CN113754437B - Production process of tantalum phosphide target material - Google Patents
Production process of tantalum phosphide target material Download PDFInfo
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- CN113754437B CN113754437B CN202110980546.8A CN202110980546A CN113754437B CN 113754437 B CN113754437 B CN 113754437B CN 202110980546 A CN202110980546 A CN 202110980546A CN 113754437 B CN113754437 B CN 113754437B
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/5154—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on phosphides
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/62605—Treating the starting powders individually or as mixtures
- C04B35/6261—Milling
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/64—Burning or sintering processes
- C04B35/645—Pressure sintering
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- 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
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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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- 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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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/74—Physical characteristics
- C04B2235/77—Density
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
Abstract
The application relates to the technical field of tantalum phosphide target production, and particularly discloses a production process of a tantalum phosphide target. The process comprises the following steps: placing tantalum phosphide with the purity of not less than 99.5% into a ball mill for ball milling to obtain 500-800-mesh tantalum phosphide powder; loading tantalum phosphide powder into a mould, installing the mould in a vacuum hot-pressing furnace, and introducing inert gas to the air pressure in the vacuum hot-pressing furnace to 0.01MPa after the air pressure in the vacuum hot-pressing furnace is less than 10 Pa; the vacuum hot pressing furnace is heated to 1300-1600 ℃ at 90-100 ℃/min, under the mechanical pressure of 12-25MPa, tantalum phosphide powder in the sintering mold is heated to room temperature along with the furnace for 30-60min, and the target blank is obtained after being taken out; and (5) carrying out mechanical processing on the target blank, and then cleaning and drying to obtain the tantalum phosphide magnetron sputtering target. The density of the tantalum phosphide target material prepared by the production process is not less than 95%, the purity is not less than 99.5%, and the tantalum phosphide target material is a good material for preparing tantalum phosphide Weyl semi-metal films.
Description
Technical Field
The application relates to the technical field of tantalum phosphide target production, in particular to a production process of tantalum phosphide targets.
Background
Tantalum phosphide is a naturally occurring Weyl semi-metallic material. In recent years, scientists prepare very thin high-conductivity Weyl semi-metal films in research on Weyl semi-metal materials, the conductivity of the film materials at room temperature is several times that of copper, impurities are very difficult to absorb due to topological effects, chemical changes are not easy to occur, heat emitted by current in a circuit is also greatly reduced, and the film materials have great value for preparing room-temperature low-energy electronic devices and provide basic conditions for manufacturing larger-scale integrated circuits. Weyl semi-metal thin film materials such as tantalum phosphide have become one of the research hotspots for global thin film materials.
Disclosure of Invention
At present, a Weyl semi-metal material such as tantalum phosphide is one of hot spot materials studied by global researchers, and in order to provide raw materials for preparing tantalum phosphide films for research work and application, the application provides a production process of a tantalum phosphide target material.
The production process of the tantalum phosphide target material adopts the following technical scheme:
a process for producing a tantalum phosphide target, the process comprising the steps of: placing tantalum phosphide with the purity of not less than 99.5% into a ball mill for ball milling to obtain 500-800-mesh tantalum phosphide powder; loading tantalum phosphide powder into a mould, installing the mould in a vacuum hot-pressing furnace, and introducing inert gas to the air pressure in the vacuum hot-pressing furnace to 0.01MPa after the air pressure in the vacuum hot-pressing furnace is less than 10 Pa; the vacuum hot pressing furnace is heated to 1300-1600 ℃ at 90-100 ℃/min, under the mechanical pressure of 12-25MPa, tantalum phosphide powder in the sintering mold is heated to room temperature along with the furnace for 30-60min, and the target blank is obtained after being taken out; and (5) carrying out mechanical processing on the target blank, and then cleaning and drying to obtain the tantalum phosphide magnetron sputtering target.
By adopting the technical scheme, the high-purity tantalum phosphide is placed in the ball mill for ball milling, so that the particle size of the tantalum phosphide powder is smaller, and when the tantalum phosphide powder is placed in a die for sintering, the tantalum phosphide powder with the small particle size has higher sintering activity, so that the compactness of the tantalum phosphide powder after sintering and forming can be improved, the internal porosity of the formed target material is greatly reduced, and the film forming performance of the tantalum phosphide target material is improved; after the die is arranged in the vacuum hot-pressing furnace, the vacuum hot-pressing furnace is vacuumized, and then inert gas is injected to adjust the air pressure in the vacuum hot-pressing furnace, so that the content of oxidizing gas in the vacuum hot-pressing furnace is removed, the tantalum phosphide powder is prevented from being oxidized in a high-temperature environment, the inert gas can play a role in heat conduction, the chemical stability of the tantalum phosphide powder is improved, and the purity of the tantalum phosphide target material is further improved; heating the vacuum hot-pressing furnace at a speed of 90-100 ℃/min to uniformly heat the tantalum phosphide powder in the die, and applying larger mechanical pressure on the tantalum phosphide powder in the die, so that the tantalum phosphide powder is sintered and molded under the condition of being far lower than the melting point of the tantalum phosphide; after the proportioning and machining of the target blank, the surface of the target is smooth, and the target is dried after cleaning, so that the tantalum phosphide magnetic control target is obtained, the relative density is above 95%, and the purity is above 99.5%, and is a good material for preparing tantalum phosphide Weyl semi-metal films.
