CN115502403A - Preparation method of large-size and high-density molybdenum target - Google Patents
Preparation method of large-size and high-density molybdenum target Download PDFInfo
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- CN115502403A CN115502403A CN202211204651.3A CN202211204651A CN115502403A CN 115502403 A CN115502403 A CN 115502403A CN 202211204651 A CN202211204651 A CN 202211204651A CN 115502403 A CN115502403 A CN 115502403A
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- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 title claims abstract description 136
- 229910052750 molybdenum Inorganic materials 0.000 title claims abstract description 103
- 239000011733 molybdenum Substances 0.000 title claims abstract description 103
- 238000002360 preparation method Methods 0.000 title claims abstract description 28
- 238000005245 sintering Methods 0.000 claims abstract description 84
- 238000007731 hot pressing Methods 0.000 claims abstract description 69
- 238000004321 preservation Methods 0.000 claims abstract description 68
- 239000013077 target material Substances 0.000 claims abstract description 29
- 238000001513 hot isostatic pressing Methods 0.000 claims abstract description 27
- 238000000034 method Methods 0.000 claims abstract description 23
- 238000000137 annealing Methods 0.000 claims abstract description 19
- 238000003825 pressing Methods 0.000 claims abstract description 19
- 238000003754 machining Methods 0.000 claims abstract description 12
- 238000010438 heat treatment Methods 0.000 claims abstract description 6
- 238000007872 degassing Methods 0.000 claims description 14
- 229920001971 elastomer Polymers 0.000 claims description 14
- 238000005488 sandblasting Methods 0.000 claims description 14
- 239000010935 stainless steel Substances 0.000 claims description 12
- 229910001220 stainless steel Inorganic materials 0.000 claims description 12
- 239000007789 gas Substances 0.000 claims description 11
- 238000004519 manufacturing process Methods 0.000 claims description 9
- 238000007873 sieving Methods 0.000 claims description 9
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 8
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- 230000001681 protective effect Effects 0.000 claims description 6
- 229910052786 argon Inorganic materials 0.000 claims description 4
- 239000002245 particle Substances 0.000 claims description 4
- 229910001209 Low-carbon steel Inorganic materials 0.000 claims description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- 238000005422 blasting Methods 0.000 claims description 2
- 238000003466 welding Methods 0.000 claims description 2
- 239000002131 composite material Substances 0.000 claims 1
- 238000011049 filling Methods 0.000 claims 1
- 239000013078 crystal Substances 0.000 abstract description 8
- 239000004973 liquid crystal related substance Substances 0.000 abstract description 5
- 238000004140 cleaning Methods 0.000 abstract description 3
- 238000000465 moulding Methods 0.000 abstract description 3
- 238000004806 packaging method and process Methods 0.000 abstract description 2
- 230000000052 comparative effect Effects 0.000 description 7
- 238000011068 loading method Methods 0.000 description 7
- 238000011534 incubation Methods 0.000 description 6
- 238000005096 rolling process Methods 0.000 description 5
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 229920003225 polyurethane elastomer Polymers 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- 238000007789 sealing Methods 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- 238000000280 densification Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 229920002635 polyurethane Polymers 0.000 description 2
- 239000004814 polyurethane Substances 0.000 description 2
- 238000004663 powder metallurgy Methods 0.000 description 2
- 230000000630 rising effect Effects 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 238000005299 abrasion Methods 0.000 description 1
- 238000007792 addition Methods 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- APUPEJJSWDHEBO-UHFFFAOYSA-P ammonium molybdate Chemical compound [NH4+].[NH4+].[O-][Mo]([O-])(=O)=O APUPEJJSWDHEBO-UHFFFAOYSA-P 0.000 description 1
- 229940010552 ammonium molybdate Drugs 0.000 description 1
- 235000018660 ammonium molybdate Nutrition 0.000 description 1
- 239000011609 ammonium molybdate Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000005341 cation exchange Methods 0.000 description 1
- 238000009694 cold isostatic pressing Methods 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000005429 filling process Methods 0.000 description 1
- 238000005242 forging Methods 0.000 description 1
- 238000000265 homogenisation Methods 0.000 description 1
- 238000005098 hot rolling Methods 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000005204 segregation Methods 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
Images
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
- 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
- B22F5/00—Manufacture of workpieces or articles from metallic powder characterised by the special shape of the product
-
- 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
Abstract
The invention relates to a preparation method of a large-size high-density molybdenum target, which comprises the following steps: sequentially annealing, cold pressing and hot-pressed sintering molybdenum powder to obtain a molybdenum blank; placing the molybdenum blank into the welded sheath, and performing hot isostatic pressing splicing to obtain a molybdenum target material; the size of the prepared molybdenum target material is more than 3000mm, and the density is more than 99.9%. According to the preparation method provided by the invention, the molybdenum powder after being screened and annealed is subjected to one-step cold press molding, then is subjected to multi-stage heating and heat preservation hot pressing furnace sintering and is dense, so that a small segment of molybdenum target blank is obtained, and is subjected to hot isostatic pressing splicing, machining, cleaning, packaging and other processes, so that the prepared molybdenum target material is high in density, fine in crystal grain and large in size, and can meet the requirements of the liquid crystal display and touch screen industry.
