CN113174573A - Preparation method of molybdenum-titanium alloy target blank - Google Patents
Preparation method of molybdenum-titanium alloy target blank Download PDFInfo
- Publication number
- CN113174573A CN113174573A CN202110475515.7A CN202110475515A CN113174573A CN 113174573 A CN113174573 A CN 113174573A CN 202110475515 A CN202110475515 A CN 202110475515A CN 113174573 A CN113174573 A CN 113174573A
- Authority
- CN
- China
- Prior art keywords
- treatment
- heat preservation
- molybdenum
- isostatic pressing
- powder
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 229910001069 Ti alloy Inorganic materials 0.000 title claims abstract description 49
- ZPZCREMGFMRIRR-UHFFFAOYSA-N molybdenum titanium Chemical compound [Ti].[Mo] ZPZCREMGFMRIRR-UHFFFAOYSA-N 0.000 title claims abstract description 49
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 238000004321 preservation Methods 0.000 claims abstract description 84
- 239000011812 mixed powder Substances 0.000 claims abstract description 44
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims abstract description 36
- 238000001513 hot isostatic pressing Methods 0.000 claims abstract description 32
- 238000009694 cold isostatic pressing Methods 0.000 claims abstract description 29
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 22
- 238000007872 degassing Methods 0.000 claims abstract description 22
- 238000002156 mixing Methods 0.000 claims abstract description 16
- 230000001681 protective effect Effects 0.000 claims abstract description 16
- 238000000034 method Methods 0.000 claims abstract description 15
- 238000003466 welding Methods 0.000 claims abstract description 5
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 12
- 239000001257 hydrogen Substances 0.000 claims description 12
- 229910052739 hydrogen Inorganic materials 0.000 claims description 12
- 239000002245 particle Substances 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 claims description 3
- 239000013077 target material Substances 0.000 abstract description 9
- 238000003754 machining Methods 0.000 abstract description 5
- 239000010408 film Substances 0.000 description 26
- 230000000052 comparative effect Effects 0.000 description 9
- 239000000463 material Substances 0.000 description 8
- 239000011733 molybdenum Substances 0.000 description 6
- 229910052750 molybdenum Inorganic materials 0.000 description 6
- 239000007787 solid Substances 0.000 description 6
- 239000010409 thin film Substances 0.000 description 5
- 238000004544 sputter deposition Methods 0.000 description 4
- 238000005477 sputtering target Methods 0.000 description 4
- 239000000956 alloy Substances 0.000 description 3
- 150000002500 ions Chemical class 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 239000010936 titanium Substances 0.000 description 3
- 229910016027 MoTi Inorganic materials 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 238000005245 sintering Methods 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
- 238000007792 addition Methods 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 238000006356 dehydrogenation reaction Methods 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000002845 discoloration Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 238000011534 incubation Methods 0.000 description 1
- 238000010884 ion-beam technique Methods 0.000 description 1
- 239000004973 liquid crystal related substance Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- -1 titanium hydride Chemical compound 0.000 description 1
- 229910000048 titanium hydride Inorganic materials 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/3407—Cathode assembly for sputtering apparatus, e.g. Target
- C23C14/3414—Metallurgical or chemical aspects of target preparation, e.g. casting, powder metallurgy
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- 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
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/14—Treatment of metallic powder
- B22F1/142—Thermal or thermo-mechanical treatment
-
- 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
- B22F3/1017—Multiple heating or additional steps
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C14/00—Alloys based on titanium
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C27/00—Alloys based on rhenium or a refractory metal not mentioned in groups C22C14/00 or C22C16/00
- C22C27/04—Alloys based on tungsten or molybdenum
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Physical Vapour Deposition (AREA)
- Powder Metallurgy (AREA)
Abstract
The invention relates to a preparation method of a molybdenum-titanium alloy target blank, which comprises the following steps: (1) performing first heat preservation treatment on molybdenum powder under a protective atmosphere, and then mixing the molybdenum powder with titanium powder to obtain mixed powder; (2) and (2) sequentially carrying out cold isostatic pressing treatment, sheathing treatment, degassing treatment, hot isostatic pressing treatment and second heat preservation treatment on the mixed powder obtained in the step (1) to obtain the molybdenum-titanium alloy target blank. According to the preparation method of the molybdenum-titanium alloy target blank, provided by the invention, through redesigning the preparation process, new heat preservation treatment is introduced at a specific process position, the brittleness of the molybdenum-titanium alloy is reduced, and when the molybdenum-titanium alloy target blank is prepared into a target material through machining and welding, the obtained film has good adhesion performance and low film resistance.
Description
Technical Field
The invention relates to the field of target material preparation, in particular to a preparation method of a molybdenum-titanium alloy target blank.
