CN113846298B - Preparation method of terbium target blank - Google Patents
Preparation method of terbium target blank Download PDFInfo
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- CN113846298B CN113846298B CN202111133849.2A CN202111133849A CN113846298B CN 113846298 B CN113846298 B CN 113846298B CN 202111133849 A CN202111133849 A CN 202111133849A CN 113846298 B CN113846298 B CN 113846298B
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- heat treatment
- forging
- blank
- protective atmosphere
- terbium
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- GZCRRIHWUXGPOV-UHFFFAOYSA-N terbium atom Chemical compound [Tb] GZCRRIHWUXGPOV-UHFFFAOYSA-N 0.000 title claims abstract description 51
- 229910052771 Terbium Inorganic materials 0.000 title claims abstract description 50
- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- 238000010438 heat treatment Methods 0.000 claims abstract description 74
- 238000005242 forging Methods 0.000 claims abstract description 65
- 239000000463 material Substances 0.000 claims abstract description 53
- 238000005096 rolling process Methods 0.000 claims abstract description 28
- 238000000034 method Methods 0.000 claims abstract description 19
- 238000005266 casting Methods 0.000 claims abstract description 8
- 230000001681 protective effect Effects 0.000 claims description 44
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 18
- 239000007789 gas Substances 0.000 claims description 18
- 238000004321 preservation Methods 0.000 claims description 16
- 230000009467 reduction Effects 0.000 claims description 13
- 229910052757 nitrogen Inorganic materials 0.000 claims description 10
- 239000011261 inert gas Substances 0.000 claims description 9
- 238000004519 manufacturing process Methods 0.000 claims description 3
- 239000013077 target material Substances 0.000 abstract description 7
- 230000008569 process Effects 0.000 abstract description 6
- 229910052761 rare earth metal Inorganic materials 0.000 description 16
- 150000002910 rare earth metals Chemical class 0.000 description 14
- 239000000843 powder Substances 0.000 description 9
- 230000000052 comparative effect Effects 0.000 description 7
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 6
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 6
- QJVKUMXDEUEQLH-UHFFFAOYSA-N [B].[Fe].[Nd] Chemical compound [B].[Fe].[Nd] QJVKUMXDEUEQLH-UHFFFAOYSA-N 0.000 description 4
- 229910045601 alloy Inorganic materials 0.000 description 4
- 239000000956 alloy Substances 0.000 description 4
- 238000004140 cleaning Methods 0.000 description 4
- 239000010410 layer Substances 0.000 description 4
- 229910001172 neodymium magnet Inorganic materials 0.000 description 4
- 238000007747 plating Methods 0.000 description 4
- 238000011282 treatment Methods 0.000 description 4
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 3
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 3
- 229910052786 argon Inorganic materials 0.000 description 3
- 229910052802 copper Inorganic materials 0.000 description 3
- 239000010949 copper Substances 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 229910052754 neon Inorganic materials 0.000 description 3
- GKAOGPIIYCISHV-UHFFFAOYSA-N neon atom Chemical compound [Ne] GKAOGPIIYCISHV-UHFFFAOYSA-N 0.000 description 3
- 229910052759 nickel Inorganic materials 0.000 description 3
- 230000003647 oxidation Effects 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- 238000004544 sputter deposition Methods 0.000 description 3
- 239000010936 titanium Substances 0.000 description 3
- 229910052719 titanium Inorganic materials 0.000 description 3
- 238000003466 welding Methods 0.000 description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 238000003754 machining Methods 0.000 description 2
- 230000007246 mechanism Effects 0.000 description 2
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 230000008685 targeting Effects 0.000 description 2
- 229910000881 Cu alloy Inorganic materials 0.000 description 1
- 229910001279 Dy alloy Inorganic materials 0.000 description 1
- 229910052692 Dysprosium Inorganic materials 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 229910052777 Praseodymium Inorganic materials 0.000 description 1
- 229910001117 Tb alloy Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000011247 coating layer Substances 0.000 description 1
- 238000010288 cold spraying Methods 0.000 description 1
- KBQHZAAAGSGFKK-UHFFFAOYSA-N dysprosium atom Chemical compound [Dy] KBQHZAAAGSGFKK-UHFFFAOYSA-N 0.000 description 1
- 239000001307 helium Substances 0.000 description 1
- 229910052734 helium Inorganic materials 0.000 description 1
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 1
- 239000000696 magnetic material Substances 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000005240 physical vapour deposition Methods 0.000 description 1
- PUDIUYLPXJFUGB-UHFFFAOYSA-N praseodymium atom Chemical compound [Pr] PUDIUYLPXJFUGB-UHFFFAOYSA-N 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 238000005488 sandblasting Methods 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
- 229910052715 tantalum Inorganic materials 0.000 description 1
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 description 1
- 238000001291 vacuum drying 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
- 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
- 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
-
- 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
Abstract
The invention relates to a preparation method of terbium target blank, which comprises the following steps: (1) Sequentially carrying out first heat treatment and first forging on a casting blank to obtain a primary material; (2) Sequentially performing second heat treatment and second forging on the primary material obtained in the step (1) to obtain an intermediate material; (3) And (3) rolling the intermediate material obtained in the step (2) to obtain a rolled material, and then carrying out third heat treatment on the rolled material to obtain the terbium target blank. The preparation method solves the problems of poor quality and short service life of the existing prepared target material, improves the accuracy of the terbium target material in the use process, and ensures that the grain size in the obtained terbium target blank is more uniform and the grain is finer.
