CN112962072A - Low-oxygen large-size aluminum-based intermetallic compound-containing alloy target material and preparation method thereof - Google Patents
Low-oxygen large-size aluminum-based intermetallic compound-containing alloy target material and preparation method thereof Download PDFInfo
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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
- C23C14/34—Sputtering
- C23C14/3407—Cathode assembly for sputtering apparatus, e.g. Target
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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
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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
- C23C14/34—Sputtering
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Abstract
The invention discloses a low-oxygen large-size aluminum-based intermetallic compound-containing alloy target material and a preparation method thereof, the target material comprises aluminum and another high-melting-point metal M, wherein M is any one of Ti, Ni, Cr or 17 rare earth metal elements, the atomic percent of M is 1-50%, and the balance is aluminum metal, the preparation method comprises the processes of material preparation, blank making, temperature equalization treatment, post-treatment and the like, and the alloy target material is finally prepared, wherein the plane size of the alloy target material is not less than 104mm2The relative density is more than 98 percent, the content of the impurity oxygen is less than 600ppm, the sum of the contents of other impurities is less than 500ppm, and the average grain size is less than 150 mu m, thus the target material can be widely used as a target material for semiconductor sputtering film formation.
Description
Technical Field
The invention belongs to the technical field of aluminum-based alloy sputtering targets for semiconductors, and particularly relates to a low-oxygen large-size aluminum-based intermetallic metal-containing alloy target and a preparation method thereof.
Background
Sputtering targets are essential raw materials for the manufacture of very large scale integrated circuits. In the preparation process of a semiconductor, metal or alloy is required to be used as a sputtering target, and a high-energy ion beam current which is generated by an ion source and formed by accelerated aggregation in high vacuum is utilized to bombard the surface of the target, so that atoms on the surface of the target leave the target and are deposited on the surface of a substrate. The semiconductor has strict requirements on the purity of metal or alloy materials of sputtering targets, internal microstructures and the like, and products meeting the process requirements can be prepared by mastering key technologies in the production process and long-term practice. The semiconductor industry has very high requirements on the quality of sputtering targets, and accordingly the sputtering targets are required to develop towards large sizes along with the manufacture of wafers with larger sizes, and simultaneously, higher requirements on the grain orientation control of the sputtering targets are provided.
Aluminum and aluminum-based alloy targets, including aluminum-nickel, aluminum-chromium, aluminum-titanium, aluminum-erbium, aluminum-scandium and other aluminum rare earth alloy targets, are a class of sputtering targets and are widely applied in semiconductor preparation. The alloys have the common characteristics that the melting point difference between metal elements in the alloys and aluminum is large, the solubility in aluminum is low, intermetallic compound phases with high brittleness and high melting points are easily formed, and when the content of the metal elements is high, the ratio of the intermetallic compound phases is large, so that the alloys are easy to brittleness and difficult to deform. So that the alloy containing the aluminum-based intermetallic compound is difficult to be prepared into the target material meeting the process requirements.
In the prior art, a patent (application number: 201710046047.5) discloses a method for preparing an aluminum-based alloy by an aluminothermic reduction method, which is only suitable for preparing a conventional intermediate alloy due to the quality reasons of uniformity, content, impurities and the like; the patent (application number: 201510185516.2) also discloses a rotary target and a preparation method thereof, wherein an electric arc spraying method is used for preparing an alloy target, the alloy content is low, the thickness is only 3-15 mm, the density is 97%, and the use is limited; the patent (application number: 201610677045.1, 201910439319.7) adopts a powder metallurgy method to prepare the alloy target material, and inevitably has the problems of easy fragmentation, high oxygen content and the like; the patent (application numbers: 201711310758.5, 201811144477.1, 201810504228.2) provides a preparation method by fusion casting, the segregation of alloy ingots is serious, secondary precipitated phase grains are coarse, and the conventional pressure processing (hot rolling or hot forging) is difficult to prepare large-size complete target materials due to the intrinsic brittleness. These methods all have their own drawbacks, and it is difficult to prepare a sputtering alloy target for a semiconductor containing a low-oxygen large-size aluminum-based intermetallic compound.
