CN112962070A - Preparation equipment and preparation method of sputtering target material - Google Patents
Preparation equipment and preparation method of sputtering target material Download PDFInfo
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- CN112962070A CN112962070A CN202110142206.8A CN202110142206A CN112962070A CN 112962070 A CN112962070 A CN 112962070A CN 202110142206 A CN202110142206 A CN 202110142206A CN 112962070 A CN112962070 A CN 112962070A
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- 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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22C—FOUNDRY MOULDING
- B22C9/00—Moulds or cores; Moulding processes
- B22C9/22—Moulds for peculiarly-shaped castings
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
- B22D21/00—Casting non-ferrous metals or metallic compounds so far as their metallurgical properties are of importance for the casting procedure; Selection of compositions therefor
- B22D21/02—Casting exceedingly oxidisable non-ferrous metals, e.g. in inert atmosphere
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- 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
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- 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
- B22D27/09—Treating the metal in the mould while it is molten or ductile ; Pressure or vacuum casting by using pressure
- B22D27/11—Treating the metal in the mould while it is molten or ductile ; Pressure or vacuum casting by using pressure making use of mechanical pressing devices
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
- B22D46/00—Controlling, supervising, not restricted to casting covered by a single main group, e.g. for safety reasons
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
- B22D47/00—Casting plants
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- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- C21D1/00—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
- C21D1/26—Methods of annealing
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F27—FURNACES; KILNS; OVENS; RETORTS
- F27B—FURNACES, KILNS, OVENS, OR RETORTS IN GENERAL; OPEN SINTERING OR LIKE APPARATUS
- F27B14/00—Crucible or pot furnaces
- F27B14/04—Crucible or pot furnaces adapted for treating the charge in vacuum or special atmosphere
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F27—FURNACES; KILNS; OVENS; RETORTS
- F27B—FURNACES, KILNS, OVENS, OR RETORTS IN GENERAL; OPEN SINTERING OR LIKE APPARATUS
- F27B14/00—Crucible or pot furnaces
- F27B14/06—Crucible or pot furnaces heated electrically, e.g. induction crucible furnaces with or without any other source of heat
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F27—FURNACES; KILNS; OVENS; RETORTS
- F27B—FURNACES, KILNS, OVENS, OR RETORTS IN GENERAL; OPEN SINTERING OR LIKE APPARATUS
- F27B14/00—Crucible or pot furnaces
- F27B14/08—Details peculiar to crucible or pot furnaces
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F27—FURNACES; KILNS; OVENS; RETORTS
- F27D—DETAILS OR ACCESSORIES OF FURNACES, KILNS, OVENS, OR RETORTS, IN SO FAR AS THEY ARE OF KINDS OCCURRING IN MORE THAN ONE KIND OF FURNACE
- F27D27/00—Stirring devices for molten material
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F27—FURNACES; KILNS; OVENS; RETORTS
- F27B—FURNACES, KILNS, OVENS, OR RETORTS IN GENERAL; OPEN SINTERING OR LIKE APPARATUS
- F27B14/00—Crucible or pot furnaces
- F27B14/04—Crucible or pot furnaces adapted for treating the charge in vacuum or special atmosphere
- F27B2014/045—Vacuum
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Abstract
The invention discloses a preparation device and a preparation method of a sputtering target material, wherein the preparation device comprises the following steps: comprises a closed cavity, a smelting and pouring device, a casting and forming device and an atmosphere treatment device; the smelting pouring device and the casting forming device are positioned in the closed cavity; the atmosphere treatment device is connected with the closed cavity through a pipeline; and conveying protective atmosphere to the closed cavity. Through the combined action of the smelting device, the casting forming device and the clean atmosphere device, unnecessary pollution brought by processing links in the smelting, stirring, cooling and forming processes is reduced, good conditions such as proper temperature, cooling speed, pressure, atmosphere and the like are provided for material preparation, the impurity content of the prepared high-purity material can be effectively controlled in the whole preparation process, and the prepared high-purity material is uniformly fused and controllably cooled and formed.
Description
Technical Field
The invention relates to a preparation device and a preparation method of a sputtering target material, and belongs to the technical field of metal material preparation.
Background
The high-purity sputtering target mainly refers to a metal or nonmetal target with the purity of 99.9-99.9999% (between 3N-6N), and is a key material for preparing surface electronic films of panels, wafers, solar cells and the like. Among them, semiconductor wafers and chips have the highest technical requirements for sputtering targets. Since the quality of the sputtering target directly affects the uniformity and performance of the conductive layer and the barrier layer of the wafer, and further affects the transmission speed and stability of the whole chip, the target is one of the core raw materials for semiconductor production.
The sputtering target for semiconductors has extremely strict standards in terms of purity of metal material, internal microstructure, and the like. If the content of impurities in the sputtering target is too high, particles are easily formed on a wafer in the sputtering process, so that a circuit is short-circuited or damaged, and the performance of the film is seriously influenced. Therefore, the machining process of the sputtering target is extremely strictly controlled, and the target with high quality is expected to be finally machined. The production of the target material needs to be processed by a plurality of processes, generally, metal raw materials are smelted and cast, and the obtained ingot or blank is subjected to plastic processing, welding, machining, cleaning and other steps to finally prepare the target material. The smelting and the casting are key steps for preparing the target material, directly influence and determine the purity and the original structure of the target material, and are the basis for improving the quality of materials by subsequent processing.
