A method and apparatus for preparing gallium phosphide from indium phosphide waste and recovering indium

Abstract

This invention provides a method and apparatus for preparing gallium phosphide and recovering indium from indium phosphide waste, belonging to the field of indium phosphide recycling technology. The method provided by this invention includes the following steps: providing a graphite open container; the graphite open container includes a first graphite open container and a second graphite open container disposed along 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, carrying out a displacement reaction under vacuum conditions, collecting indium in the first graphite open container, and collecting gallium phosphide in the second graphite open container. The method provided by this invention is simple to operate, has a short process, high efficiency, low cost, and is environmentally friendly. It realizes the conversion of second-generation indium phosphide semiconductor waste into third-generation gallium phosphide semiconductors, recovers indium and phosphorus, and eliminates the risk of spontaneous combustion of yellow phosphorus.

Description

Technical Field

[0001] This invention belongs to the field of indium phosphide recycling technology, specifically relating to a method and apparatus for preparing gallium phosphide and recycling indium from indium phosphide waste. Background Technology

[0002] Indium phosphide (InP) semiconductors are essential components of 5G optical communication systems. In recent years, with the rapid development of telecommunications and optoelectronic technologies, the consumption of InP semiconductors has been continuously increasing. Due to the low hardness, high brittleness, and easy dissociation of InP, the processing generates a large amount of waste. The ingot cutting process alone generates about 50% of the waste, and the overall yield of the processing is less than 30%, with the amount of waste increasing daily.

[0003] Currently, the main methods for recycling indium phosphide waste are wet processing and vacuum pyrolysis. Wet processing, such as an atmospheric pressure oxidation-acid leaching process, recovers indium through metal displacement. This method is simple to operate but time-consuming and generates harmful waste liquid. Vacuum pyrolysis, such as a two-stage vacuum high-temperature pyrolysis method using a tubular furnace, can recover and regenerate both indium and phosphorus. However, controlling the phosphorus conversion rate is difficult, and most of it is produced as spontaneously combusting yellow phosphorus, leading to high recycling difficulty and a high risk factor. Summary of the Invention

[0004] The purpose of this invention is to provide a method and apparatus for preparing gallium phosphide and recovering indium from indium phosphide waste. The method provided by this invention is simple to operate, has a short process, high efficiency, low cost, and is environmentally friendly. It achieves the recovery of indium and phosphorus from indium phosphide waste, realizing the transformation of waste into a new generation of high-value-added materials.

[0005] To achieve the above-mentioned objectives, the present invention provides the following technical solution:

[0006] This invention provides a method for preparing gallium phosphide and recovering indium from indium phosphide waste, comprising the following steps:

[0007] A graphite open container is provided; the graphite open container includes a first graphite open container and a second graphite open container disposed 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 displacement reaction is carried out under vacuum conditions. 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 displacement 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 displacement reaction include: a holding time of 2 to 4 hours and a pressure of 10 to 30 Pa.

[0010] Preferably, in the second graphite open container, a shelf is provided at an acute angle to the inner wall, and the bottom end of the shelf connects with the inner wall to form a storage slot with a top opening, and the high-purity gallium is placed into the storage slot of the second graphite open container.

[0011] Preferably, the bottom end of the shelf is connected to the bottom end of the inner wall.

[0012] Preferably, the acute angle is 30 to 60°.

[0013] Preferably, the molar ratio of gallium in the high-purity gallium to indium phosphide in the indium phosphide waste is 1:3 to 4.

[0014] Preferably, the indium phosphide waste contains at least 75% indium and at least 15% phosphorus by mass.

[0015] Preferably, 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%.

[0016] This invention provides an apparatus 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 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 includes a first graphite open container and a second graphite open container disposed on the upper edge of the first graphite open container.