Background
At present, the conductive film material in the flat panel display is mainly aluminum and copper, and the barrier layer material is mainly molybdenum film formed by using molybdenum as a sputtering target. Practice has shown that molybdenum-titanium alloy is one of the best materials to replace pure molybdenum. Sputtering is one of the main techniques for preparing thin film materials, which utilizes ions generated by an ion source to form ion beam flow with high speed energy through accelerated aggregation in vacuum, bombards the surface of a solid, and the ions and atoms on the surface of the solid generate kinetic energy exchange, so that the atoms on the surface of the solid leave the solid and are deposited on the surface of a substrate, and the bombarded solid is a raw material for preparing a thin film deposited by a sputtering method, and the solid is generally called as a sputtering target material.
The sputtering target is mainly used for a thin film electrode or a thin film wiring material of a flat panel display such as an LCD, a PDP and the like, and the performance thereof is remarkable. With the development of the market, the quality requirements for the film are higher. The quality of the film is inseparable from that of the target, wherein strict requirements on the purity, density, grain size and tissue uniformity of the target are required in electronic and information industries with high requirements on the quality of the target, such as integrated circuits and liquid crystal display screens. Since the corrosion resistance (discoloration) and the adherence (peeling of the film) of the film sputtered from the pure molybdenum target have some problems, researches show that the corrosion resistance, the adherence, the heat resistance and the like of the target can be obviously improved by adding Ti metal into molybdenum, but generally, the molybdenum-titanium alloy has higher oxygen/hydrogen content, so that the material is brittle and is easy to crack in the production process or scrap due to the corner collapse in the machining process, and meanwhile, when the oxygen in the molybdenum-titanium alloy is higher, the sputtered film has higher resistance, so that the reliability of electronic components is reduced, and the higher hydrogen content increases the stress of the sputtered film, and the film is easy to peel off in the processes of etching, washing and the like.
For example, CN105568236A discloses a method for preparing a molybdenum-titanium alloy sputtering target material with high purity, high density and large size, wherein molybdenum and titanium hydride are mainly selected to be mixed, cooled, sintered and rolled to prepare a molybdenum-titanium alloy material, and the hydrogen content in the prepared molybdenum-titanium alloy is easily higher and the service performance of the product is reduced because the hydrogen content in the titanium oxide content cannot be controlled and the dehydrogenation sintering technology is immature. In addition, CN103014638A provides a method for preparing a MoTi target material with improved film peeling and maintained low resistance, which comprises the steps of heat treating a MoTi sintered body mainly containing 20 to 80 atomic% of Ti and the balance of Mo under a pressure of less than 100Pa at 800 ℃ or more for 0.5 hour or more, crushing Mo/Ti powders, mixing and pressure sintering the powders, and obtaining a molybdenum-titanium alloy target material with hydrogen of 5 mass ppm or less.
However, the current molybdenum-titanium alloy material has the problems that the material is brittle when being used for target sputtering, a thin film obtained by sputtering is easy to peel off, the resistivity is high, and the like.
Disclosure of Invention
In view of the problems in the prior art, an object of the present invention is to provide a method for preparing a molybdenum-titanium alloy target blank, which solves the problems of brittle material, easy peeling of a sputtered film and high resistivity of the existing molybdenum-titanium alloy, so that the brittleness of the obtained molybdenum-titanium alloy is reduced, the sputtered film has good adhesion performance, and the film resistance is significantly reduced.
In order to achieve the purpose, the invention adopts the following technical scheme:
the invention provides a preparation method of a molybdenum-titanium alloy target blank, which comprises the following steps:
(1) performing first heat preservation treatment on molybdenum powder under a protective atmosphere, and then mixing the molybdenum powder with titanium powder to obtain mixed powder;
(2) and (2) sequentially carrying out cold isostatic pressing treatment, sheathing treatment, degassing treatment, hot isostatic pressing treatment and second heat preservation treatment on the mixed powder obtained in the step (1) to obtain the molybdenum-titanium alloy target blank.
According to the preparation method of the molybdenum-titanium alloy target blank, provided by the invention, through redesigning the preparation process, new heat preservation treatment is introduced at a specific process position, the brittleness of the molybdenum-titanium alloy is reduced, and when the molybdenum-titanium alloy target blank is prepared into a target material through machining and welding, the obtained film has good adhesion performance and low film resistance.
As a preferred technical scheme of the invention, the protective atmosphere in the step (1) comprises hydrogen.
Preferably, the first heat-preservation temperature in step (1) is 500-.
Preferably, the first heat-preservation treatment in step (1) has a heat-preservation time of 2-3h, such as 2h, 2.1h, 2.2h, 2.3h, 2.4h, 2.5h, 2.6h, 2.7h, 2.8h, 2.9h or 3h, but not limited to the recited values, and other values not recited in the range are also applicable.
