CN115488333B - Molybdenum-titanium alloy tube target and preparation method and application thereof - Google Patents
Molybdenum-titanium alloy tube target and preparation method and application thereof Download PDFInfo
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- CN115488333B CN115488333B CN202211184419.8A CN202211184419A CN115488333B CN 115488333 B CN115488333 B CN 115488333B CN 202211184419 A CN202211184419 A CN 202211184419A CN 115488333 B CN115488333 B CN 115488333B
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- 229910001069 Ti alloy Inorganic materials 0.000 title claims abstract description 160
- ZPZCREMGFMRIRR-UHFFFAOYSA-N molybdenum titanium Chemical compound [Ti].[Mo] ZPZCREMGFMRIRR-UHFFFAOYSA-N 0.000 title claims abstract description 157
- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- 238000005245 sintering Methods 0.000 claims abstract description 44
- 238000003466 welding Methods 0.000 claims abstract description 39
- 238000001513 hot isostatic pressing Methods 0.000 claims abstract description 36
- 238000002156 mixing Methods 0.000 claims abstract description 29
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 27
- 238000003754 machining Methods 0.000 claims abstract description 26
- 238000003825 pressing Methods 0.000 claims abstract description 26
- 238000010438 heat treatment Methods 0.000 claims abstract description 25
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims abstract description 24
- 238000011049 filling Methods 0.000 claims abstract description 15
- 238000005219 brazing Methods 0.000 claims abstract description 14
- 238000007872 degassing Methods 0.000 claims abstract description 14
- 238000007493 shaping process Methods 0.000 claims abstract description 11
- 239000000203 mixture Substances 0.000 claims abstract description 5
- 238000000034 method Methods 0.000 claims description 50
- 239000010935 stainless steel Substances 0.000 claims description 30
- 229910001220 stainless steel Inorganic materials 0.000 claims description 30
- 239000011812 mixed powder Substances 0.000 claims description 13
- 239000010936 titanium Substances 0.000 claims description 13
- 229910052719 titanium Inorganic materials 0.000 claims description 13
- 238000005488 sandblasting Methods 0.000 claims description 12
- 238000007789 sealing Methods 0.000 claims description 12
- 229910001209 Low-carbon steel Inorganic materials 0.000 claims description 10
- 239000012300 argon atmosphere Substances 0.000 claims description 10
- 229910000679 solder Inorganic materials 0.000 claims description 9
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims description 7
- 229910052738 indium Inorganic materials 0.000 claims description 7
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 claims description 7
- 229910052726 zirconium Inorganic materials 0.000 claims description 7
- 238000004519 manufacturing process Methods 0.000 claims description 4
- 239000002245 particle Substances 0.000 claims description 4
- 239000008188 pellet Substances 0.000 claims description 2
- 238000000465 moulding Methods 0.000 claims 1
- 229920002635 polyurethane Polymers 0.000 claims 1
- 239000004814 polyurethane Substances 0.000 claims 1
- 230000000052 comparative effect Effects 0.000 description 11
- 238000005336 cracking Methods 0.000 description 8
- 229910052750 molybdenum Inorganic materials 0.000 description 8
- 239000011733 molybdenum Substances 0.000 description 8
- 229920003225 polyurethane elastomer Polymers 0.000 description 7
- 239000000843 powder Substances 0.000 description 6
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 239000001301 oxygen Substances 0.000 description 4
- 229910052760 oxygen Inorganic materials 0.000 description 4
- 239000011248 coating agent Substances 0.000 description 3
- 238000000576 coating method Methods 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 230000007547 defect Effects 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 239000013077 target material Substances 0.000 description 3
- 238000007751 thermal spraying Methods 0.000 description 3
- 230000002411 adverse Effects 0.000 description 2
- 229910045601 alloy Inorganic materials 0.000 description 2
- 239000000956 alloy Substances 0.000 description 2
- 239000011230 binding agent Substances 0.000 description 2
- 238000003490 calendering Methods 0.000 description 2
- 238000005266 casting Methods 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000005242 forging Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 238000001755 magnetron sputter deposition Methods 0.000 description 2
- 238000004663 powder metallurgy Methods 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- UKGJZDSUJSPAJL-YPUOHESYSA-N (e)-n-[(1r)-1-[3,5-difluoro-4-(methanesulfonamido)phenyl]ethyl]-3-[2-propyl-6-(trifluoromethyl)pyridin-3-yl]prop-2-enamide Chemical compound CCCC1=NC(C(F)(F)F)=CC=C1\C=C\C(=O)N[C@H](C)C1=CC(F)=C(NS(C)(=O)=O)C(F)=C1 UKGJZDSUJSPAJL-YPUOHESYSA-N 0.000 description 1
- 229910000997 High-speed steel Inorganic materials 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 229910001182 Mo alloy Inorganic materials 0.000 description 1
- 238000000137 annealing Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 239000008199 coating composition Substances 0.000 description 1
- 238000009694 cold isostatic pressing Methods 0.000 description 1
- 238000005056 compaction Methods 0.000 description 1
- 238000001739 density measurement Methods 0.000 description 1
- 229920001971 elastomer Polymers 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 239000004973 liquid crystal related substance Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 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
- 230000000149 penetrating effect Effects 0.000 description 1
- 230000035515 penetration Effects 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000001953 recrystallisation Methods 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 238000005476 soldering Methods 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
- 239000010421 standard material Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 229910052718 tin Inorganic materials 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/02—Compacting only
- B22F3/03—Press-moulding apparatus therefor
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
- B22F3/1003—Use of special medium during sintering, e.g. sintering aid
- B22F3/1007—Atmosphere
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/12—Both compacting and sintering
- B22F3/14—Both compacting and sintering simultaneously
- B22F3/15—Hot isostatic pressing
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/24—After-treatment of workpieces or articles
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/24—After-treatment of workpieces or articles
- B22F2003/248—Thermal after-treatment
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- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Mechanical Engineering (AREA)
- Powder Metallurgy (AREA)
Abstract
The invention relates to a molybdenum-titanium alloy tube target and a preparation method and application thereof, wherein the preparation method comprises the following steps: (1) Sequentially mixing molybdenum powder and titanium powder, filling the mixture into a mold, carrying out cold pressing treatment, demolding, vacuum sintering and shaping to obtain a molybdenum-titanium alloy tube blank; (2) The molybdenum-titanium alloy tube blank obtained in the step (1) is subjected to sheath welding, degassing treatment, hot isostatic pressing splicing treatment, heat treatment and first machining to obtain a molybdenum-titanium alloy tube; (3) And (3) brazing the back tube and the molybdenum-titanium alloy tube obtained in the step (2) and carrying out second machining to obtain the molybdenum-titanium alloy tube target. According to the invention, the deformation of the tube blank is reduced by cold pressing and vacuum sintering, the large-size molybdenum-titanium alloy tube can be obtained by hot isostatic pressing splicing treatment, the internal stress is removed by heat treatment, and reasonable technological parameters are matched, so that the obtained molybdenum-titanium alloy tube target has high density, uniform internal tissue structure and fine grains, and can be used in the field of panel display.
