Heating material melting device

Abstract

The invention discloses a material heating and melting device, and relates to the technical field of material heating and melting, a crucible assembly is arranged in a reaction tube, and an induction heating assembly is arranged outside the reaction tube; the crucible assembly sequentially comprises an upper material containing crucible, a material melting funnel and a lower material receiving crucible from top to bottom, the induction heating assembly heats the upper material containing crucible, materials in the upper material containing crucible are melted, and the melted materials flow into the lower material receiving crucible through the material melting funnel; the induction heating assembly is used for preserving heat of molten materials in the lower material receiving crucible, and after the materials are molten, the lower material receiving crucible is independently disassembled and taken out; the reaction tube plays a role in isolation, a material melting area is separated from a heating area, and interference of the heating assembly on materials is avoided.

Description

Technical Field

[0001] The invention relates to the technical field of material heating and melting, and further to a material heating and melting device. Background Art

[0002] Molecular beam epitaxy (MBE) is a physical deposition technology for compound semiconductor multilayer films. The parameters of MBE raw materials play a crucial role in the deposition process and the final electrical properties of the structure. In order to obtain a stable beam current, solid ingot materials are used as raw materials; in addition, the purity of the raw materials needs to reach 6N or above, so the acquisition of high-purity rod-shaped materials is the key to obtaining high-quality MBE device materials.

[0003] In conventional processes, ingots are usually prepared using a high-frequency induction heating furnace. Figure 1 As shown, the block material 02 is placed in the crucible 01, and then the water-cooled high-frequency coil 03 is energized, and an induction current is generated inside the crucible 01 to heat itself. When the temperature reaches the melting point of the material, the raw materials inside begin to melt and mix. Then the output power of the high-frequency coil 03 is reduced, and the material is gradually cooled to obtain the final ingot.

[0004] The high-frequency induction heating furnace requires a crucible that can convert alternating electromagnetic waves into induced currents, and then into heat energy. Therefore, it is necessary to select materials that are resistant to high temperatures and have good electrical conductivity. In order to obtain high-purity ingot materials, high-purity graphite is generally used as the crucible material, or quartz is used as the crucible material and the external heating layer uses high-purity graphite. However, the procurement and processing costs of high-purity graphite are relatively high, which increases the cost of ingot operation.

[0005] In addition, in the process of high-purity material chemistry, in order to prevent oxidation or remove the oxide layer, hydrogen will be introduced into the furnace as a reducing gas to remove oxides produced by other reasons such as outgassing of crucible materials. The explosion limit of hydrogen is widely distributed, so the sealing performance of the equipment is required to be high, and improper handling can easily cause safety hazards.

[0006] When the saturated vapor pressure of the material being melted is low, the material will volatilize during the melting process and condense at a low temperature inside the chamber. Therefore, the inside of the chamber needs to be polished and cleaned after melting. The powdered pollutants generated during the cleaning process will float into the crucible after the gas is introduced in the subsequent process, causing contamination to the material inside. Especially in the preparation of small-sized ingots, the impurity contamination caused by floating pollutants will be more serious.

[0007] For those skilled in the art, how to effectively separate the chemical zone from the heating zone is a technical problem that needs to be solved at present. Summary of the invention

[0008] The core of the present invention is to provide a heating and material processing device, which isolates the induction heating component and the crucible component from each other, and can independently take out the lower receiving crucible after receiving the material. The specific scheme is as follows:

[0009] A heating device for chemical materials comprises a reaction tube, a crucible assembly and an induction heating assembly, wherein the crucible assembly is arranged inside the reaction tube; and the induction heating assembly is arranged outside the reaction tube;

[0010] The crucible assembly includes an upper material holding crucible, a material hopper, and a lower material receiving crucible from top to bottom, wherein the upper material holding crucible is used to hold the material to be heated; and the lower material receiving crucible can be separated from the crucible assembly separately;

[0011] The induction heating component is used to heat the upper material holding crucible to melt the material in the upper material holding crucible, and the melted material flows into the lower material receiving crucible through the material mixing funnel; the induction heating component is used to keep the melted material in the lower material receiving crucible warm.

[0012] Optionally, the lower end of the upper material holding crucible is inserted into the material-forming funnel to limit the circumferential position; a crucible support is arranged between the material-forming funnel and the lower material-forming crucible, and the crucible support supports the material-forming funnel above the lower material-forming crucible.

