CN117265489A - Titanium-aluminum alloy target and preparation method thereof - Google Patents
Titanium-aluminum alloy target and preparation method thereof Download PDFInfo
- Publication number
- CN117265489A CN117265489A CN202311430895.8A CN202311430895A CN117265489A CN 117265489 A CN117265489 A CN 117265489A CN 202311430895 A CN202311430895 A CN 202311430895A CN 117265489 A CN117265489 A CN 117265489A
- Authority
- CN
- China
- Prior art keywords
- smelting
- titanium
- aluminum alloy
- preparation
- alloy target
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- UQZIWOQVLUASCR-UHFFFAOYSA-N alumane;titanium Chemical compound [AlH3].[Ti] UQZIWOQVLUASCR-UHFFFAOYSA-N 0.000 title claims abstract description 57
- 229910000838 Al alloy Inorganic materials 0.000 title claims abstract description 56
- 238000002360 preparation method Methods 0.000 title claims abstract description 35
- 238000003723 Smelting Methods 0.000 claims abstract description 130
- 238000000034 method Methods 0.000 claims abstract description 45
- 238000005096 rolling process Methods 0.000 claims abstract description 31
- 238000000137 annealing Methods 0.000 claims abstract description 30
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 28
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 28
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 20
- 238000003754 machining Methods 0.000 claims abstract description 13
- 238000012545 processing Methods 0.000 claims abstract description 12
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 10
- 239000000956 alloy Substances 0.000 claims abstract description 10
- 238000002156 mixing Methods 0.000 claims abstract description 10
- 238000013461 design Methods 0.000 claims abstract description 8
- 230000008569 process Effects 0.000 claims description 16
- 239000000463 material Substances 0.000 claims description 15
- 238000001816 cooling Methods 0.000 claims description 14
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 12
- 238000001291 vacuum drying Methods 0.000 claims description 11
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 10
- 230000001681 protective effect Effects 0.000 claims description 9
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 7
- 239000011261 inert gas Substances 0.000 claims description 7
- 229910052786 argon Inorganic materials 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 6
- 239000001307 helium Substances 0.000 claims description 5
- 229910052734 helium Inorganic materials 0.000 claims description 5
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 5
- 229910052757 nitrogen Inorganic materials 0.000 claims description 5
- 239000002245 particle Substances 0.000 claims description 5
- 238000004140 cleaning Methods 0.000 claims description 2
- 239000007788 liquid Substances 0.000 claims description 2
- 230000007547 defect Effects 0.000 abstract description 11
- 239000013077 target material Substances 0.000 abstract description 10
- 238000004519 manufacturing process Methods 0.000 abstract description 9
- 238000005266 casting Methods 0.000 abstract description 6
- 238000002844 melting Methods 0.000 abstract description 5
- 230000008018 melting Effects 0.000 abstract description 5
- 238000010894 electron beam technology Methods 0.000 abstract description 4
- 238000000576 coating method Methods 0.000 description 10
- 239000012535 impurity Substances 0.000 description 10
- 239000011248 coating agent Substances 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 7
- 210000003625 skull Anatomy 0.000 description 6
- 238000001514 detection method Methods 0.000 description 5
- 239000002994 raw material Substances 0.000 description 5
- 239000007789 gas Substances 0.000 description 4
- 238000005240 physical vapour deposition Methods 0.000 description 4
- 230000009467 reduction Effects 0.000 description 4
- 210000001519 tissue Anatomy 0.000 description 4
- 238000003825 pressing Methods 0.000 description 3
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000005520 cutting process Methods 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000004663 powder metallurgy Methods 0.000 description 2
- 239000011206 ternary composite Substances 0.000 description 2
- 238000003466 welding Methods 0.000 description 2
- 229910000905 alloy phase Inorganic materials 0.000 description 1
- 238000005275 alloying Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000000110 cooling liquid Substances 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 230000001419 dependent effect Effects 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 229910003460 diamond Inorganic materials 0.000 description 1
- 239000010432 diamond Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 230000006698 induction Effects 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000001953 recrystallisation Methods 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 238000005204 segregation Methods 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- -1 transition metal carbides Chemical class 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
- B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
- B21B—ROLLING OF METAL
- B21B3/00—Rolling materials of special alloys so far as the composition of the alloy requires or permits special rolling methods or sequences ; Rolling of aluminium, copper, zinc or other non-ferrous metals
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
- B21B—ROLLING OF METAL
- B21B37/00—Control devices or methods specially adapted for metal-rolling mills or the work produced thereby
- B21B37/74—Temperature control, e.g. by cooling or heating the rolls or the product
-
- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- C21D9/00—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor
- C21D9/0068—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor for particular articles not mentioned below
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B9/00—General processes of refining or remelting of metals; Apparatus for electroslag or arc remelting of metals
- C22B9/16—Remelting metals
- C22B9/22—Remelting metals with heating by wave energy or particle radiation
- C22B9/228—Remelting metals with heating by wave energy or particle radiation by particle radiation, e.g. electron beams
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C14/00—Alloys based on titanium
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/02—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working in inert or controlled atmosphere or vacuum
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/16—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of other metals or alloys based thereon
- C22F1/18—High-melting or refractory metals or alloys based thereon
- C22F1/183—High-melting or refractory metals or alloys based thereon of titanium or alloys based thereon
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Crystallography & Structural Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- Toxicology (AREA)
- Plasma & Fusion (AREA)
- Manufacturing & Machinery (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
The invention provides a titanium-aluminum alloy target and a preparation method thereof, wherein the preparation method comprises the following steps: mixing the titanium sponge and the aluminum block according to the design requirement of alloy components, and sequentially carrying out isothermal rolling, annealing and machining after smelting to obtain the titanium-aluminum alloy target; the smelting comprises primary smelting, secondary smelting and tertiary smelting which are sequentially carried out. The invention obtains cast ingots with uniform components and tissues and no defects inside by adopting electron beam melting method for multiple times; and processing the casting blank into a target blank with fine and uniform grains by using an isothermal rolling method. The method provided by the invention can effectively control the performance of the titanium-aluminum alloy target material, and is suitable for mass production.
