of the basic cylinder module in sequence and the switching between the n panel groups of the basic cylinder module and the panel groups in the spare cylinder module (i.e., the entire duration from the start of gas supply to the end of CVD growth of zinc sulfide blocks) can avoid the occurrence of a used-up empty hydrogen sulfide cylinder as in the background art. At a certain moment in the entire duration from the start of gas supply to the end of CVD growth of zinc sulfide blocks, gas supply is provided by a certain panel group, and all panels of the panel group simultaneously supply hydrogen sulfide gas formed by vaporizing liquefied hydrogen sulfide in the hydrogen sulfide cylinder to the hydrogen sulfide gas supply main line, while the hydrogen sulfide cylinders of all panels of the other remaining panel groups will be in an idle state without gas supply, which allows the liquefied hydrogen sulfide in the hydrogen sulfide cylinder in the idle state without gas supply sufficient time to vaporize to form (i.e., regenerate) hydrogen sulfide gas, especially for the hydrogen sulfide cylinder that has been supplied with gas before this certain moment.

[0012] In the automatic hydrogen sulfide gas supply device according to the present disclosure, whether the gas supply time of the first panel group of the basic cylinder module in this cycle is less than the specified time is used to determine whether the n panel groups of the basic cylinder module are switched from the first panel group to the nth panel group in sequence to supply hydrogen sulfide or whether the gas supply is switched from the nth panel group of the basic cylinder module 1 to the panel group in the spare cylinder module. During the entire duration from the start of gas supply to the end of CVD growth of zinc sulfide blocks, the total number of switching times of the panel groups of the basic cylinder module can be reduced, thereby reducing the impact of switching on the stability of gas supply.

[0013] In the automatic hydrogen sulfide gas supply device according to the present disclosure, at a certain moment in the entire duration from the start of gas supply to the end of CVD growth of zinc sulfide blocks, gas supply is provided by a certain panel group, and all panels of the panel group simultaneously supply hydrogen sulfide gas formed by vaporizing liquefied hydrogen sulfide in the hydrogen sulfide cylinder to the hydrogen sulfide gas supply main line, thereby ensuring the reliability of gas supply of the panel group, and then ensuring the reliability of gas supply in the entire duration from the start of gas supply to the end of CVD growth of zinc sulfide blocks, thereby ensuring the reliability of stable and continuous CVD growth of zinc sulfide blocks.

[0014] In the hydrogen sulfide automatic gas supply device according to the present disclosure, the explosion-proof heating fan is used to heat and control the temperature of the hydrogen sulfide cylinders of all panel groups. Through the heating and temperature control of the explosion-proof heating fan, the temperature of all hydrogen sulfide cylinders is controlled, so that the saturated vapor pressure in all hydrogen sulfide cylinders is stabilized, thereby stabilizing the gas supply of the vaporized hydrogen sulfide gas in the hydrogen sulfide cylinders, and further stabilizing the gas supply of each panel group and the process of CVD growth of zinc sulfide blocks. BRIEF DESCRIPTION OF THE DRAWINGS

[0015] Figure 1 is a structural layout diagram of the automatic hydrogen sulfide gas supply device according to the present disclosure, wherein a deposition chamber is shown.

[0016] Figure 2 yes Figure 1 An enlarged view of a portion of the basic cylinder module.

[0017] Figure 3 yes Figure 1 An enlarged view of another portion of the basic cylinder module.

[0018] Figure 4 yes Figure 1 A magnified view of the spare cylinder module.

[0019] Figure 5 yes Figure 1 An enlarged view of a single panel of the hydrogen sulfide automatic gas supply device.

[0020] Figure 6 yes Figure 1 Schematic diagram of the support frame of the hydrogen sulfide automatic gas supply device.

[0021] Figure 7 yes Figure 1 Schematic diagram of the porous ventilation plate of the hydrogen sulfide automatic gas supply device.

[0022] Figure 8 yes Figure 1 A structural layout diagram of a portion of an example of an automatic hydrogen sulfide gas supply device, wherein n=5 and m=2.

[0023] Fig. 9 yes Figure 8 An enlarged view of a portion of the basic cylinder module.

[0024] Fig.10 yes Figure 8 An enlarged view of another portion of the basic cylinder module.

[0025] Fig.11 yes Figure 8 A magnified view of the spare cylinder module.

[0026] Fig.12 yes Figure 1 Flow chart of the gas supply procedure of the hydrogen sulfide automatic gas supply device.

[0027] Fig.13 yes Figure 1 Flow chart of the replacement gas procedure for a single panel of a hydrogen sulfide automatic gas supply device.

[0028] Fig.14 yes Figure 1 Flow chart of the working procedures of the explosion-proof heating fan of the hydrogen sulfide automatic gas supply device.

[0029] The reference numerals are described as follows:

[0030] 1000 Hydrogen sulfide automatic gas supply device P jk 8a The first argon filling pipeline

[0031] 1 Basic cylinder module P jk 8b Second argon filling pipeline

[0032] 2 Spare cylinder module P jk 9 Exhaust pipe

[0033] 3 Explosion-proof Heating Fan P jk 10 Exhaust pipe

[0034] 4 Hydrogen sulfide gas supply main line P jk 11 Vacuum generator

[0035] 5Control Cabinet P jk 12a First check valve

[0036] G i / G j Panel Group P jk 12b Second check valve

[0037] P jk Panel 6' First Cylinder Cabinet

[0038] P jk 1 Hydrogen sulfide cylinder 6" second cylinder cabinet

[0039] P jk 2 Cylinder interface 6" spare cylinder cabinet

[0040] P jk 3 Cylinder connecting pipe 61 cabinet

[0041] P jk 4 Pressure regulating valve 61a air outlet

[0042] P jk 5a First pneumatic valve 61b air return port

[0043] P jk 5b The second pneumatic valve 62 porous ventilation plate

[0044] P jk 5c The third pneumatic valve 63 support frame

[0045] P jk 5d Fourth pneumatic valve 7' first air duct

[0046] P jk 6a First digital pressure gauge 7" Second air duct

[0047] P jk 6b Second digital pressure gauge 2000 deposition chamber

[0048] P jk 7 Explosion-proof electronic scale DETAILED DESCRIPTION

[0049] It will be understood that the disclosed embodiments are merely examples of the present disclosure, which may be implemented in various forms, and therefore, the specific details disclosed herein should not be interpreted as limiting, but merely as a basis for the claims and as a representative basis for teaching one of ordinary skill in the art to implement the present disclosure in various ways.

[0050] [Automatic hydrogen sulfide gas supply device]

[0051] Reference Figures 1 to 5 as well as Fig.12According to the present disclosure, the hydrogen sulfide automatic gas supply device 1000 is suitable for supplying hydrogen sulfide gas to CVD grown zinc sulfide blocks. The hydrogen sulfide automatic gas supply device 1000 includes a basic cylinder module 1, a spare cylinder module 2, an explosion-proof heating fan 3, a hydrogen sulfide gas supply main line 4, and a control cabinet 5.

[0052] The basic cylinder module 1 includes n panel groups G i , i=1,2,...,n,n≥2,

[0053] The spare cylinder module 2 includes 1 panel group, which is defined as the n+1th panel group G n+1 ,

[0054] Each panel group G j (j=1,2,...,n+1) includes m panels P jk , j represents the panel group number, j = 1, 2, ..., n + 1, k represents the panel number in the corresponding panel group, k = 1, 2, ..., m, m ≥ 2, each panel P jk Includes a hydrogen sulfide cylinder P jk 1 , Hydrogen sulfide cylinder P jk 1 Filled with liquefied hydrogen sulfide, each panel group G j (j=1, 2, ..., n+1) is used for the panel group G when the gas supply is executed. j All panels P of (j=1,2,...,n+1) jk At the same time, the hydrogen sulfide cylinder P jk 1 The hydrogen sulfide gas formed by vaporizing the liquefied hydrogen sulfide is supplied to the hydrogen sulfide gas supply main line 4;

[0055] Explosion-proof heating fan 3 for all panel groups G j (j=1,2,...,n+1) hydrogen sulfide cylinder P jk 1 Carry out heating and temperature control;

[0056] The control cabinet 5 is connected to the hydrogen sulfide gas supply main line 4 to receive the hydrogen sulfide gas and communicate with and control the basic cylinder module 1, the spare cylinder module 2, and the explosion-proof heating fan 3;

[0057] Basic cylinder module 1 n panel group G i (i=1,2,...,n) and panel group G of spare cylinder module 2 n+1 Controlled by control cabinet 5:

[0058] After the hydrogen sulfide gas supply is started, the n panel groups G of the basic cylinder module 1 i(i=1,2,...,n) from the 1st panel group G1 to the nth panel group G n Switch to hydrogen sulfide gas supply in sequence to carry out the first cycle of gas supply.

