Refractory metal crystal growth device

Abstract

The invention discloses a refractory metal crystal growth device, and relates to the technical field of metal crystal preparation devices, the refractory metal crystal growth device comprises a furnace body, the top of the furnace body is provided with a lifting control mechanism, the lifting end of the lifting control mechanism extends into the furnace body, and a high-temperature induction melting area is arranged in the furnace body and located below the lifting end of the lifting control mechanism; the temperature gradient forming area comprises a low-temperature area and a temperature control assembly, the low-temperature area is located in the furnace body, the top end of the low-temperature area corresponds to the bottom end of the high-temperature induction melting area, and the temperature control assembly is installed in the furnace body and used for monitoring and adjusting the temperature of the high-temperature induction melting area and the low-temperature area; the material placing pipe is detachably connected to the lifting end of the lifting control mechanism, and is driven by the lifting control mechanism to sequentially extend into the high-temperature induction melting area and the low-temperature area; through the arrangement of the high-temperature induction melting area and the low-temperature area, a large temperature gradient is formed, and accurate positioning of the material containing pipe between the high-temperature induction melting area and the low-temperature area is achieved.

Description

Technical Field

[0001] The present invention relates to the technical field of metal crystal preparation devices, and more particularly to a refractory metal crystal growth device. Background Art

[0002] Refractory metal crystals have broad application prospects in high-tech fields due to their unique physical and chemical properties. Refractory metal crystals usually refer to metals with a melting point higher than 2000°C, such as tungsten (W), molybdenum (Mo), tantalum (Ta), niobium (Nb), rhenium (Re) and their alloys. These metals have high melting points, high hardness, high density, good corrosion resistance and excellent electrical conductivity, and are important basic materials for manufacturing high-temperature alloys, superconducting materials, high-performance electrodes and coatings.

[0003] At present, the commonly used methods for growing refractory metal crystals include molten salt method, vapor deposition method and smelting method, among which induction melting method has unique advantages in the field of refractory metal crystal growth due to its advantages of high efficiency, energy saving and easy to achieve precise temperature control. Induction melting method uses the principle of electromagnetic induction to generate eddy currents in a metal crucible through high-frequency current, thereby achieving metal melting and heating. The growth of refractory metal crystals often needs to be carried out under a large temperature gradient to optimize the quality and performance of the crystal. However, the existing induction melting refractory metal crystal growth devices mostly rely on natural cooling, that is, air cooling, in terms of temperature gradient control. The temperature gradient formed is limited, and it is impossible to achieve precise control of the temperature gradient, which in turn affects the growth of the crystal.

[0004] Therefore, how to provide a refractory metal crystal growth device that can accurately control the temperature gradient while forming a large temperature gradient is a problem that technical personnel in this field urgently need to solve. Summary of the invention

[0005] In view of this, the present invention provides a refractory metal crystal growth device, aiming to solve the above-mentioned technical problems.

[0006] In order to achieve the above object, the present invention adopts the following technical solution:

[0007] A refractory metal crystal growth device, comprising:

[0008] A furnace body, wherein a lifting control mechanism is installed on the top of the furnace body, a lifting end of the lifting control mechanism extends into the interior of the furnace body, and a high-temperature induction melting zone is provided inside the furnace body and below the lifting end of the lifting control mechanism;

[0009] a temperature gradient forming zone, the temperature gradient forming zone comprising a low temperature zone and a temperature control component, the low temperature zone is located inside the furnace body, and its top corresponds to the bottom of the high temperature induction melting zone, the temperature control component is installed inside the furnace body, and is used to monitor and adjust the temperature of the high temperature induction melting zone and the low temperature zone;

[0010] A material placing pipe is detachably connected to the lifting end of the lifting control mechanism, and is driven by the lifting control mechanism to extend to the high-temperature induction melting zone and the low-temperature zone in sequence.

[0011] Through the above technical scheme, the present invention provides a refractory metal crystal growth device, which drives the feeding tube to melt in the high-temperature induction melting zone through the lifting control mechanism, and then drives the feeding tube to gradually descend to the low-temperature zone, thereby generating a large temperature difference, forming a large temperature gradient, and forming conditions suitable for crystal growth, thereby achieving precise positioning of the feeding tube between the high-temperature induction melting zone and the low-temperature zone, and through the adjustment of the temperature control component, forming precise control of the temperature gradient from the high-temperature induction melting zone to the low-temperature zone.

