Method and device for preparing gallium phosphide and recovering indium from indium phosphide waste
By using graphite open containers for replacement reaction under vacuum, the indium and phosphorus in the indium phosphide waste are recovered into high-purity gallium phosphide, which solves the problems of difficulty and risk in the prior art, and achieves efficient and environmentally friendly waste conversion.
Patent Information
- Application Number
- CN202411856256.2
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-12-17
- Publication Date
- 2025-03-25
- Estimated Expiration
- 2044-12-17
AI Technical Summary
The prior art is difficult to effectively recover indium and phosphorus in indium phosphide waste, and the vacuum thermal decomposition method has the problem of high difficulty in controlling the phosphorus conversion rate and high risk coefficient.
The replacement reaction was carried out under vacuum using an open graphite container, and the waste indium phosphide was reacted with high purity gallium to collect the obtained indium and gallium phosphide. The method includes performing high temperature decomposition in a first graphite open container to recover indium and reacting with high purity gallium in a second graphite open container to synthesize gallium phosphide.
It realizes efficient recycling of indium and phosphorus in indium phosphide waste and converts it into high-value-added materials. It has simple operation, short process, high efficiency, low cost, and is environmentally friendly, avoiding the risks brought about by spontaneous combustion of yellow phosphorus.
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Figure CN119683580A_ABST
Abstract
Description
Technical Field
[0001] The invention belongs to the technical field of indium phosphide recovery, and in particular relates to a method and a device for preparing gallium phosphide and recovering indium using indium phosphide waste. Background Art
[0002] Indium phosphide (InP) semiconductors are essential components for 5G optical communication systems. In recent years, with the rapid development of telecommunications and optoelectronic technologies, the consumption of InP semiconductors has continued to grow. Due to the low hardness, high brittleness, and easy dissociation of InP, a large amount of waste is generated during the processing, of which about 50% of the waste is generated during the ingot cutting process alone. The overall processing yield is less than 30%, and the amount of waste is increasing day by day.
[0003] At present, the main methods for recycling indium phosphide waste are wet method and vacuum thermal decomposition method. The wet method, such as a method for treating indium phosphide waste by atmospheric pressure oxidation acid leaching process, recovers indium by metal replacement. This method is simple to operate, but it takes a long time and produces harmful waste liquid. The vacuum thermal decomposition method, such as a method for vacuum high-temperature thermal decomposition of indium phosphide in two stages using a tubular furnace, can achieve the recovery and regeneration of indium and phosphorus, but the conversion rate of phosphorus is difficult to control, and most of it is produced as spontaneously combusting yellow phosphorus, which makes recovery difficult and has a high risk factor. Summary of the invention
[0004] The purpose of the present invention is to provide a method and device for preparing gallium phosphide and recovering indium from indium phosphide waste. The method provided by the present invention is simple to operate, short in process, high in efficiency, low in cost, and environmentally friendly, and realizes the recovery of indium and phosphorus in indium phosphide waste, and realizes the conversion of waste into a new generation of high value-added materials.
[0005] In order to achieve the above-mentioned object of the invention, the present invention provides the following technical solutions:
[0006] The present invention provides a method for preparing gallium phosphide and recovering indium using indium phosphide waste, comprising the following steps:
[0007] Providing a graphite open container; the graphite open container comprises a first graphite open container and a second graphite open container arranged on the upper edge of the first graphite open container;
[0008] Indium phosphide waste is loaded into the first open graphite container, and high-purity gallium is loaded into the second open graphite container. A replacement reaction is performed under vacuum conditions, and indium is collected in the first open graphite container, and gallium phosphide is collected in the second open graphite container. The purity of the high-purity gallium is not less than 99.99%. During the replacement reaction, the temperature of the first open graphite container is 900-1100° C., and the temperature of the second open graphite container is 820-1020° C.
[0009] Preferably, the conditions for the replacement reaction include: a holding time of 2 to 4 hours and a pressure of 10 to 30 Pa.