[0059] In the first cycle, the gas supply is carried out to the nth panel group G. n When the gas supply is switched, the n panels in the basic cylinder module 1 are grouped G i Whether the gas supply time of the first panel group G1 in (i=1,2,...,n) in this cycle (i.e., the communication feedback from the control cabinet 5) is less than the specified time, determines whether to switch to the n panel groups G of the basic cylinder module 1 for the next cycle. i (i=1,2,...,n) from the 1st panel group G1 to the nth panel group G n Switch to hydrogen sulfide gas supply or switch to the panel group G in the spare cylinder module 2 n+1 Gas supply, when spare cylinder module 2 in panel group G n+1 When the gas supply is no longer available, switch to the n panel group G of the basic cylinder module 1 i (i=1,2,...,n) from the 1st panel group G1 to the nth panel group G n Switch to supply hydrogen sulfide in sequence, and so on, until the n panel groups G of the basic cylinder module 1 i (i=1,2,...,n) and panel group G in spare cylinder module 2 n+1 The gas supply provided together completes the CVD growth of the zinc sulfide bulk.

[0060] In more detail, the n panel groups G1, G2, ..., G n Panel Group G of Spare Cylinder Module 2 n+1 Controlled by control cabinet 5:

[0061] After the hydrogen sulfide gas supply is started, the n panel groups G1, G2, ..., G n From the 1st panel group G1 to the nth panel group G n Switching to supply hydrogen sulfide gas in sequence to carry out the first cycle of gas supply;

[0062] In the first cycle, the gas supply is carried out to the nth panel group G. n When the gas supply is switched,

[0063] If n panel groups G1, G2, ..., G in the basic cylinder module 1 are determined n If the air supply time of the first panel group G1 in this cycle is not less than the specified time, then the nth panel group G nThe gas supply is switched to the first panel group G1 in the basic cylinder module 1 to perform the operation from the first panel group G1 to the nth panel group G n Switch to the next cycle of gas supply in sequence.

[0064] If n panel groups G1, G2, ..., G in the basic cylinder module 1 are determined n If the air supply time of the first panel group G1 in this cycle is less than the specified time, then the nth panel group G n Gas supply to panel group G is switched to spare cylinder module 2 n+1 To execute Panel Group G in Spare Cylinder Module 2 n+1 To supply gas, when the panel group G in the spare cylinder module 2 n+1 When the gas supply is unable to be supplied and needs to be switched, the panel group G in the spare cylinder module 2 n+1 Switched to n panel groups G1 in basic cylinder module 1,

[0065] G2, ..., G n The first panel group G1 in the n Switch to the next cycle of gas supply in sequence.

[0066] In the next cycle, the gas supply is carried out to the nth panel group G. n When the gas supply is switched, repeat the first cycle to supply gas to the nth panel group G. n The gas supply is switched to supply gas, and so on, until the n panel groups G1, G2, ..., G n and Panel Group G in Spare Cylinder Module 2 n+1 The gas supply provided together completes the CVD growth of the zinc sulfide bulk.

[0067] In the hydrogen sulfide automatic gas supply device 1000 according to the present disclosure, all panels P jk Hydrogen sulfide cylinder P jk 1 The entire gas supply pipeline only needs to be prepared before the gas supply starts, and then the control cabinet 5 and the n panel groups G1, G2, ..., G n Panel Group G of Spare Cylinder Module 2 n+1 The communication control between the two automatically and continuously supplies hydrogen sulfide gas to the hydrogen sulfide gas supply main line 4 until the n panel groups G1, G2, ..., G n and Panel Group G in Spare Cylinder Module 2 n+1The gas supply provided together completes the CVD growth of the zinc sulfide block. In this way, no manual operation is required during the entire duration from the start of gas supply to the end of the CVD growth of the zinc sulfide block, eliminating the uncertainty caused by the human factor in the background technology, and realizing the stable and continuous automatic operation of the hydrogen sulfide gas supply during the entire duration from the start of gas supply to the end of the CVD growth of the zinc sulfide block, thereby being able to achieve stable and continuous CVD growth of the zinc sulfide block (i.e. Figure 1 (ZnS bulk is grown by CVD in deposition chamber 2000).

[0068] In the hydrogen sulfide automatic gas supply device 1000 according to the present disclosure, the n panel groups G1, G2, ..., G n Switch in sequence with the n panel groups G1, G2, ..., G of the basic cylinder module 1 n With spare cylinder module 2 in panel group G n+1 The switching between the two (i.e., the entire duration from the start of gas supply to the end of CVD growth of zinc sulfide blocks) can avoid the situation in which a certain empty hydrogen sulfide cylinder is used up as in the background art. At a certain moment in the entire duration from the start of gas supply to the end of CVD growth of zinc sulfide blocks, the gas supply is controlled by a certain panel group G. j (j=1,2,...,n+1) to provide, and the panel group G j All panels P of (j=1,2,...,n+1) jk At the same time, the hydrogen sulfide cylinder P jk 1 The hydrogen sulfide gas formed by the vaporization of the liquefied hydrogen sulfide is supplied to the hydrogen sulfide gas supply main line 4, while the remaining panel group G j All panels P of (j=1,2,...,n+1) jk Hydrogen sulfide cylinder P jk 1 The hydrogen sulfide cylinder P in the idle and unsupplied state jk 1 The liquefied hydrogen sulfide in the cylinder has sufficient time to vaporize (i.e., regenerate) hydrogen sulfide gas, especially for the hydrogen sulfide cylinder P that has been supplied with gas before a certain time. jk 1 .

[0069] Specifically, Figures 8 to 11 For example (n=5, m=2), in the first cycle, among the five panel groups G1, G2, G3, G4, and G5 of the basic cylinder module 1, when the first panel group G1 is unable to supply gas, it is switched to the second panel group G2 for gas supply. During the gas supply process of the second panel group G2, the first panel group G1 performs gas regeneration (i.e., the hydrogen sulfide cylinder P 111 and P 12 1 When the second panel group G2 cannot supply gas, it is switched to the third panel group G3 for gas supply. During the gas supply process of the third panel group G3, the first panel group G1 continues to regenerate gas (i.e., the hydrogen sulfide cylinder P 11 1 and P 12 1 Continue gas regeneration), the second panel group G2 starts gas regeneration (i.e. hydrogen sulfide cylinder P 21 1 and P 22 1 When the gas supply of the third panel group G3 reaches the point where it can no longer supply gas, it is switched to the fourth panel group G4 for gas supply. During the gas supply process of the fourth panel group G4, the first panel group G1 continues to regenerate gas (i.e., the hydrogen sulfide cylinder P 11 1 and P 12 1 Continue gas regeneration), the second panel group G2 continues gas regeneration (i.e. hydrogen sulfide cylinder P 21 1 and P 22 1 Continue gas regeneration), the third panel group G3 starts gas regeneration (i.e. hydrogen sulfide cylinder P 31 1 and P 32 1 When the gas supply of the 4th panel group G4 reaches the point where it can no longer supply gas, it is switched to the 5th panel group G5 for gas supply. During the gas supply process of the 5th panel group G4, the 1st panel group G1 continues to regenerate gas (i.e., the hydrogen sulfide cylinder P 11 1 and P 12 1 Continue gas regeneration), the second panel group G2 continues gas regeneration (i.e. hydrogen sulfide cylinder P 21 1 and P 22 1 Continue gas regeneration), the third panel group G3 continues gas regeneration (i.e. hydrogen sulfide cylinder P 31 1 and P 32 1 Continue gas regeneration), the fourth panel group G4 starts gas regeneration (i.e. hydrogen sulfide cylinder P 41 1 and P 42 1Start gas regeneration); when the fifth panel group G5 cannot supply gas, the five panel groups G1, G2, G3, G4, and G5 of the basic cylinder module 1 complete the first cycle of gas supply. At this time, the next gas supply depends on the gas supply time of the first panel group G1 of the basic cylinder module 1 in this cycle. If the gas supply time of the first panel group G1 in this cycle is not less than the specified time, the basic cylinder module 1 will circulate again; if the gas supply time of the first panel group G1 in this cycle is less than the specified time, it will switch to the panel group G6 in the spare cylinder module 2 for gas supply (that is, the hydrogen sulfide cylinder P 61 1 and P 62 1 Gas supply), during the gas supply process of panel group G6 in the spare cylinder module 2, the 5 panel groups G1, G2, G3, G4, and G5 of the basic cylinder module 1 continue to regenerate gas until the panel group G6 in the spare cylinder module 2 can no longer supply gas, and then switches to the basic cylinder module 1, and then the 5 panel groups G1, G2, G3, G4, and G5 of the basic cylinder module 1 start to switch in sequence for the second cycle of gas supply, and so on.

