CN114892136A - Tantalum target material and preparation method and application thereof - Google Patents
Tantalum target material and preparation method and application thereof Download PDFInfo
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- CN114892136A CN114892136A CN202210583501.1A CN202210583501A CN114892136A CN 114892136 A CN114892136 A CN 114892136A CN 202210583501 A CN202210583501 A CN 202210583501A CN 114892136 A CN114892136 A CN 114892136A
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- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 title claims abstract description 111
- 229910052715 tantalum Inorganic materials 0.000 title claims abstract description 108
- 239000013077 target material Substances 0.000 title claims abstract description 73
- 238000002360 preparation method Methods 0.000 title claims abstract description 27
- 238000010273 cold forging Methods 0.000 claims abstract description 62
- 238000010438 heat treatment Methods 0.000 claims abstract description 56
- 238000005097 cold rolling Methods 0.000 claims abstract description 47
- 238000001953 recrystallisation Methods 0.000 claims abstract description 23
- 238000000034 method Methods 0.000 claims description 44
- 238000005242 forging Methods 0.000 claims description 25
- 230000009467 reduction Effects 0.000 claims description 10
- 238000004544 sputter deposition Methods 0.000 claims description 9
- 238000004519 manufacturing process Methods 0.000 claims description 7
- 230000000052 comparative effect Effects 0.000 description 15
- 238000000137 annealing Methods 0.000 description 9
- 230000008569 process Effects 0.000 description 7
- 239000000843 powder Substances 0.000 description 6
- 239000007787 solid Substances 0.000 description 5
- 230000000694 effects Effects 0.000 description 4
- 238000001513 hot isostatic pressing Methods 0.000 description 4
- 238000005096 rolling process Methods 0.000 description 4
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 3
- 239000001257 hydrogen Substances 0.000 description 3
- 229910052739 hydrogen Inorganic materials 0.000 description 3
- 238000005984 hydrogenation reaction Methods 0.000 description 3
- 150000002500 ions Chemical class 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- 229910000831 Steel Inorganic materials 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 238000009694 cold isostatic pressing Methods 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000007872 degassing Methods 0.000 description 2
- 239000010408 film Substances 0.000 description 2
- 238000005098 hot rolling Methods 0.000 description 2
- 238000010884 ion-beam technique Methods 0.000 description 2
- 238000005245 sintering Methods 0.000 description 2
- 239000010959 steel Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 239000010409 thin film Substances 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 238000003801 milling Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000008520 organization Effects 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000005477 sputtering target Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000004381 surface treatment Methods 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
- B21J—FORGING; HAMMERING; PRESSING METAL; RIVETING; FORGE FURNACES
- B21J5/00—Methods for forging, hammering, or pressing; Special equipment or accessories therefor
- B21J5/002—Hybrid process, e.g. forging following casting
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/3407—Cathode assembly for sputtering apparatus, e.g. Target
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Crystallography & Structural Chemistry (AREA)
- Physical Vapour Deposition (AREA)
Abstract
The invention provides a tantalum target material and a preparation method and application thereof, wherein the preparation method of the tantalum target material comprises the following steps: and sequentially carrying out first cold forging, first heat treatment, second cold forging, second heat treatment and cold rolling on the tantalum ingot to obtain the tantalum target material. The control of the target recrystallization degree is realized through twice cold forging, twice heat treatment and cold rolling, the operation is simple and convenient, and the industrialization is easy to realize; and the prepared tantalum target material has high purity and uniform internal structure.
Description
Technical Field
The invention belongs to the field of sputtering target preparation, and particularly relates to a tantalum target and a preparation method and application thereof.
Background
Sputtering is one of the main techniques for preparing thin film materials, and is characterized in that ions generated by an ion source are accelerated and gathered in vacuum to form ion beam flow with high speed energy, the ion beam flows bombard the surface of a solid, kinetic energy exchange is carried out between the ions and atoms on the surface of the solid, the atoms on the surface of the solid leave the solid and are deposited on the surface of a substrate, and the bombarded solid is a raw material for preparing a thin film deposited by a sputtering method and is generally called as a target material.