[0017] Preferably, the apparatus for preparing gallium phosphide and recovering indium from indium phosphide waste further includes a filter, a bellows, a PU pneumatic hose, a rubber stopper, and a vacuum gauge; the filter is connected to a vacuum pump and a bellows, and the other end of the bellows is connected to a quartz tube; the PU pneumatic hose is connected to the quartz tube and an inert gas generator.

[0018] This invention provides a method for preparing gallium phosphide and recovering indium from indium phosphide waste, comprising the following steps: providing a graphite open container; the graphite open container includes a first graphite open container and a second graphite open container disposed along the upper edge of the first graphite open container; loading the indium phosphide waste into the first graphite open container, loading high-purity gallium into the second graphite open container, and carrying out a displacement 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 displacement 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 this invention adopts a raw material separation design, allowing for layered material discharge. 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, reacting with high-purity gallium to synthesize high-purity gallium phosphide. Simultaneously, controlling the temperature of the first open graphite container within 900–1100℃ and the temperature of the second open graphite container within 820–1020℃ fully enables the decomposition of indium phosphide and promotes the combination of phosphorus vapor and gallium to obtain gallium phosphide. It also facilitates the volatilization of impurities in the indium phosphide waste, thus yielding high-purity indium. The method provided by this invention is simple to operate, has a short process, high efficiency, low cost, and is environmentally friendly. It realizes the conversion of second-generation indium phosphide semiconductor waste into third-generation gallium phosphide semiconductors, recovers indium and phosphorus, and eliminates the risk of spontaneous combustion of yellow phosphorus.

[0019] Furthermore, this invention utilizes vacuum technology to promote the displacement reaction, employing a matching open graphite container to recover indium and phosphorus from indium phosphide waste in one step through a combination of vacuum thermal decomposition and vacuum synthesis; simultaneously, taking advantage of the low impurity content of indium phosphide raw materials, high-purity gallium phosphide and high-purity indium are directly prepared, transforming indium phosphide waste into usable materials in one step. Attached Figure Description

[0020] To more clearly illustrate the technical solutions in the embodiments of the present invention or the prior art, the drawings used in the embodiments will be briefly introduced below. Obviously, the drawings described below are only some embodiments of the present invention. For those skilled in the art, other drawings can be obtained based on these drawings without creative effort.

[0021] Figure 1 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 3This is a schematic diagram of an apparatus for preparing gallium phosphide and recovering indium from indium phosphide waste, wherein 1-vacuum pump; 2-filter; 3-bellows; 4-thermocouple; 5-well furnace; 6-quartz tube; 7-rubber stopper; 8-vacuum gauge; 9-graphite crucible; 10-argon gas generator. Detailed Implementation

[0024] This invention provides a method for preparing gallium phosphide and recovering indium from indium phosphide waste, comprising the following steps:

[0025] A graphite open container is provided; the graphite open container includes a first graphite open container and a second graphite open container disposed 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 displacement reaction is carried out under vacuum conditions. 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 displacement 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 this invention, unless otherwise specified, all raw materials used are commercially available products well known to those skilled in the art or prepared using methods well known to those skilled in the art.

[0028] In this invention, the graphite open container includes a first graphite open container and a second graphite open container disposed along the upper edge of the first graphite open container. In this invention, the inner wall of the second graphite open container may be provided with a top-opening storage slot, into which the high-purity gallium can be placed. In the second graphite open container of this invention, a shelf is disposed at an acute angle to the inner wall, the bottom end of which can connect with the inner wall to form a storage slot; the longitudinal section of the storage slot can be triangular. In this invention, the acute angle formed by the shelf and the inner wall of the second graphite open container can be 30–60°, that is, the bottom angle of the storage slot is 30–60°. In a specific embodiment of this invention, the acute angle formed by the shelf and the inner wall of the second graphite open container is 45°. In this invention, the graphite open container can be a graphite crucible, the first graphite open container can be a first graphite crucible, and the second graphite open container can be a second graphite crucible. In a specific embodiment of the present invention, the open graphite container is a cylinder with a height of 80 mm, and the height of the first graphite crucible and the second graphite crucible are each 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 A schematic diagram of a graphite crucible, as shown below. Figure 1 As shown, the graphite crucible of the present invention adopts a design of two stacked graphite crucibles, which are divided into a first graphite crucible and a second graphite crucible set on the upper edge of the first graphite crucible. At the connection between the two crucibles, a protruding design is formed by a placement plate, and the placement plate and the inner wall of the second graphite crucible form a placement groove with an open top.