Description
Technical Field
The invention belongs to the field of metallurgical preparation, and relates to a target, in particular to a titanium-aluminum alloy target and a preparation method thereof.
Background
With the development of the modern machining industry towards high precision, high-speed cutting, hard machining instead of grinding, dry machining (without cooling liquid) protection to the environment, cost reduction and the like, quite high requirements are put on the performance of the cutter. Therefore, development of various cutting materials excellent in wear resistance and capable of stable processing for a long period of time is a necessary trend.
Hard coatings represented by transition metal carbides, nitrides, borides, diamond films and the like have been widely used in the fields of machining tools, dies, machine parts and the like due to their characteristics of superhard properties, wear resistance and the like. Physical vapor deposition (Physical Vapor Deposition, PVD) is the dominant technology for depositing hard coatings, and a titanium aluminum nitride (TiA 1N) coating prepared by adopting the PVD method is a novel ternary composite coating developed on the basis of a binary coating, the hardness of the ternary composite coating is obviously higher than that of a TiN coating, and meanwhile, the high-temperature oxidation resistance, the film-based bonding strength, the corrosion resistance and the wear resistance of the coating are all improved. Thus, tiA1N is considered to be a more promising new coating material than TiN, and has received much attention in recent years.
The film material of the TiA1N coating is titanium-aluminum alloy. At present, two methods for manufacturing titanium-aluminum alloy targets exist, namely a powder metallurgy method and a smelting method. The powder metallurgy method is difficult to solve the problem of high content of gas impurities, and has high requirements on powder and great preparation difficulty. The smelting method has the problems of vacuum induction smelting, vacuum consumable smelting, skull smelting and the like. In either method, the problems of melting defects, component segregation, impurities and the like, and the problem of forming from ingot to target material need to be solved.
CN 104278167a discloses a method for manufacturing a high-quality titanium-aluminum alloy target, which comprises the following steps: firstly, smelting in a vacuum consumable arc furnace, and then smelting in a vacuum consumable skull furnace to prepare the titanium-aluminum alloy, wherein the method sequentially comprises a batching step, a material drying step, an electrode pressing step, an electrode welding step, a vacuum consumable arc furnace smelting step and a vacuum consumable skull furnace smelting step, and the steps comprise the following steps of: in the material drying step, the prepared raw materials of titanium sponge and metal aluminum are subjected to baking treatment to obtain baked raw materials; in the electrode pressing step, pressing the baked raw materials to obtain an electrode; in the electrode welding step, the electrode is welded to obtain a welded electrode; in the vacuum consumable arc furnace smelting step, carrying out vacuum consumable arc furnace smelting treatment on the welded electrode to obtain an ingot blank smelted by the vacuum consumable arc furnace; and in the step of smelting in the vacuum consumable skull furnace, carrying out smelting treatment on the electrode smelted in the vacuum consumable arc furnace in the vacuum consumable skull furnace to obtain an ingot cast after smelting in the vacuum consumable skull furnace. The manufacturing method provided by this patent is difficult to eliminate volatile impurities and oxide impurities at the time of smelting. In addition, the target material is obtained by directly machining an ingot, the performance of the target material is completely dependent on the quality of the ingot, and the control is not easy.
In summary, the existing target preparation method is difficult to eliminate impurities in the material. The plastic processing of the material is difficult, and key data such as crystal grains, size and the like of the target material are mainly obtained in the smelting stage, so that the effective control is difficult.
