CN113106407A - Manufacturing device and method of rare earth metal and rare earth alloy rotary target material - Google Patents
Manufacturing device and method of rare earth metal and rare earth alloy rotary target material Download PDFInfo
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- CN113106407A CN113106407A CN202110325579.9A CN202110325579A CN113106407A CN 113106407 A CN113106407 A CN 113106407A CN 202110325579 A CN202110325579 A CN 202110325579A CN 113106407 A CN113106407 A CN 113106407A
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- 229910052761 rare earth metal Inorganic materials 0.000 title claims abstract description 53
- 150000002910 rare earth metals Chemical class 0.000 title claims abstract description 53
- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 39
- 239000000956 alloy Substances 0.000 title claims abstract description 39
- 239000013077 target material Substances 0.000 title claims abstract description 32
- 238000000034 method Methods 0.000 title claims abstract description 31
- 238000004519 manufacturing process Methods 0.000 title claims description 9
- 238000005266 casting Methods 0.000 claims abstract description 41
- 230000008018 melting Effects 0.000 claims abstract description 27
- 238000002844 melting Methods 0.000 claims abstract description 26
- 238000003723 Smelting Methods 0.000 claims abstract description 16
- 238000002360 preparation method Methods 0.000 claims abstract description 13
- 238000010438 heat treatment Methods 0.000 claims description 58
- 239000000463 material Substances 0.000 claims description 47
- 238000006243 chemical reaction Methods 0.000 claims description 43
- 229910052751 metal Inorganic materials 0.000 claims description 27
- 239000002184 metal Substances 0.000 claims description 27
- 239000011261 inert gas Substances 0.000 claims description 22
- 238000005086 pumping Methods 0.000 claims description 19
- 230000033001 locomotion Effects 0.000 claims description 13
- 238000000746 purification Methods 0.000 claims description 10
- 238000012545 processing Methods 0.000 claims description 9
- 239000007789 gas Substances 0.000 claims description 7
- 239000007788 liquid Substances 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 4
- 238000007711 solidification Methods 0.000 claims description 4
- 230000008023 solidification Effects 0.000 claims description 4
- 238000009529 body temperature measurement Methods 0.000 claims description 3
- 230000008602 contraction Effects 0.000 claims description 3
- 230000004927 fusion Effects 0.000 claims description 3
- 238000007789 sealing Methods 0.000 claims description 3
- 239000007769 metal material Substances 0.000 claims description 2
- 238000000465 moulding Methods 0.000 abstract description 3
- 238000009776 industrial production Methods 0.000 abstract 1
- 230000010354 integration Effects 0.000 abstract 1
- 229910001092 metal group alloy Inorganic materials 0.000 abstract 1
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 10
- 239000012535 impurity Substances 0.000 description 10
- 239000002994 raw material Substances 0.000 description 9
- 229910052771 Terbium Inorganic materials 0.000 description 8
- GZCRRIHWUXGPOV-UHFFFAOYSA-N terbium atom Chemical compound [Tb] GZCRRIHWUXGPOV-UHFFFAOYSA-N 0.000 description 8
- 229910052692 Dysprosium Inorganic materials 0.000 description 7
- KBQHZAAAGSGFKK-UHFFFAOYSA-N dysprosium atom Chemical compound [Dy] KBQHZAAAGSGFKK-UHFFFAOYSA-N 0.000 description 7
- 230000002829 reductive effect Effects 0.000 description 7
- 229910052777 Praseodymium Inorganic materials 0.000 description 5
- 229910052786 argon Inorganic materials 0.000 description 5
- 238000003754 machining Methods 0.000 description 5
- PUDIUYLPXJFUGB-UHFFFAOYSA-N praseodymium atom Chemical compound [Pr] PUDIUYLPXJFUGB-UHFFFAOYSA-N 0.000 description 5
- 238000000605 extraction Methods 0.000 description 4
- 238000011049 filling Methods 0.000 description 4
- 238000010309 melting process Methods 0.000 description 4
- 229910001172 neodymium magnet Inorganic materials 0.000 description 4
- 238000009835 boiling Methods 0.000 description 3
- 239000000155 melt Substances 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 239000010935 stainless steel Substances 0.000 description 3
- 229910001220 stainless steel Inorganic materials 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- QJVKUMXDEUEQLH-UHFFFAOYSA-N [B].[Fe].[Nd] Chemical compound [B].[Fe].[Nd] QJVKUMXDEUEQLH-UHFFFAOYSA-N 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 229910002804 graphite Inorganic materials 0.000 description 2
- 239000010439 graphite Substances 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 208000037656 Respiratory Sounds Diseases 0.000 description 1
- 230000004308 accommodation Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000009172 bursting Effects 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005324 grain boundary diffusion Methods 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 238000001755 magnetron sputter deposition Methods 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052754 neon Inorganic materials 0.000 description 1
