Composite degassing and impurity removal device and high-purity aluminum alloy melt composite degassing and impurity removal method using same

Abstract

The invention relates to a composite degassing and impurity removing device and a high-purity aluminum alloy melt composite degassing and impurity removing method using the same. The composite gas and impurity removal device comprises a furnace body, a rotary injection assembly, at least two ultrasonic assemblies, an inert gas supply part and a vacuum system, the rotary blowing assembly is arranged in the center of the top of the furnace body; a rotating rod of the rotary blowing assembly vertically downwards extends into the furnace body from the outside of the furnace body; a gas conveying channel is arranged in the rotating rod; the ultrasonic assemblies are uniformly arranged on the peripheral side of the rotary blowing part; a vibration part of the ultrasonic assembly vertically downwards extends into the furnace body from the outside of the furnace body; the inert supply part and the vacuum system are communicated with the interior of the furnace body; efficient removal of hydrogen and oxygen in the high-purity aluminum alloy melt is achieved, the hydrogen content is preferably as low as 0.251 mL / Kg or below, and the oxygen content is preferably as low as 0.490 mL / Kg or below; and the problem of poor gas and impurity removal effect caused by introduction of new impurities is avoided.

Description

Technical Field

[0001] The present invention relates to the technical field of aluminum alloy purification, and particularly relates to a composite degassing and impurity removing device and a method for composite degassing and impurity removing of high-purity aluminum alloy melt using the same. Background Art

[0002] Aluminum has advantages such as being easy to deposit, having good etching and processing properties, high electrical conductivity, good thermal conductivity, good adhesion and bonding properties with the substrate, and low cost. Above the 90nm technology node in integrated circuit manufacturing, it is the main interconnection material and also has extensive applications in advanced packaging. As the main material for metal interconnections in integrated circuit manufacturing, the quality of ultra-high-purity aluminum alloy is crucial for the sputtering efficiency of the target and the quality of the deposited thin film during magnetron sputtering. However, molten aluminum alloy continuously generates H2 when contacting raw materials and moisture in the air. As the temperature of the aluminum alloy melt continues to drop and solidifies, its ability to dissolve hydrogen greatly decreases, and the excess hydrogen precipitates from the ingot to form pinhole defects on the ingot surface and looseness inside the ingot, seriously affecting the quality of the aluminum alloy ingot.

[0003] To obtain high-quality aluminum alloy ingots, degassing and purifying the aluminum alloy melt is an essential step. The existing degassing processes are relatively single, including degassing with refining agents, rotary spraying degassing, vacuum degassing, and ultrasonic degassing. There are problems such as introducing impurity elements during the degassing process, poor degassing effect on the aluminum alloy melt at the lower part of the crucible, and inability to eliminate composition segregation. A single degassing process will make the hydrogen content in the aluminum alloy ingot unstable and cannot meet the high requirements of high-purity aluminum alloy melt.

[0004] For example, CN117701935A discloses a purification process for aluminum alloy melt for degassing and slag removal. After adding a refining agent to the inside of the melt and stirring, the hydrogen inside the melt is removed, and then by adding a slag removal agent to the inside of the melt, the impurities inside the melt are removed. New impurity elements are easily introduced during the process of adding the refining agent and the slag removal agent, resulting in the degassing and slag removal effect not meeting the production requirements of ultra-high-purity aluminum alloy.

[0005] CN117448589A discloses an aluminum alloy refining process based on ultrasonic degassing. After skimming the slag from the melted aluminum alloy liquid after smelting, it is introduced into an on-line degassing furnace, and then an ultrasonic horn array is inserted into the aluminum alloy liquid in the on-line degassing furnace to perform ultrasonic degassing treatment on the aluminum alloy liquid after skimming the slag. However, the degassing and impurity removal effect of this process still has great room for improvement, and it cannot eliminate the problem of composition segregation, resulting in poor quality of the obtained aluminum alloy ingot.

[0006] Therefore, how to develop a new degassing and impurity removing device and method to efficiently remove gas elements such as hydrogen and oxygen and other impurities dissolved in high-purity aluminum alloy melt is an urgent problem to be solved in the field at present. Summary of the invention

[0007] In order to solve the above technical problems, the present invention provides a composite degassing and impurity removal device and a high-purity aluminum alloy melt composite degassing and impurity removal method using the same, which can efficiently remove gas elements such as hydrogen and oxygen and other impurities dissolved in the high-purity aluminum alloy melt, thereby solving the problem of poor quality of aluminum alloy ingots caused by the poor degassing and impurity removal effect of the single degassing and impurity removal process in the prior art, and meeting the production needs of high-purity aluminum alloy ingots for semiconductor sputtering targets.

[0008] To achieve this object, the present invention adopts the following technical solutions:

[0009] In a first aspect, the present invention provides a composite degassing and impurity removal device, the composite degassing and impurity removal device comprising a furnace body, a rotary spraying component, at least two ultrasonic components, an inert gas supply component and a vacuum system;

[0010] The rotary blowing assembly is arranged at the center of the top of the furnace body; the rotating rod of the rotary blowing assembly extends vertically downward from the outside of the furnace body to the inside of the furnace body; a gas delivery channel is arranged inside the rotating rod;

[0011] The ultrasonic components are evenly arranged around the rotating spraying component; the vibration component of the ultrasonic component extends vertically downward from the outside of the furnace body to the inside of the furnace body;

[0012] The inert supply component and the vacuum system are in communication with the interior of the furnace body.

