CN113373350B - Aluminum alloy ingot for target material, preparation method thereof and aluminum alloy target material - Google Patents
Aluminum alloy ingot for target material, preparation method thereof and aluminum alloy target material Download PDFInfo
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- CN113373350B CN113373350B CN202110635037.1A CN202110635037A CN113373350B CN 113373350 B CN113373350 B CN 113373350B CN 202110635037 A CN202110635037 A CN 202110635037A CN 113373350 B CN113373350 B CN 113373350B
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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
- C22C21/02—Alloys based on aluminium with silicon as the next major constituent
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
- B22D1/00—Treatment of fused masses in the ladle or the supply runners before casting
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
- B22D7/00—Casting ingots, e.g. from ferrous metals
- B22D7/005—Casting ingots, e.g. from ferrous metals from non-ferrous metals
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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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- 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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Abstract
The application relates to the technical field of target manufacturing, in particular to an aluminum alloy ingot for a target, a preparation method of the aluminum alloy ingot and an aluminum alloy target. The aluminum alloy cast ingot for the target material contains aluminum and an additive element. Wherein, the added elements in the aluminum alloy ingot satisfy the following conditions: the target content value of the additive element in the aluminum alloy ingot is a wt%, the content of the additive element in a plurality of samples is detected by multipoint sampling on the cross section of the aluminum alloy ingot to obtain a plurality of additive element content values, and the content values of the plurality of additive elements are all in the range of 0.9 a-1.1 a wt%. The aluminum alloy cast ingot for the target has uniform structure, and can achieve the purpose of inhibiting abnormal discharge of the sputtering target in the sputtering process.
Description
Technical Field
The application relates to the field of target manufacturing, in particular to an aluminum alloy ingot for a target, a preparation method of the aluminum alloy ingot and an aluminum alloy target.
Background
At present, the target material of aluminum wiring improves the stability of a thin film in a circuit by adding elements such as Si and Cu. However, the target material is likely to be abnormally discharged during sputtering.
Disclosure of Invention
The inventors have studied on an aluminum alloy target and found that the reason why abnormal discharge is likely to occur when the aluminum alloy target is sputtered is: the target material has a coarse structure (coarse structure means a structure in which the structure particle size is 5 times or more the average structure particle size), and the surface of the target material is uneven, so that many particles are generated during sputtering of the target material, and sputtering is not uniform, thereby causing abnormal discharge. The inventors further investigated and found that the reason for the occurrence of coarse structures in aluminum alloy target materials is that: when an aluminum alloy ingot is prepared, the additive elements in the aluminum alloy ingot are not uniformly distributed in the aluminum, so that a coarse structure may appear in the ingot.
An object of the embodiments of the present application is to provide an aluminum alloy ingot for a target, a method for producing the same, and an aluminum alloy target, which aim to suppress abnormal discharge during sputtering of the target.
In a first aspect, the present application provides an aluminum alloy ingot for a target, which contains aluminum and an additive element. Wherein, the added elements in the aluminum alloy ingot satisfy the following conditions: the target content value of the additive elements in the aluminum alloy ingot is a wt%, the content of the additive elements in a plurality of samples is detected by sampling at multiple points on the cross section of the aluminum alloy ingot to obtain a plurality of additive element content values, and the content values of the plurality of additive elements are all in the range of 0.9 a-1.1 a wt%.
The maximum value and the minimum value in the content values of a plurality of additive elements are within +/-10%, and the additive elements are uniformly distributed in aluminum, so that the generation of coarse and large structures can be reduced to a certain extent, and the abnormal discharge phenomenon during sputtering of the target material is reduced to a certain extent.
In some embodiments of the first aspect of the present application, the plurality of additive element content values are each in the range of 0.95a to 1.05a wt%.
Namely, the deviation of the maximum value and the minimum value in the content values of a plurality of additive elements is within +/-5%, the additive elements are more uniformly distributed in the aluminum, the generation of coarse structures can be further reduced, and the generation of abnormal discharge phenomenon during the sputtering of the target material is further reduced.