[0013] Optionally, the crucible support comprises an upper support ring, support rods and a lower support ring, and the upper support ring and the lower support ring are fixedly supported by a plurality of support rods;

[0014] The upper surface of the upper support ring supports the lower surface of the material-forming hopper; the bottom surface of the lower support ring is provided with an annular groove for inserting the lower material receiving crucible.

[0015] Optionally, an air inlet is provided at the upper end of the reaction tube and an exhaust port is provided at the lower end, the air inlet is used to introduce hydrogen into the inner cavity of the reaction tube, and the exhaust port is used to exhaust the hydrogen.

[0016] Optionally, upper condensing fins are provided at the upper part of the inner cavity of the reaction tube, and the hydrogen entering from the air inlet can directly impact the upper condensing fins. The upper condensing fins cooled by the hydrogen are used for condensing and depositing the vaporized material in the upper material holding crucible.

[0017] Optionally, lower condensing fins are provided at the lower part of the inner cavity of the reaction tube, and the lower condensing fins are used for condensing and depositing the vaporized material before it is discharged with the hydrogen.

[0018] Optionally, the crucible assembly comprises a crucible support, and an upper end portion of the crucible support is provided with a placement groove for inserting the bottom of the lower material receiving crucible;

[0019] The lower condensing fins are arranged around the outside of the crucible support; a cooling channel is arranged inside the crucible support, and the cooling channel is used for cooling fluid to pass through, so as to cool the bottom of the lower material receiving crucible and the lower condensing fins.

[0020] Optionally, it further comprises an outer cover tube disposed outside the reaction tube, the induction heating assembly comprises a high-frequency coil, an induction heater and a heat insulation cover, the high-frequency coil is disposed outside the outer cover tube, and the induction heater and the heat insulation cover are disposed in the interlayer between the reaction tube and the outer cover tube;

[0021] The heat insulation cover is arranged on the outer surface of the reaction tube and covers the induction heater, and the inner surface of the heat insulation cover is plated with a heat insulation reflective film;

[0022] Alternatively, the induction heating component is a resistance heater arranged in the interlayer between the outer cover tube and the reaction tube.

[0023] Optionally, the high-frequency coil, the induction heater and the heat-insulating cover are each provided with two independent parts corresponding to the upper material holding crucible and the lower material receiving crucible, so as to adjust the temperature of the upper material holding crucible and the lower material receiving crucible respectively.

[0024] Optionally, the outer cover tube is provided with a vacuum air inlet, and the vacuum air inlet is connected to a negative pressure source to evacuate the interlayer between the outer cover tube and the reaction tube;

[0025] And / or, a hydrogen sensor and / or a vacuum sensor is arranged in the interlayer between the outer cover tube and the reaction tube;

[0026] And / or, the outer cover tube, the reaction tube and the lower material receiving crucible are transparent devices made of quartz.

[0027] The invention provides a heating and material-processing device, wherein a crucible component is arranged inside a reaction tube, and an induction heating component is arranged outside the reaction tube; the crucible component comprises an upper material-containing crucible, a material-processing funnel, and a lower material-connecting crucible in order from top to bottom; the induction heating component heats the upper material-containing crucible to melt the material in the upper material-containing crucible, and the melted material flows into the lower material-connecting crucible through the material-processing funnel; the induction heating component is used for heat-insulating the melted material in the lower material-connecting crucible, and when the material is completely melted, the lower material-connecting crucible is separately split and taken out; the invention plays an isolating role through the reaction tube, separates the area where the material is melted from the heating area, and avoids interference of the heating component on the material. BRIEF DESCRIPTION OF THE DRAWINGS

[0028] 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 or the description of the prior art 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 work.

[0029] Figure 1 It is a schematic diagram of an existing heating and chemical material device;

[0030] Figure 2 It is an axonometric diagram of a specific embodiment of the heating and chemical material device of the present invention;

[0031] Figure 3 for Figure 2 Axonometric section drawing of

[0032] Figure 4 It is an axonometric diagram of a specific embodiment of the combination of a reaction tube and an induction heating assembly;

[0033] Figure 5 for Figure 4 Axonometric section drawing of

[0034] Figure 6 It is an axonometric schematic diagram of a specific embodiment of a crucible assembly;

[0035] Figure 7 for Figure 6 Axonometric section drawing of

[0036] Figure 8 It is an axonometric diagram of a specific embodiment of an upper material holding crucible, a material mixing funnel, a lower material receiving crucible, and a crucible support;

[0037] Fig. 9 for Figure 8 Axonometric section drawing of

[0038] Fig.10 A cross-sectional schematic diagram of a specific embodiment of a crucible support;

[0039] Fig.11 It is an axonometric diagram of a specific embodiment of the upper condensation fin;

[0040] Fig.12 It is an axonometric view from an oblique upper perspective of a specific embodiment of the crucible support;

[0041] Fig.13 It is an axonometric view from a downward angle of a specific embodiment of a crucible support;

[0042] Fig.14 It is an axonometric view of a specific embodiment of a chemical hopper.

