A device for comprehensive recovery of waste from synthesis of gallium arsenide polycrystal by vacuum method

Abstract

A kind of equipment for comprehensive recovery of waste in synthesis of gallium arsenide polycrystal by vacuum method, relating to gallium arsenide waste recovery device field, including vacuum pressure decomposition device, arsenic recovery device and gallium recovery device;Vacuum pressure decomposition device includes vacuum decomposition furnace, one end of vacuum decomposition furnace is high-temperature end, the other end is low-temperature end, arsenic recovery device includes arsenic collection tank and vacuum pump, arsenic collection tank is communicated with vacuum pump, the upper portion of arsenic collection tank is communicated with the low-temperature end of vacuum decomposition furnace by pipeline, arsenic collection tank is provided with vertically placed collection net, arsenic collection box is arranged below arsenic collection tank;Gallium recovery device includes gallium liquid cooling filter, wash gallium tank, grading overflow tank and gallium liquid collection tank.The present application aims to automatically process gallium arsenide waste, reduce personnel contact, automatic feeding, arsenic gallium automatic separation, after separation, automatic purification treatment is carried out, product purity is at least 5N or more, remaining tailings can be recycled, basically realize zero emission.

Description

TECHNICAL FIELD

[0001] The present application belongs to the field of gallium arsenide waste recovery device, and particularly relates to a device for comprehensively recovering waste from gallium arsenide polycrystal synthesis by vacuum method. BACKGROUND

[0002] During gallium arsenide polycrystal synthesis by HB / VB / VGF method, a large amount of gallium arsenide waste is inevitably produced during single crystal growth. The waste contains a large amount of gallium and arsenic and has great utilization value. However, the waste is contaminated to some extent during the previous use and does not meet the requirements of gallium arsenide crystal growth. How to reasonably and efficiently utilize the waste in an environmentally friendly manner is a problem that needs to be solved in the gallium arsenide industry. For example, the elemental mass ratio of gallium arsenide waste is 75:70, that is, the gallium arsenide waste theoretically contains 48.28% of gallium and 51.72% of arsenic. In the actual traditional wet and dry separation method, the highest recovery efficiency of gallium can only reach 42.15% and 41.83%, the recovery efficiency of gallium is not high, and arsenic cannot be recovered and used basically. Moreover, the waste causes great pollution to the environment and has a great impact on the health of operators. SUMMARY

[0003] In order to solve the problem of efficient recovery of arsenic and gallium in gallium arsenide waste, the present application provides a device for comprehensively recovering waste from gallium arsenide polycrystal synthesis by vacuum method. The present application aims to automatically process the gallium arsenide waste throughout the process, reduce personnel contact, automatically feed, automatically separate arsenic and gallium, automatically purify after separation, produce products with a purity of at least 5N, and recycle the remaining tailings, basically achieving zero emission.

[0004] The technical scheme provided by the present application is as follows: a device for comprehensively recovering waste from gallium arsenide polycrystal synthesis by vacuum method, comprising a vacuum pressure decomposition device, an arsenic recovery device and a gallium recovery device; the vacuum pressure decomposition device comprises a vacuum decomposition furnace, one end of the vacuum decomposition furnace is a high-temperature end, the other end is a low-temperature end, a feeding port is arranged above the high-temperature end, a gallium liquid collector is arranged below the high-temperature end, and a nitrogen gas inlet pipeline is arranged above the low-temperature end; the arsenic recovery device comprises a arsenic collection tank and a vacuum pump, the arsenic collection tank is communicated with the vacuum pump, the upper part of the arsenic collection tank is communicated with the low-temperature end of the vacuum decomposition furnace through a pipeline, the arsenic collection tank is provided with a vertically placed collection net, and an arsenic collection box is arranged below the arsenic collection tank; the gallium recovery device comprises a gallium liquid cooling filter, a gallium washing tank, a grading overflow tank and a gallium liquid collection tank, the gallium liquid cooling filter is located below the gallium liquid collector, the inlet of the gallium liquid cooling filter is communicated with the outlet of the gallium liquid collector through a pipeline, the gallium washing tank is located below the gallium liquid cooling filter, the gallium washing tank is connected with the outlet of the gallium liquid cooling filter through a pipeline, a stirrer is arranged in the gallium washing tank, the grading overflow tank is located below the gallium washing tank, the liquid outlet of the gallium washing tank flows into the grading overflow tank, and the outlet of the grading overflow tank is communicated with the gallium liquid collection tank through a pipeline.