In the prior art, a high-purity target material is prepared by a high vacuum melting technology and can be used for preparing a blank of a single-metal target material with a simple structure; the powder metallurgy blank making technology is used for preparing refractory metal target materials, but the oxygen content is difficult to control effectively, so that the oxygen content of the metal target materials is higher. When the common vacuum melting technology is adopted to prepare the multi-element alloy target material, the defects of high impurity content, element segregation, incompact tissue, fragile blank and the like are easily caused due to the fusion of multiple elements, the mutual influence and action among elements, phases and intermetallic compound characteristics in the alloy, so that the multi-element alloy target material is difficult to prepare the qualified blank through the conventional melting technology. Therefore, there is a need to develop a method and apparatus for preparing a new high-purity material, especially a method and apparatus for preparing a high-purity alloy target.
Disclosure of Invention
The invention aims to overcome the defects and shortcomings of the prior art and provides a preparation device and a preparation method of a sputtering target. The equipment provided by the invention integrates a smelting device for heating, melting and uniformly stirring a high-purity material melt, a casting molding device for casting and molding the melt and implementing speed-controlled cooling, a clean space device for atmosphere protection of a processing area and a processing material and other auxiliary facilities for ensuring the normal operation of the system, reduces unnecessary pollution caused by processing links in the processes of smelting, stirring, cooling and molding through the combined action of the smelting device, the casting molding device and the clean atmosphere device, provides proper conditions of temperature, cooling speed, pressure, atmosphere and the like for material preparation, ensures that the prepared high-purity material can effectively control the content of impurities in the whole preparation process, and is uniformly fused and controllably cooled and molded.
In order to achieve the purpose, the invention adopts the following technical scheme:
the invention relates to preparation equipment of a sputtering target, which comprises a closed cavity, a smelting and pouring device, a casting and forming device and an atmosphere treatment device; the smelting pouring device and the casting forming device are positioned in the closed cavity; the atmosphere treatment device is connected with the closed cavity through a pipeline; conveying protective atmosphere to the closed cavity;
the melting and pouring device consists of a crucible, a melting and heating device, a melt stirring device and a crucible rotating device; the melting heating device is used for heating materials in the crucible, the crucible rotating device is used for enabling the crucible to rotate, and the melt stirring device is used for stirring melts in the crucible.
In the invention, the smelting and pouring device and the casting and forming device are both positioned in the closed cavity, and the atmosphere treatment device is connected with the closed cavity through a pipeline; and conveying protective atmosphere to the closed cavity, so that smelting, pouring and casting molding are carried out under the protective atmosphere, wherein the smelting and pouring device consists of a crucible, a smelting and heating device, a melt stirring device and a crucible rotating device, the metal material can be rapidly melted and uniformly stirred under the condition of no environmental pollution, and homogeneous melt with low impurity content is obtained.
Preferably, the smelting heating device is selected from a medium-frequency or high-frequency induction coil heating device or a vacuum arc heating device; the vacuum arc heating device is preferably a consumable electrode vacuum arc heating device.
When the crucible is heated by adopting the medium-frequency or high-frequency induction coil heating device, the temperature rise rate of the material in the crucible can be 50-600 ℃/s, the temperature deviation at constant temperature is not higher than 100 ℃, and more preferably the temperature deviation at constant temperature is not higher than 20 ℃, so that the material is ensured to be rapidly melted and is subjected to constant temperature treatment at the specified temperature.
When the vacuum arc heating device is adopted, the temperature rise rate of the material in the crucible can be 50-1000 ℃/s, the temperature deviation at constant temperature is not higher than 100 ℃, and further preferably the temperature deviation at constant temperature is not higher than 20 ℃, so that the material is rapidly melted and is subjected to constant temperature treatment at the specified temperature.
The preferred consumable electrode vacuum arc heating device further reduces the risk of unnecessary contamination of the electrodes.
Preferably, the melt stirring device is a consumable stirrer stirring device.
The melt flow is stirred in a mode of mechanically stirring the melt by taking the preparation material as a stirrer, so that the uniformity of the melt is improved, and unnecessary pollution risks are reduced;
in a preferred scheme, the crucible is a water-cooled copper crucible.
The water-cooled copper crucible has low temperature under the action of water cooling, so that the melt is in a near suspension state in the metal material smelting state, the crucible is not or less contacted with the melt material, and the melt and the crucible are ensured not to react.
In a preferable scheme, a ceramic film is deposited on the inner surface of the crucible, and the thickness of the ceramic film is 0.5-10 μm.
Further preferably, the ceramic film is selected from a boron nitride film or an aluminum nitride film.
The ceramic film on the inner surface of the crucible does not react with the melt material to provide isolation.
Preferably, the crucible rotating device is used for rotating the crucible and pouring and discharging the crucible to the casting forming device. The crucible is rotated by the crucible rotating device for fixed-point pouring, the melted melt is transferred to the cooling mold, on one hand, the discharging process can be evolved, and on the other hand, continuous discharging can be realized.
According to the preferred scheme, the casting forming device comprises a casting blank die, a cooling and stirring device, an upper pressing forming device, a lower pressing forming device, a blank heat preservation device, a die supporting column and a die tray; the bottom edge of the casting blank mold is fixed on a mold tray, the lower part of the mold tray is supported by a mold support column, the upper pressing forming device is positioned right above the casting blank mold, the lower pressing forming device is positioned right below the casting blank mold, the upper pressing forming device and the lower pressing forming device can move up and down, apply pressure to the casting blank mold and push the cooled and formed blank to a blank heat preservation device from the casting blank mold, and the blank heat preservation device is positioned below the casting blank mold; the cooling and stirring device surrounds the outer side of the die and provides non-contact stirring for the melt in the casting blank die.