[0043] The figure includes:

[0044] Reaction tube 1, air inlet 11, exhaust port 12, upper condensation fins 13, lower condensation fins 14;

[0045] Crucible assembly 2, upper material holding crucible 21, material hopper 22, lower material receiving crucible 23, crucible support 24, upper support ring 241, support rod 242, lower support ring 243, annular groove 2431, crucible support 25, placement groove 251, cooling channel 252;

[0046] Induction heating assembly 3 , high frequency coil 31 , induction heater 32 , heat insulation cover 33 , outer cover tube 4 , vacuum air inlet 41 . DETAILED DESCRIPTION

[0047] In order to enable those skilled in the art to better understand the technical solution of the present invention, the heating and material processing device of the present invention will be described in detail below in conjunction with the accompanying drawings and specific implementation methods.

[0048] The present invention provides a heating and chemical material device, combined with Figure 2 , Figure 3 , Figure 4 , Figure 5 As shown, it includes structures such as a reaction tube 1, a crucible assembly 2, and an induction heating assembly 3. The reaction tube 1 is a shell structure with a hollow interior. In the structure shown in the accompanying drawings of the present invention, the reaction tube 1 includes a cylindrical outer shell and end covers arranged at both ends, and the cylindrical outer shell and the end covers at both ends together form an internal hollow accommodation space. The crucible assembly 2 is arranged inside the reaction tube 1, and the crucible assembly 2 is relatively isolated from the outside world by the reaction tube 1. The induction heating assembly 3 is arranged outside the reaction tube 1, and the induction heating assembly 3 generates heat to heat the crucible assembly 2, but the induction heating assembly 3 and the crucible assembly 2 are respectively arranged in different spaces, and the induction heating assembly 3 and the crucible assembly 2 are isolated by the reaction tube 1.

[0049] Combination Figure 6 , Figure 7 As shown, the crucible assembly 2 includes an upper material holding crucible 21, a material hopper 22, and a lower material receiving crucible 23 from top to bottom. The upper material holding crucible 21 is used to hold the material to be heated, and the solid material particles are placed in the upper material holding crucible 21; the upper end opening of the upper material holding crucible 21 is used to put in the material, and the lower end opening is used to discharge the material. The solid material is put in from the upper end opening. The upper material holding crucible 21 is a melting container for the material. The solid particles are heated and melted in the upper material holding crucible 21 to form a liquid and are discharged from the lower outlet.

[0050] The upper material holding crucible 21 is surrounded by the induction heating assembly 3, and the induction heating assembly 3 heats the upper material holding crucible 21, so that the upper material holding crucible 21 reaches a sufficient temperature and melts the material inside, and the material changes from solid to liquid. The melted material is discharged from the lower end of the upper material holding crucible 21, enters the material hopper 22, and flows into the lower material receiving crucible 23 through the material hopper 22, and the melted material is received by the lower material receiving crucible 23. The cross-sectional area of ​​the inner cavity of the material hopper 22 is larger at the top and smaller at the bottom, so that the liquid material converges from the top to the bottom, and guides the material to flow into the lower material receiving crucible 23.

[0051] It should be noted that the upper material holding crucible 21 and the material-forming funnel 22 can be two independent components, or the upper material holding crucible 21 and the material-forming funnel 22 can be an integrated structure. Figure 8 , Fig. 9 As shown, the upper material holding crucible 21 and the material-forming funnel 22 are independently arranged, the upper material holding crucible 21 is a cylindrical shape of equal diameter, the bottom end of the upper material holding crucible 21 is inserted into the upper end of the material-forming funnel 22, and the bottom end of the upper material holding crucible 21 is supported by the material-forming funnel 22. When materials are placed in the upper material holding crucible 21, the materials are supported by the material-forming funnel 22. If an integrated structure is adopted, the bottom end of the upper material holding crucible 21 and the material-forming funnel 22 are integrally formed and manufactured.