- GKAOGPIIYCISHV-UHFFFAOYSA-N neon atom Chemical compound [Ne] GKAOGPIIYCISHV-UHFFFAOYSA-N 0.000 description 1
- 230000036961 partial effect Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000002093 peripheral effect Effects 0.000 description 1
- 238000004663 powder metallurgy Methods 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 238000005057 refrigeration Methods 0.000 description 1
- 229910052706 scandium Inorganic materials 0.000 description 1
- SIXSYDAISGFNSX-UHFFFAOYSA-N scandium atom Chemical compound [Sc] SIXSYDAISGFNSX-UHFFFAOYSA-N 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 230000002269 spontaneous effect Effects 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 238000004861 thermometry Methods 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 239000010937 tungsten Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/3407—Cathode assembly for sputtering apparatus, e.g. Target
- C23C14/3414—Metallurgical or chemical aspects of target preparation, e.g. casting, powder metallurgy
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
- B22D23/00—Casting processes not provided for in groups B22D1/00 - B22D21/00
- B22D23/06—Melting-down metal, e.g. metal particles, in the mould
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
- B22D27/00—Treating the metal in the mould while it is molten or ductile ; Pressure or vacuum casting
- B22D27/04—Influencing the temperature of the metal, e.g. by heating or cooling the mould
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
- B22D27/00—Treating the metal in the mould while it is molten or ductile ; Pressure or vacuum casting
- B22D27/15—Treating the metal in the mould while it is molten or ductile ; Pressure or vacuum casting by using vacuum
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/14—Metallic material, boron or silicon
- C23C14/16—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon
- C23C14/165—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon by cathodic sputtering
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
The invention discloses a preparation device and a preparation method of a rare earth metal or alloy rotary target material, which can realize the integration of casting and molding of metal alloy, complete the melting and casting molding in the same space and effectively improve the quality of the rotary target material. The preparation method adopting the equipment can be directly molded and demoulded after smelting. The method is simple and easy to operate, and is suitable for industrial production; the equipment and the method can obtain the rotary target material with high purity, uniform and stable components and high yield.
Description
Technical Field
The invention is used in the field of rare earth metal and alloy target materials thereof, and particularly relates to a manufacturing device and a manufacturing method of a rotary target material.
Background
At present, rare earth or rare earth alloy target materials are widely used in the rare earth permanent magnet industry, the magnetic refrigeration industry, the OLED display industry and other industries to improve the product performance. For example, in the rare earth permanent magnet industry, in order to improve the coercive force and high-temperature usability of a neodymium iron boron (NdFeB) permanent magnet material, a commonly used method at present is to sputter a heavy rare earth metal dysprosium (Dy), terbium (Tb) and other targets on the surface of the neodymium iron boron (NdFeB) material in a magnetron sputtering coating mode to form a covering layer, and diffuse the rare earth metal into a magnet through high-position grain boundary diffusion so as to achieve the purposes of improving the coercive force of the magnet and using a small amount of rare earth, thereby reducing the cost.
The existing rare earth metal or rare earth alloy rotary target material manufacturing method has the following two modes:
the method comprises the following steps: heating the massive metal raw material in a vacuum melting furnace to be in a liquid state, then casting the massive metal raw material in a mould, and demoulding to obtain a blank. The disadvantages of this method are:
1) when the method is used for processing, the surface of a blank is uneven, a large processing allowance is needed, the yield is low, and the yield is only about 30 percent generally; the yields is low, because the mould temperature is lower in the casting process to and easy crackle, lead to appearing the waste product.
2) Meanwhile, under the process condition, because the blank machining allowance is large, the machining amount of the subsequent machining procedure is large, and a large amount of time is needed for machining.