[0012] Preferably, in the above-mentioned refractory metal crystal growth device, the low temperature zone includes a support column and a low temperature chamber, the support column is fixed to the bottom of the furnace body, the low temperature chamber is a cylindrical structure and is fixed to the top surface of the support column, and an annular heat insulation board is fixed between the top of the low temperature chamber and the bottom of the high temperature induction melting zone. The support column provides physical support for the low temperature chamber, while the low temperature chamber provides an isolated environment for maintaining a stable temperature in the low temperature zone; the annular heat insulation board: located between the high temperature induction melting zone and the low temperature zone, effectively isolates heat transfer and maintains a temperature gradient, which is crucial for temperature control during crystal growth.

[0013] Preferably, in the above-mentioned refractory metal crystal growth device, the temperature control component includes a first thermocouple, a second thermocouple and a temperature measuring unit, the first thermocouple is embedded in the upper surface of the annular heat insulation board, and the second thermocouple is embedded in the lower surface of the annular heat insulation board; the temperature measuring unit is installed on the inner wall of the furnace body and is electrically connected to the first thermocouple and the second thermocouple through wires. The first thermocouple and the second thermocouple monitor the temperature of the high-temperature induction melting zone and the low-temperature zone respectively, and provide accurate temperature readings. The temperature measuring unit cooperates with the first thermocouple and the second thermocouple to realize real-time monitoring and processing of temperature data, thereby improving the accuracy and response speed of temperature control.

[0014] Preferably, in the above-mentioned refractory metal crystal growth device, the temperature control component further includes a refrigerator, the refrigerator is located outside the furnace body, and its outlet end is connected to the low-temperature chamber through a refrigerant transmission pipeline. The refrigerator provides a refrigerant, which is transmitted to the low-temperature chamber through a pipeline, effectively reducing the temperature of the low-temperature zone, enhancing the flexibility and accuracy of temperature control, and the refrigerant medium is liquid nitrogen.

[0015] Preferably, in the above-mentioned refractory metal crystal growth device, the high-temperature induction melting zone includes a graphite sleeve and an electromagnetic induction coil, the graphite sleeve is fixed inside the furnace body, and the electromagnetic induction coil is located outside the graphite sleeve. The magnetic field generated by the electromagnetic induction coil acts on the graphite sleeve, causing the graphite sleeve to heat up, and the graphite sleeve then transfers the heat to the feeding tube to melt the raw material inside the feeding tube; the graphite sleeve can conduct heat well and can also shield the eddy magnetic field generated by the induced current to reduce the disturbance to the raw material; if there is no graphite sleeve, the magnetic field generated by the electromagnetic induction coil can directly act on the raw material, so that the raw material is affected by the magnetic field and forms eddy currents, which is not conducive to the growth of single crystals after solidification due to the large internal stress.

[0016] Preferably, in the above-mentioned refractory metal crystal growth device, the electromagnetic induction coil is a copper tube coil, and its internal channel is used to circulate cooling medium. The thermal efficiency and stability of the electromagnetic induction coil are improved, and the design of circulating cooling medium effectively prevents the coil from overheating and prolongs the service life of the coil; the cooling medium can be cooling water.

[0017] Preferably, in the above-mentioned refractory metal crystal growth device, quartz wool is provided between the inner side of the electromagnetic induction coil and the outer side of the graphite sleeve, and a refractory brick shell is provided on the outer side of the electromagnetic induction coil, which provides additional heat insulation and protection, ensures the safety and durability of the electromagnetic induction coil in a high temperature environment, and also protects the furnace body from the influence of high temperature.

[0018] Preferably, in the above-mentioned refractory metal crystal growth device, an induction power supply is installed on the inner wall of the furnace body, and the induction power supply is electrically connected to the electromagnetic induction coil to provide a stable power supply for the electromagnetic induction coil to ensure continuous heating of the high-temperature induction melting zone.

[0019] Preferably, in the above-mentioned refractory metal crystal growth device, the feeding tube is a pointed cone-shaped corundum tube, and the top end of the pointed cone-shaped corundum tube is fastened to the lifting end of the lifting control mechanism through a vacuum joint. The pointed cone-shaped structure allows the crystal to grow in one direction, growing a crystal of a specific shape.