The casting molding device provided by the invention is used for controlling the cooling speed after a melt is poured into a mold, and has the functions of pressure, mold constraint, blank heat preservation and the like in the molding process, and the provided compression molding mode is to carry out cooling molding under the specified pressure of the upper compression molding device and the lower compression molding device and the constraint condition of the mold; after the blank is cooled and formed, the blank can be pushed to the heat preservation device from the die by the upper pressing forming device to be annealed, and the die is still kept at the original position after being fixed by the die supporting column and the die tray.
Further preferably, the cooling stirring device is selected from a vibrating stirring device or an electromagnetic stirring device.
The cooling stirring device surrounds the outer side of the die and provides non-contact stirring for the melt in the casting blank die, and the timely stirring device aims to reduce or eliminate the segregation phenomenon caused by local cooling solidification of the blank in the cooling process and is beneficial to uniform nucleation and solidification of the material.
Preferably, a circulating cooling water pipeline is arranged on the outer side of the casting blank die.
A circulating cooling water pipeline is arranged on the outer side of the casting blank die and is used for introducing cooling water to cool the casting blank die, and the melt is rapidly cooled at a controllable cooling speed after being poured into the die.
In the preferred scheme, the blank heat preservation device adopts a resistance wire heating mode or an intermediate frequency induction heating mode.
The rated temperature of the blank heat preservation device is 600 ℃, 900 ℃ or 1300 ℃; the accuracy of the rated temperature is +/-5 ℃.
The rated temperature of the blank heat preservation device is selected according to the annealing temperature required actually, the rated temperature is not lower than the annealing temperature, but the rated temperature is too high, the requirement of the heat preservation device is higher, generally, a closer temperature is selected, the blank heat preservation device can carry out annealing treatment on the blank in time, the occurrence of the cracking phenomenon of the blank is reduced, a certain homogenization treatment effect is achieved, and the medium-frequency induction heating mode also has the advantage of high heating speed.
Preferably, the atmosphere treatment device comprises a circulating atmosphere device, an atmosphere cleaning device, an atmosphere temperature control device and a vacuum pumping device; the atmosphere circulating device comprises a protective atmosphere one-way valve, an atmosphere circulating pump and a protective atmosphere storage device; the protective atmosphere check valve controls the supply of protective atmosphere; one end of the atmosphere circulating pump is connected with the protective atmosphere storage device, the other end of the atmosphere circulating pump is connected with the atmosphere cleaning device through a pipeline, a protective gas source is conveyed to the atmosphere cleaning device, and oxygen removal, impurity removal and dust reduction are carried out on the protective atmosphere; one end of the atmosphere cleaning device is connected with the atmosphere temperature control device through a pipeline, and the temperature of the clean atmosphere from the atmosphere cleaning device is adjusted; the other end of the atmosphere cleaning device is connected with the sealed cavity and used for conveying the protective atmosphere subjected to temperature regulation to the sealed cavity, and the vacuum pumping device is connected with the sealed cavity through a pipeline and used for vacuumizing the sealed cavity.
The atmosphere treatment device can provide a high-vacuum environment for the closed cavity, ensure that the material is smelted and cast in the heated state in the cavity and can be subjected to high-vacuum treatment, and is protected by the circularly clean atmosphere, and the protective atmosphere can play a role in quick cooling and constant temperature through temperature regulation.
In the invention, the sealed cavity can be filled with specified atmosphere and the atmosphere in the cavity is promoted to circulate by the atmosphere circulating device; the protective atmosphere is selected from one of high-purity nitrogen and high-purity argon.
Preferably, the atmosphere circulating pump is a high-temperature gas circulating pump, and the service temperature of the high-temperature gas circulating pump is less than or equal to 600 ℃.
Further preferably, the atmosphere cleaning device comprises a dust removal device and an oxygen removal device, wherein the oxygen removal device contains an oxygen removal purification material, the oxygen removal purification material is selected from oxygen absorption metals, and the oxygen absorption metals are selected from at least one of lithium, sodium, calcium and rare earth elements.
In the invention, the form of the strong oxygen absorption metal is powder, melt or porous material; in order to ensure the strong oxygen absorption effect, the oxygen-removing purification material can be heated and can be added or replaced at proper time.
Preferably, the vacuum pumping device comprises a vacuum pumping device and a vacuum valve, and the vacuum pumping device is selected from a mechanical pump, a roots pump and a diffusion pump three-stage vacuum pump.
The original atmosphere in the sealed cavity can be pumped by the vacuum pumping device, so that the original atmosphere in the cavity can be pumpedThe vacuum degree reaches 1 x 10-2Pa below, high sealing performance of the sealed cavity, and the pressure rise rate of the air pressure in the cavity in the sealed state is not more than 2Pa/h, preferably the vacuum degree in the cavity reaches 6 multiplied by 10-3Pa below, and the pressure rise rate of the air pressure in the cavity is not more than 0.5Pa/h in a sealed state.
According to the preferred scheme, the atmosphere temperature control device consists of an atmosphere cooling device, an atmosphere heating device, an atmosphere temperature control device and a one-way valve, and the range of the atmosphere temperature control device for adjusting the temperature of the protective atmosphere is-50-600 ℃.
According to the invention, the temperature of the protective atmosphere passing through the atmosphere temperature control device is regulated and controlled by the atmosphere temperature control device, so that the protective atmosphere with the temperature range of-50-600 ℃ can be provided.
The temperature is controlled timely by an intelligent temperature control system; the temperature of the atmosphere can be adjusted to adjust the cooling speed of the melt and the blank at different stages, so that the blank is cooled at a controlled speed at the stage of the cooling and forming process of the casting and forming part.