The target is an extremely important key material required for manufacturing semiconductor chips, and the internal organization structure of a target product has strict requirements, so that the sputtering rate and the uniformity of a deposited film are seriously influenced.
Tantalum, a typical metal material, is ductile and has a small coefficient of expansion, and has extremely high corrosion resistance and toughness. The tantalum target is a typical metal target, and is widely applied to various fields due to the important characteristics of good corrosion resistance, good electromagnetic shielding performance, capability of being used as an energy material and the like.
CN103147050A discloses a production method of a high-purity tantalum target, which comprises the steps of (1) placing a tantalum block with the size of 5-10 mm multiplied by 5-10 mm in a hydrogenation furnace for hydrogen absorption; (2) crushing the tantalum after hydrogen absorption into powder of-200 meshes, placing the powder in a steel sheath, heating and exhausting according to a certain speed and stage, then placing the steel sheath in a hot isostatic pressing machine for sintering, wherein the sintering temperature is 1100-1500 ℃, the atmosphere pressure is 50-200 MPa, and finally machining and cutting the powder into a specified shape. According to the method, the obtained powder is directly subjected to degassing treatment, the powder is low in loose packing density and easy to escape, subsequent hot isostatic pressing is influenced, the deformation amount of the sintered target material is large, and the yield is low.
CN113235056A discloses a preparation method of a high-purity tantalum target material, which comprises the following steps: placing the high-purity tantalum source in a hydrogenation furnace, vacuumizing, introducing hydrogen for heating after vacuumizing, and stopping heating after the pressure in the hydrogenation furnace is not reduced any more to obtain a tantalum hydride source; crushing the obtained tantalum hydride source, and then sequentially carrying out cold isostatic pressing, degassing treatment and hot isostatic pressing to obtain a high-purity tantalum target material; the preparation method adopts tantalum hydride powder, and combines a cold isostatic pressing process and a hot isostatic pressing process, so that the oxygen content of the obtained tantalum target material is effectively reduced, the yield of the tantalum target material is improved, and the method has a good industrial application prospect.
CN103028898A discloses a preparation method of a high-performance tantalum target material, which comprises the steps of firstly preparing a forging blank from a tantalum ingot by a cold forging and hot forging method, then rolling by a hot rolling method, finally leveling, blanking, milling and carrying out surface treatment according to the size of a finished product to obtain the tantalum target material. The method adopts a cold forging and hot forging process to forge a tantalum ingot, and then adopts a hot rolling process to roll a forged blank, so as to obtain the high-performance tantalum target material meeting the use requirement of a high-end sputtering base station.
CN104419901B discloses a method for manufacturing a tantalum target, which comprises hot forging a tantalum ingot, and then performing an annealing process on the hot forged tantalum ingot to form a first tantalum target blank; rolling the first tantalum target blank to form a second tantalum target blank; and carrying out secondary annealing process on the second tantalum target blank to obtain the tantalum target. The tantalum target formed by the technical scheme has fine internal crystal grains and uniform internal structure, and effectively avoids the defects of layering and the like in the tantalum target, so that the sputtering rate of the tantalum target and the quality of a formed tantalum film in the subsequent use process are improved.
However, the above-mentioned technical solutions do not make detailed studies on the recrystallization degree of the tantalum target material, and the problems of non-uniform internal structure, non-uniform plating, and the like are likely to occur in the prior art.
Therefore, how to provide a target with controllable recrystallization degree while ensuring uniform internal structure of the target is a problem to be solved at present.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide a tantalum target material and a preparation method and application thereof, wherein the preparation method of the tantalum target material comprises the following steps: and sequentially carrying out first cold forging, first heat treatment, second cold forging, second heat treatment and cold rolling on the tantalum ingot to obtain the tantalum target material. The control of the target recrystallization degree is realized through twice cold forging, twice heat treatment and cold rolling, the operation is simple and convenient, and the industrialization is easy to realize; the prepared tantalum target material has high purity and uniform internal structure.