[0070] In the hydrogen sulfide automatic gas supply device 1000 according to the present disclosure, it is determined whether the gas supply time of the first panel group G1 of the basic cylinder module 1 in this cycle is less than the specified time to determine whether the n panel groups G1, G2, ..., G3 of the basic cylinder module 1 are to be operated. n From the 1st panel group G1 to the nth panel group G n Switch to hydrogen sulfide gas supply from the nth panel group G of the basic cylinder module 1 n Switch to Panel Group G in Spare Cylinder Module 2 n+1 Gas supply, during the entire duration from the start of gas supply to the end of CVD growth of zinc sulfide bulk, can reduce the panel groups G1, G2, ..., G n The total number of switching times can be reduced, thereby reducing the impact of switching on the stability of the gas supply.

[0071] In the hydrogen sulfide automatic gas supply device 1000 according to the present disclosure, at a certain moment in the entire duration from the start of gas supply to the end of CVD growth of zinc sulfide blocks, the gas is supplied by a certain panel group G j (j=1,2,...,n+1) to provide, and the panel group G j All panels P of (j=1,2,...,n+1) jk At the same time, the hydrogen sulfide cylinder P jk 1 The hydrogen sulfide gas formed by the vaporization of the liquefied hydrogen sulfide is supplied to the hydrogen sulfide gas supply main line 4, thus ensuring that the panel group G j(j=1, 2, ..., n+1) The reliability of gas supply is ensured, thereby ensuring the reliability of gas supply during the entire duration from the start of gas supply to the end of CVD growth of zinc sulfide bulk, thereby ensuring the reliability of stable and continuous CVD growth of zinc sulfide bulk.

[0072] In the hydrogen sulfide automatic gas supply device 1000 according to the present disclosure, the explosion-proof heating fan 3 is used to heat all the panel groups G j (j=1,2,...,n+1) hydrogen sulfide cylinder P jk 1 Heating and temperature control are performed, and the explosion-proof heating fan 3 is used to heat and control the temperature, so that all hydrogen sulfide cylinders P jk 1 The temperature of all hydrogen sulfide cylinders P jk 1 The saturated vapor pressure in the hydrogen sulfide cylinder P is stable, so that jk 1 The gas supply of vaporized hydrogen sulfide gas is stable, so that each panel group G j The gas supply of (j=1, 2, ..., n+1) is stable and the process of CVD growth of zinc sulfide bulk is stable.

[0073] In one example, multiple panel groups G j (j=1,2,...,n+1) Panel group G to be supplied with gas when switching between j (j=1,2,...,n+1) Panel group G that switches and stops supplying gas j (j=1,2,...,n+1) delay closing. Specifically, when the first panel group G1 switches to the second panel group G2, the second G2 switches to the air supply, and the first panel group G1 delays closing, and so on to the n-1th panel group G n-1 Switch to panel group G n ; The nth panel group G n Switch to panel group G (n+1) n+1 When the n+1th panel group G n+1 Switch to gas supply, nth panel group G n Delayed closing; n+1th panel group G n+1 When switching to the first panel group G1, the first panel group G1 switches to air supply, and the n+1th panel group G n+1 Delayed closing. Specifically, for example, the delay time is 5-30s.

[0074] Reference Fig.12 In one example, the n panel groups G of the basic cylinder module 1 i (i=1,2,...,n)(i.e. G1, G 2、 ...、Gn ) from the first panel group G1 to the nth panel group G n Switch and spare cylinder module 2 in panel group G n+1 Switched to n panel group G in basic cylinder module 1 i (i=1,2,...,n)(i.e. G1, G 2、 ...、G n ) is executed when one of the following conditions is met:

[0075] Condition 1: Corresponding panel group G j Each panel P of (j=1,2,...,n+1) jk Hydrogen sulfide cylinder P jk 1 The net weight of hydrogen sulfide in the container is less than the prescribed weight;

[0076] Condition 2: Corresponding panel group G j Each panel P of (j=1,2,...,n+1) jk Hydrogen sulfide cylinder P jk 1 The gas supply pressure of hydrogen sulfide gas in the tank is lower than the specified gas supply pressure;

[0077] The nth panel group G n Gas supply to panel group G is switched to spare cylinder module 2 n+1 To execute Panel Group G in Spare Cylinder Module 2 n+1 Gas supply is performed under the following conditions:

[0078] Condition 3: The gas supply time of the first panel group G1 of the basic cylinder module 1 in this cycle is less than the specified time.

[0079] Specifically, in one example, the specified weight is 1-5 kg; the specified air supply pressure is 2-8 kg / cm 2 ; The specified time is 0.5-6h. Accordingly, before the first cycle of gas supply begins, the n panel groups G of the basic cylinder module 1 i (i=1,2,...,n)(i.e. G1, G 2、 ...、G n ) and Panel Group G in Spare Cylinder Module 2 n+1 Each panel P jk Hydrogen sulfide cylinder P jk 1 The net weight of hydrogen sulfide is 10-30kg, the pressure of hydrogen sulfide gas in the bottle is 1.5-3.5MPa, and the gas supply pressure of hydrogen sulfide gas is 1-10kg / cm 2 .