[0030] In this invention, the indium phosphide waste contains at least 75% indium and at least 15% phosphorus by mass. The indium phosphide waste may also contain impurities, including at least one of calcium, sodium, and magnesium. The mass fraction of calcium in the indium phosphide waste may be 0.2%–0.3%, the mass fraction of sodium may be 0.05%–0.06%, and the mass fraction of magnesium may be 0.02%–0.03%. In a specific embodiment of this invention, the indium phosphide waste is a defective product generated during the manufacturing process of an indium phosphide single crystal production enterprise in Yunnan Province. It is disc-shaped, resembling a CD. ICP-OES testing shows that the indium phosphide waste contains the main elements indium and phosphorus, and trace amounts of impurities such as calcium, sodium, and magnesium. Specifically, 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, the particle size of which is 3mm.

[0031] In this invention, the purity of the high-purity gallium is not less than 99.99%; in a specific embodiment of this invention, the purity of the gallium is 99.999%.

[0032] In this invention, the molar ratio of gallium in the high-purity gallium to indium phosphide in the indium phosphide waste can be 1:3 to 4; in a specific embodiment of this 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 A schematic diagram of a graphite crucible filled with indium phosphide waste and high-purity gallium, as shown. Figure 2 As shown, indium phosphide waste is placed in the first graphite crucible, and high-purity gallium is placed in the storage tank at the bottom of the second graphite crucible. This allows the phosphorus vapor generated by the thermal decomposition of indium phosphide waste in the first graphite crucible to volatilize into the second graphite crucible, where it is synthesized with gallium to produce gallium phosphide. Gallium phosphide can be collected in the second graphite crucible. Indium generated by the decomposition of indium phosphide is retained in the first graphite crucible. In other words, the existence of the storage tank can achieve both layered feeding of raw materials and separate collection of gallium phosphide and indium.

[0034] This invention involves loading indium phosphide waste into a first open graphite container and high-purity gallium into a second open graphite container, and then conducting a displacement reaction under vacuum conditions. In a specific embodiment of this invention, after the indium phosphide waste and high-purity gallium are loaded, the open graphite container containing the materials is placed at the bottom of a quartz tube, and the quartz tube is placed into a pit furnace. The inert gas used in this invention can be argon. Before the displacement reaction, the pressure inside the quartz tube can be evacuated to the pressure required for the displacement reaction, and then an inert gas is introduced into the reaction system to expel the air. In this invention, the inert gas is introduced to prevent oxidation of indium and phosphorus and to create a vacuum environment. In a specific embodiment of this invention, the inert gas is introduced for 10 minutes. In this invention, during the displacement 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. In a specific embodiment of the present invention, during the displacement reaction, the temperature of the first open graphite container is 900℃, 950℃, 1000℃, 1050℃, or 1100℃, and the temperature of the second open graphite container is 820℃, 870℃, 920℃, 970℃, or 1020℃. The conditions for the displacement reaction of the present invention may include: a holding time of 2–4 hours, a heating rate to the temperature of the first or second open graphite container of 8–12℃ / min, and a pressure of 10–30 Pa. In a specific embodiment of the present invention, the holding time for the displacement reaction is 2 hours; the heating rate to the temperature of the first or second open graphite container is 8℃ / min, 10℃ / min, or 12℃ / min; and the pressure is 10 Pa, 20 Pa, or 30 Pa. After the displacement reaction is completed, the present invention can cool the obtained reactants to room temperature, collect indium in a first open graphite container, and collect gallium phosphide in a second open graphite container. The purity of indium in the present invention can be no less than 97%, and the direct indium recovery rate 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 to 4N5. In specific embodiments of the present invention, the purity of indium is 97.2%, 99.9%, or 99.95%; the direct indium recovery rate is 90%, 98%, or 99%; the synthesis rate of gallium phosphide is 85%, 90%, or 95%; and the purity level of gallium phosphide is 4N or 4N5.