[0013] The composite degassing and impurity removal device of the present invention is mainly used for degassing and impurity removal of high-purity alloy melts, such as high-purity aluminum alloy melts.

[0014] The present invention integrates a rotary spraying component, an ultrasonic component and a vacuum system, and the three work in conjunction with each other. Fine inert gas bubbles formed by rotary spraying with the assistance of ultrasound evenly enter the high-purity alloy melt, so that the inert gas bubbles are efficiently combined with hydrogen, oxygen and other impurities in the high-purity alloy melt to remove the corresponding elements. The vacuum system is combined to perform vacuum standing to inhibit the dissolution of hydrogen and oxygen gases, promote gas discharge, further improve the degassing and impurity removal effect, and more fully absorb hydrogen, oxygen and inclusions. The entire process is short and the required equipment is simple. There is no need to introduce refining agents and slag removal agents, which avoids the introduction of impurity elements and reduces the processing cost.

[0015] Preferably, a rotor is provided at the bottom of the rotating rod.

[0016] Preferably, a first motor is connected to the top of the rotating rod.

[0017] Preferably, a protective component is provided on the outer side of the rotating rod.

[0018] Preferably, a first air guide port is provided on the protection component, and the first air guide port communicates with the gas delivery channel of the rotating rod.

[0019] In the present invention, the rotary spraying and blowing assembly drives the rotating rod and the rotor to rotate through a first motor, and forms bubbles of inert gas in the gas delivery channel into the high-purity alloy melt, combines with dissolved gas elements such as hydrogen and oxygen and other impurities, and then carries them out of the high-purity alloy melt, so as to achieve degassing and impurity removal.

[0020] Preferably, the ultrasonic assembly further includes an ultrasonic generating component and an ultrasonic adjusting component.

[0021] Preferably, the ultrasonic adjusting component and the ultrasonic generating component are sequentially arranged from top to bottom on the vibration component near the top inside the furnace body.

[0022] Preferably, a sealing component is provided between the ultrasonic adjusting component and the top inside the furnace body.

[0023] Preferably, the sealing component includes a rubber sealing ring.

[0024] The present invention preferably provides the sealing component, so that the inside of the furnace body is a closed environment, effectively reducing the entry of the external environment into the furnace body. Combined with the rotary spraying and blowing assembly, the ultrasonic assembly and the vacuum system, the inert gas bubbles are finer and more uniform, the residence time in the high-purity alloy melt is increased, and it is more effective to contact with hydrogen, oxygen and inclusions in the melt, thereby improving the degassing and impurity removal efficiency; at the same time, the closed environment can also reduce heat loss.

[0025] Preferably, outside the furnace body, a second motor, an output shaft and a signal adjusting plate are arranged on the ultrasonic assembly from top to bottom.

[0026] Preferably, the vacuum system includes a mechanical pump and a molecular pump.

[0027] The present invention further preferably provides that the vacuum system includes a mechanical pump and a molecular pump, and the two work together to quickly reach a high vacuum state inside the furnace body, shortening the degassing and impurity removal time.

[0028] Preferably, the intake valve of the mechanical pump is connected to the inside of the furnace body through a second air guide port.

[0029] Preferably, the exhaust valve of the mechanical pump is connected to the molecular pump through a gas pipe.

[0030] The molecular pump in the composite degassing and impurity removal device of the present invention needs to be preheated in advance.

[0031] Preferably, the inert gas supply component is connected to the first air guide port and the second air guide port through a gas pipe.

[0032] Preferably, heating components are provided on the inner side and the bottom of the furnace body.

[0033] The present invention further preferably provides that heating components are provided on the inner side and the bottom of the furnace body, aiming to ensure that the melting temperature of the high-purity aluminum alloy melt is maintained during the degassing and impurity removal process, always in a molten state, and prevent cooling and solidification.

[0034] Preferably, a fluid channel communicating with the outside of the furnace body is provided at the bottom of the furnace body.

[0035] Preferably, a blocking component is provided in the fluid channel.

[0036] In the present invention, a blocking component is provided in the fluid channel. The blocking component blocks the fluid channel during the degassing and impurity removal process to ensure a closed environment. After the degassing and impurity removal, the blocking component is removed, so that the high-purity alloy melt flows out from the fluid channel.

[0037] In a second aspect, the present invention provides a composite degassing and impurity removal method for a high-purity aluminum alloy melt, and the composite degassing and impurity removal method is carried out by using the composite degassing and impurity removal device described in the first aspect.

[0038] The composite degassing and impurity removal method for a high-purity aluminum alloy melt of the present invention combines the three processes of rotary spraying, ultrasonic assistance, and vacuum standing by using the composite degassing and impurity removal device described in the first aspect, efficiently removes hydrogen, oxygen, and other inclusions in the high-purity aluminum alloy melt, successfully obtains high-quality high-purity aluminum alloy ingots, provides high-quality target materials for the semiconductor sputtering field, and the composite degassing and impurity removal method has a simple process flow, does not require adding refining agents and slag removal agents, avoids introducing new impurities, and greatly reduces the cost.

[0039] Preferably, the composite degassing and impurity removal method includes the following steps:

[0040] (1) Place the high-purity aluminum alloy melt in the furnace body, evacuate the furnace body to a vacuum environment, and then fill it with an inert gas;

[0041] (2) Under ultrasonic assistance, inject the inert gas bubbles formed by rotary spraying into the high-purity aluminum alloy melt described in step (1) for the first degassing and impurity removal;

[0042] (3) The high-purity aluminum alloy melt after the first degassing in step (2) is subjected to a second degassing and impurity removal by vacuum standing to obtain an ultra-high-purity aluminum alloy melt.