Description
Technical Field
The invention belongs to the technical field of target preparation, and particularly relates to a preparation method of a large-size high-density molybdenum target.
Background
In the field of panel display, a core target material is a molybdenum target material, and a flat panel display is mainly used in two product production links of a display panel and a touch screen panel, so that the flat panel display has huge market demand. With the development of the panel industry, the size requirement of the target is gradually increased, and the requirements on the compactness and the fineness of grains of the target are higher. Currently known methods for producing molybdenum targets include rolling methods and powder metallurgy methods.
Although the target material prepared by the powder metallurgy method has uniform components, no segregation, fine crystal grains and high purity, the current industrial process cannot prepare large size (more than 1000 mm) and cannot meet the requirements of the liquid crystal display and touch screen industries.
The rolling method is the most mature process for preparing the large-size molybdenum target at present. CN104342619A discloses a method for manufacturing molybdenum target material, which comprises the following steps: the densification treatment of molybdenum powder is realized through a hot-pressing sintering process to obtain a first molybdenum target blank, and then the further densification treatment of the first molybdenum target blank is gradually realized through a multi-stage hot rolling treatment process, so that the molybdenum target with molybdenum particle grains smaller than 50 microns and the density as high as 99.94% is obtained. Compared with the molybdenum target obtained by the existing molybdenum target manufacturing method, the molybdenum target obtained by the method has smaller molybdenum grain granularity, more uniform grain size, higher density, better electrical property and mechanical processing property, and can completely meet the sputtering requirement of the molybdenum target.
CN114574821A discloses a preparation method of a large-size molybdenum target, wherein ammonium molybdate is taken as a raw material, ammonia dissolution and cation exchange treatment are firstly carried out, and then high-purity molybdenum powder is obtained by hydrogen reduction after evaporation crystallization; carrying out cold isostatic pressing and hydrogen sintering on the obtained high-purity molybdenum powder to prepare a high-purity molybdenum plate blank; pre-forging and cogging the obtained high-purity molybdenum plate blank by adopting a one-fire one-pass processing mode to obtain a pre-forged blank, and then performing multi-pass cross rolling by adopting a one-fire two-pass processing mode to obtain a rolled plate blank; and carrying out surface chemical corrosion on the obtained rolled plate blank, and then carrying out homogenization annealing treatment on the corroded plate blank to finally obtain the large-size molybdenum target material.
However, when the rolling method is adopted to prepare the large-size molybdenum target material in the prior art, the rolling cannot be carried out in multiple directions due to the influence of the size, so that the internal structure of the target material is easily uneven, and the problems of high oxygen content and the like exist.
Therefore, the preparation method of the large-size molybdenum target material with high density and uniform internal organizational structure is of great significance.
Disclosure of Invention
The invention aims to provide a preparation method of a large-size and high-density molybdenum target material, and by adopting the preparation method provided by the invention, the size of the obtained molybdenum target material is larger than 3000mm, the density is high, and the crystal grains are uniform.
In order to achieve the purpose, the invention adopts the following technical scheme:
in a first aspect, the invention provides a preparation method of a large-size and high-density molybdenum target material, which comprises the following steps:
(1) Sequentially annealing, cold pressing and hot-pressed sintering molybdenum powder to obtain a molybdenum blank;
(2) And (2) placing the molybdenum blank obtained in the step (1) into the welded sheath, and performing hot isostatic pressing splicing to obtain the molybdenum target.
According to the invention, after molybdenum powder is annealed and deoxidized, the molybdenum powder is added into a cold pressing mold, firstly, the molybdenum powder is subjected to primary cold pressing molding, then the molybdenum powder is placed into a hot pressing furnace to be sintered and compacted, so that a small-segment molybdenum target blank is obtained, and finally, the molybdenum target with large size and high density is prepared by hot isostatic pressing and splicing.
As a preferable technical scheme of the invention, the molybdenum powder with the granularity less than or equal to 3um is obtained by sieving before the annealing in the step (1).
In the present invention, the particle size of the molybdenum powder after the sieving treatment is 3 μm or less, and may be, for example, 1 μm, 1.4 μm, 1.8 μm, 2 μm, 2.5 μm or 3 μm, but is not limited to the values listed, and other values not listed in the numerical range are also applicable.
As a preferred embodiment of the present invention, the annealing in step (1) is performed under a protective gas.
Preferably, the protective gas comprises argon or nitrogen.
Preferably, the annealing temperature in step (1) is 300-350 ℃, such as 300 ℃, 310 ℃, 320 ℃, 330 ℃, 340 ℃ or 350 ℃, but not limited to the recited values, and other values not recited in the range of values are also applicable.
Preferably, the annealing time in step (1) is 0.5-1h, such as 0.5h, 0.6h, 0.7h, 0.8h, 0.9h or 1h, but not limited to the recited values, and other values not recited in the range of values are also applicable.
In the invention, the molybdenum powder after sieving is annealed, so that the oxygen content in the powder can be reduced.
As a preferred technical scheme of the invention, the cold pressing in the step (1) is carried out in a rubber sleeve die.
In the invention, the material of the rubber sleeve mould is polyurethane, and the rubber sleeve made of polyurethane is not adhered to the material, so that the demoulding is easier. And cleaning and drying the rubber sleeve mould before use.