The method 2 comprises the following steps: the method comprises the steps of preparing a product blank by adopting a powder metallurgy method, pressing and sintering rare earth metal or rare earth alloy powder with a proper particle size, then performing subsequent machining, and binding the rare earth metal or rare earth alloy powder on a cheap metal back plate to obtain a molded rare earth target material or rare earth alloy target material. The disadvantages of this method are:
1) the rare earth metal is very active, the powder of the rare earth metal is extremely easy to generate spontaneous combustion, and the danger coefficient of the blank processed by the method is high.
2) Rare earth metals are very active and easy to oxidize, the processing cost is very high, and the price is usually 5-20 times of that of metals with the same specification.
The existing preparation method of the rare earth metal rotary target has low yield, high processing difficulty, no contribution to production and high cost. Meanwhile, continuous multiple casting production cannot be carried out. In view of the above disadvantages, a new apparatus and method for preparing a rare earth metal or alloy rotary target material is urgently needed.
Disclosure of Invention
In order to solve the problems in the prior art, the invention designs the rare earth metal or rare earth alloy rotary target material preparation equipment and the preparation method thereof, which have simple structure and are easy to realize industrial application, so as to solve the problems of high processing cost and low yield of the rare earth metal or rare earth alloy rotary target material.
In order to achieve the purpose, the invention adopts the following technical scheme: the equipment for preparing the rare earth metal or alloy rotary target comprises a reaction box body, wherein the reaction box body is a sealed cavity, and at least one extraction opening is formed in the reaction box body. A fusion casting device is arranged in the reaction box body. The fusion casting device comprises an outer wall, an inner cavity, a separable top plate and a separable bottom plate, and is mounted in the reaction box body in a suspension manner. The separable top plate and the separable bottom plate are respectively arranged right above and right below the outer wall. The bottom plate just below the outer wall needs not to be less than the external diameter of outer wall, and the bottom plate can form an accommodation space with the outer wall cooperation for place the material. The roof directly over the outer wall is less than the outer wall internal diameter, when realizing longitudinal movement through the actuating lever, can imbed and exert thrust in the vertical direction in the outer wall, pushes out the outer wall with material and inner chamber. The bottom plate can realize longitudinal movement through the driving rod, and the materials and the inner cavity are moved out of the outer wall.
The outer periphery of the outer wall is provided with a heating device in a surrounding way. The inner cavity is arranged inside the outer wall, the inner cavity is cylindrical and is vertically arranged on the bottom plate, and the bottom plate is detachably connected with the inner cavity.
Further, the heating device is divided into an upper heating device and a lower heating device which can be heated independently.
Furthermore, a base can be arranged on the bottom plate and used for fixing the position of the inner cavity.
Further, a sealing structure is arranged at the matching position between the bottom plate and the outer wall to prevent liquid leakage.
Further, the outer wall and the inner cavity may be annular in cross-section.
Furthermore, the equipment comprises a feeding device, wherein a feeding hopper is arranged on the feeding device and is fixedly connected with the feeding device through a driving rod; the driving rod can perform parallel contraction motion along the horizontal direction and can perform rotary motion along the axis of the driving rod, and the charging hopper performs parallel motion and/or rotary motion along with the driving rod.
Furthermore, observation and temperature measurement windows are arranged on the reaction box body.
Further, an inert gas supply device and a vacuum pumping device are connected to the outside of the reaction box body; an air supply pipe of the inert gas supply device is communicated with an air extraction opening on the reaction box body; the exhaust tube of the vacuum pumping device is communicated with the exhaust opening of the reaction box body.
Further, one or more than one casting device may be provided in the reaction box.
A preparation method of a rare earth metal or alloy rotary target material comprises the following steps:
s1 feeding: and respectively placing the prepared materials in a casting device and a feeding device. The materials can be added by the feeding device according to the requirement in the smelting process.
S2 smelting: opening the top plate, filling the well-sampled rare earth metal raw material between the inner cavity and the outer wall, opening the vacuumizing device to vacuumize the reaction box body, and when the vacuum degree in the reaction box body reaches 10-10-3When Pa, stopping vacuumizing and filling inert gas, setting the temperature of a heating device to be 30-100 ℃ above the melting point of the material, and starting smelting to obtain a crude metal or alloy melt;
s2 purification: through the observation port, after the materials are observed to be completely melted, the vacuumizing device is started to vacuumize and purify the reaction box body, and the vacuum degree in the reaction box body is 10-10-3When Pa, stopping vacuumizing;
s3 forming: adjusting the temperature of the casting device to be 30-100 ℃ below the melting point through a heating device, reducing the temperature of the lower part of the heating device to enable a product at the bottom of the device to be solidified firstly, confirming that the upper surface of the material is solidified through an observation port, completing demolding within 1-3 min, stripping an inner cavity after cooling to the room temperature, and processing to obtain the rare earth metal or alloy rotary target material.