[0010] Preferably, a storage rack is provided in the second open graphite container at an acute angle to the inner wall, the bottom end of the storage rack is connected to the inner wall to form a storage groove with an open top, and the high-purity gallium is loaded into the storage groove of the second open graphite container.
[0011] Preferably, the bottom end of the storage rack is connected to the bottom end of the inner wall.
[0012] Preferably, the acute angle is 30-60°.
[0013] Preferably, the molar ratio of gallium in the high-purity gallium to indium phosphide in the indium phosphide waste is 1:3-4.
[0014] Preferably, the mass fraction of indium in the indium phosphide waste is not less than 75%, and the mass fraction of phosphorus is not less than 15%.
[0015] Preferably, the indium phosphide waste also includes impurities, and the impurities include at least one of calcium, sodium and magnesium; the mass fraction of calcium in the indium phosphide waste is 0.2% to 0.3%, the mass fraction of sodium is 0.05% to 0.06%, and the mass fraction of magnesium is 0.02% to 0.03%.
[0016] The present invention provides a device for preparing gallium phosphide and recovering indium from indium phosphide waste, comprising a vacuum pump, a heating device, a pit furnace, a quartz tube, a graphite open container and an inert gas generator; the vacuum pump and the inert gas generator are respectively connected to the quartz tube; the heating device is used for heating the pit furnace; the quartz tube is inside the pit furnace; the graphite open container is inside the quartz tube; the graphite open container comprises a first graphite open container and a second graphite open container arranged on the upper edge of the first graphite open container.
[0017] Preferably, the device for preparing gallium phosphide and recovering indium using indium phosphide waste also includes a filter, a bellows, a PU pneumatic hose, a rubber stopper and a vacuum gauge; the filter is connected to the vacuum pump and the bellows, and the other end of the bellows is connected to the quartz tube; the PU pneumatic hose is connected to the quartz tube and the inert gas generating device.
[0018] The present invention provides a method for preparing gallium phosphide and recovering indium using indium phosphide waste, comprising the following steps: providing a graphite open container; the graphite open container comprises a first graphite open container and a second graphite open container arranged on the upper edge of the first graphite open container; loading indium phosphide waste into the first graphite open container, loading high-purity gallium into the second graphite open container, performing a substitution reaction under vacuum conditions, collecting indium in the first graphite open container, and collecting gallium phosphide in the second graphite open container; the purity of the high-purity gallium is not less than 99.99%; during the substitution reaction, the temperature of the first graphite open container is 900-1100°C, and the temperature of the second graphite open container is 820-1020°C. The graphite open container of the present invention adopts a raw material separation design, and can discharge materials in layers. The indium phosphide waste is placed in the first open container, and the phosphorus vapor obtained after high-temperature decomposition can volatilize into the second open container and react with high-purity gallium to synthesize high-purity gallium phosphide. At the same time, the temperature of the first graphite open container is controlled within 900-1100°C, and the temperature of the second graphite open container is controlled within 820-1020°C, which can fully realize the decomposition of indium phosphide, promote the combination of phosphorus vapor and gallium to obtain gallium phosphide, and realize the volatilization of impurities in indium phosphide waste, which is conducive to obtaining high-purity indium. The method provided by the present invention is simple to operate, short in process, high in efficiency, low in cost, and environmentally friendly, and realizes the conversion of second-generation indium phosphide semiconductor waste into third-generation gallium phosphide semiconductors, indium and phosphorus can be recovered, and the risk of spontaneous combustion of yellow phosphorus is eliminated.