In a preferred embodiment of the present invention, the molybdenum powder and the titanium powder in the mixed powder in the step (1) may be, for example, 1:1, 1:1.01, 1:1.02, 1:1.03, 1:1.04, 1:1.05, 1:1.06, 1:1.07, 1:1.08, 1:1.09 or 1:1.1 in terms of atomic percentage content, but are not limited to the above-mentioned values, and other values not listed in this range are also applicable.
Preferably, the mixing time in step (1) is 24-48h, such as 24h, 26h, 28h, 30h, 32h, 34h, 36h, 38h, 40h, 42h, 44h, 46h or 48h, but not limited to the recited values, and other values not recited in the range are also applicable.
As a preferred embodiment of the present invention, the particle size of the molybdenum powder in the mixed powder in the step (1) is 8 to 15 μm, for example, 8 μm, 9 μm, 10 μm, 11 μm, 12 μm, 13 μm, 14 μm or 15 μm, but is not limited to the above-mentioned values, and other values not shown in the above-mentioned range are also applicable.
Preferably, the particle size of the titanium powder in the mixed powder of step (1) is 45-70 μm, for example, 45 μm, 50 μm, 55 μm, 60 μm, 65 μm or 70 μm, but not limited to the values listed, and other values not listed in the range are also applicable.
As a preferred embodiment of the present invention, the cold isostatic pressing treatment in step (2) is carried out at a pressure of 190-250MPa, and may be, for example, 190MPa, 192MPa, 194MPa, 196MPa, 198MPa, 200MPa, 202MPa, 204MPa, 206MPa, 208MPa, 210MPa, 212MPa, 214MPa, 216MPa, 218MPa, 220MPa, 222MPa, 224MPa, 226MPa, 228MPa, 230MPa, 232MPa, 234MPa, 236MPa, 238MPa, 240MPa, 242MPa, 244MPa, 246MPa, 248MPa or 250MPa, but the present invention is not limited thereto, and other values not listed in this range are also applicable.
Preferably, the cold isostatic pressing treatment in step (2) is performed for 5-15min, such as 5min, 6min, 7min, 8min, 9min, 10min, 11min, 12min, 13min, 14min or 15min, but not limited to the recited values, and other values not recited in the range are also applicable.
As a preferable technical scheme of the invention, the sheathing treatment in the step (2) is to place the mixed powder after the cold isostatic pressing treatment in a sheathing and then weld the sheathing.
As a preferred embodiment of the present invention, the temperature of the degassing treatment in the step (2) is 450 ℃ to 700 ℃, for example, 450 ℃, 460 ℃, 470 ℃, 480 ℃, 490 ℃, 500 ℃, 510 ℃, 520 ℃, 530 ℃, 540 ℃, 550 ℃, 560 ℃, 570 ℃, 580 ℃, 590 ℃, 600 ℃, 610 ℃, 620 ℃, 630 ℃, 640 ℃, 650 ℃, 660 ℃, 670 ℃, 680 ℃, 690 ℃ or 700 ℃, but is not limited to the recited values, and other values not recited in the range are also applicable.
Preferably, the degassing treatment in step (2) is terminated at a vacuum degree of < 0.001Pa in the jacket, and may be, for example, 0.0001Pa, 0.0002Pa, 0.0003Pa, 0.0004Pa, 0.0005Pa, 0.0006Pa, 0.0007Pa, 0.0008Pa or 0.0009Pa, but not limited to the above-mentioned values, and other values not listed in this range may be similarly applied.
In a preferred embodiment of the present invention, the holding temperature of hot isostatic pressing in step (2) is 1050-1150 ℃, for example 1050 ℃, 1060 ℃, 1070 ℃, 1080 ℃, 1090 ℃, 1100 ℃, 1110 ℃, 1120 ℃, 1130 ℃, 1140 ℃, or 1150 ℃, but not limited to the above-mentioned values, and other values not listed in the above-mentioned range are also applicable.
Preferably, the hot isostatic pressing pressure in step (2) is 140-180MPa, and may be, for example, 140MPa, 142MPa, 144MPa, 146MPa, 148MPa, 150MPa, 152MPa, 154MPa, 156MPa, 158MPa, 160MPa, 162MPa, 164MPa, 166MPa, 168MPa, 170MPa, 172MPa, 174MPa, 176MPa, 178MPa or 180MPa, etc., but is not limited to the recited values, and other values not recited in this range are equally applicable.
Preferably, the hot isostatic pressing in step (2) is carried out for 4-6h, for example, 4h, 4.2h, 4.4h, 4.6h, 4.8h, 5h, 5.2h, 5.4h, 5.6h, 5.8h or 6h, etc., but not limited to the recited values, and other values not recited in the range are also applicable.
