CN110670032A - Molybdenum-nickel-copper multi-element alloy sputtering target material and preparation method thereof - Google Patents
Molybdenum-nickel-copper multi-element alloy sputtering target material and preparation method thereof Download PDFInfo
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- CN110670032A CN110670032A CN201911037789.7A CN201911037789A CN110670032A CN 110670032 A CN110670032 A CN 110670032A CN 201911037789 A CN201911037789 A CN 201911037789A CN 110670032 A CN110670032 A CN 110670032A
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- HMXCSHJQBPUTDP-UHFFFAOYSA-N [Mo].[Cu].[Ni] Chemical compound [Mo].[Cu].[Ni] HMXCSHJQBPUTDP-UHFFFAOYSA-N 0.000 title claims abstract description 66
- 229910001325 element alloy Inorganic materials 0.000 title claims abstract description 65
- 239000013077 target material Substances 0.000 title claims abstract description 38
- 238000005477 sputtering target Methods 0.000 title claims abstract description 33
- 238000002360 preparation method Methods 0.000 title abstract description 8
- 238000000137 annealing Methods 0.000 claims abstract description 22
- 238000000034 method Methods 0.000 claims abstract description 17
- 238000005245 sintering Methods 0.000 claims abstract description 17
- 238000009694 cold isostatic pressing Methods 0.000 claims abstract description 15
- 238000001513 hot isostatic pressing Methods 0.000 claims abstract description 15
- 238000005098 hot rolling Methods 0.000 claims abstract description 15
- 238000003754 machining Methods 0.000 claims abstract description 8
- 238000002156 mixing Methods 0.000 claims abstract description 8
- 239000010949 copper Substances 0.000 claims abstract description 6
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims description 29
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 24
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 19
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 14
- 239000011812 mixed powder Substances 0.000 claims description 14
- 239000002994 raw material Substances 0.000 claims description 14
- 238000007789 sealing Methods 0.000 claims description 13
- 238000003466 welding Methods 0.000 claims description 9
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 7
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 7
- 229910001069 Ti alloy Inorganic materials 0.000 claims description 7
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 7
- 229910052799 carbon Inorganic materials 0.000 claims description 7
- 238000001816 cooling Methods 0.000 claims description 7
- 238000000227 grinding Methods 0.000 claims description 7
- 238000010438 heat treatment Methods 0.000 claims description 7
- 229910052742 iron Inorganic materials 0.000 claims description 7
- 229910052760 oxygen Inorganic materials 0.000 claims description 7
- 239000001301 oxygen Substances 0.000 claims description 7
- 229910052700 potassium Inorganic materials 0.000 claims description 7
- 239000011591 potassium Substances 0.000 claims description 7
- 238000004321 preservation Methods 0.000 claims description 7
- 229910052751 metal Inorganic materials 0.000 abstract description 16
- 239000002184 metal Substances 0.000 abstract description 16
- 239000000919 ceramic Substances 0.000 abstract description 6
- 239000003566 sealing material Substances 0.000 abstract description 6
- 238000004070 electrodeposition Methods 0.000 abstract description 4
- 238000002844 melting Methods 0.000 abstract description 4
- 230000008018 melting Effects 0.000 abstract description 4
- 238000001465 metallisation Methods 0.000 abstract description 4
- 239000000843 powder Substances 0.000 abstract description 4
- 229910001182 Mo alloy Inorganic materials 0.000 abstract description 2
- 238000000889 atomisation Methods 0.000 abstract description 2
- 230000002035 prolonged effect Effects 0.000 abstract description 2
- 239000000956 alloy Substances 0.000 description 9
- 229910045601 alloy Inorganic materials 0.000 description 7
- 238000001514 detection method Methods 0.000 description 5
- 230000007547 defect Effects 0.000 description 3
- 238000001000 micrograph Methods 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 238000001878 scanning electron micrograph Methods 0.000 description 3
- 229910018054 Ni-Cu Inorganic materials 0.000 description 2
- 229910018481 Ni—Cu Inorganic materials 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 229910000881 Cu alloy Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 238000005538 encapsulation Methods 0.000 description 1
- 230000017525 heat dissipation Effects 0.000 description 1
- 238000000462 isostatic pressing Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 238000012858 packaging process Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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Classifications
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- 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
-
- B22F1/0003—
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/02—Compacting only
- B22F3/04—Compacting only by applying fluid pressure, e.g. by cold isostatic pressing [CIP]
-
- 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
- B22F3/18—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces by using pressure rollers
-
- 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
-