Description
Technical Field
The invention relates to the field of targets, in particular to a preparation method of terbium target blanks.
Background
At present, in the preparation of permanent magnetic materials such as neodymium iron boron and the like, surface terbium permeation treatment is needed to replace terbium doping in the materials so as to reduce the use amount of Tb. The purity of the terbium target used conventionally is between 99.5% and 99.99%.
The preparation method of the rotary rare earth target material for the neodymium-iron-boron permanent magnet material is disclosed in CN110983277A, and comprises the following steps: (1) Providing a cylindrical or tubular metal material as a target base pipe, and performing sand blasting on the surface of the target base pipe; (2) Providing rare earth metal powder or rare earth alloy powder with an average particle diameter D50 of 10-80 mu m, wherein the rare earth metal powder is one of dysprosium, terbium or praseodymium, the rare earth alloy powder is an alloy of dysprosium and terbium, the oxygen content of the rare earth metal powder is lower than 1500ppm, and the oxygen content of the rare earth alloy powder is lower than 1500ppm; (3) And forming a spray coating layer on the surface of the target substrate tube by cold spraying the rare earth metal powder or the rare earth alloy powder. The rotary rare earth target for the neodymium-iron-boron permanent magnet material prepared by the method improves the utilization rate of the rare earth element deposited to the target in the process of preparing the rotary rare earth target by the rare earth element, greatly reduces the production cost and improves the coercive force of the neodymium-iron-boron permanent magnet material.
As CN109352153a discloses a preparation method for forming a rare earth metal target, the rare earth metal target is formed on a targeting mechanism by means of plasma overlaying, specifically, the targeting mechanism is made into a liner tube (1), and rare earth metal powder is formed on the outer surface of the liner tube (1) by means of plasma overlaying.
However, the target prepared by the preparation method has the problems of unstable quality, poor sputtering accuracy and the like.
Disclosure of Invention
In view of the problems existing in the prior art, the invention aims to provide a preparation method of terbium target blanks, which solves the problems of poor quality and short service life of the target materials prepared at present, improves the accuracy of terbium target materials in the use process, ensures that the grain sizes in the obtained terbium target blanks are more uniform, and ensures that the grains are finer at the same time.
To achieve the purpose, the invention adopts the following technical scheme:
the invention provides a preparation method of terbium target blank, which comprises the following steps:
(1) Sequentially carrying out first heat treatment and first forging on a casting blank to obtain a primary material;
(2) Sequentially performing second heat treatment and second forging on the primary material obtained in the step (1) to obtain an intermediate material;
(3) And (3) rolling the intermediate material obtained in the step (2) to obtain a rolled material, and then carrying out third heat treatment on the rolled material to obtain the terbium target blank.
According to the preparation method provided by the invention, through adopting the specific combination of multiple deformation treatments and the heat treatment after rolling for the blank processing mode in the preparation process, the grain size of the obtained terbium target blank is ensured to have good uniformity, meanwhile, the grain size in the terbium target blank is obviously reduced, the density of the target is improved, the grain size of the grains in the obtained terbium target blank is 110-200 mu m, and the extremely difference value of the grain sizes is 10-15 mu m.