[0052] The lower material receiving crucible 23 and the material-forming funnel 22 are detachable and separable. The lower material receiving crucible 23 can be separated separately from the crucible assembly 2, so that the melted material can be taken out, and the liquid high-temperature material enters the lower material receiving crucible 23, and is cooled and solidified in the lower material receiving crucible 23. The upper material holding crucible 21 and the material-forming funnel 22 temporarily store the material, and when the material is melted, it is completely discharged into the lower material receiving crucible 23, and the lower material receiving crucible 23 receives the liquid material. Since the upper material holding crucible 21 and the material-forming funnel 22 cannot store liquid materials, the material will basically flow completely into the lower material receiving crucible 23 after melting. The upper material holding crucible 21 and the material-forming funnel 22 can be reused. After each material receiving, only the lower material receiving crucible 23 is taken out separately and replaced with a new lower material receiving crucible 23.

[0053] In addition to being used to heat the material in the upper material holding crucible 21, the induction heating component 3 is also used to keep the melted material in the lower material holding crucible 23 warm. The temperature of the lower material holding crucible 23 is lower than that of the upper material holding crucible 21. The melted material enters the lower material holding crucible 23 and still maintains a relatively high temperature, which can prevent the material in the lower material holding crucible 23 from cooling and solidifying too quickly, and helps to improve the uniformity of the cooling and solidification of the material.

[0054] The heating and melting device provided by the present invention has an isolation effect through the reaction tube 1, which physically isolates the melting space from the heating space to prevent the heating component from interfering with the material. The lower material receiving crucible 23 of the crucible assembly 2 can be taken out separately, and only part of the structure needs to be replaced.

[0055] Based on the above solution, the present invention provides a specific arrangement of the crucible assembly 2. Figure 7 , Figure 8 , Fig. 9 , Fig.14 As shown, the lower end of the upper material-carrying crucible 21 is inserted into the material-carrying hopper 22 to limit the circumferential position. The upper end of the material-carrying hopper 22 is provided with a circle of cylindrical structures, which can match the upper material-carrying crucible 21. The upper material-carrying crucible 21 is a cylindrical hollow tube structure that penetrates from top to bottom. The lower end of the upper material-carrying crucible 21 can be inserted into the upper part of the material-carrying funnel 22. A crucible support 24 is provided between the material-carrying funnel 22 and the lower material-carrying crucible 23. The crucible support 24 plays a supporting role. The crucible support 24 supports the material-carrying funnel 22 above the lower material-carrying crucible 23. The part of the crucible support 24 contacts the upper end of the lower material-carrying crucible 23, so that the discharge outlet at the lower end of the material-carrying funnel 22 extends to the middle position above the lower material-carrying crucible 23. The lower end of the material-carrying funnel 22 should be slightly lower than the upper edge of the lower material-carrying crucible 23.

[0056] Combination Fig.12 , Fig.13 As shown, the crucible support 24 includes an upper support ring 241, a support rod 242 and a lower support ring 243. The upper support ring 241 and the lower support ring 243 are fixedly supported by a plurality of support rods 242. Figure 8 , Fig. 9 As shown, it is supported by three support rods 242.

[0057] The upper surface of the upper support ring 241 is a circle of circular rings, which can support the lower surface of the material funnel 22; the upper surface of the upper support ring 241 can be a circle of planes, and a circle of matching plane support surfaces is correspondingly set on the material funnel 22, and the two are in contact to form support; the upper surface of the upper support ring 241 can also be a conical surface, which matches and contacts the conical contraction surface of the material funnel 22.

[0058] Combination Fig. 9 , Fig.13 As shown, the bottom surface of the lower support ring 243 is provided with an annular groove 2431 for inserting the lower material crucible 23, and the upper end edge of the lower material crucible 23 can be just embedded in the annular groove 2431, which not only realizes axial support but also radial limitation, ensuring stable cooperation between the lower support ring 243 and the lower material crucible 23.

