CN115029674B - Low-segregation aluminum scandium alloy target material and preparation method thereof - Google Patents
Low-segregation aluminum scandium alloy target material and preparation method thereof Download PDFInfo
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- 238000005204 segregation Methods 0.000 title claims abstract description 26
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 229910000542 Sc alloy Inorganic materials 0.000 title claims abstract description 11
- LUKDNTKUBVKBMZ-UHFFFAOYSA-N aluminum scandium Chemical compound [Al].[Sc] LUKDNTKUBVKBMZ-UHFFFAOYSA-N 0.000 title claims abstract description 11
- 239000013077 target material Substances 0.000 title claims abstract description 10
- 239000000843 powder Substances 0.000 claims abstract description 96
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 53
- 239000000956 alloy Substances 0.000 claims abstract description 53
- 238000005245 sintering Methods 0.000 claims abstract description 41
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 25
- 239000001301 oxygen Substances 0.000 claims abstract description 25
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 25
- 239000011258 core-shell material Substances 0.000 claims abstract description 20
- 238000007731 hot pressing Methods 0.000 claims abstract description 16
- 238000002156 mixing Methods 0.000 claims abstract description 16
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 13
- 238000005303 weighing Methods 0.000 claims description 12
- 239000011812 mixed powder Substances 0.000 claims description 7
- 239000007789 gas Substances 0.000 claims description 6
- 238000011049 filling Methods 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 4
- 239000011230 binding agent Substances 0.000 abstract description 5
- 230000005540 biological transmission Effects 0.000 abstract description 5
- 238000010438 heat treatment Methods 0.000 abstract description 5
- 238000000034 method Methods 0.000 description 9
- 238000003723 Smelting Methods 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 8
- 238000005336 cracking Methods 0.000 description 5
- 229910052706 scandium Inorganic materials 0.000 description 4
- 238000004663 powder metallurgy Methods 0.000 description 3
- 238000000137 annealing Methods 0.000 description 2
- 238000005266 casting Methods 0.000 description 2
- 229910052451 lead zirconate titanate Inorganic materials 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 238000005096 rolling process Methods 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 239000011162 core material Substances 0.000 description 1
- 238000007580 dry-mixing Methods 0.000 description 1
- HFGPZNIAWCZYJU-UHFFFAOYSA-N lead zirconate titanate Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Ti+4].[Zr+4].[Pb+2] HFGPZNIAWCZYJU-UHFFFAOYSA-N 0.000 description 1
- 238000009766 low-temperature sintering Methods 0.000 description 1
- 238000001755 magnetron sputter deposition Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000010295 mobile communication Methods 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/14—Treatment of metallic powder
- B22F1/145—Chemical treatment, e.g. passivation or decarburisation
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/17—Metallic particles coated with metal
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/12—Both compacting and sintering
- B22F3/14—Both compacting and sintering simultaneously
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C21/00—Alloys based on aluminium
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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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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
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Abstract
A low segregation aluminum scandium alloy target material adopts a core-shell structure of an Al coated Sc, the Sc content is 20-50at%, the component fluctuation is within +/-0.2%, the oxygen content is less than 200ppm, and the relative density is not less than 99.5% of the AlSc alloy target material; the preparation method comprises the following steps: adding Sc powder and Al powder of a binder, mixing the powder, performing heat treatment on the sintered powder to obtain AlSc alloy powder with a core-shell structure, and performing hot-pressing sintering to obtain a low-segregation aluminum scandium alloy target; after the alloy powder is formed, the secondary segregation phenomenon caused by the different properties of the two powders in the later transmission process does not exist, and the AlSc alloy target with low segregation can be obtained after the later hot-pressing sintering.
Description
Technical Field
The invention belongs to the technical field of magnetron sputtering target manufacturing, and particularly relates to a low-segregation aluminum scandium alloy target and a preparation method thereof.