[0005] Further, the equipment for comprehensively recycling waste of gallium arsenide polycrystal synthesis by vacuum method further comprises an automatic control system, the automatic control system comprises a controller, a solenoid valve A on a connecting pipeline between a feeding port and the vacuum decomposition furnace, a vacuum gauge A, a solenoid valve B and a flow sensor A on a nitrogen inlet pipeline, a gravity sensor at the lower end of the gallium liquid collector, a solenoid valve C on a connecting pipeline between the arsenic collection tank and the low-temperature end of the vacuum decomposition furnace, a vacuum gauge B, a solenoid valve D and a flow sensor B on a connecting pipeline between the arsenic collection tank and the vacuum pump, and a solenoid valve E at the lower end of the gallium washing tank; the vacuum gauge, the flow sensor and the gravity sensor transmit detection signals to the input end of the controller, and the controller sends corresponding instructions to each solenoid valve through the output end, so that automatic control is realized.

[0006] Further, the gallium liquid cooling filter comprises a filter box body, a filtering step is arranged in the filter box body, a vertical filtering plate is arranged at the external corner of each filtering step, the height of the upper end face of the filtering partition plate gradually decreases along the direction of the lower step, the filtering step and the filtering plate are both hollow double-layer plate structures, the hollow cavities of the filtering step and the filtering plate are communicated, a cooling liquid inlet is arranged outside the filter box body and is communicated with the upper end of each filtering plate, and a cooling liquid outlet is arranged at the lower part of the filter box body.

[0007] Further, a vertical partition plate is arranged in the grading overflow tank, the grading overflow tank is divided into two tanks by the partition plate, a drainage port is communicated with the bottom of one tank, and a gallium liquid discharge port is communicated with the bottom of the other tank.

[0008] Further, a three-stage filtering purifier is arranged at the rear end of the vacuum pump.

[0009] Further, the equipment for comprehensively recycling waste of gallium arsenide polycrystal synthesis by vacuum method further comprises a sound wave vibrator, the sound wave vibrator is connected with the collection net, so that the arsenic on the collection net is shaken off through sound wave vibration.

[0010] The beneficial effects of the present application are as follows:

[0011] 1. The present application can adjust the temperature and vacuum degree of the decomposition furnace at any time, so that the decomposition efficiency is ensured, the arsenic after decomposition is collected through the collection net, the gallium liquid after decomposition is cooled and filtered through the cooling and filtering device, the step plays a role of cooling and preliminary purification, the gallium liquid after preliminary purification is further washed through the gallium washing tank, and then the water and the gallium liquid are separated through the grading overflow tank, so that the effect of high recovery is achieved.

[0012] 2. The automatic control system in the application plays the role of automatic feeding, automatic temperature measurement and automatic discharging, so as to reduce the labor participation, labor intensity and labor cost as much as possible in the whole process.

[0013] 3. The recovered arsenic and gallium have higher purity, so that the waste material can be fully reused.

[0014] 4. The filtering steps and filtering plates in the cooling filter in the application play the role of cooling and filtering, and achieve double functions through the most simplified design. BRIEF DESCRIPTION OF DRAWINGS

[0015] Figure 1 is the structural schematic diagram of the whole application.

[0016] Figure 2 is the structural schematic diagram of the vacuum decomposition device in the application.

[0017] Figure 3 is the structural schematic diagram of the arsenic recovery device in the application.

[0018] Figure 4 is the structural schematic diagram of the gallium recovery device in the application.

