CN117144307A - Preparation method of aluminum-silicon-copper sputtering target material - Google Patents
Preparation method of aluminum-silicon-copper sputtering target material Download PDFInfo
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- CN117144307A CN117144307A CN202311138486.0A CN202311138486A CN117144307A CN 117144307 A CN117144307 A CN 117144307A CN 202311138486 A CN202311138486 A CN 202311138486A CN 117144307 A CN117144307 A CN 117144307A
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- -1 aluminum-silicon-copper Chemical compound 0.000 title claims abstract description 82
- 238000005477 sputtering target Methods 0.000 title claims abstract description 29
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 239000013077 target material Substances 0.000 title claims abstract description 16
- 239000002994 raw material Substances 0.000 claims abstract description 141
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 117
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 115
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 115
- 239000010703 silicon Substances 0.000 claims abstract description 114
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 112
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 95
- 239000000956 alloy Substances 0.000 claims abstract description 95
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 81
- 229910052802 copper Inorganic materials 0.000 claims abstract description 81
- 239000010949 copper Substances 0.000 claims abstract description 81
- 238000005266 casting Methods 0.000 claims abstract description 49
- 238000002844 melting Methods 0.000 claims abstract description 31
- 230000008018 melting Effects 0.000 claims abstract description 31
- 229910000881 Cu alloy Inorganic materials 0.000 claims abstract description 23
- 238000007670 refining Methods 0.000 claims abstract description 21
- 238000007872 degassing Methods 0.000 claims abstract description 20
- 238000001816 cooling Methods 0.000 claims abstract description 12
- 239000002893 slag Substances 0.000 claims abstract description 8
- 238000003756 stirring Methods 0.000 claims description 56
- 238000000034 method Methods 0.000 claims description 29
- 238000010438 heat treatment Methods 0.000 claims description 27
- 238000005096 rolling process Methods 0.000 claims description 26
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 24
- 238000002156 mixing Methods 0.000 claims description 19
- 239000000498 cooling water Substances 0.000 claims description 18
- 230000006698 induction Effects 0.000 claims description 16
- 238000011282 treatment Methods 0.000 claims description 15
- 238000003754 machining Methods 0.000 claims description 14
- 229910052786 argon Inorganic materials 0.000 claims description 12
- 238000004519 manufacturing process Methods 0.000 claims description 11
- 239000011888 foil Substances 0.000 claims description 9
- 239000007789 gas Substances 0.000 claims description 9
- 230000001681 protective effect Effects 0.000 claims description 5
- 238000007664 blowing Methods 0.000 claims description 4
- 238000004220 aggregation Methods 0.000 abstract description 9
- 230000002776 aggregation Effects 0.000 abstract description 9
- 238000005204 segregation Methods 0.000 abstract description 5
- 239000011248 coating agent Substances 0.000 description 34
- 238000000576 coating method Methods 0.000 description 34
- 238000003801 milling Methods 0.000 description 18
- 238000005553 drilling Methods 0.000 description 12
- 239000011265 semifinished product Substances 0.000 description 12
- 239000007788 liquid Substances 0.000 description 9
- 229910000838 Al alloy Inorganic materials 0.000 description 8
- 239000000047 product Substances 0.000 description 8
- 238000005520 cutting process Methods 0.000 description 7
- 238000005097 cold rolling Methods 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 6
- 239000006185 dispersion Substances 0.000 description 4
- 238000007711 solidification Methods 0.000 description 3
- 230000008023 solidification Effects 0.000 description 3
- 229920001169 thermoplastic Polymers 0.000 description 3
- 239000004416 thermosoftening plastic Substances 0.000 description 3
- 229910000676 Si alloy Inorganic materials 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 238000004544 sputter deposition Methods 0.000 description 2
- 238000004781 supercooling Methods 0.000 description 2
- 229910018594 Si-Cu Inorganic materials 0.000 description 1
- 229910008465 Si—Cu Inorganic materials 0.000 description 1
- 238000003723 Smelting Methods 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 238000005275 alloying Methods 0.000 description 1
- CSDREXVUYHZDNP-UHFFFAOYSA-N alumanylidynesilicon Chemical compound [Al].[Si] CSDREXVUYHZDNP-UHFFFAOYSA-N 0.000 description 1
- WPPDFTBPZNZZRP-UHFFFAOYSA-N aluminum copper Chemical compound [Al].[Cu] WPPDFTBPZNZZRP-UHFFFAOYSA-N 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000004512 die casting Methods 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 238000007667 floating Methods 0.000 description 1
- 238000002354 inductively-coupled plasma atomic emission spectroscopy Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000011863 silicon-based powder Substances 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23P—METAL-WORKING NOT OTHERWISE PROVIDED FOR; COMBINED OPERATIONS; UNIVERSAL MACHINE TOOLS
- B23P15/00—Making specific metal objects by operations not covered by a single other subclass or a group in this subclass
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/02—Making non-ferrous alloys by melting
- C22C1/026—Alloys based on aluminium
-
- 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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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Physical Vapour Deposition (AREA)
Abstract
The invention provides a preparation method of an aluminum-silicon-copper sputtering target material, which comprises the following steps: providing an aluminum raw material, a silicon raw material and a copper raw material, and dividing the aluminum raw material into two parts; (II) melting a part of aluminum raw materials to obtain an aluminum melt, adding silicon raw materials and copper raw materials into the aluminum melt, performing primary melting at a first temperature to obtain a primary alloy melt, adding the rest of aluminum raw materials into the aluminum silicon copper alloy melt, and performing secondary melting at a second temperature to obtain a secondary alloy melt; (III) sequentially carrying out degassing refining and slag skimming on the secondary alloy melt to obtain a purified alloy melt; (IV) casting and cooling the purified alloy melt in sequence to obtain an aluminum-silicon-copper cast ingot; the first temperature is greater than the second temperature. The invention solves the problem of Si element aggregation in the high-purity aluminum-silicon-copper alloy and can avoid the phenomenon of silicon segregation in the alloy ingot casting.
