CN113754437A - Production process of tantalum phosphide target material - Google Patents
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- CN113754437A CN113754437A CN202110980546.8A CN202110980546A CN113754437A CN 113754437 A CN113754437 A CN 113754437A CN 202110980546 A CN202110980546 A CN 202110980546A CN 113754437 A CN113754437 A CN 113754437A
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- 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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- 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
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Abstract
The application relates to the technical field of production of tantalum phosphide targets, and particularly discloses a production process of a tantalum phosphide target. The process comprises the following steps: placing tantalum phosphide with the purity being equal to or larger than 99.5 percent in a ball mill for ball milling to obtain tantalum phosphide powder with 500-800 meshes; putting tantalum phosphide powder into a mould, installing the mould in a vacuum hot-pressing furnace, and introducing inert gas until the pressure in the vacuum hot-pressing furnace is 0.01MPa after the pressure in the vacuum hot-pressing furnace is less than 10 Pa; sintering the tantalum phosphide powder in the mold for 30-60min at the temperature of 90-100 ℃/min-1300-1600 ℃ under the mechanical pressure of 12-25MPa in a vacuum hot-pressing furnace, cooling to room temperature along with the furnace, and taking out to obtain a target blank; and (4) cleaning and drying the target blank after machining to obtain the tantalum phosphide magnetron sputtering target. The compactness of the tantalum phosphide target material prepared by the production process is larger than or equal to 95%, the purity is larger than or equal to 99.5%, and the tantalum phosphide Weyl semimetal film is a good material for preparing the tantalum phosphide Weyl semimetal film.
Description
Technical Field
The application relates to the technical field of production of tantalum phosphide targets, in particular to a production process of a tantalum phosphide target.
Background
Tantalum phosphide is a naturally occurring Weyl semimetal material. In recent years, in the research on the Weyl semimetal material, scientists have prepared an extremely thin Weyl semimetal film with high conductivity, the conductivity of the film material at room temperature is several times that of copper, and the film material is extremely difficult to absorb impurities due to topological effect and difficult to generate chemical change, so that the heat emitted by current in a circuit can be greatly reduced, and the film material has great value for preparing electronic devices with low energy consumption at room temperature and provides a basic condition for manufacturing larger-scale integrated circuits. Weyl semimetal thin film materials such as tantalum phosphide have become one of the research hotspots of global thin film materials.
Disclosure of Invention
At present, Weyl semimetal materials such as tantalum phosphide and the like are one of hot materials researched by global researchers, and the application provides a production process of tantalum phosphide target materials 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, which adopts the following technical scheme:
a production process of a tantalum phosphide target material comprises the following steps: placing tantalum phosphide with the purity being equal to or larger than 99.5 percent in a ball mill for ball milling to obtain tantalum phosphide powder with 500-800 meshes; putting tantalum phosphide powder into a mould, installing the mould in a vacuum hot-pressing furnace, and introducing inert gas until the pressure in the vacuum hot-pressing furnace is 0.01MPa after the pressure in the vacuum hot-pressing furnace is less than 10 Pa; sintering the tantalum phosphide powder in the mold for 30-60min at the temperature of 90-100 ℃/min-1300-1600 ℃ under the mechanical pressure of 12-25MPa in a vacuum hot-pressing furnace, cooling to room temperature along with the furnace, and taking out to obtain a target blank; and (4) cleaning and drying the target blank after machining 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 the die for sintering, the small-particle-size tantalum phosphide powder has higher sintering activity, the compactness of the tantalum phosphide powder after sintering and forming can be improved, the internal porosity of the target after forming is greatly reduced, and the film-making performance of the tantalum phosphide target is improved; after the die is installed in the vacuum hot-pressing furnace, the vacuum hot-pressing furnace is firstly vacuumized, then inert gas is injected to adjust the air pressure in the vacuum hot-pressing furnace, and the content of oxidizing gas in the vacuum hot-pressing furnace is removed, so that 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 prepared tantalum phosphide target material is further improved; heating the vacuum hot-pressing furnace at the speed of 90-100 ℃/min to ensure that the tantalum phosphide powder in the die is uniformly heated, and applying higher 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; and (3) after the target blank is proportioned and machined, the surface of the target is smooth, and the target is cleaned and dried to obtain the tantalum phosphide magnetic control target, wherein the relative density of the tantalum phosphide magnetic control target is more than 95 percent, the purity of the tantalum phosphide magnetic control target is more than 99.5 percent, and the tantalum phosphide Weyl semimetal film is a good material for preparing the tantalum phosphide Weyl semimetal film.