Background
The high-purity AlSc alloy target is mainly used for sputtering a high-purity AlScN film, has stronger and better piezoelectric performance compared with the existing piezoelectric films such as AlN, znO, lead zirconate titanate (PZT) and the like, and is a core material for manufacturing high-frequency mobile communication (5G) radio-frequency filter chips, MEMS miniature advanced sensors and the like. The preparation method for preparing AlSc alloy targets at present mainly comprises two steps: the first method is a smelting mode, but because of large difference of melting points of Al and Sc, the solid solubility of Sc in Al is very low, and as the content of Sc increases, the solid-liquid solidification interval increases, and the finally obtained AlSc alloy target blank has serious component segregation phenomenon; the second mode is powder metallurgy mode, and is mostly carried out by adopting a mode of mixing simple substance Al powder and AlSc alloy powder and then pressing, and although the segregation phenomenon of the AlSc alloy target material finally obtained is reduced compared with smelting mode, secondary segregation is easy to generate in the later transmission process due to different densities of the two powders after the Al powder and AlSc alloy powder are mixed, and AlSc alloy powder with larger density is easy to be deposited at the bottom of a die during powder transferring, so that component segregation is caused.
Disclosure of Invention
Aiming at the problem of component segregation of the prior AlSc alloy target, the patent provides a low-segregation aluminum scandium alloy target, which is a AlSc alloy target adopting an Al-coated Sc core-shell structure, wherein the Sc content is 20-50at%, the component fluctuation is within +/-0.2%, the oxygen content is less than 200ppm, and the relative density is not less than 99.5%. The principle of the method is that the capillary action between the micro-moist large-particle Sc powder and the dry small-particle Al powder is adopted to enable the Al powder to be uniformly adsorbed on the surface of the Sc powder, and then a sintering neck is formed between the Sc powder and the Al powder in a low-temperature sintering mode to form the core-shell structure AlSc alloy powder of the Al coated Sc. The AlSc alloy powder with the core-shell structure has uniform components, no secondary segregation phenomenon caused by different properties of two powders in the later transmission process after the alloy powder is formed, and the AlSc alloy target with low segregation can be obtained after the later hot-press sintering.
The invention also discloses a method for preparing the low-segregation aluminum scandium alloy target, which comprises the following steps: and mixing Sc powder and Al powder with a binder, performing heat treatment on the sintered powder to obtain core-shell structure AlSc alloy powder, and performing hot-pressing sintering to obtain the low-segregation aluminum scandium alloy target. Specifically, the method comprises the following steps:
Weighing Sc powder with purity of more than 3N, oxygen content of less than 300ppm and granularity of 60-100 mu m, and pouring the Sc powder into a powder mixer;
Step (2), weighing alcohol with corresponding volume according to the proportion of adding 1-5 mL of alcohol into each 100g of Sc powder, pouring the alcohol into a powder mixer in the step (1) for filling Ar gas and mixing for 1-2 h to obtain Sc powder with slightly moist surface;
Weighing 5-10 mu m Al powder with the corresponding proportioning purity of more than 5N and the oxygen content of less than 100ppm after the mixing is finished, placing the Al powder in a powder mixer in the step (2), and continuously filling Ar gas for mixing for 2-5 h to obtain mixed powder of the Al powder adsorbed on the surface of Sc powder;
Step (4), placing the AlSc mixed powder obtained in the step (3) in a vacuum sintering furnace for drying and sintering, removing alcohol, and enabling an Al powder and an Sc powder to form a sintering neck to be adhered together to form the core-shell structure AlSc alloy powder of the Al coated Sc, wherein the sintering temperature is 100-300 ℃ and the sintering time is 1-3 hours;
And (5) carrying out hot-pressing sintering on the core-shell structure AlSc alloy powder obtained in the step (4), wherein the hot-pressing temperature is 300-650 ℃, the sintering pressure is 20-30 MPa, the sintering time is 3-5 h, and finally obtaining the AlSc alloy target material with Sc content fluctuation within +/-0.2%, oxygen content less than 200ppm and relative density not less than 99.5%.
Compared with the prior art, the technical scheme has the following advantages:
(1) Avoiding component segregation: the core-shell structure AlSc alloy powder prepared by the method has uniform components, no secondary segregation phenomenon caused by different properties of two powders in the later transmission process, and the AlSc alloy target with low segregation can be obtained after the later hot-pressing sintering.
(2) The cracking does not occur: the AlSc alloy target prepared by adopting a common smelting mode or a powder metallurgy mode has a large number of brittle phases and stress which are easy to crack, and when the preparation of the AlSc alloy target is carried out by adopting the core-shell structure AlSc alloy powder coated with Sc by adopting the preparation method, the Al has strong nuclear plasticity, can be used as a binder in the later pressure sintering process to prevent the AlSc brittle phases from cracking, and can further reduce the possibility of cracking by deforming and releasing the internal stress generated in the partial sintering process;
(3) The oxygen content is low: the oxygen content in AlSc alloy targets is mainly brought by Sc, the oxygen content in Al powder is low, and the oxygen content in AlSc alloy targets can be effectively reduced by using large-size Sc powder to prepare core-shell structure AlSc alloy powder.