[0080] Reference Figures 1 to 5 In one example, each panel P jk (j=1,2,...,n+1,k=1,2,..,m) also includes the cylinder interface P jk 2 、Cylinder connecting pipe P jk 3 , Pressure regulating valve P jk 4 , the first pneumatic valve P jk 5a , the first digital pressure gauge P jk 6a , explosion-proof electronic scale P jk 7 Each panel P jk (j=1,2,...,n+1,k=1,2,..,m) hydrogen sulfide cylinder P jk 1 It has a valve (not shown) that can be opened and closed manually. The valve is located in the hydrogen sulfide cylinder P. jk 1 Bottle body and cylinder interface P jk 2 At the beginning of the first cycle of air supply, each panel P jk (j=1,2,...,n+1,k=1,2,..,m) hydrogen sulfide cylinder P jk 1 The valve itself is opened manually, in panel group G of basic cylinder module 1 i (i=1,2,...,n)(i.e. G1, G 2、 ...、G n ) and Panel Group G in Spare Cylinder Module 2 n+1 When the gas supply provided together completes the CVD growth of zinc sulfide bulk, each panel P jk (j=1,2,...,n+1,k=1,2,..,m) hydrogen sulfide cylinder P jk 1 The valve itself is closed manually. Cylinder interface P jk 2 Connect to the cylinder connection pipe P jk 3 One end of the cylinder connection pipe P jk 3 The other end is connected to the hydrogen sulfide gas supply main line 4. Pressure regulating valve P jk 4 Set up the cylinder connecting pipe P jk 3 Upper, pressure regulating valve P jk 4 Communicate with control cabinet 5, pressure regulating valve P jk 4For regulating via cylinder port P jk 2 Connect the pipe P to the cylinder jk 3 The hydrogen sulfide cylinder P jk 1 The gas supply pressure of hydrogen sulfide gas formed by the vaporization of liquefied hydrogen sulfide. The first pneumatic valve P jk 5a Set up the cylinder connecting pipe P jk 3 On and in the pressure regulating valve P jk 4 Downstream of the first pneumatic valve P jk 5a The first pneumatic valve P is connected to the control cabinet 5. jk 5a is used to open and close the cylinder connected to the pipeline P under the control of the control cabinet 5. jk 3 The first digital pressure gauge P is connected and disconnected with the hydrogen sulfide gas supply main line 4. jk 6a At the cylinder interface P jk 2 And pressure regulating valve P jk 4 The position between them is connected to the cylinder connecting pipe P jk 3 , the first digital pressure gauge P jk 6a The first digital pressure gauge P is connected to the control cabinet 5. jk 6a Used to detect gas from the cylinder interface P jk 2 Connect the pipe P to the cylinder jk 3 The hydrogen sulfide cylinder P jk 1 The liquefied hydrogen sulfide vaporizes to form hydrogen sulfide gas in the pressure regulating valve P jk 4 The pressure before. Explosion-proof electronic scale P jk 7 For monitoring hydrogen sulfide cylinder P jk 1 The net weight of hydrogen sulfide in the chamber is communicated with the control cabinet 5. In this example, the first pneumatic valve P jk 5a The first pneumatic valve P jk 5a It is connected to the control cabinet 5 to realize the manual operation of the hydrogen sulfide cylinder P except before the gas supply starts and after the CVD growth of zinc sulfide blocks is completed. jk 1In addition to its own valve, during the entire duration of the gas supply start and the end of CVD growth of zinc sulfide blocks, the cylinder is connected to the pipeline P jk 3 The hydrogen sulfide gas supplied to the hydrogen sulfide gas supply main line 4 is automatically controlled without manual operation. jk 6a The communication between the control cabinet 5 realizes the monitoring of the above condition 2, through the explosion-proof electronic scale P jk 7 The communication between the control cabinet 5 realizes the monitoring of the above-mentioned condition 1, through the first pneumatic valve P jk 5a The opening and closing of the control cabinet 5 and the communication with the control cabinet 5 realize the monitoring of the above-mentioned condition 3.

[0081] Specifically, each panel P jk (j=1,2,...,n+1,k=1,2,..,m) pressure regulating valve P jk 4 , the first pneumatic valve P jk 5a , the first digital pressure gauge P jk 6a , explosion-proof electronic scale P jk 7 Control: In each panel P jk When (j=1, 2, ..., n+1, k=1, 2, ..., m) is supplied with air, the control cabinet 5 controls the first pneumatic valve P jk 5a Open, control cabinet 5 controls the pressure regulating valve P jk 4 To adjust the hydrogen sulfide cylinder P jk 1 Via cylinder port P jk 2 Connect the pipe P to the cylinder jk 3 The supply pressure of hydrogen sulfide gas supplied to the hydrogen sulfide gas supply main line 4 is shown in the first digital pressure gauge P jk 6a Display the gas supply pressure and communicate it to the control cabinet 5, explosion-proof electronic scale P jk 7 Real-time monitoring of hydrogen sulfide cylinder P jk 1 The weight of the hydrogen sulfide gas is measured and communicated to the control cabinet 5.

[0082] Reference Figures 1 to 5 In one example, each panel P jk (j=1,2,...,n+1,k=1,2,..,m) also includes a first argon gas filling pipeline P jk8a , the second argon gas filling pipeline P jk 8b , exhaust pipe P jk 9 、Tailpipe P jk 10 , Second pneumatic valve P jk 5b 、The third pneumatic valve P jk 5c , the fourth pneumatic valve P jk 5d 、Vacuum generator P jk 11 , Second digital pressure gauge P jk 6b , the first check valve P jk 12a , Second check valve P jk 12b . The first argon gas filling pipeline P jk 8a One end is at the cylinder interface P jk 2 And pressure regulating valve P jk 4 The position between them is connected to the cylinder connecting pipe P jk 3 , the first argon gas filling pipeline P jk 8a The other end of the first check valve P is connected to a first argon gas supply source (not shown). jk 12a Set in the first argon gas filling pipeline P jk 8a , the first check valve P jk 12a The argon gas supplied by the first argon gas supply source is controlled to flow through the first argon gas filling pipe P jk 8a Connect pipe P to cylinder jk 3 One-way flow and prevent cylinder connection pipe P jk 3 The hydrogen sulfide gas in the pump is connected to the first argon gas supply source. jk 9 One end is at the cylinder interface P jk 2 And pressure regulating valve P jk 4 The position between them is connected to the cylinder connecting pipe P jk 3 . Second argon gas filling pipeline P jk 8b One end is connected to the exhaust pipe P jk 9The other end of the second argon gas filling pipe P jk 8b The other end of the second check valve P is connected to a second argon gas supply source (not shown). jk 12b Set in the second argon gas filling pipeline P jk 8b , the second one-way valve P jk 12b The argon gas supplied by the second argon gas supply source is controlled to flow through the second argon gas filling pipe P jk 8b To the exhaust pipe P jk 9 One-way flow and prevent cylinder connection pipe P jk 3 The hydrogen sulfide gas in the second pneumatic valve P is connected to the second argon gas supply source. jk 5b Set in the first argon gas filling pipeline P jk 8a And located in the first argon gas filling pipeline P jk 8a The one end of the first check valve P jk 12a and communicate with the control cabinet 5. The third pneumatic valve P jk 5c Installed in the exhaust pipe P jk 9 And in the exhaust pipe P jk 9 The fourth pneumatic valve P jk 5d Set in the second argon gas filling pipeline P jk 8b And in the second argon gas filling pipe P jk 8b The one end and the second one-way valve P jk 12b and communicate with the control cabinet 5. jk 10 One end is connected to the exhaust pipe P jk 9 The other end and the second argon filling pipe P jk 8b The other end of the tail pipe P jk 10 The other end is used to exhaust the air outwards. jk 11 Installed in the tailpipe P jk 10 , and communicates with the control cabinet 5, the vacuum generator P jk11 Used to connect pipe P to replace cylinder jk 3 The residual hydrogen sulfide gas forms a negative pressure. jk 6b Installed in the tailpipe P jk 10 And located at the vacuum generator P jk 11 and tailpipe P jk 10 The first argon gas supply source and the second argon gas supply source can be independent of each other or integrated into one.

[0083] Further, refer to Fig.13 Combined with Figure 5 , the first pneumatic valve P jk 5a , Second pneumatic valve P jk 5b 、The third pneumatic valve P jk 5c , the fourth pneumatic valve P jk 5d 、Vacuum generator P jk 11 The control cabinet 5 controls each panel P before the gas supply starts. jk (j=1,2,...,n+1,k=1,2,..,m) execute the gas replacement procedure,

[0084] The gas replacement procedure includes the following steps:

[0085] S1, manually close the valve of the cylinder itself, close each panel P jk The first pneumatic valve P of (j=1,2,...,n+1,k=1,2,..,m) jk 5a , Second pneumatic valve P jk 5b 、The third pneumatic valve P jk 5c , the fourth pneumatic valve P jk 5d ,

[0086] S2, control cabinet 5 controls the second pneumatic valve P jk 5b Open, through the first argon filling pipe P jk 8a Fill the cylinder with high purity argon gas and connect the pipe P jk 3 After the first time, control cabinet 5 controls the

[0087] Two pneumatic valves P jk5b closure;

[0088] S3, second pneumatic valve P jk 5b When opening, the control cabinet 5 controls the linkage of the fourth pneumatic valve P jk 5d Open, through the second argon filling pipe P jk 8b Fill the tail gas pipe P with high purity argon jk 10 , control cabinet 5 controls the vacuum generator P jk 11 Generates negative pressure,

[0089] S4, second pneumatic valve P jk 5b While closing, the control cabinet 5 controls the third pneumatic valve P jk 5c Open the second time, in the vacuum generator P jk 11 Under the negative pressure, the residual gas in the cylinder connecting pipe P jk 3 The hydrogen sulfide gas in the jk 9 and tailpipe P jk 10 The exhaust gas is pumped into the exhaust gas treatment system (not shown) for treatment. After the second time, the control cabinet 5 controls the third pneumatic valve P jk 5c Close, and complete a panel gas replacement (i.e., complete a panel gas replacement by using the inflation-extraction method);

[0090] S5, repeating steps S2 to S4 to complete the specified number of panel gas replacements. Note that in the repeated step S3, the control cabinet 5 does not need to control the linkage of the fourth pneumatic valve P jk 5d Open, that is, the fourth pneumatic valve P during the first panel gas replacement to the last panel gas replacement process jk 5d It is always open;

[0091] S6, when the last panel gas replacement is completed, the third pneumatic valve P jk 5c Close and simultaneously link the fourth pneumatic valve P jk 5d Close and complete the gas replacement procedure.