Preferably, the ball mill is a planetary ball mill, and the proportion of large, medium and small ball milling balls is 1: 1: 1, wherein the diameter of a large ball is 8mm, the diameter of a middle ball is 5.2mm, and the diameter of a small ball is 3.8 mm; ball-material ratio 2.8: 1; the revolution of the ball mill is 200 r/min; the ball milling time is 2-2.5 h.
Preferably, the tantalum phosphide powder is pre-pressed at a pressure of 2-5MPa when being loaded into a mold and placed in a vacuum hot-pressing furnace.
Through adopting above-mentioned technical scheme, when carrying out hot briquetting to the tantalum phosphide powder, use 2-5 MPa's pressure earlier to carry out the pre-compaction to the powder, play preliminary design's effect to the powder, and can prevent when adjusting atmospheric pressure in the vacuum hot pressing stove, the powder escapes from the mould, flies apart in the vacuum hot pressing stove.
Preferably, 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.
Preferably, the relative density of the target is not less than 95%, and the purity of the target is not less than 99.5%.
Preferably, when the tantalum phosphide powder is added into the die, the mass of the tantalum phosphide powder is calculated in advance according to the required target specification.
Preferably, the mold is made of graphite.
Preferably, the machined target is subjected to ultrasonic cleaning.
In summary, the present application has the following beneficial effects:
1. according to the method, tantalum phosphide powder is used as a target material, the tantalum phosphide powder is placed in a die, the tantalum phosphide powder is subjected to vacuum hot pressing, and sintering molding is carried out at a temperature far lower than the melting point of the 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 the development and progress of the research of Weyl semimetal thin film materials in China and the application of the Weyl semimetal thin film materials 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 the tantalum phosphide, the tantalum phosphide powder is placed in an inert gas environment, and great 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 is not less than 95%, and the purity is not less than 95.5%.
3. Placing the tantalum phosphide in the ball mill in this application and carrying out the ball-milling, further reducing the particle diameter when the tantalum phosphide powder carries out the sintering, improved the sintering activity of tantalum phosphide powder to increased the compactedness behind the tantalum phosphide powder sintering shaping, reduced the inside porosity after the target shaping by a wide margin, improved the membrane performance of tantalum phosphide target.
Drawings
FIG. 1 is a flow chart of a process provided herein.
Detailed Description
The present application will be described in further detail with reference to the following drawings and examples.
Examples
Example 1
The specification of the tantalum phosphide target material prepared in the embodiment 1 is a target material with phi of 50mm and thickness of 10 mm. In other embodiments, the target specification may be a round target with a diameter of 27-460mm and a thickness of 1-50mm, or a rectangular target with a length × width of (80-400mm) × (80-400mm), and according to the specification of the tantalum phosphide target to be prepared, a graphite mold with a diameter 5mm larger than the required target diameter is selected, and a 2mm margin is left for the target blank. In the embodiment 1 of the application, a graphite material mold with the diameter of phi 55mm is selected. In the embodiment 1 of the application, the prepared target blank has the specification of phi 55mm and the thickness of 12 mm.
Referring to fig. 1, in this example 1, the process for producing a tantalum phosphide target material includes the following steps:
s1, adding the tantalum phosphide with the purity of more than 99.5% into a planetary ball mill, and ball-milling the tantalum phosphide powder to powder with the particle size of 500-800 meshes, wherein the time is consumed for 2-2.5 h; wherein, big ball diameter 8mm in the planet ball mill, well ball 5.2mm, pellet 3.8mm, big ball, well ball and pellet 1: 1: 1, ball material ratio of 2.8: 1, revolving the ball mill for 200 r/min;
s2, reserving machining allowance according to the specification of the required tantalum phosphide target material and the specification of the selected graphite die, and calculating and weighing the mass of the required tantalum phosphide powder: m ═ n ρ V; wherein n is the relative density (95%) of the target material; rho is the tantalum phosphide density; v ═ pi × 552×12/4000cm3；
S3, uniformly loading the precisely weighed tantalum phosphide powder into a graphite mold, placing the graphite mold into a vacuum hot-pressing furnace, pre-pressing the tantalum phosphide powder at the pressure of 2-5MPa, introducing argon gas until the air pressure in the vacuum hot-pressing furnace is 0.01MPa, heating to 600 ℃ from room temperature at the speed of 90 ℃/min, heating to 1300-. The detected relative density of the tantalum phosphide target material and the tantalum phosphide is equal to or larger than 95 percent, and the detected purity is equal to or larger than 99.99 percent.
The present embodiment is only for explaining the present application, and it is not limited to the present application, and those skilled in the art can make modifications of the present embodiment without inventive contribution as needed after reading the present specification, but all of them are protected by patent law within the scope of the claims of the present application.