[0035] This invention controls the temperature of the first graphite open container within the range of 900–1100°C and the temperature of the second graphite open container within the range of 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 this invention is simple to operate, has a short process, high efficiency, low cost, and is environmentally friendly. It realizes the recovery of indium and phosphorus from indium phosphide waste, while eliminating the risk of spontaneous combustion of yellow phosphorus. Moreover, this invention utilizes vacuum technology to promote the displacement reaction. Using a matching graphite open container, indium phosphide waste is recovered in one step through a combination of vacuum thermal decomposition and vacuum synthesis. At the same time, taking advantage of the low impurity content of indium phosphide raw material, high-purity gallium phosphide and high-purity indium are directly prepared, transforming indium phosphide waste into usable materials in one step.

[0036] This invention also provides an apparatus 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 this invention, the heating device can be a thermocouple equipped with a temperature control device; the inert gas generator can be an argon gas generator. In this invention, the apparatus for preparing gallium phosphide and recovering indium from indium phosphide waste may further include a filter, a bellows, a PU pneumatic hose, a sealing component, and a vacuum gauge. The sealing component in this invention can be a rubber stopper. In this 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; the graphite open container is inside the quartz tube. The graphite open container of this invention includes a first graphite open container and a second graphite open container disposed along the upper edge of the first graphite open container. The heating device of this invention is used to heat a pit furnace, and the rubber stopper can be used to create a sealed environment for the quartz tube; the vacuum gauge can be connected to the rubber stopper to measure the pressure inside the quartz tube. In a specific embodiment of this invention, the open graphite container is a graphite crucible; the apparatus 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 generator.

[0037] The technical solutions of this invention will be clearly and completely described below with reference to the embodiments thereof. Obviously, the described embodiments are only a part of the embodiments of this invention, and not all of them. All other embodiments obtained by those skilled in the art based on the embodiments of this invention without creative effort are within the scope of protection of this invention.

[0038] The indium phosphide waste used in this example is a defective product generated during the manufacturing process of an indium phosphide single crystal production enterprise in Yunnan. It is disc-shaped and resembles an optical disc. ICP-OES testing shows that the indium phosphide waste contains the main elements indium and phosphorus, as well as trace amounts of impurity elements such as calcium, sodium, and magnesium. 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 high-purity gallium used in the examples has a purity of 99.999% and was produced by a gallium arsenide semiconductor manufacturing company in Yunnan.

[0040] Example 1

[0041] In this embodiment, the graphite crucible is cylindrical with a height of 80 mm and an inner diameter of 50 mm. Specifically, it includes a first graphite crucible (40 mm high, inner diameter) and a second graphite crucible (40 mm high) disposed along the upper edge of the first graphite crucible. In this embodiment, a shelf is provided in the second graphite crucible at a 30° acute angle to the inner wall. The bottom end of the shelf connects to the inner wall to form a top-opening storage slot (for storing high-purity gallium). The bottom end of the shelf connects to the bottom end of the inner wall, and the longitudinal section of the storage slot is triangular.

[0042] In this embodiment, a schematic diagram of the apparatus for preparing gallium phosphide and recovering indium from indium phosphide waste is shown below. 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 stopper; 8 is a vacuum gauge; 9 is a graphite crucible; and 10 is an argon gas generator. The filter connects 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. The rubber stopper is used to create a sealed environment for the quartz tube. The vacuum gauge is connected to the rubber stopper and is used to measure the pressure inside the quartz tube.

[0043] The specific operation of recycling and regenerating indium phosphide waste using the aforementioned device is as follows:

[0044] (1) Crush 200g of indium phosphide waste and pack the resulting indium phosphide waste particles (3mm in diameter) into the first graphite crucible. Pack 50g of high-purity gallium into the storage slot of the second graphite crucible (the molar ratio of gallium to indium phosphide is 1:4). Place the graphite crucible containing the materials at the bottom of the quartz tube and put it into the pit furnace. Turn on the vacuum pump to evacuate the pressure inside the quartz tube to 10Pa. Then turn on the argon generator and 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 thermocouple temperature control device to make the temperature in the system rise at a uniform rate of 10℃ / min. When the temperature of the temperature control device reaches 900℃, stop heating (at this time, the temperature of the area where the indium phosphide waste is located is 900℃, and the temperature of the area where the high-purity gallium is located is 820℃). Keep the temperature at 900℃ for 2 hours to allow the indium phosphide and gallium to undergo a displacement reaction.

[0046] After the reaction was completed, the apparatus was cooled to room temperature, and material A was collected in the first graphite crucible and material B was collected in the second graphite crucible.

[0047] X-ray photoelectron spectroscopy (XPS) and inductively coupled plasma mass spectrometry (ICP-MS) were performed on materials A and B obtained in Example 1. The results showed that material A was indium and material B was gallium phosphide. This confirms that the apparatus and method provided by the present invention can prepare gallium phosphide and indium using indium phosphide waste and high-purity gallium.

[0048] The results showed that the purity of indium obtained in Example 1 was 97.2%, and the direct indium recovery rate was 98%; the synthesis rate of gallium phosphide obtained was 85%, and the purity level was 4N.

[0049] Example 2

[0050] Gallium phosphide and indium were prepared using the method and apparatus of Example 1, with the difference being that the temperature of the temperature control device was adjusted to 1000°C (at which time the temperature of the area where the indium phosphide waste was located was 1000°C, and the temperature of the area where the high-purity gallium was located was 920°C), and the other conditions were 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 indium recovery rate was 99%; the synthesis rate of gallium phosphide obtained was 95%, and the purity level was 4N.

[0052] Example 3

[0053] Gallium phosphide and indium were prepared using the method and apparatus of Example 1, with the difference being that the temperature of the temperature control device was adjusted to 1100°C (at which time the temperature of the area where the indium phosphide waste was located was 1100°C, and the temperature of the area where the high-purity gallium was located was 1000°C), and the other conditions were the same as in Example 1.

[0054] The results showed that the purity of indium obtained in Example 3 was 99.95%, and the direct indium recovery rate was 90% (due to the volatilization of indium); the synthesis rate of gallium phosphide obtained was 90%, and the purity level was 4N5.

[0055] Although the above embodiments have provided a detailed description of the present invention, they are only some embodiments of the present invention, and not all embodiments. People can obtain other embodiments based on these embodiments without creative effort, 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, Includes the following steps: A graphite open container is provided; the graphite open container includes a first graphite open container and a second graphite open container disposed 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 displacement reaction is carried out under vacuum conditions. 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 displacement 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 for the displacement reaction include: a holding 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 graphite open container, a shelf is provided at an acute angle to the inner wall. The bottom end of the shelf connects with the inner wall to form a storage slot with an open top. The high-purity gallium is placed into the storage slot of the second graphite open container.

4. The method according to claim 3, characterized in that, The bottom end of the shelf 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 to 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 to 4.

7. The method according to claim 1 or 6, characterized in that, The indium phosphide waste contains at least 75% indium and at least 15% phosphorus by mass.

8. The method according to claim 7, characterized in that, The indium phosphide waste also includes impurities, including 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. An apparatus for preparing gallium phosphide and recovering indium from indium phosphide waste, characterized in that, The device includes 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 includes a first graphite open container and a second graphite open container disposed on the upper edge of the first graphite open container.

10. The apparatus 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 a quartz tube; the PU pneumatic hose is connected to the quartz tube and an inert gas generator.

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