CN110777343A - Preparation method of molybdenum planar sputtering target - Google Patents
Preparation method of molybdenum planar sputtering target Download PDFInfo
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- CN110777343A CN110777343A CN201911072981.XA CN201911072981A CN110777343A CN 110777343 A CN110777343 A CN 110777343A CN 201911072981 A CN201911072981 A CN 201911072981A CN 110777343 A CN110777343 A CN 110777343A
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- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 title claims abstract description 182
- 229910052750 molybdenum Inorganic materials 0.000 title claims abstract description 138
- 239000011733 molybdenum Substances 0.000 title claims abstract description 138
- 238000005477 sputtering target Methods 0.000 title claims abstract description 35
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 239000013077 target material Substances 0.000 claims abstract description 42
- 238000000034 method Methods 0.000 claims abstract description 28
- 238000000137 annealing Methods 0.000 claims abstract description 22
- 238000005096 rolling process Methods 0.000 claims abstract description 16
- 239000012535 impurity Substances 0.000 claims abstract description 15
- 239000013078 crystal Substances 0.000 claims abstract description 14
- 238000009768 microwave sintering Methods 0.000 claims abstract description 14
- 238000009694 cold isostatic pressing Methods 0.000 claims abstract description 13
- 238000005242 forging Methods 0.000 claims abstract description 13
- 239000002994 raw material Substances 0.000 claims abstract description 13
- 238000010894 electron beam technology Methods 0.000 claims abstract description 12
- 238000002844 melting Methods 0.000 claims abstract description 12
- 230000008018 melting Effects 0.000 claims abstract description 12
- 238000005245 sintering Methods 0.000 claims description 20
- 238000003825 pressing Methods 0.000 claims description 15
- 238000010438 heat treatment Methods 0.000 claims description 8
- 238000003754 machining Methods 0.000 claims description 7
- 238000000746 purification Methods 0.000 claims description 4
- 238000003723 Smelting Methods 0.000 claims description 2
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- 238000005265 energy consumption Methods 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 238000001755 magnetron sputter deposition Methods 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000004663 powder metallurgy Methods 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
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
-
- 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
- B22F3/105—Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B9/00—General processes of refining or remelting of metals; Apparatus for electroslag or arc remelting of metals
- C22B9/16—Remelting metals
- C22B9/22—Remelting metals with heating by wave energy or particle radiation
- C22B9/228—Remelting metals with heating by wave energy or particle radiation by particle radiation, e.g. electron beams
-
- 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
- C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
-
- 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
- B22F3/105—Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding
- B22F2003/1054—Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding by microwave
Abstract
A method for preparing molybdenum planar sputtering target material relates to the technical field of sputtering target material preparation, molybdenum powder with purity more than or equal to 99.95% is selected as raw material, the molybdenum powder is pressed into molybdenum green compact by cold isostatic pressing, and then the molybdenum green compact is sintered into molybdenum slab in a microwave sintering furnace under vacuum condition; and purifying the sintered molybdenum plate blank by using an electron beam melting method, processing the molybdenum plate blank into a molybdenum target material by adopting a processing mode of forging and cogging firstly and then cross rolling, and processing the molybdenum target material into a finished molybdenum sputtering target material according to a specified specification machine after vacuum annealing. The invention has the beneficial effects that: the molybdenum sputtering target material prepared by the invention has the advantages of high purity, low impurity content, high density, fine and uniform crystal grains, certain crystal orientation and excellent performance.
Description
Technical Field
The invention belongs to the technical field of sputtering target preparation, and particularly relates to a preparation method of a molybdenum planar sputtering target.
Background
Molybdenum has been widely used in the field of magnetron sputtering target material coating because of its high melting point, good electrical and thermal conductivity, low thermal expansion coefficient, good corrosion resistance, environmental friendliness and other excellent properties. With the development of modern science and technology, the target material is required to have higher and higher purity, higher density, fine and uniform crystal grains and certain crystal orientation. The molybdenum target material prepared by the traditional powder metallurgy method has the defects of long sintering time, high sintering temperature, high energy consumption, large crystal grains, high impurity content and the like.