[0092] Through the first pneumatic valve P jk 5a , Second pneumatic valve P jk 5b 、The third pneumatic valve Pjk 5c , the fourth pneumatic valve P jk 5d 、Vacuum generator P jk 11 The communication between the control cabinet 5 and the execution of steps S1 to S6 realizes the jk (j=1,2,...,n+1,k=1,2,..,m) Automatically replace gas before gas supply starts to avoid hydrogen sulfide gas leakage, personnel poisoning, reduce manual operation, and avoid adverse consequences caused by manual operation errors.

[0093] Specifically, in one example, the purity of the high-purity argon gas in step S2 and step S3 is not less than 5N; in step S2, the pressure of the high-purity argon gas is 2-10 kg / cm 2 , the first time is 3-15s; in step S3, the pressure of high-purity argon gas is 3-15kg / cm 2 , vacuum generator P jk 11 The negative pressure generated is 2-5kg / cm 2 ; In step S4, the second time is 5-10s; in step S5, the number of panel gas replacements is 20-100 times.

[0094] Note that all panel groups G j All panels P (j=1,2,...,n+1) jk (j=1,2,...,n+1,k=1,2,..,m) hydrogen sulfide cylinder P jk 1 The total weight of the liquefied hydrogen sulfide filled meets the identification basis of major hazardous sources in the unit inventory. Based on this and all panel groups G j The number of (j=1, 2, ..., n+1) and each panel group G j (j=1,2,...,n+1) panel P jk (j=1,2,...,n+1,k=1,2,..,m),determine the total number of panels P jk (j=1,2,...,n+1,k=1,2,..,m) hydrogen sulfide cylinder P jk 1 The quantity of hydrogen sulfide before the gas supply begins. Figures 8 to 11 In one example, n=5, m=2. That is, the basic cylinder module 1 includes five panel groups G1, G2, G3, G4, and G5, the spare cylinder module 2 includes one panel group G6, and the six panel groups G1, G2, G3, G4, G5, and G6 each include two panels.

[0095] Reference Figure 1 and Figure 8 as well as Figure 6 and Figure 7 In one example, the hydrogen sulfide automatic gas supply device 1000 further includes a first cylinder cabinet 6', a second cylinder cabinet 6", and a spare cylinder cabinet 6''. The n panel groups G of the basic cylinder module 1 i (i=1,2,...,n) are divided into the first cylinder cabinet 6' and the second cylinder cabinet 6", and each panel group G of the basic cylinder module 1 i One of the panels P i1 In the first cylinder cabinet 6', each panel group G of the basic cylinder module 1 i Another panel in P i2 In the second cylinder cabinet 6", the panel group G of the spare cylinder module 2 n+1 Each of the first cylinder cabinet 6', the second cylinder cabinet 6' and the spare cylinder cabinet 6'' includes a cabinet body 61, a porous ventilation plate 62 and a support frame 63. The cabinet body 61 is a closed space with a cabinet door, and is provided with an air outlet 61a at the top and an air return port 61b at the bottom. The porous ventilation plate 62 is arranged above the bottom of the cabinet body 61. The support frame 63 is arranged above the porous ventilation plate 62, and the support frame 63 is provided with corresponding and supporting panels P jk (j=1,2,...,n+1,k=1,2,..,m) hydrogen sulfide cylinder P jk 1 The hydrogen sulfide automatic gas supply device 1000 further includes a first air duct 7' and a second air duct 7", wherein the first air duct 7' connects the air outlet 61a of the three cabinets 61 and the explosion-proof heating fan 3, and the second air duct 7" connects the return air outlet 61b of the three cabinets 61 and the explosion-proof heating fan 3. Figure 1 , the aforementioned explosion-proof electronic scale P jk 7 Located on the corresponding support beam 631 of the support frame 63 .

[0096] In addition, in one example, the hydrogen sulfide automatic gas supply device 1000 further includes a plurality of digital display thermometers (not shown), and the return air outlet 61b of each cabinet 61 is provided with a corresponding digital display thermometer, which is used to monitor the temperature at the return air outlet 61b of the corresponding cabinet 61 and is connected to the control cabinet 5 for communication, and the digital display thermometer and the explosion-proof heating fan 3 are linked under the control of the control cabinet 5. Specifically, refer to Fig.14 When the temperature at the return air outlet 61b of each cabinet 61 is lower than the target temperature, the control cabinet 5 controls the explosion-proof heating fan 3 to turn on. When the temperature at the return air outlet 61b is higher than the target temperature, the control cabinet controls the explosion-proof heating fan 3 to turn off. The working procedure of the explosion-proof heating fan 3 is the same as that of the panel group G. j (j=1,2,...,n+1) Gas supply program linkage, when panel group Gi (j=1,2,...,n+1) When the air supply program is started, the working program of the explosion-proof heating fan 3 is started at the same time. For example, the working temperature of the explosion-proof heating fan 3 is 15-50℃; the target temperature is 15-50℃.

[0097] [application]

[0098] When applied to deposition chamber 2000, there are a total of 12 hydrogen sulfide cylinders, 6 panel groups, 2 hydrogen sulfide cylinders in each panel group, and the net weight of each hydrogen sulfide cylinder is 10-30kg. Among them, the 10 hydrogen sulfide cylinders of the basic cylinder module 1 weigh a total of 100-300kg, and the 2 hydrogen sulfide cylinders of the spare cylinder module 2 weigh a total of 20-60kg; the working temperature of the explosion-proof heating fan 3 is 15-50℃, and the hydrogen sulfide gas pressure in the hydrogen sulfide cylinder is 1.5-3.5MPa; when the deposition chamber 2000 is produced, the set flow rate of hydrogen sulfide is 2-6L / min, and the gas supply time of the basic cylinder module 1 and the spare cylinder module 2 is 15-70 days.

[0099] Application Example 1

[0100] Hydrogen sulfide automatic gas supply device 1000 uses Figures 1 to 7 Configuration and n = 5, m = 2 (corresponding to Figures 8 to 11 )as well as Fig.12 Gas supply procedures, Fig.13 and the gas replacement procedure of the aforementioned steps S1 to S6 and Fig.14 Explosion-proof heating fan working procedures;

[0101] Before the first gas supply cycle begins, the five panel groups G1, G2, G3, G4, G5 of the basic cylinder module 1 and the panel group G6 of the spare cylinder module 2 are jk (j=1,2,3,4,5,k=1,2) hydrogen sulfide cylinder P jk 1 The net weight of hydrogen sulfide is 10kg, the pressure of hydrogen sulfide gas in the bottle is 2.8MPa, and the gas supply pressure of hydrogen sulfide gas is 5kg / cm 2 ;

[0102] During the gas supply procedure:

[0103] The prescribed weight for condition 1 is 1 kg;

[0104] The specified air supply pressure of condition 2 is 6kg / cm 2 ;

[0105] The prescribed time for condition 3 is 1h;

[0106] The switching delay time between panel groups G1, G2, G3, G4, G5, and G6 is 6s;

[0107] During the replacement gas procedure:

[0108] In step S2, the purity of the high-purity argon gas is 5N, and the pressure of the high-purity argon gas is 7kg / cm 2 , the first time is 4s;

[0109] In step S3, the purity of the high-purity argon gas is 5N, and the pressure of the high-purity argon gas is 10kg / cm 2 , vacuum generator P jk 11 The negative pressure generated is 4kg / cm 2 ;

[0110] In step S4, the second time is 8s;

[0111] In step S5, the number of times the panel gas is replaced is 80 times;

[0112] Explosion-proof heating fan working procedure:

[0113] The working temperature of explosion-proof heating fan 3 is 45°C;

[0114] The target temperature is 40°C.