- 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
-
- 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
- B22F2003/247—Removing material: carving, cleaning, grinding, hobbing, honing, lapping, polishing, milling, shaving, skiving, turning the surface
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/24—After-treatment of workpieces or articles
- B22F2003/248—Thermal after-treatment
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- 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
- B22F2999/00—Aspects linked to processes or compositions used in powder metallurgy
Abstract
The invention discloses a molybdenum-nickel-copper multi-element alloy sputtering target material and a preparation method thereof, wherein the molybdenum-nickel-copper multi-element alloy sputtering target material comprises the following components in parts by mass: 5-45% of Ni, 1-10% of Cu and the balance of Mo, wherein the sum of the mass percentages of the components is 100%; the molybdenum-nickel-copper multi-element alloy target material is obtained through mixing, cold isostatic pressing, hot isostatic pressing, sheath removal, one-fire multi-pass hot rolling, annealing, machining and the like. According to the preparation method, the molybdenum-nickel-copper powder is uniformly mixed, so that the situation that a conventional atomization method cannot be adopted due to high melting point of a pure molybdenum alloy is avoided; by setting sintering process parameters, the problem that three metal powders in the multi-element alloy have large difference in melting points and are difficult to sinter is solved; the problems of poor precision and safety caused by ceramic metallization by an electrodeposition method are solved by metallizing a sputtering target; the prepared molybdenum-nickel-copper multi-element alloy sputtering target material has good air tightness, moisture resistance and humidity resistance, high density and high purity, and the service life of the ceramic-metal sealing material is prolonged.
Description
Technical Field
The invention belongs to the technical field of ceramic-metal sealing, and particularly relates to a molybdenum-nickel-copper multi-element alloy sputtering target material and a preparation method of the molybdenum-nickel-copper multi-element alloy sputtering target material.
Background
The study of ceramic-to-metal sealing technology started in 1935, which is a subject that has emerged with the development of vacuum electronic devices. In recent years, with the continuous development of new ceramic materials, the application of ceramic-metal sealing technology also extends to the industries of semiconductor and integrated circuit packaging, laser devices, atomic energy and high-energy physics, aerospace, chemical metallurgy, medical equipment and the like.
Particularly, in recent years, the development of electric automobiles and charging facilities thereof is rapid, the demand of new energy automobile parts is also increased in a blowout mode, and a contactor, which is a key part, plays an indispensable role in the safety and reliability of new energy automobiles. The quality of the packaging process of the ceramic shell and the electrode material of the contactor, namely the sealing and welding process of ceramic and metal, directly influences the quality of the contactor. Therefore, a reliable ceramic-metal sealing process is important. In addition, the encapsulation of the arc extinguish chamber of the dc contactor in the power transmission and distribution network equipment, the welding of the heat sink material and the high-power chip in the high-power device, and the metallization of the ceramic heat dissipation plate all face similar problems.
The film formed by the molybdenum-nickel-copper multi-element alloy material can keep good thermal, electrical and mechanical properties of ceramics, has the advantages of good air tightness, difficult deliquescence and the like, can be welded with metal parts after metallization, can ensure that a device shell has better mechanical property and air tightness, and is a perfect solution for the problem of ceramic-metal connection. However, at present, the ceramic-metal sealing material using molybdenum-nickel-copper multi-element metal as a matrix is mainly realized by an electrodeposition process method, the sealing quality is far different from that of the ceramic-metal sealing material formed by sputtering deposition of a molybdenum-nickel-copper alloy material, and the requirements of precision and safety of products cannot be met.
Disclosure of Invention
The invention aims to provide a molybdenum-nickel-copper multi-element alloy sputtering target material which has good air tightness, moisture resistance and humidity resistance, high density and high purity.
The invention also aims to provide a preparation method of the molybdenum-nickel-copper multi-element alloy sputtering target material, which solves the problems of poor precision and safety of the electrodeposition process.
The technical scheme adopted by the invention is that the molybdenum-nickel-copper multi-element alloy sputtering target material comprises the following components in parts by mass: 5-45% of Ni element, 1-10% of Cu element and the balance of Mo element, wherein the mass fraction percentage of the components is 100%.