Disclosure of Invention
The invention aims to solve the technical problem of providing a preparation method of a molybdenum planar sputtering target, and solves the problems of long sintering time, high sintering temperature, high energy consumption, large crystal grains, high impurity content and the like of a molybdenum target produced by a traditional method.
The technical scheme adopted by the invention for solving the technical problems is as follows: a preparation method of a molybdenum planar sputtering target comprises the following steps:
(1) molybdenum powder with the purity of more than or equal to 99.95 percent is selected as a raw material, and the molybdenum powder is pressed into a molybdenum green body through cold isostatic pressing;
(2) sintering the molybdenum green compact pressed in the step (1) into a molybdenum plate blank in a microwave sintering furnace under a vacuum condition;
(3) purifying the molybdenum plate blank sintered in the step (2) by using an electron beam melting method, so that the purity of the molybdenum plate blank is improved to more than 99.999% from 99.95%, and the content of gas impurities C, N, O is reduced to less than 5 ppm;
and finally, machining the molybdenum plate blank into a molybdenum target material by adopting a machining mode of forging and cogging firstly and then cross rolling, and machining the molybdenum target material into a finished molybdenum sputtering target material according to a specified specification after vacuum annealing.
The granularity of the raw material molybdenum powder selected in the step (1) is 3-4 microns, the content of K in the molybdenum powder is less than or equal to 20ppm, and the content of O in the molybdenum powder is less than or equal to 800 ppm.
When the molybdenum powder is subjected to cold isostatic pressing to form a molybdenum green body in the step (1), the pressing pressure is 180-200 Pa, and the pressure maintaining time is 10-13 min.
The conditions for sintering the molybdenum green compact into the molybdenum plate blank in the step (2) under the vacuum condition of the microwave sintering furnace are as follows: and rapidly heating the molybdenum green body to 1500-1600 ℃, preserving heat for 10-30 min, and sintering to obtain the molybdenum plate blank with the density of more than or equal to 95%.
The molybdenum plate blank subjected to impurity removal and purification by electron beam melting in the step (4) is subjected to crushing of coarse columnar crystals in an initial molybdenum ingot in a forging and cogging manner, and then is subjected to pressure processing by a cross rolling method, wherein the total deformation is 70-90%.
The molybdenum plate blank processed in the step (4) is subjected to vacuum annealing at 1050-1150 ℃ and the vacuum degree of more than or equal to 1.0 multiplied by 10
-3Pa, and keeping the temperature for 1 hour.
The invention has the beneficial effects that: according to the invention, the molybdenum green blank is sintered into the molybdenum plate blank by adopting a microwave sintering method under vacuum, the sintering temperature is low, the time is short, and the purification effect is good by adopting an electronic smelting method for purification; the preparation method solves the problems of long sintering time, high sintering temperature, high energy consumption, large crystal grains and high impurity content of the molybdenum target material produced by the traditional method, and the prepared molybdenum sputtering target material has high purity, low impurity content, high density, fine and uniform crystal grains, certain crystal orientation and excellent performance.
Detailed Description
The following description of specific embodiments (examples) of the present invention will enable those skilled in the art to better understand the present invention.
A preparation method of a molybdenum planar sputtering target material comprises the following specific preparation processes: molybdenum powder with the purity of more than or equal to 99.95 percent is selected as a raw material, and a molybdenum plate blank is prepared through powder filling, cold isostatic pressing and microwave sintering. Further purifying the molybdenum plate blank by electron beam melting to obtain a high-purity molybdenum plate blank with the purity of more than or equal to 99.999 percent; the purified high-purity molybdenum ingot is processed into a molybdenum target material by adopting a pressure processing mode of firstly forging and cogging and then cross rolling, and finally, the molybdenum target material is processed into a finished molybdenum sputtering target material according to a specified specification after vacuum annealing.
Preferably, when molybdenum powder is selected, the molybdenum powder with the particle size of 3-4 microns, uniform particle size, normally distributed particle size, good dispersibility and no obvious agglomeration phenomenon is used as a raw material, and the content of K in the molybdenum powder is less than or equal to 20ppm and the content of O in the molybdenum powder is less than or equal to 800 ppm.