The invention also provides a method for preparing the sputtering target material by applying the equipment, which comprises the following steps of placing the sputtering target material into a crucible, and vacuumizing the sealed cavity to ensure that the vacuum degree in the sealed cavity is less than or equal to 5 multiplied by 10-3Pa; and then introducing a room-temperature circulating protective atmosphere into the sealed cavity, heating the crucible to melt the raw material of the sputtering target material, fully melting, preserving the heat of the melt, stirring the melt in the heat preservation process, rotating the crucible after heat preservation is finished, pouring the melt into a casting mold, simultaneously carrying out non-contact stirring, controlling the temperature of the introduced protective atmosphere in the pouring process to be-50-600 ℃, pressurizing a casting blank mold after pouring is finished, controlling the temperature of the introduced protective atmosphere in the pressure preservation process to be 100-600 ℃, pushing the obtained blank into a blank heat preservation device for annealing after pressure preservation is finished, and cooling to room temperature after annealing treatment to obtain the sputtering target material.
Preferably, the non-contact stirring is vibration stirring or electromagnetic stirring, and preferably electromagnetic stirring. The inventors have found that non-contact stirring of the melt during casting results in a more homogeneous texture of the final material.
In the preferable scheme, the pressure for pressurizing the casting blank die is 1-100 MPa, and the pressure maintaining time is 1-20 min.
Preferably, the protective atmosphere is treated by an atmosphere cleaning device, and the oxygen partial pressure is less than 0.01Pa, preferably less than 0.001Pa, and more preferably less than 0.0001 Pa.
Further preferably, when the sputtering target is selected from high-melting-point-difference alloys, the temperature of the introduced protective atmosphere in the casting process is controlled to be-50-20 ℃, and preferably-20-0 ℃.
Further preferably, when the sputtering target is selected from a high melting point difference alloy, the casting blank mold is water-cooled during casting.
The high melting point difference alloy in the invention contains a high melting point phase and a low melting point phase, wherein the melting point difference between the high melting point phase and the low melting point phase is more than 100 ℃, and the high melting point phase accounts for 5-90% of the weight of the whole alloy, such as Al-Ti, Al-Cr, Al-Ni, aluminum rare earth alloy and the like with the high melting point phase element accounting for 5-35%.
Further preferably, when the sputtering target is selected from easily deformable pure metals or alloys with the alloy content not higher than 5%, the temperature of the introduced protective atmosphere is controlled to be 20-200 ℃; the easily deformable pure metal is selected from at least one of aluminum, magnesium, copper, titanium and rare earth.
Further preferably, when the sputtering target material is selected from a hard-to-deform pure metal or an intermetallic compound, the temperature of the protective atmosphere is controlled to be 200-600 ℃, the hard-to-deform pure metal is selected from at least one of chromium, niobium and tantalum, and the hard-to-deform intermetallic compound is selected from at least one of Al-Ti, Al-Cr, Al-Ni and aluminum rare earth alloy with 100 percent of intermetallic compound phase with the melting point higher than 1300 ℃.
Further preferably, when the sputtering target is selected from a hard-to-deform pure metal or an intermetallic compound, the temperature of the casting die is controlled to 200 ℃ to 600 ℃.
The method for preparing the sputtering target material has three stages in the casting and forming process, including the stage 1: the melt is poured from the crucible into the mould and the solidification period is the solidification stage of the melt (i.e. the pouring stage)
And (2) stage: pressurizing a casting blank die and maintaining pressure to obtain a blank densification stage;
and (3) stage: the blank annealing period in the heat preservation device is a blank annealing stage, and the three stages are subjected to staged speed-controlled cooling.
Stage 1: in the melt solidification stage, three different cooling speeds of quick cooling, intermediate cooling or slow cooling are selected according to different processing materials, the cooling speed is controlled by controlling the temperature of protective atmosphere in the whole process, the lower the temperature is, the higher the cooling speed is, wherein a quick cooling mode is selected when a high-melting-point-difference alloy is smelted into a casting blank, the temperature of the introduced protective atmosphere is controlled to be-50-20 ℃, preferably-20-0 ℃, a casting blank mold is preferably a water-cooling mold, the high-melting-point-difference alloy contains a high-melting-point phase and a low-melting-point phase, the melting point difference is more than 100 ℃, the high-melting-point phase accounts for 5-90% of the weight of the whole alloy, such as Al-Ti, Al-Cr, Al-Ni and aluminum rare earth alloy with 5-35% of alloy elements, and the melt is quickly solidified and segregation and the like are reduced by quick cooling in the; for easily deformable pure metals such as aluminum, magnesium, copper, titanium, rare earth and the like or alloys with the alloy content not higher than 5%, a cold cooling mode is selected when a casting blank is smelted, the temperature of protective atmosphere is controlled to be 20-200 ℃, a casting blank die is a normal-temperature die, and the normal cooling speed in the solidification process can meet the requirement of the casting blank; for other hard-to-deform pure metals or intermetallic compounds, a slow cooling mode is selected when a casting blank is smelted, the temperature of introduced protective atmosphere is controlled to be higher than 200 ℃, a casting blank mold is a high-temperature mold, casting defects such as segregation, porosity, cracks and the like are easily caused due to the high fast flow of a cooling melt in the solidification process, and a slow cooling speed is needed;
and (2) stage: in the blank densification stage, the introduced protective atmosphere is controlled to be a circularly clean high-temperature atmosphere, the temperature is controlled to be 100-600 ℃, and the blank is densified (molded) at a higher temperature;
and (3) stage: and in the blank annealing stage, the temperature of the blank heat preservation device is controlled within a rated temperature range for heat preservation annealing, and the temperature of introduced protective atmosphere can not be controlled in the stage. After densification treatment, the blank is subjected to heat preservation and annealing in a blank heat preservation device, and the effects of homogenization and annealing are achieved.