In order to achieve the purpose, the invention adopts the following technical scheme:
one of the purposes of the invention is to provide a preparation method of a tantalum target material, which comprises the following steps:
and sequentially carrying out first cold forging, first heat treatment, second cold forging, second heat treatment and cold rolling on the tantalum ingot to obtain the tantalum target material.
According to the invention, through the first cold forging, the first heat treatment, the second cold forging, the second heat treatment and the cold rolling, the control of the target recrystallization degree is realized, the operation is simple and convenient, and the industrialization is easy to realize.
The method has the advantages that the tantalum target material obtained by the method is a target material which is not completely recrystallized, and the preparation of the target material which is not completely recrystallized reduces recrystallization annealing procedures, improves production efficiency and reduces processing cost; in the sputtering process, the coating is more uniform and the effect is more obvious.
As a preferred embodiment of the present invention, the purity of the tantalum ingot is 4N or more, and may be, for example, 4N2, 4N5, 4N8, 5N, 5N2, 5N5, 5N7, 6N, etc., but the tantalum ingot is not limited to the above-mentioned values, and other values not listed in the above-mentioned range of values are also applicable.
In a preferred embodiment of the present invention, the temperature of the first cold forging is 10 to 30 ℃, for example, 10 ℃, 12 ℃, 14 ℃, 16 ℃, 18 ℃, 20 ℃, 22 ℃, 24 ℃, 26 ℃, 28 ℃, 30 ℃ or the like, but is not limited to the above-mentioned values, and other values not listed in the above-mentioned range of values are also applicable.
Preferably, the forging ratio of the first cold forging is 1.0 to 2.5, and may be, for example, 1.0, 1.1, 1.2, 1.3, 1.4, 1.5, 1.6, 1.7, 1.8, 1.9, 2.0, 2.1, 2.2, 2.3, 2.4, 2.5, etc., but is not limited to the values listed, and other values not listed in the above numerical range are also applicable.
In a preferred embodiment of the present invention, the temperature of the first heat treatment is 900-.
It is worth to say that the temperature of the first heat treatment is 900-; if the temperature is higher than 1200 ℃, the final target recrystallization degree is affected, and the use effect of the target is finally affected.
Preferably, the time of the first heat treatment is 30 to 120min, and may be, for example, 30min, 40min, 50min, 60min, 70min, 80min, 90min, 100min, 110min, 120min, etc., but is not limited to the enumerated values, and other non-enumerated values within the above-mentioned range of values are also applicable.
In a preferred embodiment of the present invention, the temperature of the second cold forging is 10 to 30 ℃, for example, 10 ℃, 12 ℃, 14 ℃, 16 ℃, 18 ℃, 20 ℃, 22 ℃, 24 ℃, 26 ℃, 28 ℃, 30 ℃ or the like, but is not limited to the above-mentioned values, and other values not listed in the above-mentioned range of values are also applicable.
Preferably, the forging ratio of the second cold forging is 1.0 to 2.5, and may be, for example, 1.0, 1.1, 1.2, 1.3, 1.4, 1.5, 1.6, 1.7, 1.8, 1.9, 2.0, 2.1, 2.2, 2.3, 2.4, 2.5, etc., but is not limited to the enumerated values, and other values not enumerated in the above numerical range are also applicable.
In a preferred embodiment of the present invention, the temperature of the second heat treatment is 1000-.
It is worth explaining that the temperature of the second heat treatment is 1000-; if the temperature is higher than 1200 ℃, the final target recrystallization degree is affected, and the use effect of the target is finally affected.
Preferably, the time of the second heat treatment is 30 to 120min, and may be, for example, 30min, 40min, 50min, 60min, 70min, 80min, 90min, 100min, 110min, 120min, etc., but is not limited to the enumerated values, and other non-enumerated values within the above-mentioned range of values are also applicable.