The present invention is also characterized in that,
the density of the molybdenum-nickel-copper multi-element alloy sputtering target material is not lower than 9.8g/cm3。
The technical scheme adopted by the invention is that the preparation method of the molybdenum-nickel-copper multi-element alloy sputtering target material comprises the following steps:
step 2, carrying out cold isostatic pressing on the mixed powder in the step 1 to obtain an initial blank;
step 3, putting the initial blank in the step 2 into a titanium alloy sheath, vacuumizing, sealing and welding, then putting into a hot isostatic pressing sintering furnace, and removing the sheath after furnace cooling to obtain a densified blank;
step 4, carrying out one-fire multi-pass hot rolling on the densified blank in the step 4 to obtain a secondary densified blank;
step 5, annealing the secondary densified blank in the step 4 to obtain a molybdenum-nickel-copper multi-element alloy plate;
and 6, machining and grinding the molybdenum-nickel-copper multi-element alloy plate obtained in the step 5 to obtain a molybdenum-nickel-copper multi-element alloy target finished product.
The present invention is also characterized in that,
in the step 1, the mass purity of the molybdenum powder is not less than 99.9 percent, the content of potassium in the molybdenum powder is not more than 40ppm, the content of iron is not more than 20ppm, the content of carbon is not more than 20ppm, and the content of oxygen is not more than 500 ppm;
the mass purity of the nickel powder is not lower than 99.7%;
the mass purity of the copper powder is not lower than 99.9%.
The mixer in the step 1 is a three-dimensional mixer or any one of a V-shaped mixer or a roller mixer.
The cold isostatic pressing parameters in the step 2 are as follows: the pressure is 100MPa-200MPa, and the pressure maintaining time is 5min-20 min.
The parameters of the hot isostatic pressing sintering furnace in the step 3 are as follows: 100MPa-200MPa, the pressure maintaining time is 60min-300min, and the temperature is 1000 ℃ and 1500 ℃.
The parameters of the one-fire multi-pass hot rolling in the step 4 are as follows: the heating temperature is 1100-1200 ℃, the pass deformation rate is 15-25 percent, and the total deformation rate is 30-55 percent.
The annealing parameters in the step 5 are as follows: the annealing temperature is 700 ℃ and 900 ℃, and the heat preservation time is 2-6 h.
In the step 6, the molybdenum-nickel-copper multi-element alloy target finished product consists of the following components in percentage by mass: 5-45% of Ni element, 1-10% of Cu element and the balance of Mo element, wherein the mass fraction percentage of the components is 100%;
the density of the finished product of the molybdenum-nickel-copper multi-element alloy target material is not less than 9.8g/cm3。
The invention has the beneficial effects that:
(1) according to the preparation method of the molybdenum-nickel-copper multi-element alloy sputtering target material, the molybdenum-nickel-copper multi-element alloy powder is uniformly mixed, so that the situation that a conventional atomization method cannot be adopted due to high melting point of single pure molybdenum alloy is avoided; by setting sintering process parameters, the problem that three metal powders in the molybdenum-nickel-copper multi-element alloy have large melting point difference and are difficult to sinter is solved; the problems of poor precision and safety caused by ceramic metallization by the conventional electrodeposition method are solved by metallizing the sputtering target;
(2) the molybdenum-nickel-copper multi-element alloy sputtering target material prepared by the invention has the characteristics of good air tightness, moisture resistance, high density, high purity and the like, prolongs the service life of a ceramic-metal sealing material, and has good practical value.
Drawings
FIG. 1 is a scanning electron microscope image of a Mo-Ni-Cu multi-element alloy sputtering target material prepared in example 1 of the invention;
FIG. 2 is a scanning electron microscope image of a Mo-Ni-Cu multi-element alloy sputtering target material prepared in example 2 of the invention;
fig. 3 is a scanning electron microscope image of the molybdenum-nickel-copper multi-component alloy sputtering target prepared in example 3 of the present invention.
Detailed Description
The present invention will be described in detail below with reference to the accompanying drawings and specific embodiments.
The invention relates to a molybdenum-nickel-copper multi-element alloy sputtering target material which comprises the following components in parts by mass: 5-45% of Ni element, 1-10% of Cu element and the balance of Mo element, wherein the mass fraction percentage of the components is 100%. Wherein the density of the molybdenum-nickel-copper multi-element alloy sputtering target material is not less than 9.8g/cm3. The molybdenum-nickel-copper multi-element alloy sputtering target material meets the requirements of precision and safety of the ceramic-metal sealing material, and the service life of the ceramic-metal sealing material is prolonged.