Preferably, when the high-purity molybdenum powder is pressed into a molybdenum plate blank through cold isostatic pressing, the pressing pressure is 180-200 MPa, and the pressure maintaining time is 10-13 min.
Preferably, when the molybdenum green body is sintered to be the molybdenum plate blank in a microwave sintering furnace under the vacuum condition, the sintering temperature is 1500-1600 ℃, and the heat preservation time is 10-30 min.
Preferably, the prepared high-purity molybdenum plate blank is subjected to pressure processing in a mode of forging, cogging and cross rolling to prepare a molybdenum target material, the total deformation is 70-90%, the rolling temperature is 1200-1300 ℃, the rolling pass is 3-4 times, the pass deformation is 20-25%, annealing is performed in a vacuum annealing furnace after rolling is completed, the annealing temperature is 1050-1150 ℃, and the vacuum degree is more than or equal to 1.0 x 10
- 3Pa, and keeping the temperature for 1 hour.
Preferably, machining is carried out according to specified specifications, the purity of the finished molybdenum sputtering target material is more than or equal to 99.999 percent, the density is more than or equal to 99 percent, the C, N, O content is less than 5ppm, the molybdenum sputtering target material has uniform crystal grain size, the average crystal grain is 20-30 μm, and the crystal orientation takes {100} <011> as the preferential texture orientation.
Example 1
A preparation method of a molybdenum planar sputtering target comprises the following steps:
(1) selecting molybdenum powder with the purity of more than or equal to 99.95 percent and the granularity of 3 mu m as a raw material, pressing the molybdenum powder into a molybdenum green body by cold isostatic pressing, wherein the content of K in the molybdenum powder is less than or equal to 20ppm, and the content of O in the molybdenum powder is less than or equal to 800ppm, and the pressing pressure is 180Pa, and the pressure maintaining time is 13 min;
(2) rapidly heating the molybdenum green body to 1500 ℃ in a microwave sintering furnace under a vacuum condition, preserving heat for 30min, and sintering into a molybdenum plate blank with the density of more than or equal to 95%;
(3) purifying the molybdenum plate blank sintered in the step (2) by using an electron beam melting method, so that the purity of the molybdenum plate blank is improved to more than 99.999% from 99.95%, and the content of gas impurities C, N, O is reduced to less than 5 ppm;
(4) finally, the molybdenum plate blank is processed into the molybdenum target material by adopting the processing mode of forging and cogging firstly and then cross rolling, the total deformation is 70 percent, and the molybdenum target material is processed into the finished molybdenum sputtering target material according to a specified specification machine after vacuum annealing, wherein the annealing temperature is 1050 ℃, and the vacuum degree is more than or equal to 1.0 multiplied by 10
-3Pa, and keeping the temperature for 1 hour.
Example 2
A preparation method of a molybdenum planar sputtering target comprises the following steps:
(1) selecting molybdenum powder with the purity of more than or equal to 99.95 percent and the granularity of 4 mu m as a raw material, pressing the molybdenum powder into a molybdenum green body by cold isostatic pressing, wherein the content of K in the molybdenum powder is less than or equal to 20ppm, and the content of O in the molybdenum powder is less than or equal to 800ppm, and the pressing pressure is 200Pa, and the pressure maintaining time is 10 min;
(2) rapidly heating the molybdenum green body to 1600 ℃ in a microwave sintering furnace under vacuum condition, preserving heat for 10min, and sintering into a molybdenum plate blank with the density of more than or equal to 95%;
(3) purifying the molybdenum plate blank sintered in the step (2) by using an electron beam melting method, so that the purity of the molybdenum plate blank is improved to more than 99.999% from 99.95%, and the content of gas impurities C, N, O is reduced to less than 5 ppm;
(4) finally, the molybdenum plate blank is processed into a molybdenum target material by adopting a processing mode of forging and cogging firstly and then cross rolling, the total deformation is 90 percent, and the molybdenum target material is processed into a finished molybdenum sputtering target material by a machine according to the specified specification after vacuum annealing, wherein the annealing temperature is 1150 ℃, and the vacuum degree is more than or equal to 1.0 multiplied by 10
-3Pa, and keeping the temperature for 1 hour.