In a preferred embodiment of the present invention, the cold rolling temperature is 10 to 30 ℃, for example, 10 ℃, 12 ℃, 14 ℃, 16 ℃, 18 ℃, 20 ℃, 22 ℃, 24 ℃, 26 ℃, 28 ℃, 30 ℃ or the like, but the cold rolling temperature is not limited to the above-mentioned values, and other values not listed in the above-mentioned range of values are also applicable.
Preferably, the cold rolling has a deformation of 60 to 90%, for example, 60%, 62%, 64%, 66%, 68%, 70%, 72%, 74%, 76%, 78%, 80%, 82%, 84%, 86%, 88%, 90%, etc., but is not limited to the recited values, and other values not recited in the above range are also applicable.
It is worth to say that the deformation amount of the cold rolling is 60-90%, and if the deformation amount is less than 60%, the uniformity of the whole target recrystallization degree is influenced due to insufficient target deformation rate; if the deformation rate is higher than 90%, the product deforms due to the overlarge deformation rate, and subsequent target processing is influenced.
Preferably, the rolling is performed by a rolling reduction of 0.5 to 5.0mm per pass, for example, 0.5mm, 0.7mm, 1.0mm, 1.2mm, 1.5mm, 1.8mm, 2.0mm, 2.2mm, 2.5mm, 2.7mm, 3.0mm, 3.3mm, 3.5mm, 3.8mm, 4.0mm, 4.2mm, 4.5mm, 4.7mm, 5.0mm, etc., but not limited to the values listed, and other values not listed in the above-mentioned range of values are also applicable.
As a preferred technical scheme of the invention, the preparation method of the tantalum target material comprises the following steps:
performing first cold forging on tantalum ingots with the purity of more than or equal to 4N at the temperature of 10-30 ℃, and controlling the forging ratio of the first cold forging to be 1.0-2.5; performing a first heat treatment at 900-; performing second cold forging at 10-30 ℃, wherein the forging ratio of the second cold forging is controlled to be 1.0-2.5; performing a second heat treatment at 1000-; and (3) cold rolling at 10-30 ℃, and controlling the reduction of 0.5-5.0mm and the deformation of 60-90% in each pass during cold rolling to obtain the tantalum target material.
It is a second object of the present invention to provide a tantalum target material obtained by the method according to the first object, wherein the degree of recrystallization of the tantalum target material is 20 to 40%, for example, 20%, 22%, 25%, 28%, 30%, 33%, 35%, 37%, 40%, etc., but not limited to the recited values, and other values not recited in the above range of values are also applicable.
It is worth to say that the tantalum target material with the recrystallization degree of 20-40% has more uniform coating and more obvious effect when being used for sputtering the target material with the recrystallization degree of 20-40%.
The third object of the present invention is to provide an application of the second object of the tantalum target material, wherein the tantalum target material is used for sputter coating.
The recitation of numerical ranges herein includes not only the above-recited numerical values, but also any numerical values between non-recited numerical ranges, and is not intended to be exhaustive or to limit the invention to the precise numerical values encompassed within the range for brevity and clarity.
Compared with the prior art, the invention has the beneficial effects that:
(1) according to the preparation method of the tantalum target material, the control of the target material recrystallization degree is realized through the first cold forging, the first heat treatment, the second cold forging, the second heat treatment and the cold rolling, the operation is simple and convenient, and the industrialization is easy to realize;
(2) the tantalum target material has high purity and uniform internal structure.
Detailed Description
The technical solution of the present invention is further explained by the following embodiments. It should be understood by those skilled in the art that the examples are only for the understanding of the present invention and should not be construed as the specific limitations of the present invention.