Disclosure of Invention
Aiming at the defects existing in the prior art, the invention aims to provide a titanium-aluminum alloy target and a preparation method thereof. The invention obtains cast ingots with uniform components and tissues and no defects inside by adopting electron beam melting method for multiple times; and processing the casting blank into a target blank with fine and uniform grains by using an isothermal rolling method. The method can effectively control the performance of the titanium-aluminum alloy target material, and is suitable for mass production.
To achieve the purpose, the invention adopts the following technical scheme:
in a first aspect, the invention provides a preparation method of a titanium-aluminum alloy target, which comprises the following steps:
mixing the titanium sponge and the aluminum block according to the design requirement of alloy components, and sequentially carrying out isothermal rolling, annealing and machining after smelting to obtain the titanium-aluminum alloy target;
the smelting comprises primary smelting, secondary smelting and tertiary smelting which are sequentially carried out.
The invention can obtain the cast ingot with uniform composition and structure and internal object defects through multiple smelting; and processing the casting blank into a target blank with fine and uniform grains by using an isothermal rolling method. The method can effectively control the performance of the titanium-aluminum alloy target material, and is suitable for mass production.
In a preferred embodiment of the present invention, the average particle diameter of the titanium sponge is 10 to 20mm, for example, 10mm, 12mm, 14mm, 16mm, 18mm or 20mm, but the average particle diameter is not limited to the above-mentioned values, and other values not mentioned in the numerical range are equally applicable.
The average particle diameter of the aluminum block is preferably 10 to 20mm, and may be, for example, 10mm, 12mm, 14mm, 16mm, 18mm or 20mm, but not limited to the values recited, and other values not recited in the numerical range are equally applicable.
The invention adopts the titanium sponge as the preparation raw material, so that the cost of the raw material can be reduced on the basis of not reducing the performance of the target material.
Preferably, the weight of the aluminum block is 1.5-3 wt% higher than the theoretical value, for example, 1.5wt%, 1.7wt%, 1.9wt%, 2.1wt%, 2.3wt%, 2.5wt%, 2.7wt% or 3wt%, but not limited to the recited values, and other non-recited values within the range of values are equally applicable.
Considering the burning loss of materials in the subsequent smelting process, the addition amount of the aluminum block should be higher than the theoretical required weight, but the addition amount of the aluminum block is not too high because: when the addition amount is too high, the alloy proportion is changed, so that the performance of the product is affected.
As a preferable technical scheme of the invention, the method also comprises a pretreatment process for the titanium sponge and the aluminum block before mixing.
Preferably, the pretreatment comprises ultrasonic cleaning, drying and cooling which are sequentially performed.
Preferably, the cleaning liquid in the ultrasonic cleaning comprises absolute ethyl alcohol.
Preferably, the drying comprises vacuum drying.
The vacuum drying temperature is preferably 100 to 150 ℃, and may be, for example, 100 ℃, 110 ℃, 120 ℃, 130 ℃, 140 ℃, or 150 ℃, but is not limited to the values recited, and other values not recited in the numerical range are equally applicable.
Preferably, the vacuum drying time is 2-3h, for example, 2h, 2.2h, 2.4h, 2.6h, 2.8h or 3h, but not limited to the recited values, and other values not recited in the numerical range are equally applicable.
The cooling is preferably terminated at 20 to 30 ℃, and may be, for example, 20 ℃, 22 ℃, 24 ℃, 26 ℃, 28 ℃, or 30 ℃, but is not limited to the values recited, and other values not recited in the numerical range are equally applicable.
The pretreatment process can remove impurities on the surfaces of the titanium sponge and the aluminum block, is beneficial to reducing the defects of the cast ingot, and ensures the purity of the cast ingot.
As a preferable technical scheme of the invention, the vacuum degree in the primary smelting, the secondary smelting and the tertiary smelting is less than or equal to 5 multiplied by 10 -2 Pa may be, for example, 5X 10 -2 Pa、4×10 -2 Pa、3×10 -2 Pa、2×10 -2 Pa or 1X 10 -2 Pa, but not limited to the recited values, other values not recited in the numerical range are equally applicable.
Preferably, the primary smelting, the secondary smelting and the tertiary smelting are all followed by post-treatment.
Preferably, the post-treatment includes sequentially performing a vacuum state maintaining and a temperature lowering process.
Preferably, the time for maintaining the vacuum state is 3-4 hours, for example, 3 hours, 3.2 hours, 3.4 hours, 3.6 hours, 3.8 hours or 4 hours, but not limited to the recited values, and other values not recited in the numerical range are equally applicable.
The invention still bursts out of the vacuum state after smelting to maintain the purity of the cast ingot, and the too short time can cause the defect of the cast ingot and/or enrich impurities of the cast ingot, thereby affecting the performance of an alloy target, and the too long time can reduce the production efficiency.