[0019] Furthermore, the present invention utilizes vacuum technology to promote the replacement reaction, and adopts a matching open graphite container to recover indium and phosphorus in one step by combining vacuum thermal decomposition with vacuum synthesis of indium phosphide waste; at the same time, by utilizing the characteristic of indium phosphide raw materials with few impurities, high-purity gallium phosphide and high-purity indium are directly prepared, and indium phosphide waste is converted into usable materials in one step. BRIEF DESCRIPTION OF THE DRAWINGS
[0020] In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings required for use in the embodiments will be briefly introduced below. Obviously, the drawings described below are only some embodiments of the present invention. For ordinary technicians in this field, other drawings can be obtained based on these drawings without paying creative labor.
[0021] Figure 1 is a schematic diagram of an open graphite container;
[0022] Figure 2 A schematic diagram of a graphite crucible filled with indium phosphide waste and high-purity gallium;
[0023] Figure 3The present invention is a schematic diagram of a device for preparing gallium phosphide and recovering indium from indium phosphide waste, wherein: 1 is a vacuum pump; 2 is a filter; 3 is a bellows; 4 is a thermocouple; 5 is a well furnace; 6 is a quartz tube; 7 is a rubber stopper; 8 is a vacuum gauge; 9 is a graphite crucible; and 10 is an argon generator. DETAILED DESCRIPTION
[0024] The present invention provides a method for preparing gallium phosphide and recovering indium using indium phosphide waste, comprising the following steps:
[0025] Providing a graphite open container; the graphite open container comprises a first graphite open container and a second graphite open container arranged on the upper edge of the first graphite open container;
[0026] Indium phosphide waste is loaded into the first open graphite container, and high-purity gallium is loaded into the second open graphite container. A replacement reaction is performed under vacuum conditions, and indium is collected in the first open graphite container, and gallium phosphide is collected in the second open graphite container. The purity of the high-purity gallium is not less than 99.99%. During the replacement reaction, the temperature of the first open graphite container is 900-1100° C., and the temperature of the second open graphite container is 820-1020° C.
[0027] In the present invention, unless otherwise specified, the raw materials used are commercially available products well known to those skilled in the art or are prepared by methods well known to those skilled in the art.
[0028] In the present invention, the graphite open container includes a first graphite open container and a second graphite open container arranged on the upper edge of the first graphite open container. In the present invention, the inner wall of the second graphite open container may be provided with a storage groove with a top opening, and the high-purity gallium may be loaded into the storage groove of the second graphite open container. In the second graphite open container of the present invention, a storage rack is provided at an acute angle with the inner wall, and the bottom end of the storage rack may be connected with the inner wall to form a storage groove; the longitudinal section of the storage groove may be a triangle. In the present invention, the acute angle formed by the storage rack and the inner wall of the second graphite open container may be 30 to 60°, that is, the bottom angle of the storage groove is 30 to 60°. In a specific embodiment of the present invention, the acute angle formed by the storage rack and the inner wall of the second graphite open container is 45°. In the present invention, the graphite open container may be a graphite crucible, the first graphite open container may be a first graphite crucible, and the second graphite open container may be a second graphite crucible. In a specific embodiment of the present invention, the graphite open container is a cylinder with a height of 80 mm, and the heights of the first graphite crucible and the second graphite crucible are respectively 40 mm; the inner diameter of the graphite crucible is 50 mm, and the inner diameters of the first graphite crucible and the second graphite crucible are the same as the inner diameter of the graphite crucible.
[0029] Figure 1 is a schematic diagram of a graphite crucible, such as Figure 1 As shown, the graphite crucible of the present invention adopts a design of two layers of graphite crucibles stacked together, which is divided into a first graphite crucible and a second graphite crucible arranged on the upper edge of the first graphite crucible. A placing plate is used to form a convex design at the connection between the two crucibles, and the placing plate and the inner wall of the second graphite crucible form a placing groove with a top opening.