Preferably, the ball mill is a planetary ball mill, and the ratio of large, medium and small ball is 1:1:1, wherein the diameter of the large sphere is 8mm, the diameter of the middle sphere is 5.2mm, and the diameter of the small sphere is 3.8mm; ball-to-material ratio 2.8:1, a step of; ball mill revolution is 200r/min; ball milling time is 2-2.5h.
Preferably, the tantalum phosphide powder is put into a die and is pre-pressed with a pressure of 2-5MPa when placed in a vacuum hot-pressing furnace.
By adopting the technical scheme, when tantalum phosphide powder is subjected to hot press forming, the powder is pre-pressed by using the pressure of 2-5MPa, the powder is subjected to preliminary shaping, and the powder can be prevented from escaping from a die and scattering in a vacuum hot press furnace when the air pressure is regulated in the vacuum hot press furnace.
Preferably, the vacuum autoclave is warmed from room temperature to 600℃at a rate of 90℃per minute and from 600℃to 1300-1600℃at a rate of 100℃per minute.
Preferably, the relative compactness of the target is larger than or equal to 95%, and the purity of the target is larger than or equal to 99.5%.
Preferably, the mass of tantalum phosphide powder is pre-calculated according to the desired target specification when the tantalum phosphide powder is added to the mold.
Preferably, the mold is made of graphite.
Preferably, the target after the machining is subjected to ultrasonic cleaning.
In summary, the present application has the following beneficial effects:
1. the application adopts the tantalum phosphide powder as the target material, the tantalum phosphide powder is placed in a die, the tantalum phosphide powder is subjected to vacuum hot pressing, and sintered and formed at a temperature far lower than the melting point of tantalum phosphide, so that the tantalum phosphide target is obtained, and the magnetron sputtering target for preparing the high-performance tantalum phosphide Weyl semi-metal film is provided for research work and application. The production technology of the tantalum phosphide target material and the high-performance tantalum phosphide product have promotion effects on development and progress of Weyl semi-metal film material research in China and application of the Weyl semi-metal film material in larger scale integrated circuits.
2. When the tantalum phosphide powder is molded and sintered, the sintering temperature is far lower than the melting point of tantalum phosphide, the tantalum phosphide powder is placed in an inert gas environment, and large mechanical pressure is applied to the tantalum phosphide powder, so that the production cost can be reduced, the relative density of the obtained tantalum phosphide target material is not less than 95%, and the purity is not less than 95.5%.
3. In this application with the tantalum phosphide in place the ball mill and carry out the ball-milling, further reduce the particle diameter of tantalum phosphide powder when carrying out the sintering, improved the sintering activity of tantalum phosphide powder to increased the compactness after the tantalum phosphide powder sintering shaping, reduced the inside porosity behind the target shaping by a wide margin, improved the membranous property of tantalum phosphide target.
Drawings
Fig. 1 is a flow chart of a process provided herein.
Detailed Description
The present application is described in further detail below with reference to the drawings and examples.
Examples
Example 1
The tantalum phosphide target prepared in this example 1 had a specification of Φ50mm and a thickness of 10 mm. In other embodiments, the target may have a circular target with a diameter of 27-460mm and a thickness of 1-50mm, or a rectangular target with a length x width = (80-400 mm) × (80-400 mm), and according to the required specification for preparing the tantalum phosphide target, a graphite mold with a diameter of 5mm larger than the required target is selected, and a 2mm allowance is left in the target blank. In the embodiment 1 of the application, a graphite mold with the diameter of 55mm is selected. In example 1 of the present application, the target blank prepared had a specification of Φ55mm and a thickness of 12mm.