[0115] The flow rate of hydrogen sulfide supplied to the control cabinet 5 was 3 L / min, and the entire duration from the start of gas supply to the end of the CVD growth of the zinc sulfide block was 33 days.

[0116] Application Example 2

[0117] Hydrogen sulfide automatic gas supply device 1000 uses Figures 1 to 7 Configuration and n = 5, m = 2 (corresponding to Figures 8 to 11 )as well as Fig.12 Gas supply procedures, Fig.13 and the gas replacement procedure of the aforementioned steps S1 to S6 and Fig.14 Explosion-proof heating fan working procedures;

[0118] Before the first gas supply cycle begins, the five panel groups G1, G2, G3, G4, G5 of the basic cylinder module 1 and the panel group G6 of the spare cylinder module 2 are jk (j=1,2,3,4,5,k=1,2) hydrogen sulfide cylinder P jk 1 The net weight of hydrogen sulfide is 25kg, the pressure of hydrogen sulfide gas in the bottle is 1.5MPa, and the gas supply pressure of hydrogen sulfide gas is 2kg / cm 2 ;

[0119] During the gas supply procedure:

[0120] The prescribed weight for condition 1 is 5 kg;

[0121] The specified air supply pressure of condition 2 is 4kg / cm 2 ;

[0122] The prescribed time for condition 3 is 5h;

[0123] The switching delay time between panel groups G1, G2, G3, G4, G5, and G6 is 10s;

[0124] During the replacement gas procedure:

[0125] In step S2, the purity of the high-purity argon gas is 5N, and the pressure of the high-purity argon gas is 5kg / cm 2 , the first time is 10s;

[0126] In step S3, the purity of the high-purity argon gas is 5N, and the pressure of the high-purity argon gas is 6kg / cm 2 , vacuum generator P jk 11 The negative pressure generated is 2.5kg / cm 2 ;

[0127] In step S4, the second time is 6s;

[0128] In step S5, the number of times the panel gas is replaced is 30 times;

[0129] Explosion-proof heating fan working procedure:

[0130] The working temperature of explosion-proof heating fan 3 is 40°C;

[0131] The target temperature is 15°C.

[0132] The flow rate of hydrogen sulfide supplied to the control cabinet 5 was 6 L / min, and the entire duration from the start of gas supply to the end of CVD growth of the zinc sulfide block was 20 days.

[0133] Application Example 3

[0134] Hydrogen sulfide automatic gas supply device 1000 uses Figures 1 to 7 Configuration and n = 5, m = 2 (corresponding to Figures 8 to 11 )as well as Fig.12 Gas supply procedures, Fig.13 and the gas replacement procedure of the aforementioned steps S1 to S6 and Fig.14 Explosion-proof heating fan working procedures;

[0135] Before the first gas supply cycle begins, the five panel groups G1, G2, G3, G4, G5 of the basic cylinder module 1 and the panel group G6 of the spare cylinder module 2 are jk (j=1,2,3,4,5,k=1,2) hydrogen sulfide cylinder P jk1 The net weight of hydrogen sulfide is 20kg, the pressure of hydrogen sulfide gas in the bottle is 1.7MPa, and the gas supply pressure of hydrogen sulfide gas is 3kg / cm 2 ;

[0136] During the gas supply procedure:

[0137] The prescribed weight for condition 1 is 3 kg;

[0138] The specified air supply pressure of condition 2 is 4kg / cm 2 ;

[0139] The prescribed time for condition 3 is 3h;

[0140] The switching delay time between panel groups G1, G2, G3, G4, G5, and G6 is 25s;

[0141] During the replacement gas procedure:

[0142] In step S2, the purity of the high-purity argon gas is 5N, and the pressure of the high-purity argon gas is 6kg / cm 2 , the first time is 8s;

[0143] In step S3, the purity of the high-purity argon gas is 5N, and the pressure of the high-purity argon gas is 7kg / cm 2 , vacuum generator P jk 11 The negative pressure generated is 3kg / cm 2 ;

[0144] In step S4, the second time is 10s;

[0145] In step S5, the number of times the panel gas is replaced is 60 times;

[0146] Explosion-proof heating fan working procedure:

[0147] The working temperature of explosion-proof heating fan 3 is 30°C;

[0148] The target temperature is 20°C.

[0149] The flow rate of hydrogen sulfide supplied to the control cabinet 5 was 2 L / min, and the entire duration from the start of gas supply to the end of the CVD growth of the zinc sulfide block was 48 days.

[0150] The above detailed description is used to describe multiple exemplary embodiments, but this document is not intended to be limited to the explicitly disclosed combinations. Therefore, unless otherwise stated, the various features disclosed herein can be combined together to form multiple additional combinations that are not shown for the sake of simplicity.

Claims

1. A hydrogen sulfide automatic gas supply device, suitable for supplying hydrogen sulfide gas to CVD growth of zinc sulfide blocks, characterized in that: The hydrogen sulfide automatic gas supply device (1000) comprises a basic steel cylinder module (1), a spare steel cylinder module (2), an explosion-proof heating fan (3), a hydrogen sulfide gas supply main line (4), and a control cabinet (5); The basic cylinder module (1) includes n panel groups (G i , i=1,2,...,n), n≥2, The spare cylinder module (2) includes one panel group, which is defined as the n+1th panel group (G n+1 ), Each panel group (G j , j = 1, 2, ..., n + 1) includes m panels (P jk , j represents the panel group number, j = 1, 2, ..., n + 1, k represents the panel number in the corresponding panel group, k = 1, 2, ..., m), m ≥ 2, each panel (P jk ) includes a hydrogen sulfide cylinder (P jk 1 ), hydrogen sulfide cylinder (P jk 1 ) is filled with hydrogen sulfide liquefied gas, each panel group (G j , j = 1, 2, ..., n + 1) is used for the panel group (G j , j=1,2,...,n+1)of all panels (P jk ) At the same time, place the hydrogen sulfide cylinder (P jk 1 ) is supplied to the hydrogen sulfide gas supply main line (4), Explosion-proof heating fans (3) are used to heat all panel groups (G j , j=1,2,...,n+1) of hydrogen sulfide cylinder (P jk 1 ) to carry out heating and temperature control; The control cabinet (5) is connected to the hydrogen sulfide gas supply main line (4) to receive the hydrogen sulfide gas and communicate with and control the basic cylinder module (1), the spare cylinder module (2), and the explosion-proof heating fan (3); n panels of the basic cylinder module (1) (G i , i = 1, 2, ..., n) and the panel group (G n+1 ) is controlled by the control cabinet (5) to: After the hydrogen sulfide gas supply is started, the n panel groups (G i , i=1,2,...,n) from the first panel group (G1) to the nth panel group (G n ) are switched to supply hydrogen sulfide gas in sequence to carry out the first cycle of gas supply, In the first cycle of gas supply to the nth panel group (G n ) gas supply to be switched, according to the n panel groups (G i , i=1,2,...,n) in the first panel group (G1) in this cycle is less than the specified time to determine whether to switch to the n panel groups (G1) of the basic cylinder module (1) for the next cycle. i , i=1,2,...,n) from the first panel group (G1) to the nth panel group (G n ) is switched to hydrogen sulfide gas supply or to the panel group (G n+1 ) gas supply, when the panel group (G n+1 ) When the gas supply is no longer available, switch to the n panel groups (G i , i=1,2,...,n) from the first panel group (G1) to the nth panel group (G n ) are switched in sequence to supply hydrogen sulfide, and so on, until the n panel groups (G i , i = 1, 2, ..., n) and the panel group (G in the spare cylinder module (2) n+1 ) together with the gas supply to complete the CVD growth of zinc sulfide bulk.

2. The automatic hydrogen sulfide gas supply device according to claim 1, characterized in that: Multiple panel groups (G j , j=1,2,...,n) when switching between the panel groups (G j ,j=1,2,...,n) switch, the panel group (G j , j=1,2,...,n) delay closing.

3. The automatic hydrogen sulfide gas supply device according to claim 2, characterized in that: The delay time is 5-30s.