Claims (8)
1. The production process of the tantalum phosphide target is characterized by comprising the following steps of: placing tantalum phosphide with the purity being equal to or larger than 99.5 percent in a ball mill for ball milling to obtain tantalum phosphide powder with 500-800 meshes; putting tantalum phosphide powder into a mould, installing the mould in a vacuum hot-pressing furnace, and introducing inert gas until the pressure in the vacuum hot-pressing furnace is 0.01MPa after the pressure in the vacuum hot-pressing furnace is less than 10 Pa; sintering the tantalum phosphide powder in the mold for 30-60min at the temperature of 90-100 ℃/min-1300-1600 ℃ under the mechanical pressure of 12-25MPa in a vacuum hot-pressing furnace, cooling to room temperature along with the furnace, and taking out to obtain a target blank; and (4) cleaning and drying the target blank after machining to obtain the tantalum phosphide magnetron sputtering target.
2. The production process of the tantalum phosphide target material as claimed in claim 1, wherein the production process comprises the following steps: the ball mill is a planetary ball mill, and the proportion of large, medium and small ball milling balls is 1: 1: 1, wherein the diameter of a large ball is 8mm, the diameter of a middle ball is 5.2mm, and the diameter of a small ball is 3.8 mm; ball-material ratio 2.8: 1; the revolution of the ball mill is 200 r/min; the ball milling time is 2-2.5 h.
3. The production process of the tantalum phosphide target material as claimed in claim 1, wherein the production process comprises the following steps: and (3) putting the tantalum phosphide powder into a mould, and pre-pressing the tantalum phosphide powder at the pressure of 2-5MPa when the tantalum phosphide powder is placed in a vacuum hot-pressing furnace.
4. The production process of the tantalum phosphide target material as claimed in claim 1, wherein the production process comprises the following steps: the vacuum hot-pressing furnace is heated from room temperature to 600 ℃ at the speed of 90 ℃/min, and from 600 ℃ to 1300-1600 ℃ at the speed of 100 ℃/min.
5. The production process of the tantalum phosphide target material as claimed in claim 1, wherein the production process comprises the following steps: the relative density of the target is not less than 95%, and the purity of the target is not less than 99.5%.
6. The production process of the tantalum phosphide target material as claimed in claim 1, wherein the production process comprises the following steps: when the tantalum phosphide powder is added into a die, the quality of the tantalum phosphide powder is calculated in advance according to the required target specification.
7. The production process of the tantalum phosphide target material as claimed in claim 1, wherein the production process comprises the following steps: the mould is made of graphite.
8. The production process of the tantalum phosphide target material as claimed in claim 1, wherein the production process comprises the following steps: and carrying out ultrasonic cleaning on the machined target material.
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| CN202110980546.8A CN113754437B (en) | 2021-08-25 | 2021-08-25 | Production process of tantalum phosphide target material |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114014655A (en) * | 2021-12-17 | 2022-02-08 | 江西海特新材料有限公司 | Production process of manganese phosphide target material |
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| JP2000309865A (en) * | 1999-02-25 | 2000-11-07 | Nikko Materials Co Ltd | Ni-P ALLOY SPUTTERING TARGET AND ITS MANUFACTURE |
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| 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 |
| CN106133185A (en) * | 2014-03-27 | 2016-11-16 | 捷客斯金属株式会社 | Comprise Ni P alloy or the sputtering target of Ni Pt P alloy and manufacture method thereof |
| CN108655403A (en) * | 2018-06-25 | 2018-10-16 | 河南科技大学 | A kind of preparation method of electronic material high-purity tantalum target |
| CN111632730A (en) * | 2020-06-08 | 2020-09-08 | 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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- 2021-08-25 CN CN202110980546.8A patent/CN113754437B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| JP2000309865A (en) * | 1999-02-25 | 2000-11-07 | Nikko Materials Co Ltd | Ni-P ALLOY SPUTTERING TARGET AND ITS MANUFACTURE |
| CN102367568A (en) * | 2011-10-20 | 2012-03-07 | 宁波江丰电子材料有限公司 | Preparation method of high-purity tantalum target material |
| CN106133185A (en) * | 2014-03-27 | 2016-11-16 | 捷客斯金属株式会社 | Comprise Ni P alloy or the sputtering target of Ni Pt P alloy and manufacture method thereof |
| 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 |
| CN108655403A (en) * | 2018-06-25 | 2018-10-16 | 河南科技大学 | A kind of preparation method of electronic material high-purity tantalum target |
| CN111632730A (en) * | 2020-06-08 | 2020-09-08 | 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 |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114014655A (en) * | 2021-12-17 | 2022-02-08 | 江西海特新材料有限公司 | Production process of manganese phosphide target material |
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