[0059] Furthermore, the present invention provides an air inlet 11 at the upper end of the reaction tube 1 and an exhaust port 12 at the lower end. The air inlet 11 is used to introduce hydrogen into the inner cavity of the reaction tube 1, and the exhaust port 12 is used to exhaust the hydrogen. Figure 3 , Figure 5As shown, hydrogen gas input from the gas inlet 11 enters the reaction tube 1 and can contact the crucible assembly 2. The hydrogen gas acts as a reducing gas to remove oxides generated by other reasons such as degassing of the crucible material. The hydrogen gas is finally discharged from the reaction tube 1 from the exhaust port 12. The gas inlet 11 is arranged on the upper end cover of the reaction tube 1, and the exhaust port 12 is arranged on the lower end cover of the reaction tube 1. Since the hydrogen gas only enters the interior of the reaction tube 1, the reaction tube 1 separates the hydrogen zone from the heating zone, thereby solving the safety problem.

[0060] Combination Figure 3 , Figure 5 As shown, an upper condensation fin 13 is provided at the upper part of the inner cavity of the reaction tube 1. The hydrogen entering from the air inlet 11 can directly impact the upper condensation fin 13. Due to the impact of the low-temperature hydrogen entering from the outside, the upper condensation fin 13 is cooled. The upper condensation fin 13 cooled by the hydrogen is used for condensation and deposition of the vaporized material in the upper material holding crucible 21, which can greatly reduce the condensation of the vaporized material at the air inlet 11 and cause blockage. Fig.11 As shown, the upper condensation fin 13 includes a plurality of parallel and spaced flat plates, the area of ​​which is smaller than the cross-sectional area of ​​the inner cavity of the reaction tube 1, and the plurality of flat plates are fixed to each other through support columns and fixedly mounted on the upper end surface of the reaction tube 1. The flat plates constituting the upper condensation fin 13 may be complete flat plates or may be provided with through holes, and the plate surface of the upper condensation fin 13 may be perpendicular to the inflow direction of hydrogen or may be parallel to the inflow direction of hydrogen, and these specific structures shall all be included in the protection scope of the present invention.

[0061] Combination Figure 3 , Figure 5 As shown, lower condensing fins 14 are provided at the lower part of the inner cavity of the reaction tube 1. The lower condensing fins 14 are used for condensing and depositing the vaporized material before it is discharged with the hydrogen. The hydrogen carries the excited material, first passes through the lower condensing fins 14, and then passes through the exhaust port 12, thereby reducing the cooling and condensation of the vaporized material at the exhaust port 12, and avoiding the exhaust port 12 from being blocked by the condensed material.

[0062] Combination Figure 3 , Figure 5 , Figure 6 , Figure 7 , Fig.10 As shown, the crucible assembly 2 includes a crucible support 25, which is used to support the lower material crucible 23. The upper end of the crucible support 25 is provided with a placement groove 251 for inserting the bottom of the lower material crucible 23. When the bottom end of the lower material crucible 23 is inserted into the placement groove 251, the bottom surface of the placement groove 251 provides an upward supporting force for the lower material crucible 23. The side wall of the placement groove 251 is used to radially limit the lower material crucible 23 to ensure that the lower material crucible 23 is stably supported.

[0063] like Figure 3 , Figure 5 As shown, the lower condensation fins 14 are arranged around the outside of the crucible support 25. The lower condensation fins 14 include a cylinder that fits the outer surface of the crucible support 25, and a plurality of annular plate structures are arranged on the outer surface of the cylinder. A cooling channel 252 is arranged inside the crucible support 25. As shown by the arrow in the figure, the cooling channel 252 is used for cooling fluid to pass through. The cooling fluid can be a coolant or an inert gas such as nitrogen. The cooling fluid flows through the cooling channel 252 to cool the crucible support 25, thereby cooling the bottom of the lower material crucible 23 and the lower condensation fins 14. The bottom end of the lower material crucible 23 is cooled by the crucible support 25, so that the liquid material inside the lower material crucible 23 is gradually cooled from bottom to top along the axial direction, so that the material inside can be cooled more evenly. The crucible support 25 provides cold energy to the lower condensing fins 14 , so that the lower condensing fins 14 can be kept at a low temperature continuously, thereby continuously condensing the vaporized material on the lower condensing fins 14 .