Example 1
The embodiment provides a tantalum target material and a preparation method thereof, wherein the preparation method of the tantalum target material comprises the following steps:
performing first cold forging on a tantalum ingot with the purity of 4N5 at 20 ℃, and controlling the forging ratio of the first cold forging to be 1.6; performing a first heat treatment at 1000 deg.C for 90 min; performing second cold forging at 20 ℃, wherein the forging ratio of the second cold forging is controlled to be 2.0; performing a second heat treatment at 1100 deg.C for 60 min; and (3) cold rolling at 20 ℃, and controlling the reduction of 2.0mm and the deformation of the cold rolling of 80% in each pass during the cold rolling to obtain the tantalum target material.
Example 2
The embodiment provides a tantalum target material and a preparation method thereof, wherein the preparation method of the tantalum target material comprises the following steps:
performing first cold forging on a tantalum ingot with the purity of 5N at 30 ℃, and controlling the forging ratio of the first cold forging to be 1.0; performing a first heat treatment at 1200 deg.C for 30 min; performing second cold forging at 30 ℃, wherein the forging ratio of the second cold forging is controlled to be 2.5; performing a second heat treatment at 1200 deg.C for 30 min; and (3) cold rolling at 30 ℃, and controlling the reduction of 0.5mm and the deformation of the cold rolling of 70% in each pass during the cold rolling to obtain the tantalum target material.
Example 3
The embodiment provides a tantalum target material and a preparation method thereof, wherein the preparation method of the tantalum target material comprises the following steps:
performing first cold forging on a tantalum ingot with the purity of 4N at 10 ℃, and controlling the forging ratio of the first cold forging to be 2.5; performing a first heat treatment at 900 deg.C for 120 min; performing second cold forging at 10 ℃, wherein the forging ratio of the second cold forging is controlled to be 1.5; performing a second heat treatment at 1000 deg.C for 120 min; and (3) cold rolling at 10 ℃, and controlling the reduction of 5.0mm and the deformation of the cold rolling of 90% in each pass during the cold rolling to obtain the tantalum target material.
Example 4
The embodiment provides a tantalum target material and a preparation method thereof, wherein the preparation method of the tantalum target material comprises the following steps:
performing first cold forging on a tantalum ingot with the purity of 4N5 at 15 ℃, and controlling the forging ratio of the first cold forging to be 2.0; performing a first heat treatment at 1100 deg.C for 60 min; performing second cold forging at 15 ℃, wherein the forging ratio of the second cold forging is controlled to be 1.0; performing a second heat treatment at 1100 deg.C for 90 min; and (3) cold rolling at 15 ℃, and controlling the reduction of 3.0mm and the deformation of cold rolling of 60% in each pass during cold rolling to obtain the tantalum target material.
Example 5
The present embodiment provides a tantalum target material and a method for preparing the same, which is different from the method described in embodiment 1 only in that: the temperature of the first heat treatment is 800 ℃.
Example 6
The present embodiment provides a tantalum target material and a method for preparing the same, which is different from the method described in embodiment 1 only in that: the temperature of the first heat treatment was 1300 ℃.
Example 7
The present embodiment provides a tantalum target material and a method for preparing the same, which is different from the method described in embodiment 1 only in that: the temperature of the second heat treatment is 900 ℃.
Example 8
The present embodiment provides a tantalum target material and a method for preparing the same, which is different from the method described in embodiment 1 only in that: the temperature of the second heat treatment was 1300 ℃.
Example 9
The present embodiment provides a tantalum target material and a method for preparing the same, which is different from the method described in embodiment 1 only in that: the cold rolling deformation was 50%.
Example 10
The present embodiment provides a tantalum target material and a method for preparing the same, which is different from the method described in embodiment 1 only in that: the cold rolling deformation was 95%.
Comparative example 1
The present comparative example provides a tantalum target material and a method for preparing the same, with reference to the method of example 1, except that: carrying out primary cold forging and primary heat treatment; namely, the preparation method of the tantalum target material comprises the following steps:
performing cold forging on a tantalum ingot with the purity of 4N5 at the temperature of 20 ℃, and controlling the forging ratio of the cold forging to be 1.6; performing heat treatment at 1000 deg.C for 150 min; and (3) cold rolling at 20 ℃, and controlling the reduction of 2.0mm and the deformation of the cold rolling of 80% in each pass during the cold rolling to obtain the tantalum target material.