The invention is further illustrated by the drawings and the detailed description which follow, but are not meant to limit the scope of the invention.
Drawings
FIG. 1 is a flow chart of a low segregation aluminum scandium alloy target preparation. Wherein, include: and mixing Sc powder and Al powder with a binder, performing heat treatment on the sintered powder to obtain core-shell structure AlSc alloy powder, and performing hot-pressing sintering to obtain the low-segregation aluminum scandium alloy target.
Detailed Description
For a better understanding of the present invention, the present invention will be described in detail below with reference to specific examples and comparative examples.
Examples 1 to 8
1. Weighing Sc powder: weighing Sc powder with purity of 3N, oxygen content of less than 300ppm and granularity of 60-100 mu m, and pouring into a powder mixer;
2. Adding alcohol and mixing: weighing alcohol with corresponding volume according to the proportion of adding 1mL of alcohol into each 100g of Sc powder, pouring the alcohol into a powder mixer, and filling Ar gas for mixing for 2 hours to obtain Sc powder with slightly moist surface;
3. Mixing Al powder: after the mixing is finished, 80at% of Al powder with the proportioning purity of 5N, the oxygen content of less than 100ppm and the granularity of 10 mu m is weighed, and placed in a powder mixer, ar gas is continuously filled for mixing for 5 hours, so that mixed powder of the Al powder adsorbed on the surface of Sc powder is obtained;
4. and (3) drying and sintering: placing the AlSc mixed powder in a vacuum sintering furnace for drying and sintering, removing alcohol, and enabling an Al powder and an Sc powder to form a sintering neck to be adhered together to form core-shell structure AlSc alloy powder of the Al-coated Sc, wherein the sintering temperature is 300 ℃, and the sintering time is 3 hours;
5. hot pressing and sintering: and (3) carrying out hot-pressing sintering on the obtained core-shell structure AlSc alloy powder, wherein the hot-pressing temperature is 300-650 ℃, the sintering pressure is 30MPa, the sintering time is 3-5 h, and finally, the AlSc alloy target material with Sc content fluctuation within +/-0.2%, oxygen content less than 200ppm, relative density not less than 99.5% and no crack is obtained.
Comparative example 1
1. Weighing: al blocks and Sc blocks in the proportion of Al-20at% Sc are weighed.
2. Smelting: and (3) placing the Al blocks and the Sc blocks into a smelting furnace for heating and smelting, wherein the smelting temperature is 1300 ℃, and the heat preservation is carried out for 20min.
3. Casting: casting the smelted AlSc alloy liquid into a mould for cooling to obtain AlSc alloy cast ingot;
4. And (3) rolling and annealing: and carrying out heat treatment annealing after rolling on AlSc alloy ingots to obtain AlSc alloy targets with cracks, wherein the fluctuation of Sc content is +/-7%, the oxygen content is 95ppm, and the relative density is not less than 99.5%.
Comparative example 2
1. Weighing Al powder and Sc powder: weighing Al powder with granularity of 1.5 mu m, purity of 5N, oxygen content of less than 150ppm and proportion of Al-20at% Sc, and Sc powder with granularity of 1.5 mu m, purity of 3N and oxygen content of less than 600 ppm;
2. dry blending: pouring Al powder and Sc powder into the mixed powder and carrying out dry mixing for 5 hours;
3. Hot pressing and sintering: and (3) placing the mixed AlSc alloy powder in a hot-pressing sintering furnace for sintering, wherein the hot-pressing temperature is 650 ℃, the sintering time is 5 hours, and finally, the AlSc alloy target material with Sc content fluctuation of +/-2%, oxygen content of 240ppm and no crack is obtained.
The main preparation processes and performances of AlSc alloy targets in examples 1 to 8 and comparative examples 1 and 2 are shown in Table 1.
Table 1 main preparation process of alloy targets of examples and comparative examples AlSc, fluctuation of composition, oxygen content and conditions of cracks
As can be seen from the results shown in table 1, the present technical solution has the following advantages:
(1) Avoiding component segregation: the core-shell structure AlSc alloy powder prepared by the method has uniform components, no secondary segregation phenomenon caused by different properties of two powders in the later transmission process, and the AlSc alloy target with low segregation can be obtained after the later hot-pressing sintering, wherein the fluctuation of the components is less than 0.18%, and the fluctuation of the components serving as a comparative example is more than 2%.