In some embodiments of the first aspect of the present application, the additive element is Cu, the target Cu content value is 0.5 wt%, and the Cu content values are obtained by performing multi-point sampling on the cross section of the aluminum-copper alloy ingot to detect the Cu content in a plurality of samples, and are each in a range of 0.45 to 0.55 wt%.
If the target Cu content in the aluminum-copper alloy ingot is 0.5 wt%, the Cu content distributed at each part of the aluminum-copper alloy ingot is within 0.45-0.55 wt% (the deviation is within +/-10%), which indicates that the copper is distributed in the ingot more uniformly, and the generation of coarse structures in the aluminum-copper alloy ingot can be reduced, so that the abnormal discharge phenomenon during sputtering of the aluminum-copper alloy target is reduced.
In some embodiments of the first aspect of the present application, the additive element is Si, the target Si content value is 1 wt%, and the Si content values are obtained by performing multi-point sampling on the cross section of the al-Si alloy ingot to detect the Si content in a plurality of samples, and are each in a range of 0.9 to 1.1 wt%.
If the target content of Si in the aluminum-silicon alloy ingot is 1 wt%, the content of Si distributed at each part of the aluminum-silicon alloy ingot is within 0.9-1.1 wt% (the deviation is within +/-10%), which indicates that the Si is distributed in the ingot more uniformly, and the generation of coarse structures in the aluminum-silicon alloy ingot can be reduced, so that the abnormal discharge phenomenon during sputtering of the aluminum-silicon alloy target material is reduced.
The second aspect of the present application provides a method for preparing an aluminum alloy ingot for a target, which mainly comprises: in the hot top casting process, a stirring mechanism is adopted to stir molten aluminum alloy liquid at the hot top or/and the diversion trench or/and the melting furnace, and an aluminum alloy ingot is obtained by casting.
The molten aluminum alloy liquid is stirred to obtain an ingot with uniform structure, and the target material obtained by processing the ingot can improve the formation of relatively large concave-convex parts on the surface of the target material due to coarsening of the structure, thereby realizing the purpose of inhibiting abnormal discharge of the sputtering target material in the sputtering process.
In some embodiments of the second aspect of the present application, further comprising: in the hot top casting process, a heating mechanism is added at the hot top to control the temperature of the hot top within +/-3% of the temperature of the molten aluminum alloy liquid.
The molten aluminum alloy liquid in the hot top part can be heated more uniformly to form a uniform structure, and the distribution of the additive elements in the cross section of the finally obtained cast ingot is more uniform.
In some embodiments of the second aspect of the present application, the stirring mechanism is a rotary stirring mechanism during hot top casting; the rotation speed of the stirring mechanism is more than 30 rpm.
In some embodiments of the second aspect of the present application, the stirring mechanism is a vibrating stirring mechanism during hot top casting; the vibration frequency of the vibration type stirring mechanism is more than 50 times/min.
In some embodiments of the second aspect of the present application, the stirring mechanism is an ultrasonic stirrer during hot top casting; the ultrasonic frequency of the ultrasonic stirrer is above 100 kHz.
The third aspect of the present application provides an aluminum alloy target material, which is obtained by processing the aluminum alloy ingot for the target material provided by the first aspect.
The aluminum alloy target provided by the application has the advantages that the grain structure is uniform, the surface is regular, and the purpose of inhibiting abnormal discharge is achieved in the sputtering process.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present application, the drawings needed to be used in the embodiments are briefly described below, it should be understood that the following drawings only illustrate some embodiments of the present application and therefore should not be considered as limiting the scope, and for those skilled in the art, other related drawings can be obtained from the drawings without inventive efforts and also belong to the protection scope of the present application.
Fig. 1 is a schematic structural diagram of an apparatus in a hot top casting process according to an embodiment of the present application.