Comparative example 2
The present comparative example provides a tantalum target material and a method for preparing the same, with reference to the method of example 1, except that: cold rolling is omitted; namely, the preparation method of the tantalum target material comprises the following steps:
performing first cold forging on a tantalum ingot with the purity of 4N5 at 20 ℃, and controlling the forging ratio of the first cold forging to be 1.6; performing a first heat treatment at 1000 deg.C for 90 min; performing second cold forging at 20 ℃, wherein the forging ratio of the second cold forging is controlled to be 2.0; and carrying out second heat treatment at 1100 ℃ for 60min to obtain the tantalum target material.
Comparative example 3
The present comparative example provides a tantalum target material and a method for preparing the same, with reference to the method of example 1, except that: annealing after the cold rolling is finished; namely, the preparation method of the tantalum target material comprises the following steps:
performing first cold forging on a tantalum ingot with the purity of 4N5 at 20 ℃, and controlling the forging ratio of the first cold forging to be 1.6; performing a first heat treatment at 1000 deg.C for 90 min; performing second cold forging at 20 ℃, wherein the forging ratio of the second cold forging is controlled to be 2.0; performing a second heat treatment at 1100 deg.C for 60 min; cold rolling at 20 ℃, and controlling the reduction of 2.0mm and the deformation of the cold rolling to be 80% in each pass during the cold rolling; annealing at 1200 ℃ for 30min to obtain the tantalum target material.
The tantalum target materials obtained in the above examples and comparative examples were tested by the following methods:
degree of recrystallization: after the tantalum target material to be detected is ground, polished and corroded, the recrystallization degree of the tantalum target material is detected and analyzed by using a scanning electron microscope;
uniformity: the uniformity of the internal tissue of the tantalum target is characterized by using a conductivity meter, the larger the conductivity fluctuation is, the worse the uniformity of the target is, the fluctuation generally exceeds +/-10%, the target tissue is considered to be non-uniform, and the fluctuation does not exceed +/-10%, the target tissue is considered to be uniform; testing the conductivity fluctuation of N targets, wherein the uniformity is (the number of uniform targets/N) multiplied by 100%;
the results of the crystallinity tests of the tantalum targets obtained in the above examples and comparative examples are shown in Table 1.
TABLE 1
| Item | Degree of recrystallization/%) | Uniformity/%) |
| Example 1 | 25 | 98 |
| Example 2 | 24 | 96 |
| Example 3 | 32 | 97 |
| Example 4 | 29 | 96 |
| Example 5 | 34 | 89 |
| Example 6 | 42 | 92 |
| Example 7 | 26 | 88 |
| Example 8 | 43 | 92 |
| Example 9 | 48 | 85 |
| Example 10 | 28 | 93 |
| Comparative example 1 | 51 | 82 |
| Comparative example 2 | 90 | 86 |
| Comparative example 3 | 95 | 95 |
From table 1, the following points can be seen:
(1) as can be seen from the examples 1-4, the invention controls the recrystallization degree of the tantalum target material to be 20-40% through the first cold forging, the first heat treatment, the second cold forging, the second heat treatment and the cold rolling, and the tantalum target material has high purity and uniform internal structure;
(2) comparing example 1 with examples 5 and 6, it can be seen that the temperature of the first heat treatment in example 5 is 800 ℃ which is lower than the preferred temperature of 900-1200 ℃ of the present invention, resulting in incomplete annealing and reduced uniformity; since the temperature of the first heat treatment in example 6 was 1300 ℃ which is more than the preferred 900-1200 ℃ of the present invention, the degree of recrystallization was increased;
(3) comparing example 1 with examples 7 and 8, it can be seen that the temperature of the second heat treatment in example 7 is 900 ℃ which is lower than the preferred temperature of 1000 ℃ and 1200 ℃ of the present invention, resulting in incomplete annealing and reduced uniformity; since the temperature of the second heat treatment in example 8 was 1300 ℃ which is more than the preferred temperature of 1000 ℃ and 1200 ℃ of the present invention, the degree of recrystallization was increased;
(4) comparing example 1 with examples 9 and 10, it can be seen that since the deformation amount of the cold rolling in example 9 is 50%, which is lower than the preferable 60-90% of the present invention, the target deformation ratio is insufficient, resulting in a decrease in uniformity; since the deformation amount of the cold rolling in the embodiment 10 is 95%, which is more than 60-90% preferred by the invention, the uniformity and the recrystallization degree of the cold rolling are not changed greatly, but the deformation rate is too large, so that the product deformation is caused, and the subsequent target processing is influenced;
(5) comparing example 1 with comparative examples 1 to 3, it can be seen that only one cold forging and one heat treatment were performed in comparative example 1, resulting in a decrease in uniformity; in the comparative example 2, cold rolling is omitted, the target material has high recrystallization degree and reduced uniformity; comparative example 3 annealing was performed after the cold rolling was completed, and the recrystallization degree of the target material was greatly improved by the annealing.