[0030] In the present invention, the mass fraction of indium in the indium phosphide waste can be not less than 75%, and the mass fraction of phosphorus can be not less than 15%. The indium phosphide waste of the present invention may also include impurities, and the impurities may include at least one of calcium, sodium and magnesium; the mass fraction of calcium in the indium phosphide waste may be 0.2% to 0.3%, the mass fraction of sodium may be 0.05% to 0.06%, and the mass fraction of magnesium may be 0.02% to 0.03%. In a specific embodiment of the present invention, the indium phosphide waste is a defective product produced during the manufacturing process of a certain indium phosphide single crystal production enterprise in Yunnan, which is disc-shaped and looks like a CD. Through ICP-OES detection, the indium phosphide waste contains the main elements indium, phosphorus, and trace impurity elements such as calcium, sodium and magnesium, wherein the mass fraction of indium is 78.229%, the mass fraction of phosphorus is 18.303%, the mass fraction of calcium is 0.249%, the mass fraction of sodium is 0.059%, and the mass fraction of magnesium is 0.028%. In a specific embodiment of the present invention, the indium phosphide waste can be crushed before use to obtain indium phosphide waste particles, and the particle size of the indium phosphide waste particles is 3 mm.
[0031] In the present invention, the purity of the high-purity gallium is not less than 99.99%; in a specific embodiment of the present invention, the purity of the gallium is 99.999%.
[0032] In the present invention, the molar ratio of gallium in the high-purity gallium to indium phosphide in the indium phosphide waste can be 1:3-4; in a specific embodiment of the present invention, the molar ratio of gallium in the high-purity gallium to indium phosphide in the indium phosphide waste is 1:3, 1:3.5 or 1:4.
[0033] Figure 2 Schematic diagram of a graphite crucible filled with indium phosphide waste and high purity gallium, as shown in Figure 2 As shown, indium phosphide waste is placed in the first graphite crucible, and high-purity gallium is placed in the storage groove at the bottom of the second graphite crucible, so that the phosphorus vapor generated by the thermal decomposition of the indium phosphide waste in the first graphite crucible can volatilize into the second graphite crucible and synthesize with gallium to produce gallium phosphide, which can be collected in the second graphite crucible; the indium generated by the decomposition of indium phosphide is retained in the first graphite crucible; that is, the existence of the storage groove can realize both the layered feeding of raw materials and the separate collection of gallium phosphide and indium.
[0034] The present invention loads the indium phosphide waste into the first graphite open container of the graphite open container, loads the high-purity gallium into the second graphite open container of the graphite open container, and performs a replacement reaction under vacuum conditions. In a specific embodiment of the present invention, after the indium phosphide waste and the high-purity gallium are loaded, the graphite open container containing the materials is placed at the bottom of the quartz tube, and the quartz tube is placed in a pit furnace. The inert gas of the present invention can be argon. Before the replacement reaction, the present invention can pump the pressure inside the quartz tube to the pressure required for the replacement reaction, and then introduce an inert gas into the reaction system to discharge the air in the system. In the present invention, the introduction of the inert gas is to prevent the oxidation of indium and phosphorus and to create a vacuum environment. In a specific embodiment of the present invention, the time for the introduction of the inert gas is 10 minutes. In the present invention, when the replacement reaction is carried out, the temperature of the first graphite open container is 900-1100°C, and the temperature of the second graphite open container is 820-1020°C. In a specific embodiment of the present invention, during the replacement reaction, the temperature of the first graphite open container is 900°C, 950°C, 1000°C, 1050°C or 1100°C, and the temperature of the second graphite open container is 820°C, 870°C, 920°C, 970°C or 1020°C. The conditions of the replacement reaction of the present invention may include: the insulation time may be 2 to 4 hours, the heating rate of heating to the temperature of the first graphite open container or the temperature of the second graphite open container may be 8 to 12°C / min, and the pressure may be 10 to 30Pa; in a specific embodiment of the present invention, the insulation time of the replacement reaction is 2 hours; the heating rate of heating to the temperature of the first graphite open container or the temperature of the second graphite open container is 8°C / min, 10°C / min or 12°C / min; the pressure is 10Pa, 20Pa or 30Pa. After the replacement reaction is completed, the present invention can reduce the obtained reaction materials to room temperature, collect indium in the first open graphite container, and collect gallium phosphide in the second open graphite container. The purity of the indium of the present invention can be no less than 97%, and the direct yield of indium can be no less than 90%; the synthesis rate of gallium phosphide can be no less than 85%, and the purity level can be 4N~4N5. In a specific embodiment of the present invention, the purity of indium is 97.2%, 99.9% or 99.95%; the direct yield of indium is 90%, 98% or 99%; the synthesis rate of gallium phosphide is 85%, 90% or 95%; the purity level of gallium phosphide is 4N or 4N5.