In a preferred embodiment of the present invention, the second heat-retaining treatment in step (2) is performed under a vacuum degree of < 0.005Pa, and may be, for example, 0.004Pa, 0.0038Pa, 0.0036Pa, 0.0034Pa, 0.0032Pa, 0.003Pa, 0.0028Pa, 0.0026Pa, 0.0024Pa, 0.0022Pa, 0.002Pa, 0.0018Pa, 0.0016Pa, 0.0014Pa, 0.0012Pa, 0.001Pa, 0.0008Pa, 0.0006Pa, 0.0004Pa or 0.0002Pa, but not limited to the above-mentioned values, and other values not yet mentioned in this range are also applicable.
Preferably, the second heat-preservation treatment in step (2) is performed at a heat-preservation temperature of 1000-.
Preferably, the second incubation period in step (2) is 2-4h, such as 2h, 2.1h, 2.2h, 2.3h, 2.4h, 2.5h, 2.6h, 2.7h, 2.8h, 2.9h, 3h, 3.1h, 3.2h, 3.3h, 3.4h, 3.5h, 3.6h, 3.7h, 3.8h, 3.9h or 4h, etc., but not limited to the recited values, and other values not recited in this range are also applicable.
According to the technical scheme provided by the invention, the crystal phase of the obtained molybdenum-titanium alloy target blank is optimized by adding a new heat preservation process, so that the brittleness of the molybdenum-titanium alloy is reduced, the adhesion performance of the obtained film is good, and the resistance of the obtained film is obviously reduced due to the optimization of the crystal phase of the alloy target blank after deposition.
As a preferred technical scheme of the invention, the preparation method comprises the following steps:
(1) performing first heat preservation treatment on molybdenum powder under a protective atmosphere, and then mixing the molybdenum powder with titanium powder to obtain mixed powder;
(2) sequentially carrying out cold isostatic pressing treatment, sheathing treatment, degassing treatment, hot isostatic pressing treatment and second heat preservation treatment on the mixed powder obtained in the step (1) to obtain a molybdenum-titanium alloy target blank;
the protective atmosphere of step (1) comprises hydrogen; the heat preservation temperature of the first heat preservation treatment is 500-600 ℃; the heat preservation time of the first heat preservation treatment is 2-3 h; the molybdenum powder and the titanium powder in the mixed powder are 1 (1-1.1) in atomic percentage; the mixing time is 24-48 h; the granularity of the molybdenum powder in the mixed powder is 8-15 mu m; the granularity of the titanium powder in the mixed powder is 45-70 mu m;
the pressure of the cold isostatic pressing treatment in the step (2) is 190-250 MPa; the time of the cold isostatic pressing treatment is 5-15 min; the sheath treatment is to place the mixed powder after the cold isostatic pressing treatment in a sheath and then weld the sheath; the temperature of the degassing treatment is 450-700 ℃; the end point of the degassing treatment is that the vacuum degree in the sheath is less than 0.001 Pa; the heat preservation temperature of the hot isostatic pressing is 1050-1150 ℃; the pressure of the hot isostatic pressing is 140-180 MPa; the hot isostatic pressing time is 4-6 h; the second heat preservation treatment is carried out under the vacuum degree of less than 0.005 Pa; the heat preservation temperature of the second heat preservation treatment is 1000-1200 ℃; the heat preservation time of the second heat preservation treatment is 2-4 h.
Compared with the prior art, the invention at least has the following beneficial effects:
(1) according to the preparation method of the molybdenum-titanium alloy target blank, provided by the invention, through redesigning the preparation process, new heat preservation treatment is introduced at a specific process position, the brittleness of the molybdenum-titanium alloy is reduced, and when the molybdenum-titanium alloy target blank is prepared into a target material through machining and welding, the obtained film has good adhesion performance and low film resistance.
(2) The fracture brittleness of the obtained molybdenum-titanium alloy target blank is more than or equal to 1100MPa, the film adhesive force of the film obtained when the target blank is used for coating is more than or equal to 180N, and the film resistance is less than or equal to 25 mu omega cm.
Detailed Description
To better illustrate the invention and to facilitate the understanding of the technical solutions thereof, typical but non-limiting examples of the invention are as follows:
example 1
The preparation method of the molybdenum-titanium alloy target blank provided by the embodiment comprises the following steps:
(1) performing first heat preservation treatment on molybdenum powder under a protective atmosphere, and then mixing the molybdenum powder with titanium powder to obtain mixed powder;
(2) and (2) sequentially carrying out cold isostatic pressing treatment, sheathing treatment, degassing treatment, hot isostatic pressing treatment and second heat preservation treatment on the mixed powder obtained in the step (1) to obtain the molybdenum-titanium alloy target blank.