Preferably, the pressure of the cold pressing in step (1) is 200-300MPa, such as 200MPa, 220MPa, 240MPa, 260MPa, 280MPa or 300MPa, but not limited to the recited values, and other values not recited in the numerical range are also applicable.
Preferably, the cold pressing in step (1) has a dwell time of 5-40min, such as 5min, 10min, 15min, 20min, 25min, 30min, 35min or 40min, but not limited to the recited values, and other values not recited in the range of values are also applicable.
In the invention, deoxidized molybdenum powder is filled into a cold pressing die cavity, the die filling process needs to be completed on a vibration platform, and an upper rubber plug and a lower rubber plug are well sealed; and demolding after cold pressing.
As a preferable technical scheme of the invention, the hot-pressing sintering in the step (1) is carried out in a vacuum hot-pressing sintering furnace.
Preferably, the vacuum degree of the hot-pressing sintering in the step (1) is less than 5X 10 -3 Pa, for example, may be 1X 10 -4 Pa、1×10 -3 Pa、2×10 -3 Pa、3×10 -3 Pa or 4X 10 -3 Pa, etc., but are not limited to the recited values, and other values within the range of values not recited are equally applicable.
Preferably, the pressure of the hot pressing sintering in step (1) is 30-50MPa, such as 30MPa, 34MPa, 38MPa, 40MPa, 44MPa, 48MPa or 50MPa, but not limited to the values listed, and other values not listed in the numerical range are also applicable.
Preferably, the hot-pressing sintering of step (1) includes a first hot-pressing sintering and a second hot-pressing sintering which are performed sequentially.
Preferably, the temperature increase rate of the first hot press sintering is 8 to 10 ℃/min, for example, 8 ℃/min, 8.4 ℃/min, 8.8 ℃/min, 9 ℃/min, 9.4 ℃/min, 9.8 ℃/min, or 10 ℃/min, etc., but is not limited to the values listed, and other values not listed in the numerical range are also applicable.
Preferably, the temperature rise end point of the first hot press sintering is 800 to 1000 ℃, for example, 800 ℃, 840 ℃, 880 ℃, 900 ℃, 940 ℃, 980 ℃ or 1000 ℃, etc., but not limited to the recited values, and other values not recited in the range of values are also applicable.
Preferably, the holding time of the first hot press sintering is 1 to 3 hours, for example, 1 hour, 1.4 hours, 1.8 hours, 2 hours, 2.4 hours, 2.8 hours or 3 hours, etc., but not limited to the recited values, and other values not recited in the numerical range are also applicable.
Preferably, the temperature increase rate of the second hot press sintering is 3 to 5 ℃/min, and for example, it may be 3 ℃/min, 3.4 ℃/min, 3.8 ℃/min, 4 ℃/min, 4.4 ℃/min, 4.8 ℃/min, or 5 ℃/min, etc., but is not limited to the values listed, and other values not listed in the numerical range are also applicable.
Preferably, the temperature rise end point of the second hot press sintering is 1200 to 1500 ℃, for example, 1200 ℃, 1250 ℃, 1300 ℃, 1350 ℃, 1400 ℃, 1450 ℃, or 1500 ℃, etc., but is not limited to the recited values, and other values not recited in the range of values are also applicable.
Preferably, the holding time of the second hot press sintering is 2-3h, such as 2h, 2.2h, 2.4h, 2.6h, 2.8h or 3h, etc., but not limited to the recited values, and other values not recited in the range of the values are also applicable.
As a preferable technical means of the present invention, the hot press sintering in the step (1) is followed by machining.
Preferably, the flatness of the machined molybdenum blank is < 0.5mm, and may be, for example, 0.01mm, 0.05mm, 0.1mm, 0.2mm, 0.3mm, 0.4mm, etc., but is not limited to the values recited, and other values not recited within the range of values are equally applicable.
Preferably, the height of the machined molybdenum billet is 400-500mm, for example 400mm, 420mm, 440mm, 460mm, 480mm or 500mm, but not limited to the recited values, and other values not recited in the numerical range are equally applicable.
As a preferable technical scheme of the invention, the sheath in the step (2) is made of stainless steel or low-carbon steel.
In the invention, the carbon content in the low-carbon steel is less than 0.25%.
Preferably, the inner surface of the sheath in step (2) is sandblasted.
Preferably, the grit blasting has a roughness of Ra12-18 μm, such as 12 μm, 13 μm, 14 μm, 15 μm, 16 μm, 17 μm or 18 μm, but not limited to the values recited, and other values not recited within the range of values are equally applicable.
According to the invention, the sheath is subjected to sand blasting treatment, cleaned and dried, and then welded into a box shape.
As a preferable technical scheme of the invention, degassing treatment is carried out before the hot isostatic pressing splicing in the step (2).
Preferably, the degassing temperature is 500-750 ℃, for example can be 500 ℃, 550 ℃, 600 ℃, 650 ℃, 700 ℃ or 750 ℃, but not limited to the enumerated values, in the range of other values are also applicable.
Preferably, the degassing placeFinal vacuum degree of < 5X 10 -3 Pa, for example, may be 7X 10 -4 Pa、5×10 - 4 Pa、3×10 -4 Pa、1×10 -4 Pa or 3X 10 -3 Pa, etc., but are not limited to the recited values, and other values within the range of values not recited are equally applicable.