Icon: 110-hot top; 120-a stirring mechanism; 130-a diversion trench; 140-melting furnace.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present application clearer, the technical solutions in the embodiments of the present application will be clearly and completely described below. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
In the description of the present application, "above", "below" and "within" include the number itself; the range of "numerical value a to numerical value b" includes both values "a" and "b", and "unit of measure" in "numerical value a to numerical value b + unit of measure" represents both "unit of measure" of "numerical value a" and "numerical value b".
The aluminum alloy ingot for the target material of the embodiment of the present application, the preparation method thereof, and the aluminum alloy ingot are specifically described below.
The application provides an aluminum alloy ingot for a target, which contains aluminum and an additive element. Wherein, the added elements in the aluminum alloy ingot satisfy the following conditions: the target content value of the additive elements in the aluminum alloy ingot is a wt%, the content of the additive elements in a plurality of samples is detected by sampling at multiple points on the cross section of the aluminum alloy ingot to obtain a plurality of content values of the additive elements, and the content values of the additive elements are all within the range of 0.9 a-1.1 a wt% (the deviation is within +/-10%).
For example: taking an aluminum alloy ingot provided by the application, slitting the aluminum alloy ingot to obtain a cross section, taking six samples (in other embodiments, 7 samples, 8 samples, 9 samples and the like can be taken, and the application is not limited), detecting the content of the additive elements in the six samples to obtain six additive element content values, wherein the six additive element content values are respectively 0.9a wt%, 0.95a wt%, 0.98a wt%, 1.05a wt% or 1.1a wt%, and therefore, the six additive element content values are all in the range of 0.9 a-1.1 a wt%.
Alternatively, the plurality of additive element content values are all in the range of 0.95a to 1.05a wt% (all within ± 5%). For example: six samples of another aluminum alloy ingot were taken by the above method to examine the content of the additive elements, and six additive element content values were obtained, which were 0.95a wt%, 0.98a wt%, 1a wt%, 1.01a wt%, 1.03a wt%, or 1.05a wt%, respectively, so that the six additive element content values were all in the range of 0.95a to 1.05a wt%.
In one embodiment, if the additive element is Cu, the ingot is an aluminum-copper ingot, the target Cu content value in the aluminum-copper ingot is 0.5 wt%, and the Cu content values in a plurality of samples are detected by multi-point sampling on the cross section of the aluminum-copper alloy ingot to obtain a plurality of Cu content values, wherein the Cu content values are all within the range of 0.45-0.55 wt% (the deviation is within +/-10%). Optionally, the Cu content values are all within a range of 0.48-0.52 wt% (all within + -4%).
In another embodiment, if the additive element is Si, the target Si content value is 1 wt%, and the Si content in a plurality of samples is detected by multi-point sampling on the cross section of the aluminum-silicon alloy ingot to obtain a plurality of Si content values, wherein the plurality of Si content values are all within the range of 0.9-1.1 wt% (the deviation is within +/-10%). Alternatively, the plurality of Si content values are each in the range of 0.98 to 1.02 wt% (each within. + -. 2%).
The aluminum alloy ingot with the uniformly distributed additive elements can be used for preparing an aluminum alloy target material, and the defect of abnormal discharge of the target material during sputtering can be avoided to a certain extent.
The processing method is generally as follows: and forging, rolling, heat treating and cutting the cast ingot to obtain the aluminum alloy target.
The method of making an aluminum alloy ingot generally comprises: batching, smelting and casting, whereas casting is usually carried out by hot-top casting processes. In order to obtain an aluminum alloy ingot with more uniformly distributed added elements, the process of the hot top casting process is improved.
FIG. 1 is a schematic structural diagram of an apparatus for hot top casting according to an embodiment of the present application. Referring to fig. 1, the apparatus includes a melting furnace 140, a guiding gutter 130 and a hot top 110 according to the flow direction of hot top casting, wherein aluminum and additive elements are melted in the melting furnace 140 to form an aluminum alloy liquid, and the aluminum alloy liquid is transported into the hot top 110 through the guiding gutter 130, and then aluminum alloy ingot casting is performed. The hot top casting process comprises the following specific steps: and stirring the molten aluminum alloy liquid in the hot top part 110, or/and the guide groove 130, or/and the melting furnace 140 by using a stirring mechanism 120, and casting to obtain an aluminum alloy ingot.