The protective atmosphere in the step (1) is hydrogen; the heat preservation temperature of the first heat preservation treatment is 550 ℃; the heat preservation time of the first heat preservation treatment is 2.5 hours; the molybdenum powder and the titanium powder in the mixed powder are 1:1 in atomic percentage; the mixing time is 36 h; the granularity of the molybdenum powder in the mixed powder is 8 mu m; the granularity of the titanium powder in the mixed powder is 45 mu m;
the pressure of the cold isostatic pressing treatment in the step (2) is 220 MPa; the time of the cold isostatic pressing treatment is 10 min; the sheath treatment is to place the mixed powder after the cold isostatic pressing treatment in a sheath and then weld the sheath; the temperature of the degassing treatment is 550 ℃; the end point of the degassing treatment is that the vacuum degree in the sheath is 0.0001 Pa; the heat preservation temperature of the hot isostatic pressing is 11100 ℃; the pressure of the hot isostatic pressing is 160 MPa; the hot isostatic pressing time is 5 h; the second heat preservation treatment is carried out under the vacuum degree of 0.001 Pa; the heat preservation temperature of the second heat preservation treatment is 1100 ℃; the heat preservation time of the second heat preservation treatment is 3 hours.
The properties of the obtained molybdenum-titanium alloy target blank are detailed in table 1.
Example 2
The preparation method of the molybdenum-titanium alloy target blank provided by the embodiment comprises the following steps:
(1) performing first heat preservation treatment on molybdenum powder under a protective atmosphere, and then mixing the molybdenum powder with titanium powder to obtain mixed powder;
(2) and (2) sequentially carrying out cold isostatic pressing treatment, sheathing treatment, degassing treatment, hot isostatic pressing treatment and second heat preservation treatment on the mixed powder obtained in the step (1) to obtain the molybdenum-titanium alloy target blank.
The protective atmosphere of step (1) comprises hydrogen; the heat preservation temperature of the first heat preservation treatment is 500 ℃; the heat preservation time of the first heat preservation treatment is 2 hours; the molybdenum powder and the titanium powder in the mixed powder are 1:1.1 in atomic percentage; the mixing time is 48 hours; the granularity of the molybdenum powder in the mixed powder is 12 mu m; the granularity of the titanium powder in the mixed powder is 55 mu m;
the pressure of the cold isostatic pressing treatment in the step (2) is 250 MPa; the time of the cold isostatic pressing treatment is 5 min; the sheath treatment is to place the mixed powder after the cold isostatic pressing treatment in a sheath and then weld the sheath; the temperature of the degassing treatment is 700 ℃; the end point of the degassing treatment is that the vacuum degree in the sheath is 0.0005 Pa; the heat preservation temperature of the hot isostatic pressing is 1050 ℃; the pressure of the hot isostatic pressing is 140 MPa; the hot isostatic pressing time is 6 h; the second heat preservation treatment is carried out under the vacuum degree of less than 0.003 Pa; the heat preservation temperature of the second heat preservation treatment is 1200 ℃; the heat preservation time of the second heat preservation treatment is 4 hours.
The properties of the obtained molybdenum-titanium alloy target blank are detailed in table 1.
Example 3
The preparation method of the molybdenum-titanium alloy target blank provided by the embodiment comprises the following steps:
(1) performing first heat preservation treatment on molybdenum powder under a protective atmosphere, and then mixing the molybdenum powder with titanium powder to obtain mixed powder;
(2) and (2) sequentially carrying out cold isostatic pressing treatment, sheathing treatment, degassing treatment, hot isostatic pressing treatment and second heat preservation treatment on the mixed powder obtained in the step (1) to obtain the molybdenum-titanium alloy target blank.
The protective atmosphere of step (1) comprises hydrogen; the heat preservation temperature of the first heat preservation treatment is 600 ℃; the heat preservation time of the first heat preservation treatment is 3 hours; the molybdenum powder and the titanium powder in the mixed powder are 1:1 in atomic percentage; the mixing time is 24 hours; the granularity of the molybdenum powder in the mixed powder is 15 mu m; the granularity of the titanium powder in the mixed powder is 70 mu m;
the pressure of the cold isostatic pressing treatment in the step (2) is 190 MPa; the time of the cold isostatic pressing treatment is 15 min; the sheath treatment is to place the mixed powder after the cold isostatic pressing treatment in a sheath and then weld the sheath; the temperature of the degassing treatment is 450 ℃; the end point of the degassing treatment is that the vacuum degree in the sheath is 0.0007 Pa; the heat preservation temperature of the hot isostatic pressing is 1150 ℃; the pressure of the hot isostatic pressing is 180 MPa; the hot isostatic pressing time is 4 h; the second heat preservation treatment is carried out under the vacuum degree less than 0.004 Pa; the heat preservation temperature of the second heat preservation treatment is 1000 ℃; the heat preservation time of the second heat preservation treatment is 2 hours.
The properties of the obtained molybdenum-titanium alloy target blank are detailed in table 1.
Comparative example 1
The difference from example 1 is that the first soaking treatment is not performed, and the properties of the obtained molybdenum-titanium alloy target blank are detailed in table 1.
Comparative example 2
The difference from example 1 is that the second heat-insulating treatment is not performed, and the properties of the obtained molybdenum-titanium alloy target blank are detailed in table 1.