Preferably, inert gas is introduced in the cooling process.
According to the invention, inert gas is introduced in the cooling process, so that the cooling process can be accelerated.
In a preferred embodiment of the present invention, the primary smelting power is 200 to 250kW, for example, 200kW, 210kW, 220kW, 230kW, 240kW or 250kW, but the present invention is not limited to the values listed, and other values not listed in the numerical range are equally applicable.
Preferably, the control rate of the primary smelting is 70 to 100kg/h, and may be, for example, 70kg/h, 80kg/h, 90kg/h or 100kg/h, but not limited to the values listed, and other values not listed in the numerical range are equally applicable.
In a preferred embodiment of the present invention, the secondary smelting power is 200 to 250kW, for example, 200kW, 210kW, 220kW, 230kW, 240kW or 250kW, but not limited to the values listed, and other values not listed in the numerical range are equally applicable.
Preferably, the control rate of the secondary smelting is 70 to 100kg/h, and may be, for example, 70kg/h, 80kg/h, 90kg/h or 100kg/h, but not limited to the values listed, and other values not listed in the numerical range are equally applicable. In a preferred embodiment of the present invention, the power of the third smelting is 200 to 250kW, for example, 200kW, 210kW, 220kW, 230kW, 240kW or 250kW, but the present invention is not limited to the values listed, and other values not listed in the numerical range are equally applicable.
Preferably, the control speed of the three-time smelting is 70 to 100kg/h, for example, 70kg/h, 80kg/h, 90kg/h or 100kg/h, but the control speed is not limited to the listed values, and other values not listed in the numerical range are equally applicable.
The primary smelting and the secondary smelting mainly finish alloying of materials, and ingot materials need to be turned over and placed in the secondary smelting process; the purpose of the third smelting is refining and impurity removal.
In a preferred embodiment of the present invention, the isothermal rolling temperature is 1100 to 1200 ℃, for example, 1100 ℃, 1120 ℃, 1140 ℃, 1160 ℃, 1180 ℃ or 1200 ℃, but the present invention is not limited to the above-mentioned values, and other values not mentioned in the above-mentioned value range are equally applicable.
In the isothermal rolling process, a casting blank can be processed into a target blank with fine and uniform grains, rolling deformation is difficult due to the fact that the temperature is too high, cracking and other problems occur, and when the temperature is too low, meeting metallographic phase and structure are transformed, and the grains grow.
Preferably, the reduction ratio per pass in the isothermal rolling is 5 to 8%, for example, the first 5%, 5.5%, 6%, 6.5%, 7%, 7.5% or 8%, but not limited to the values recited, and other values not recited in the numerical range are equally applicable.
In a preferred embodiment of the present invention, the annealing temperature is 600 to 1200 ℃, for example, 600 ℃, 700 ℃, 800 ℃, 900 ℃, 1000 ℃, 1100 ℃, or 1200 ℃, but the annealing temperature is not limited to the values listed, and other values not listed in the numerical range are equally applicable.
Preferably, the annealing time is 12-24 h, for example, 12h, 13h, 14h, 15h, 16h, 17h, 18h, 19h, 20h, 21h, 22h, 23h or 24h, but not limited to the recited values, and other values not recited in the numerical range are equally applicable.
The annealing temperature is 600-1200 ℃, the alloy phase and the structure are transformed when the annealing temperature is too high, the crystal grains grow up, the recrystallization can not be realized when the annealing temperature is too low, and the rolling state texture is generated.
Preferably, the annealing process is performed under a protective atmosphere.
Preferably, the protective atmosphere comprises any one or a combination of at least two of argon, nitrogen or helium, typically but not limited to combinations comprising: a combination of argon and nitrogen, a combination of argon and helium, a combination of nitrogen and helium, or a combination of argon, nitrogen and helium.
As a preferred technical scheme of the invention, the preparation method provided by the first aspect of the invention comprises the following steps:
(1) Ultrasonic cleaning is carried out on the titanium sponge and the aluminum block by adopting absolute ethyl alcohol, then vacuum drying is carried out for 2-3 hours at the temperature of 100-150 ℃, and cooling is carried out to 20-30 ℃;
(2) Mixing titanium sponge and aluminum blocks according to the design requirement of alloy components, wherein the weight of the aluminum blocks is 1.5-3 wt% higher than the theoretical value; then sequentially carrying out primary smelting, secondary smelting and tertiary smelting;
wherein the vacuum degree in the primary smelting, the secondary smelting and the tertiary smelting is less than or equal to 5 multiplied by 10 -2 Pa; the primary smelting, the secondary smelting and the tertiary smelting are all followed by post-treatment, and the post-treatment comprises: maintaining the vacuum state for 3-4 h, and then introducing inert gas to cool;
the power of the primary smelting is 200-250 kW, and the control speed is 70-100 kg/h; the power of the secondary smelting is 200-250 kW, and the control speed is 70-100 kg/h; the power of the third smelting is 200-250 kW, and the control speed is 70-100 kg/h;
(3) Carrying out isothermal rolling on the ingot material smelted in the step (2), wherein the isothermal rolling temperature is 1100-1200 ℃; the processing rate of each pass is 5-8%;
(4) Annealing the target blank rolled in the step (3) in a protective atmosphere, wherein the annealing temperature is 600-1200 ℃ and the annealing time is 12-24 hours;
(5) And (3) machining the annealed target blank in the step (4) to a specified size to obtain the titanium-aluminum alloy target.