Further, the inert gas may be argon or neon or a mixture of the two.
Compared with the prior art, the invention has the following beneficial technical effects:
1. the equipment provided by the invention adopts a vacuum melting method to melt rare earth metal or rare earth alloy, so that the melting, casting and molding of the rotary target material can be integrated, the problems that the melting and casting are separately carried out in two spaces in the prior art, the product quality is influenced by mutual interference in the melting and casting processes, the product is easy to crack and the like are solved, and the rotary target material with high purity, uniform and stable components and high yield can be obtained after demolding.
2. The equipment controls the bottom of the product to be solidified firstly by changing the heating mode of the heating device, simultaneously maintains the surface of the melt to be in a high-temperature molten state, and finally cools the whole surface simultaneously, so that the whole surface is not cooled from the outer edge to the center gradually, and the defects of hole bursting and hole shrinkage can be effectively eliminated.
3. The rotary target material prepared by the invention is not limited by size.
4. The invention optimizes the process, eliminates the transmission process of smelting and casting, effectively reduces the mixing of impurities, improves the safety of operators and avoids contacting high-temperature molten liquid or castings. In addition, the temperature of the metal is easily lost during the conveying process, so that the product quality is unstable.
5. The invention optimizes the process for the problems that the melting point difference of volatile materials or materials is not easy to control and the chemical components are not easy to be uniform and stable in the vacuum melting process, and provides equipment capable of effectively inhibiting the volatile materials from volatilizing so as to ensure that the chemical components of the melted alloy are uniform and stable.
Drawings
FIG. 1 is a schematic view of the structure of the apparatus of the present invention.
FIG. 2 is a schematic view of the first state of the apparatus of the present invention.
FIG. 3 is a diagram illustrating a second state of the apparatus according to the present invention.
In the figure.
1-rotating target material preparation equipment.
100-reaction box.
110-fusion casting apparatus.
111-outer wall.
112-top plate.
113-bottom plate.
114-lumen.
115-heating means.
116-drive rod connected to the top plate.
117-drive rod connected to the bottom plate.
120-observation and thermometry windows.
130-feeding device.
131-a loading hopper.
132-drive rod connected to the hopper.
140-pumping port.
200-inert gas supply device, the gas supply pipe is communicated with the pumping hole of the reaction box body.
201-gas control means.
300-a vacuum extractor, and an extraction pipe is communicated with the extraction opening of the vacuum extractor 100.
301-vacuum control means.
400-materials.
Detailed Description
The present invention will be described in further detail with reference to the following drawings and specific examples so that those skilled in the art can better understand the present invention and can practice the present invention, but the examples are not intended to limit the present invention.
Referring to fig. 1, the present invention provides an apparatus for preparing a rare earth metal or alloy rotary target, which includes a reaction chamber body 100, wherein the reaction chamber body 100 is a closed chamber, and at least one pumping hole 140 is formed in the reaction chamber body 100. At least one casting device 110 is arranged in the reaction box body 100, the casting device 110 is suspended in the reaction box body, and the casting device 110 comprises an outer wall 111, a separable top plate 112 and a bottom plate 113, an inner cavity 114 and a heating device 115. Heating device 115 encircles the setting in outer wall 111 periphery, and cylindric inner chamber 114 sets up in the inside of outer wall, vertical installation on bottom plate 113, and bottom plate 113 can be dismantled with inner chamber 114 and be connected, but inner chamber 114 relative outer wall 111 vertical movement, and disposable material or reusable material can be selected for use according to the material to the inner chamber.
The heating device 115 is divided into an upper heating device and a lower heating device, which can independently perform heating. That is, the upper heating means and the lower heating means may be set to the same or different temperatures, so that the heating means 115 can achieve various heating states. In the process of smelting the metal or the alloy, the upper part and the lower part can be simultaneously heated or only an upper heating device or a lower heating device is arranged for heating independently according to the requirement. The temperature can be set to be the same or different when the upper and lower parts are heated simultaneously. During the forming process of the metal or the alloy, the upper heating device keeps the smelting temperature, and the lower heating device reduces the temperature to ensure that the bottom of the metal or the alloy is firstly solidified and simultaneously keeps the high-temperature molten state of the metal. After complete solidification, the material 400 and the cavity 114 can be moved out of the outer wall 111 together with the bottom plate 113 by moving the bottom plate 113 longitudinally by the driving rod. The heating device adjusts the heating power through the power meter, controls the temperature, and if accurate temperature control is needed, a real-time temperature measuring system can be added, and the power is adjusted in real time through a computer.