Disclosure of Invention
In order to solve the problems in the prior art, the invention aims to provide an alloy target material containing low-oxygen large-size aluminum-based intermetallic compounds and a preparation method thereof.
In order to achieve the technical purpose, the invention adopts the following technical scheme:
an alloy target material of a low-oxygen large-size aluminum-based intermetallic compound comprises aluminum and another high-melting-point metal M, wherein the M is any one of Ti, Ni, Cr or 17 rare earth metal elements, the atomic percentage of the M is 1-50%, and the balance is aluminum metal; the plane size of the alloy target is not less than 1 multiplied by 104mm2The relative density is more than 98 percent, the content of the impurity oxygen is less than 600ppm, the sum of the contents of other impurities is less than 500ppm, and the average grain size is less than 150 mu m.
Preferably, the oxygen content of the alloy target is less than 100ppm, the sum of the contents of other impurities is less than 80ppm, and the average grain size is less than 80 μm.
More preferably, the oxygen content of the alloy target is less than 40ppm, the sum of the contents of other impurities is less than 10ppm, and the average grain size is less than 40 μm.
The invention also provides a preparation method of the alloy target, which comprises the following steps:
(1) ingredients
Mixing high-purity metal aluminum, high-purity metal M and an additive X according to a set atomic ratio to obtain a mixture, wherein the additive X is at least one of intermediate alloy of aluminum and the metal M and hydride of the metal M;
(2) blank making
Heating the mixture to be molten, and then pouring the mixture into a mold to obtain a blank;
(3) temperature equalization treatment
Carrying out temperature equalization treatment on the blank and then cooling;
(4) post-treatment
And (3) hot-pressing or hot-rolling the blank subjected to uniform temperature treatment to prepare a large-size plate blank, annealing and machining to prepare the target.
Preferably, in the step (1), the addition amount of the additive X is 0.1-20% of the total weight of the mixture, and more preferably 1-10%.
Preferably, in the step (1), the additive X is a mixture of an intermediate alloy of aluminum and a metal M and a hydride of the metal M, and the mass ratio of the intermediate alloy of aluminum and the metal M to the hydride of M is 0.2-5: 1, more preferably 0.5 to 2: 1.
in the invention, the intermediate alloy of aluminum and metal M is used as an additive, so that the uniform fusion of pure aluminum and pure M is facilitated during melting, and the intermediate alloy is easy to solidify firstly during cooling to play roles in nucleating mass points, rapidly fusing and refining grains; and the hydride of the metal M is further added, which is easy to decompose at high temperature to obtain free active hydrogen, is easy to combine with oxygen in the environment to form gaseous water vapor, plays a role in removing oxygen, and hydrogen in the melt is easy to separate from the melt and float out of the liquid level to take impurities out of the melt, and plays a role in removing impurities. The two are mixed and cooperated to play the roles of homogenizing the melt, removing oxygen and impurities and refining crystal grains.
Preferably, in the step (1), the high-purity metal aluminum and the high-purity metal M are both subjected to oxygen removal and impurity removal treatment, for example, surface impurities are removed by remelting, or surface activation treatment and cleaning with alcohol and airing, so as to reduce the impurity content of the raw material, wherein the purity of the high-purity metal aluminum and the high-purity metal M is not lower than 99.95%; more preferably, the purity of the high-purity metal aluminum and the high-purity metal M is not lower than 99.995 percent; most preferably, the purity of the high-purity metal aluminum and the high-purity metal M is not lower than 99.9995%.
Preferably, in the step (2), the mixture is placed in a crucible, the temperature is raised to 200-600 ℃, and the temperature is kept for 1-20 min; heating to a temperature higher than the melting point by more than 10 ℃ at a speed of 20-200 ℃/min, melting, fully stirring uniformly, and standing for 5-30 min; pouring the mixture into a mold with controllable cooling speed, cooling to 100-600 ℃, and controlling the cooling speed to be not lower than 1 ℃/s; the cooling rate is preferably controlled to not less than 50 ℃/s, and more preferably to not less than 100 ℃/s. In the invention, the preferable cooling speed is controlled so that the low-melting-point phase and the high-melting-point phase of the melt are rapidly solidified, and the segregation and layering phenomena caused by the first solidification and abnormal growth of the high-melting-point phase are reduced, so that the blank is more homogenized. The crucible is preferably a non-pollution crucible which does not react with the melt and reduces unnecessary pollution caused by the crucible, such as a water-cooled copper crucible or a crucible which is protected by a high-temperature coating which does not react with the melt.