(2) The cracking does not occur: the AlSc alloy target prepared by adopting a common smelting mode or a powder metallurgy mode has the phenomenon that a large amount of brittle phases and stresses are easy to crack in comparative examples, and when the patent adopts core-shell structure AlSc alloy powder coated with Sc by Al to prepare AlSc alloy target, the Al has strong nuclear plasticity, and can be used as a 'binder' to prevent AlSc brittle phases from cracking in the later pressure sintering process.
(3) The oxygen content is low: the oxygen content in AlSc alloy targets is mainly brought by Sc, the oxygen content in Al powder is low, and the oxygen content in AlSc alloy targets can be effectively reduced by using large-size Sc powder to prepare core-shell structure AlSc alloy powder. As a result of the examples of the present invention, the oxygen content was less than 140ppm, and comparative example 2 was more than 200ppm.
Claims (1)
1. A preparation method of a low-segregation aluminum scandium alloy target material comprises the steps of providing a core-shell structure of an Al coated Sc, wherein the Sc content is 20-50at%, the component fluctuation is within +/-0.2%, the oxygen content is less than 200ppm, and the relative density is not less than 99.5% of AlSc alloy target material;
the preparation method comprises the following steps:
Weighing Sc powder with purity of more than 3N, oxygen content of less than 300ppm and granularity of 60-100 mu m, and pouring the Sc powder into a powder mixer;
Step (2), weighing alcohol with corresponding volume according to the proportion of adding 1-5 mL of alcohol into each 100g of Sc powder, pouring the alcohol into a powder mixer in the step (1) for filling Ar gas and mixing for 1-2 h to obtain Sc powder with slightly moist surface;
Weighing 5-10 mu m Al powder with the corresponding proportioning purity of more than 5N and the oxygen content of less than 100ppm after the mixing is finished, placing the Al powder in a powder mixer in the step (2), and continuously filling Ar gas for mixing for 2-5 h to obtain mixed powder of the Al powder adsorbed on the surface of Sc powder;
step (4), placing AlSc mixed powder obtained in the step (3) in a vacuum sintering furnace for drying and sintering, removing alcohol, and enabling an Al powder and an Sc powder to form a sintering neck to be adhered together to form Al-coated Sc core-shell structure AlSc alloy powder, wherein the sintering temperature is 100-300 ℃ and the sintering time is 1-3 hours;
and (5) carrying out hot-pressing sintering on the core-shell structure AlSc alloy powder obtained in the step (4), wherein the hot-pressing temperature is 300-650 ℃, the sintering pressure is 20-30 MPa, and the sintering time is 3-5 h, so as to obtain the AlSc alloy target.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108441827A (en) * | 2018-04-17 | 2018-08-24 | 长沙迅洋新材料科技有限公司 | Aluminium-scandium alloy target preparation method |
| CN110093588A (en) * | 2019-05-24 | 2019-08-06 | 福建阿石创新材料股份有限公司 | A kind of fine grain aluminium-scandium alloy target and its preparation method and application |
| CN111485207A (en) * | 2020-06-08 | 2020-08-04 | 福建阿石创新材料股份有限公司 | Fine-grain homogeneous high-scandium-content aluminum-scandium alloy sintering target material and preparation method and application thereof |
| CN111910160A (en) * | 2020-07-15 | 2020-11-10 | 湖南稀土金属材料研究院 | Preparation method of aluminum-scandium target material |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108441827A (en) * | 2018-04-17 | 2018-08-24 | 长沙迅洋新材料科技有限公司 | Aluminium-scandium alloy target preparation method |
| CN110093588A (en) * | 2019-05-24 | 2019-08-06 | 福建阿石创新材料股份有限公司 | A kind of fine grain aluminium-scandium alloy target and its preparation method and application |
| CN111485207A (en) * | 2020-06-08 | 2020-08-04 | 福建阿石创新材料股份有限公司 | Fine-grain homogeneous high-scandium-content aluminum-scandium alloy sintering target material and preparation method and application thereof |
| CN111910160A (en) * | 2020-07-15 | 2020-11-10 | 湖南稀土金属材料研究院 | Preparation method of aluminum-scandium target material |
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