[0019] In the figure: 1, feeding port; 2, electromagnetic valve A; 3, vacuum decomposition furnace; 4, high-temperature end; 5, flow sensor A; 6, nitrogen inlet pipeline; 7, electromagnetic valve B; 8, vacuum gauge A; 9, low-temperature end; 10, gallium liquid collector; 11, gravity sensor; 12, electromagnetic valve C; 13, collection net; 14, arsenic collection tank; 15, vacuum gauge B; 16, electromagnetic valve D; 17, flow sensor B; 18, vacuum pump; 19, exhaust port; 20, three-stage filtering purifier; 21, arsenic collection box; 22, filter box; 23, filtering step; 24, filtering plate; 25, cooling liquid inlet; 26, cooling liquid outlet; 27, stirrer; 28, gallium washing tank; 29, electromagnetic valve E; 30, grading overflow tank; 31, partition plate; 32, gallium liquid discharge port; 33, gallium liquid collection tank; 34, water discharge port. DETAILED DESCRIPTION

[0020] The technical solutions in the embodiments of the application will be described clearly and completely below with reference to the drawings in the embodiments of the application. Obviously, the described embodiments are only part of the embodiments of the application, rather than all the embodiments of the application. Based on the embodiments in the application, all other embodiments obtained by those skilled in the art without creative work fall within the protection scope of the application.

[0021] As Figure 1As shown, the embodiment includes a vacuum pressure decomposition device, an arsenic recovery device, and a gallium recovery device. The present application is a technical system type invention, and multiple systems are connected and coordinated with each other.

[0022] Figure 2 The vacuum pressure decomposition device is provided with a vacuum decomposition furnace 3, which is the most core component of the vacuum pressure decomposition device. One end of the vacuum decomposition furnace 3 is a high-temperature end 4, and the other end is a low-temperature end 9. The high-temperature end 4 is controlled in temperature by an adjustable temperature electric heating device to ensure the decomposition efficiency, and the arsenic sublimation enters the low-temperature section. An adding port 1 is arranged above the high-temperature end 4, and the automatic feeding is controlled by an electromagnetic valve A2. A gallium liquid collector 10 is arranged below the high-temperature end 4, and the melted gallium liquid and impurities enter the gallium liquid collector 10. A nitrogen gas inlet pipeline 6 is arranged above the low-temperature end 9. The electromagnetic valve B7 can be automatically opened or closed to adjust the gas inlet amount under the condition that the vacuum degree and time reach a certain value, so that the arsenic will not condense at the furnace opening of the low-temperature end 9 under the action of the nitrogen gas.

[0023] Figure 3 The arsenic recovery device is provided with a collection tank 14 and a vacuum pump 18, which are the core components of the arsenic recovery device. The collection tank 14 is communicated with the vacuum pump 18, and the upper part of the collection tank 14 is communicated with the low-temperature end 9 of the vacuum decomposition furnace 3 through a pipeline, so that the sublimated arsenic enters the collection tank 14 from the vacuum decomposition furnace 3. The collection tank 14 is provided with a vertically placed collection net 13, and the arsenic condenses into flocculent solid on the collection net 13 in the collection tank 14. The collection net 13 can be vibrated at high frequency by a sound wave vibrator, so that the arsenic is shaken off to the lower arsenic collection box 21. The arsenic collection box 21 is provided with a gravity sensing device, and when the weight reaches a certain value, the electromagnetic valve C12 of the arsenic gas inlet of the collection tank 14 is closed, the vacuum is eliminated, the lower arsenic collection box 21 is opened, and the arsenic falls into the lower arsenic collection box 21. The product is taken away regularly.

[0024] Figure 4The gallium recovery device is provided with a gallium liquid cooling filter, a gallium washing tank 28, a grading overflow tank 30 and a gallium liquid collecting tank 33. The gallium liquid cooling filter is located below the gallium liquid collector 10, and the inlet of the gallium liquid cooling filter is communicated with the outlet of the gallium liquid collector 10 through a pipeline. The gallium liquid cooling filter comprises a filter box 22, and a filtering step 23 is arranged in the filter box 22. A vertical filter plate 24 is arranged at the outer corner of each filtering step 23. The height of the upper end surface of the filtering partition plate decreases in sequence along the direction of the lower step. The filtering step 23 and the filter plate 24 are both hollow double-layer plate structures, and the hollow cavities of the filtering step 23 and the filter plate 24 are communicated. A cooling liquid inlet 25 is arranged outside the filter box 22, and the cooling liquid inlet 25 is communicated with the upper end of each filter plate 24. A cooling liquid outlet 26 is arranged at the lower part of the filter box 22. The low-temperature cooling water enters the upper part of each filter plate 24 from the cooling liquid inlet 25, flows from the filtering step 23 to the cooling liquid outlet 26 to complete the cooling cycle, and the gallium liquid with impurities flows along the filtering step 23 in sequence. The impurities with heavy quality are deposited at the filtering step 23 and separated from the gallium liquid.