[0043] Preferably, the purity of the high-purity aluminum alloy melt in step (1) is ≥4N8, and for example, it can be 4N8, 5N, 5N5, 5N8, or 6N, etc.

[0044] Preferably, the degree of vacuum in the vacuum environment in step (1) is 100 - 300 Pa, for example, it can be 100 Pa, 120 Pa, 150 Pa, 180 Pa, 200 Pa, 220 Pa, 250 Pa, 280 Pa or 300 Pa, etc.

[0045] The present invention further preferably sets the degree of vacuum in the vacuum environment in step (1) to be 100 - 300 Pa, which is beneficial to exhausting the air in the furnace body, thereby avoiding elements such as hydrogen and oxygen in the air from redissolving into the ultra-high purity aluminum alloy melt and increasing the subsequent burden of degassing and impurity removal.

[0046] Preferably, in step (1), an inert gas is filled until the air pressure in the furnace body is 100 kPa - 105 kPa, for example, it can be 100 kPa, 101 kPa, 102 kPa, 103 kPa, 104 kPa or 105 kPa, etc.

[0047] Preferably, the inert gas in step (1) includes argon and / or nitrogen, and is preferably argon.

[0048] In the composite degassing and impurity removal method of the present invention, step (1) can be repeated multiple times until the air in the furnace body is exhausted and filled with an inert gas until the air pressure inside the furnace body returns to about 1 standard atmospheric pressure.

[0049] Preferably, when performing the rotary injection in step (2), the rotational speed of the rotor is 200 - 500 r / min, for example, it can be 200 r / min, 250 r / min, 300 r / min, 350 r / min, 400 r / min, 450 r / min or 500 r / min, etc.

[0050] The present invention further preferably sets the rotational speed of the rotor to be 200 - 500 r / min when performing the rotary injection in step (2), which is beneficial to fully converting the inert gas into inert gas bubbles, so as to enter the ultra-high purity aluminum alloy melt and combine with the dissolved hydrogen, oxygen and other inclusions therein to achieve the degassing and impurity removal effect; if the rotational speed of the rotor is too low during the rotary injection, it will cause the inert gas bubbles to be too large, so that they will quickly escape from the aluminum alloy melt, and the surface area of the too-large inert gas bubbles will be reduced comprehensively, and the ability to adsorb gas will also be weakened, resulting in a reduction in the degassing and impurity removal efficiency; if the rotational speed of the rotor is too high during the rotary injection, a funnel-shaped depression will appear near the rotating graphite rod, resulting in the coalescence of the floating bubbles and weakening the degassing and impurity removal effect. At the same time, it is very likely to cause splashing of the aluminum liquid and affect the safety of the equipment.

[0051] Preferably, when performing the rotary injection in step (2), the gas flow rate of the inert gas is 3 - 6 m 3 / h, for example, it can be 3 m 3 / h, 3.5 m3 / h, 4 m 3 / h, 4.5 m 3 / h, 5 m 3 / h, 5.5 m 3 / h or 6 m 3 / h, etc.

[0052] Preferably, the ultrasonic power of the ultrasonic assistance in step (2) is 500 - 1500 W, for example, it can be 500 W, 700 W, 900 W, 1100 W, 1300 W or 1500 W, etc., and preferably it is 800 - 1200 W.

[0053] The present invention further preferably has the ultrasonic power of the ultrasonic assistance in step (2) being 800 - 1200 W, which is beneficial to the fragmentation and refinement of the inert gas bubbles, thereby increasing the total surface area of the bubbles, providing a larger area for gases such as hydrogen and impurities to adsorb, and at the same time diffusing the bubbles to various positions of the high-purity aluminum alloy melt, that is, the bubbles are more dispersed, and the degassing and impurity removal effects are better; in addition, cavitation bubbles will be generated in the aluminum alloy melt during the ultrasonic assistance process, and some cavitation bubbles will collapse in a short time, and during this process, the diffusion of "H atoms / ions", etc. into the inert gas bubbles will be accelerated; and some non-collapsed cavitation bubbles will carry "H atoms / ions" into the inert gas bubbles, causing the bubbles to grow and float out from the surface of the aluminum alloy melt; if the ultrasonic power is too low, the ultrasonic cavitation effect will be low, and its promoting effect on the combined degassing is limited, resulting in poor combined degassing and impurity removal effects; if the ultrasonic power is too high, the non-collapsed cavitation bubbles will decrease, reducing the degassing and impurity removal efficiency.

[0054] Preferably, the ultrasonic frequency of the ultrasonic assistance in step (2) is 15 KHz - 25 KHz, for example, it can be 15 KHz, 18 KHz, 20 KHz, 22 KHz or 25 KHz, etc.

[0055] Preferably, the time for the first degassing and impurity removal in step (2) is 20 - 50 min, for example, it can be 20 min, 25 min, 30 min, 35 min, 40 min, 45 min or 50 min, etc.

[0056] Preferably, the vacuum degree of the vacuum static state in step (3) is 10 - 50 Pa, for example, it can be 10 Pa, 15 Pa, 20 Pa, 25 Pa, 30 Pa, 35 Pa, 40 Pa, 45 Pa or 50 Pa, etc.