[0035] The present invention controls the temperature of the first graphite open container within 900-1100°C and the temperature of the second graphite open container within 820-1020°C, which can fully realize the decomposition of indium phosphide and promote the combination of phosphorus vapor and gallium to obtain gallium phosphide. The method provided by the present invention is simple to operate, short in process, high in efficiency, low in cost, and environmentally friendly, and realizes the recovery of indium and phosphorus in indium phosphide waste, while eliminating the risk of spontaneous combustion of yellow phosphorus. Moreover, the present invention utilizes vacuum technology to promote the replacement reaction, adopts a matching graphite open container, and recovers indium and phosphorus in one step by combining vacuum thermal decomposition and vacuum synthesis of indium phosphide waste; at the same time, the characteristics of less impurities in indium phosphide raw materials are utilized to directly prepare high-purity gallium phosphide and high-purity indium, and in one step, the indium phosphide waste is converted into usable materials.
[0036] The present invention also provides a device for preparing gallium phosphide and recovering indium from indium phosphide waste, comprising a vacuum pump, a heating device, a pit furnace, a quartz tube, a graphite open container and an inert gas generator. In the present invention, the heating device can be a thermocouple equipped with a temperature control device; the inert gas generator can be an argon generator. In the present invention, the device for preparing gallium phosphide and recovering indium from indium phosphide waste can also include a filter, a bellows, a PU pneumatic hose, a sealing component and a vacuum gauge. The sealing component of the present invention can be a rubber stopper. In the present invention, the filter can be connected to the vacuum pump and the bellows, and the other end of the bellows can be connected to the quartz tube; the PU pneumatic hose can connect the quartz tube and the inert gas generator; the quartz tube is inside the pit furnace; and the graphite open container is inside the quartz tube. The graphite open container of the present invention includes a first graphite open container and a second graphite open container arranged on the upper edge of the first graphite open container. The heating device of the present invention is used to heat the pit furnace, the rubber plug can be used to create a closed environment for the quartz tube; the vacuum gauge can be connected to the rubber plug to measure the pressure inside the quartz tube. In a specific embodiment of the present invention, the graphite open container is a graphite crucible; the device for preparing gallium phosphide and recovering indium from indium phosphide waste includes a vacuum pump, a heating device, a pit furnace, a quartz tube, a graphite crucible and an argon gas generator.
[0037] The technical solutions in the present invention will be described clearly and completely below in conjunction with the embodiments of the present invention. Obviously, the described embodiments are only a part of the embodiments of the present invention, not all of them. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.
[0038] The indium phosphide waste used in the embodiment is a defective product produced in the manufacturing process of a certain indium phosphide single crystal production enterprise in Yunnan. It is disc-shaped and looks like a CD. According to ICP-OES detection, the indium phosphide waste contains the main elements indium and phosphorus, and trace impurity elements such as calcium, sodium and magnesium, wherein the mass fraction of indium is 78.229%, the mass fraction of phosphorus is 18.303%, the mass fraction of calcium is 0.249%, the mass fraction of sodium is 0.059%, and the mass fraction of magnesium is 0.028%;
[0039] The purity of the high-purity gallium used in the embodiment is 99.999%, and it is produced by a gallium arsenide semiconductor production enterprise in Yunnan.