Description
Technical Field
The invention belongs to the technical field of magnetron sputtering coating, relates to a tube target, a preparation method and application thereof, and in particular relates to a molybdenum-titanium alloy tube target, a preparation method and application thereof.
Background
The targets are mainly divided into a planar target and a tubular target, and compared with the planar target, the tubular target has the characteristics of high utilization rate, uniform coating composition and the like, and is a standard material in the magnetron sputtering coating technology. In the field of panel display, the size requirements for targets with molybdenum and molybdenum alloy as cores are gradually increased, and the welding combination rate and plane requirements for the targets are higher.
The main tube target production methods at present are a thermal spraying method, a casting method and a powder metallurgy method. The thermal spraying method is to spray the metal powder on the workpiece by adopting a plasma thermal spraying mode, and the pipe target prepared by the method has low density, nonuniform structure, a large number of holes and high oxygen content, and can only be used in coating industries with low requirements such as glass; the casting method is to directly cast the target material onto the liner tube, but can only be used for the target material with lower melting points such as Sn, zn and the like; the tube target prepared by the powder metallurgy method has uniform components, fine grains and high purity, and can meet the requirements of liquid crystal display and touch screen industries.
CN 100566921a discloses a method for preparing a high-density molybdenum tube, after isostatic compaction of molybdenum powder, sintering under the protection of hydrogen to prepare a circular molybdenum tube blank, forging, extruding, annealing, and then machining, cleaning and drying to obtain the high-density molybdenum tube. The molybdenum tube prepared by the method has higher density, but is easy to crack during forging and has lower material utilization rate.
CN 111304607a discloses a method for manufacturing molybdenum-titanium alloy target, which comprises the following steps: mixing molybdenum powder and titanium powder under the protection of inert gas; cold isostatic pressing of the mixed powder; performing pressure sintering on the formed molybdenum-titanium mixed powder to obtain a molybdenum-titanium ingot; calendering the molybdenum-titanium ingot to reach the required size; and performing heat treatment on the molybdenum-titanium plate after the rolling to form a recrystallization structure required by target sputtering, thereby obtaining the target plate. The molybdenum-titanium alloy target provided by the invention can be not limited by the size of equipment, but the calendaring process has higher cost and is not suitable for large-scale production, and meanwhile, the material utilization rate is lower.
CN 101642813a discloses a method for preparing molybdenum tube, which comprises mixing raw material molybdenum powder with water-based binder solution uniformly, centrifuging, drying, degumming, presintering, sintering at high temperature, and polishing; a molybdenum tube was obtained. The molybdenum tube prepared by the method has lower density, reduces the purity of the material due to the introduction of the binder, and increases the oxygen content.
Aiming at the defects of the prior art, a molybdenum-titanium alloy tube target with higher density, fine grains and high material utilization rate is needed to be provided.
Disclosure of Invention
The invention aims to provide a molybdenum-titanium alloy tube target, a preparation method and application thereof, wherein the molybdenum-titanium alloy tube target with a large size of more than 3000mm is obtained by combining cold pressing and pressureless vacuum sintering, and the obtained small-section molybdenum-titanium alloy tube is subjected to hot isostatic pressing splicing treatment, and has the advantages of low deformation, no cracking phenomenon, higher density and fine grains.
In order to achieve the aim of the invention, the invention adopts the following technical scheme:
in a first aspect, the present invention provides a method for preparing a molybdenum-titanium alloy tube target, the method comprising the steps of:
(1) Sequentially mixing molybdenum powder and titanium powder, filling the mixture into a mold, carrying out cold pressing treatment, demolding, vacuum sintering and shaping to obtain a molybdenum-titanium alloy tube blank;
(2) The molybdenum-titanium alloy tube blank obtained in the step (1) is subjected to sheath welding, degassing treatment, hot isostatic pressing splicing treatment, heat treatment and first machining to obtain a molybdenum-titanium alloy tube;
(3) And (3) brazing the back tube and the molybdenum-titanium alloy tube obtained in the step (2) and carrying out second machining to obtain the molybdenum-titanium alloy tube target.
The preparation method provided by the invention combines cold pressing and vacuum sintering, so that the problem of large deformation of the tube blank in the forming process can be effectively reduced; further carrying out hot isostatic pressing splicing treatment on the small-section molybdenum-titanium alloy tube blank after vacuum sintering to obtain a large-size molybdenum-titanium alloy tube with the diameter of more than 3000 mm; internal stress is removed through heat treatment, so that the problem of cracking of a pipe target caused by stress release in a machining process can be solved; meanwhile, reasonable technological parameters are matched, the obtained molybdenum-titanium alloy tube target is high in density, uniform in internal tissue structure and fine in crystal grains, and the technical requirements of panel display can be met.
Preferably, the particle size of the molybdenum powder in step (1) is in the range of 3-5. Mu.m, for example, 3 μm, 3.5 μm, 4 μm, 4.5 μm or 5 μm, but not limited to the values recited, other values not recited in the range of values are equally applicable.