Comparative example 3
The difference from example 1 is only that the hot isostatic pressing pressure is 30MPa and the properties of the obtained molybdenum-titanium alloy target blank are specified in Table 1.
Comparative example 4
The difference from example 1 is that the hot isostatic pressing temperature is 2h, and the properties of the obtained molybdenum-titanium alloy target blank are detailed in table 1.
TABLE 1
| Brittle fracture/MPa | Film adhesion/N | Film resistance/mu omega cm | |
| Example 1 | 1300 | 200 | 25 |
| Example 2 | 1100 | 180 | 23 |
| Example 3 | 1150 | 190 | 22 |
| Comparative example 1 | 800 | 120 | 35 |
| Comparative example 2 | 600 | 100 | 47 |
| Comparative example 3 | 650 | 105 | 49 |
| Comparative example 4 | 570 | 95 | 68 |
According to the results of the embodiment and the comparative example, the molybdenum-titanium alloy prepared by the method has low brittleness by introducing heat preservation treatment at a specific position and adjusting the technological parameters of hot isostatic pressing, and the film prepared by machining and welding the molybdenum-titanium alloy into the target material has good adhesion performance and low film resistance when being coated.
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.
The preferred embodiments of the present invention have been described in detail, however, the present invention is not limited to the specific details of the above embodiments, and various simple modifications may be made to the technical solution of the present invention within the technical idea of the present invention, and these simple modifications are within the protective scope of the present invention.
It should be noted that the various technical features described in the above embodiments can be combined in any suitable manner without contradiction, and the invention is not described in any way for the possible combinations in order to avoid unnecessary repetition.
In addition, any combination of the various embodiments of the present invention is also possible, and the same should be considered as the disclosure of the present invention as long as it does not depart from the spirit of the present invention.
Claims (10)
1. The preparation method of the molybdenum-titanium alloy target blank is characterized by comprising the following steps of:
(1) performing first heat preservation treatment on molybdenum powder under a protective atmosphere, and then mixing the molybdenum powder with titanium powder to obtain mixed powder;
(2) and (2) sequentially carrying out cold isostatic pressing treatment, sheathing treatment, degassing treatment, hot isostatic pressing treatment and second heat preservation treatment on the mixed powder obtained in the step (1) to obtain the molybdenum-titanium alloy target blank.
2. The method of claim 1, wherein the protective atmosphere of step (1) comprises hydrogen;
preferably, the heat preservation temperature of the first heat preservation treatment in the step (1) is 500-600 ℃;
preferably, the heat preservation time of the first heat preservation treatment in the step (1) is 2-3 h.
3. The preparation method according to claim 1 or 2, wherein the molybdenum powder and the titanium powder in the mixed powder in the step (1) are 1 (1-1.1) in terms of atomic percentage;
preferably, the mixing time of step (1) is 24-48 h.
4. The production method according to any one of claims 1 to 3, wherein the particle size of the molybdenum powder in the mixed powder of step (1) is 8 to 15 μm;
preferably, the particle size of the titanium powder in the mixed powder in the step (1) is 45-70 μm.
5. The preparation method according to any one of claims 1 to 4, wherein the pressure of the cold isostatic pressing treatment in step (2) is 190-250 MPa;
preferably, the time of the cold isostatic pressing treatment in the step (2) is 5-15 min.
6. The method according to any one of claims 1 to 5, wherein the sheathing treatment in step (2) is performed by placing the mixed powder after the cold isostatic pressing treatment in a sheathing and then welding the sheathing.
7. The method according to any one of claims 1 to 6, wherein the degassing treatment in step (2) is carried out at a temperature of 450 ℃ to 700 ℃;
preferably, the end point of the degassing treatment in the step (2) is that the vacuum degree in the sheath is less than 0.001 Pa.
8. The method according to any one of claims 1 to 7, wherein the holding temperature for hot isostatic pressing in step (2) is 1050-;
preferably, the pressure of the hot isostatic pressing in the step (2) is 140-180 MPa;
preferably, the hot isostatic pressing time in step (2) is 4-6 h.
9. The production method according to any one of claims 1 to 8, wherein the second heat-insulating treatment in the step (2) is carried out at a vacuum degree of < 0.005 Pa;
preferably, the heat preservation temperature of the second heat preservation treatment in the step (2) is 1000-1200 ℃;
preferably, the heat preservation time of the second heat preservation treatment in the step (2) is 2-4 h.