Description
Technical Field
The invention belongs to the technical field of high-purity aluminum preparation, and relates to a preparation method of an aluminum-silicon-copper sputtering target material.
Background
Aluminum is a metal material which is inferior to steel in world use amount, pure aluminum has better plasticity, electric conduction, thermal conductivity and corrosion resistance, but has low strength, and in order to improve the toughness and other comprehensive properties, alloy elements are added for alloying, so as to form deformed aluminum alloy and cast aluminum alloy which meet the corresponding required properties. The alloyed aluminum alloy has the characteristics of good casting performance, cutting processability, wear resistance, corrosion resistance, high specific strength and the like.
The aluminum-silicon-copper aluminum alloy ingot is die-casting aluminum alloy with good comprehensive performance, and is widely applied to the semiconductor manufacturing industry nowadays. At present, the high-purity aluminum sputtering target material has extremely high requirements on components, and has increasingly severe requirements on various performances of aluminum-silicon-copper aluminum alloy ingots and higher requirements on casting process control.
CN111719059a discloses a method for preparing fine-grain high-purity aluminum-silicon-copper alloy target blanks for sputtering, preparing aluminum-copper intermediate alloy and aluminum-silicon intermediate alloy, melting the intermediate alloy and high-purity aluminum with purity of 99.9995% in a vacuum melting furnace, and obtaining alloy liquid after complete melting; carrying out on-line refining on the alloy liquid by adopting high-purity argon; performing bipolar filtration on the alloy liquid subjected to online refining; casting the alloy liquid subjected to the two-stage filtration to obtain the fine-grain high-purity aluminum-silicon-copper alloy target blank for sputtering.
CN115488295a discloses a preparation method of high-purity aluminum silicon copper cast ingot for target material, which comprises the steps of melting aluminum raw material to obtain aluminum liquid; filling copper powder and silicon powder into an aluminum foil bag to obtain a powder bag, and adding the powder bag into aluminum liquid to obtain aluminum-silicon-copper alloy liquid; sequentially degassing and deslagging the aluminum-silicon-copper alloy liquid to obtain a purified alloy melt; and (3) casting and cooling the alloy melt purified in the steps in sequence to obtain the aluminum-silicon-copper cast ingot. The preparation method provided by the invention can fully promote the dispersion of aluminum, silicon and copper, promote the uniformity of components, shorten the smelting time and avoid the generation of hot cracks and feather-shaped grains.
However, in the process of producing the high-temperature aluminum-silicon-copper alloy with thermoplastic deformation, cracks are easily generated due to aggregation of silicon elements in the alloy, so that the performance of the product is reduced or the product is invalid.
Disclosure of Invention
Aiming at the defects existing in the prior art, the invention aims to provide the preparation method of the aluminum-silicon-copper sputtering target material, which solves the problem of Si element aggregation in high-purity aluminum-silicon-copper alloy and can avoid the phenomenon of Si aggregation in alloy cast ingots.
To achieve the purpose, the invention adopts the following technical scheme:
the invention provides a preparation method of an aluminum-silicon-copper sputtering target material, which comprises the following steps:
providing an aluminum raw material, a silicon raw material and a copper raw material, and dividing the aluminum raw material into two parts;
(II) melting a part of aluminum raw materials to obtain an aluminum melt, adding silicon raw materials and copper raw materials into the aluminum melt, performing primary melting at a first temperature to obtain a primary alloy melt, adding the rest of aluminum raw materials into the aluminum silicon copper alloy melt, and performing secondary melting at a second temperature to obtain a secondary alloy melt;
(III) sequentially carrying out degassing refining and slag skimming on the secondary alloy melt to obtain a purified alloy melt;
(IV) casting and cooling the purified alloy melt in sequence to obtain an aluminum-silicon-copper cast ingot;
the first temperature is greater than the second temperature.
According to the method provided by the invention, firstly, the aluminum raw material is melted, and then the silicon raw material and the copper raw material are added, so that the silicon is uniformly dispersed; meanwhile, after the aluminum raw material, the silicon raw material and the copper raw material are mixed, the aluminum, silicon and copper are firstly melted at a high temperature, and then the temperature is reduced to melt the aluminum, silicon and copper secondarily, so that the problem of refractory silicon element is solved, the uniformity of silicon in the aluminum, silicon and copper is improved, and the problem that an ingot is cracked after thermoplastic deformation due to Si element aggregation in the production of the high-purity aluminum, silicon and copper alloy can be avoided.
As a preferable technical scheme of the invention, in the step (I), the purities of the aluminum raw material, the silicon raw material and the copper raw material are all more than or equal to 99.999 percent.
Preferably, the mass ratio of the silicon raw material to the copper raw material is (1-3): 1, for example, 1:1, 1.2:1, 1.5:1, 2:1, 2.2:1, 2.5:1 or 3:1, but not limited to the recited values, and other non-recited values within the range of values are equally applicable.
In the step (ii), the silicon raw material and the copper raw material are coated with aluminum foil to obtain a silicon coated body and a copper coated body, and the silicon coated body and the copper coated body are added into the aluminum melt.
In the invention, the silicon raw material and the copper raw material are preferably massive raw materials, and the aluminum foil is used for respectively coating the silicon raw material and the copper raw material, so that the problem of floating up of the silicon raw material and the copper raw material due to lighter mass during feeding can be prevented.