In a second aspect, the invention provides a titanium-aluminum alloy target, which is obtained by adopting the preparation method provided in the first aspect.
The titanium-aluminum alloy target provided by the invention has uniform components and tissues, no defects in the interior and low gas impurity content; the grains are fine and uniform.
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:
(1) The titanium-aluminum alloy target provided by the invention has uniform components and tissues, no defects in the interior and low gas impurity content; fine and uniform grains;
(2) In the preparation method provided by the invention, the electron beam melting method is adopted for a plurality of times to obtain cast ingots with uniform components and tissues and no defects inside;
(3) In the preparation method provided by the invention, an isothermal rolling method is adopted to process a casting blank into a target blank with fine and uniform grains;
(4) The preparation method provided by the invention can effectively control the performance of the titanium-aluminum alloy target material, and is suitable for mass production.
Detailed Description
The technical scheme of the invention is further described by the following specific embodiments. It will be apparent to those skilled in the art that the examples are merely to aid in understanding the invention and are not to be construed as a specific limitation thereof.
Example 1
The embodiment provides a titanium-aluminum alloy target, and the preparation method of the titanium-aluminum alloy target comprises the following steps:
(1) Ultrasonic cleaning is carried out on the titanium sponge and the aluminum block by adopting absolute ethyl alcohol, then vacuum drying is carried out for 2.5 hours at the temperature of 120 ℃, and cooling is carried out to 25 ℃;
(2) Mixing titanium sponge and aluminum blocks according to the design requirement of alloy components, wherein the weight of the aluminum blocks is higher than 2 weight percent of theoretical value; then sequentially carrying out primary smelting, secondary smelting and tertiary smelting;
wherein the vacuum degree in the primary smelting, the secondary smelting and the tertiary smelting is 4.5 multiplied by 10 -2 Pa; the primary smelting, the secondary smelting and the tertiary smelting are all followed by post-treatment, and the post-treatment comprises: maintaining the vacuum state for 3.5 hours, and then introducing inert gas to cool;
the power of the primary smelting is 225kW, and the control speed is 135kg/h; the power of the secondary smelting is 225kW, and the control speed is 135kg/h; the power of the third smelting is 225kW, and the control speed is 135kg/h;
(3) Carrying out isothermal rolling on the ingot material smelted in the step (2), wherein the isothermal rolling temperature is 1150 ℃; the processing rate of each pass is 6%;
(4) Annealing the target blank rolled in the step (3) in a protective atmosphere, wherein the annealing temperature is 1000 ℃ and the annealing time is 18 hours;
(5) And (3) machining the annealed target blank in the step (4) to a specified size to obtain the titanium-aluminum alloy target.
Example 2
The embodiment provides a titanium-aluminum alloy target, and the preparation method of the titanium-aluminum alloy target comprises the following steps:
(1) Ultrasonic cleaning is carried out on the titanium sponge and the aluminum block by adopting absolute ethyl alcohol, then vacuum drying is carried out for 2 hours at the temperature of 100-150 ℃, and cooling is carried out to 30 ℃;
(2) Mixing titanium sponge and aluminum blocks according to the design requirement of alloy components, wherein the weight of the aluminum blocks is higher than 1.5wt% of the theoretical value; then sequentially carrying out primary smelting, secondary smelting and tertiary smelting;
wherein the vacuum degree in the primary smelting, the secondary smelting and the tertiary smelting is 2.5 multiplied by 10 -2 Pa; the primary smelting, the secondary smelting and the tertiary smelting are all followed by post-treatment, and the post-treatment comprises: maintaining the vacuum state for 3 hours, and then introducing argon gas to cool;
the power of the primary smelting is 100kW, and the control speed is 70kg/h; the power of the secondary smelting is 100kW, and the control speed is 70kg/h; the power of the third smelting is 100kW, and the control speed is 70kg/h;
(3) Carrying out isothermal rolling on the ingot material smelted in the step (2), wherein the isothermal rolling temperature is 1100 ℃; the processing rate of each pass is 5%;
(4) Annealing the target blank rolled in the step (3) in a protective atmosphere, wherein the annealing temperature is 600 ℃ and the annealing time is 24 hours;
(5) And (3) machining the annealed target blank in the step (4) to a specified size to obtain the titanium-aluminum alloy target.