[0057] The present invention further preferably has the vacuum degree of the vacuum static state in step (3) being 10 - 50 Pa, which is beneficial to the desorption and precipitation of hydrogen dissolved in the aluminum alloy melt; if the vacuum degree of the vacuum static state is too high, the hydrogen partial pressure in the aluminum alloy melt will be high, reducing the degassing efficiency.

[0058] Preferably, the time for the second degassing and impurity removal in step (3) is 10 - 40 min, for example, it can be 10 min, 15 min, 20 min, 25 min, 30 min, 35 min or 40 min, etc., and preferably 20 - 40 min.

[0059] The present invention further preferably sets the time for the second degassing and impurity removal in step (3) (i.e., the time for the vacuum static state) to be 20 - 40 min, which is beneficial for gas to escape from the aluminum alloy melt. If the time for the second degassing and impurity removal is too short, the degassing and impurity removal effect will become poor; if the time for the second degassing and impurity removal is too long, the production efficiency will become low.

[0060] It should be noted that during the vacuum static state of the present invention, the desorption and precipitation of hydrogen and oxygen are not instantaneously completed, mainly including three stages: (1) Diffusion of hydrogen: Hydrogen atoms inside the aluminum alloy melt diffuse towards the surface or the bubble interface; (2) Nucleation and growth of bubbles: Hydrogen molecules form bubbles under low pressure and gradually grow; (3) Floating and escaping of bubbles: Bubbles float and escape from the aluminum alloy melt.

[0061] As a further preferred technical solution of the present invention, the composite degassing and impurity removal method includes the following steps:

[0062] (1) Place a high-purity aluminum alloy melt with a purity ≥ 4N8 in the furnace body, and after pumping the inside of the furnace body to a vacuum environment with a vacuum degree of 100 - 300 Pa, fill it with an inert gas until the air pressure inside the furnace body is 100 kPa - 105 kPa;

[0063] (2) Under the ultrasonic assistance with an ultrasonic power of 500 - 1500 W and an ultrasonic frequency of 15 - 25 KHz, inject the inert gas bubbles formed by rotary spraying into the high-purity aluminum alloy melt in step (1) for the first degassing and impurity removal for 20 - 50 min; when rotary spraying, the rotation speed of the rotor is 200 - 500 r / min, and the gas flow rate of the inert gas during rotary spraying is 3 - 6 m 3 / h;

[0064] (3) The high-purity aluminum alloy melt after the first degassing in step (2) is subjected to the second degassing and impurity removal for 10 - 40 min through vacuum static state under a vacuum degree of 10 - 50 Pa to obtain an ultra-high-purity aluminum alloy melt.

[0065] Compared with the prior art, the present invention has at least the following beneficial effects:

[0066] (1) The composite degassing and impurity removal device provided by the present invention combines a rotary spraying component, an ultrasonic component and a vacuum system, and the three work in conjunction with each other, and combined with a highly closed and sealed environment, it can efficiently remove hydrogen, oxygen and other inclusions in a high-purity alloy melt. At the same time, after the degassing is completed, the alloy slag remains at the bottom of the furnace and is easy to remove. In addition, the composite degassing and impurity removal device has a simple structure, is easy to operate, and has strong applicability.

[0067] (2) The composite degassing and impurity removal method for high-purity aluminum alloy melt provided by the present invention is carried out using the composite degassing and impurity removal device described in the first aspect, and rotary blowing is performed under the assistance of ultrasound to perform the first degassing and impurity removal, and then the second degassing and impurity removal is performed in combination with vacuum standing, so as to achieve efficient removal of hydrogen and oxygen in the high-purity aluminum alloy melt. The hydrogen content in the product is preferably as low as below 0.251 mL / Kg, and the oxygen content is preferably as low as below 0.490 mL / Kg, thereby meeting the production requirements of high-purity aluminum alloy melt for semiconductor sputtering target ingots. BRIEF DESCRIPTION OF THE DRAWINGS

[0068] Figure 1 1 is a schematic diagram of the front view of the structure of the composite degassing and impurity removal device for high-purity aluminum alloy melt provided in Example 1 of the present invention;

[0069] Figure 2 1 is a schematic side view of the structure of a composite degassing and impurity removal device for a high-purity aluminum alloy melt provided in Example 1 of the present invention;

[0070] Figure 3 1 is a schematic diagram of the top view of the structure of the composite degassing and impurity removal device for high-purity aluminum alloy melt provided in Example 1 of the present invention;

[0071] In the figure: 1. furnace body; 2. rotary blowing assembly; 21. rotating rod; 22. rotor; 23. protective sleeve; 24. first motor; 25. first air inlet; 3. ultrasonic assembly; 31. first vibration rod; 32. ultrasonic generator; 33. ultrasonic regulator; 34. signal adjustment board; 35. output shaft; 36. second motor; 4. argon gas bottle; 5. heating assembly; 6. air pipe; 7. rubber sealing ring; 8. blocking ring; 9. fluid channel; 10. mechanical pump; 11. exhaust valve; 12. second air inlet; 13. molecular pump. DETAILED DESCRIPTION

[0072] The technical solution of the present invention is further described below in conjunction with the accompanying drawings and through specific implementation methods. However, the following examples are only simplified examples of the present invention and do not represent or limit the scope of protection of the present invention. The scope of protection of the present invention shall be subject to the claims.

[0073] In the composite degassing and impurity removal method described in the following embodiment, the high-purity aluminum alloy melt in step (1) is placed in a graphite crucible and then placed in the furnace body.

[0074] 1. Embodiment

[0075] Embodiment 1

[0076] This embodiment provides a composite degassing and impurity removal device, as Figures 1 to 3 shown. The composite degassing and impurity removal device includes a furnace body 1, a rotary injection assembly 2, two ultrasonic assemblies 3, an argon gas cylinder 4, and a vacuum system;

[0077] The rotary injection assembly 2 is arranged at the central position on the top of the furnace body 1; the rotating rod 21 of the rotary injection assembly 2 extends vertically downward from the outside of the furnace body 1 to the inside of the furnace body 1; a gas delivery channel is arranged inside the rotating rod 21; a rotor 22 is arranged at the bottom of the rotating rod 21; the top of the rotating rod 21 is connected to a first motor 24; a protective sleeve 23 is arranged outside the rotating rod 21; a first air guide port 25 is arranged on the protective component, and the first air guide port 25 communicates with the gas delivery channel of the rotating rod 21;

[0078] The ultrasonic assemblies 3 are evenly arranged on the periphery of the rotary injection component; the vibrating rods of the ultrasonic assemblies 3 extend vertically downward from the outside of the furnace body 1 to the inside of the furnace body 1; the ultrasonic assembly 3 further includes an ultrasonic generator 32 and an ultrasonic regulator 33; the ultrasonic regulator 33 and the ultrasonic generator 32 are arranged on the vibrating rod near the inner top of the furnace body 1 in sequence from top to bottom; a rubber sealing ring 7 is arranged between the ultrasonic regulator 33 and the inner top of the furnace body 1; outside the furnace body 1, the ultrasonic assemblies 3 are provided with a second motor 36, an output shaft 35, and a signal regulating plate 34 from top to bottom;

[0079] The argon gas cylinder 4 and the vacuum system are connected to the inside of the furnace body 1; the vacuum system includes a mechanical pump 10 and a molecular pump 13; the intake valve of the mechanical pump 10 is connected to the inside of the furnace body 1 through a second air guide port 12; the exhaust valve 11 of the mechanical pump 10 is connected to the molecular pump 13 through a gas pipe 6; the argon gas cylinder 4 is connected to the first air guide port 25 and the second air guide port 12 through a gas pipe 6;

[0080] A heating assembly 5 is arranged on the inner side and the bottom of the furnace body 1; a fluid channel 9 communicating with the outside of the furnace body 1 is arranged at the bottom of the furnace body 1; a blocking ring 8 is arranged in the fluid channel 9.

[0081] This embodiment also provides a method for composite degassing and impurity removal of high-purity aluminum alloy melt. The composite degassing and impurity removal method is carried out by using the composite degassing and impurity removal device provided in this embodiment. The composite degassing and impurity removal method includes the following steps:

[0082] (1) Place the high-purity aluminum alloy melt with a purity of 5N in the furnace body 1. After evacuating the inside of the furnace body 1 to a vacuum environment with a vacuum degree of 200 Pa, fill it with argon until the air pressure inside the furnace body 1 is 101.325 kPa;

[0083] (2) Under the ultrasonic assistance with an ultrasonic power of 1000 W and an ultrasonic frequency of 20 KHz, inject the argon gas bubbles formed by rotary injection into the high-purity aluminum alloy melt in step (1) for the first degassing and impurity removal for 30 min; when performing the rotary injection, the rotation speed of the rotor 22 is 400 r / min, and the gas flow rate of argon during the rotary injection is 5 m 3 / h;

[0084] (3) The high-purity aluminum alloy melt after the first degassing in step (2) is subjected to the second degassing and impurity removal for 30 min by vacuum standing under a vacuum degree of 30 Pa to obtain an ultra-high-purity aluminum alloy melt.

[0085] In this embodiment, the hydrogen content in the high-purity aluminum alloy melt is 0.225 mL / Kg, and the oxygen content is 0.471 mL / Kg.

[0086] Example 2

[0087] This embodiment provides a composite degassing and impurity removal device, which includes a furnace body, a rotary injection component, 3 ultrasonic components, an argon gas cylinder, and a vacuum system;

[0088] The rotary injection component is arranged at the central position on the top of the furnace body; the rotating rod of the rotary injection component extends vertically downward from the outside of the furnace body to the inside of the furnace body; a gas delivery channel is arranged inside the rotating rod; a rotor is arranged at the bottom of the rotating rod; the top of the rotating rod is connected with a first motor; a protective sleeve is arranged on the outside of the rotating rod; a first air guide port is arranged on the protective component, and the first air guide port is communicated with the gas delivery channel of the rotating rod;

[0089] The ultrasonic components are uniformly arranged on the periphery of the rotary injection component; the vibrating rod of the ultrasonic component extends vertically downward from the outside of the furnace body to the inside of the furnace body; the ultrasonic component further includes an ultrasonic generator and an ultrasonic regulator; the ultrasonic regulator and the ultrasonic generator are arranged on the vibrating rod near the top inside the furnace body in sequence from top to bottom; a rubber sealing ring is arranged between the ultrasonic regulator and the top inside the furnace body; outside the furnace body, the ultrasonic component is provided with a second motor, an output shaft, and a signal regulating plate from top to bottom;

[0090] The argon gas cylinder and the vacuum system are connected to the interior of the furnace body; the vacuum system includes a mechanical pump and a molecular pump; the intake valve of the mechanical pump is connected to the interior of the furnace body through a second air guide port; the exhaust valve of the mechanical pump is connected to the molecular pump through a gas pipe; the argon gas cylinder is connected to the first air guide port and the second air guide port through a gas pipe;

[0091] Heating components are provided on the inner side and the bottom of the furnace body; a fluid channel communicating with the outside of the furnace body is provided at the bottom of the furnace body; a plug ring is provided in the fluid channel.

[0092] This embodiment also provides a method for compound degassing and impurity removal of high-purity aluminum alloy melt. The compound degassing and impurity removal method is carried out by using the compound degassing and impurity removal device provided in this embodiment. The compound degassing and impurity removal method includes the following steps:

[0093] (1) Place the high-purity aluminum alloy melt with a purity of 4N8 in the furnace body, and after pumping the interior of the furnace body to a vacuum environment with a vacuum degree of 100 Pa, fill it with argon gas until the air pressure in the furnace body is 100 kPa;

[0094] (2) Under the ultrasonic assistance with an ultrasonic power of 800 W and an ultrasonic frequency of 15 KHz, inject argon gas bubbles formed by rotary spraying into the high-purity aluminum alloy melt described in step (1) for the first degassing and impurity removal for 50 min; when rotary spraying, the rotation speed of the rotor is 200 r / min, and the gas flow rate of argon gas during rotary spraying is 6 m 3 / h;

[0095] (3) The high-purity aluminum alloy melt after the first degassing in step (2) is subjected to the second degassing and impurity removal for 10 min through vacuum static settling under a vacuum degree of 10 Pa to obtain an ultra-high-purity aluminum alloy melt.

[0096] In this embodiment, the hydrogen content in the high-purity aluminum alloy melt is 0.251 mL / Kg, and the oxygen content is 0.490 mL / Kg.

[0097] Example 3

[0098] This embodiment provides a compound degassing and impurity removal device, which includes a furnace body, a rotary spraying component, 4 ultrasonic components, an argon gas cylinder and a vacuum system;

[0099] The rotary spraying component is arranged at the central position on the top of the furnace body; the rotating rod of the rotary spraying component extends vertically downward from the outside of the furnace body into the interior of the furnace body; a gas delivery channel is arranged inside the rotating rod; a rotor is arranged at the bottom of the rotating rod; the top of the rotating rod is connected to a first motor; a protective sleeve is arranged outside the rotating rod; a first air guide port is arranged on the protective component, and the first air guide port communicates with the gas delivery channel of the rotating rod;

[0100] The ultrasonic component is uniformly arranged on the circumferential side of the rotary spraying component; the vibrating rod of the ultrasonic component vertically extends downward from the outside of the furnace body into the furnace body; the ultrasonic component further includes an ultrasonic generator and an ultrasonic regulator; the ultrasonic regulator and the ultrasonic generator are sequentially arranged on the vibrating rod near the inner top of the furnace body from top to bottom; a rubber sealing ring is arranged between the ultrasonic regulator and the inner top of the furnace body; outside the furnace body, the ultrasonic component is provided with a second motor, an output shaft and a signal regulating plate from top to bottom;

[0101] The argon gas cylinder and the vacuum system are communicated with the inside of the furnace body; the vacuum system includes a mechanical pump and a molecular pump; the intake valve of the mechanical pump is connected with the inside of the furnace body through a second air guide port; the exhaust valve of the mechanical pump is connected with the molecular pump through a gas pipe; the argon gas cylinder is connected with the first air guide port and the second air guide port through a gas pipe;

[0102] The inner side and the bottom of the furnace body are provided with a heating component; the bottom of the furnace body is provided with a fluid channel communicated with the outside of the furnace body; a blocking ring is arranged in the fluid channel.

[0103] This embodiment also provides a method for compound degassing and impurity removal of high-purity aluminum alloy melt. The compound degassing and impurity removal method is carried out by using the compound degassing and impurity removal device provided in this embodiment. The compound degassing and impurity removal method includes the following steps:

[0104] (1) Place the high-purity aluminum alloy melt with a purity of 5N5 in the furnace body, and after pumping the inside of the furnace body to a vacuum environment with a vacuum degree of 300 Pa, fill it with argon until the air pressure in the furnace body is 105 kPa;

[0105] (2) Under the ultrasonic assistance with an ultrasonic power of 1200 W and an ultrasonic frequency of 25 KHz, spray the argon gas bubbles formed by rotary spraying into the high-purity aluminum alloy melt in step (1) for the first degassing and impurity removal for 20 min; when rotating and spraying, the rotation speed of the rotor is 500 r / min, and the gas flow rate of argon during rotating and spraying is 3 m 3 / h;

[0106] (3) The high-purity aluminum alloy melt after the first degassing in step (2) is subjected to the second degassing and impurity removal for 40 min through vacuum static settling under a vacuum degree of 50 Pa to obtain an ultra-high-purity aluminum alloy melt.

[0107] In this embodiment, the hydrogen content in the high-purity aluminum alloy melt is 0.209 mL / Kg, and the oxygen content is 0.453 mL / Kg.

[0108] Example 4

[0109] This embodiment provides a method for compound degassing and impurity removal of high-purity aluminum alloy melt. Except that the rotation speed of the rotor during the rotary injection in step (2) is 180 r / min, the rest are the same as those in Embodiment 1.

[0110] Embodiment 5

[0111] This embodiment provides a method for compound degassing and impurity removal of high-purity aluminum alloy melt. Except that the rotation speed of the rotor during the rotary injection in step (2) is 550 r / min, the rest are the same as those in Embodiment 1.

[0112] Embodiment 6

[0113] This embodiment provides a method for compound degassing and impurity removal of high-purity aluminum alloy melt. Except that the ultrasonic power of the ultrasonic assistance in step (2) is 500 W, the rest are the same as those in Embodiment 1.

[0114] Embodiment 7

[0115] This embodiment provides a method for compound degassing and impurity removal of high-purity aluminum alloy melt. Except that the ultrasonic power of the ultrasonic assistance in step (2) is 1500 W, the rest are the same as those in Embodiment 1.

[0116] Embodiment 8

[0117] This embodiment provides a method for compound degassing and impurity removal of high-purity aluminum alloy melt. Except that the vacuum degree of the vacuum static in step (3) is 60 Pa, the rest are the same as those in Embodiment 1.

[0118] Embodiment 9

[0119] This embodiment provides a method for compound degassing and impurity removal of high-purity aluminum alloy melt. Except that the time of the second degassing and impurity removal in step (3) is 10 min, the rest are the same as those in Embodiment 1.

[0120] Embodiment 10

[0121] This embodiment provides a method for compound degassing and impurity removal of high-purity aluminum alloy melt. Except that the time of the second degassing and impurity removal in step (3) is 45 min, the rest are the same as those in Embodiment 1.

[0122] II. Comparative Example

[0123] Comparative Example 1

[0124] This comparative example provides a compound degassing and impurity removal device. The ultrasonic component is not provided in the compound degassing and impurity removal device, and the rest are the same as those in Embodiment 1.

[0125] This comparative example also provides a method for composite degassing and impurity removal of high-purity aluminum alloy melt. Except that there is no ultrasonic assistance in step (2), the rest are the same as those in Example 1.

[0126] Comparative Example 2

[0127] This comparative example provides a method for composite degassing and impurity removal of high-purity aluminum alloy melt. Except that step (3) is not carried out, that is, vacuum standing is not carried out, the rest are the same as those in Example 1.

[0128] III. Tests and Results

[0129] The hydrogen content and oxygen content of the ultra-high-purity aluminum alloy melt samples obtained in the above examples and comparative examples were tested using LECO analysis technology, and the test results are shown in Table 1;

[0130] Table 1

[0131]

[0132]

[0133] It can be seen from the data in Table 1 that:

[0134] (1) Considering Examples 1 to 3 comprehensively, it can be known that the composite degassing and impurity removal device provided by the present invention and the method for composite degassing and impurity removal of high-purity aluminum alloy melt using the same can effectively reduce the hydrogen content in the high-purity aluminum alloy melt to below 0.251 mL / kg and the oxygen content to below 0.490 mL / kg, meeting the production requirements of high-purity aluminum alloy melt.

[0135] (2) Considering Examples 1, 4 and 5 comprehensively, it can be known that in Example 4, the rotation speed of the rotor during the rotary injection in step (2) is too low, resulting in an increase in the hydrogen content to 0.291 mL / kg and the oxygen content to 0.573 mL / kg in the obtained product; in Example 5, the rotation speed of the rotor during the rotary injection in step (2) is too high, which does not significantly improve the removal effect of hydrogen and oxygen in the product, but instead leads to an increase in the hydrogen content and oxygen content in the product and an increase in energy consumption; thus, it is shown that the present invention further preferably sets the rotation speed of the rotor during the rotary injection in step (2) to 200 - 500 r / min, further improving the removal effect of hydrogen and oxygen in the product and ensuring low energy consumption at the same time.

[0136] (3) From the combination of Example 1, Example 6 and Example 7, it can be seen that the ultrasonic power of the ultrasonic assistance described in step (2) of Example 6 is too low, resulting in the increase of the hydrogen content in the obtained product to 0.243 mL / kg and the oxygen content to 0.515 mL / kg; the ultrasonic power of the ultrasonic assistance described in step (2) of Example 7 is too high, and there is no obvious reduction in the hydrogen and oxygen contents in the product; thus, it is shown that the ultrasonic power of the ultrasonic assistance described in step (2) of the present invention is further preferably 800 - 1200 W, which further improves the degassing effect while ensuring low energy consumption and low processing cost.

[0137] (4) From the combination of Example 1, Example 8 to Example 10, it can be seen that the vacuum degree of the vacuum standing described in step (3) of Example 8 is too low, and the time of the second degassing and impurity removal (vacuum standing) in Example 9 is too short, both of which result in the increase of the hydrogen and oxygen contents in the product; the time of the second degassing and impurity removal in Example 10 is too long, and there is no obvious reduction in the hydrogen and oxygen contents in the product; thus, it is shown that the vacuum degree of the vacuum standing of the present invention is further preferably 10 - 50 Pa, and the time of the second degassing and impurity removal is further preferably 20 - 40 min, which further improves the removal effect of hydrogen and oxygen in the high-purity aluminum alloy melt.