In a preferred embodiment of the present invention, the temperature of the heat treatment in the step (1) is 500 to 700 ℃, for example, 500 ℃, 510 ℃, 520 ℃, 530 ℃, 540 ℃, 550 ℃, 560 ℃, 570 ℃, 580 ℃, 590 ℃, 600 ℃, 610 ℃, 620 ℃, 630 ℃, 640 ℃, 650 ℃, 660 ℃, 670 ℃, 680 ℃, 690 ℃, 700 ℃, or the like, but the heat treatment is not limited to the values listed, and other combinations not listed in the range are equally applicable.
Preferably, the heat treatment in step (1) has a holding time of 2-4h, for example, but not limited to, 2h, 2.1h, 2.2h, 2.3h, 2.4h, 2.5h, 2.6h, 2.7h, 2.8h, 2.9h, 3h, 3.1h, 3.2h, 3.3h, 3.4h, 3.5h, 3.6h, 3.7h, 3.8h, 3.9h, or 4h, and the like, and other non-enumerated combinations within this range are equally applicable.
As a preferred embodiment of the present invention, the first forging in step (1) includes upsetting and drawing sequentially.
Preferably, the first forging in step (1) is performed 2-3 times.
In a preferred embodiment of the present invention, the temperature of the second heat treatment in the step (2) is 450 to 550 ℃, and for example, it may be 450 ℃, 460 ℃, 470 ℃, 480 ℃, 490 ℃, 500 ℃, 510 ℃, 520 ℃, 530 ℃, 540 ℃, 550 ℃, or the like, but not limited to the values recited, and other combinations not recited in the range are equally applicable.
Preferably, the second heat treatment in step (2) has a holding time of 2-4h, for example, but not limited to, 2h, 2.1h, 2.2h, 2.3h, 2.4h, 2.5h, 2.6h, 2.7h, 2.8h, 2.9h, 3h, 3.1h, 3.2h, 3.3h, 3.4h, 3.5h, 3.6h, 3.7h, 3.8h, 3.9h, or 4h, and the like, and other non-enumerated combinations within this range are equally applicable.
As a preferred embodiment of the present invention, the second forging in step (2) includes upsetting and drawing sequentially.
Preferably, the second forging in step (2) is performed 2-3 times.
In a preferred embodiment of the present invention, the reduction amount of the initial rolling in the step (3) is 20 to 30%, for example, 20%, 21%, 22%, 23%, 24%, 25%, 26%, 27%, 28%, 29% or 30%, etc., but the present invention is not limited to the above-mentioned values, and other combinations not mentioned in the above-mentioned ranges are equally applicable. The reduction is reduced every time until the reduction of the last time is 0, namely, the reduction of 1%, 2%, 3%, 4% or 5% and the like can be reduced in sequence, the humidity of the area is controlled in the rolling process, the humidity is controlled below 60%, and the terbium target oxidation is slowed down.
In a preferred embodiment of the present invention, the temperature of the third heat treatment in the step (3) is 100 to 200 ℃, for example, 100 ℃, 105 ℃, 110 ℃, 115 ℃, 120 ℃, 125 ℃, 130 ℃, 135 ℃, 140 ℃, 145 ℃, 150 ℃, 155 ℃, 160 ℃, 165 ℃, 170 ℃, 175 ℃, 180 ℃, 185 ℃, 190 ℃, 195 ℃, 200 ℃, or the like, but the temperature is not limited to the values recited, and other combinations not recited in the range are equally applicable.
Preferably, the third heat treatment in step (3) has a holding time of 0.5-2h, for example, 0.5h, 0.6h, 0.7h, 0.8h, 0.9h, 1h, 1.1h, 1.2h, 1.3h, 1.4h, 1.5h, 1.6h, 1.7h, 1.8h, 1.9h or 2h, and the like, but not limited to the recited values, and other non-recited combinations within this range are equally applicable.
As a preferred embodiment of the present invention, the first forging in step (1) is preferably performed under a protective atmosphere, and the protective gas in the protective atmosphere includes nitrogen and/or inert gas.
As a preferred technical scheme of the invention, the second forging in the step (2) is performed under a protective atmosphere;
preferably, the protective gas in the protective atmosphere comprises nitrogen and/or inert gas.
In the invention, the upsetting end point is stopped when the upsetting end point is 30-50% of the height of the upsetting blank, the drawing end point is stopped when the drawing end point is 1.5-3 times of the height of the blank, and the next round of forging and stretching is started.
In the present invention, the inert gas may be helium, neon, argon, or the like.
In the invention, the processed target blank is used as a target material to be welded with a copper-containing backboard after being machined, the copper-containing backboard can be a copper backboard or a copper alloy backboard, the welding surface of the processed terbium target material can be selectively subjected to plating treatment before welding, and the plating can be a titanium layer or a nickel layer so as to reduce or reduce oxidation and increase binding and bonding strength. The surface treatment can select a PVD sputtering titanium plating or nickel plating mode, so that a titanium layer or a nickel layer with the thickness of 5-10um is added on the surface, and the binding surface is effectively placed to oxidize and bind poorly. The surface can also be electrochemically nickel-plated by means of anodic oxidation.
And (5) machining the terbium target assembly obtained by welding, and cleaning, drying and packaging in a dust-free room after machining. In the cleaning process, contact with water is avoided, and organic solvents such as alcohol and the like can be adopted for cleaning. Drying in a vacuum drying oven at 70-100deg.C for 30-60min after cleaning.
As a preferable technical scheme of the invention, the preparation method comprises the following steps:
(1) Sequentially carrying out first heat treatment and first forging on a casting blank to obtain a primary material; the temperature of the heat treatment is 500-700 ℃; the heat preservation time of the heat treatment is 2-4h; the first forging and extending comprises upsetting and drawing which are sequentially carried out; the first forging is carried out for 2-3 times; the first forging and stretching are carried out under a protective atmosphere; the protective gas in the protective atmosphere comprises nitrogen and/or inert gas;
(2) Sequentially performing second heat treatment and second forging on the primary material obtained in the step (1) to obtain an intermediate material; the temperature of the second heat treatment is 450-550 ℃; the heat preservation time of the second heat treatment is 2-4h; the second forging and stretching comprises upsetting and drawing which are sequentially carried out; the second forging is carried out for 2-3 times; the second forging and stretching are carried out under a protective atmosphere; the protective gas in the protective atmosphere comprises nitrogen and/or inert gas;
(3) Rolling the intermediate material obtained in the step (2) to obtain a rolled material, and then carrying out third heat treatment on the rolled material to obtain the terbium target blank; the rolling reduction of the initial rolling in the rolling is 20-30%; the temperature of the third heat treatment is 100-200 ℃; the heat preservation time of the third heat treatment is 0.5-2h.
Compared with the prior art, the invention has at least the following beneficial effects:
(1) According to the preparation method provided by the invention, through adopting the specific combination of multiple deformation treatments and the heat treatment after rolling for the blank processing mode in the preparation process, the grain size of the obtained terbium target blank is ensured to have good uniformity, meanwhile, the grain size in the terbium target blank is obviously reduced, the density of the target is improved, the grain size of the grains in the obtained terbium target blank is 110-200 mu m, and the extremely difference value of the grain sizes is 10-15 mu m.
(2) After the terbium target blank is welded and bound with the backboard, the sputtering process can be accurately controlled, the service life of the terbium target assembly is obviously prolonged by 10-20% compared with the prior art, and the terbium target utilization rate is improved by 10-20% compared with the prior art.
Detailed Description
For a better illustration of the present invention, which is convenient for understanding the technical solution of the present invention, exemplary but non-limiting examples of the present invention are as follows:
example 1
The embodiment provides a preparation method of terbium target blank, which comprises the following steps:
(1) Sequentially carrying out first heat treatment and first forging on a casting blank to obtain a primary material; the temperature of the heat treatment is 600 ℃; the heat preservation time of the heat treatment is 3 hours; the first forging and extending comprises upsetting and drawing which are sequentially carried out; the first forging is carried out for 2 times; the first forging and stretching are carried out under a protective atmosphere; the protective gas in the protective atmosphere is nitrogen; the upsetting end point is stopped when the upsetting blank height is 40%, the drawing end point is stopped when the drawing end point is 2 times of the blank height, and the next round of forging and stretching is started;
(2) Sequentially performing second heat treatment and second forging on the primary material obtained in the step (1) to obtain an intermediate material; the temperature of the second heat treatment is 500 ℃; the heat preservation time of the second heat treatment is 2-4h; the second forging and stretching comprises upsetting and drawing which are sequentially carried out; the second forging is carried out for 3 times; the second forging and stretching are carried out under a protective atmosphere; the protective gas in the protective atmosphere is argon; the upsetting end point is stopped when the upsetting height is 50% of the upsetting blank height, the drawing end point is stopped when the drawing height is 3 times of the blank height, and the next round of forging and stretching is started;
(3) Rolling the intermediate material obtained in the step (2) to obtain a rolled material, and then carrying out third heat treatment on the rolled material to obtain the terbium target blank; the reduction of initial rolling in the rolling is 25%, and the reduction of each pass is reduced by 5%; the temperature of the third heat treatment is 150 ℃; the heat preservation time of the third heat treatment is 1.2h.
The properties of the terbium target blank obtained are detailed in table 1.
Example 2
The embodiment provides a preparation method of terbium target blank, which comprises the following steps:
(1) Sequentially carrying out first heat treatment and first forging on a casting blank to obtain a primary material; the temperature of the heat treatment is 500 ℃; the heat preservation time of the heat treatment is 4 hours; the first forging and extending comprises upsetting and drawing which are sequentially carried out; the first forging is performed 3 times; the first forging and stretching are carried out under a protective atmosphere; the protective gas in the protective atmosphere is argon; the upsetting end point is stopped when the upsetting height is 30% of the upsetting blank height, the drawing end point is stopped when the drawing height is 2 times of the blank height, and the next round of forging and stretching is started;
(2) Sequentially performing second heat treatment and second forging on the primary material obtained in the step (1) to obtain an intermediate material; the temperature of the second heat treatment is 550 ℃; the heat preservation time of the second heat treatment is 2h; the second forging and stretching comprises upsetting and drawing which are sequentially carried out; the second forging is carried out for 2 times; the second forging and stretching are carried out under a protective atmosphere; the protective gas in the protective atmosphere is nitrogen; the upsetting end point is stopped when the upsetting blank height is 45%, the drawing end point is stopped when the drawing end point is 1 time of the blank height, and the next round of forging and stretching is started; (3) Rolling the intermediate material obtained in the step (2) to obtain a rolled material, and then carrying out third heat treatment on the rolled material to obtain the terbium target blank; the reduction of initial rolling in the rolling is 20%, and the reduction of each pass is reduced by 2%; the temperature of the third heat treatment is 100 ℃; the heat preservation time of the third heat treatment is 2h.
The properties of the terbium target blank obtained are detailed in table 1.
Example 3
The embodiment provides a preparation method of terbium target blank, which comprises the following steps:
(1) Sequentially carrying out first heat treatment and first forging on a casting blank to obtain a primary material; the temperature of the heat treatment is 700 ℃; the heat preservation time of the heat treatment is 2 hours; the first forging and extending comprises upsetting and drawing which are sequentially carried out; the first forging is carried out for 2 times; the first forging and stretching are carried out under a protective atmosphere; the protective gas in the protective atmosphere is a mixed gas of nitrogen and neon; the upsetting end point is stopped when the upsetting blank height is 30%, the drawing end point is stopped when the drawing end point is 1.5 times of the blank height, and the next round of forging and stretching is started;
(2) Sequentially performing second heat treatment and second forging on the primary material obtained in the step (1) to obtain an intermediate material; the temperature of the second heat treatment is 450 ℃; the heat preservation time of the second heat treatment is 4 hours; the second forging and stretching comprises upsetting and drawing which are sequentially carried out; the second forging is carried out for 2 times; the second forging and stretching are carried out under a protective atmosphere; the protective gas in the protective atmosphere is a mixed gas of nitrogen and neon; the upsetting end point is stopped when the upsetting blank height is 32%, the drawing end point is stopped when the drawing end point is 1.7 times of the blank height, and the next round of forging and stretching is started;
(3) Rolling the intermediate material obtained in the step (2) to obtain a rolled material, and then carrying out third heat treatment on the rolled material to obtain the terbium target blank; the reduction of initial rolling in the rolling is 30%, and the reduction of each pass is reduced by 6%; the temperature of the third heat treatment is 200 ℃; the heat preservation time of the third heat treatment is 0.5h.