Preferably, in the step (3), the blank is cooled to room temperature after being subjected to temperature equalization for 0.5-48 hours at 100-600 ℃.
Preferably, both the blank making in the step (2) and the temperature equalization treatment in the step (3) are in an anaerobic environment, and the oxygen partial pressure in the anaerobic environment is not higher than 0.05Pa, preferably not higher than 0.001Pa, and further preferably not higher than 0.0001 Pa.
Preferably, in the step (4), the strain rate of hot pressing or hot rolling is not higher than 10mm/s, preferably not higher than 1mm/s, more preferably not higher than 0.1 mm/s; in the present invention, the preferred strain rate facilitates the coordinated deformation between the soft phase (α -Al phase) and the hard phase (intermetallic phase) in the alloy, reducing the phenomenon of cracking of the billet during deformation.
The working principle is as follows:
in the invention, the material is melted and processed in the environment of less oxygen, oxygen control and oxygen reduction by a multi-channel and multi-means, such as the control of the purity of the raw material, the control of the anaerobic environment, the treatment of removing oxygen and impurities and the action of additives, and the content of oxygen and other impurities in the blank is limited and reduced to the maximum extent, thereby improving the cleanliness of the blank; the cooling speed of the poured blank is controlled in a speed control cooling mode, so that the solidification environment is improved, the segregation and layering phenomena are reduced, the uniformity of the material is further improved by means of melt stirring, blank temperature equalization treatment, post-processing treatment and the like, and the homogeneity degree of the blank is improved; through the deformation processing with controllable speed, the coordinated deformation of each phase in the alloy is effectively promoted, so that the blank is not easy to crack in the deformation process, the structure and the structure of the material are favorably improved, and the compactness of the material is improved. In a word, the invention can prepare high-quality blank with low content of oxygen and other impurities, good compactness, uniform components and controllable crystal grains under the synergistic action of the above means.
Compared with the prior art, the invention has the advantages that:
1. the target material has low impurity and oxygen content: the raw materials have high purity, and the impurity content is greatly reduced by deoxidizing and removing impurities; the blank adopts a pollution-free crucible blank making process, so that the introduction of impurities in the synthesis process is avoided; the whole preparation process of the large-size target blank is treated in an anaerobic environment, so that the introduction of impurities such as oxygen is greatly reduced; the additive X can react with and be separated from partial impurities in the melt, so that the impurity content in the blank can be effectively removed, and an alloy product with low impurity and oxygen content can be obtained, so that the oxygen content of the target impurity is less than 600ppm, the sum of the other impurity contents is less than or equal to 100ppm, even the oxygen content is less than 40ppm, and the sum of the other impurity contents is less than or equal to 10 ppm.
2. The target material has good density: through the hot pressing or hot rolling treatment with controllable strain rate, the target material has good integrity, air holes and impurities in the material can be obviously eliminated, and the density of the material is improved.
3. The uniformity of the components is good: the component uniformity of the large-size target material is ensured by uniformly stirring and cooling the melt at a controlled speed in the blank making process and carrying out long-time temperature equalization treatment in a low-temperature state.
4. The crystal orientation of crystal grains is controllable: the blank is annealed after hot pressing or hot rolling, the components of the material are uniform, the crystal orientation of crystal grains is controllable, and the average crystal grain size can be controlled to be less than 150 mu m or even less than 40 mu m.
Based on the above, the method solves the difficulty that the low-oxygen large-size aluminum-containing intermetallic compound-containing alloy target is difficult to prepare, obtains the large-size high-quality target with low content of oxygen and other impurities, good compactness, uniform components and controllable crystal grains, is favorable for uniformly sputtering and forming a film in the semiconductor preparation process, and finally obtains the wafer with good stability and low rejection rate.
Detailed Description
The present invention is further described in detail below by way of examples, and the scope of the patent protection of the present invention includes, but is not limited to, these.