The stage speed-controlled cooling setting and the process can realize the quick solidification and slow cooling of the blank, and finally obtain the homogeneous blank.
Compared with the prior art, the invention has the following advantages and effects:
high-purity materials with strict requirements, particularly high-purity alloy materials or target materials containing multiple phases, particularly the preparation of high-purity metals such as aluminum, magnesium, copper, titanium, rare earth and the like and alloys thereof, mainly have the requirements of three aspects of impurity content control, organization and defect control, uniformity control and the like, and the processing conditions and the environment are particularly important. The invention prevents impurity pollution and provides good processing conditions in the processes of smelting, cooling and forming by integrating the combined action of a specified smelting and pouring device, a casting and forming device, a clean atmosphere device and the like so as to reduce the increase of impurity content, melt, homogenize, cool and form under proper process conditions, effectively ensure that the prepared high-purity material avoids impurity pollution in the whole preparation process, and uniformly fuse and controllably cool and form.
The invention relates to an impurity content control technology, which skillfully utilizes a plurality of measures for isolating substance interference except for melt of a system related device, and comprises the following steps: the stirring mode during heating and the stirring mode during cooling of the melt are preferably an electromagnetic stirring mode, and the crucible and the melt are in a near-suspended non-contact state or an isolation state without reaction, so that unnecessary impurities and the increase of the content of the impurities caused by the fact that external substances are mixed into the high-temperature melt during smelting are reduced to the greatest extent; the whole process is in a circulating clean protective atmosphere, the original or newly generated impurity atmosphere in the protective atmosphere can be effectively purified, and the increase of the impurity content such as oxygen content and the like caused by the reaction of the material and gas at a high temperature is reduced to the maximum extent. Through the effective guarantee of the measures, the preparation method and the equipment can effectively control the impurity content of the high-purity material, so that the impurity content of the material is not increased or even reduced in the processing process of the preparation method and the equipment.
The invention relates to a tissue and defect control technology, which can rapidly melt raw materials and stir and fuse different raw materials by a heating device with rapid temperature rise, timely temperature control and constant temperature; the device is used for controlling the cooling speed in stages during cooling, and the cooling speed in different stages can be controlled, such as rapid cooling and solidification under a liquid-solid phase mixing state to refine crystal grains, and slower cooling speed during solid state to reduce the generation of internal stress and cracks; the compression molding mode furthest lightens the generation of shrinkage cavities and micro-cavities and improves the density of the material.
The homogeneity control technology related by the invention adopts a non-contact stirring mode of a melt and a cooling process through a system related device, so that various components in the melt are effectively mixed in an all-round way, and the materials are ensured to be uniformly mixed in a molten state; the crucible device capable of controlling the turning smelting can properly remelt materials, and improve the uniformity of the materials by repeatedly turning smelting for many times; through the stepwise speed-controlled cooling mode and the compression molding mode, the material can be rapidly cooled and solidified so as to keep the homogeneous state of the material.
By combining the various devices and technologies, the high-purity preparation method and the high-purity preparation equipment can meet the preparation requirements of high-purity materials, particularly multi-phase alloy targets, and the structure, uniformity, defects and impurity content of the materials are effectively controlled by the technical means, so that the blanks of the high-purity targets with guaranteed quality are finally prepared. Moreover, the preparation system finally provided by the invention has a simple structure, is simple and convenient to operate, and is beneficial to industrial production.
Drawings
FIG. 1 is a schematic diagram of an apparatus for preparing a sputtering target according to the present invention.
In the figure, 1-a closed cavity; 2-smelting and pouring device; 3-casting a molding device; 4-a circulating atmosphere device; 5-atmosphere cleaning device; 6-atmosphere temperature control device; 7-vacuum pumping-off device; 8-a crucible; 9-a smelting heating device; 10-crucible rotation means; 11-a melt stirring device; 12-casting blank mould; 13-cooling the stirring device; 14-upper pressure forming device; 15-pressing down the forming device; 16-blank heat preservation device; 17-a die support post; 18-a mould tray; 19-protective atmosphere check valve; 20-a protective atmosphere storage device; 21-atmosphere circulating pump; 22-atmosphere cooling means; 23-atmosphere heating means; 24-atmosphere temperature control means; 25-vacuum extraction equipment; 26-vacuum valve
Detailed Description
Example 1
A high-purity metal material smelting device comprises a closed cavity 1, a smelting and pouring device 2, a casting and forming device 3, an atmosphere treatment device and other auxiliary facilities for ensuring normal operation of the device; the smelting and pouring device 2 and the casting and forming device 3 are arranged in a closed cavity, wherein the atmosphere treatment device consists of a circulating atmosphere device 4, an atmosphere cleaning device 5, an atmosphere temperature control device 6 and a vacuum pumping device 7, and is connected with the closed cavity and provides protective atmosphere for the closed cavity.
The smelting and pouring device is composed of four parts, namely a crucible 8, a smelting heating device 9, a crucible rotating device 10 and a melt stirring device 11, wherein:
the smelting heating device 9 is a high-frequency induction coil heating device, the melt stirring device 11 is an electromagnetic stirrer device, the crucible is a water-cooled copper crucible, and a layer of aluminum nitride ceramic film is deposited on the inner surface of the crucible, and the thickness of the film is 5 mu m; the crucible rotating device has the function of rotating the crucible and pouring at fixed points, can transfer the smelted melt into a casting blank die,
the casting forming device 3 is composed of a casting blank die 12, a cooling stirring device 13, an upper pressing forming device 14, a lower pressing forming device 15, a blank heat preservation device 16, a die supporting column 17, a die tray 18 and the like, wherein:
the cooling and stirring device 13 is an electromagnetic stirring device; the casting blank mold is provided with a water cooling device, the casting blank mold 12 is cooled by adopting a circulating cooling water mode, and the melt is rapidly cooled after being poured into the mold; the blank heat preservation device 16 adopts a resistance wire heating mode, the rated temperature is less than or equal to 600 ℃, and the temperature precision is +/-5 ℃;
the atmosphere treatment device consists of a circulating atmosphere device 4, an atmosphere cleaning device 5, an atmosphere temperature control device 6 and a vacuum pumping device 7, and is communicated with the sealed cavity through a pipeline and a valve. Wherein:
the atmosphere circulating device comprises a protective atmosphere one-way valve, a protective atmosphere storage device, an atmosphere circulating pump and the like, and the protective atmosphere used in the invention is high-purity argon; the atmosphere circulating pump is a GRG type vertical high-temperature gas circulating pump;
the atmosphere cleaning device 5 comprises a dust removal device and an oxygen removal purification device, wherein the oxygen removal material is sodium melt, so that the oxygen partial pressure of the atmosphere is less than 0.0001 Pa;
the vacuum pumping device 7 consists of a vacuum pumping device 25 and a vacuum valve 26, the vacuum pumping device consists of three-stage vacuum pumps such as a mechanical pump, a roots pump and a diffusion pump, and can pump the original atmosphere in the cavity to ensure that the vacuum degree in the cavity reaches 5 multiplied by 10-3Pa below, the sealing property of the cavity is high, and the pressure rise rate of the air pressure in the cavity is not more than 0.5Pa/h in a sealing state;
the atmosphere temperature control device 6 consists of an atmosphere cooling device 22, an atmosphere heating device 23, an atmosphere temperature control device 24 and a one-way valve, and the temperature is controlled timely through an intelligent temperature control system.
By the equipment, the Al-30Ti alloy is smelted and formed by pressure casting. The raw materials are high-purity aluminum and high-purity titanium, and the purity of the raw materials is more than or equal to 99.9995%. After the raw materials are added into the crucible, the atmosphere in the cavity is pumped out in advance through a vacuum pump, so that the vacuum degree in the furnace is 5 multiplied by 10-3Introducing high-purity argon below Pa to make the pressure in the cavity 800mbar and the oxygen partial pressure less than 0.0001 Pa; heating the raw materials by high-frequency induction until the raw materials are fully melted, preserving heat for 10 minutes, and electromagnetically stirring the melt in the heat preservation process; pouring into a water-cooled pressure casting mold for rapid cooling, starting a cooling electromagnetic stirring device, and simultaneously applying pressure to the poured blank by an upper pressure forming device, wherein the pressure is set to be 100MPa, and the pressure maintaining time is 5 minutes; then the blank is pushed into a heat preservation cavity to carry out annealing treatment at 560 ℃ for 4 hours. After argon is filled, a gas circulating pump is started, and the atmosphere cleaning device starts to work; the atmosphere temperature is room temperature during smelting, and temperature control is not carried out; when pouring, the atmosphere temperature is set to-15 ℃; the atmosphere temperature was set to 200 ℃ after the pressure holding. During annealing, the temperature of the blank holding device was set at 560 ℃ for 4 hours. To be treatedAnd cooling the blank along with the furnace after the annealing treatment, and taking out. The final preparation yielded a large-size ingot with a titanium content of 30.01 wt.%, a composition uniformity (maximum of the composition deviation range at 5 points at different locations in the percentage of the average composition of the element, the same in the following examples) of ± 1.85%, a size specification of 150mm in diameter × 50mm in height, a target impurity oxygen content of 7.8ppm, a total of other impurity contents of less than 10.5ppm, a relative density (relative density ═ actual density of the ingot/density of the ingot × 100%) of 99.5%, and an average grain size of 90.2 μm.
Example 2
The casting blank die is a conventional carbon steel die, the casting blank die 12 is cooled without adopting a circulating cooling water mode, and the melt is normally cooled by protective atmosphere after being poured into the die; the blank heat preservation device 16 adopts a resistance wire heating mode, the rated temperature is less than or equal to 900 ℃, and the temperature precision is +/-5 ℃; . The other apparatus was the same as in example 1.
Through the equipment, pure cerium is smelted and pressure cast to form. The raw material is high-purity cerium, and the purity of the raw material is more than or equal to 99.995%. After the raw materials are added into the crucible, the atmosphere in the cavity is pumped out in advance through a vacuum pump, so that the vacuum degree in the furnace is 5 multiplied by 10-3Introducing high-purity argon below Pa to make the pressure in the cavity 800mbar and the oxygen partial pressure less than 0.0001 Pa; heating the raw materials by high-frequency induction until the raw materials are fully melted, preserving heat for 10 minutes, and electromagnetically stirring the melt in the heat preservation process; pouring into a pressure casting mold for cooling, starting a cooling electromagnetic stirring device, and simultaneously applying pressure to the poured blank by an upper pressure forming device, wherein the pressure is set to be 100MPa, and the pressure maintaining time is 5 minutes; then the blank is pushed into a heat preservation cavity to carry out annealing treatment at 700 ℃ for 4 hours. After argon is filled, a gas circulating pump is started, and the atmosphere cleaning device starts to work; the atmosphere temperature is room temperature during smelting, and temperature control is not carried out; when pouring, setting the atmosphere temperature to be 100 ℃; the atmosphere temperature was set to 200 ℃ after the pressure holding. During annealing, the temperature of the blank holding device was set at 700 ℃ for 4 hours. And cooling the blank along with the furnace after annealing treatment, and taking out. Finally preparing a large-size blank with the size specification of diameter 150mm multiplied by 50mm high, the oxygen content of the target material impurity is 10.8ppm, and the total content of other impuritiesAnd less than 15.5ppm, a relative density of 99.5%, and an average grain size of 120.6. mu.m.
Example 3
The casting blank die is a heat-resistant (600 ℃) resistant stainless steel die, the casting blank die 12 is cooled without adopting a circulating cooling water mode, and the melt is normally cooled through a protective atmosphere after being poured into the die; the blank heat preservation device 16 adopts a resistance wire heating mode, the rated temperature is less than or equal to 1300 ℃, and the temperature precision is +/-5 ℃; . The other apparatus was the same as in example 1.
By the equipment, the Al-50Sc alloy is smelted and formed by pressure casting. The raw materials are high-purity aluminum and high-purity scandium, and the purity of the raw materials is more than or equal to 99.995%. After the raw materials are added into the crucible, the atmosphere in the cavity is pumped out in advance through a vacuum pump, so that the vacuum degree in the furnace is 5 multiplied by 10-3Introducing high-purity argon below Pa to make the pressure in the cavity 800mbar and the oxygen partial pressure less than 0.0001 Pa; heating the raw materials by high-frequency induction until the raw materials are fully melted, preserving heat for 10 minutes, and electromagnetically stirring the melt in the heat preservation process; pouring into a pressure casting mold for cooling, starting a cooling electromagnetic stirring device, and simultaneously applying pressure to the poured blank by an upper pressure forming device, wherein the pressure is set to be 100MPa, and the pressure maintaining time is 5 minutes; then the blank is pushed into a heat preservation cavity to carry out annealing treatment at 1000 ℃ for 4 hours. After argon is filled, a gas circulating pump is started, and the atmosphere cleaning device starts to work; the atmosphere temperature is room temperature during smelting, and temperature control is not carried out; during pouring, the atmosphere temperature is set to 560 ℃; the atmosphere temperature after the pressure holding was set to 560 ℃. During annealing, the temperature of the blank holding device was set at 1000 ℃ for 4 hours. And cooling the blank along with the furnace after annealing treatment, and taking out. Finally, a large-size blank is prepared, the size specification is that the diameter is 150mm multiplied by the height is 50mm, the scandium mass percent content is 50.09 wt.%, the component uniformity is +/-1.25%, the oxygen content of the target impurity is 30.8ppm, the sum of the contents of other impurities is less than 65.5ppm, the relative density is 99.3%, and the average grain size is 80.7 μm.
Comparative example 1
A high-purity metal material smelting device comprises a closed cavity, a smelting and pouring device, a casting and forming device, a circulating atmosphere device, an atmosphere cleaning device, an atmosphere temperature control device, a vacuum pumping device and other auxiliary facilities for ensuring the normal operation of the device, wherein the casting and forming device does not comprise an upper and lower pressing and forming device, and the other devices are the same as those in embodiment 1.
By the equipment, the Al-30Ti alloy is smelted and cast to form. The procedure was the same as in example 1 except that densification was not performed. Finally, a large-size blank is prepared, wherein the mass percent content of titanium is 29.94 wt.%, the component uniformity is +/-3.45%, the size specification is that the diameter is 150mm multiplied by 20mm, the content of oxygen of impurities in the target material is 8.1ppm, the sum of the contents of other impurities is less than 10.2ppm, the relative density is 94.5%, and the average grain size is 95.2 μm. The compactness is low.
Comparative example 2
The other conditions are the same as those of example 1, except that the protective atmosphere is always room temperature, and finally a large-size blank is prepared, wherein the mass percent content of titanium in the center of the target blank is 26.34 wt.%, the mass percent content of titanium at the edge of the target blank is 32.84 wt.%, the uniformity of components is +/-10.8%, the size specification is 150mm in diameter and 50mm in height, the oxygen content of impurities in the target material is 8.1ppm, the sum of the contents of other impurities is less than 10.2ppm, the relative density is 97.2%, and the average grain size is 95.2 μm. Because the cooling speed of the blank after casting is difficult to control, the edge of the die is cooled quickly, the components with higher melting points (titanium-rich components) are solidified and partially gathered, the core temperature is higher along with the cooling, and the components with lower melting points (aluminum-rich components) are solidified later, so that the aluminum in the core is higher and the component deviation is large; when pressure maintaining is carried out, the environment temperature is low, the temperature reduction is fast, the blank cannot achieve a good densification effect, and the compactness is low.
Claims (10)
1. A preparation equipment of sputtering target material is characterized in that: comprises a closed cavity, a smelting and pouring device, a casting and forming device and an atmosphere treatment device; the smelting pouring device and the casting forming device are positioned in the closed cavity; the atmosphere treatment device is connected with the closed cavity through a pipeline; conveying protective atmosphere to the closed cavity;
the melting and pouring device consists of a crucible, a melting and heating device, a melt stirring device and a crucible rotating device; the melting heating device is used for heating materials in the crucible, the crucible rotating device is used for enabling the crucible to rotate, and the melt stirring device is used for stirring melts in the crucible.
2. The apparatus of claim 1, wherein:
the smelting heating device is selected from a medium-frequency or high-frequency induction coil heating device or a vacuum arc heating device;
the melt stirring device is a consumable stirrer stirring device;
the crucible is a water-cooled copper crucible;
a ceramic film is deposited on the inner surface of the crucible, and the thickness of the ceramic film is 0.5-10 microns.
3. The apparatus of claim 1, wherein:
the casting forming device comprises a casting blank die, a cooling and stirring device, an upper pressing forming device, a lower pressing forming device, a blank heat preservation device, a die supporting column and a die tray; the bottom edge of the casting blank mold is fixed on a mold tray, the lower part of the mold tray is supported by a mold support column, the upper pressing forming device is positioned right above the casting blank mold, the lower pressing forming device is positioned right below the casting blank mold, the upper pressing forming device and the lower pressing forming device can move up and down, apply pressure to the casting blank mold and push the cooled and formed blank to a blank heat preservation device from the casting blank mold, and the blank heat preservation device is positioned below the casting blank mold; the cooling and stirring device surrounds the outer side of the die and provides non-contact stirring for the melt in the casting blank die.
4. The apparatus of claim 1, wherein:
the cooling stirring device is selected from a vibration stirring device or an electromagnetic stirring device;
a circulating cooling water pipeline is arranged outside the casting blank mould;
the blank heat preservation device adopts a resistance wire heating mode or a medium-frequency induction heating mode.
5. The apparatus of claim 1, wherein:
the atmosphere treatment device comprises a circulating atmosphere device, an atmosphere cleaning device, an atmosphere temperature control device and a vacuum pumping device;
the atmosphere circulating device comprises a protective atmosphere one-way valve, an atmosphere circulating pump and a protective atmosphere storage device; the protective atmosphere check valve controls the supply of protective atmosphere; one end of the atmosphere circulating pump is connected with the protective atmosphere storage device, the other end of the atmosphere circulating pump is connected with the atmosphere cleaning device through a pipeline, a protective gas source is conveyed to the atmosphere cleaning device, and oxygen removal, impurity removal and dust reduction are carried out on the protective atmosphere; one end of the atmosphere cleaning device is connected with the atmosphere temperature control device through a pipeline, and the temperature of the clean atmosphere from the atmosphere cleaning device is adjusted; the other end of the atmosphere cleaning device is connected with the sealed cavity and used for conveying the protective atmosphere subjected to temperature regulation to the sealed cavity, and the vacuum pumping device is connected with the sealed cavity through a pipeline and used for vacuumizing the sealed cavity.
6. The apparatus of claim 5, wherein:
the atmosphere cleaning device comprises a dust removal device and an oxygen removal device, wherein the oxygen removal device contains an oxygen removal purification material, the oxygen removal purification material is selected from oxygen absorption metal, and the oxygen absorption metal is selected from at least one of lithium, sodium, calcium and rare earth elements;
the vacuum pumping device consists of vacuum pumping equipment and a vacuum valve, wherein the vacuum pumping equipment consists of a mechanical pump, a roots pump and a diffusion pump three-stage vacuum pump.
7. The apparatus of claim 5, wherein: the atmosphere temperature control device is composed of an atmosphere cooling device, an atmosphere heating device, an atmosphere temperature control device and a one-way valve, and the range of the atmosphere temperature control device for adjusting the temperature of the protective atmosphere is-50-600 ℃.
8. A method of preparing a sputter target using an apparatus for preparing a sputter target according to any of claims 1 to 7, characterized in that: comprises the following steps of placing sputtering target material in a crucible, and vacuumizing a sealed cavity to ensure that the vacuum degree in the sealed cavity is less than or equal to 5 multiplied by 10-3Pa; then introducing a room-temperature protective atmosphere in a circulating state into the sealed cavity, heating the crucible to melt the raw materials of the sputtering target material, preserving heat of the melt after the raw materials are fully melted, stirring the melt in the heat preservation process, rotating the crucible after the heat preservation is finished, pouring the melt into a casting mold, and cooling a casting blank mold by water in the pouring process and simultaneously stirring in a non-contact manner; and controlling the temperature of introduced protective atmosphere in the pouring process to be-50-600 ℃, pressurizing a casting blank mold after pouring, controlling the temperature of introduced protective atmosphere in the pressure maintaining process to be 100-600 ℃, pushing the obtained blank into a blank heat preservation device for annealing after pressure maintaining, and cooling to room temperature after annealing treatment to obtain the sputtering target.
9. The method of claim 8, wherein:
the non-contact stirring is vibration stirring or electromagnetic stirring,
pressurizing a casting blank mold at the pressure of 1-100 MPa for 1-20 min;
the protective atmosphere is treated by an atmosphere cleaning device, and the oxygen partial pressure is less than 0.01 Pa.
10. The method of claim 8, wherein:
when the sputtering target is selected from high-melting-point-difference alloy, controlling the temperature of protective atmosphere introduced in the casting process to be-50-20 ℃,
when the sputtering target is selected from high-melting-point-difference alloy, water cooling is carried out on a casting blank die in the pouring process;
when the sputtering target material is selected from easily-deformed pure metal or alloy with the alloy content not higher than 5%, controlling the temperature of protective atmosphere to be 20-200 ℃; the easily deformable pure metal is selected from at least one of aluminum, magnesium, copper and titanium;
when the sputtering target material is selected from a hard-to-deform pure metal or an intermetallic compound, controlling the temperature of the introduced protective atmosphere to be 200-600 ℃, wherein the hard-to-deform pure metal is selected from at least one of chromium, niobium and tantalum, and the hard-to-deform intermetallic compound is selected from at least one of Al-Ti, Al-Cr, Al-Ni and aluminum rare earth alloy with 100% of intermetallic compound phase with the melting point higher than 1300 ℃;
when the sputtering target is selected from hard-to-deform pure metal or intermetallic compound, the temperature of the casting blank mold is controlled to be 200-600 ℃.
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| CN114212977A (en) * | 2021-12-17 | 2022-03-22 | 上海大学 | Double-heating-cavity high-temperature fusion casting device for preparing quartz glass products |
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