Example 1
The mass purity of the molybdenum powder is 99.9 percent, the potassium content in the molybdenum powder is 38ppm, the iron content is 15ppm, the carbon content is 13ppm, and the oxygen content is 500 ppm; the mass purity of the nickel powder is not lower than 99.7%; the mass purity of the copper powder is not lower than 99.9%.
Step 2, carrying out cold isostatic pressing on the mixed powder in the step 1 to obtain an initial blank;
the cold isostatic pressing parameters are: the pressure is 100MPa, and the dwell time is 20 min.
Step 3, putting the initial blank in the step 2 into a titanium alloy sheath, vacuumizing, sealing and welding, then putting into a hot isostatic pressing sintering furnace, and removing the sheath after furnace cooling to obtain a densified blank; putting the blank into an isostatic pressing sintering furnace to densify the initial blank at high temperature and high pressure;
the parameters of the hot isostatic pressing sintering furnace are as follows: 100MPa, the pressure maintaining time is 60min, and the temperature is 1500 ℃.
Step 4, carrying out one-fire multi-pass hot rolling on the densified blank in the step 4 to obtain a secondary densified blank;
the parameters of the one-fire multi-pass hot rolling are as follows: the heating temperature is 1100 ℃, the pass deformation rate is 18 percent, and the total deformation rate is 40 percent.
Step 5, annealing the secondary densified blank in the step 4, and eliminating the internal stress of the blank to obtain a molybdenum-nickel-copper multi-element alloy plate;
the annealing parameters are as follows: the annealing temperature is 750 ℃, and the heat preservation time is 4 h.
And 6, machining and grinding the molybdenum-nickel-copper multi-element alloy plate obtained in the step 5 to obtain a molybdenum-nickel-copper multi-element alloy target finished product.
As shown in fig. 1, an SEM image of the prepared mo-ni-cu multi-alloy target product shows that the mo-ni-cu multi-alloy target has uniform particles, close arrangement and fewer hole defects. Through detection, the density of the finished product of the molybdenum-nickel-copper multi-element alloy target material prepared in the embodiment is 9.82g/cm3。
Example 2
The mass purity of the molybdenum powder is 99.9%, the content of potassium in the molybdenum powder is 36ppm, the content of iron is 15ppm, the content of carbon is 15ppm, and the content of oxygen is 470 ppm; the mass purity of the nickel powder is not lower than 99.7%; the mass purity of the copper powder is not lower than 99.9%.
Step 2, carrying out cold isostatic pressing on the mixed powder in the step 1 to obtain an initial blank;
the cold isostatic pressing parameters are: the pressure is 110MPa, and the dwell time is 18 min.
Step 3, putting the initial blank in the step 2 into a titanium alloy sheath, vacuumizing, sealing and welding, then putting into a hot isostatic pressing sintering furnace, and removing the sheath after furnace cooling to obtain a densified blank;
the parameters of the hot isostatic pressing sintering furnace are as follows: 175MPa, the dwell time is 120min, and the temperature is 1250 ℃.
Step 4, carrying out one-fire multi-pass hot rolling on the densified blank in the step 4 to obtain a secondary densified blank;
the parameters of the one-fire multi-pass hot rolling are as follows: the heating temperature is 1100 ℃, the pass deformation rate is 18 percent, and the total deformation rate is 40 percent.
Step 5, annealing the secondary densified blank in the step 4 to obtain a molybdenum-nickel-copper multi-element alloy plate;
the annealing parameters are as follows: the annealing temperature is 750 ℃, and the heat preservation time is 4 h.
And 6, machining and grinding the molybdenum-nickel-copper multi-element alloy plate obtained in the step 5 to obtain a molybdenum-nickel-copper multi-element alloy target finished product.
As shown in fig. 2, an SEM image of the prepared mo-ni-cu multi-alloy target product shows that the mo-ni-cu multi-alloy target has uniform particles, close arrangement and fewer hole defects. Through detection, the density of the finished product of the molybdenum-nickel-copper multi-element alloy target material prepared in the embodiment is 9.80g/cm3。
Example 3
The mass purity of the molybdenum powder is 99.9 percent, the potassium content in the molybdenum powder is 38ppm, the iron content is 18ppm, the carbon content is 10ppm, and the oxygen content is 490 ppm; the mass purity of the nickel powder is not lower than 99.7%; the mass purity of the copper powder is not lower than 99.9%.
Step 2, carrying out cold isostatic pressing on the mixed powder in the step 1 to obtain an initial blank;
the cold isostatic pressing parameters are: the pressure is 120MPa, and the dwell time is 15 min.
Step 3, putting the initial blank in the step 2 into a titanium alloy sheath, vacuumizing, sealing and welding, then putting into a hot isostatic pressing sintering furnace, and removing the sheath after furnace cooling to obtain a densified blank;
the parameters of the hot isostatic pressing sintering furnace are as follows: 200MPa, the pressure maintaining time is 300min, and the temperature is 1100 ℃.
Step 4, carrying out one-fire multi-pass hot rolling on the densified blank in the step 4 to obtain a secondary densified blank;
the parameters of the one-fire multi-pass hot rolling are as follows: the heating temperature is 1130 ℃, the pass deformation rate is 20 percent, and the total deformation rate is 50 percent.
Step 5, annealing the secondary densified blank in the step 4 to obtain a molybdenum-nickel-copper multi-element alloy plate;
the annealing parameters are as follows: the annealing temperature is 800 ℃, and the heat preservation time is 4 h.
And 6, machining and grinding the molybdenum-nickel-copper multi-element alloy plate obtained in the step 5 to obtain a molybdenum-nickel-copper multi-element alloy target finished product.
As shown in fig. 3, an SEM image of the prepared mo-ni-cu multi-alloy target product shows that the mo-ni-cu multi-alloy target has uniform particles, close arrangement and fewer hole defects. Through detection, the density of the finished product of the molybdenum-nickel-copper multi-element alloy target material prepared in the embodiment is 9.82g/cm3。
Example 4
The mass purity of the molybdenum powder is 99.9 percent, the potassium content in the molybdenum powder is 35ppm, the iron content is 15ppm, the carbon content is 18ppm, and the oxygen content is 430 ppm; the mass purity of the nickel powder is not lower than 99.7%; the mass purity of the copper powder is not lower than 99.9%.
Step 2, carrying out cold isostatic pressing on the mixed powder in the step 1 to obtain an initial blank;
the cold isostatic pressing parameters are: the pressure is 150MPa, and the dwell time is 8 min.
Step 3, putting the initial blank in the step 2 into a titanium alloy sheath, vacuumizing, sealing and welding, then putting into a hot isostatic pressing sintering furnace, and removing the sheath after furnace cooling to obtain a densified blank;
the parameters of the hot isostatic pressing sintering furnace are as follows: 120MPa, the pressure maintaining time is 250min, and the temperature is 1350 ℃.
Step 4, carrying out one-fire multi-pass hot rolling on the densified blank in the step 4 to obtain a secondary densified blank;
the parameters of the one-fire multi-pass hot rolling are as follows: the heating temperature is 1130 ℃, the pass deformation rate is 20 percent, and the total deformation rate is 50 percent.
Step 5, annealing the secondary densified blank in the step 4 to obtain a molybdenum-nickel-copper multi-element alloy plate;
the annealing parameters are as follows: the annealing temperature is 800 ℃, and the heat preservation time is 4 h.
And 6, machining and grinding the molybdenum-nickel-copper multi-element alloy plate obtained in the step 5 to obtain a molybdenum-nickel-copper multi-element alloy target finished product.
Through detection, the density of the finished product of the molybdenum-nickel-copper multi-element alloy target material prepared in the embodiment is 9.82g/cm3。
Example 5
The mass purity of the molybdenum powder is 99.9 percent, the potassium content in the molybdenum powder is 38ppm, the iron content is 10ppm, the carbon content is 13ppm, and the oxygen content is 460 ppm; the mass purity of the nickel powder is not lower than 99.7%; the mass purity of the copper powder is not lower than 99.9%.
Step 2, carrying out cold isostatic pressing on the mixed powder in the step 1 to obtain an initial blank;
the cold isostatic pressing parameters are: the pressure is 200MPa, and the dwell time is 5 min.
Step 3, putting the initial blank in the step 2 into a titanium alloy sheath, vacuumizing, sealing and welding, then putting into a hot isostatic pressing sintering furnace, and removing the sheath after furnace cooling to obtain a densified blank;
the parameters of the hot isostatic pressing sintering furnace are as follows: 100MPa, the pressure maintaining time is 300min, and the temperature is 1350 ℃.
Step 4, carrying out one-fire multi-pass hot rolling on the densified blank in the step 4 to obtain a secondary densified blank;
the parameters of the one-fire multi-pass hot rolling are as follows: the heating temperature is 1150 ℃, the pass deformation rate is 23 percent, and the total deformation rate is 46 percent.