In the present invention, the degassing treatment is carried out until the degree of vacuum is less than 5X 10 -3 And closing after Pa.
Preferably, the pressure for hot isostatic pressing splicing in step (2) is 150-200Mpa, such as 150Mpa, 160Mpa, 170Mpa, 180Mpa, 190Mpa or 200Mpa, but not limited to the recited values, and other values not recited in the numerical range are also applicable.
Preferably, the hot isostatic pressing splicing in the step (2) comprises a first heat preservation, a second heat preservation and a third heat preservation which are sequentially carried out.
Preferably, the temperature increase rate of the first heat preservation is 8 to 10 ℃/min, for example, 8 ℃/min, 8.4 ℃/min, 8.8 ℃/min, 9 ℃/min, 9.4 ℃/min, 9.8 ℃/min, or 10 ℃/min, etc., but is not limited to the values listed, and other values not listed in the numerical range are also applicable.
Preferably, the temperature rise end point of the first heat preservation is 500 to 650 ℃, for example, 500 ℃, 540 ℃, 580 ℃, 600 ℃, 620 ℃ or 650 ℃, etc., but not limited to the recited values, and other values not recited in the numerical range are also applicable.
Preferably, the first incubation time is 2-3h, such as 2h, 2.2h, 2.4h, 2.6h, 2.8h or 3h, but not limited to the recited values, and other values not recited in the range of values are also applicable.
Preferably, the second incubation temperature is increased at a rate of 5-7 deg.C/min, such as 5 deg.C/min, 5.4 deg.C/min, 5.8 deg.C/min, 6 deg.C/min, 6.4 deg.C/min, 6.8 deg.C/min, or 7 deg.C/min, but not limited to the values recited, and other values not recited within the range of values are equally applicable.
Preferably, the end point of the second incubation temperature rise is 950 to 1050 ℃, for example 950 ℃, 970 ℃, 990 ℃, 1000 ℃, 1020 ℃, 1040 ℃, or 1050 ℃ and the like, but is not limited to the recited values, and other values not recited in the range of values are also applicable.
Preferably, the second incubation time is 2-3h, such as 2h, 2.2h, 2.4h, 2.6h, 2.8h or 3h, etc., but not limited to the recited values, and other values in the range of values not recited are equally applicable.
Preferably, the temperature increase rate of the third incubation is 2-3 deg.C/min, such as 2 deg.C/min, 2.2 deg.C/min, 2.4 deg.C/min, 2.6 deg.C/min, 2.8 deg.C/min, or 3 deg.C/min, but not limited to the values listed, and other values not listed in the range of values are also applicable.
Preferably, the temperature rise end point of the third heat preservation is 1100 to 1400 ℃, for example 1100 ℃, 1150 ℃, 1200 ℃, 1250 ℃, 1300 ℃, 1350 ℃ or 1400 ℃, etc., but is not limited to the recited values, and other values not recited in the numerical range are also applicable.
Preferably, the third incubation time is 2-3h, such as 2h, 2.2h, 2.4h, 2.6h, 2.8h or 3h, etc., but not limited to the recited values, and other values in the range of values not recited are equally applicable.
In the invention, the molybdenum blank after hot isostatic pressing splicing is machined, and the molybdenum target is obtained after removing the sheath.
In a preferred embodiment of the present invention, the size of the molybdenum target is greater than 3000mm, for example 3100mm, 3300mm, 3500mm, 4000mm, 4500mm, or 5000mm, but the present invention is not limited thereto, and other values not listed in the numerical range are also applicable.
The molybdenum target may have a density of > 99.9%, for example, 99.91%, 99.92%, 99.93%, 99.95%, 99.97%, or 99.99%, etc., but the density is not limited to the values listed, and other values not listed in the numerical range are also applicable.
As a preferred technical scheme of the invention, the preparation method comprises the following steps:
(1) Sieving molybdenum powder to obtain molybdenum powder with the particle size of less than or equal to 3 mu m, annealing for 0.5-1h at 300-350 ℃ under protective gas, then loading the molybdenum powder into a rubber sleeve die, carrying out cold pressing under 200-300MPa and maintaining the pressure for 5-40min, carrying out hot-pressing sintering and machining to obtain a molybdenum blank;
the hot-pressing sintering is carried out in a vacuum hot-pressing sintering furnace, and the vacuum degree of the hot-pressing sintering is less than 5 multiplied by 10 -3 Pa, the pressure is 30-50Mpa;
the hot-pressing sintering comprises a first hot-pressing sintering and a second hot-pressing sintering which are sequentially carried out;
the first hot-pressing sintering is carried out, the temperature is raised to 800-1000 ℃ at the speed of 8-10 ℃/min, and the temperature is kept for 1-3h;
the second hot-pressing sintering is carried out, the temperature is raised to 1200-1500 ℃ at the speed of 3-5 ℃/min, and the temperature is kept for 2-3h;
the flatness of the machined molybdenum billet is less than 0.5mm, and the height of the machined molybdenum billet is 400-500mm;
(2) Placing the molybdenum blank in the step (1) into a sheath after welding, and then sequentially degassing at 500-750 ℃ until the vacuum degree is less than 5 multiplied by 10 -3 Pa, and carrying out hot isostatic pressing splicing under the pressure of 150-200Mpa to obtain the molybdenum target material with the size of more than 3000mm and the density of more than 99.9 percent;
the inner surface of the sheath is subjected to sand blasting treatment, and the roughness of the sand blasting treatment is Ra12-18 mu m;
the hot isostatic pressing splicing comprises a first heat preservation, a second heat preservation and a third heat preservation which are sequentially carried out;
the first heat preservation is carried out, the temperature is raised to 500-650 ℃ at the speed of 8-10 ℃/min, and the heat preservation is carried out for 2-3h;
the second heat preservation is carried out, the temperature is raised to 950-1050 ℃ at the speed of 5-7 ℃/min, and the heat preservation is carried out for 2-3h;
and the third heat preservation is carried out, wherein the temperature is raised to 1100-1400 ℃ at the speed of 2-3 ℃/min, and the heat preservation is carried out for 2-3h.