The properties of the terbium target blank obtained are detailed in table 1.
Comparative example 1
The only difference from example 1 is that the third heat treatment was moved to before the first heat treatment, and the properties of the obtained terbium target blank are detailed in table 1.
Comparative example 2
The difference from comparative example 1 was only that the temperature of the third heat treatment was adjusted to 900℃and the properties of the resultant terbium target blank were shown in Table 1.
Comparative example 3
The only difference from example 1 is that no third heat treatment is performed after rolling, and the properties of the obtained terbium target blank are shown in Table 1.
Comparative example 4
The only difference from example 1 is that the first forging and the second forging were replaced by rolling, and the properties of the obtained terbium target blank are shown in Table 1.
Comparative example 5
The difference from example 1 is only that the material of the cast ingot is changed to tantalum, and the properties of the obtained terbium target ingot are shown in Table 1.
TABLE 1
As can be seen from the results of the above examples and comparative examples, the preparation method provided by the present invention ensures that the grain size of the terbium target blank has good uniformity by the specific design of the deformation process in the preparation process and the specific heat treatment after rolling, and at the same time, the grain size of the terbium target blank is significantly reduced, the density of the target is improved, the grain size of the terbium target blank is 100-200 μm, and the extremely poor grain size is 10-15 μm. The density of the obtained target blank can reach more than 98 percent.
The applicant states that the detailed structural features of the present invention are described by the above embodiments, but the present invention is not limited to the above detailed structural features, i.e. it does not mean that the present invention must be implemented depending on the above detailed structural features. It should be apparent to those skilled in the art that any modifications of the present invention, equivalent substitutions of selected components of the present invention, addition of auxiliary components, selection of specific modes, etc., are within the scope of the present invention and the scope of the disclosure.
The preferred embodiments of the present invention have been described in detail above, but the present invention is not limited to the specific details of the above embodiments, and various simple modifications can be made to the technical solution of the present invention within the scope of the technical concept of the present invention, and all the simple modifications belong to the protection scope of the present invention.
In addition, the specific features described in the above embodiments may be combined in any suitable manner, and in order to avoid unnecessary repetition, various possible combinations are not described further.
Moreover, any combination of the various embodiments of the invention can be made without departing from the spirit of the invention, which should also be considered as disclosed herein.
Claims (15)
1. A method for preparing a terbium target blank, comprising the steps of:
(1) Sequentially carrying out first heat treatment and first forging on a casting blank to obtain a primary material;
(2) Sequentially performing second heat treatment and second forging on the primary material obtained in the step (1) to obtain an intermediate material;
(3) Rolling the intermediate material obtained in the step (2) to obtain a rolled material, and then carrying out third heat treatment on the rolled material to obtain a terbium target blank;
the temperature of the first heat treatment in the step (1) is 500-700 ℃; the temperature of the second heat treatment in the step (2) is 450-550 ℃; the temperature of the third heat treatment in the step (3) is 100-200 ℃; the heat preservation time of the third heat treatment is 0.5-2h;
the grain size of the obtained terbium target blank is 110-200 mu m, and the difference of the grain sizes is 10-15 mu m.
2. The method of claim 1, wherein the heat treatment in step (1) is carried out for a period of 2 to 4 hours.
3. The method of making as defined in claim 1 wherein said first forging in step (1) includes sequentially upsetting and drawing.
4. The method of claim 1, wherein the first stretching in step (1) is performed 2-3 times.
5. The method of claim 1, wherein the second heat treatment in step (2) is performed for a holding time of 2 to 4 hours.
6. The method of making as defined in claim 1 wherein said second forging in step (2) includes sequentially upsetting and drawing.