A detachable top plate 112 and a detachable bottom plate 113 are provided directly above and below the outer wall 111, respectively. The top plate 112 is smaller than the inner diameter of the outer wall 111 and is longitudinally moved by the drive rod 116. When the casting device is in an uncapped state, the top plate is separated from the outer wall, and materials can be added. When the top plate is embedded in the outer wall, the casting device is in a closed state, and a pushing force is applied in a vertical direction to push the material and the inner cavity 114 out of the outer wall 111. Preferably, the diameter of the top plate is designed to be 1-2cm smaller than the inner diameter of the outer wall, so that the demolding of the workpiece is facilitated, the workpiece is not easy to deform, and the residual quantity on the outer wall is small.
The bottom plate 113 of the casting device is not smaller than the outer diameter of the outer wall 111, when the outer wall 111 and the bottom plate 113 are in a closed state, as shown in fig. 2, the bottom plate and the outer wall are matched to form an accommodating space, and a sealing structure is arranged at the matching position between the bottom plate and the outer wall to prevent liquid leakage. When the melting is finished and the material is formed, the driving rod is controlled to move the bottom plate 113 longitudinally and downwards to the position right below the melting and casting device, at this time, the outer wall 111 and the bottom plate 113 are separated, and the material and the inner cavity are moved out of the outer wall 111 together, as shown in fig. 3, a schematic diagram of a second state of the equipment is shown.
An inert gas supply device 200 is provided outside the reaction chamber body 100, and a gas supply pipe of the inert gas supply device 200 is communicated with the pumping port 140. The gas control device 201 can be manually opened and closed, or can be connected with a furnace gas pressure detection device through a computer to be automatically opened and closed. The vacuum extractor 300 is located outside the reaction chamber 100, and the exhaust tube of the vacuum extractor 300 is communicated with the exhaust port 140 of the reaction chamber 100. The vacuum control device 301 can be manually opened and closed, or can be connected with a furnace air pressure detection device through a computer to be automatically opened and closed. According to actual conditions, the vacuumizing device and the inert gas device can be communicated by adopting the same air pumping hole, or the air pumping holes can be respectively and independently arranged, and the less the air pumping hole is, the more the airtightness is easy to achieve.
A feeding device 130 is arranged in the reaction box 100, and the feeding device 130 comprises a driving rod 132 and a feeding hopper 131 fixed on the driving rod; the hopper 131 is used for adding volatile components or increasing the feeding amount of a single furnace; the driving rod 132 can perform parallel contraction movement along the horizontal direction and can perform rotation movement along the axis thereof, and the hopper 131 performs parallel movement and/or rotation movement along the driving rod to pour the material in the hopper 131 into the casting device 110.
The reaction chamber body 100 is provided with an observation and temperature measurement window 120. The device of the invention is provided with peripheral equipment such as a power supply, a temperature control system, a cooling system, a vacuum degree control system and the like, which are not shown in figures 1-3.
A preparation method of a rare earth metal or alloy rotary target material comprises the following steps:
s1 sample preparation: the drive rod is operated to set the bottom plate 113 and the top plate 112 to the first state, so that the upper part of the casting device is open and the bottom part is closed. The sampled rare earth metal material 400 is filled between the inner cavity 114 and the outer wall 111.
S2 cleaning: opening the pumping hole 140 and the vacuum extractor 300 on the reaction box 100, and pumping vacuum to the reaction box 100 to remove impurities in the reaction cavity until the vacuum degree in the reaction box 100 reaches 10-10-3When Pa, the vacuum-pumping device 300 is turned off, and the inert gas supply device 200 is turned on to fill the inert gas, so that the reaction chamber 100 is under the protection of the inert gas. Inert protective gas is filled in the reactor to prevent the materials from being oxidized at high temperature. And when the pressure of the inert gas in the reaction box body 100 reaches 10-90 KPa, closing the inert gas supply device 200.