[0020] Preferably, in the above-mentioned refractory metal crystal growth device, an atmosphere control unit is also included, which is installed on the outside of the furnace body and connected to the connection interface of the vacuum joint through a connecting pipeline. The atmosphere control unit is connected to the connection interface of the vacuum joint through a connecting pipeline, and the air in the tapered corundum tube can be pumped out to form a vacuum; it can also control the inert gas connected to quantitatively fill the corundum tube, which is already in a vacuum environment, to provide a controllable atmosphere environment in the furnace and ensure the quality of refractory metal crystal growth; the atmosphere control unit serves as an atmosphere adjustment device, the connecting pipeline serves as a transmission channel, and the vacuum joint serves as a connection interface, which together realize the precise control and adjustment of the atmosphere in the furnace.

[0021] It can be seen from the above technical solutions that, compared with the prior art, the present invention discloses a refractory metal crystal growth device, which has the following beneficial effects:

[0022] 1. The present invention realizes the continuous process from melting to crystal growth of refractory metals through the cooperation of the high-temperature induction melting zone and the temperature gradient forming zone, thereby improving the efficiency of crystal growth.

[0023] 2. The present invention ensures the temperature stability of the melting zone and the low-temperature zone through the precise monitoring and adjustment function of the temperature control component, providing a suitable temperature environment for crystal growth. At the same time, through the monitoring of the first thermocouple and the second thermocouple, and the cooperation of the temperature measuring unit and the refrigerator, the temperature of the high-temperature induction melting zone and the low-temperature zone is precisely controlled, forming a suitable temperature gradient, which is conducive to the crystal growth of refractory metals. BRIEF DESCRIPTION OF THE DRAWINGS

[0024] 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 embodiments of the present invention. For ordinary technicians in this field, other drawings can be obtained based on the provided drawings without paying creative work.

[0025] Figure 1 The accompanying drawing is a schematic structural diagram of a refractory metal crystal growth device provided by the present invention.

[0026] in:

[0027] 1-furnace body;

[0028] 2-Lifting control mechanism;

[0029] 21-lifting end;

[0030] 3-High temperature induction melting zone;

[0031] 31-graphite sleeve; 32-electromagnetic induction coil;

[0032] 4- low temperature zone;

[0033] 41-support column; 42-low temperature chamber;

[0034] 5- Temperature control component;

[0035] 51-first thermocouple; 52-second thermocouple; 53-temperature measuring unit; 54-refrigerating machine; 55-refrigerant transmission pipeline;

[0036] 6-feeding tube;

[0037] 7- Inductive power supply;

[0038] 8- Vacuum connector;

[0039] 9-Control module. DETAILED DESCRIPTION

[0040] The following will be combined with the drawings in the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. 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.

[0041] See attached Figure 1 , the embodiment of the present invention discloses a refractory metal crystal growth device, comprising:

[0042] A furnace body 1, a lifting control mechanism 2 is installed on the top of the furnace body 1, a lifting end 21 of the lifting control mechanism 2 extends into the furnace body 1, and a high-temperature induction melting zone 3 is provided inside the furnace body 1 and below the lifting end 21 of the lifting control mechanism 2;

[0043] The temperature gradient forming zone includes a low temperature zone 4 and a temperature control component 5. The low temperature zone 4 is located inside the furnace body 1, and its top corresponds to the bottom of the high temperature induction melting zone 3. The temperature control component 5 is installed inside the furnace body 1 to monitor and adjust the temperature of the high temperature induction melting zone 3 and the low temperature zone 4;

[0044] The material placing pipe 6 is detachably connected to the lifting end 21 of the lifting control mechanism 2 , and driven by the lifting control mechanism 2 , extends to the high-temperature induction melting zone 3 and the low-temperature zone 4 in sequence.