Step 5, annealing the secondary densified blank in the step 4 to obtain a molybdenum-nickel-copper multi-element alloy plate;
the annealing parameters are as follows: the annealing temperature is 850 ℃, and the heat preservation time is 3 h.
And 6, machining and grinding the molybdenum-nickel-copper multi-element alloy plate obtained in the step 5 to obtain a molybdenum-nickel-copper multi-element alloy target finished product.
Through detection, the density of the finished product of the molybdenum-nickel-copper multi-element alloy target material prepared in the embodiment is 9.81g/cm3。
Claims (10)
1. The molybdenum-nickel-copper multi-element alloy sputtering target is characterized by comprising the following components in parts by mass: 5-45% of Ni element, 1-10% of Cu element and the balance of Mo element, wherein the mass fraction percentage of the components is 100%.
2. The molybdenum nickel copper multi-element alloy sputtering target material according to claim 1, wherein the density of the molybdenum nickel copper multi-element alloy sputtering target material is not lower than 9.8g/cm3。
3. The method for preparing the molybdenum-nickel-copper multi-element alloy sputtering target material according to claim 1 or 2, which comprises the following steps:
step 1, taking raw materials of molybdenum powder, nickel powder and copper powder, placing the raw materials into a mixer, and uniformly mixing to obtain mixed powder;
step 2, carrying out cold isostatic pressing on the mixed powder in the step 1 to obtain an initial blank;
step 3, putting the initial blank in the step 2 into a titanium alloy sheath, vacuumizing, sealing and welding, then putting into a hot isostatic pressing sintering furnace, and removing the sheath after furnace cooling to obtain a densified blank;
step 4, carrying out one-fire multi-pass hot rolling on the densified blank in the step 4 to obtain a secondary densified blank;
step 5, annealing the secondary densified blank in the step 4 to obtain a molybdenum-nickel-copper multi-element alloy plate;
and 6, machining and grinding the molybdenum-nickel-copper multi-element alloy plate obtained in the step 5 to obtain a molybdenum-nickel-copper multi-element alloy target finished product.
4. The method for preparing the molybdenum-nickel-copper multi-element alloy sputtering target material according to claim 3, wherein the molybdenum powder in the step 1 has a mass purity of not less than 99.9%, a potassium content in the molybdenum powder is not more than 40ppm, an iron content in the molybdenum powder is not more than 20ppm, a carbon content in the molybdenum powder is not more than 20ppm, and an oxygen content in the molybdenum powder is not more than 500 ppm;
the mass purity of the nickel powder is not lower than 99.7%;
the mass purity of the copper powder is not lower than 99.9%.
5. The method for preparing the molybdenum-nickel-copper multi-element alloy sputtering target material according to claim 3, wherein the mixer in the step 1 is a three-dimensional mixer, a V-shaped mixer or a roller mixer.
6. The method for preparing the molybdenum-nickel-copper multi-element alloy sputtering target material according to claim 3, wherein the cold isostatic pressing parameters in the step 2 are as follows: the pressure is 100MPa-200MPa, and the pressure maintaining time is 5min-20 min.
7. The method for preparing the molybdenum-nickel-copper multi-element alloy sputtering target material according to claim 3, wherein the parameters of the hot isostatic pressing sintering furnace in the step 3 are as follows: 100MPa-200MPa, the pressure maintaining time is 60min-300min, and the temperature is 1000 ℃ and 1500 ℃.
8. The method for preparing the molybdenum-nickel-copper multi-element alloy sputtering target material according to claim 3, wherein the parameters of the one-fire multi-pass hot rolling in the step 4 are as follows: the heating temperature is 1100-1200 ℃, the pass deformation rate is 15-25 percent, and the total deformation rate is 30-55 percent.
9. The method for preparing the molybdenum-nickel-copper multi-element alloy sputtering target material according to claim 3, wherein the annealing parameters in the step 5 are as follows: the annealing temperature is 700 ℃ and 900 ℃, and the heat preservation time is 2-6 h.
10. The method for preparing the molybdenum-nickel-copper multi-element alloy sputtering target material according to claim 3, wherein the finished molybdenum-nickel-copper multi-element alloy target material in the step 6 comprises the following components in parts by mass: 5-45% of Ni element, 1-10% of Cu element and the balance of Mo element, wherein the mass fraction percentage of the components is 100%;
the density of the finished product of the molybdenum-nickel-copper multi-element alloy target material is not less than 9.8g/cm3。
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