S3 feeding: the prepared materials are respectively placed in the casting device 110 and the feeding device 130. The material can be added by the feeding device according to the requirement in the smelting process.
S4 smelting: the temperature of the casting device 110 is adjusted to be 30-100 ℃ above the melting point of the material by the heating device 115, so that the material is heated and melted to obtain a crude metal or alloy melt. The inner chamber 114 may be a disposable material or a reusable material depending on the material. Further, during the smelting process, the second portion of raw materials can be added by adding materials through the feeding device 130 as needed. After the second part of the raw material is completely melted, the purification step is carried out. If the melting point of the second part of raw materials is different from that of the first part of raw materials greatly, the heating power is reduced on the basis of the original set temperature (the set temperature is reduced when automatic temperature control is adopted), then the second part of raw materials are added immediately, the melting process is utilized to reduce the temperature, and meanwhile, the first part of raw materials is not solidified.
S5 purification: through the observation port 120, after the materials are observed to be completely melted, the vacuumizing device 300 is started to vacuumize the reaction box body 100, remove low-boiling-point impurities generated in the melting process, and refine the molten metal to obtain refined metal or alloy melt. The vacuum degree in the reaction box body 100 is 10-10-3And Pa, the vacuum-pumping device 300 is closed. In the purification process, the temperature of the heating device is controlled to be 30-200 ℃ above the melting point of the material, and inert gas can be filled and vacuum-pumped for refining for multiple times according to the impurity requirements of the product.
S6 forming: the temperature of the casting device 110 is adjusted to be 30-100 ℃ below the melting point through the heating device 115, the temperature of the heating device at the lower part is firstly reduced, the temperature of the heating device at the upper part is slightly higher than the temperature of the heating device at the lower part by 20-50 ℃, and a product at the bottom of the casting device is firstly solidified, so that liquid leakage during demolding is avoided. And (4) finishing demoulding within 1-3 min after confirming that the upper surface of the material is solidified through the observation port 120, otherwise, causing difficulty in subsequent demoulding. The actuator rod is operated to move the base plate 113 longitudinally downward to separate the base plate from the outer wall, i.e., from the first state to the second state. And cooling to room temperature to obtain the rare earth metal or alloy rotary target blank, processing, and binding on a sputtering back plate to obtain the rotary target. The drive rod is also operable to move the top plate 112 longitudinally into engagement with the outer wall during stripping, applying a pushing force in a vertical direction to assist stripping.
Example 1
According to the preparation steps of the rare earth metal or alloy rotary target material, equipment is adjusted, the prepared metal praseodymium block is placed in a casting device, a graphite mold is selected as an inner cavity, an inert gas device is opened after vacuumizing and impurity removing, argon is filled in the inert gas device, and vacuum melting is started (the argon protection pressure is-0.7 MPa). The heating device adopts a lower heating device mode, and the temperature is increased to 950-1000 ℃. The upper part and the lower part can be heated simultaneously and selected according to requirements. The smelting situation is observed through the observation hole 120, partial materials can be supplemented by the feeding device according to the product requirements, and the molten metal is purified and refined after the supplemented materials are completely melted.
Starting a vacuumizing device, vacuumizing to remove low-boiling-point impurities generated in the smelting process, wherein the vacuum degree in the reaction box body 100 is 10-10-3And Pa, the vacuum-pumping device 300 is closed. The steps of filling inert gas and vacuumizing can be carried out for a plurality of times according to the impurity requirements of the product to purify and refine the molten metal. In the purification process, the temperature of the heating device is controlled to be 30-200 ℃ above the melting point of the material. According to different rare earth types, the temperature control range of the heating device is 1000-1800 ℃, for example, the melting point of metal praseodymium is 931 ℃, and the temperature of the praseodymium target material is 1000-1100 ℃; the melting point of terbium metal is 1356 ℃, and the temperature is controlled to be 1400-1550 ℃; metal scandium meltAt 1663 ℃, and controlling the temperature to be 1690-1800 ℃.
After purification is finished, the temperature of the heating device at the lower part is firstly reduced by the heating device, so that the temperature of the casting device is reduced to 850-900 ℃, and meanwhile, the temperature of the heating device at the upper part is slightly higher than that of the heating device at the lower part. Through the observation hole 120, after the solidification of the upper surface of the material is confirmed, the driving rod is operated to change the bottom plate 113 from the first state to the second state, at the moment, the bottom of the casting device is in an open state, meanwhile, the driving rod is operated to embed the top plate 112 into the outer wall 111 to apply downward thrust, and the demolding is completed within 1-3 min. After the product is completely solidified, the product is pushed to the lower part of the melt casting device, the graphite is stripped after the product is cooled and discharged out of the furnace, and the relative density of the product is measured by a solid density tester to be 99.5 percent. The closer the product density is to the theoretical density, the less the internal defects of the product are, generally 99% can meet the use requirement, and the higher-quality product needs to reach 99.5%. And processing the obtained target blank into the required size and precision, and binding the target blank on a stainless steel pipe to obtain the metal praseodymium rotary target. And weighing the product finally bound to the stainless steel pipe, and dividing the weighed product by the weight of the blank obtained by the method to calculate the yield to 90%.
Example 2
According to the preparation steps of the rare earth metal or alloy rotary target material, equipment is adjusted, a prepared metal terbium block (the melting point of terbium is 1356 ℃ and the boiling point of terbium is 3230 ℃) is placed into a casting device, metal dysprosium (the melting point of dysprosium is 1412 ℃ and the boiling point of dysprosium is 2562 ℃) is placed into a feeding hopper, a tungsten mold is used as an inner cavity, an inert gas device is opened after vacuumizing and impurity removal, argon is filled into the inert gas device, vacuum melting is started (the argon protection pressure is-0.7 MPa), and a heating device adopts a lower part heating mode and is heated to 1400-1450 ℃. After terbium is melted, a metal dysprosium block is fed into the casting device by using a feeding device, and because dysprosium has a higher melting point than terbium but a lower boiling point than terbium, the loss of dysprosium can be reduced by separately feeding. After the melting is completed, the molten metal is purified and refined.
Starting a vacuumizing device, vacuumizing to remove low-boiling-point impurities generated in the smelting process, wherein the vacuum degree in the reaction box body 100 is 10-10-3When Pa, the vacuum pumping is closedAn apparatus 300. In the purification process, the temperature of the heating device is controlled to be 30-200 ℃ above the melting point of the material at 1440-1550 ℃. The steps of filling inert gas and vacuumizing can be carried out for a plurality of times according to the impurity requirements of the product to purify and refine the molten metal.
After the purification is finished, the temperature of the heating device at the lower part is firstly reduced to 1300-1350 ℃, and meanwhile, the temperature of the heating device at the upper part is slightly higher than that of the heating device at the lower part. Through the observation hole 120, after the solidification of the upper surface of the material is confirmed, the driving rod is operated to change the bottom plate 113 from the first state to the second state, at the moment, the bottom of the casting device is in an open state, meanwhile, the driving rod is operated to embed the top plate 112 into the outer wall 111 to apply downward thrust, and the demolding is completed within 1-3 min. After the product is completely solidified, the product is pushed to the lower part of the melt casting device, the inner cavity is stripped after the product is cooled and discharged out of the furnace, and the relative density of the product is measured to reach 99.8 percent by adopting a solid density tester; the obtained target is processed into the required size and precision and is bound on a stainless steel tube to obtain the metal praseodymium rotary target, and the yield reaches 92%.
While the invention has been described with reference to specific embodiments, it will be understood by those skilled in the art that various changes in form and details may be made therein without departing from the spirit and scope of the invention. Therefore, the scope of the present invention should not be limited to the embodiments disclosed, but includes various alternatives and modifications without departing from the present invention, which are encompassed by the claims.
Claims (9)
1. A preparation equipment of rare earth metal or alloy rotary target material is characterized in that: the equipment comprises a reaction box body (100), wherein the reaction box body (100) is a closed cavity, a casting device (110) is arranged in the reaction box body (100), and at least one pumping hole (140) is formed in the reaction box body (100);
the fusion casting device (110) comprises an outer wall (111), an inner cavity (114), a separable top plate (112) and a bottom plate (113); the casting device (110) is arranged in the reaction box body in a suspended mode;
a heating device (115) is arranged around the periphery of the outer wall (111);
the top plate (112) is arranged right above the outer wall (111) and longitudinally moves through the driving rod (116), and the top plate (112) is smaller than the inner diameter of the outer wall (111) and can be embedded into the outer wall to apply thrust in the vertical direction;
the bottom plate (113) is arranged right below the outer wall (111) and longitudinally moves through the driving rod (117), the outer diameter of the outer wall (111) is not required to be smaller than that of the bottom plate (113), and the bottom plate and the outer wall are matched to form an accommodating space for placing materials;
the inner cavity (114) is cylindrical and is vertically arranged on the bottom plate (113), and the bottom plate (113) is detachably connected with the inner cavity (114).