In the step (II), a part of aluminum raw materials are sent into a vacuum induction furnace and heated to 750-830 ℃ for melting to obtain aluminum melt, then the silicon raw materials and copper raw materials are added into the vacuum induction furnace, the temperature is raised to a first temperature, and the primary melting is carried out to obtain the primary alloy melt.
The heating temperature of the aluminum raw material in the vacuum induction furnace may be 750 to 830 ℃, for example, 750 ℃, 760 ℃, 770 ℃, 780 ℃, 790 ℃, 800 ℃, 810 ℃, 820 ℃, or 830 ℃, but is not limited to the values listed, and other values not listed in the range are equally applicable.
The first temperature is preferably 900 to 1200 ℃, and may be 900 ℃, 920 ℃, 950 ℃, 1000 ℃, 1050 ℃, 1100 ℃, 1150 ℃, or 1200 ℃, for example, but is not limited to the values listed, and other values not listed in the range are equally applicable.
The silicon content of the primary alloy melt is preferably 8 to 13% by mass, and may be, for example, 8%, 8.5%, 9%, 9.5%, 9.8%, 10%, 10.5%, 10.8%, 11%, 11.5%, 12%, 12.5% or 13%, but is not limited to the values recited, and other values not recited in the numerical range are equally applicable.
In the invention, aluminum raw materials are placed into a vacuum induction furnace, silicon raw materials and copper raw materials are placed into a charging chamber in the vacuum induction furnace, after the aluminum raw materials are melted, the silicon raw materials and the copper raw materials in the charging chamber are sent into aluminum melt, and the temperature is increased to a first temperature for continuous heating, so that the silicon raw materials and the copper raw materials are melted and dispersed in the aluminum melt.
In the step (ii), the remaining aluminum raw material and the aluminum-silicon-copper alloy melt are placed in a crucible to perform the secondary melting, so as to obtain the secondary alloy melt.
The second temperature is preferably 740 to 760 ℃, and may be 740 ℃, 742 ℃, 745 ℃, 750 ℃, 753 ℃, 755 ℃, 758 ℃, or 760 ℃, for example, but is not limited to the recited values, and other non-recited values within the range are equally applicable.
The mass ratio of silicon in the secondary alloy melt is preferably 0.5 to 2%, and may be, for example, 0.5%, 0.6%, 0.8%, 1%, 1.2%, 1.3%, 1.5%, 1.6%, 1.8% or 2%, but is not limited to the recited values, and other non-recited values within the range are equally applicable.
In a preferred embodiment of the present invention, in the step (ii), the silicon raw material and the copper raw material are added to the aluminum melt, and then the aluminum melt is subjected to a primary stirring treatment.
The time of the one stirring treatment is preferably 10 to 15 minutes, and may be, for example, 10 minutes, 11 minutes, 12 minutes, 13 minutes, 14 minutes or 15 minutes, but is not limited to the listed values, and other non-listed values within the range are equally applicable.
Preferably, the secondary stirring treatment is performed after the residual aluminum raw material is added into the aluminum-silicon-copper alloy melt.
Preferably, the secondary stirring and mixing comprises at least four stages of stirring and mixing.
Preferably, the stirring and mixing time is 20 to 30min, for example, 20min, 21min, 22min, 23min, 24min, 25min, 26min, 27min, 28min, 29min or 30min, but the stirring and mixing time is not limited to the recited values, and other non-recited values within the range of the values are equally applicable.
As a preferred embodiment of the present invention, in the step (iii), the degassing refining includes: and (5) rotary blowing protective gas to the secondary alloy melt.
The rotational speed of the rotary blowing is preferably 400 to 500r/min, and may be, for example, 400r/min, 420r/min, 425r/min, 430r/min, 440r/min, 445r/min, 450r/min, 460r/min, 480r/min, 490r/min or 500r/min, but not limited to the values listed, and other values not listed in the range of values are equally applicable, and further preferably 420 to 450r/min.
Preferably, the shielding gas comprises argon.
Preferably, the flow rate of the shielding gas is 3-6 m 3 /h, for example, may be 3m 3 /h、3.5m 3 /h、4m 3 /h、4.5m 3 /h、5m 3 /h、5.5m 3 /h or 6m 3 And/h, but is not limited to the recited values, and other non-recited values within this range are equally applicable.
Preferably, the degassing refining time is 70 to 100min, for example, 70min, 75min, 78min, 80min, 85min, 88min, 90min, 95min, 98min or 100min, but not limited to the recited values, and other non-recited values within the range are equally applicable.
The temperature of the degassing refining is preferably 700 to 800 ℃, and may be 700 ℃, 715 ℃, 720 ℃, 730 ℃, 740 ℃, 745 ℃, 750 ℃, 755 ℃, 760 ℃, 770 ℃, 780 ℃, 790 ℃, or 800 ℃, for example, but the method is not limited to the above-mentioned values, and other values not mentioned in the above-mentioned value range are equally applicable.
In the step (iv), the purified alloy melt is stirred three times during the casting process.
Preferably, the three-time stirring treatment is an electromagnetic stirring treatment.
The invention carries out electromagnetic stirring on the purified alloy melt in the casting process, and can inhibit the segregation problem of silicon element in the solidification process of the purified alloy melt.
The casting temperature is preferably 700 to 720 ℃, and may be 700 ℃, 702 ℃, 705 ℃, 710 ℃, 713 ℃, 715 ℃, 718 ℃, or 720 ℃, for example, but is not limited to the recited values, and other non-recited values within the range are equally applicable.
Preferably, the casting speed is 70 to 120mm/min, for example, 70mm/min, 75mm/min, 80mm/min, 85mm/min, 90mm/min, 95mm/min, 100mm/min, 105mm/min, 110mm/min, 115mm/min or 120mm/min, but not limited to the recited values, and other non-recited values within the range of values are equally applicable.