[0025] The gallium washing tank 28 is located below the gallium liquid cooling filter device, and the gallium washing tank 28 is connected with the outlet of the gallium liquid cooling filter device through a pipeline. The gallium washing tank 28 is provided with a stirrer 27, which plays a role of fully washing gallium. The grading overflow tank 30 is located below the gallium washing tank 28, and the liquid outlet of the gallium washing tank 28 flows into the grading overflow tank 30. The outlet of the grading overflow tank 30 is communicated with the gallium liquid collecting tank 33 through a pipeline. The grading overflow tank 30 is provided with a vertical partition plate 31, which divides the grading overflow tank 30 into two tanks. One tank is communicated with a water drain 34 at the bottom, and the other tank is communicated with a gallium liquid discharge outlet 32 at the bottom.

[0026] The embodiment also comprises an automatic control system, which comprises a controller, electromagnetic valve A2 on the connecting pipeline between the feeding port 1 and the vacuum decomposition furnace 3, vacuum gauge A8, electromagnetic valve B7 and flow sensor A5 on the nitrogen inlet pipeline 6, gravity sensor 11 at the lower end of the gallium liquid collector 10, electromagnetic valve C12 on the connecting pipeline between the arsenic collecting tank 14 and the low-temperature end 9 of the vacuum decomposition furnace 3, vacuum gauge B15, electromagnetic valve D16 and flow sensor B17 on the connecting pipeline between the arsenic collecting tank 14 and the vacuum pump 18, and electromagnetic valve E29 at the lower end of the gallium washing tank 28. All the vacuum gauges, flow sensors and gravity sensor 11 transmit detection signals to the input end of the controller, and the controller sends corresponding instructions to each electromagnetic valve through the output end, so as to realize automatic feeding, automatic temperature measurement and automatic discharging, reduce manual participation in the whole process, reduce labor intensity and labor cost. The application realizes automatic processing of the gallium arsenide waste material throughout the whole process, reduces personnel contact, realizes automatic feeding, automatic separation of arsenic and gallium, automatic purification treatment after separation, and the purity of the product is at least 5N or above, the remaining tailings can be recycled, and zero emission is basically realized.

[0027] The nitrogen is discharged by the vacuum pump 18, the gas outlet of the vacuum pump 18 is connected with the three-stage filtering purifier 20 (an oil and dust removal tank), and the tail gas content of the exhaust outlet 19 measured meets the national emission standard and can be directly discharged.

[0028] The arsenic and gallium product after decomposition by the application can reach 5N or above through GDMS detection, no excess waste material is produced, the tailings of insufficient decomposition do not need to be treated, will continue to be decomposed after automatic feeding, and will produce very little waste liquid, which can be treated by chemical precipitation and acid-base treatment to meet the emission standard.