4. The automatic hydrogen sulfide gas supply device according to claim 1, characterized in that: n panels of the basic cylinder module (1) (G i , i=1,2,...,n) from the first panel group (G1) to the nth panel group (G n ) and the panel group (G) in the spare cylinder module (2) in turn. n+1 ) is switched to the n panel groups (G) in the basic cylinder module (1) i , i=1,2,...,n) in the first panel group (G1) is executed when one of the following conditions is met: Condition 1: The corresponding panel group (G j , j=1,2,...,n+1) panels (P jk ) of hydrogen sulfide cylinder (P jk 1 ) has a net weight of hydrogen sulfide less than the prescribed weight; Condition 2: The corresponding panel group (G j , j=1,2,...,n+1) panels (P jk ) of hydrogen sulfide cylinder (P jk 1 ) The gas supply pressure of hydrogen sulfide gas in the container is lower than the prescribed gas supply pressure; The nth panel group (G n ) is supplied to the panel group (G) switched to the spare cylinder module (2) n+1 ) to execute the panel group (G n+1 ) Gas supply is carried out under the following conditions: Condition 3: The gas supply time of the first panel group (G1) of the basic cylinder module (1) in this cycle is less than the specified time.

5. The automatic hydrogen sulfide gas supply device according to claim 4, characterized in that: The specified weight is 1-5kg; The specified air supply pressure is 2-8kg / cm 2 ; The prescribed time is 0.5-6h; Before the first gas cycle begins, the n panels (G i , i = 1, 2, ..., n) and the panel group (G in the spare cylinder module (2) n+1 ) in each panel (P jk ) of hydrogen sulfide cylinder (P jk 1 ) has a net weight of 10-30kg of hydrogen sulfide, a pressure of 1.5-3.5MPa of hydrogen sulfide gas in the bottle, and a gas supply pressure of 1-10kg / cm 2 .

6. The automatic hydrogen sulfide gas supply device according to claim 1, characterized in that: Each panel (P jk , j = 1, 2, ..., n + 1, k = 1, 2, ..., m) also includes a cylinder interface (P jk 2 )、Cylinder connecting pipe (P jk 3 ), pressure regulating valve (P jk 4 )、The first pneumatic valve (P jk 5a )、The first digital pressure gauge (P jk 6a ), explosion-proof electronic scale (P jk 7 ), Each panel (P jk , j=1,2,...,n+1,k=1,2,..,m) of hydrogen sulfide cylinder (P jk 1 ) has a valve that can be opened and closed manually. The valve is located in the hydrogen sulfide cylinder (P jk 1 ) of the bottle body and the cylinder interface (P jk 2 ), at the beginning of the first cycle of air supply, each panel (P jk , j=1,2,...,n+1,k=1,2,..,m) of hydrogen sulfide cylinder (P jk 1 ) to manually open the valve on the basic cylinder module (1) panel group (G i , i = 1, 2, ..., n) and the panel group (G in the spare cylinder module (2) n+1 ) together to complete the CVD growth of zinc sulfide blocks, each panel (P jk , j=1,2,...,n+1,k=1,2,..,m) of hydrogen sulfide cylinder (P jk 1 ) The valve itself is manually closed; Cylinder interface (P jk 2 ) is connected to the cylinder connection pipe (P jk 3 ) at one end; Cylinder connecting pipe (P jk 3 ) is connected to the hydrogen sulfide gas supply main line (4); Pressure regulating valve (P jk 4 ) is set on the cylinder connecting pipe (P jk 3 ) on the pressure regulating valve (P jk 4 ) is connected to the control cabinet (5) for communication, and the pressure regulating valve (P jk 4 ) is used to adjust the cylinder port (P jk 2 ) and cylinder connecting pipe (P jk 3 ) from hydrogen sulfide cylinders (P jk 1 ) gas supply pressure of hydrogen sulfide gas formed by vaporizing liquefied hydrogen sulfide; The first pneumatic valve (P jk 5a ) is set on the cylinder connecting pipe (P jk 3 ) and is on the pressure regulating valve (P jk 4 ) downstream, the first pneumatic valve (P jk 5a ) is connected to the control cabinet (5) for communication, and the first pneumatic valve (P jk 5a) is used to open and close the cylinder connected to the pipeline (P) under the control of the control cabinet (5) jk 3 ) is connected and disconnected with the hydrogen sulfide gas supply main line (4); The first digital pressure gauge (P jk 6a ) at the cylinder interface (P jk 2 ) and pressure regulating valve (P jk 4 ) is connected to the cylinder connecting pipe (P jk 3 ), the first digital pressure gauge (P jk 6a ) is connected to the control cabinet (5) for communication, and the first digital pressure gauge (P jk 6a ) is used to detect gas from the cylinder interface (P jk 2 ) and cylinder connecting pipe (P jk 3 ) from hydrogen sulfide cylinders (P jk 1 ) of liquefied hydrogen sulfide vaporizes to form hydrogen sulfide gas in the pressure regulating valve (P jk 4 )Previous pressure; Explosion-proof electronic scale (P jk 7 ) is used to monitor hydrogen sulfide cylinders (P jk 1 ) and is connected to the control cabinet (5) for communication.

7. The automatic hydrogen sulfide gas supply device according to claim 6, characterized in that: Each panel (P jk , j=1,2,...,n+1,k=1,2,..,m) pressure regulating valve (P jk 4 )、The first pneumatic valve (P jk 5a )、The first digital pressure gauge (P jk 6a ), explosion-proof electronic scale (P jk 7 ) is controlled to: In each panel (P jk , j = 1, 2, ..., n + 1, k = 1, 2, ..., m) is executed to supply air, the control cabinet (5) controls the first pneumatic valve (P jk 5a ) is opened, and the control cabinet (5) controls the pressure regulating valve (P jk 4 ) to adjust the hydrogen sulfide cylinder (P jk 1 ) through the cylinder port (P jk 2 ) and cylinder connecting pipe (P jk 3 ) is supplied to the hydrogen sulfide gas supply main line (4), the first digital pressure gauge (P jk 6a ) displays the gas supply pressure and communicates it to the control cabinet (5), the explosion-proof electronic scale (P jk 7 ) Real-time monitoring of hydrogen sulfide cylinders (P jk 1 ) and communicates it to the control cabinet (5).

8. The automatic hydrogen sulfide gas supply device according to claim 6, characterized in that: Each panel (P jk , j = 1, 2, ..., n + 1, k = 1, 2, ..., m) also includes a first argon gas filling pipeline (P jk 8a )、Second argon gas filling pipeline (P jk 8b )、Exhaust pipe (P jk 9 )、Tailpipe(P jk 10 )、Second pneumatic valve (P jk 5b )、The third pneumatic valve (P jk 5c )、The fourth pneumatic valve (P jk 5d )、Vacuum generator(P jk 11 )、Second digital pressure gauge (P jk 6b ), the first one-way valve (P jk 12a ), the second one-way valve (P jk 12b ); The first argon filling pipe (P jk 8a ) at the cylinder interface (P jk 2 ) and pressure regulating valve (P jk 4 ) is connected to the cylinder connecting pipe (P jk 3 ), the first argon gas filling pipeline (P jk 8a ) is connected to a first argon gas supply source; The first check valve (P jk 12a ) is arranged in the first argon gas filling pipeline (P jk 8a ), the first check valve (P jk 12a ) is used to control the argon gas supplied by the first argon gas supply source through the first argon gas filling pipeline (P jk 8a ) Connect the pipe to the cylinder (P jk 3 ) unidirectional flow and prevent the cylinder connection pipe (P jk 3 ) is connected to a first argon gas supply source; Air extraction pipe (P jk 9 ) at the cylinder interface (P jk 2 ) and pressure regulating valve (P jk 4 ) is connected to the cylinder connecting pipe (P jk 3 ); The second argon filling pipe (P jk 8b ) is connected to the exhaust pipe (P jk 9 ) at the other end, the second argon gas filling pipe (P jk 8b ) is connected to a second argon gas supply source; The second check valve (P jk 12b ) is arranged in the second argon gas filling pipeline (P jk 8b ), the second check valve (P jk 12b ) is used to control the argon gas supplied by the second argon gas supply source through the second argon gas filling pipeline (P jk 8b ) to the exhaust pipe (P jk 9 ) unidirectional flow and prevent the cylinder connection pipe (P jk 3 ) is connected to a second argon gas supply source; The second pneumatic valve (P jk 5b ) is arranged in the first argon gas filling pipeline (P jk 8a ) and located in the first argon gas filling pipeline (P jk 8a ) and the first one-way valve (P jk 12a ) and is connected to the control cabinet (5) for communication; The third pneumatic valve (P jk 5c ) is installed in the exhaust pipe (P jk 9 ) and in the exhaust pipe (P jk 9 ) between the two ends and communicated with the control cabinet (5); The fourth pneumatic valve (P jk 5d ) is arranged in the second argon gas filling pipeline (P jk 8b ) and in the second argon filling pipe (P jk 8b ) and a second one-way valve (P jk 12b ) and is connected to the control cabinet (5) for communication; Tail pipe (P jk 10 ) is connected to the exhaust pipe (P jk 9 ) and a second argon gas filling pipe (P jk 8b ) of the other end, the tailpipe (P jk 10 ) is used for exhausting air to the outside; Vacuum generator (P jk 11 ) is installed in the tailpipe (P jk 10 ), and is connected to the control cabinet (5) for communication, the vacuum generator (P jk 11 ) is used to connect the pipe to the replacement cylinder (P jk 3 ) forms a negative pressure when the residual hydrogen sulfide gas is removed; The second digital pressure gauge (P jk 6b ) is installed in the tailpipe (P jk 10 ) and is located in the vacuum generator (P jk 11 ) and tailpipe (P jk 10 ) and is communicatively connected with the control cabinet (5).