The recitation of numerical ranges herein includes not only the above-recited numerical values, but also any numerical values between non-recited numerical ranges, and is not intended to be exhaustive or to limit the invention to the precise numerical values encompassed within the range for brevity and clarity.
Compared with the prior art, the invention has the following beneficial effects:
according to the preparation method provided by the invention, the molybdenum powder after being screened and annealed is subjected to one-step cold press molding, then is subjected to multi-stage heating and heat preservation hot pressing furnace sintering and is dense, so that a small-section molybdenum target blank is obtained, and the molybdenum target material prepared by the steps of hot isostatic pressing splicing, machining, cleaning, packaging and the like is high in density, fine in crystal grain and large in size, so that the requirements of the liquid crystal display and touch screen industry can be met.
Drawings
Fig. 1 is a grain diagram of a molybdenum target prepared in example 1 of the present invention.
Detailed Description
The technical solution of the present invention is further described below by way of specific embodiments. It should be understood by those skilled in the art that the examples are only for the understanding of the present invention and should not be construed as the specific limitations of the present invention.
Example 1
The embodiment provides a preparation method of a large-size high-density molybdenum target, which comprises the following steps:
(1) Sieving molybdenum powder to obtain molybdenum powder with the granularity of less than or equal to 3 mu m, then introducing argon gas for annealing at 320 ℃ for 1h, then loading the molybdenum powder into a polyurethane rubber sleeve die, completing a die loading procedure on a vibration platform, sealing an upper rubber plug and a lower rubber plug, then carrying out cold pressing at 250MPa, maintaining the pressure for 20min, then demoulding, and carrying out hot-pressing sintering and machining on the obtained molybdenum blank in a vacuum hot-pressing sintering furnace to obtain a molybdenum blank with the flatness of 0.2mm and the height of 450 mm;
the vacuum degree of the hot-pressing sintering is 1 multiplied by 10 -3 Pa, 40Mpa of pressure; the hot-pressing sintering comprises a first hot-pressing sintering and a second hot-pressing sintering which are sequentially carried out;
the first hot-pressing sintering is carried out, the temperature is increased to 900 ℃ at the speed of 9 ℃/min, and the temperature is kept for 2h;
the second hot-pressing sintering is carried out, wherein the temperature is increased to 1400 ℃ at a speed of 4 ℃/min, and the temperature is kept for 3h;
(2) Placing the molybdenum blank in the step (1) into a welded stainless steel sheath, and performing degassing treatment at 600 ℃ until the vacuum degree is 1 x 10 -3 Closing gas after Pa, performing hot isostatic pressing splicing under the pressure of 170Mpa, and cooling to room temperature along with the furnace, and finallyThen machining the molybdenum blank, removing the sheath and obtaining a molybdenum target material;
the stainless steel sheath is box-shaped; the inner surface of the stainless steel sheath is subjected to sand blasting treatment, and the roughness of the sand blasting treatment is Ra14 micrometers;
the hot isostatic pressing splicing comprises a first heat preservation, a second heat preservation and a third heat preservation which are sequentially carried out;
the first heat preservation is carried out, the temperature is raised to 600 ℃ at the speed of 9 ℃/min, and the heat preservation is carried out for 2.5h;
the second heat preservation is carried out, the temperature is raised to 1000 ℃ at the speed of 6 ℃/min, and the heat preservation is carried out for 2.5h;
and the temperature of the third heat preservation is raised to 1300 ℃ at the speed of 2 ℃/min and is preserved for 2.5h.
Fig. 1 is a grain diagram of the molybdenum target prepared in example 1, and it can be seen that the grains of the molybdenum target are fine and meet the requirements of the liquid crystal display and touch screen industries.