The molten aluminum alloy liquid is stirred to obtain an ingot with uniform structure, and the target material obtained by processing the ingot can improve the formation of relatively large concave-convex parts on the surface of the target material due to coarsening of the structure, thereby realizing the purpose of inhibiting abnormal discharge of the sputtering target material in the sputtering process.
If the molten aluminum alloy liquid is stirred in the melting furnace 140, the aluminum element and the additive element in the molten aluminum alloy liquid can be uniformly mixed so that the structure of the aluminum alloy ingot obtained subsequently becomes uniform. However, the molten aluminum alloy may be layered after being uniformly mixed by the stirring mechanism 120 in the melting furnace 140 and passing through the guide chute 130 and the hot top 110, and thus the stirring effect needs to be further improved. If the molten aluminum alloy liquid is stirred in the hot top 110, the aluminum element and the additive element in the molten aluminum alloy liquid can be uniformly mixed, so that the structure of the aluminum alloy cast ingot obtained subsequently is uniform, and the stirring effect is good. However, the molten aluminum alloy liquid itself contains alumina, which floats on the surface of the molten aluminum alloy liquid on the hot top, and if it is stirred by the stirring mechanism 120, alumina may enter the aluminum alloy ingot, and alumina impurities may be present in the ingot, and the ingot casting effect needs to be further improved.
If the molten aluminum alloy liquid is stirred in the diversion trench 130, the aluminum element and the additive element in the molten aluminum alloy liquid can be uniformly mixed, so that the structure of the aluminum alloy cast ingot obtained subsequently is uniform, and the stirring effect is good. And the molten alloy liquid after passing through the guiding gutter 130 directly enters the hot top 110, so that the aluminum element and the additive element in the molten alloy liquid can be prevented from layering, and meanwhile, alumina floats on the surface of the hot top and cannot enter the molten alloy liquid below, so that the ingot casting structure is uniform, and alumina impurities cannot exist.
It should be noted that: in the actual hot top casting process, stirring may be performed at one or more positions of the melting furnace 140, the guiding gutter 130 and the hot top 110, which is not limited in this application.
If the target content of the added element is awt%: during batching, the aluminum alloy ingot is obtained by mixing the components according to the proportion that the content of the added elements is awt percent and the content of aluminum is (100-a) wt percent, then carrying out hot top casting after smelting, and stirring molten aluminum alloy liquid at the hot top by adopting a stirring mechanism during the hot top casting, and casting. In the aluminum alloy ingot, the content of the additive elements in a plurality of samples is detected by sampling at multiple points on the cross section of the aluminum alloy ingot to obtain a plurality of additive element content values, and the content values of the plurality of additive elements are all within the range of 0.9 a-1.1 a wt% (the deviation is within +/-10%).
Optionally, a heating mechanism is added to the hot top during the hot top casting process to control the temperature of the hot top within ± 3% of the temperature of the molten aluminum alloy liquid. In other words, the temperature of the hot top is in the range of the molten aluminum alloy melt temperature x (0.97 to 1.03). Stirring the hot top at the temperature until the hot top is solidified into an ingot, and forming a uniform structure; stirring at the above temperature makes the distribution of the additive elements more uniform in the cross section of the ingot to be finally obtained. In the aluminum alloy ingot, the content of the additive elements in a plurality of samples is detected by sampling at multiple points on the cross section of the aluminum alloy ingot to obtain a plurality of additive element content values, and the content values of the plurality of additive elements are all within the range of 0.95 a-1.05 a wt% (the deviation is within +/-5%).