[0064] Combination Figure 2 , Figure 3 As shown, the heating and chemical material device of the present invention also includes an outer cover tube 4 which is arranged outside the reaction tube 1, and the outer cover tube 4 and the reaction tube 1 together form an annular cavity. The induction heating assembly 3 includes a high-frequency coil 31, an induction heater 32 and a heat insulation cover 33. The high-frequency coil 31 is arranged outside the outer cover tube 4, and the high-frequency coil 31 adopts a water-cooled copper coil; the high-frequency coil 31 is spirally wound outside the outer cover tube 4, the induction heater 32 and the heat insulation cover 33 are arranged in the interlayer between the reaction tube 1 and the outer cover tube 4, the induction heater 32 is fixed on the outer surface of the reaction tube 1, and the heat insulation cover 33 is fixed on the outer surface of the reaction tube 1; because the induction heater 32 is isolated from the chemical material chamber inside the reaction tube 1, graphite or other metal materials with lower purity can be used, which greatly reduces the use cost. The heat shield 33 is disposed on the outer surface of the reaction tube 1 and covers the outside of the induction heater 32. The heater 32 is disposed in the annular space surrounded by the heat shield 33 and the reaction tube 1. The inner surface of the heat shield 33 is plated with a heat-insulating reflective film, such as a gold film or other materials. The heat-insulating reflective film can reflect heat and make the heat more concentrated on one side of the reaction tube 1, thereby heating the crucible assembly 2 inside the reaction tube 1, increasing the heating efficiency and reducing the temperature of the outer cover tube 4. The angle between the upper and lower heat shields 33 that wrap the upper and lower induction heaters 32 and the induction heaters 32 can be designed and adjusted according to the position of the internal crucible and funnel to increase the heating area.

[0065] In addition to realizing induction heating by cooperating between the high-frequency coil 31 and the induction heater 32, the induction heater 32 can also be replaced with a resistance heater, which is located in the interlayer formed by the reaction tube 1 and the outer cover tube 4, so as to realize the resistance heating process. When in use, the interlayer formed by the reaction tube 1 and the outer cover tube 4 is evacuated, and the service life of the heater can be increased under the vacuum state. A heat-insulating reflective structure can also be provided corresponding to the induction heater 32.

[0066] Water cooling structures are respectively provided at the upper and lower end covers of the outer cover tube 4, so that the sealing ring between the crucible support 25 and the lower end, the sealing ring between the reaction tube 1 and the upper end cover and other components can be cooled to prevent high temperature deformation. In addition, the upper end of the outer cover tube 4 can cooperate with the upper condensation fins 13 to transfer cold energy, and the upper end of the outer cover tube 4 can cooperate with the lower condensation fins 14 to transfer cold energy, so as to better cool and collect the vaporized materials.

[0067] Specifically, combined Figure 3 , Figure 4 As shown, the high-frequency coil 31, the induction heater 32 and the heat-insulating cover 33 are respectively provided with two independent parts corresponding to the upper material holding crucible 21 and the lower material receiving crucible 23, that is, the upper material holding crucible 21 is provided with a set of high-frequency coils 31, induction heaters 32 and heat-insulating covers 33, and the lower material receiving crucible 23 is provided with a set of high-frequency coils 31, induction heaters 32 and heat-insulating covers 33. The induction current is generated by the high-frequency coil 31, so that the induction heater 32 generates heat. The two high-frequency coils 31 can be independently adjusted to adjust the current, so as to adjust the temperature of the upper material holding crucible 21 and the lower material receiving crucible 23 respectively; the upper material holding crucible 21 needs to be heated to melt the material, and has a higher temperature, such as 450°C, while the lower material receiving crucible 23 only needs to be kept warm, and the required temperature is lower, such as 390°C.

[0068] The heating structure of the present invention adopts two-stage heating, the upper material holding crucible 21 is heated by the upper induction heater 32, and the lower material receiving crucible 23 is heated by the lower induction heater 32. The upper and lower heaters are heated independently, and the temperature is set independently, and the heating power of each area can be adjusted independently according to the state of the material.

[0069] When the material in the lower crucible 23 is cooled and solidified, a gradual cooling method from bottom to top is adopted. In addition to the above-mentioned method of using the crucible support 25 to provide cooling from the lower end, the current of the lower high-frequency coil 31 can also be adjusted to achieve this, for example, by reducing the power of the high-frequency coil; the axial position of the lower high-frequency coil 31 can also be adjusted to achieve this; the bottom of the lower crucible 23 is cooled and solidified first, and the solid-liquid interface gradually moves upward. This method can effectively gather impurity elements with a segregation coefficient less than 1 to the micro end, and can also effectively remove defects such as internal bubbles to ensure the consistency of the final ingot.

[0070] During the cooling process of the present invention, an inert cooling gas such as nitrogen is introduced into the reaction tube 1, and the power of the high-frequency coil 31 is reduced, and the crucible support 25 provides cooling from the bottom, so that the bottom is cooled and solidified first, and the solid-liquid interface gradually moves upward. This method can effectively gather impurity elements with a segregation coefficient less than 1 toward the micro end, and can also effectively eliminate defects such as internal bubbles, thereby ensuring the consistency of the final ingot.