[0045] In order to further optimize the above technical solution, the lifting end 21 is a multi-stage lifting rod, which is driven by the lifting control mechanism to realize the step-by-step lifting of the multi-stage lifting rod; in this embodiment, the lifting end 21 includes a first-stage lifting rod 211 and a second-stage lifting rod 212; the first-stage lifting rod 211 and the second-stage lifting rod 212 are both hollow rods, and the driving shaft for driving the first-stage lifting rod 211 and the second-stage lifting rod 212 is also set to a hollow structure, and a vacuum bellows is installed inside it, and a vacuum flange structure is installed at the end of the second-stage lifting rod 212, and one end of the vacuum flange structure It is connected to the vacuum bellows located inside the driving shaft, the first-stage lifting rod 211 and the second-stage lifting rod 212, and the other end is connected to the vacuum joint 8. The atmosphere control unit realizes the vacuum environment inside the pointed conical corundum tube through the vacuum bellows, and can also control the access to inert gas to quantitatively fill the pointed conical corundum tube in the vacuum environment. That is, the gas is transported through the gas path bellows and finally reaches the vacuum joint of the pointed conical corundum tube and enters the inside of the pointed conical corundum tube. The purpose of this structural setting is to ensure the sealing performance of the overall structure and to ensure the stability and continuity of the gas supply.

[0046] In order to further optimize the above technical solution, the low temperature zone 4 includes a support column 41 and a low temperature chamber 42. The support column 41 is fixed to the bottom of the furnace body 1. The low temperature chamber 42 is a cylindrical structure and is fixed to the top surface of the support column 41. An annular heat insulation plate is fixed between the top of the low temperature chamber 42 and the bottom end of the high temperature induction melting zone 3.

[0047] In order to further optimize the above technical solution, the temperature control component 5 includes a first thermocouple 51, a second thermocouple 52 and a temperature measuring unit 53. The first thermocouple 51 is embedded in the upper surface of the annular insulation board, and the second thermocouple 52 is embedded in the lower surface of the annular insulation board; the temperature measuring unit 53 is installed on the inner wall of the furnace body 1, and is electrically connected to the first thermocouple 51 and the second thermocouple 52 through wires.

[0048] In order to further optimize the above technical solution, the temperature control component 5 also includes a refrigerator 54 , which is located outside the furnace body 1 , and an outlet end of the refrigerator 54 is connected to the low-temperature chamber 42 through a refrigerant transmission pipeline 55 .

[0049] In order to further optimize the above technical solution, the high temperature induction melting zone 3 includes a graphite sleeve 31 and an electromagnetic induction coil 32 . The graphite sleeve 31 is fixed inside the furnace body 1 , and the electromagnetic induction coil 32 is located outside the graphite sleeve 31 .

[0050] In order to further optimize the above technical solution, the electromagnetic induction coil 32 is a copper tube coil, and its internal channel is used for circulating cooling medium.

[0051] In order to further optimize the above technical solution, quartz wool is provided between the inner side of the electromagnetic induction coil 32 and the outer side of the graphite sleeve 31 , and a refractory brick shell is provided on the outer side of the electromagnetic induction coil 32 .

[0052] In order to further optimize the above technical solution, an induction power supply 7 is installed on the inner wall of the furnace body 1 , and the induction power supply 7 is electrically connected to the electromagnetic induction coil 32 .

[0053] In order to further optimize the above technical solution, the placing tube 6 is a pointed conical corundum tube, and the top end of the pointed conical corundum tube is fastened to the lifting end 21 of the lifting control mechanism 2 through a vacuum joint 8.

[0054] In order to further optimize the above technical solution, an atmosphere control unit is also included. The atmosphere control unit is installed on the outside of the furnace body 1 and can also be directly connected to the connection interface of the vacuum joint 8 through a connecting pipeline to achieve a vacuum environment inside the tapered corundum tube and the filling of inert gas.

[0055] In order to further optimize the above technical solution, a control module 9 is also included which is installed on the outside of the furnace body 1. The control module 9 is used to control the operation of the above components and the adjustment of different parameters, such as the lifting speed of the lifting control mechanism 2, the temperature control of the amount of liquid nitrogen introduced into the refrigerator 54 and the flow rate, the flow rate / amount of inert gas introduced into the atmosphere control unit, the heating temperature of the electromagnetic induction coil 32, etc.

[0056] The embodiments of the present invention are:

[0057] The metal to be grown is placed inside the feeding tube 6, which is connected to the control end of the lifting control mechanism through the vacuum joint 8, and the lifting end 21 of the lifting control mechanism 2 is controlled to descend through the control module 9, and the feeding tube containing the metal to be grown is transported to the high-temperature induction melting zone 3 for melting, and then the lifting end 21 of the lifting control mechanism 2 is controlled to slowly descend to the low-temperature chamber 42, and enters the low-temperature chamber 42 from the high-temperature induction melting zone 3, thereby generating a huge temperature gradient, which is more suitable for the growth of material crystals.