As a preferred embodiment of the present invention, in the step (iv), the cooling mode includes: and (3) adopting cooling water to cool the purified alloy melt to obtain the aluminum-silicon-copper cast ingot.
Preferably, the flow rate of the cooling water is 200 to 500L/min, for example, 200L/min, 220L/min, 250L/min, 280L/min, 300L/min, 320L/min, 350L/min, 400L/min, 420L/min, 450L/min, 480L/min or 500L/min, but not limited to the recited values, and other non-recited values within the range of the values are equally applicable.
The temperature of the cooling water is preferably 10 to 20 ℃, and may be, for example, 10 ℃, 12 ℃, 14 ℃, 15 ℃, 16 ℃, 17 ℃, 18 ℃, 19 ℃, or 20 ℃, but is not limited to the values recited, and other values not recited in the range are equally applicable.
The invention adopts the casting device to cast the purified alloy melt, an electromagnetic stirring mechanism can be arranged on a distributor of the casting device, when the purified alloy melt is injected into the distributor, electromagnetic stirring is carried out to uniformly disperse aluminum, silicon and copper, and then large-flow cooling water is utilized to cool, so that the purified alloy melt is solidified, and a dummy bar is started to run downwards, thus obtaining the aluminum, silicon and copper cast ingot.
The invention adopts larger cooling water flow, smaller casting speed and lower water temperature during casting, can increase the supercooling degree of the cast ingot in the cooling process, so that the cast ingot is rapidly cooled, and the segregation of silicon elements in the aluminum-silicon-copper cast ingot is effectively reduced by combining the stirring effect.
As a preferable technical scheme of the invention, the preparation method further comprises the following steps: and rolling, heat treatment and machining are sequentially carried out on the aluminum-silicon-copper ingot to obtain the aluminum-silicon-copper sputtering target material.
It should be noted that, the rolling, heat treatment and machining are not limited in the present invention, and any method known to those skilled in the art for rolling, heat treatment and machining that can be used for target production may be used in the rolling, heat treatment and machining, so as to help those skilled in the art to better understand the overall technical scheme and working process of the present invention, the present invention provides the following specific production process by way of example:
(1) Placing an aluminum-silicon-copper cast ingot on a cold rolling mill platform, opening a roller until the thickness of the aluminum-silicon-copper cast ingot is reduced by 3mm, enabling the rolling direction of each rolling to be consistent, reducing the rolling direction by 3mm each time, and reserving 2-3 mm as machining allowance on the basis of the thickness of a finished product;
(2) Then placing the aluminum-silicon-copper cast ingot in a heating furnace, adjusting the temperature to 400 ℃, and preserving the heat to finish heat treatment to obtain a target semi-finished product;
(3) And fixing the target semi-finished product on a milling machine table sign, completing cutting operation according to the operation instruction of the milling machine, and sequentially performing target milling and drilling operation by adopting a lathe and a drilling machine.
The numerical ranges recited herein include not only the above-listed point values, but also any point values between the above-listed numerical ranges that are not listed, and are limited in space and for the sake of brevity, the present invention is not intended to be exhaustive of the specific point values that the stated ranges include.
Compared with the prior art, the invention has the beneficial effects that:
according to the preparation method of the aluminum-silicon-copper sputtering target material, firstly, an aluminum raw material is melted, and then a silicon raw material and a copper raw material are added, so that uniform silicon dispersion is facilitated; meanwhile, after the aluminum raw material, the silicon raw material and the copper raw material are mixed, the aluminum, silicon and copper are firstly melted at a high temperature, and then the temperature is reduced to melt the aluminum, silicon and copper secondarily, so that the problem that the silicon element is refractory is solved, and under the triple effects of stirring for many times, improving the supercooling degree in the solidification process and electromagnetic stirring, the Si element is uniformly distributed in the cast ingot, so that the problem that the cast ingot is cracked after thermoplastic deformation due to Si element aggregation in the production of the high-purity aluminum, silicon and copper alloy can be avoided.
Drawings
Fig. 1 is a schematic view of a casting apparatus according to an embodiment of the present invention.
Wherein, 1-the dispenser; 2-an electromagnetic stirring mechanism; 3-cooling water; 4-dummy bars; 5-purifying the alloy melt; 6-aluminum-silicon-copper ingot casting.
Detailed Description
It is to be understood that in the description of the present invention, the terms "first," "second," and the like are used for descriptive purposes only and are not to be construed as indicating or implying a relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defining "a first", "a second", etc. may explicitly or implicitly include one or more such feature. In the description of the present invention, unless otherwise indicated, the meaning of "a plurality" is two or more.
The technical scheme of the invention is further described below by the specific embodiments with reference to the accompanying drawings.