[0071] Combination Figure 3 As shown, the outer cover tube 4 is provided with a vacuum air inlet 41, which is connected to a negative pressure source to evacuate the interlayer between the outer cover tube 4 and the reaction tube 1. During the heating process, the vacuum state between the outer cover tube 4 and the reaction tube 1 is maintained as much as possible, and no air conducts heat. In addition, the heat insulation reflective film on the inner surface of the heat insulation cover 33 is used to reduce heat conduction to the outside, so that more heat is applied to the reaction tube 1. Inert gas can also be flushed into the interlayer between the outer cover tube 4 and the reaction tube 1.

[0072] Specifically, a hydrogen sensor can be set in the interlayer between the outer cover tube 4 and the reaction tube 1. Since there is no hydrogen flowing between the outer cover tube 4 and the reaction tube 1, there is no hydrogen under normal circumstances. When cracks appear in the reaction tube 1, hydrogen leaks into the interlayer between the outer cover tube 4 and the reaction tube 1, and an alarm is given through the hydrogen sensor, and heating is stopped in time when hydrogen leaks. Since the interlayer between the outer cover tube 4 and the reaction tube 1 is in a vacuum negative pressure state and basically does not contain oxygen, even if hydrogen enters, it is not easy to explode, thereby improving the safety of the equipment.

[0073] A vacuum sensor can also be set in the interlayer between the outer cover tube 4 and the reaction tube 1. The vacuum sensor is used to detect whether the amount of air in the interlayer exceeds a set value. A decrease in the vacuum degree in the interlayer indicates that there is a leak in the outer cover tube 4 or the sealing structure, and heating needs to be stopped for treatment.

[0074] Specifically, the outer cover tube 4, the reaction tube 1 and the lower material receiving crucible 23 in the present invention are transparent devices made of quartz. The use of the quartz tube can increase the visualization of the internal chemical state, facilitate operation and observation, and can conveniently observe the real-time state of the internal material.

[0075] The present invention separates the internal material-making device (crucible assembly 2) of the reaction tube 1 from the external induction heating assembly 3. The sealing structures at both ends of the reaction tube 1 are simple and easy to disassemble, and can be directly connected to a clean area. When cleaning other internal structures, no pollution is caused to the internal pipelines. The upper material-holding crucible 21, the material-making funnel 22, and the lower material-receiving crucible 23 used for the material-making are made of quartz material and are easy to disassemble, which is convenient for subsequent wet chemical treatment and helps to improve the cleanliness of the material. In addition, the separation structure is conducive to the selection and combination of different materials. The interior of the reaction tube 1 is made of materials with high purity, and both ends can be connected to a clean area. The loading and unloading processes are all completed in the clean area; the disassembly and cleaning of the internal material-making structure are also completed in the clean area, further reducing the pollution caused by disassembly.

[0076] The crucible assembly 2 in the material-chemical area is a separated structure, which is conducive to the selection and combination of materials and the subsequent wet chemical cleaning; the induction heater 32 is placed in a vacuum state (or inert gas) in an independent area, and can use materials and metals with lower purity to reduce cost investment; the external heat insulation cover 33 is set with heat insulation reflective material to increase heating efficiency and adjustability.

[0077] A hydrogen detection structure is added between the outer cover tube 4 and the reaction tube 1 to increase the buffer zone and reduce the risk of hydrogen use. The whole is divided into two upper and lower crucibles, and is controlled by two independent heaters, with a high degree of freedom.

[0078] The above description of the disclosed embodiments enables one skilled in the art to implement or use the present invention. Various modifications to these embodiments will be apparent to one skilled in the art, and the general principles defined herein may be implemented in other embodiments without departing from the spirit or scope of the present invention. Therefore, the present invention will not be limited to the embodiments shown herein, but rather to the widest scope consistent with the principles and novel features disclosed herein.