Preferably, the particle size of the titanium powder in step (1) is in the range of 20-50. Mu.m, for example 20 μm, 25 μm, 30 μm, 40 μm or 50. Mu.m, but not limited to the values recited, other values not recited in the range of values being equally applicable.
Preferably, the titanium content of the mixed powder obtained in the step (1) is 10-75wt%, for example, 10wt%, 25wt%, 40wt%, 60wt% or 75wt%, but is not limited to the recited values, and other non-recited values in the range of values are equally applicable.
Preferably, the mixed medium of step (1) comprises zirconium spheres and/or titanium spheres.
Preferably, the mass ratio of the mixed pellets in the step (1) is (0.5-1.75): 1, for example, 0.5:1, 0.75:1, 1:1, 1.25:1, 1.5:1 or 1.75:1, but not limited to the recited values, and other non-recited values in the range of values are equally applicable.
Preferably, the mixing time in step (1) is 12-48 hours, for example, 12 hours, 18 hours, 26 hours, 36 hours or 48 hours, but not limited to the recited values, and other non-recited values in the range of values are equally applicable.
Preferably, the mixing of step (1) is performed in an argon atmosphere.
The mixing is carried out in an argon atmosphere, so that the titanium powder and the molybdenum powder can be effectively prevented from being oxidized, and the purity of the finished product is reduced.
Preferably, the mold used for the mold filling in the step (1) comprises a polyurethane rubber sleeve.
The mould used for die filling adopts a polyurethane rubber sleeve, so that the adhesion with mixed powder can be avoided, and the die is easier to demould.
Preferably, the inner core of the die used for die filling in the step (1) comprises a chrome-plated high-speed steel tube.
Preferably, the step (1) further comprises the step of cleaning and drying the mold before the mold is assembled.
Preferably, the die filling in the step (1) is performed on a vibrating platform, and two ends of a die used for die filling are sealed by rubber plugs.
Preferably, the pressure of the cold pressing treatment in the step (1) is 200-300MPa, for example, 200MPa, 220MPa, 250MPa, 255MPa, 270MPa, 290MPa or 300MPa, but not limited to the values listed, and other values not listed in the numerical range are equally applicable, preferably 255-290MPa.
The pressure of the cold pressing treatment is in a reasonable range, the mixed powder can be preliminarily provided with a certain density, the follow-up vacuum sintering and hot isostatic pressing splicing treatment is facilitated, and the excessive or insufficient pressure brings adverse effects to the density of the molybdenum-titanium alloy tube target.
Preferably, the cold pressing treatment in step (1) is performed for a period of time ranging from 5 to 40min, for example, from 5min, 10min, 20min, 30min or 40min, but not limited to the values recited, and other values not recited in the range of values are equally applicable, preferably from 20 to 30min.
Preferably, the temperature of the vacuum sintering in step (1) is 1200-1950 ℃, such as 1200 ℃, 1400 ℃, 1500 ℃, 1800 ℃ or 1950 ℃, but not limited to the values listed, and other values not listed in the range are equally applicable, preferably 1400-1500 ℃.
The high temperature of the vacuum sintering can lead to the growth of alloy grains, and the high hardness is unfavorable for the subsequent machining; too low a temperature can reduce the density of the target.
Preferably, the time of vacuum sintering in step (1) is 5-10h, for example, 5h, 6h, 7h, 8h, 9h or 10h, but not limited to the recited values, and other non-recited values in the range of values are equally applicable.
Preferably, the vacuum degree of the vacuum sintering in the step (1) is less than 5 multiplied by 10 -3 Pa may be, for example, 4.5X10 -3 Pa、4×10 -3 Pa、3.5×10 -3 Pa、3×10 -3 Pa or 2X 10 -3 Pa, but not limited to the recited values, other non-recited values within the range of values are equally applicable.
The invention combines cold pressing and vacuum sintering, and can reduce the deformation of one-step forming by step forming, and can control the gas content of the target material, thereby reducing the deformation of the tube blank in the forming process.
Preferably, the shaping in the step (1) is carried out to ensure that the pipe diameters of the obtained molybdenum-titanium alloy pipe blanks of all sections are consistent.
Preferably, the outer sheath used in the sheath welding and sealing in the step (2) is a stainless steel pipe and/or a low carbon steel pipe with the contact surface of the molybdenum-titanium alloy pipe blank subjected to sand blasting treatment.
Preferably, in the step (2), the inner sheath used for the sheath welding seal is a stainless steel pipe and/or a low carbon steel pipe with the contact surface of the molybdenum-titanium alloy pipe blank subjected to sand blasting treatment.
The sand blasting can remove an oxide layer on the surface of the sheath, which is difficult to clean, so that the introduction of impurities in the sintering process of the target is reduced, and the purity of the target is further ensured.
Preferably, the thickness of the inner sheath is 5-12mm, for example, 5mm, 6mm, 8mm, 10mm or 12mm, but is not limited to the recited values, and other non-recited values within the range of values are equally applicable. .
Preferably, the step of envelope sealing in step (2) comprises: and coaxially welding the inner sheath and the outer sheath on the stainless steel bottom plate to form an annular cavity, stacking the molybdenum-titanium alloy tube blanks in the annular cavity, and then welding the stainless steel cover plate at the other ends of the inner sheath and the outer sheath.
Preferably, the temperature of the degassing treatment in step (2) is 500-750 ℃, for example 500 ℃, 550 ℃, 600 ℃, 700 ℃ or 750 ℃, but not limited to the values listed, and other values not listed in the range of values are equally applicable.
The deaeration treatment has a larger influence on the oxygen content of the molybdenum-titanium alloy tube target, and the higher the deaeration treatment temperature is, the lower the oxygen content in the final product is.
Preferably, the degassing treatment in step (2) is terminated by a vacuum level of < 5X 10 -3 Pa may be, for example, 4.5X10 -3 Pa、4×10 -3 Pa、3.5×10 -3 Pa、3×10 -3 Pa or 2X 10 -3 Pa, but not limited to the recited values, other non-recited values within the range of values are equally applicable.
Preferably, the temperature of the hot isostatic pressing splicing treatment in the step (2) is 1000-1500 ℃, for example, 1000 ℃, 1100 ℃, 1200 ℃, 1300 ℃, 1350 ℃, 1380 ℃, 1400 ℃, 1450 ℃, or 1500 ℃, but not limited to the values listed, other values not listed in the numerical range are applicable as well, and preferably 1380-1450 ℃.
The temperature of the hot isostatic pressing splicing treatment is too low, the molybdenum-titanium alloy tube blanks cannot be tightly spliced, the structure of the sheath can be damaged due to the too high temperature, and the sheath is easy to deform or crack.
Preferably, the pressure of the hot isostatic pressing splicing treatment in the step (2) is 150-200MPa, for example, 150MPa, 160MPa, 170MPa, 180MPa, 190MPa or 200MPa, but not limited to the values listed, and other values not listed in the numerical range are equally applicable, preferably 160-190MPa.
The pressure of the hot isostatic pressing splicing treatment is too low, and equal and enough stress cannot be applied to the sheath in all directions to form the molybdenum-titanium alloy tube blank; the compactness of the molybdenum-titanium alloy tube blank is not increased any more due to the excessively high pressure, but the sheath is deformed or cracked, and the energy loss is increased.
Preferably, the heat-preserving and pressure-maintaining time of the hot isostatic pressing splicing treatment in the step (2) is 6-9h, for example, 6h, 6.5h, 7h, 8h or 9h, but is not limited to the recited values, and other non-recited values in the numerical range are equally applicable, preferably 8-9h.
Preferably, after the hot isostatic pressing splicing treatment and before the heat treatment, the stainless steel bottom plate and the stainless steel cover plate in the step (2) are removed.
Preferably, the temperature of the heat treatment in step (2) is 350-650 ℃, for example, 350 ℃, 400 ℃, 450 ℃, 500 ℃, 550 ℃, 600 ℃ or 650 ℃, but not limited to the recited values, other non-recited values within the range of values are equally applicable, preferably 400-550 ℃.
Preferably, the time of the heat treatment in step (2) is 1-2h, for example, 1h, 1.2h, 1.5h, 1.8h or 2h, but not limited to the recited values, and other non-recited values in the range of values are equally applicable.
Preferably, the heat treatment in step (2) is followed by air cooling to room temperature.
The heat treatment can effectively remove the internal stress of the molybdenum-titanium alloy tube blank, thereby solving the problem that the molybdenum-titanium alloy tube target is cracked due to stress release in the subsequent machining process.
Preferably, the solder used in the soldering in step (3) comprises indium solder.
Preferably, the brazing temperature in step (3) is 230-250 ℃, for example 230 ℃, 235 ℃, 240 ℃, 245 ℃ or 250 ℃, but is not limited to the recited values, and other non-recited values in the range of values are equally applicable.
Preferably, the brazing in step (3) is followed by furnace cooling to room temperature.
Preferably, the back tube of step (3) comprises a titanium tube and/or a titanium alloy tube.
As a preferred technical scheme of the preparation method according to the first aspect of the present invention, the preparation method comprises the following steps:
(1) Mixing molybdenum powder with the thickness of 3-5 mu m and titanium powder with the thickness of 20-50 mu m in sequence for 12-48 hours in argon atmosphere, and filling the mixture into a die; then cold-pressing for 5-40min under 200-300MPa, and demoulding; vacuum sintering at 1200-1950deg.C for 5-10h and shaping to obtain molybdenum-titanium alloy tube blank;
the titanium content in the mixed powder obtained by mixing is 10-75wt%; the mass ratio of the mixed balls is (0.5-1.75): 1; the vacuum degree of the vacuum sintering is less than 5 multiplied by 10 -3 Pa；
(2) The molybdenum-titanium alloy tube blank obtained in the step (1) is subjected to sheath welding and sealing and degassing treatment at 500-750 ℃ until the vacuum degree is less than 5 multiplied by 10 -3 Pa; then performing hot isostatic pressing splicing treatment for 6-9h at 1000-1500 ℃ and 150-200MPa, performing heat treatment for 1-2h at 350-650 ℃ and performing first machining to obtain a molybdenum-titanium alloy tube;
the steps of the sheath welding seal comprise: coaxially welding the inner and outer jackets on a stainless steel bottom plate to form an annular cavity, stacking the molybdenum-titanium alloy tube blanks in the annular cavity, and then welding a stainless steel cover plate at the other ends of the inner and outer jackets;
(3) And (3) brazing the back tube and the molybdenum-titanium alloy tube obtained in the step (2) at 230-250 ℃ and carrying out second machining to obtain the molybdenum-titanium alloy tube target.
In a second aspect, the invention provides a molybdenum-titanium alloy tube target, which is prepared by the preparation method in the first aspect.
The molybdenum-titanium alloy tube target provided by the invention has the advantages that the compactness can reach 99.5%, the internal tissue structure is uniform, and the molybdenum-titanium alloy tube target can be spliced into a finished product with a larger size according to requirements, so that the molybdenum-titanium alloy tube target is suitable for the panel display technology.
The molybdenum-titanium alloy tube target may have a length of > 3000mm, for example 3200mm, 3400mm, 3600mm, 3800mm or 4000mm, but is not limited to the recited values, and other non-recited values within the range of values are equally applicable.
In a third aspect, the present invention provides the use of a molybdenum titanium alloy tube target according to the second aspect for use in the field of display panels.
Compared with the prior art, the invention has the following beneficial effects:
according to the preparation method of the molybdenum-titanium alloy tube target, cold pressing is performed firstly, and then vacuum sintering is performed, so that the deformation of a tube blank in the forming process can be remarkably reduced; performing hot isostatic pressing splicing treatment on the obtained small-section molybdenum-titanium alloy tube blank to obtain a large-size molybdenum-titanium alloy tube with the diameter of more than 3000 mm; internal stress is removed through heat treatment, so that the problem of cracking of a pipe target caused by stress release in a machining process can be solved; meanwhile, reasonable technological parameters are matched, the density of the obtained molybdenum-titanium alloy tube target can reach 100%, the internal tissue structure is uniform, the crystal grains are fine, deformation or cracking phenomenon is less, and the technical requirement of panel display can be met.
Drawings
Fig. 1 is a schematic structural view of a jacket seal provided in embodiment 1 of the present invention.
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 molybdenum-titanium alloy tube target with the length of 3200mm, and the preparation method of the molybdenum-titanium alloy tube target comprises the following steps:
(1) Mixing molybdenum powder with the thickness of 4 mu m and titanium powder with the thickness of 30 mu m in an argon atmosphere for 26 hours, and filling a polyurethane rubber sleeve mold; then cold-pressing for 25min under 270MPa, and demoulding; vacuum sintering at 1600 ℃ for 8 hours and shaping to obtain a molybdenum-titanium alloy tube blank;
the titanium content in the mixed powder obtained by the mixing is 40wt%; the mass ratio of the zirconium balls to the powder in the mixing is 1.25:1; the vacuum degree of the vacuum sintering is 3.5X10 -3 Pa；
(2) The molybdenum-titanium alloy tube blank obtained in the step (1) is subjected to sheath welding and sealing and degassing treatment at 600 ℃ until the vacuum degree is 3.5 multiplied by 10 - 3 Pa; then carrying out hot isostatic pressing splicing treatment for 8.5h at 1400 ℃ and 170MPa, heat treatment for 1.5h at 500 ℃ and first machining to obtain a molybdenum-titanium alloy tube;
the steps of the sheath welding seal comprise: coaxially welding a stainless steel pipe and a low-carbon steel pipe which are subjected to sand blasting treatment on the contact surface of the molybdenum-titanium alloy pipe blank on a stainless steel bottom plate to form an annular cavity, stacking the molybdenum-titanium alloy pipe blank in the annular cavity, and then welding a stainless steel cover plate on the other ends of an inner sheath and an outer sheath; the schematic structure of the sheath seal is shown in figure 1;
(3) And (3) brazing the titanium alloy tube and the molybdenum-titanium alloy tube obtained in the step (2) by using indium solder at 240 ℃ and carrying out second machining to obtain the molybdenum-titanium alloy tube target.
Example 2
The embodiment provides a molybdenum-titanium alloy tube target with the length of 3400mm, and the preparation method of the molybdenum-titanium alloy tube target comprises the following steps:
(1) Mixing molybdenum powder with the thickness of 4.5 mu m and titanium powder with the thickness of 25 mu m in sequence in argon atmosphere for 18 hours, and filling a polyurethane rubber sleeve mold; then cold-pressing for 20min under 290MPa, and demoulding; vacuum sintering for 6h at 1800 ℃ and shaping to obtain a molybdenum-titanium alloy tube blank;
the titanium content in the mixed powder obtained by the mixing is 60wt%; the mass ratio of the zirconium balls to the powder in the mixing is 1.5:1; the vacuum degree of the vacuum sintering is 3 multiplied by 10 -3 Pa；
(2) The molybdenum-titanium alloy tube blank obtained in the step (1) is subjected to sheath welding and sealing and degassing treatment at 700 ℃ until the tube blank is trueThe air degree is 3 multiplied by 10 -3 Pa; then carrying out hot isostatic pressing splicing treatment for 8h at 1450 ℃ and 160MPa, carrying out heat treatment for 1.2h at 550 ℃ and carrying out first machining to obtain a molybdenum-titanium alloy tube;
the steps of the sheath welding seal comprise: coaxially welding a stainless steel pipe and a low-carbon steel pipe which are subjected to sand blasting treatment on the contact surface of the molybdenum-titanium alloy pipe blank on a stainless steel bottom plate to form an annular cavity, stacking the molybdenum-titanium alloy pipe blank in the annular cavity, and then welding a stainless steel cover plate on the other ends of an inner sheath and an outer sheath;
(3) And (3) brazing the titanium alloy tube and the molybdenum-titanium alloy tube obtained in the step (2) by using indium solder at 245 ℃ and carrying out second machining to obtain the molybdenum-titanium alloy tube target.
Example 3
The embodiment provides a molybdenum-titanium alloy tube target with the length of 3600mm, and the preparation method of the molybdenum-titanium alloy tube target comprises the following steps:
(1) Mixing molybdenum powder with the thickness of 3.5 mu m and titanium powder with the thickness of 40 mu m in sequence in argon atmosphere for 36 hours, and filling a polyurethane rubber sleeve mold; then cold pressing for 30min under 255MPa, and demoulding; vacuum sintering for 9h at 1400 ℃ and shaping to obtain a molybdenum-titanium alloy tube blank;
the titanium content in the mixed powder obtained by the mixing is 25wt%; the mass ratio of the zirconium balls to the powder in the mixing is 1:1; the vacuum degree of the vacuum sintering is 4 multiplied by 10 -3 Pa；
(2) The molybdenum-titanium alloy tube blank obtained in the step (1) is subjected to sheath welding and sealing and degassing treatment at 550 ℃ until the vacuum degree is 4 multiplied by 10 -3 Pa; then performing hot isostatic pressing splicing treatment for 9 hours at 1380 ℃ and 190MPa, performing heat treatment for 1.8 hours at 400 ℃ and performing first machining to obtain a molybdenum-titanium alloy tube;
the steps of the sheath welding seal comprise: coaxially welding a stainless steel pipe and a low-carbon steel pipe which are subjected to sand blasting treatment on the contact surface of the molybdenum-titanium alloy pipe blank on a stainless steel bottom plate to form an annular cavity, stacking the molybdenum-titanium alloy pipe blank in the annular cavity, and then welding a stainless steel cover plate on the other ends of an inner sheath and an outer sheath;
(3) And (3) brazing the titanium alloy tube and the molybdenum-titanium alloy tube obtained in the step (2) by using indium solder at 235 ℃ and carrying out second machining to obtain the molybdenum-titanium alloy tube target.
Example 4
The embodiment provides a molybdenum-titanium alloy tube target with the length of 3800mm, and the preparation method of the molybdenum-titanium alloy tube target comprises the following steps:
(1) Sequentially mixing molybdenum powder with the thickness of 5 mu m and titanium powder with the thickness of 20 mu m in an argon atmosphere for 12 hours, and filling a polyurethane rubber sleeve mold; then cold-pressing for 5min under 300MPa, and demoulding; vacuum sintering at 1950 ℃ for 5 hours and shaping to obtain a molybdenum-titanium alloy tube blank;
the titanium content in the mixed powder obtained by the mixing is 75wt%; the mass ratio of the zirconium balls to the powder in the mixing is 1.75:1; the vacuum degree of the vacuum sintering is 2 multiplied by 10 -3 Pa；
(2) The molybdenum-titanium alloy tube blank obtained in the step (1) is subjected to sheath welding and sealing and degassing treatment at 750 ℃ until the vacuum degree is 2 multiplied by 10 -3 Pa; then carrying out hot isostatic pressing splicing treatment for 6h at 1500 ℃ and 150MPa, heat treatment for 1h at 650 ℃ and first machining to obtain a molybdenum-titanium alloy tube;
the steps of the sheath welding seal comprise: coaxially welding a stainless steel pipe and a low-carbon steel pipe which are subjected to sand blasting treatment on the contact surface of the molybdenum-titanium alloy pipe blank on a stainless steel bottom plate to form an annular cavity, stacking the molybdenum-titanium alloy pipe blank in the annular cavity, and then welding a stainless steel cover plate on the other ends of an inner sheath and an outer sheath;
(3) And (3) brazing the titanium alloy tube and the molybdenum-titanium alloy tube obtained in the step (2) by using indium solder at the temperature of 250 ℃ and carrying out second machining to obtain the molybdenum-titanium alloy tube target.
Example 5
The embodiment provides a molybdenum-titanium alloy tube target with the length of 4000mm, and the preparation method of the molybdenum-titanium alloy tube target comprises the following steps:
(1) Mixing molybdenum powder with the thickness of 3 mu m and titanium powder with the thickness of 50 mu m in sequence in argon atmosphere for 48 hours, and filling a polyurethane rubber sleeve mold; then cold-pressing for 40min under 200MPa, and demoulding; vacuum sintering for 10h at 1200 ℃ and shaping to obtain a molybdenum-titanium alloy tube blank;
the titanium content in the mixed powder obtained by the mixing is 10wt%; the mass ratio of the zirconium balls to the powder in the mixing is 0.5:1; the vacuum degree of the vacuum sintering is 4.5 multiplied by 10 -3 Pa；
(2) The molybdenum-titanium alloy tube blank obtained in the step (1) is subjected to sheath welding and sealing and degassing treatment at 500 ℃ until the vacuum degree is 4.5 multiplied by 10 - 3 Pa; then carrying out hot isostatic pressing splicing treatment for 7h at 1000 ℃ and 200MPa, heat treatment for 2h at 350 ℃ and first machining to obtain a molybdenum-titanium alloy tube;
the steps of the sheath welding seal comprise: coaxially welding a stainless steel pipe and a low-carbon steel pipe which are subjected to sand blasting treatment on the contact surface of the molybdenum-titanium alloy pipe blank on a stainless steel bottom plate to form an annular cavity, stacking the molybdenum-titanium alloy pipe blank in the annular cavity, and then welding a stainless steel cover plate on the other ends of an inner sheath and an outer sheath;
(3) And (3) brazing the titanium alloy tube and the molybdenum-titanium alloy tube obtained in the step (2) by using indium solder at 230 ℃ and carrying out second machining to obtain the molybdenum-titanium alloy tube target.
Example 6
This example provides a molybdenum-titanium alloy tube target, which is different from example 1 in that the cold pressing treatment in step (1) is performed under 190MPa, except that the molybdenum-titanium alloy tube target is prepared in the same manner as in example 1.
Example 7
This example provides a molybdenum-titanium alloy tube target, which is different from example 1 in that the cold pressing treatment in step (1) is performed under the same pressure as that in example 1 except that the pressure is adjusted to 310 MPa.
Example 8
This example provides a molybdenum-titanium alloy tube target, which is different from example 1 in that the vacuum sintering temperature in step (1) is adjusted to 1150 ℃, and the other steps are the same as in example 1.
Example 9
This example provides a molybdenum-titanium alloy tube target, which is different from example 1 in that the vacuum sintering temperature in step (1) is adjusted to 2000 c, and the process is the same as example 1.
Example 10
The present example provides a molybdenum-titanium alloy tube target, which is different from example 1 in that the temperature of the hot isostatic pressing splicing treatment in step (2) is adjusted to 950 ℃, and the other steps are the same as example 1.
Example 11
The present example provides a molybdenum-titanium alloy tube target, which is different from example 1 in that the temperature of the hot isostatic pressing splicing treatment in step (2) is adjusted to 1550 ℃, and the other steps are the same as example 1.
Example 12
The present example provides a molybdenum-titanium alloy tube target, which is different from example 1 in that the method for producing the molybdenum-titanium alloy tube target is the same as example 1 except that the pressure of the hot isostatic pressing splice treatment in step (2) is adjusted to 140 MPa.
Example 13
The present example provides a molybdenum-titanium alloy tube target, and the preparation method of the molybdenum-titanium alloy tube target is different from that of example 1 in that the pressure of the hot isostatic pressing splicing treatment in the step (2) is adjusted to 210MPa, and the other steps are the same as those of example 1.
Example 14
The present embodiment provides a molybdenum-titanium alloy tube target, and the preparation method of the molybdenum-titanium alloy tube target is different from that of embodiment 1 in that in the step of envelope welding in step (2), the stainless steel tube and the low carbon steel tube are not subjected to sand blasting treatment, and the rest are the same as embodiment 1.
Comparative example 1
This comparative example provides a molybdenum-titanium alloy tube target, which is different from example 1 in that step (1) has no vacuum sintering step, and the rest is the same as example 1.
Comparative example 2
This comparative example provides a molybdenum-titanium alloy tube target, which is different from example 1 in that step (2) has no heat treatment step, and the rest is the same as example 1.
Performance testing
The actual density of the molybdenum-titanium alloy tube targets provided in examples 1-14 and comparative examples 1 and 2 is measured according to GB/T3850-2015 density measurement method of compact sintered Metal Material and hard alloy, theoretical density is calculated according to theoretical formula, and theoretical density is calculated according to the calculation formula: density = actual density/theoretical density x 100%, the results obtained are shown in table 1;
the molybdenum-titanium alloy tube targets provided in examples 1 to 14 and comparative examples 1 and 2 were observed for uniformity of internal structure by using a scanning electron microscope and the grain size was measured, and the results are shown in table 1;
the molybdenum-titanium alloy tube targets provided in examples 1 to 14 and comparative examples 1 and 2 were subjected to defect measurement by an ultrasonic scanning imager, and the results are shown in table 1.
TABLE 1
| Density (%) | Grain size (mum) | With or without deformation or cracking | |
| Example 1 | 100 | 22.47 | Without any means for |
| Example 2 | 100 | 26.25 | Without any means for |
| Example 3 | 99.2 | 22.36 | Without any means for |
| Example 4 | 99.0 | 27.28 | Without any means for |
| Example 5 | 98.9 | 20.66 | Without any means for |
| Example 6 | 98.8 | 23.58 | Without any means for |
| Example 7 | 100 | 23.22 | With cracks |
| Example 8 | 97.6 | 21.68 | Without any means for |
| Example 9 | 100 | 59.46 | With cracks |
| Example 10 | 98.7 | 22.34 | Without any means for |
| Example 11 | 90.3 | 23.47 | - |
| Example 12 | 99.8 | 25.95 | Without any means for |
| Example 13 | 100 | 24.47 | With microcracks |
| Example 14 | 100 | 23.67 | Without any means for |
| Comparative example 1 | 99.9 | 21.88 | Distortion and deformation |
| Comparative example 2 | 100 | 23.21 | With penetrating cracks |
As can be seen from Table 1, by comparing the embodiment 1 with the embodiment 2-5, reasonable cold pressing pressure, vacuum sintering temperature and hot isostatic pressing splicing processing parameters are selected, the obtained molybdenum-titanium alloy tube target has good compactness, uniform internal structure and fine grains, and no crack or deformation defect;
as can be seen from comparison of examples 1 and 6 and 7, the excessive cold pressing pressure has adverse effect on the compactness of the molybdenum-titanium alloy tube target, and the excessive cold pressing pressure can cause cracking of the molybdenum-titanium alloy tube target; as can be seen from comparison of examples 1 and 8 and 9, the vacuum sintering temperature is too low, the density of the molybdenum-titanium alloy tube target is reduced, the vacuum sintering temperature is too high, the grain size is large, and the molybdenum-titanium alloy tube target is cracked in the processing process due to the excessive hardness; as can be seen from comparison of examples 1 and 10 and 11, the temperature of the hot isostatic pressing splicing treatment is too low, the density of the molybdenum-titanium alloy tube target is reduced, the temperature is too high, the sheath is melted, and the density of the molybdenum-titanium alloy tube target is severely reduced; as can be seen from comparison of examples 1 and 12 and 13, the pressure of the hot isostatic pressing splicing treatment is too low to apply equal and sufficient stress to the sheath in each direction so as to form the molybdenum-titanium alloy tube target; the density of the molybdenum-titanium alloy tube target is not increased any more due to the excessively high pressure, and microcracks are generated on the molybdenum-titanium alloy tube target. As can be seen from the comparison of the embodiment 1 and the embodiment 14, the inner and outer jackets are not subjected to sand blasting treatment, so that the influence on the density and the grain size is small, but the introduction of impurities in the sintering process is increased, and the purity of the molybdenum-titanium alloy tube target is further reduced;
as can be seen from the comparison of the example 1 and the comparative example 1, the direct hot isostatic pressing splicing treatment without the vacuum sintering step can cause the excessive shrinkage of the molybdenum-titanium alloy tube target to generate distortion; as is clear from the comparison between example 1 and comparative example 2, the internal stress of the molybdenum-titanium alloy tube blank cannot be removed without the heat treatment step, and the penetration crack is generated.
In summary, the preparation method of the molybdenum-titanium alloy tube target provided by the invention comprises the steps of cold pressing and vacuum sintering, so that the deformation of the tube blank in the forming process can be obviously reduced; performing hot isostatic pressing splicing treatment on the obtained small-section molybdenum-titanium alloy tube blank to obtain a large-size molybdenum-titanium alloy tube with the diameter of more than 3000 mm; internal stress is removed through heat treatment, so that the problem of cracking of a pipe target caused by stress release in a machining process can be solved; meanwhile, reasonable technological parameters are matched, the density of the obtained molybdenum-titanium alloy tube target can reach 100%, the internal tissue structure is uniform, the crystal grains are fine, deformation or cracking phenomenon is less, and the technical requirement of panel display can be met.
The foregoing is merely illustrative of the present invention, and the present invention is not limited thereto, and it should be apparent to those skilled in the art that any changes or substitutions that fall within the technical scope of the present invention disclosed herein are within the scope of the present invention.
Claims (29)
1. A method for preparing a molybdenum-titanium alloy tube target, which is characterized by comprising the following steps:
(1) Sequentially mixing molybdenum powder and titanium powder, filling the mixture into a mold, carrying out cold pressing treatment, demolding, vacuum sintering and shaping to obtain a molybdenum-titanium alloy tube blank;
(2) The molybdenum-titanium alloy tube blank obtained in the step (1) is subjected to sheath welding, degassing treatment, hot isostatic pressing splicing treatment, heat treatment and first machining to obtain a molybdenum-titanium alloy tube;
(3) The back tube and the molybdenum-titanium alloy tube obtained in the step (2) are subjected to brazing and second machining to obtain the molybdenum-titanium alloy tube target;
the pressure of the cold pressing treatment in the step (1) is 255-290MPa;
the cold pressing treatment time in the step (1) is 20-30min;
the temperature of the vacuum sintering in the step (1) is 1400-1500 ℃;
the time of the vacuum sintering in the step (1) is 5-10h;
the vacuum degree of the vacuum sintering in the step (1) is less than 5 multiplied by 10 -3 Pa。
2. The method according to claim 1, wherein the particle size of the molybdenum powder in step (1) is in the range of 3 to 5 μm.