7. The method of claim 1, wherein the second stretching in step (2) is performed 2-3 times.
8. The method according to claim 1, wherein the reduction of the initial rolling in the step (3) is 20 to 30%.
9. The method of claim 1, wherein the first forging in step (1) is performed under a protective atmosphere.
10. The method of claim 9, wherein the shielding gas in the protective atmosphere comprises an inert gas.
11. The method of claim 9, wherein the protective gas in the protective atmosphere comprises nitrogen.
12. The method of claim 1, wherein the second forging in step (2) is performed under a protective atmosphere.
13. The method of claim 12, wherein the shielding gas in the protective atmosphere comprises an inert gas.
14. The method of claim 12, wherein the protective gas in the protective atmosphere comprises nitrogen.
15. The preparation method according to any one of claims 1 to 14, characterized in that the preparation method comprises the steps of:
(1) Sequentially carrying out first heat treatment and first forging on a casting blank to obtain a primary material; the temperature of the heat treatment is 500-700 ℃; the heat preservation time of the heat treatment is 2-4h; the first forging and extending comprises upsetting and drawing which are sequentially carried out; the first forging is carried out for 2-3 times; the first forging and stretching are carried out under a protective atmosphere; the protective gas in the protective atmosphere comprises inert gas;
(2) Sequentially performing second heat treatment and second forging on the primary material obtained in the step (1) to obtain an intermediate material; the temperature of the second heat treatment is 450-550 ℃; the heat preservation time of the second heat treatment is 2-4h; the second forging and stretching comprises upsetting and drawing which are sequentially carried out; the second forging is carried out for 2-3 times; the second forging and stretching are carried out under a protective atmosphere; the protective gas in the protective atmosphere comprises inert gas;
(3) Rolling the intermediate material obtained in the step (2) to obtain a rolled material, and then carrying out third heat treatment on the rolled material to obtain the terbium target blank; the rolling reduction of the initial rolling in the rolling is 20-30%; the temperature of the third heat treatment is 100-200 ℃; the heat preservation time of the third heat treatment is 0.5-2h.
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2003277899A (en) * | 2002-03-25 | 2003-10-02 | Kurimoto Ltd | Magnesium alloy member and its production method |
| WO2010110134A1 (en) * | 2009-03-27 | 2010-09-30 | 日鉱金属株式会社 | Lanthanum target for sputtering |
| CN102378825A (en) * | 2009-03-31 | 2012-03-14 | 吉坤日矿日石金属株式会社 | Lanthanum target for sputtering |
| WO2014026639A1 (en) * | 2012-08-16 | 2014-02-20 | 宁夏东方钽业股份有限公司 | Method for preparing high-performance tantalum target |
| CN104451567A (en) * | 2014-12-29 | 2015-03-25 | 宁夏东方钽业股份有限公司 | Tantalum target and manufacturing method thereof |
| CN106637100A (en) * | 2015-10-30 | 2017-05-10 | 有研稀土新材料股份有限公司 | Rare-earth metal target material and preparation method thereof |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP4974362B2 (en) * | 2006-04-13 | 2012-07-11 | 株式会社アルバック | Ta sputtering target and manufacturing method thereof |
| JP5828350B2 (en) * | 2014-04-11 | 2015-12-02 | 三菱マテリアル株式会社 | Manufacturing method of material for cylindrical sputtering target |
-
2021
- 2021-09-27 CN CN202111133849.2A patent/CN113846298B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2003277899A (en) * | 2002-03-25 | 2003-10-02 | Kurimoto Ltd | Magnesium alloy member and its production method |
| WO2010110134A1 (en) * | 2009-03-27 | 2010-09-30 | 日鉱金属株式会社 | Lanthanum target for sputtering |
| CN102356180A (en) * | 2009-03-27 | 2012-02-15 | 吉坤日矿日石金属株式会社 | Lanthanum target for sputtering |
| CN102378825A (en) * | 2009-03-31 | 2012-03-14 | 吉坤日矿日石金属株式会社 | Lanthanum target for sputtering |
| WO2014026639A1 (en) * | 2012-08-16 | 2014-02-20 | 宁夏东方钽业股份有限公司 | Method for preparing high-performance tantalum target |
| CN104451567A (en) * | 2014-12-29 | 2015-03-25 | 宁夏东方钽业股份有限公司 | Tantalum target and manufacturing method thereof |
| CN106637100A (en) * | 2015-10-30 | 2017-05-10 | 有研稀土新材料股份有限公司 | Rare-earth metal target material and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 廖映华.机械制造实践.西南交通大学出版社,2009,53. * |
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