Claims

1. A device for the comprehensive recycling of waste from gallium arsenide polycrystalline synthesis using a vacuum method, characterized in that: The application relates to a vacuum pressure decomposition device, an arsenic recovery device and a gallium recovery device; the vacuum pressure decomposition device comprises a vacuum decomposition furnace (3), the vacuum decomposition furnace (3) has a high-temperature end (4) at one end and a low-temperature end (9) at the other end, a feeding opening (1) is arranged above the high-temperature end (4), a gallium liquid collector (10) is arranged below the high-temperature end (4), and a nitrogen gas inlet pipeline (6) is arranged above the low-temperature end (9); the arsenic recovery device comprises an arsenic collecting tank (14) and a vacuum pump (18), the arsenic collecting tank (14) is communicated with the vacuum pump (18), the upper portion of the arsenic collecting tank (14) is communicated with the low-temperature end (9) of the vacuum decomposition furnace (3) through a pipeline, the arsenic collecting tank (14) is provided with a vertically-arranged collecting net (13), and an arsenic collecting box (21) is arranged below the arsenic collecting tank (14); the gallium recovery device comprises a gallium liquid cooling filter, a gallium washing tank (28), a grading overflow tank (30) and a gallium liquid collecting tank (33), the gallium liquid cooling filter is arranged below the gallium liquid collector (10), the inlet of the gallium liquid cooling filter is communicated with the outlet of the gallium liquid collector (10) through a pipeline, the gallium washing tank (28) is arranged below the gallium liquid cooling filter, the gallium washing tank (28) is connected with the outlet of the gallium liquid cooling filter through a pipeline, a stirrer (27) is arranged in the gallium washing tank (28), the grading overflow tank (30) is arranged below the gallium washing tank (28), liquid in the gallium washing tank (28) flows into the grading overflow tank (30), and the outlet of the grading overflow tank (30) is communicated with the gallium liquid collecting tank (33) through a pipeline.

2. The device for comprehensive recovery of waste from synthesis of gallium arsenide polycrystals by vacuum method according to claim 1, characterized in that it comprises: An automatic control system is further arranged, the automatic control system comprises a controller, an electromagnetic valve A (2) arranged on a connecting pipeline between the feeding opening (1) and the vacuum decomposition furnace (3), a vacuum gauge A (8), an electromagnetic valve B (7) and a flow sensor A (5) arranged on the nitrogen gas inlet pipeline (6), a gravity sensor (11) arranged at the lower end of the gallium liquid collector (10), an electromagnetic valve C (12) arranged on a connecting pipeline between the arsenic collecting tank (14) and the low-temperature end (9) of the vacuum decomposition furnace (3), a vacuum gauge B (15), an electromagnetic valve D (16) and a flow sensor B (17) arranged on a connecting pipeline between the arsenic collecting tank (14) and the vacuum pump (18), an electromagnetic valve E (29) arranged at the lower end of the gallium washing tank (28), and all the vacuum gauges, flow sensors and the gravity sensor (11) transmit detection signals to the input end of the controller, corresponding instructions are sent to all the electromagnetic valves through the output end of the controller, so that automatic control is realized.

3. The device for comprehensive recovery of waste from synthesis of gallium arsenide polycrystals by vacuum method according to claim 1, characterized in that it comprises: The gallium liquid cooling filter comprises a filter box (22), a filter step (23) is arranged inside the filter box (22), a vertical filter plate (24) is arranged at the external corner of each filter step (23), the height of the upper end face of the filter partition plate decreases in turn along the direction of the lower step, the filter step (23) and the filter plate (24) are both hollow double-layer plate structures, the hollow cavities of the filter step (23) and the filter plate (24) are communicated, a cooling liquid inlet (25) is arranged outside the filter box (22), the cooling liquid inlet (25) is communicated with the upper end of each filter plate (24) respectively, and a cooling liquid outlet (26) is arranged at the lower part of the filter box (22).

4. The apparatus for comprehensive recovery of waste materials from synthesis of gallium arsenide polycrystals by vacuum method according to claim 3, characterized in that: The grading overflow tank (30) is provided with a vertical partition plate (31), the grading overflow tank (30) is divided into two tanks by the partition plate (31), one tank is communicated with a water drainage port (34) at the bottom, and the other tank is communicated with a gallium liquid discharge port (32) at the bottom.

5. The apparatus for comprehensive recovery of waste materials from synthesis of gallium arsenide polycrystals by vacuum method according to claim 1, characterized in that it comprises: The rear end of the vacuum pump (18) is provided with a three-stage filter purifier (20).

6. The apparatus for comprehensive recovery of waste materials from synthesis of gallium arsenide polycrystals by vacuum method according to claim 1, characterized in that it comprises: Further comprising a sound wave vibrator, the sound wave vibrator is connected with the collecting net (13), so that the arsenic on the collecting net (13) is shaken off through sound wave vibration.

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