Example 3
The embodiment provides a titanium-aluminum alloy target, and the preparation method of the titanium-aluminum alloy target comprises the following steps:
(1) Ultrasonic cleaning is carried out on the titanium sponge and the aluminum block by adopting absolute ethyl alcohol, then vacuum drying is carried out for 3 hours at the temperature of 100-150 ℃, and cooling is carried out to 20 ℃;
(2) Mixing titanium sponge and aluminum blocks according to the design requirement of alloy components, wherein the weight of the aluminum blocks is higher than 3 weight percent of theoretical value; then sequentially carrying out primary smelting, secondary smelting and tertiary smelting;
wherein the vacuum degree in the primary smelting, the secondary smelting and the tertiary smelting is 5 multiplied by 10 -2 Pa; the primary smelting, the secondary smelting and the tertiary smelting are all followed by post-treatment, and the post-treatment comprises: maintaining the vacuum state for 4 hours, and then introducing inert gas to cool;
the power of the primary smelting is 250kW, and the control speed is 100kg/h; the power of the secondary smelting is 100kW, and the control speed is 70kg/h; the power of the third smelting is 100kW, and the control speed is 70kg/h;
(3) Carrying out isothermal rolling on the ingot material smelted in the step (2), wherein the isothermal rolling temperature is 1200 ℃; the processing rate of each pass is 8%;
(4) Annealing the target blank rolled in the step (3) in a protective atmosphere, wherein the annealing temperature is 1200 ℃ and the annealing time is 12 hours;
(5) And (3) machining the annealed target blank in the step (4) to a specified size to obtain the titanium-aluminum alloy target.
Example 4
The embodiment provides a titanium-aluminum alloy target, and the preparation method of the titanium-aluminum alloy target is different from embodiment 1 only in that:
the pretreatment process of step (1) is omitted in this embodiment.
Example 5
The embodiment provides a titanium-aluminum alloy target, and the preparation method of the titanium-aluminum alloy target is different from embodiment 1 only in that:
in this example, the vacuum level in the smelting in the step (2) is changed to 6.5X10 -2 Pa。
Example 6
The embodiment provides a titanium-aluminum alloy target, and the preparation method of the titanium-aluminum alloy target is different from embodiment 1 only in that:
in this embodiment, the post-treatment process performed after the primary smelting, the secondary smelting and the tertiary smelting in the step (2) is omitted.
Example 7
The embodiment provides a titanium-aluminum alloy target, and the preparation method of the titanium-aluminum alloy target is different from embodiment 1 only in that:
in this example, the isothermal rolling temperature in step (3) was changed to 1000 ℃.
Example 8
The embodiment provides a titanium-aluminum alloy target, and the preparation method of the titanium-aluminum alloy target is different from embodiment 1 only in that:
in this example, the isothermal rolling temperature in step (3) was changed to 1300 ℃.
Example 9
The embodiment provides a titanium-aluminum alloy target, and the preparation method of the titanium-aluminum alloy target is different from embodiment 1 only in that:
in this example, the reduction ratio of each pass of isothermal rolling in the step (3) was changed to 4%.
Example 10
The embodiment provides a titanium-aluminum alloy target, and the preparation method of the titanium-aluminum alloy target is different from embodiment 1 only in that:
in this example, the reduction ratio of each pass of isothermal rolling in the step (3) was changed to 10%.
Example 11
The embodiment provides a titanium-aluminum alloy target, and the preparation method of the titanium-aluminum alloy target is different from embodiment 1 only in that:
the temperature of the annealing in the step (4) is changed to 500 ℃ in the embodiment.
Example 12
The embodiment provides a titanium-aluminum alloy target, and the preparation method of the titanium-aluminum alloy target is different from embodiment 1 only in that:
in this example, the annealing temperature in step (4) was changed to 1300 ℃.
Comparative example 1
This comparative example provides a titanium-aluminum alloy target, the preparation method of which differs from example 1 only in that:
the comparative example changes the primary smelting, the secondary smelting and the tertiary smelting which are sequentially carried out in the step (2) into disposable smelting.
Comparative example 2
This comparative example provides a titanium-aluminum alloy target, the preparation method of which differs from example 1 only in that:
this comparative example changes the isothermal rolling described in step (3) to conventional rolling.
And (3) performance detection:
the titanium-aluminum alloy targets provided in examples 1 to 12 and comparative examples 1 to 2 were subjected to target purity detection, oxygen content detection, grain size detection, and relative density detection, and the results are shown in table 1.