Example 2
The embodiment provides a preparation method of a large-size and high-density molybdenum target, which comprises the following steps:
(1) Sieving molybdenum powder to obtain molybdenum powder with the granularity of less than or equal to 3 microns, annealing for 0.5h at 350 ℃ under the protection of nitrogen, then loading the molybdenum powder into a polyurethane rubber sleeve die, completing the die loading process on a vibration platform, sealing an upper rubber plug and a lower rubber plug, then carrying out cold pressing at 300MPa, maintaining the pressure for 10min, and then demoulding, and carrying out hot-pressing sintering and machining on the obtained molybdenum blank in a vacuum hot-pressing sintering furnace to obtain a molybdenum blank with the flatness of 0.3mm and the height of 400 mm;
the vacuum degree of the hot-pressing sintering is 5 multiplied by 10 -4 Pa, pressure 50Mpa; the hot-pressing sintering comprises a first hot-pressing sintering and a second hot-pressing sintering which are sequentially carried out;
the first hot-pressing sintering is carried out, the temperature is raised to 1000 ℃ at the speed of 10 ℃/min, and the temperature is kept for 1h;
heating the second hot-pressing sintering to 1500 ℃ at the speed of 5 ℃/min and preserving heat for 2.5h;
(2) Placing the molybdenum blank in the step (1) into a welded stainless steel sheath, and degassing at 500 ℃ until the vacuum degree is 5 multiplied by 10 -4 Closing gas after Pa, performing hot isostatic pressing splicing under the pressure of 200Mpa, cooling to room temperature along with the furnace, machining the molybdenum blank, and removing the sheath to obtain the molybdenum target material;
the stainless steel sheath is box-shaped; the inner surface of the stainless steel sheath is subjected to sand blasting treatment, and the roughness of the sand blasting treatment is Ra18 mu m;
the hot isostatic pressing splicing comprises a first heat preservation, a second heat preservation and a third heat preservation which are sequentially carried out;
the first heat preservation is carried out, the temperature is raised to 650 ℃ at the speed of 10 ℃/min, and the heat preservation is carried out for 2h;
the second heat preservation is carried out, the temperature is raised to 1050 ℃ at the speed of 7 ℃/min, and the heat preservation is carried out for 2h;
and the temperature of the third heat preservation is raised to 1400 ℃ at the speed of 3 ℃/min and is preserved for 2h.
Example 3
The embodiment provides a preparation method of a large-size high-density molybdenum target, which comprises the following steps:
(1) Sieving molybdenum powder to obtain molybdenum powder with the granularity of less than or equal to 3 mu m, then introducing argon gas for annealing at 300 ℃ for 1h, then loading the molybdenum powder into a polyurethane rubber sleeve die, completing a die loading procedure on a vibration platform, sealing an upper rubber plug and a lower rubber plug, then carrying out cold pressing at 200MPa, maintaining the pressure for 40min, then demoulding, and carrying out hot-pressing sintering and machining on the obtained molybdenum blank in a vacuum hot-pressing sintering furnace to obtain a molybdenum blank with the flatness of 0.1mm and the height of 500mm;
the vacuum degree of the hot-pressing sintering is 1 multiplied by 10 -4 Pa, pressure of 30Mpa; the hot-pressing sintering comprises a first hot-pressing sintering and a second hot-pressing sintering which are sequentially carried out;
the first hot-pressing sintering is carried out, the temperature is raised to 800 ℃ at the speed of 8 ℃/min, and the temperature is kept for 3h;
the second hot-pressing sintering is carried out, the temperature is raised to 1200 ℃ at the speed of 3 ℃/min, and the temperature is kept for 3h;
(2) Placing the molybdenum blank in the step (1) into a welded stainless steel sheath, and performing degassing treatment at 750 ℃ until the vacuum degree is 7 x 10 -4 Closing gas after Pa, performing hot isostatic pressing splicing under the pressure of 150Mpa, and cooling to room temperature along with the furnaceThen machining the molybdenum blank, removing the sheath and obtaining a molybdenum target material;
the stainless steel sheath is box-shaped; the inner surface of the stainless steel sheath is subjected to sand blasting treatment, and the roughness of the sand blasting treatment is Ra12 microns;
the hot isostatic pressing splicing comprises a first heat preservation, a second heat preservation and a third heat preservation which are sequentially carried out;
the first heat preservation is carried out, the temperature is raised to 500 ℃ at the speed of 8 ℃/min, and the heat preservation is carried out for 3h;
raising the temperature to 950 ℃ at the second heat preservation speed of 5 ℃/min and preserving the heat for 3h;
and the temperature of the third heat preservation is raised to 1100 ℃ at the speed of 2 ℃/min and is preserved for 3h.
Example 4
The embodiment provides a preparation method of a large-size and high-density molybdenum target, and the conditions are the same as those in the embodiment 1 except that the temperature rise rate of the second hot-pressing sintering in the step (1) is 9 ℃/min.
Example 5
The embodiment provides a preparation method of a large-size and high-density molybdenum target, which is the same as that in the embodiment 1 except that the hot-pressing sintering in the step (1) adopts a one-step sintering method, the temperature is raised to 1400 ℃ at a rate of 9 ℃/min, and the temperature is kept for 5 hours.
Example 6
This example provides a method for preparing a large-size high-density molybdenum target, which is the same as example 1 except that the inner surface of the stainless steel sheath in step (2) is not subjected to sand blasting.
Example 7
This example provides a method for preparing a large-size and high-density molybdenum target, which is the same as that in example 1 except that the degassing temperature in step (2) is 400 ℃.
Example 8
The embodiment provides a preparation method of a large-size and high-density molybdenum target, and the conditions are the same as those in the embodiment 1 except that the hot isostatic pressing splicing pressure in the step (2) is 100 Mpa.
Example 9
The embodiment provides a preparation method of a large-size and high-density molybdenum target, and the conditions are the same as those in the embodiment 1 except that the hot isostatic pressing splicing pressure in the step (2) is 250 Mpa.