In one embodiment, if the additive element is Cu and the target Cu content is 0.5 wt%, the additive elements are mixed according to the proportion that the Cu content is 0.5 wt% and the Al content is 99.5 wt% during batching, and then the mixture is smelted and then subjected to hot top casting, and during the hot top casting, a stirring mechanism is adopted to stir molten aluminum-copper alloy liquid at the hot top, so that an aluminum-copper alloy ingot is obtained through casting. In the aluminum-copper alloy ingot, the Cu content in a plurality of samples is sampled and detected at multiple points on the cross section of the aluminum-copper alloy ingot to obtain a plurality of Cu content values, and the Cu content values are all within the range of 0.45-0.55 wt% (the deviation is within +/-10%). The structure in the cast ingot can be uniform, the coarse structure on the surface of the target material can be prevented, and abnormal discharge in the sputtering process can be effectively inhibited.
In another embodiment, if the additive element is Si, and the target content of Si is 1 wt%, then during compounding, the Si content is 1 wt% and the Al content is 99 wt%, and then the mixture is mixed, and then the mixture is smelted and then hot top cast, and during the hot top cast, the molten aluminum-silicon alloy liquid at the hot top is stirred by a stirring mechanism, and cast to obtain the aluminum-silicon alloy ingot. In the aluminum-silicon alloy ingot, the content of Si in a plurality of samples is sampled and detected at multiple points on the cross section of the aluminum-silicon alloy ingot to obtain a plurality of Si content values, and the Si content values are all within the range of 0.98-1.02 wt% (the deviation is within +/-10%). The structure in the cast ingot can be uniform, the coarse structure on the surface of the target material can be prevented, and the abnormal discharge in the sputtering process can be effectively inhibited.
In one embodiment, the stirring mechanism may be a rotary stirring mechanism, and the molten aluminum alloy liquid at the hot top is stirred by the rotary stirring mechanism to obtain an aluminum alloy ingot. Wherein the rotation speed of the rotary stirring mechanism is more than 30 rpm. Illustratively, the rotational speed of the rotary stirring mechanism is 30rpm, 100rpm, 200rpm, 300rpm, or 500 rpm.
In another embodiment, the rotary stirring mechanism may be a propeller stirrer, a turbine stirrer, a paddle stirrer, an anchor stirrer, a ribbon stirrer, or the like.
In the hot top casting process, the stirring mechanism can also be a vibrating stirring mechanism, and the vibrating stirring mechanism is adopted to stir the molten aluminum alloy liquid at the hot top to obtain an aluminum alloy ingot. Wherein the vibration frequency of the vibration type stirring mechanism is more than 50 times/minute. Illustratively, the vibration frequency of the vibratory agitation mechanism is 50 times/minute, 100 times/minute, 200 times/minute, 300 times/minute, 400 times/minute, or 500 times/minute.
In another embodiment, in the hot top casting process, the stirring mechanism is an ultrasonic stirrer, and the molten aluminum alloy liquid on the hot top is stirred by the ultrasonic stirrer to obtain an aluminum alloy ingot. Wherein the ultrasonic frequency of the ultrasonic stirrer is more than 100 kHz. Illustratively, the ultrasonic frequency of the ultrasonic agitator is 100kHz, 200kHz, 300kHz, 400kHz, or 500 kHz.
It should be noted that: the stirring of the molten alloy 140 does not necessarily mean that the stirring mechanism 120 is inserted into the molten alloy 140, and if the stirring is performed by an ultrasonic stirrer, it may not be inserted into the molten alloy 140.
In the hot top casting process, the temperature of the hot top is controlled to be related to the temperature of the molten alloy liquid, the temperature of the hot top is within +/-3% of the temperature of the molten alloy liquid, namely the temperature value of the hot top is within the range of x (0.97-1.03) of the temperature of the molten alloy liquid. For example: the temperature of the molten alloy is 720 ℃, the temperature of the hot top is 720 x 0.97-720 x 1.03 ℃, namely the temperature of the hot top is 698-742 ℃. Optionally, the temperature of the hot top is between 700 and 740 ℃. Can prevent the solidification segregation of the alloy liquid in the solidification process so as to obtain an alloy ingot with a uniform structure.