TABLE 1
In conclusion, the invention obtains the cast ingot with uniform composition and structure and no defect inside by adopting electron beam melting method for multiple times; and processing the casting blank into a target blank with fine and uniform grains by using an isothermal rolling method. The method provided by the invention can effectively control the performance of the titanium-aluminum alloy target material, and is suitable for mass production.
While the foregoing is directed to embodiments of the present invention, other and further details of the invention may be had by the present invention, it should be understood that the foregoing description is merely illustrative of the present invention and that no limitations are intended to the scope of the invention, except insofar as modifications, equivalents, improvements or modifications are within the spirit and principles of the invention.
Claims (10)
1. The preparation method of the titanium-aluminum alloy target is characterized by comprising the following steps of:
mixing the titanium sponge and the aluminum block according to the design requirement of alloy components, and sequentially carrying out isothermal rolling, annealing and machining after smelting to obtain the titanium-aluminum alloy target;
the smelting comprises primary smelting, secondary smelting and tertiary smelting which are sequentially carried out.
2. The method according to claim 1, wherein the average particle diameter of the titanium sponge is 10 to 20mm;
preferably, the average particle diameter of the aluminum block is 10-20 mm;
preferably, the weight of the aluminum block is 1.5 to 3wt% higher than the theoretical value.
3. The preparation method according to claim 1 or 2, wherein the pre-mixing further comprises a pretreatment process of the titanium sponge and the aluminum block;
preferably, the pretreatment comprises ultrasonic cleaning, drying and cooling which are sequentially carried out;
preferably, the cleaning liquid in the ultrasonic cleaning comprises absolute ethyl alcohol;
preferably, the drying comprises vacuum drying;
preferably, the temperature of the vacuum drying is 100-150 ℃;
preferably, the time of vacuum drying is 2-3 hours;
preferably, the end point of the cooling is 20-30 ℃.
4. A method according to any one of claims 1 to 3, wherein the vacuum degree in the primary smelting, the secondary smelting and the tertiary smelting is 5 x 10 or less -2 Pa；
Preferably, the primary smelting, the secondary smelting and the tertiary smelting are all followed by post-treatment;
preferably, the post-treatment comprises a vacuum state maintaining and cooling process which are sequentially carried out;
preferably, the time for maintaining the vacuum state is 3-4 hours;
preferably, inert gas is introduced in the cooling process.
5. The method according to any one of claims 1 to 4, wherein the power of the primary smelting is 200 to 250kW;
preferably, the control speed of the primary smelting is 70-100 kg/h.
6. The method according to any one of claims 1 to 5, wherein the power of the secondary smelting is 200 to 250kW;
preferably, the control speed of the secondary smelting is 70-100 kg/h.
7. The method according to any one of claims 1 to 6, wherein the power of the three smelting is 200 to 250kW;
preferably, the control speed of the three smelting is 70-100 kg/h.
8. The method of any one of claims 1-7, wherein the isothermal rolling temperature is 1100-1200 ℃;
preferably, the processing rate of each pass in the isothermal rolling is 5-8%;
preferably, the annealing temperature is 600-1200 ℃;
preferably, the annealing time is 12-24 hours;
preferably, the annealing process is performed under a protective atmosphere;
preferably, the protective atmosphere comprises any one or a combination of at least two of argon, nitrogen or helium.
9. The preparation method according to any one of claims 1 to 8, characterized in that the preparation method comprises the steps of:
(1) Ultrasonic cleaning is carried out on the titanium sponge and the aluminum block by adopting absolute ethyl alcohol, then vacuum drying is carried out for 2-3 hours at the temperature of 100-150 ℃, and cooling is carried out to 20-30 ℃;
(2) Mixing titanium sponge and aluminum blocks according to the design requirement of alloy components, wherein the weight of the aluminum blocks is 1.5-3 wt% higher than the theoretical value; then sequentially carrying out primary smelting, secondary smelting and tertiary smelting;
wherein the vacuum degree in the primary smelting, the secondary smelting and the tertiary smelting is less than or equal to 5 multiplied by 10 -2 Pa; the primary smelting, the secondary smelting and the tertiary smelting are all followed by post-treatment, and the post-treatment comprises: maintaining the vacuum state for 3-4 h, and then introducing inert gas to cool;
the power of the primary smelting is 200-250 kW, and the control speed is 70-100 kg/h; the power of the secondary smelting is 200-250 kW, and the control speed is 70-100 kg/h; the power of the third smelting is 200-250 kW, and the control speed is 70-100 kg/h;
(3) Carrying out isothermal rolling on the ingot material smelted in the step (2), wherein the isothermal rolling temperature is 1100-1200 ℃; the processing rate of each pass is 5-8%;
(4) Annealing the target blank rolled in the step (3) in a protective atmosphere, wherein the annealing temperature is 600-1200 ℃ and the annealing time is 12-24 hours;
(5) And (3) machining the annealed target blank in the step (4) to a specified size to obtain the titanium-aluminum alloy target.