Example 10
The embodiment provides a preparation method of a large-size and high-density molybdenum target, and the conditions are the same as those in embodiment 1 except that the heating rates of the second heat preservation and the third heat preservation in step (2) are both 9 ℃/min.
Example 11
The embodiment provides a preparation method of a large-size and high-density molybdenum target, and the conditions are the same as those in embodiment 1 except that the end point temperature of the third heat preservation in step (2) is 1000 ℃.
Example 12
The embodiment provides a preparation method of a large-size and high-density molybdenum target, and the conditions are the same as those in embodiment 1 except that the end point temperature of the third heat preservation in step (2) is 1500 ℃.
Comparative example 1
The comparative example provides a preparation method of a large-size and high-density molybdenum target, and the conditions are the same as those in example 1 except that annealing is not performed in step (1).
Comparative example 2
The comparative example provides a preparation method of a large-size and high-density molybdenum target, and the conditions are the same as those in example 1 except that hot-pressing sintering is not performed in step (1).
The molybdenum targets prepared in the above examples and comparative examples were respectively subjected to target size, grain size and density tests, and the specific results are shown in table 1.
TABLE 1
From table 1 it can be derived:
(1) By adopting the preparation method of the molybdenum target material provided by the embodiment 1-3 of the invention, the size of the obtained molybdenum target material is more than 3000mm, the size of the crystal grain is less than 24 mu m, and the density is as high as more than 99.99 percent;
(2) It can be known from the combination of the embodiment 1 and the embodiments 4 to 5 that when the temperature rising rate of the second hot-pressing sintering is too high or the one-step sintering method is adopted, the temperature rising is faster, so that the internal crystal grains grow too large, and the density of the target material is reduced;
(3) It can be seen from the combination of examples 1 and 6 that, when the inner surface of the sheath is not subjected to sand blasting, although the influence on the grain size and the density of the prepared molybdenum target material is not large, the influence on the purity of the product is large, so that the purity of the molybdenum target material is greatly reduced, and the abrasion problems such as rust and the like occur on the inner wall of the sheath;
(4) It can be seen from the combination of the embodiment 1 and the embodiment 7 that when the degassing treatment temperature is too low, the vacuum degree cannot meet the requirement, and further the crystal grains of the molybdenum target material become large and the density is reduced;
(5) It can be known from the combination of the embodiment 1 and the embodiments 10 to 12 that when the temperature rise rate is unreasonable and the temperature rise end point temperature is too low or too high during the hot isostatic pressing splicing process, the size of the grains of the molybdenum target material cannot be controlled easily, the refinement of the grains cannot be perfected, and the density of the target material is reduced;
(6) It can be known from the combination of the embodiment 1 and the comparative example 1 that when the annealing treatment is not performed, the oxygen content in the molybdenum powder is too high to meet the requirements of the liquid crystal display and touch screen industries; combining example 1 and comparative example 2, it can be seen that when hot-pressing sintering is not performed, hot isostatic pressing splicing is directly performed on the molybdenum blank obtained by cold pressing, so that the crystal grains grow excessively and are distributed in a mixed manner.
The applicant declares that the present invention illustrates the detailed structural features of the present invention through the above embodiments, but the present invention is not limited to the above detailed structural features, that is, it does not mean that the present invention must be implemented depending on the above detailed structural features. It should be understood by those skilled in the art that any modifications of the present invention, equivalent substitutions of selected components of the present invention, additions of auxiliary components, selection of specific modes, etc., are within the scope and disclosure of the present invention.
Claims (10)
1. A preparation method of a large-size high-density molybdenum target is characterized by comprising the following steps:
(1) Sequentially annealing, cold pressing and hot-pressed sintering molybdenum powder to obtain a molybdenum blank;
(2) And (3) placing the molybdenum blank obtained in the step (1) into a welded sheath, and performing hot isostatic pressing splicing to obtain the molybdenum target.
2. The preparation method according to claim 1, wherein the molybdenum powder with the grain size less than or equal to 3 μm is obtained by sieving before the annealing in the step (1).
3. The production method according to claim 1 or 2, wherein the annealing of step (1) is performed under a protective gas;
preferably, the protective gas comprises argon or nitrogen;
preferably, the annealing temperature of the step (1) is 300-350 ℃;
preferably, the annealing time of the step (1) is 0.5-1h.
4. A method of manufacturing as claimed in any one of claims 1 to 3 wherein the cold pressing of step (1) is performed in a gum cover mold;
preferably, the pressure of the cold pressing in the step (1) is 200-300MPa;
preferably, the cold pressing of step (1) has a dwell time of 5-40min.
5. The production method according to any one of claims 1 to 4, wherein the hot press sintering of step (1) is performed in a vacuum hot press sintering furnace;
preferably, the vacuum degree of the hot-pressing sintering in the step (1) is less than 5X 10 -3 Pa；
Preferably, the pressure of the hot-pressing sintering in the step (1) is 30-50MPa;
preferably, the hot-pressing sintering of step (1) includes a first hot-pressing sintering and a second hot-pressing sintering which are performed in sequence;
preferably, the heating rate of the first hot-pressing sintering is 8-10 ℃/min;
preferably, the temperature rise end point of the first hot-pressing sintering is 800-1000 ℃;
preferably, the heat preservation time of the first hot-pressing sintering is 1-3h;
preferably, the heating rate of the second hot-pressing sintering is 3-5 ℃/min;
preferably, the temperature rise end point of the second hot-pressing sintering is 1200-1500 ℃;
preferably, the holding time of the second hot-pressing sintering is 2-3h.