The application also provides an aluminum alloy target material, and the aluminum alloy target material is prepared by the preparation method of the aluminum alloy ingot for the target material.
The features and properties of the present application are described in further detail below with reference to examples.
Example 1
The embodiment provides an aluminum-copper alloy ingot for a target, and the preparation method of the ingot comprises the following steps:
taking high-purity aluminum and high-purity copper according to the mass ratio of 99.5:0.5, putting the high-purity aluminum and the high-purity copper into a smelting furnace for smelting to obtain molten aluminum-copper alloy liquid, and flowing the molten alloy liquid into a crucible of a casting furnace for casting. At this time, the temperature of the molten alloy in the crucible was 720 ℃ and the temperature of the hot top was controlled to 700-. Stirring paddles are inserted into the casting furnace to stir the molten aluminum-copper alloy liquid at the hot top, the rotating speed of the stirring paddles is 60rpm, and the molten aluminum-copper alloy liquid is cast at the casting speed of 120mm/min
The ingot of (1). And (4) analyzing the components of the obtained aluminum-copper alloy cast ingot by using an X-ray fluorescence device. The cross sections of the ingot at the initial stage, the middle stage and the end stage of the ingot are respectively taken for detection, 1 point (detection point 1) is taken at the center of each cross section, 5 points (detection points 2-6 in sequence) are further taken from the center to the periphery for detection, and the detection results are shown in table 1.
TABLE 1 Cu content values in Al-Cu alloy ingots
| Cu content wt% | Detection point 1 | Detection point 2 | Detection point 3 | Detection point 4 | Detection point 5 | Detection point 6 |
| Initial stage | 0.52 | 0.52 | 0.49 | 0.52 | 0.48 | 0.50 |
| Middle stage | 0.51 | 0.49 | 0.51 | 0.49 | 0.52 | 0.49 |
| End period | 0.49 | 0.50 | 0.52 | 0.51 | 0.48 | 0.49 |
As can be seen from table 1, in the aluminum-copper alloy ingot provided in this embodiment, the content of Cu is 0.48 to 0.52 wt%, and it can be calculated that the deviation of the content of Cu in the aluminum-copper alloy ingot is within ± 4%.
Example 2
The embodiment provides an aluminum-silicon alloy ingot for a target material, and the preparation method of the ingot comprises the following steps:
high-purity aluminum and high-purity silicon are taken according to the mass ratio of 99: 1. And putting the high-purity aluminum and the high-purity silicon into a smelting furnace for smelting to obtain molten aluminum-silicon alloy liquid. The molten alloy is poured into a crucible of a casting furnace and cast. Stirring the molten Al-Si alloy liquid at the hot top by inserting an ultrasonic vibrator into a casting furnace, wherein the frequency of the ultrasonic vibrator is 150kHz, and casting is carried out at a casting speed of 120mm/min
The ingot of (1). And analyzing the components of the obtained aluminum-silicon alloy cast ingot by adopting an X-ray fluorescence device. The results of the above sampling and testing are shown in Table 2.
TABLE 2 Si content values in Al-Si alloy ingots
| Si content wt% | Detection point 1 | Detection point 2 | Detection point 3 | Detection point 4 | Detection point 5 | Detection point 6 |
| Initial stage | 1.09 | 0.94 | 1.03 | 1.07 | 0.92 | 1.02 |
| Middle stage | 0.91 | 1.06 | 0.97 | 0.97 | 1.02 | 1.08 |
| End period | 1.03 | 1.00 | 0.92 | 1.08 | 1.04 | 0.95 |
As can be seen from table 2, in the aluminum-silicon alloy ingot provided in this example, the Si content is 0.91 to 1.09 wt%, and it can be calculated that the deviations of the Si content in the aluminum-silicon alloy ingot are within ± 9%.
As can be seen from the comparison between example 1 and example 2, in the process of preparing the aluminum alloy ingot, the molten alloy liquid at the hot top is stirred, and the temperature at the hot top is controlled, so that the distribution of the added elements can be more uniform.