9. The automatic hydrogen sulfide gas supply device according to claim 8, characterized in that: The first pneumatic valve (P jk 5a )、Second pneumatic valve (P jk 5b )、The third pneumatic valve (P jk 5c )、The fourth pneumatic valve (P jk 5d )、Vacuum generator(P jk 11 ) is controlled by the control cabinet (5) so that before the gas supply starts, each panel (P jk , j=1,2,...,n+1,k=1,2,..,m) execute the gas replacement procedure, The gas replacement procedure includes the following steps: S1, manually close the valve of the cylinder and close all panels (P jk , j=1,2,...,n+1, k=1,2,..,m) of the first pneumatic valve (P jk 5a )、Second pneumatic valve (P jk 5b )、The third pneumatic valve (P jk 5c )、The fourth pneumatic valve (P jk 5d ), S2, control cabinet (5) controls the second pneumatic valve (P jk 5b ) is opened, and the first argon gas filling pipeline (P jk 8a ) Fill the cylinder with high purity argon gas and connect it to the pipe (P jk 3 ), after the first time, the control cabinet (5) controls the second pneumatic valve (P jk 5b )closure; S3, second pneumatic valve (P jk 5b ) is opened, and the control cabinet (5) controls the linkage fourth pneumatic valve (P jk 5d ) is opened, and the second argon filling pipe (P jk 8b ) Fill the tail gas pipe with high purity argon (P jk 10 ), the control cabinet (5) controls the vacuum generator (P jk 11 ) produces negative pressure, S4, second pneumatic valve (P jk 5b ) is closed while the control cabinet (5) controls the third pneumatic valve (P jk 5c ) Open the second time, in the vacuum generator (P jk 11 ) under the negative pressure, the residual in the cylinder connecting pipe (P jk 3 ) through the exhaust pipe (P jk 9 ) and tailpipe (P jk 10 ) is pumped into the exhaust gas treatment system for treatment. After the second time, the control cabinet (5) controls the third pneumatic valve (P jk 5c ) is closed, completing a panel gas replacement; S5, repeating steps S2 to S4 to complete the panel gas replacement for a specified number of times; S6, when the last panel gas replacement is completed, the third pneumatic valve (P jk 5c ) is closed and the fourth pneumatic valve (P jk 5d ) is closed to complete the gas replacement procedure.

10. The automatic hydrogen sulfide gas supply device according to claim 9, characterized in that: The purity of the high-purity argon gas in step S2 and step S3 is not less than 5N; In step S2, the pressure of high-purity argon gas is 2-10 kg / cm 2 , the first time is 3-15s; In step S3, the pressure of high-purity argon gas is 3-15 kg / cm 2 , vacuum generator (P jk 11 ) The negative pressure generated is 2-5kg / cm 2 ; In step S4, the second time is 5-10s; In step S5, the panel gas is replaced 20-100 times.

11. The automatic hydrogen sulfide gas supply device according to claim 1, characterized in that: All panel groups (G j , j=1,2,...,n+1)of all panels (P jk , j=1,2,...,n+1,k=1,2,..,m) of hydrogen sulfide cylinder (P jk 1 ) The total weight of the liquefied hydrogen sulfide filled meets the basis for identifying major hazardous sources within the unit inventory.

12. The automatic hydrogen sulfide gas supply device according to claim 1, characterized in that: n=5, m=2.

13. The automatic hydrogen sulfide gas supply device according to claim 12, characterized in that: The hydrogen sulfide automatic gas supply device (1000) further comprises a first steel cylinder cabinet (6'), a second steel cylinder cabinet (6") and a spare steel cylinder cabinet (6'"); n panels of the basic cylinder module (1) (G i , i = 1, 2, ..., n) are divided into the first cylinder cabinet (6') and the second cylinder cabinet (6"), and each panel group (G i ) in a panel (P i1 ) In the first cylinder cabinet (6'), each panel group (G i ) in another panel (P i2 ) in the second cylinder cabinet (6”), Panel assembly for spare cylinder module (2) (G n+1 ) into the spare cylinder cabinet (6”); Each of the first steel cylinder cabinet (6'), the second steel cylinder cabinet (6") and the spare steel cylinder cabinet (6'") comprises a cabinet body (61), a porous ventilation plate (62) and a support frame (63); The cabinet body (61) is a closed space with a cabinet door, and is provided with an air outlet (61a) at the top and an air return outlet (61b) at the bottom; A porous ventilation plate (62) is arranged above the bottom of the cabinet (61); The support frame (63) is arranged above the porous ventilation plate (62), and the support frame (63) is provided with a corresponding panel (P jk , j=1,2,...,n+1,k=1,2,..,m) of hydrogen sulfide cylinder (P jk 1 ) of a plurality of support beams (631); The hydrogen sulfide automatic gas supply device (1000) further comprises a first air duct (7') and a second air duct (7"). The first air duct (7') connects the air outlets (61a) of the three cabinets (61) and the explosion-proof heating fan (3). The second air duct (7") connects the return air ports (61b) of the three cabinets (61) and the explosion-proof heating fan (3).

14. The automatic hydrogen sulfide gas supply device according to claim 13, characterized in that: The hydrogen sulfide automatic gas supply device (1000) also includes a plurality of digital temperature gauges. The return air outlet (61b) of each cabinet (61) is provided with a corresponding digital temperature meter, which is used to monitor the temperature at the return air outlet (61b) of the corresponding cabinet (61) and is connected to the control cabinet (5) for communication. The digital temperature meter and the explosion-proof heating fan (3) are linked under the control of the control cabinet (5).

15. The automatic hydrogen sulfide gas supply device according to claim 14, characterized in that: When the temperature at the return air outlet (61b) of each cabinet (61) is lower than the target temperature, the control cabinet (5) controls the explosion-proof heating fan (3) to turn on; when the temperature at the return air outlet (61b) is higher than the target temperature, the control cabinet controls the explosion-proof heating fan (3) to turn off. Explosion-proof heating fan (3) working procedures and panel group (G j , j=1,2,...,n+1) gas supply program linkage, when the panel group (G i , j=1,2,...,n+1) When the air supply program is started, the working program of the explosion-proof heating fan (3) is started at the same time.

16. The automatic hydrogen sulfide gas supply device according to claim 15, characterized in that: The working temperature of the explosion-proof heating fan (3) is 15-50°C; The target temperature is 15-50°C.

17. The automatic hydrogen sulfide gas supply device according to claim 13, characterized in that: Each panel (P jk ) also includes explosion-proof electronic scales (P jk 7 ), explosion-proof electronic scale (P jk 7 ) is used to monitor hydrogen sulfide cylinders (P jk 1 ) and is located on the corresponding support beam (631) of the support frame (63).

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