In a specific embodiment, the invention provides a preparation method of an aluminum silicon copper sputtering target material, which comprises the following steps:
(1) Providing an aluminum raw material, a silicon raw material and a copper raw material, wherein the purity of the aluminum raw material, the silicon raw material and the copper raw material is more than or equal to 99.999 percent, the mass ratio of the silicon raw material to the copper raw material is (1-3): 1, and dividing the aluminum raw material into two parts;
(2) Feeding a part of aluminum raw materials into a vacuum induction furnace, and heating to 750-830 ℃ to melt to obtain aluminum melt;
(3) Coating the silicon raw material and the copper raw material by utilizing aluminum foil to obtain a silicon coating body and a copper coating body, adding the silicon coating body and the copper coating body into the aluminum melt, melting for one time at 900-1200 ℃, stirring for 10-15 min to obtain a primary alloy melt, adding the rest aluminum raw material into the aluminum-silicon-copper alloy melt, placing into a crucible, melting for the second time at 740-760 ℃ and stirring for the second time to obtain a secondary alloy melt, wherein the mass ratio of silicon in the primary alloy melt is 8-13%, and the mass ratio of silicon in the secondary alloy melt is 0.5-2%;
(4) The secondary alloy melt is rotated and blown with protective gas to realize degassing refining, the protective gas comprises argon, and the flow rate of the protective gas is 3-6 m 3 And/h, the rotating speed is 400-500 r/min, the degassing and refining time is 70-100 min, the temperature is 700-800 ℃, and then slag skimming is carried out to obtain purified alloy melt 5;
(5) Casting the purified alloy melt 5, and carrying out three stirring treatments, wherein the casting temperature is 700-720 ℃, the speed is 70-120 mm/min, cooling water 3 is adopted to cool the purified alloy melt 5, the flow rate of the cooling water 3 is 200-500L/min, and the temperature is 10-20 ℃, so as to obtain an aluminum-silicon-copper cast ingot 6;
(6) And (3) rolling, heat treatment and machining the aluminum-silicon-copper ingot 6 in sequence to obtain the aluminum-silicon-copper sputtering target material.
The rolling, heat treatment and machining are not limited in the present invention, and any method known to those skilled in the art for rolling, heat treatment and machining can be used for target production, and in order to help those skilled in the art to better understand the overall technical scheme and working process of the present invention, the present invention provides the following specific production process:
s1, placing an aluminum-silicon-copper cast ingot 6 on a cold rolling mill platform, opening a roller until the thickness of the aluminum-silicon-copper cast ingot 6 is reached, then descending for 3mm, wherein the rolling direction of each rolling is consistent, each rolling is descending for 3mm, and 2-3 mm is reserved as machining allowance on the basis of the thickness of a finished product;
s2, placing the aluminum-silicon-copper cast ingot 6 in a heating furnace, adjusting the temperature to 400 ℃, and preserving heat to finish heat treatment to obtain a target semi-finished product;
s3, fixing the target semi-finished product on a milling machine table sign, completing cutting operation according to the operation instruction of the milling machine, and sequentially performing target milling and drilling operation by adopting a lathe and a drilling machine.
In some embodiments, the secondary stirring and mixing of the present invention comprises at least four stirring and mixing steps, wherein the stirring and mixing time is 20-30 min.
In some embodiments, the invention adopts a casting device to cast the purified alloy melt 5, as shown in fig. 1, an electromagnetic stirring mechanism 2 can be arranged on a distributor 1 of the casting device, when the purified alloy melt 5 is injected into the distributor 1, electromagnetic stirring is performed to uniformly disperse aluminum, silicon and copper, and then the purified alloy melt 5 is solidified by using high-flow cooling water 3 to start a dummy bar 4 to run downwards, so as to obtain an aluminum, silicon and copper cast ingot 6.
Example 1
The embodiment provides a preparation method of an aluminum-silicon-copper sputtering target, which specifically comprises the following steps:
(1) Providing an aluminum raw material, a silicon raw material and a copper raw material with the purity of 99.9995%, wherein the mass ratio of the silicon raw material to the copper raw material is 2:1, and dividing the aluminum raw material into two parts;
(2) Feeding a part of aluminum raw materials into a vacuum induction furnace, and heating to 800 ℃ to melt to obtain aluminum melt;
(3) Respectively coating a silicon raw material and a copper raw material by using an aluminum foil to obtain a silicon coating body and a copper coating body, placing the silicon coating body and the copper coating body in a charging chamber in a vacuum induction furnace, then adding the silicon coating body and the copper coating body into an aluminum melt, carrying out primary melting under the condition of 1200 ℃ and carrying out primary stirring treatment for 15min to obtain a primary alloy melt, adding the rest aluminum raw material into the aluminum-silicon-copper alloy melt, placing the aluminum melt into a crucible, carrying out secondary melting under the condition of 750 ℃, and carrying out four-section stirring and mixing, wherein the time of each stirring and mixing is 25min, and obtaining a secondary alloy melt, and the silicon content in the primary alloy melt is 10%, and the silicon content in the secondary alloy melt is 1%;
(4) Argon is blown into the secondary alloy melt in a rotating way to carry out degassing refining, the rotating speed is 450r/min, and the flow rate of the argon is 5m 3 And (h) degassing and refining for 90min at 760 ℃, and removing slag to obtain purified alloy melt 5;
(5) Placing the purified alloy melt 5 into a casting device for casting, when the purified alloy melt 5 is injected into a distributor 1 of the casting device, carrying out electromagnetic stirring by utilizing an electromagnetic stirring mechanism 2 on the distributor 1 to uniformly disperse aluminum, silicon and copper, wherein the casting temperature is 720 ℃, the casting speed is 80mm/min, and cooling by adopting cooling water 3 with the flow rate of 300L/min and the temperature of 10 ℃ to solidify the purified alloy melt 5, and starting a dummy bar 4 to run downwards to obtain an aluminum, silicon and copper cast ingot 6;
(6) Placing an aluminum-silicon-copper cast ingot 6 on a cold rolling mill platform, opening a roller until the thickness of the aluminum-silicon-copper cast ingot 6 is reached, then descending for 3mm, wherein the rolling direction of each rolling is consistent, each rolling is descending for 3mm, and 2mm is reserved as machining allowance on the basis of the thickness of a finished product;
(7) Then placing the aluminum-silicon-copper cast ingot 6 in a heating furnace, adjusting the temperature to 400 ℃, and preserving the heat to finish heat treatment to obtain a target semi-finished product;
(8) And fixing the target semi-finished product on a milling machine table sign, finishing cutting operation according to the operation instruction of the milling machine, and sequentially performing target milling and drilling operation by adopting a lathe and a drilling machine to obtain the aluminum-silicon-copper sputtering target.