Example 1
The preparation process of the Al-10Ti alloy target material comprises the following steps:
(1) the atomic ratio of the aluminum to the titanium is 9:1, the raw materials are high-purity aluminum and high-purity titanium, the purity of the raw materials is more than or equal to 99.95 percent, the additive X is added in an amount which is 5 percent of the total weight, and during the oxygen and impurity removing treatment, 5 percent of oxalic acid activating solution is used for surface activation treatment and is cleaned by alcohol and dried;
(2) and (3) blank making, namely putting the prepared materials into a crucible, heating to 500 ℃, and keeping the temperature for 15 minutes. Then heating to 1350 deg.C (Al-10Ti melting point about 1290 deg.C) at 50 deg.C/min, stirring, and standing for 10 min. Then pouring the mixture into a mold with controllable cooling speed, and cooling to 600 ℃, wherein the cooling speed is controlled at 60 ℃/s. The crucible is a pollution-free crucible protected by a boron nitride protective coating on the surface, and the coating does not react with the melt, so that unnecessary pollution brought by the crucible is reduced.
(3) And (4) carrying out temperature equalization treatment, namely carrying out temperature equalization on the blank in an environment at 150 ℃ for 24 hours, and then cooling the blank to room temperature.
(4) The blank after post-treatment and temperature equalization can be processed into a large-size plate blank by hot rolling with the strain rate of 2mm/s, and then annealed and machined to obtain the target material, wherein the size specification is 150mm in diameter and 2mm in height.
In the whole blank making and temperature equalizing treatment process, the raw materials and the blanks are in an anaerobic environment, and the oxygen partial pressure in the anaerobic environment is less than 0.05 Pa.
Finally, the large-size target is prepared, and the corresponding additive composition and the detection result of the target are shown in the table, wherein 5 points are taken from different parts of the upper surface and the lower surface of the target for analyzing alloy elements, impurity content, relative density and grain size (mum), the result in the table 1 is obtained, and the component deviation is the maximum difference of the 5-point titanium component analysis. As a result, the atomic ratio of titanium in the four alloys is about 10%, but the oxygen content and other impurity contents of the alloy A4 without the additive are uniformly high, the average uniform grain size is large, the relative density is low, and the composition deviation is large; after the intermediate alloy is added, the grain size and the component deviation are obviously reduced, and the content of oxygen and other impurities can be reduced by adding the hydride; the addition of a mixture of intermetallic and hydride showed good results.
Table 1 data table of the test results of different targets
Example 2
The preparation process of the Al-10Sc alloy target material is as follows:
(1) the atomic ratio of the ingredient aluminum to scandium is 90:10, the raw materials are high-purity aluminum, high-purity scandium and an additive X, the purity of the raw materials is more than or equal to 99.9998%, and impurities on the surface of the high-purity metal are removed through remelting during the deoxidization and impurity removal treatment of the high-purity metal; wherein the additive X is a scandium hydride substance and accounts for 3 percent of the total weight of the raw materials.
(2) And (3) blank making, namely putting the prepared materials into a crucible, heating to 580 ℃, and keeping the temperature for 5 minutes. Then heating to 1200 deg.C (the melting point of Al-10Sc alloy is about 1100 deg.C) at 50 deg.C/min, stirring, and standing for 20 min. Then pouring the mixture into a mold with controllable cooling speed, cooling the mixture to 580 ℃, and controlling the cooling speed to be 200 ℃/s. The crucible is a water-cooled copper crucible protected by a boron nitride protective coating on the surface, and the crucible is not contacted with the melt, so that unnecessary pollution brought by the crucible is reduced.
(3) Temperature equalization treatment the blank is equalized at 580 ℃ for 1 hour and then furnace-cooled to room temperature.
(4) The blank after post-treatment and temperature equalization can be processed into a large-size plate blank by hot rolling with the strain rate of 8mm/s, and then the large-size plate blank is annealed and machined to prepare the target.
In the whole blank making and temperature equalizing treatment process, the raw materials and the blanks are in an anaerobic environment, and the oxygen partial pressure in the anaerobic environment is less than 0.0001 Pa.
Finally, the large-size target is prepared, wherein the atomic percent content of scandium is 10.01 at.%, the deviation of components is +/-0.23%, the size specification is that the diameter is 350mm and the height is 10mm, the content of impurity oxygen of the target is 7.8ppm, the sum of the contents of other impurities is less than 6.5ppm, the relative density is 99.8%, and the average grain size is 30.25 mu m.
Example 3
The preparation process of the Al-15Cr alloy target material comprises the following steps:
(1) the atomic ratio of the ingredient aluminum to scandium is 85:15, the raw materials are high-purity aluminum, high-purity chromium and additive X, the purity of the raw materials is more than or equal to 99.98 percent, and the high-purity metal is subjected to surface activation treatment and is cleaned by alcohol and dried in the air when the high-purity metal is subjected to deoxidization and impurity removal treatment; wherein the additive X is Al-50Cr intermediate alloy and accounts for 6 percent of the total weight of the raw materials.
(2) And (3) blank making, namely putting the prepared materials into a crucible, heating to 480 ℃, and preserving heat for 10 minutes. Then the temperature is increased to 1050 ℃ (the melting point of the Al-15Cr alloy is about 980 ℃) by 30 ℃/min for melting, and the mixture is placed for 15 minutes after being fully stirred uniformly. Then pouring the mixture into a mold with controllable cooling speed, cooling the mixture to 560 ℃, and controlling the cooling speed to be 200 ℃/s. The crucible is a water-cooled copper crucible protected by a boron nitride protective coating on the surface, and the crucible is not contacted with the melt, so that unnecessary pollution brought by the crucible is reduced.
(3) Temperature equalization treatment the blank is equalized at 560 ℃ for 1 hour and then furnace-cooled to room temperature.
(4) The blank after post-treatment and temperature equalization can be processed into a large-size plate blank by hot rolling with the strain rate of 0.05mm/s, and then the large-size plate blank is annealed and machined to prepare the target.
In the whole blank making and temperature equalizing treatment process, the raw materials and the blanks are in an anaerobic environment, and the oxygen partial pressure in the anaerobic environment is less than 0.001 Pa.
Finally, the large-size target is prepared, wherein the atomic percent content of chromium is 14.91 at.%, the size specification is that the diameter is 200mm multiplied by the height is 30mm, the oxygen content of the target impurity is 267.9ppm, the sum of the contents of other impurities is less than 134.6ppm, the relative density is 99.9%, and the average grain size is 18.6 mu m.
Example 4
The preparation process of the Al-15Cr alloy target material comprises the following steps:
(1) the atomic ratio of the ingredient aluminum to scandium is 85:15, the raw materials are high-purity aluminum, high-purity chromium and additive X, the purity of the raw materials is more than or equal to 99.98 percent, and the high-purity metal is subjected to surface activation treatment and is cleaned by alcohol and dried in the air when the high-purity metal is subjected to deoxidization and impurity removal treatment; wherein the additive X is Al-50Cr intermediate alloy and accounts for 6 percent of the total weight of the raw materials.
(2) And (3) blank making, namely putting the prepared materials into a crucible, heating to 480 ℃, and preserving heat for 10 minutes. Then the temperature is increased to 1050 ℃ (the melting point of the Al-15Cr alloy is about 980 ℃) by 30 ℃/min for melting, and the mixture is placed for 15 minutes after being fully stirred uniformly. Then pouring the mixture into a mold with controllable cooling speed, cooling the mixture to 560 ℃, and controlling the cooling speed to be 200 ℃/s. The crucible is a water-cooled copper crucible protected by a boron nitride protective coating on the surface, and the crucible is not contacted with the melt, so that unnecessary pollution brought by the crucible is reduced.
(3) Temperature equalization treatment the blank is equalized at 560 ℃ for 1 hour and then furnace-cooled to room temperature.
(4) The blank after post-treatment and temperature equalization can be processed into a large-size plate blank by hot rolling with the strain rate of 20mm/s, and then the large-size plate blank is annealed and machined to prepare the target.
In the whole blank making and temperature equalizing treatment process, the raw materials and the blanks are in an anaerobic environment, and the oxygen partial pressure in the anaerobic environment is less than 0.001 Pa.
Finally, the large-size target is prepared, the atomic percent content of chromium is 15.01 at.%, the blank is cracked, the oxygen content of the target impurity is 252.1ppm, the sum of the contents of other impurities is less than 136.7ppm, the relative density is 98.1%, and the average grain size is 132.2 μm.
Claims (10)
1. An alloy target material of a low-oxygen large-size aluminum-based intermetallic compound is characterized in that: the alloy comprises aluminum and another high-melting-point metal M, wherein M is any one of Ti, Ni, Cr or 17 rare earth metal elements, the atomic percentage of M is 1-50%, and the balance is aluminum metal; the plane size of the alloy target is not less than 1 multiplied by 104mm2The relative density is more than 98 percent, the content of the impurity oxygen is less than 600ppm, the sum of the contents of other impurities is less than 500ppm, and the average grain size is less than 150 mu m.
2. The low-oxygen large-size aluminum-based intermetallic compound-containing alloy target according to claim 1, characterized in that: the oxygen content of the alloy target is less than 100ppm, the sum of the contents of other impurities is less than 80ppm, and the average grain size is less than 80 mu m.
3. The low-oxygen large-size aluminum-based intermetallic compound-containing alloy target according to claim 2, wherein: the oxygen content of the alloy target is less than 40ppm, the sum of the contents of other impurities is less than 10ppm, and the average grain size is less than 40 mu m.
4. The method for preparing an alloy target material of a low-oxygen large-size aluminum-based intermetallic compound according to any of claims 1 to 3, comprising the steps of:
(1) ingredients
Mixing high-purity metal aluminum, high-purity metal M and an additive X according to a set atomic ratio to obtain a mixture, wherein the additive X is at least one of intermediate alloy of aluminum and the metal M and hydride of the metal M;
(2) blank making
Heating the mixture to be molten, and then pouring the mixture into a mold to obtain a blank;
(3) temperature equalization treatment
Carrying out temperature equalization treatment on the blank and then cooling;
(4) post-treatment
And (3) hot-pressing or hot-rolling the blank subjected to uniform temperature treatment to prepare a large-size plate blank, annealing and machining to prepare the target.
5. The method of claim 4, wherein: in the step (1), the addition amount of the additive X is 0.1-20% of the total weight of the mixture.
6. The method of claim 4, wherein: in the step (1), the additive X is a mixture of an intermediate alloy of aluminum and metal M and a hydride of high-purity metal M, and the mass ratio of the intermediate alloy of aluminum and metal M to the hydride of M is 0.2-5: 1.
7. the method of claim 4, wherein: in the step (1), the high-purity metal aluminum and the high-purity metal M are subjected to deoxidization and impurity removal treatment, wherein the purities of the high-purity metal aluminum and the high-purity metal M are not lower than 99.95%.
8. The method of claim 4, wherein: in the step (2), placing the mixture in a crucible, heating to 200-600 ℃, and preserving heat for 1-20 min; heating to a temperature higher than the melting point by more than 10 ℃ at a speed of 20-200 ℃/min, melting, fully stirring uniformly, and standing for 5-30 min; pouring the mixture into a mold with controllable cooling speed, cooling to 100-600 ℃, and controlling the cooling speed to be not less than 1 ℃/s.
9. The method of claim 4, wherein: in the step (3), the blank is cooled to room temperature after being subjected to temperature equalization for 0.5-48 h at the temperature of 100-600 ℃;
both the blank making in the step (2) and the temperature equalizing treatment in the step (3) are in an anaerobic environment, and the oxygen partial pressure in the anaerobic environment is not higher than 0.05 Pa.
10. The method of claim 4, wherein: in the step (4), the strain rate of hot pressing or hot rolling is not higher than 10 mm/s.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202110142280.XA CN112962072B (en) | 2021-02-02 | 2021-02-02 | Low-oxygen large-size aluminum-based intermetallic compound-containing alloy target and preparation method thereof |
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| CN202110142280.XA CN112962072B (en) | 2021-02-02 | 2021-02-02 | Low-oxygen large-size aluminum-based intermetallic compound-containing alloy target and preparation method thereof |
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| CN112962072A true CN112962072A (en) | 2021-06-15 |
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