10. The method of any one of claims 1 to 9, comprising the steps of:
(1) performing first heat preservation treatment on molybdenum powder under a protective atmosphere, and then mixing the molybdenum powder with titanium powder to obtain mixed powder;
(2) sequentially carrying out cold isostatic pressing treatment, sheathing treatment, degassing treatment, hot isostatic pressing treatment and second heat preservation treatment on the mixed powder obtained in the step (1) to obtain a molybdenum-titanium alloy target blank;
the protective atmosphere of step (1) comprises hydrogen; the heat preservation temperature of the first heat preservation treatment is 500-600 ℃; the heat preservation time of the first heat preservation treatment is 2-3 h; the molybdenum powder and the titanium powder in the mixed powder are 1 (1-1.1) in atomic percentage; the mixing time is 24-48 h; the granularity of the molybdenum powder in the mixed powder is 8-15 mu m; the granularity of the titanium powder in the mixed powder is 45-70 mu m;
the pressure of the cold isostatic pressing treatment in the step (2) is 190-250 MPa; the time of the cold isostatic pressing treatment is 5-15 min; the sheath treatment is to place the mixed powder after the cold isostatic pressing treatment in a sheath and then weld the sheath; the temperature of the degassing treatment is 450-700 ℃; the end point of the degassing treatment is that the vacuum degree in the sheath is less than 0.001 Pa; the heat preservation temperature of the hot isostatic pressing is 1050-1150 ℃; the pressure of the hot isostatic pressing is 140-180 MPa; the hot isostatic pressing time is 4-6 h; the second heat preservation treatment is carried out under the vacuum degree of less than 0.005 Pa; the heat preservation temperature of the second heat preservation treatment is 1000-1200 ℃; the heat preservation time of the second heat preservation treatment is 2-4 h.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110475515.7A CN113174573A (en) | 2021-04-29 | 2021-04-29 | Preparation method of molybdenum-titanium alloy target blank |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110475515.7A CN113174573A (en) | 2021-04-29 | 2021-04-29 | Preparation method of molybdenum-titanium alloy target blank |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN113174573A true CN113174573A (en) | 2021-07-27 |
Family
ID=76925478
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202110475515.7A Pending CN113174573A (en) | 2021-04-29 | 2021-04-29 | Preparation method of molybdenum-titanium alloy target blank |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN113174573A (en) |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114029484A (en) * | 2021-11-08 | 2022-02-11 | 宁波江丰电子材料股份有限公司 | Preparation method of tantalum-titanium alloy target material |
| CN115261809A (en) * | 2022-07-25 | 2022-11-01 | 宁波江丰电子材料股份有限公司 | Preparation method of tubular target material |
| CN115433910A (en) * | 2022-09-19 | 2022-12-06 | 宁波江丰电子材料股份有限公司 | Ternary alloy target for flat panel display and preparation method thereof |
| CN115488333A (en) * | 2022-09-27 | 2022-12-20 | 宁波江丰电子材料股份有限公司 | Molybdenum-titanium alloy tube target and preparation method and application thereof |
| CN115502403A (en) * | 2022-09-29 | 2022-12-23 | 宁波江丰电子材料股份有限公司 | Preparation method of large-size and high-density molybdenum target |
| GB2609058A (en) * | 2021-07-19 | 2023-01-25 | Jiangsu Cisri Hipex Tech Co Ltd | Method for producing molybdenum alloy targets |
| CN116377403A (en) * | 2023-04-27 | 2023-07-04 | 西安理工大学 | Preparation method of molybdenum-titanium target |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103014638A (en) * | 2011-09-26 | 2013-04-03 | 日立金属株式会社 | MoTi target material and method for manufacturing for the same |
| CN103849839A (en) * | 2012-12-04 | 2014-06-11 | 光洋应用材料科技股份有限公司 | Aluminum-titanium alloy sputtering target material and production method thereof |
| CN104480446A (en) * | 2014-12-30 | 2015-04-01 | 山东昊轩电子陶瓷材料有限公司 | Molybdenum-titanium alloy target material and production method thereof |
| CN107083528A (en) * | 2009-04-10 | 2017-08-22 | 圣戈班涂敷技术公司 | Molybdenum base target and the method that target is prepared by thermal spray |
| TW201730360A (en) * | 2015-10-27 | 2017-09-01 | 塔沙Ｓｍｄ公司 | Low resistivity tungsten film and tungsten target with improved characteristics |
-
2021
- 2021-04-29 CN CN202110475515.7A patent/CN113174573A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107083528A (en) * | 2009-04-10 | 2017-08-22 | 圣戈班涂敷技术公司 | Molybdenum base target and the method that target is prepared by thermal spray |
| CN103014638A (en) * | 2011-09-26 | 2013-04-03 | 日立金属株式会社 | MoTi target material and method for manufacturing for the same |
| CN103849839A (en) * | 2012-12-04 | 2014-06-11 | 光洋应用材料科技股份有限公司 | Aluminum-titanium alloy sputtering target material and production method thereof |
| CN104480446A (en) * | 2014-12-30 | 2015-04-01 | 山东昊轩电子陶瓷材料有限公司 | Molybdenum-titanium alloy target material and production method thereof |
| TW201730360A (en) * | 2015-10-27 | 2017-09-01 | 塔沙Ｓｍｄ公司 | Low resistivity tungsten film and tungsten target with improved characteristics |
Non-Patent Citations (1)
| Title |
|---|
| 应宗荣主编: "《料科学与工程 材料成形原理与工艺》", 31 January 2005 * |
Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US12043892B2 (en) | 2021-07-19 | 2024-07-23 | Jiangsu CISRI HIPEX Technology Co., Ltd. | Method for producing molybdenum alloy targets |
| GB2609058A (en) * | 2021-07-19 | 2023-01-25 | Jiangsu Cisri Hipex Tech Co Ltd | Method for producing molybdenum alloy targets |
| GB2609058B (en) * | 2021-07-19 | 2023-08-09 | Jiangsu Cisri Hipex Tech Co Ltd | Method for producing molybdenum alloy targets |
| CN114029484B (en) * | 2021-11-08 | 2023-09-12 | 宁波江丰电子材料股份有限公司 | Preparation method of tantalum-titanium alloy target |
| CN114029484A (en) * | 2021-11-08 | 2022-02-11 | 宁波江丰电子材料股份有限公司 | Preparation method of tantalum-titanium alloy target material |
| CN115261809A (en) * | 2022-07-25 | 2022-11-01 | 宁波江丰电子材料股份有限公司 | Preparation method of tubular target material |
| CN115261809B (en) * | 2022-07-25 | 2024-05-14 | 宁波江丰电子材料股份有限公司 | Preparation method of tubular target |
| CN115433910A (en) * | 2022-09-19 | 2022-12-06 | 宁波江丰电子材料股份有限公司 | Ternary alloy target for flat panel display and preparation method thereof |
| CN115488333B (en) * | 2022-09-27 | 2023-12-29 | 宁波江丰电子材料股份有限公司 | Molybdenum-titanium alloy tube target and preparation method and application thereof |
| CN115488333A (en) * | 2022-09-27 | 2022-12-20 | 宁波江丰电子材料股份有限公司 | Molybdenum-titanium alloy tube target and preparation method and application thereof |
| CN115502403A (en) * | 2022-09-29 | 2022-12-23 | 宁波江丰电子材料股份有限公司 | Preparation method of large-size and high-density molybdenum target |
| CN116377403A (en) * | 2023-04-27 | 2023-07-04 | 西安理工大学 | Preparation method of molybdenum-titanium target |
| CN116377403B (en) * | 2023-04-27 | 2024-02-02 | 西安理工大学 | Preparation method of molybdenum-titanium target |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN113174573A (en) | Preparation method of molybdenum-titanium alloy target blank | |
| JP5716768B2 (en) | Oxide sintered body, target, transparent conductive film obtained using the same, and transparent conductive substrate | |
| CN111304606A (en) | Preparation method of defect-free high-purity nickel-vanadium target blank and target prepared by using defect-free high-purity nickel-vanadium target blank | |
| CN113913751B (en) | Cu-high-entropy alloy film and preparation method thereof | |
| CN110539067A (en) | Diffusion welding method for high-purity copper target | |
| JP2024530077A (en) | Molybdenum alloy target material, its preparation method and application | |
| CN114855131A (en) | Preparation method of molybdenum alloy target, molybdenum alloy target and application | |
| CN113073295B (en) | Preparation method and application of tungsten sputtering target blank | |
| CN114075651A (en) | Tantalum-silicon dioxide sputtering target material and preparation method thereof | |
| CN116377403B (en) | Preparation method of molybdenum-titanium target | |
| CN114934202B (en) | Tantalum-molybdenum alloy target material and preparation method and application thereof | |
| CN112501568B (en) | Micro-nano multilayer structure composite material and preparation method and application thereof | |
| WO2017020535A1 (en) | Copper/aluminium alloy crystal oscillation plate coating process | |
| CN113878221A (en) | Method for improving welding quality of tungsten target | |
| CN111088484A (en) | Method for preparing metal oxide film | |
| CN110144483A (en) | A kind of copper magnesium alloy and preparation method thereof | |
| EP4249628A1 (en) | Sputtering target and manufacturing method therefor | |
| KR20220128268A (en) | Sputtering target and manufacturing method thereof | |
| CN111270210B (en) | Ruthenium sputtering target with high oriented crystal grains and preparation method thereof | |
| CN111235536B (en) | Iridium sputtering target with high oriented crystal grains and preparation method thereof | |
| CN115537746B (en) | Aluminum scandium alloy target material and preparation method and application thereof | |
| CN118048546A (en) | Molybdenum alloy sputtering target material and preparation method thereof | |
| CN117139372A (en) | Preparation method of strong-texture high-purity copper target material | |
| CN113957403A (en) | High-strength Al-Cr metallic glass coating and preparation method thereof | |
| CN114855132A (en) | Tantalum-titanium alloy target material and preparation method and application thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20210727 |