Referring to fig. 1, in this embodiment 1, the production process of the tantalum phosphide target material includes the following steps:
s1, adding tantalum phosphide with the purity of more than 99.5% into a planetary ball mill, and ball milling tantalum phosphide powder to powder of 500-800 meshes, wherein the time is 2-2.5 hours; wherein, big ball diameter 8mm, well ball 5.2mm, pellet 3.8mm in the planetary ball mill, big ball, well ball and pellet 1:1:1, setting, ball-to-material ratio 2.8:1, ball mill revolution is 200r/min;
s2, according to the specification of the required tantalum phosphide target material, selecting graphiteAnd (3) die specification, leaving machining allowance, and calculating and weighing the mass of the required tantalum phosphide powder: m=n ρv; wherein n is the relative density of the target material (taking 95 percent); ρ is the tantalum phosphide density; v=pi×55 2 ×12/4000cm 3 ；
And S3, uniformly loading the precisely weighed tantalum phosphide powder into a graphite mold, placing the graphite mold into a vacuum hot-pressing furnace, prepressing the tantalum phosphide powder under the pressure of 2-5MPa, introducing argon gas into the vacuum hot-pressing furnace until the air pressure in the vacuum hot-pressing furnace is 0.01MPa, heating the vacuum hot-pressing furnace to 600 ℃ at the rate of 90 ℃/min, heating the vacuum hot-pressing furnace to 1300-1600 ℃ at the rate of 100 ℃/min, compacting the tantalum phosphide powder under the pressure of 12-25MPa, preserving the heat for 30-60min, cooling the vacuum hot-pressing furnace to the room temperature along with the furnace, taking out the target blank, and processing the target blank by a grinding machine, ultrasonically cleaning, drying and packaging the target blank to obtain the tantalum phosphide magnetron sputtering target. The relative density of the tantalum phosphide target material and the tantalum phosphide is detected to be not less than 95 percent, and the purity is detected to be not less than 99.99 percent.
The present embodiment is merely illustrative of the present application and is not intended to be limiting, and those skilled in the art, after having read the present specification, may make modifications to the present embodiment without creative contribution as required, but is protected by patent laws within the scope of the claims of the present application.
Claims (5)
1. The production process of the tantalum phosphide target material is characterized by comprising the following steps of:
placing tantalum phosphide with the purity of not less than 99.5% into a ball mill for ball milling to obtain 500-800-mesh tantalum phosphide powder; the ball mill is a planetary ball mill, the ratio of big ball to middle ball to small ball is 1:1:1, wherein the diameter of the big ball is 8mm, the diameter of the middle ball is 5.2mm, and the diameter of the small ball is 3.8mm; ball-to-material ratio is 2.8:1; ball mill revolution is 200r/min; ball milling time is 2-2.5h;
loading tantalum phosphide powder into a mould, installing the mould in a vacuum hot-pressing furnace, and prepressing the tantalum phosphide powder at the pressure of 2-5 MPa; after the air pressure in the vacuumizing hot-pressing furnace is less than 10Pa, introducing inert gas to the air pressure in the vacuumizing hot-pressing furnace to 0.01MPa; heating the vacuum hot-pressing furnace to 1300-1600 ℃ at 90-100 ℃/min, sintering tantalum phosphide powder in the die for 30-60min under the mechanical pressure of 12-25MPa, cooling to room temperature along with the furnace, and taking out to obtain a target blank;
cleaning and drying the target blank after machining to obtain a tantalum phosphide magnetron sputtering target; the relative compactness of the target is not less than 95%, and the purity of the target is not less than 99.5%.
2. A process for producing a tantalum phosphide target according to claim 1, wherein the vacuum hot-pressing furnace is heated from room temperature to 600 ℃ at a rate of 90 ℃/min and from 600 ℃ to 1300-1600 ℃ at a rate of 100 ℃/min.
3. A process for producing a tantalum phosphide target according to claim 1, wherein the mass of tantalum phosphide powder is calculated in advance according to the required target specification when adding tantalum phosphide powder into a mold.
4. The process for producing a tantalum phosphide target material according to claim 1, wherein said mold is graphite.
5. A process for producing a tantalum phosphide target according to claim 1, wherein the machined target is subjected to ultrasonic cleaning.
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| JP3628575B2 (en) * | 1999-02-25 | 2005-03-16 | 株式会社日鉱マテリアルズ | Ni-P alloy sputtering target and method for producing the same |
| CN102367568B (en) * | 2011-10-20 | 2014-04-23 | 宁波江丰电子材料有限公司 | Preparation method of high-purity tantalum target material |
| EP3106540B1 (en) * | 2014-03-27 | 2018-04-25 | JX Nippon Mining & Metals Corp. | Method of producing a ni-p alloy or a ni-pt-p alloy sputtering target |
| CN104496473A (en) * | 2014-12-30 | 2015-04-08 | 山东昊轩电子陶瓷材料有限公司 | Production method of high-density conductive niobium oxide target |
| CN108655403B (en) * | 2018-06-25 | 2020-08-28 | 河南科技大学 | Preparation method of high-purity tantalum target material for electronic material |
| CN111632730B (en) * | 2020-06-08 | 2022-06-28 | 福建阿石创新材料股份有限公司 | Extrusion grinding equipment and method for recycling ITO powder from ITO residual target/waste target |
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