Example 2
The embodiment provides a preparation method of an aluminum-silicon-copper sputtering target, which specifically comprises the following steps:
(1) Providing an aluminum raw material, a silicon raw material and a copper raw material with the purity of 99.9995%, wherein the mass ratio of the silicon raw material to the copper raw material is 2.5:1, and dividing the aluminum raw material into two parts;
(2) Feeding a part of aluminum raw materials into a vacuum induction furnace, and heating to 750 ℃ to melt to obtain aluminum melt;
(3) Respectively coating a silicon raw material and a copper raw material by using an aluminum foil to obtain a silicon coating body and a copper coating body, placing the silicon coating body and the copper coating body in a charging chamber in a vacuum induction furnace, then adding the silicon coating body and the copper coating body into an aluminum melt, carrying out primary melting under the condition of 950 ℃ and carrying out primary stirring treatment for 10min to obtain a primary alloy melt, adding the rest aluminum raw material into the aluminum-silicon-copper alloy melt, placing the aluminum melt into a crucible, carrying out secondary melting under the condition of 740 ℃ and carrying out four-section stirring and mixing, wherein the time of each stirring and mixing is 20min, and obtaining a secondary alloy melt, and the silicon content in the primary alloy melt is 8%, and the silicon content in the secondary alloy melt is 0.5%;
(4) Argon is blown into the secondary alloy melt in a rotating way to carry out degassing refining, the rotating speed is 400r/min, and the flow rate of the argon is 3m 3 And (h) degassing and refining for 70min at 800 ℃, and removing slag to obtain purified alloy melt 5;
(5) Placing the purified alloy melt 5 into a casting device for casting, when the purified alloy melt 5 is injected into a distributor 1 of the casting device, carrying out electromagnetic stirring by utilizing an electromagnetic stirring mechanism 2 on the distributor 1 to uniformly disperse aluminum, silicon and copper, wherein the casting temperature is 700 ℃, the casting speed is 70mm/min, cooling by adopting cooling water 3 with the flow of 200L/min and the temperature of 15 ℃ to solidify the purified alloy melt 5, and starting a dummy bar 4 to run downwards to obtain an aluminum, silicon and copper cast ingot 6;
(6) Placing an aluminum-silicon-copper cast ingot 6 on a cold rolling mill platform, opening a roller until the thickness of the aluminum-silicon-copper cast ingot 6 is reached, then descending for 3mm, wherein the rolling direction of each rolling is consistent, each rolling is descending for 3mm, and 2mm is reserved as machining allowance on the basis of the thickness of a finished product;
(7) Then placing the aluminum-silicon-copper cast ingot 6 in a heating furnace, adjusting the temperature to 400 ℃, and preserving the heat to finish heat treatment to obtain a target semi-finished product;
(8) And fixing the target semi-finished product on a milling machine table sign, finishing cutting operation according to the operation instruction of the milling machine, and sequentially performing target milling and drilling operation by adopting a lathe and a drilling machine to obtain the aluminum-silicon-copper sputtering target.
Example 3
The embodiment provides a preparation method of an aluminum-silicon-copper sputtering target, which specifically comprises the following steps:
(1) Providing an aluminum raw material, a silicon raw material and a copper raw material with the purity of 99.9995%, wherein the mass ratio of the silicon raw material to the copper raw material is 1.5:1, and dividing the aluminum raw material into two parts;
(2) Feeding a part of aluminum raw materials into a vacuum induction furnace, and heating to 830 ℃ to melt to obtain aluminum melt;
(3) Respectively coating a silicon raw material and a copper raw material by using an aluminum foil to obtain a silicon coating body and a copper coating body, placing the silicon coating body and the copper coating body in a charging chamber in a vacuum induction furnace, then adding the silicon coating body and the copper coating body into an aluminum melt, carrying out primary melting at 1000 ℃ and carrying out primary stirring treatment for 12min to obtain a primary alloy melt, adding the rest aluminum raw material into the aluminum-silicon-copper alloy melt, placing the aluminum-silicon-copper alloy melt into a crucible, carrying out secondary melting at 740 ℃ and carrying out four-section stirring and mixing, wherein the time of each stirring and mixing is 20min, and obtaining a secondary alloy melt, and the silicon content in the primary alloy melt is 13%, and the silicon content in the secondary alloy melt is 2%;
(4) Argon is blown into the secondary alloy melt in a rotating way to carry out degassing refining, the rotating speed is 500r/min, and the flow rate of the argon is 6m 3 And (h) degassing and refining for 100min at 700 ℃, and removing slag to obtain purified alloy melt 5;
(5) Placing the purified alloy melt 5 into a casting device for casting, when the purified alloy melt 5 is injected into a distributor 1 of the casting device, carrying out electromagnetic stirring by utilizing an electromagnetic stirring mechanism 2 on the distributor 1 to uniformly disperse aluminum, silicon and copper, wherein the casting temperature is 720 ℃, the speed is 120mm/min, cooling by adopting cooling water 3 with the flow rate of 500L/min and the temperature of 20 ℃ to solidify the purified alloy melt 5, and starting a dummy bar 4 to run downwards to obtain an aluminum, silicon and copper cast ingot 6;
(6) Placing an aluminum-silicon-copper cast ingot 6 on a cold rolling mill platform, opening a roller until the thickness of the aluminum-silicon-copper cast ingot 6 is reached, then descending for 3mm, wherein the rolling direction of each rolling is consistent, each rolling is descending for 3mm, and 2mm is reserved as machining allowance on the basis of the thickness of a finished product;
(7) Then placing the aluminum-silicon-copper cast ingot 6 in a heating furnace, adjusting the temperature to 400 ℃, and preserving the heat to finish heat treatment to obtain a target semi-finished product;
(8) And fixing the target semi-finished product on a milling machine table sign, finishing cutting operation according to the operation instruction of the milling machine, and sequentially performing target milling and drilling operation by adopting a lathe and a drilling machine to obtain the aluminum-silicon-copper sputtering target.