3. The method according to claim 1, wherein the particle size of the titanium powder in step (1) is in the range of 20 to 50. Mu.m.
4. The method according to claim 1, wherein the titanium content of the mixed powder obtained in the step (1) is 10 to 75wt%.
5. The method of claim 1, wherein the mixed media of step (1) comprises zirconium spheres or titanium spheres.
6. The method according to claim 1, wherein the mass ratio of the mixed pellets in the step (1) is (0.5-1.75): 1.
7. The method of claim 1, wherein the mixing in step (1) is for a period of 12 to 48 hours.
8. The method of claim 1, wherein the mixing of step (1) is performed in an argon atmosphere.
9. The method of claim 1, wherein the mold used for the molding in step (1) comprises a polyurethane gum cover.
10. The method according to claim 1, wherein the outer jacket used in the jacket sealing in the step (2) is a stainless steel pipe or a low carbon steel pipe with a contact surface of a molybdenum-titanium alloy pipe blank subjected to sand blasting.
11. The method according to claim 10, wherein the inner sheath used in the sheath sealing in the step (2) is a stainless steel pipe or a low carbon steel pipe with a contact surface of a molybdenum-titanium alloy pipe blank subjected to sand blasting.
12. The method of claim 11, wherein the step of envelope sealing in step (2) comprises: and coaxially welding the inner sheath and the outer sheath on the stainless steel bottom plate to form an annular cavity, stacking the molybdenum-titanium alloy tube blanks in the annular cavity, and then welding the stainless steel cover plate at the other ends of the inner sheath and the outer sheath.
13. The method according to claim 1, wherein the temperature of the degassing treatment in step (2) is 500 to 750 ℃.
14. The method according to claim 1, wherein the degassing treatment in step (2) is terminated by a vacuum level of < 5X 10 -3 Pa。
15. The method of claim 1, wherein the hot isostatic pressing splice treatment in step (2) is performed at a temperature of 1000-1500 ℃.
16. The method of claim 15, wherein the hot isostatic pressing splice treatment in step (2) is performed at a temperature of 1380-1450 ℃.
17. The method of claim 1, wherein the pressure of the hot isostatic pressing splice treatment in step (2) is 150-200MPa.
18. The method of claim 17, wherein the pressure of the hot isostatic pressing splice treatment in step (2) is 160-190MPa.
19. The method of claim 1, wherein the hot isostatic pressing splice treatment of step (2) is performed for a dwell time of 6-9 hours.
20. The method of claim 19, wherein the hot isostatic pressing splice treatment of step (2) is performed for a dwell time of 8-9 hours.
21. The method according to claim 1, wherein the temperature of the heat treatment in step (2) is 350 to 650 ℃.
22. The method of claim 21, wherein the heat treatment in step (2) is performed at a temperature of 400-550 ℃.
23. The method according to claim 1, wherein the time of the heat treatment in the step (2) is 1 to 2 hours.
24. The method of claim 1, wherein the solder used in the brazing in step (3) comprises indium solder.
25. The method of claim 1, wherein the brazing in step (3) is performed at a temperature of 230-250 ℃.
26. The method of claim 1, wherein the backing tube of step (3) comprises a titanium tube or a titanium alloy tube.
27. The preparation method according to claim 1, characterized in that the preparation method comprises the steps of:
(1) Mixing molybdenum powder with the thickness of 3-5 mu m and titanium powder with the thickness of 20-50 mu m in sequence for 12-48 hours in argon atmosphere, and filling the mixture into a die; then cold-pressing for 20-30min under 255-290MPa, and demoulding; vacuum sintering at 1400-1500 deg.c for 5-10 hr and shaping to obtain molybdenum-titanium alloy pipe blank;
the titanium content in the mixed powder obtained by mixing is 10-75wt%; the mass ratio of the mixed balls is (0.5-1.75): 1; the vacuum degree of the vacuum sintering is less than 5 multiplied by 10 -3 Pa；
(2) The molybdenum-titanium alloy tube blank obtained in the step (1) is subjected to sheath welding and sealing and degassing treatment at 500-750 ℃ until the vacuum degree is less than 5 multiplied by 10 -3 Pa; then performing hot isostatic pressing splicing treatment for 6-9h at 1000-1500 ℃ and 150-200MPa, performing heat treatment for 1-2h at 350-650 ℃ and performing first machining to obtain a molybdenum-titanium alloy tube;
the steps of the sheath welding seal comprise: coaxially welding the inner and outer jackets on a stainless steel bottom plate to form an annular cavity, stacking the molybdenum-titanium alloy tube blanks in the annular cavity, and then welding a stainless steel cover plate at the other ends of the inner and outer jackets;
(3) And (3) brazing the back tube and the molybdenum-titanium alloy tube obtained in the step (2) at 230-250 ℃ and carrying out second machining to obtain the molybdenum-titanium alloy tube target.
28. A molybdenum-titanium alloy tube target, characterized in that the molybdenum-titanium alloy tube target is produced by the production method according to any one of claims 1 to 27;
the length of the molybdenum-titanium alloy tube target is more than 3000mm.
29. Use of the molybdenum-titanium alloy tube target according to claim 28, wherein the molybdenum-titanium alloy tube target is used in the field of display panels.
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| CN104480437A (en) * | 2014-12-30 | 2015-04-01 | 山东昊轩电子陶瓷材料有限公司 | Production method for integrally formed cylindrical target |
| CN108941584A (en) * | 2018-09-07 | 2018-12-07 | 韶关市欧莱高新材料有限公司 | A kind of preparation method of long molybdenum tube sputtering target material |
| CN113174573A (en) * | 2021-04-29 | 2021-07-27 | 宁波江丰电子材料股份有限公司 | Preparation method of molybdenum-titanium alloy target blank |
| CN114086130A (en) * | 2021-11-16 | 2022-02-25 | 宁波江丰电子材料股份有限公司 | Preparation method of tungsten-titanium alloy tube target |
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