[0040] Example 1
[0041] In this embodiment, the graphite crucible is a cylinder with a height of 80 mm and an inner diameter of 50 mm, and specifically includes a first graphite crucible (height of 40 mm, inner diameter) and a second graphite crucible (height of 40 mm) arranged on the upper edge of the first graphite crucible. In this embodiment, a storage rack is arranged at an acute angle of 30° with the inner wall, and the bottom end of the storage rack is connected to the inner wall to form a storage groove with an open top (for storing high-purity gallium), and the bottom end of the storage rack is connected to the bottom end of the inner wall, and the longitudinal section of the storage groove is a triangle.
[0042] In this embodiment, the schematic diagram of the device for preparing gallium phosphide and recovering indium from indium phosphide waste is as follows: Figure 3 As shown, 1 is a vacuum pump; 2 is a filter; 3 is a bellows; 4 is a thermocouple; 5 is a pit furnace; 6 is a quartz tube; 7 is a rubber plug; 8 is a vacuum gauge; 9 is a graphite crucible; 10 is an argon generator; wherein the filter is connected to the vacuum pump and the bellows, and the other end of the bellows is connected to the quartz tube; the PU pneumatic hose connects the quartz tube and the inert gas generator; the quartz tube is inside the pit furnace; the graphite crucible is inside the quartz tube; the thermocouple is equipped with a temperature control device for heating the pit furnace, and the rubber plug is used to create a closed environment for the quartz tube; the vacuum gauge is connected to the rubber plug to measure the pressure inside the quartz tube.
[0043] The device is used to recycle and regenerate indium phosphide waste, and the specific operations are as follows:
[0044] (1) 200 g of indium phosphide waste was crushed, and the obtained indium phosphide waste particles (particle size of 3 mm) were loaded into the first graphite crucible of the graphite crucible, and 50 g of high-purity gallium was loaded into the storage tank of the second graphite crucible of the graphite crucible (the molar ratio of gallium to indium phosphide was 1:4), and the graphite crucible containing the materials was placed at the bottom of the quartz tube and placed in the pit furnace. The vacuum pump was turned on to pump the pressure inside the quartz tube to 10 Pa, and then the argon generator was turned on to continuously introduce argon into the quartz tube (for 10 minutes) to keep the system in a vacuum, oxygen-free and dry state.
[0045] (2) Turn off the argon generator and turn on the temperature control device of the thermocouple to increase the temperature in the system at a uniform rate of 10°C / min. When the temperature of the temperature control device reaches 900°C, stop heating (the temperature of the area where the indium phosphide waste is located is 900°C, and the temperature of the area where the high-purity gallium is located is 820°C). Keep the temperature at 900°C for 2 hours to allow the indium phosphide and gallium to undergo a substitution reaction.
[0046] After the reaction is completed, the device is cooled to room temperature, and material A is collected in the first graphite crucible, and material B is collected in the second graphite crucible.
[0047] The material A and the material B obtained in Example 1 were subjected to X-ray photoelectron spectroscopy (XPS) and inductively coupled plasma-mass spectrometry (ICP-MS) detection, and the results showed that the material A was indium and the material B was gallium phosphide. It was confirmed that the device and method provided by the present invention can prepare gallium phosphide and indium using indium phosphide waste and high-purity gallium.
[0048] The results show that the purity of indium obtained in Example 1 is 97.2%, and the direct yield of indium is 98%; the synthesis rate of gallium phosphide obtained is 85%, and the purity level is 4N.
[0049] Example 2
[0050] The method and apparatus of Example 1 are used to prepare gallium phosphide and indium using indium phosphide waste and high-purity gallium. The difference is that the temperature of the temperature control device is adjusted to 1000°C (at this time, the temperature of the area where the indium phosphide waste is located is 1000°C, and the temperature of the area where the high-purity gallium is located is 920°C), and the other conditions are the same as in Example 1.