The above-mentioned embodiments are intended to illustrate the objects, technical solutions and advantages of the present invention in further detail, and it should be understood that the above-mentioned embodiments are only exemplary embodiments of the present invention, and are not intended to limit the present invention, and any modifications, equivalents, improvements and the like made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. The preparation method of the tantalum target is characterized by comprising the following steps:
and sequentially carrying out first cold forging, first heat treatment, second cold forging, second heat treatment and cold rolling on the tantalum ingot to obtain the tantalum target material.
2. The method of claim 1, wherein the tantalum ingot has a purity of 4N or more.
3. The production method according to claim 1 or 2, wherein the temperature of the first cold forging is 10 to 30 ℃;
preferably, the forging ratio of the first cold forging is 1.0 to 2.5.
4. The method according to any one of claims 1 to 3, wherein the temperature of the first heat treatment is 900-1200 ℃;
preferably, the time of the first heat treatment is 30-120 min.
5. The production method according to any one of claims 1 to 4, wherein the temperature of the second cold forging is 10 to 30 ℃;
preferably, the forging ratio of the second cold forging is 1.0 to 2.5.
6. The method according to any one of claims 1 to 5, wherein the temperature of the second heat treatment is 1000-1200 ℃;
preferably, the time of the second heat treatment is 30-120 min.
7. The method for manufacturing according to any one of claims 1 to 6, wherein the temperature of the cold rolling is 10 to 30 ℃;
preferably, the deformation amount of the cold rolling is 60-90%;
preferably, the reduction amount of each pass in the cold rolling is 0.5-5.0 mm.
8. The method according to any one of claims 1 to 7, wherein the method for preparing the tantalum target material comprises the following steps:
performing first cold forging on tantalum ingots with the purity of more than or equal to 4N at the temperature of 10-30 ℃, and controlling the forging ratio of the first cold forging to be 1.0-2.5; performing a first heat treatment at 900-; performing second cold forging at 10-30 ℃, wherein the forging ratio of the second cold forging is controlled to be 1.0-2.5; performing a second heat treatment at 1000-; and (3) cold rolling at 10-30 ℃, and controlling the reduction of 0.5-5.0mm and the deformation of 60-90% in each pass during cold rolling to obtain the tantalum target material.
9. A tantalum target obtained by the method according to any one of claims 1 to 8, wherein the tantalum target has a degree of recrystallization of 20 to 40%.
10. Use of a tantalum target according to claim 9 for sputter coating.
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| US20150211107A1 (en) * | 2012-08-16 | 2015-07-30 | Ningxia Orient Tantalum Industry Co., Ltd. | Method for preparing high-performance tantalum target |
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| CN107532287A (en) * | 2015-05-22 | 2018-01-02 | 捷客斯金属株式会社 | Tantalum spattering target and its manufacture method |
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