Comparative example 1
Comparative example 1 is different from example 1 in that the molten aluminum-copper alloy liquid on the hot top is not stirred by the stirring paddle and the temperature of the hot top is not controlled. The results of the above sampling test are shown in Table 3.
TABLE 3 Cu content values in Al-Cu alloy ingots
| Cu content wt% | Detection point 1 | Detection point 2 | Detection point 3 | Detection point 4 | Detection point 5 | Detection point 6 |
| Initial stage | 0.58 | 0.51 | 0.47 | 0.53 | 0.39 | 0.59 |
| Middle stage | 0.41 | 0.59 | 0.52 | 0.42 | 0.49 | 0.47 |
| End period | 0.52 | 0.54 | 0.62 | 0.45 | 0.56 | 0.61 |
As can be seen from Table 3, the Cu content of the Al-Cu alloy ingot provided by the comparative example is 0.39-0.62 wt%, and the Cu content of the Al-Cu alloy ingot can be calculated to be within + -24%. As can be seen from the comparison between tables 1 and 3, the distribution of Cu in the aluminum-copper alloy ingot provided in example 1 is more uniform, which indicates that the distribution of Cu in the obtained aluminum-copper alloy ingot can be more uniform by stirring the molten aluminum-copper alloy liquid at the hot top with the stirring paddle and controlling the temperature at the hot top during the hot top casting process.
Comparative example 2
Comparative example 2 differs from example 2 in that the molten aluminum-silicon alloy liquid at the hot top is not stirred with an ultrasonic vibrator. The results of the above sampling and testing are shown in Table 4.
TABLE 4 Si content values in Al-Si alloy ingots
| Si content wt% | Detection point 1 | Detection point 2 | Detection point 3 | Detection point 4 | Detection point 5 | Detection point 6 |
| Initial stage | 0.73 | 0.85 | 1.21 | 0.87 | 1.08 | 1.23 |
| Middle stage | 0.78 | 1.25 | 1.02 | 1.05 | 1.14 | 0.95 |
| End period | 1.15 | 0.94 | 0.77 | 1.16 | 0.85 | 1.12 |
As can be seen from table 4, in the aluminum-silicon alloy ingot provided in this example, the Si content is 0.73 to 1.25 wt%, and it can be calculated that the deviations of the Si content in the aluminum-silicon alloy ingot are within ± 27%. As can be seen from the comparison between tables 2 and 4, the distribution of Si in the al-Si alloy ingot provided in example 2 is more uniform, which indicates that the distribution of Si in the obtained al-Si alloy ingot can be more uniform by stirring the molten al-Si alloy liquid at the hot top using the ultrasonic vibrator during the hot top casting.
Test example 1
The ingots provided in examples 1-2 and comparative examples 1-2 were prepared into targets by the following processes: and forging, rolling, heat treating and cutting the cast ingot to obtain the aluminum alloy target. The target was mounted on a DC sputtering apparatus, and continuous sputtering was performed at 10kWh with the sputtering pressure set to 0.4Pa and the substrate temperature set to room temperature using argon as a sputtering gas, and the number of times of abnormal discharge was counted as shown in table 5.
TABLE 5 number of abnormal discharges of target
| Example 1 | Example 2 | Comparative example 1 | Comparative example 2 | |
| Number of abnormal discharges (times/hr) | 1 | 2 | 7 | 12 |
As can be seen from table 5, after the ingot provided in the embodiment of the present application is made into a target, the problem of abnormal discharge generated during sputtering of the target can be effectively solved, and the occurrence of abnormal discharge during sputtering of the target can be reduced.
The embodiments described above are some, but not all embodiments of the present application. The detailed description of the embodiments of the present application is not intended to limit the scope of the claimed application, but is merely representative of selected embodiments of the application. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present application.