[0051] The results showed that the purity of indium obtained in Example 2 was 99.9%, and the direct yield of indium was 99%; the synthesis rate of gallium phosphide obtained was 95%, and the purity level was 4N.
[0052] Example 3
[0053] The method and apparatus of Example 1 are used to prepare gallium phosphide and indium using indium phosphide waste and high-purity gallium. The difference is that the temperature of the temperature control device is adjusted to 1100°C (at this time, the temperature of the area where the indium phosphide waste is located is 1100°C, and the temperature of the area where the high-purity gallium is located is 1000°C), and the other conditions are the same as in Example 1.
[0054] The results show that the purity of indium obtained in Example 3 is 99.95%, and the direct yield of indium is 90% (this is due to the volatilization of indium); the synthesis rate of gallium phosphide obtained is 90%, and the purity level is 4N5.
[0055] Although the above embodiment describes the present invention in detail, it is only a part of the embodiments of the present invention, not all of the embodiments. People can also obtain other embodiments based on this embodiment without creativity, and these embodiments all fall within the protection scope of the present invention.
Claims
1. A method for preparing gallium phosphide and recovering indium from indium phosphide waste, characterized in that: The following steps are involved: Providing a graphite open container; the graphite open container comprises a first graphite open container and a second graphite open container arranged on the upper edge of the first graphite open container; Indium phosphide waste is loaded into the first open graphite container, and high-purity gallium is loaded into the second open graphite container. A replacement reaction is performed under vacuum conditions, and indium is collected in the first open graphite container, and gallium phosphide is collected in the second open graphite container. The purity of the high-purity gallium is not less than 99.99%. During the replacement reaction, the temperature of the first open graphite container is 900-1100° C., and the temperature of the second open graphite container is 820-1020° C.
2. The method according to claim 1, characterized in that The conditions of the replacement reaction include: a heat preservation time of 2 to 4 hours and a pressure of 10 to 30 Pa.
3. The method according to claim 1, characterized in that: In the second open graphite container, a storage rack is arranged at an acute angle with the inner wall, the bottom end of the storage rack is connected to the inner wall to form a storage groove with an open top, and the high-purity gallium is loaded into the storage groove of the second open graphite container.
4. The method according to claim 3, characterized in that: The bottom end of the storage rack is connected to the bottom end of the inner wall.
5. The method according to claim 3, characterized in that: The acute angle is 30-60°.
6. The method according to claim 1, characterized in that The molar ratio of gallium in the high-purity gallium to indium phosphide in the indium phosphide waste is 1:3-4.
7. The method according to claim 1 or 6, characterized in that: The mass fraction of indium in the indium phosphide waste is not less than 75%, and the mass fraction of phosphorus is not less than 15%.
8. The method according to claim 7, characterized in that The indium phosphide waste also includes impurities, which include at least one of calcium, sodium and magnesium; the mass fraction of calcium in the indium phosphide waste is 0.2% to 0.3%, the mass fraction of sodium is 0.05% to 0.06%, and the mass fraction of magnesium is 0.02% to 0.03%.
9. A device for preparing gallium phosphide and recovering indium from indium phosphide waste, characterized in that: It comprises a vacuum pump, a heating device, a pit furnace, a quartz tube, a graphite open container and an inert gas generator; the vacuum pump and the inert gas generator are respectively connected to the quartz tube; the heating device is used to heat the pit furnace; the quartz tube is inside the pit furnace; the graphite open container is inside the quartz tube; the graphite open container comprises a first graphite open container and a second graphite open container arranged on the upper edge of the first graphite open container.
10. The device according to claim 9, characterized in that It also includes a filter, a bellows, a PU pneumatic hose, a sealing component and a vacuum gauge; the filter is connected to the vacuum pump and the bellows, and the other end of the bellows is connected to the quartz tube; the PU pneumatic hose is connected to the quartz tube and the inert gas generating device.
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