10. A titanium-aluminum alloy target, characterized in that the titanium-aluminum alloy target is obtained by the preparation method according to any one of claims 1 to 9.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311430895.8A CN117265489A (en) | 2023-10-31 | 2023-10-31 | Titanium-aluminum alloy target and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311430895.8A CN117265489A (en) | 2023-10-31 | 2023-10-31 | Titanium-aluminum alloy target and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN117265489A true CN117265489A (en) | 2023-12-22 |
Family
ID=89214415
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202311430895.8A Pending CN117265489A (en) | 2023-10-31 | 2023-10-31 | Titanium-aluminum alloy target and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN117265489A (en) |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112725658A (en) * | 2020-12-10 | 2021-04-30 | 先导薄膜材料（广东）有限公司 | Preparation method of titanium-aluminum alloy target |
| CN113444902A (en) * | 2021-06-29 | 2021-09-28 | 哈尔滨工业大学 | Preparation method of low-oxygen low-nitrogen titanium-aluminum alloy ingot |
| CN115896714A (en) * | 2022-12-30 | 2023-04-04 | 宝鸡市飞腾金属材料股份有限公司 | High-performance ultra-long large-sized rotating titanium tube target material for large wafer and preparation process |
| CN116275068A (en) * | 2023-03-21 | 2023-06-23 | 宁波江丰电子材料股份有限公司 | Preparation method of titanium-aluminum alloy target |
-
2023
- 2023-10-31 CN CN202311430895.8A patent/CN117265489A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112725658A (en) * | 2020-12-10 | 2021-04-30 | 先导薄膜材料（广东）有限公司 | Preparation method of titanium-aluminum alloy target |
| CN113444902A (en) * | 2021-06-29 | 2021-09-28 | 哈尔滨工业大学 | Preparation method of low-oxygen low-nitrogen titanium-aluminum alloy ingot |
| CN115896714A (en) * | 2022-12-30 | 2023-04-04 | 宝鸡市飞腾金属材料股份有限公司 | High-performance ultra-long large-sized rotating titanium tube target material for large wafer and preparation process |
| CN116275068A (en) * | 2023-03-21 | 2023-06-23 | 宁波江丰电子材料股份有限公司 | Preparation method of titanium-aluminum alloy target |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN111411285A (en) | Al and Ti microalloyed high-strength and high-toughness medium-entropy alloy and preparation method thereof | |
| CN106319463B (en) | A kind of preparation method of rolling processing tungsten-titanium alloy target material | |
| CN112063907B (en) | Multi-principal-element high-temperature alloy and preparation method thereof | |
| WO2021046927A1 (en) | Nickel-rhenium alloy rotary tubular target material containing trace rare earth elements and preparation method therefor | |
| CN114481053B (en) | Magnesium zinc aluminum nickel vanadium alloy target and manufacturing method thereof | |
| TW201533248A (en) | High-purity tantalum powder and preparation method therefor | |
| CN110904364B (en) | Preparation method of aluminum alloy target material | |
| JPH06264232A (en) | Ta sputtering target and its production | |
| CN111676411A (en) | Microalloyed high-toughness dynamic sealing material and preparation method thereof | |
| CN114939654A (en) | High-entropy alloy powder for laser additive manufacturing and preparation method and application thereof | |
| CN113215494B (en) | Preparation method of aviation invar alloy plate | |
| CN112725658B (en) | Preparation method of titanium-aluminum alloy target | |
| CN110735068B (en) | Preparation method and application of cobalt-tantalum-zirconium alloy target | |
| CN117265489A (en) | Titanium-aluminum alloy target and preparation method thereof | |
| CN114807646B (en) | Nickel-based alloy plate blank and preparation method thereof | |
| JPH06264233A (en) | Sputtering target for producing tft | |
| CN114000073A (en) | Process method for improving internal structure of high-purity nickel target material | |
| CN113046704B (en) | Preparation method of low-oxygen large-size aluminum-based intermetallic compound-containing alloy target | |
| CN112680680A (en) | Processing method of Pt-25Ag alloy material | |
| CN115747731B (en) | Preparation method of metal scandium rare earth target material | |
| CN112962072B (en) | Low-oxygen large-size aluminum-based intermetallic compound-containing alloy target and preparation method thereof | |
| CN112962069B (en) | Intermetallic compound-containing aluminum alloy target and preparation method thereof | |
| CN111590071B (en) | Molybdenum-niobium alloy target material and preparation method thereof | |
| JPS6229481B2 (en) | ||
| CN116393705B (en) | Titanium alloy material for 3D printing and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination |