Distillation and purification device and target material recovery system

Abstract

The utility model provides a distillation purification device and a target material recovery system. The distillation and purification device comprises a distillation module, a collection module and a heat insulation module, the distillation module comprises a cover plate and a first container with a top opening; the cover plate is arranged above the top opening of the first container; a cover plate opening smaller than the diameter of the cover plate is formed in the cover plate; the collecting module comprises a second container with an opening in the bottom and a cooling device arranged on the periphery of the second container, and the opening in the bottom of the second container is formed above the cover plate; the cover plate opening extends into the second container to form a cover plate opening extending part, and the first container and the second container are communicated through the cover plate opening and the cover plate opening extending part; the heat insulation module comprises a first heat insulation element which is arranged on the periphery of the opening of the first container and used for external heat insulation of the first container and the second container. When the device or the system is used for recovering the alloy cast ingot, the recovery rate can be improved, and the purity of the recovered alloy cast ingot is improved.

Description

Technical Field

[0001] The utility model relates to a distillation purification device and a target material recovery system. Background Art

[0002] Aluminum-scandium (Al-Sc) alloy targets are ideal piezoelectric thin film materials for preparing radio frequency filter chips, and are increasingly widely used in optoelectronic devices, electronic components, and microelectromechanical systems (MEMS).

[0003] At present, the utilization rate of target materials is generally around 20%~50%; at the same time, since scandium (Sc) is a rare metal, the recycling of Al-Sc targets is of great significance.

[0004] Patent CN202210914816.X discloses a method for recycling and reusing sputtering target components. The method uses physical separation to separate the sputtering target components, obtaining a backing plate and sputtering target. The sputtering target is then subjected to alkaline and acid leaching, water washing, drying, smelting, standing, and casting to obtain a metal ingot. Al-Sc targets have a high Sc content and are chemically active. During the acid-base leaching process, they react with the leaching solution, resulting in significant loss. This method is also prone to introducing impurities, which can affect the purity of the alloy ingot. Therefore, this method is not suitable for recycling Al-Sc targets.

[0005] Patent CN202310242989.6 discloses a target material recycling and reuse method. The method involves analyzing the etching curve of the sputtered target material and determining the target material's recovery area based on the etching curve. Based on the target material's finished size requirements, the target material's recovery area is then wire-cut to produce a target block. The sputtering channels in the target block are then smoothed to produce the finished target material. This method avoids unusable target material residue areas and produces targets smaller than the original specifications. This method also results in a low material recovery rate. Utility Model Content

[0006] The technical problem to be solved by the present invention is to overcome the defects of low purity and low recovery rate of alloys recovered by the prior art, and to provide a distillation purification device and a target material recovery system; the device or system of the present application can be used to recover rare earth metals or rare earth alloy target materials, and can improve their recovery rate and the purity of the recovered products; the rare earth metals can be metals such as Sc, La, Ce, Y, Dy, Er, etc., and the rare earth alloy target material can be an aluminum-scandium alloy ingot.

[0007] The utility model solves the above technical problems through the following technical solutions:

[0008] The utility model provides a distillation purification device, which includes a distillation module, a collection module and an insulation module; the distillation module includes a cover plate and a first container with a top opening; the cover plate is arranged above the top opening of the first container; the cover plate is provided with a cover plate opening smaller than the cover plate diameter; the collection module includes a second container with a bottom opening and a cooling device arranged on the periphery of the second container, and the bottom opening of the second container is arranged above the cover plate; the cover plate opening extends toward the interior of the second container to form a cover plate opening extension, and the first container and the second container are connected through the cover plate opening and the cover plate opening extension; the insulation module includes a first insulation element, which is arranged on the periphery of the opening of the first container and is used to insulate the first container from the outside of the second container.

[0009] In the present invention, the first container may be a "crucible" for distilling and purifying the substance; the second container may be a "collector" for condensing and collecting the target substance.

[0010] In the present invention, by providing an opening smaller than the diameter of the cover plate on the cover plate, the backflow of high-boiling-point and low-melting-point metals during the distillation process can be effectively prevented; however, this design does not affect the condensation collection of metals with higher melting points.

[0011] In some embodiments, the cooling device includes a cooling coil and a cooling baffle, the cooling coil is wound around the periphery of the side wall surface of the second container, and the cooling baffle is arranged above the top surface of the second container.

[0012] In some embodiments, the first container is made of a metal with a high melting point, preferably tungsten or tantalum.

[0013] In some embodiments, the top surface of the second container is a planar structure.

[0014] In some embodiments, the distillation purification device includes a furnace body with a hollow interior, and the distillation module, the collection module, and the insulation module are all arranged in the furnace body.

[0015] In a specific embodiment, the cooling medium pipeline of the cooling device passes through the outer wall surface of the furnace body and is connected to a cooling medium source provided outside the furnace body.

[0016] In some embodiments, the distillation module further includes a second thermal insulation element, which is a barrel-shaped structure with an open top. The top opening of the second thermal insulation element is connected to the lower surface of the first thermal insulation element to form a distillation area for placing the first container.

[0017] In a specific embodiment, a heating element is further provided in the distillation zone.

[0018] In a specific embodiment, the first thermal insulation element is a thermal insulation board; and the second thermal insulation element is a thermal insulation screen.

[0019] In some embodiments, the length of the cover plate opening extension does not exceed 2 cm.

[0020] In some embodiments, the distillation and purification device is a distillation and purification device for recovering rare earth alloys, preferably a distillation and purification device for recovering aluminum-scandium targets.

[0021] The utility model also provides a target material recovery system, which comprises an impurity removal device, the above-mentioned distillation purification device, and a vacuum suspension melting device which are connected in sequence.

[0022] In the present invention, the impurity removal device and the vacuum suspension smelting device are both conventional devices in the art.

[0023] In the present invention, the target material recovery system is a recovery system for collecting aluminum-scandium target materials.

[0024] The positive progress effect of this utility model is:

[0025] (1) By structurally designing the distillation purification device, the distillation module and the collection module can form two temperature zones, which facilitates the efficient collection of the target substance by distillation, improves the recovery purity and recovery rate of the target substance, and avoids the difficulty of condensing the target substance in the collection module due to the similar temperature of the distillation module and the collection module.

[0026] (2) The device or system of the present application can be used to recover rare earth metals or rare earth alloy targets, and can improve their recovery rate and the purity of the recovered products; the rare earth metals can be metals such as Sc, La, Ce, Y, Dy, Er, etc., and the rare earth alloy target can be an aluminum-scandium alloy ingot. BRIEF DESCRIPTION OF THE DRAWINGS

[0027] Figure 1 Schematic diagram of the structure of the distillation purification device in Example 1.

[0028] Figure 2 This is a process flow chart of the recovery method of the aluminum-scandium alloy target in Example 1.

[0029] Description of reference numerals:

[0030] Furnace body 1

[0031] Heat insulation board 2

[0032] Heating element 3

[0033] Heat shield 4

[0034] First container 5

[0035] Cover 6

[0036] Cover opening 61

[0037] Cover opening extension 62

[0038] Second container 7

[0039] Cooling coil 8

[0040] Cooling baffle 9

[0041] Cooling coil water inlet 10

[0042] Cooling coil water outlet 11

[0043] Cooling baffle water inlet 12

[0044] Cooling baffle water outlet 13. DETAILED DESCRIPTION

[0045] The present invention will be described more clearly and completely with reference to the following preferred embodiments and the accompanying drawings.

[0046] The relationship between the liquidus point of the aluminum-scandium target used in the following examples or comparative examples and its components is shown in Table 1 below. Table 1 shows the Sc content in the aluminum-scandium target and the liquidus point of the target.

[0047] Table 1

[0048]

[0049] Example 1

[0050] This embodiment provides a distillation purification device; Figure 1 Schematic diagram of the structure of the distillation purification device of this embodiment.

[0051] The distillation purification device includes a furnace body 1 with a hollow interior, and a distillation module, a collection module and an insulation module are all arranged in the furnace body 1; the distillation module includes a cover plate 6 and a first container 5 with an opening at the top; the cover plate 6 is arranged above the top opening of the first container 5; the cover plate 6 is provided with a cover plate opening 61 smaller than the diameter of the cover plate 6; the collection module includes a second container 7 with an opening at the bottom, and a cooling device arranged at the periphery of the second container 7, the cooling device includes a cooling coil 8 and a cooling baffle 9, the cooling coil 8 is wound around the periphery of the side wall surface of the second container 7, the cooling baffle 9 is arranged above the top surface of the second container 7, and the cooling coil 8 is respectively provided with a cooling coil water inlet 10 and a cooling coil water outlet The cooling baffle 9 is provided with a cooling baffle water inlet 12 and a cooling baffle water outlet 13; the cooling medium pipeline of the cooling device passes through the outer wall of the furnace body 1 and is connected to the cooling medium source provided outside the furnace body 1; the first container 5 is made of tantalum; the top surface of the second container 7 is a horizontal structure; the bottom opening of the second container 7 is provided above the cover plate 6; the cover plate opening 61 extends into the interior of the second container 7 to form a cover plate opening extension 62, and the first container 5 and the second container 7 are connected through the cover plate opening 61; the thermal insulation module includes a first thermal insulation element, which is provided on the periphery of the opening of the first container 5 and is used to thermally insulate the first container 5 from the outside of the second container 7;

[0052] The distillation module also includes a second thermal insulation element, which is a barrel-shaped structure with an open top. The top opening of the second thermal insulation element is connected to the lower surface of the first thermal insulation element to form a distillation area for placing the first container 5; a heating body 3 is also provided in the distillation area; the first thermal insulation element is an insulation board 2; the second thermal insulation element is an insulation screen 4; the length of the cover opening extension 62 is 1 cm.

[0053] This embodiment also provides a target material recovery system, which includes an impurity removal device, the above-mentioned distillation purification device and a vacuum suspension melting device connected in sequence; the process of using the target material recovery system to recover aluminum-scandium alloy target material is as follows: Figure 2 As shown; Figure 2 : is a process flow chart of the method for recycling the aluminum-scandium alloy target in this embodiment; the method for recycling the aluminum-scandium alloy target comprises the following steps:

[0054] (1) Removing the backing plate: The Al-Sc alloy target material has a size of 304×6 mm, a scandium content of 10 at.%, and a copper backing plate. The Al-Sc alloy sputtering target material and the backing plate are bonded with indium. Place the Al-Sc alloy target material on a heating platform at 230°C. After unbundling, scrape off the indium on the bonding surface of the target material to reduce the indium content in the Al-Sc alloy target material to less than 0.1%.

[0055] (2) Impurity removal: Cut the Al-Sc alloy sputtering target into alloy blocks with the longest side less than 100 mm, put them into a tungsten crucible, put the tungsten crucible into a vacuum carbon tube furnace, and evacuate to a vacuum degree of 1×10 -2 After 1 hour, heating was started, the temperature was raised to 1000°C, and the heating was stopped after keeping the temperature for 1 hour.

[0056] (3) Distillation purification: After cooling to below 70°C, install a tantalum collector and evacuate to 1×10 -2 After 3 hours, heating was started, the temperature was raised to 1650℃, and the temperature was kept for 4 hours before the heating was stopped.

[0057] (4) Vacuum suspension melting: When the furnace temperature cools down to below 70°C, remove the collector, peel off the collected metal from the collector and place it in a vacuum suspension furnace, and evacuate to 6×10 -3 Pa, fill with argon to 0.06Mpa for melting; the melting temperature is 50~100℃ higher than the liquidus point of the alloy components, and the temperature is kept for 10min to obtain an aluminum-scandium alloy ingot.

[0058] After sampling and GDMS testing, the purity of the obtained aluminum-scandium alloy ingot was higher than 4N (99.99%), and the metal recovery rate was 87.3%.

[0059] Example 2

[0060] The only difference from Example 1 is that the scandium content of the Al—Sc alloy target is 20 at.%.

[0061] After sampling and GDMS testing, the purity of the obtained aluminum-scandium alloy ingot was higher than 4N (99.99%), and the metal recovery rate was 86.4%.

[0062] Example 3

[0063] The only difference from Example 1 is that the scandium content of the Al-Sc alloy target is 30 at.%, the distillation purification temperature is 1700° C., and the time is 5 h.

[0064] After sampling and GDMS testing, the alloy purity was higher than 4N (99.99%) and the metal recovery rate was 90.1%.

[0065] Comparative Example 1

[0066] This comparative example does not use the distillation purification apparatus of Example 1. During the distillation purification process of this comparative example, no water-cooling sleeve is used on the outside of the collector, resulting in the temperature of the collector being in the range of 900-1100°C.

[0067] In this comparative example, the lower part of the collector was damaged due to metal reflux, and the metal yield remaining in the collector was 34.2%. The alloy purity was higher than 4N (99.99%) after GDMS detection.

[0068] Effect Example 1

[0069] The obtained aluminum-scandium alloy ingot is tested for purity. Purity = 100% minus the total metal impurity content in the obtained aluminum-scandium alloy ingot. The total metal impurity content refers to the mass content of other metal elements other than aluminum and scandium as determined by glow discharge mass spectrometry (GDMS).

[0070] The metal recovery rate of the obtained aluminum-scandium alloy ingot is calculated as follows: Metal recovery rate = weight of the obtained aluminum-scandium alloy ingot / (weight of the aluminum-scandium target - weight of the backing plate) × 100%.

[0071] The results are shown in Table 2.

[0072] Table 2

[0073]

[0074] As shown in Table 2, compared with Comparative Example 1, Examples 1-3 performed heat treatment to remove impurities at a specific temperature and adopted specific distillation purification equipment, and the recovered aluminum-scandium alloy ingots had higher purity and recovery rate.

Claims

1. A distillation purification device, characterized in that: It includes a distillation module, a collection module and an insulation module; The distillation module includes a cover plate and a first container with an opening at the top; the cover plate is arranged above the top opening of the first container; the cover plate is provided with a cover plate opening smaller than the diameter of the cover plate; The collection module includes a second container with a bottom opening, and a cooling device disposed on the periphery of the second container, wherein the bottom opening of the second container is disposed above the cover plate; the cover plate opening extends into the interior of the second container to form a cover plate opening extension, and the first container and the second container are connected through the cover plate opening and the cover plate opening extension; The heat insulation module includes a first heat insulation element, which is arranged at the periphery of the opening of the first container and is used to heat-insulate the first container from the outside of the second container.

2. The distillation purification device according to claim 1, characterized in that The cooling device includes a cooling coil and a cooling baffle. The cooling coil is wound around the periphery of the side wall surface of the second container, and the cooling baffle is arranged above the top surface of the second container.

3. The distillation purification device according to claim 1, characterized in that The material of the first container is tungsten or tantalum; The top surface of the second container is a planar structure.

4. The distillation purification device according to claim 1, characterized in that The distillation and purification device includes a furnace body with a hollow interior, and the distillation module, the collection module and the insulation module are all arranged in the furnace body.

5. The distillation purification device according to claim 4, characterized in that: The cooling medium pipeline of the cooling device passes through the outer wall surface of the furnace body and is connected to a cooling medium source arranged outside the furnace body.

6. The distillation purification device according to claim 1, characterized in that: The distillation module also includes a second thermal insulation element, which is a barrel-shaped structure with an open top. The top opening of the second thermal insulation element is connected to the lower surface of the first thermal insulation element to form a distillation area for placing the first container.

7. The distillation purification device according to claim 6, characterized in that A heating element is also provided in the distillation zone.

8. The distillation purification device according to claim 6, characterized in that: The first thermal insulation element is a thermal insulation board; The second thermal insulation element is a thermal insulation screen.

9. The distillation purification device according to claim 1, characterized in that: The length of the cover plate opening extension portion does not exceed 2 cm.

10. A target material recovery system, characterized in that: The method comprises an impurity removal device, a distillation purification device according to any one of claims 1 to 9, and a vacuum suspension melting device, which are connected in sequence.

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