Example 4
The embodiment provides a method for preparing an aluminum-silicon-copper sputtering target, which is different from embodiment 1 in that: in the step (5), the casting speed was 60mm/min, and the other operation steps and process parameters were the same as in example 1.
Example 5
The embodiment provides a method for preparing an aluminum-silicon-copper sputtering target, which is different from embodiment 1 in that: in the step (5), the casting speed was 130mm/min, and the other operation steps and process parameters were the same as in example 1.
Example 6
The embodiment provides a method for preparing an aluminum-silicon-copper sputtering target, which is different from embodiment 1 in that: in the step (5), the flow rate of the cooling water 3 was 160L/min, and the other operation steps and process parameters were the same as those of example 1.
Example 7
The embodiment provides a method for preparing an aluminum-silicon-copper sputtering target, which is different from embodiment 1 in that: in the step (5), electromagnetic stirring was not performed, and the other operation steps and process parameters were the same as in example 1.
Example 8
The embodiment provides a method for preparing an aluminum-silicon-copper sputtering target, which is different from embodiment 1 in that: in the step (3), the rest of the aluminum raw material is added into the aluminum-silicon-copper alloy melt, and is placed into a crucible, and is subjected to secondary melting at 750 ℃ and a period of stirring and mixing, wherein the stirring and mixing time is 25min, and the rest of the operation steps and the process parameters are the same as those of the embodiment 1.
Comparative example 1
The comparative example provides a preparation method of an aluminum-silicon-copper sputtering target material, which comprises the following steps:
(1) Providing an aluminum raw material, a silicon raw material and a copper raw material with the purity of 99.9995%, wherein the mass ratio of the silicon raw material to the copper raw material is 2:1;
(2) Feeding an aluminum raw material into a vacuum induction furnace, heating to 800 ℃ to melt to obtain an aluminum melt, respectively coating a silicon raw material and a copper raw material by utilizing an aluminum foil to obtain a silicon coating body and a copper coating body, placing the silicon coating body and the copper coating body into a charging chamber in the vacuum induction furnace, then adding the silicon coating body and the copper coating body into the aluminum melt, melting the aluminum melt at 800 ℃, and stirring the aluminum melt for 15min to obtain a primary alloy melt, wherein the silicon content in the primary alloy melt is 1%;
(4) Argon is blown into the primary alloy melt in a rotating way, degassing refining is carried out, the rotating speed is 450r/min, and the flow rate of the argon is 5m 3 And (h) degassing and refining for 90min at 760 ℃, and removing slag to obtain purified alloy melt 5;
(5) Placing the purified alloy melt 5 into a casting device for casting, when the purified alloy melt 5 is injected into a distributor 1 of the casting device, carrying out electromagnetic stirring by utilizing an electromagnetic stirring mechanism 2 on the distributor 1 to uniformly disperse aluminum, silicon and copper, wherein the casting temperature is 720 ℃, the casting speed is 80mm/min, and cooling by adopting cooling water 3 with the flow rate of 300L/min and the temperature of 10 ℃ to solidify the purified alloy melt 5, and starting a dummy bar 4 to run downwards to obtain an aluminum, silicon and copper cast ingot 6;
(6) Placing an aluminum-silicon-copper cast ingot 6 on a cold rolling mill platform, opening a roller until the thickness of the aluminum-silicon-copper cast ingot 6 is reached, then descending for 3mm, wherein the rolling direction of each rolling is consistent, each rolling is descending for 3mm, and 2mm is reserved as machining allowance on the basis of the thickness of a finished product;
(7) Then placing the aluminum-silicon-copper cast ingot 6 in a heating furnace, adjusting the temperature to 400 ℃, and preserving the heat to finish heat treatment to obtain a target semi-finished product;
(8) And fixing the target semi-finished product on a milling machine table sign, finishing cutting operation according to the operation instruction of the milling machine, and sequentially performing target milling and drilling operation by adopting a lathe and a drilling machine to obtain the aluminum-silicon-copper sputtering target.
The invention detects the Si element distribution condition of the aluminum-silicon-copper cast ingots obtained in examples 1 to 8 and comparative example 1, and specifically comprises the following steps:
samples were taken at the center of the ingot, 1/2 of the diameter from the center, and at the edge of the ingot, and the samples were each subjected to silicon composition analysis by ICP-OES detection technique, with the results shown in table 1.
The al-si-cu sputtering targets obtained in examples 1 to 8 and comparative example 1 were observed for cracks after completion of processing, and the results are shown in table 1.
TABLE 1
As is clear from Table 1, the centers of the Al-Si-Cu sputtering targets obtained in examples 1 to 3 are well separated from the centers by 1/2 of the diameter and the silicon element content at the edges of the targets, and the Si aggregation phenomenon does not occur due to uniform dispersion of the Si in the materials.
Example 4 the cold shut phenomenon occurred due to the casting speed being too low, and the ingot was scrapped. The casting speed in example 5 was too high, and Si aggregation appeared in the ingot, resulting in cracking in the processing. As can be seen from table 1, the cooling of the ingot was slower due to the lower amount of the cast cooling water 3 of example 6, compared to example 1, resulting in uneven Si dispersion.
Compared with the embodiment 1, the silicon element content difference of different positions of the aluminum-silicon-copper sputtering target material in the embodiment 7 is increased, and cracks appear after the processing is finished, mainly because the electromagnetic stirring process is added in the casting process in the embodiment 1, so that the aluminum-silicon-copper in the alloy liquid distribution process is uniformly dispersed, and the segregation of the silicon element in the solidification process is effectively avoided.
As can be seen from comparison between example 1 and example 8, the difference in silicon content at different positions in example 8 is larger than that in example 1, mainly because in example 8, after the rest of the aluminum raw material is mixed with the aluminum-silicon-copper alloy melt, only a section of stirring and mixing are performed, so that the aluminum-silicon-copper in the alloy melt is unevenly mixed, and segregation of silicon element occurs.
As can be seen from Table 1, the deviation of the silicon element content in the center, 1/2 of the diameter from the center, and the edge of the ingot in comparative example 1 is significantly higher than that in example 1, mainly due to the lower melting temperature in comparative example 1, the difficulty in melting the silicon raw material, which results in aggregation, whereas in example 1, part of the aluminum raw material is melted during the melting of the aluminum raw material, the silicon raw material and the copper raw material, and after the addition of the silicon raw material and the copper raw material, the melting temperature is increased, so that the silicon can be sufficiently melted and dispersed in the aluminum melt, which is advantageous for improving the uniformity of the silicon element.
The applicant declares that the above is only a specific embodiment of the present invention, but the scope of the present invention is not limited thereto, and it should be apparent to those skilled in the art that any changes or substitutions that are easily conceivable within the technical scope of the present invention disclosed by the present invention fall within the scope of the present invention and the disclosure.
Claims (10)
1. The preparation method of the aluminum-silicon-copper sputtering target material is characterized by comprising the following steps of:
providing an aluminum raw material, a silicon raw material and a copper raw material, and dividing the aluminum raw material into two parts;
(II) melting a part of aluminum raw materials to obtain an aluminum melt, adding silicon raw materials and copper raw materials into the aluminum melt, performing primary melting at a first temperature to obtain a primary alloy melt, adding the rest of aluminum raw materials into the aluminum silicon copper alloy melt, and performing secondary melting at a second temperature to obtain a secondary alloy melt;
(III) sequentially carrying out degassing refining and slag skimming on the secondary alloy melt to obtain a purified alloy melt;
(IV) casting and cooling the purified alloy melt in sequence to obtain an aluminum-silicon-copper cast ingot;
the first temperature is greater than the second temperature.
2. The production method according to claim 1, wherein in the step (i), purities of the aluminum raw material, the silicon raw material and the copper raw material are all 99.999% or more;
preferably, the mass ratio of the silicon raw material to the copper raw material is (1-3): 1.
3. the production method according to claim 1 or 2, wherein in step (ii), the silicon raw material and the copper raw material are coated with aluminum foil, respectively, to obtain a silicon coated body and a copper coated body, and the silicon coated body and the copper coated body are added to the aluminum melt.
4. A method according to any one of claims 1 to 3, wherein in step (ii), the part of the aluminum raw material is fed into a vacuum induction furnace, heated to 750 to 830 ℃ and melted to obtain the aluminum melt, and then the silicon raw material and the copper raw material are added into the vacuum induction furnace, heated to a first temperature and melted once to obtain the primary alloy melt;
preferably, the first temperature is 900-1200 ℃;
preferably, the mass ratio of silicon in the primary alloy melt is 8-13%.
5. The method according to any one of claims 1 to 4, wherein in step (ii), the remaining aluminum raw material and aluminum-silicon-copper alloy melt are placed in a crucible to perform the secondary melting, so as to obtain the secondary alloy melt;
preferably, the second temperature is 740-760 ℃;
preferably, the mass ratio of silicon in the secondary alloy melt is 0.5-2%.
6. The production method according to any one of claims 1 to 5, wherein in the step (ii), after the silicon raw material and the copper raw material are added to the aluminum melt, a stirring treatment is performed once;
preferably, the time of the one-time stirring treatment is 10-15 min;
preferably, after the residual aluminum raw material is added into the aluminum-silicon-copper alloy melt, secondary stirring treatment is carried out;
preferably, the secondary stirring and mixing comprises at least four stages of stirring and mixing;
preferably, the stirring and mixing time is 20-30 min.
7. The process of any one of claims 1 to 6, wherein in step (iii), the degassing refining comprises: rotary blowing protective gas to the secondary alloy melt;
preferably, the rotating speed of the rotary blowing is 400-500 r/min, and more preferably 420-450 r/min;
preferably, the shielding gas comprises argon;
preferably, the flow rate of the shielding gas is 3-6 m 3 /h；
Preferably, the degassing refining time is 70-100 min;
preferably, the temperature of the degassing refining is 700-800 ℃.
8. The production method according to any one of claims 1 to 7, wherein in the step (iv), the purified alloy melt is subjected to three stirring treatments during the casting;
preferably, the three-time stirring treatment is an electromagnetic stirring treatment;
preferably, the casting temperature is 700-720 ℃;
preferably, the casting speed is 70-120 mm/min.
9. The method of any one of claims 1-8, wherein in step (iv), the cooling means comprises: adopting cooling water to cool the purified alloy melt to obtain the aluminum-silicon-copper cast ingot;
preferably, the flow rate of the cooling water is 200-500L/min;
preferably, the temperature of the cooling water is 10 to 20 ℃.
10. The method of any one of claims 1-9, further comprising: and rolling, heat treatment and machining are sequentially carried out on the aluminum-silicon-copper ingot to obtain the aluminum-silicon-copper sputtering target material.
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