Claims

1. A heating and chemical material device, characterized in that: It comprises a reaction tube (1), a crucible assembly (2), and an induction heating assembly (3), wherein the crucible assembly (2) is arranged inside the reaction tube (1); and the induction heating assembly (3) is arranged outside the reaction tube (1); The crucible assembly (2) comprises, from top to bottom, an upper material holding crucible (21), a material hopper (22), and a lower material receiving crucible (23); the upper material holding crucible (21) is used to hold materials to be heated; the lower material receiving crucible (23) can be separated separately from the crucible assembly (2); The induction heating component (3) is used to heat the upper material holding crucible (21) to melt the material in the upper material holding crucible (21), and the melted material flows into the lower material receiving crucible (23) through the material melting funnel (22); the induction heating component (3) is used to keep the melted material in the lower material receiving crucible (23) warm.

2. The heating and chemical material device according to claim 1, characterized in that: The lower end of the upper material holding crucible (21) is inserted into the material-forming hopper (22) to limit the circumferential position; a crucible support (24) is provided between the material-forming hopper (22) and the lower material-forming crucible (23), and the crucible support (24) supports the material-forming hopper (22) above the lower material-forming crucible (23).

3. The heating and chemical material device according to claim 2, characterized in that: The crucible support (24) comprises an upper support ring (241), support rods (242) and a lower support ring (243); the upper support ring (241) and the lower support ring (243) are fixedly supported by a plurality of support rods (242); The upper surface of the upper support ring (241) supports the lower surface of the material-forming funnel (22); and the bottom surface of the lower support ring (243) is provided with an annular groove (2431) for inserting the lower material receiving crucible (23).

4. The heating and chemical material device according to claim 1, characterized in that: An air inlet (11) is arranged at the upper end of the reaction tube (1), and an air outlet (12) is arranged at the lower end; the air inlet (11) is used to introduce hydrogen into the inner cavity of the reaction tube (1), and the air outlet (12) is used to discharge the hydrogen.

5. The heating and chemical material device according to claim 4, characterized in that: An upper condensation fin (13) is arranged at the upper part of the inner cavity of the reaction tube (1), and the hydrogen entering from the air inlet (11) can directly impact the upper condensation fin (13). The upper condensation fin (13) cooled by the hydrogen is used for condensing and depositing the vaporized material in the upper material holding crucible (21).

6. The heating and chemical material device according to claim 4 or 5, characterized in that: A lower condensation fin (14) is provided at the lower part of the inner cavity of the reaction tube (1), and the lower condensation fin (14) is used for condensing and depositing vaporized materials before they are discharged with the hydrogen.

7. The heating and chemical material device according to claim 6, characterized in that: The crucible assembly (2) comprises a crucible support (25), the upper end of the crucible support (25) being provided with a placement groove (251) for inserting the bottom of the lower material receiving crucible (23); The lower condensing fins (14) are arranged around the outside of the crucible support (25); a cooling channel (252) is arranged inside the crucible support (25), and the cooling channel (252) is used for allowing a cooling fluid to pass through, thereby cooling the bottom of the lower material receiving crucible (23) and the lower condensing fins (14).

8. The heating and chemical material device according to claim 1, characterized in that: It also includes an outer cover tube (4) which is arranged outside the reaction tube (1); The induction heating assembly (3) comprises a high-frequency coil (31), an induction heater (32) and a heat insulation cover (33); the high-frequency coil (31) is arranged outside the outer cover tube (4); the induction heater (32) and the heat insulation cover (33) are arranged in a sandwich layer between the reaction tube (1) and the outer cover tube (4); The heat insulation cover (33) is arranged on the outer surface of the reaction tube (1) and covers the outside of the induction heater (32); the inner surface of the heat insulation cover (33) is plated with a heat insulation reflective film; Alternatively, the induction heating component (3) is a resistance heater arranged in the interlayer between the outer cover tube (4) and the reaction tube (1).

9. The heating and chemical material device according to claim 8, characterized in that: The high-frequency coil (31), the induction heater (32) and the heat-insulating cover (33) are each provided with two independent parts corresponding to the upper material holding crucible (21) and the lower material receiving crucible (23), so as to adjust the temperature of the upper material holding crucible (21) and the lower material receiving crucible (23) respectively.

10. The heating and chemical material device according to claim 8, characterized in that: The outer cover tube (4) is provided with a vacuum air inlet (41), and the vacuum air inlet (41) is connected to a negative pressure source so as to evacuate the interlayer between the outer cover tube (4) and the reaction tube (1); and / or, a hydrogen sensor and / or a vacuum sensor is arranged in the interlayer between the outer cover tube (4) and the reaction tube (1); And / or, the outer cover tube (4), the reaction tube (1) and the lower material crucible (23) are transparent devices made of quartz.

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