[0138] (5) From the combination of Example 1, Comparative Example 1 and Comparative Example 2, it can be seen that since the ultrasonic component is not provided in the degassing and impurity removal device in Comparative Example 1, that is, there is no ultrasonic assistance during the rotary injection process, the hydrogen content in the obtained product increases to 0.411 mL / kg and the oxygen content increases to 0.813 mL / kg; since the composite degassing and impurity removal method in Comparative Example 2 does not perform vacuum standing, that is, only the first degassing and impurity removal is carried out, the hydrogen content in the obtained product increases to 0.327 mL / kg and the oxygen content increases to 0.718 mL / kg; thus, it is shown that the composite degassing and impurity removal device of the present invention sets the rotary injection component, the ultrasonic component and the vacuum system to work together, and performs composite degassing and impurity removal by rotary injection combined with vacuum standing under ultrasonic assistance, which significantly reduces the hydrogen and oxygen contents in the high-purity aluminum alloy melt and provides high-quality ingots for semiconductor sputtering targets.

[0139] The applicant declares that the above is only the specific implementation manner of the present invention, but the protection scope of the present invention is not limited thereto. Those skilled in the art should understand that any changes or substitutions that can be easily thought of by those skilled in the art within the technical scope disclosed by the present invention fall within the protection scope and the disclosure scope of the present invention.

Claims

1. A composite degassing and impurity removal device, characterized in that: The composite degassing and impurity removal device comprises a furnace body, a rotary spraying component, at least two ultrasonic components, an inert gas supply component and a vacuum system; The rotary blowing assembly is arranged at the center of the top of the furnace body; the rotating rod of the rotary blowing assembly extends vertically downward from the outside of the furnace body to the inside of the furnace body; a gas delivery channel is arranged inside the rotating rod; The ultrasonic components are evenly arranged around the rotating spraying component; the vibration component of the ultrasonic component extends vertically downward from the outside of the furnace body to the inside of the furnace body; The inert supply component and the vacuum system are in communication with the interior of the furnace body.

2. The composite degassing and impurity removal device according to claim 1, characterized in that: A rotor is disposed at the bottom of the rotating rod; Preferably, a first motor is connected to the top of the rotating rod; Preferably, a protective component is provided on the outer side of the rotating rod; Preferably, a first air guide port is provided on the protection component, and the first air guide port is communicated with the gas delivery channel of the rotating rod.

3. The composite degassing and impurity removal device according to claim 1 or 2, characterized in that: The ultrasonic component also includes an ultrasonic generating component and an ultrasonic regulating component; Preferably, the ultrasonic regulating component and the ultrasonic generating component are sequentially arranged from top to bottom on the vibration component close to the top of the furnace body; Preferably, a sealing component is provided between the ultrasonic adjustment component and the top of the furnace body; Preferably, outside the furnace body, the ultrasonic component is provided with a second motor, an output shaft and a signal adjustment board from top to bottom.

4. The composite degassing and impurity removal device according to any one of claims 1 to 3, characterized in that: The vacuum system includes a mechanical pump and a molecular pump; Preferably, the air inlet valve of the mechanical pump is connected to the interior of the furnace body through the second air guide port; Preferably, the exhaust valve of the mechanical pump is connected to the molecular pump via an air pipe; Preferably, the inert gas supply component is connected to the first gas guide port and the second gas guide port through a gas pipe.

5. The composite degassing and impurity removal device according to any one of claims 1 to 4, characterized in that: A heating assembly is provided inside the furnace body and at the bottom of the furnace body; Preferably, the bottom of the furnace body is provided with a fluid channel communicating with the outside of the furnace body; Preferably, a blocking component is provided in the fluid channel.

6. A composite degassing and impurity removal method for high-purity aluminum alloy melt, characterized in that: The composite degassing and impurity removal method is carried out using the composite degassing and impurity removal device as described in any one of claims 1 to 5.

7. The composite degassing and impurity removal method according to claim 6, characterized in that: The composite degassing and impurity removal method comprises the following steps: (1) placing a high-purity aluminum alloy melt in a furnace body, and evacuating the furnace body to a vacuum environment and then filling it with an inert gas; (2) spraying inert gas bubbles formed by rotary blowing under the assistance of ultrasound into the high-purity aluminum alloy melt in step (1) to perform a first degassing and impurity removal; (3) Step (2) The high-purity aluminum alloy melt after the first degassing is placed in a vacuum state for a second degassing and impurity removal to obtain an ultra-high-purity aluminum alloy melt.

8. The composite degassing and impurity removal method according to claim 6 or 7, characterized in that: The purity of the high-purity aluminum alloy melt in step (1) is ≥4N8; Preferably, the vacuum degree of the vacuum environment in step (1) is 100-300 Pa; Preferably, in step (1), the inert gas is charged until the gas pressure in the furnace body reaches 100 kPa to 105 kPa; Preferably, the inert gas in step (1) comprises argon and / or nitrogen, preferably argon.

9. The composite degassing and impurity removal method according to any one of claims 6 to 8, characterized in that: During the rotary spraying in step (2), the rotation speed of the rotor is 200 to 500 r / min; Preferably, the flow rate of the inert gas during the rotary spraying in step (2) is 3 to 6 m 3 / h; Preferably, the ultrasonic power of the ultrasonic assistance in step (2) is 500 to 1500 W, preferably 800 to 1200 W; Preferably, the ultrasonic frequency of the ultrasonic assistance in step (2) is 15 to 25 KHz; Preferably, the time for the first degassing and impurity removal in step (2) is 20 to 50 minutes.

10. The composite degassing and impurity removal method according to any one of claims 6 to 9, characterized in that: The vacuum degree of the vacuum standing in step (3) is 10 to 50 Pa; Preferably, the time for the second degassing and impurity removal in step (3) is 10 to 40 minutes, preferably 20 to 40 minutes.

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