Claims (8)
1. A preparation method of an aluminum alloy ingot for a target material is characterized by comprising the following steps: in the hot top casting process, stirring the molten aluminum alloy liquid in the diversion trench by using a stirring mechanism, and not stirring the molten aluminum alloy liquid in the hot top to obtain an aluminum alloy ingot by casting;
the aluminum alloy ingot contains aluminum and an additive element;
wherein the added elements in the aluminum alloy ingot meet the following conditions:
the target content value of the additive element in the aluminum alloy ingot is a wt%, the content of the additive element in a plurality of samples is detected by sampling at multiple points on the cross section of the aluminum alloy ingot to obtain a plurality of additive element content values, and the plurality of additive element content values are all in the range of 0.9 a-1.1 a wt%.
2. The method according to claim 1, wherein the additive element content values are each in the range of 0.95 to 1.05a wt%.
3. The preparation method of claim 2, wherein the additive element is Cu, the target Cu content value is 0.5 wt%, and the Cu content values are obtained by sampling and detecting the Cu content in a plurality of samples at multiple points on the cross section of the aluminum-copper alloy ingot, and are all in the range of 0.45-0.55 wt%.
4. The preparation method according to claim 2, wherein the additive element is Si, the target Si content value is 1 wt%, and the Si content values are obtained by performing multi-point sampling on the cross section of the aluminum-silicon alloy ingot and detecting the Si content in a plurality of samples, and are all in the range of 0.9-1.1 wt%.
5. The method for preparing an aluminum alloy ingot for a target according to any one of claims 1 to 4, further comprising:
in the hot top casting process, a heating mechanism is added at the hot top so as to control the temperature of the hot top within +/-3% of the temperature of the molten aluminum alloy liquid.
6. The method for preparing an aluminum alloy ingot for a target according to any one of claims 1 to 4, wherein in the hot top casting process, the stirring mechanism is a rotary stirring mechanism;
the rotating speed of the rotary stirring mechanism is more than 30 rpm.
7. The method for preparing an aluminum alloy ingot for a target according to any one of claims 1 to 4, wherein in the hot top casting process, the stirring mechanism is a vibrating stirring mechanism;
the vibration frequency of the vibration type stirring mechanism is more than 50 times/minute.
8. The method for preparing an aluminum alloy ingot for a target according to any one of claims 1 to 4, wherein in the hot top casting process, the stirring mechanism is an ultrasonic stirrer;
the ultrasonic frequency of the ultrasonic stirrer is more than 100 kHz.
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| CN106925735A (en) * | 2015-12-30 | 2017-07-07 | 北京有色金属研究总院 | A kind of device and method for preparing big specification high-quality aluminium alloy cast ingot |
| CN109628897A (en) * | 2018-12-06 | 2019-04-16 | 新疆众和股份有限公司 | A kind of high-purity alusil alloy sputtering target material blank and preparation method thereof |
| CN110270670A (en) * | 2019-07-30 | 2019-09-24 | 中南大学 | The method that a kind of ultrasonic wave added heat top D.C.casting prepares big specification 2XXX line aluminium alloy billet |
| CN110592406A (en) * | 2019-10-10 | 2019-12-20 | 新疆众和股份有限公司 | Preparation method of high-purity aluminum-copper alloy target blank for sputtering |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106925735A (en) * | 2015-12-30 | 2017-07-07 | 北京有色金属研究总院 | A kind of device and method for preparing big specification high-quality aluminium alloy cast ingot |
| CN109628897A (en) * | 2018-12-06 | 2019-04-16 | 新疆众和股份有限公司 | A kind of high-purity alusil alloy sputtering target material blank and preparation method thereof |
| CN110270670A (en) * | 2019-07-30 | 2019-09-24 | 中南大学 | The method that a kind of ultrasonic wave added heat top D.C.casting prepares big specification 2XXX line aluminium alloy billet |
| CN110592406A (en) * | 2019-10-10 | 2019-12-20 | 新疆众和股份有限公司 | Preparation method of high-purity aluminum-copper alloy target blank for sputtering |
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