2. The apparatus for preparing rare earth metal or alloy rotary target material according to claim 1, wherein: the heating device (115) is divided into an upper heating device and a lower heating device which can respectively and independently heat.
3. The apparatus for preparing rare earth metal or alloy rotary target material according to claim 1, wherein: and a base is arranged on the bottom plate (113) and used for fixing the position of the inner cavity (114).
4. The apparatus for preparing rare earth metal or alloy rotary target material according to claim 1, wherein: and a sealing structure is arranged at the matching position between the bottom plate and the outer wall to prevent liquid leakage.
5. The apparatus for preparing a rare earth metal or alloy rotary target according to claims 1-4, wherein: the device is characterized by further comprising a feeding device (130), wherein a feeding hopper (131) is arranged on the feeding device (130) and fixedly connected with the feeding device through a driving rod (132); the driving rod (132) can perform parallel contraction motion along the horizontal direction and can perform rotation motion along the axis of the driving rod.
6. The apparatus for preparing rare earth metal or alloy rotary target material according to claim 1, wherein: an observation and temperature measurement window (120) is arranged on the reaction box body (100).
7. The apparatus for preparing rare earth metal or alloy rotary target material according to claim 1, wherein: the outside of the reaction box body (100) is connected with an inert gas supply device (200) and a vacuum-pumping device (300); a gas supply pipe of the inert gas supply device (200) is communicated with the pumping hole (140);
the air exhaust pipe of the vacuum-pumping device (300) is communicated with the air exhaust port (140).
8. A method for manufacturing a rare earth metal or alloy rotary target material is characterized by comprising the following steps:
a smelting step: after the metal material is filled, vacuumizing, and setting the temperature of a heating device (115) to be 30-100 ℃ above the melting point of the material to obtain a crude metal or alloy melt;
a purification step: after the materials are completely melted, starting a vacuumizing device (300) to vacuumize again for purification;
a forming step: setting the temperature of the heating device (115) to be 30-100 ℃ below the melting point; firstly, lowering a lower heating device, and simultaneously keeping the temperature of the upper heating device slightly higher than that of the lower heating device by 20-50 ℃;
after the solidification of the surface of the material is confirmed, demolding is completed within 1-3 min; and after cooling to room temperature, stripping the inner cavity and processing to obtain the rare earth metal or alloy rotary target material.
9. The method for manufacturing a rare earth metal or alloy rotary target according to claim 8, wherein: the prepared materials are respectively placed in a casting device (110) and a feeding device (130) before the smelting step, and the materials are added by the feeding device according to needs in the smelting process.
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| CN115074681A (en) * | 2022-06-21 | 2022-09-20 | 许杰富 | Rare earth metal rotary target material preparation equipment |
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| JP2014105359A (en) * | 2012-11-28 | 2014-06-09 | Jx Nippon Mining & Metals Corp | Method for producing high purity neodymium, high purity neodymium, sputtering target produced by using high purity neodymium, permanent magnet including high purity neodymium as component |
| JP2015134377A (en) * | 2015-03-02 | 2015-07-27 | Jx日鉱日石金属株式会社 | Melting continuous casting apparatus for high purity ingot and melting continuous casting method for high purity ingot |
| CN106637100A (en) * | 2015-10-30 | 2017-05-10 | 有研稀土新材料股份有限公司 | Rare-earth metal target material and preparation method thereof |
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| JPH01156467A (en) * | 1987-12-14 | 1989-06-20 | Seiko Epson Corp | Manufacture of sputtering target |
| CN101133181A (en) * | 2005-03-10 | 2008-02-27 | 株式会社爱发科 | Method for producing a target |
| JP2014105359A (en) * | 2012-11-28 | 2014-06-09 | Jx Nippon Mining & Metals Corp | Method for producing high purity neodymium, high purity neodymium, sputtering target produced by using high purity neodymium, permanent magnet including high purity neodymium as component |
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| CN115074681A (en) * | 2022-06-21 | 2022-09-20 | 许杰富 | Rare earth metal rotary target material preparation equipment |
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