6. The method according to any one of claims 1 to 5, wherein the hot press sintering of step (1) is followed by machining;
preferably, the flatness of the machined molybdenum billet is less than 0.5mm;
preferably, the height of the machined molybdenum billet is 400-500mm.
7. The method according to any one of claims 1 to 6, wherein the sheath in the step (2) is made of stainless steel or low carbon steel;
preferably, the inner surface of the sheath in the step (2) is subjected to sand blasting;
preferably, the grit blasting has a roughness of Ra12-18 μm.
8. The production method according to any one of claims 1 to 7, wherein the hot isostatic pressing splicing in step (2) is preceded by a degassing treatment;
preferably, the temperature of the degassing treatment is 500-750 ℃;
preferably, the degassing treatment has an end-point vacuum of < 5X 10 -3 Pa；
Preferably, the pressure of the hot isostatic pressing splicing in the step (2) is 150-200MPa;
preferably, the hot isostatic pressing splicing in the step (2) comprises a first heat preservation, a second heat preservation and a third heat preservation which are sequentially carried out;
preferably, the temperature rise rate of the first heat preservation is 8-10 ℃/min;
preferably, the temperature rise end point of the first heat preservation is 500-650 ℃;
preferably, the first heat preservation time is 2-3h;
preferably, the temperature rise rate of the second heat preservation is 5-7 ℃/min;
preferably, the temperature rise end point of the second heat preservation is 950-1050 ℃;
preferably, the heat preservation time of the second heat preservation is 2-3h;
preferably, the temperature rise rate of the third heat preservation is 2-3 ℃/min;
preferably, the temperature rise end point of the third heat preservation is 1100-1400 ℃;
preferably, the heat preservation time of the third heat preservation is 2-3h.
9. The method according to any one of claims 1 to 8, wherein the size of the molybdenum target in step (2) is more than 3000mm;
preferably, the density of the molybdenum target material obtained in the step (2) is more than 99.9%.
10. The method for preparing a composite material according to any one of claims 1 to 9, comprising the steps of:
(1) Sieving molybdenum powder to obtain molybdenum powder with the particle size of less than or equal to 3 microns, then annealing for 0.5-1h at 300-350 ℃ under protective gas, then filling the molybdenum powder into a rubber sleeve die, carrying out cold pressing under 200-300MPa and maintaining the pressure for 5-40min, carrying out hot pressing sintering and machining to obtain a molybdenum blank;
the hot-pressing sintering is carried out in a vacuum hot-pressing sintering furnace, and the vacuum degree of the hot-pressing sintering is less than 5 multiplied by 10 -3 Pa, the pressure is 30-50Mpa;
the hot-pressing sintering comprises a first hot-pressing sintering and a second hot-pressing sintering which are sequentially carried out;
the first hot-pressing sintering is carried out, the temperature is raised to 800-1000 ℃ at the speed of 8-10 ℃/min, and the temperature is kept for 1-3h;
the second hot-pressing sintering is carried out, the temperature is raised to 1200-1500 ℃ at the speed of 3-5 ℃/min, and the temperature is kept for 2-3h;
the flatness of the machined molybdenum billet is less than 0.5mm, and the height of the machined molybdenum billet is 400-500mm;
(2) Placing the molybdenum blank in the step (1) into a sheath after welding, and then sequentially degassing at 500-750 ℃ until the vacuum degree is less than 5 multiplied by 10 -3 Pa, and carrying out hot isostatic pressing splicing under the pressure of 150-200Mpa to obtain the molybdenum target material with the size of more than 3000mm and the density of more than 99.9 percent;
the inner surface of the sheath is subjected to sand blasting treatment, and the roughness of the sand blasting treatment is Ra12-18 mu m;
the hot isostatic pressing splicing comprises a first heat preservation, a second heat preservation and a third heat preservation which are sequentially carried out;
the first heat preservation is carried out, the temperature is raised to 500-650 ℃ at the speed of 8-10 ℃/min, and the heat preservation is carried out for 2-3h;
the second heat preservation is carried out, the temperature is raised to 950-1050 ℃ at the speed of 5-7 ℃/min, and the heat preservation is carried out for 2-3h;
and the third heat preservation is carried out, the temperature is raised to 1100-1400 ℃ at the speed of 2-3 ℃/min, and the heat preservation is carried out for 2-3h.
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| CN116835981A (en) * | 2023-07-05 | 2023-10-03 | 宁波江丰电子材料股份有限公司 | Metal oxide target material and preparation method and application thereof |
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| CN111304607A (en) * | 2020-04-03 | 2020-06-19 | 山东格美钨钼材料股份有限公司 | Method for manufacturing molybdenum-titanium alloy target |
| AU2020103694A4 (en) * | 2020-11-26 | 2021-02-04 | Henan University Of Science And Technology | A preparation method of molybdenum target material |
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| 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 |
| CN114939661A (en) * | 2022-05-23 | 2022-08-26 | 安泰天龙(北京)钨钼科技有限公司 | Preparation method of molybdenum alloy tube target material, molybdenum alloy tube target material and application |
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