[0058] In this specification, each embodiment is described in a progressive manner, and each embodiment focuses on the differences from other embodiments. The same or similar parts between the embodiments can be referred to each other. For the device disclosed in the embodiment, since it corresponds to the method disclosed in the embodiment, the description is relatively simple, and the relevant parts can be referred to the method part.

[0059] 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 refractory metal crystal growth device, characterized in that: include: A furnace body (1), a lifting control mechanism (2) is installed on the top of the furnace body (1), a lifting end (21) of the lifting control mechanism (2) extends into the interior of the furnace body (1), and a high-temperature induction melting zone (3) is provided inside the furnace body (1) and below the lifting end (21) of the lifting control mechanism (2); a temperature gradient forming zone, the temperature gradient forming zone comprising a low temperature zone (4) and a temperature control component (5), the low temperature zone (4) being located inside the furnace body (1), and the top end of the low temperature zone (4) corresponding to the bottom end of the high temperature induction melting zone (3), the temperature control component (5) being installed inside the furnace body (1) and used for monitoring and adjusting the temperature of the high temperature induction melting zone (3) and the low temperature zone (4); A material placing pipe (6), wherein the material placing pipe (6) is detachably connected to a lifting end (21) of the lifting control mechanism (2), and is driven by the lifting control mechanism (2) to sequentially extend to the inside of the high-temperature induction melting zone (3) and the low-temperature zone (4).

2. A refractory metal crystal growth device according to claim 1, characterized in that: The low temperature zone (4) comprises a support column (41) and a low temperature chamber (42), wherein the support column (41) is fixed to the bottom of the furnace body (1), the low temperature chamber (42) is a cylindrical structure and is fixed to the top surface of the support column (41), and an annular heat insulation plate is fixed between the top end of the low temperature chamber (42) and the bottom end of the high temperature induction smelting zone (3).

3. A refractory metal crystal growth device according to claim 2, characterized in that: The temperature control component (5) comprises a first thermocouple (51), a second thermocouple (52) and a temperature measuring unit (53); the first thermocouple (51) is embedded in the upper surface of the annular heat insulation board, and the second thermocouple (52) is embedded in the lower surface of the annular heat insulation board; the temperature measuring unit (53) is installed on the inner wall of the furnace body (1) and is electrically connected to the first thermocouple (51) and the second thermocouple (52) respectively through wires.

4. A refractory metal crystal growth device according to claim 2, characterized in that: The temperature control component (5) also includes a refrigerator (54), which is located outside the furnace body (1) and has an outlet end connected to the low-temperature chamber (42) via a refrigerant transmission pipeline (55).

5. The refractory metal crystal growth device according to claim 1, characterized in that: The high-temperature induction melting zone (3) comprises a graphite sleeve (31) and an electromagnetic induction coil (32); the graphite sleeve (31) is fixed inside the furnace body (1), and the electromagnetic induction coil (32) is located outside the graphite sleeve (31).

6. A refractory metal crystal growth device according to claim 5, characterized in that: The electromagnetic induction coil (32) is a copper tube coil, and its internal channel is used for circulating cooling medium.

7. A refractory metal crystal growth device according to claim 6, characterized in that: Quartz wool is provided between the inner side of the electromagnetic induction coil (32) and the outer side of the graphite sleeve (31), and a refractory brick shell is provided on the outer side of the electromagnetic induction coil (32).

8. The refractory metal crystal growth device according to claim 6, characterized in that: An induction power source (7) is installed on the inner wall of the furnace body (1), and the induction power source (7) is electrically connected to the electromagnetic induction coil (32).

9. The refractory metal crystal growth device according to claim 1, characterized in that: The material placement tube (6) is a pointed conical corundum tube, and the top end of the pointed conical corundum tube is fastened to the lifting end (21) of the lifting control mechanism (2) via a vacuum joint (8).

10. The refractory metal crystal growth device according to claim 9, characterized in that: It also comprises an atmosphere control unit, which is installed on the outside of the furnace body (1) and is connected to the connection interface of the vacuum joint (8) through a connecting pipeline.

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