Example 3
A preparation method of a molybdenum planar sputtering target comprises the following steps:
(1) selecting molybdenum powder with the purity of more than or equal to 99.95 percent and the granularity of 3.5 mu m as a raw material, pressing the molybdenum powder into a molybdenum green body by cold isostatic pressing, wherein the content of K in the molybdenum powder is less than or equal to 20ppm, and the content of O in the molybdenum powder is less than or equal to 800ppm, and the pressing pressure is 190Pa, and the pressure maintaining time is 11 min;
(2) rapidly heating the molybdenum green body to 1550 ℃ in a microwave sintering furnace under a vacuum condition, preserving heat for 20min, and sintering into a molybdenum plate blank with the density of more than or equal to 95%;
(3) purifying the molybdenum plate blank sintered in the step (2) by using an electron beam melting method, so that the purity of the molybdenum plate blank is improved to more than 99.999% from 99.95%, and the content of gas impurities C, N, O is reduced to less than 5 ppm;
(4) finally, the molybdenum plate blank is processed into a molybdenum target material by adopting a processing mode of forging and cogging firstly and then cross rolling, the total deformation is 80 percent, and the molybdenum target material is processed into a finished molybdenum sputtering target material by a machine according to the specified specification after vacuum annealing, wherein the annealing temperature is 1100 ℃, and the vacuum degree is more than or equal to 1.0 multiplied by 10
-3Pa, and keeping the temperature for 1 hour.
Example 4
A preparation method of a molybdenum planar sputtering target comprises the following steps:
(1) selecting molybdenum powder with the purity of more than or equal to 99.95 percent and the granularity of 3.8 mu m as a raw material, pressing the molybdenum powder into a molybdenum green body by cold isostatic pressing, wherein the content of K in the molybdenum powder is less than or equal to 20ppm, and the content of O in the molybdenum powder is less than or equal to 800ppm, and the pressing pressure is 185Pa, and the pressure maintaining time is 12 min;
(2) rapidly heating the molybdenum green body to 1580 ℃ in a microwave sintering furnace under a vacuum condition, preserving heat for 15min, and sintering the molybdenum green body into a molybdenum plate blank with the density of more than or equal to 95%;
(3) purifying the molybdenum plate blank sintered in the step (2) by using an electron beam melting method, so that the purity of the molybdenum plate blank is improved to more than 99.999% from 99.95%, and the content of gas impurities C, N, O is reduced to less than 5 ppm;
(4) finally, the molybdenum plate blank is processed into the molybdenum target material by adopting the processing mode of forging and cogging firstly and then cross rolling, the total deformation is 75 percent, and the molybdenum target material is processed into the finished molybdenum sputtering target material according to a specified specification machine after vacuum annealing, wherein the annealing temperature is 1120 ℃, the vacuum degree is more than or equal to 1.0 multiplied by 10
-3Pa, and keeping the temperature for 1 hour.
Example 5
A preparation method of a molybdenum planar sputtering target comprises the following steps:
(1) selecting molybdenum powder with the purity of more than or equal to 99.95 percent and the granularity of 3.3 mu m as a raw material, pressing the molybdenum powder into a molybdenum green body by cold isostatic pressing, wherein the content of K in the molybdenum powder is less than or equal to 20ppm, and the content of O in the molybdenum powder is less than or equal to 800ppm, and the pressing pressure is 195Pa, and the pressure maintaining time is 11.5 min;
(2) rapidly heating the molybdenum green compact to 1530 ℃ in a microwave sintering furnace under a vacuum condition, preserving heat for 25min, and sintering into a molybdenum plate blank with the density of more than or equal to 95%;
(3) purifying the molybdenum plate blank sintered in the step (2) by using an electron beam melting method, so that the purity of the molybdenum plate blank is improved to more than 99.999% from 99.95%, and the content of gas impurities C, N, O is reduced to less than 5 ppm;
(4) finally, the molybdenum plate blank is processed into the molybdenum target material by adopting the processing mode of forging and cogging firstly and then cross rolling, the total deformation is 85 percent, and the molybdenum target material is processed into the finished molybdenum sputtering target material according to a specified specification machine after vacuum annealing, wherein the annealing temperature is 1080 ℃, the vacuum degree is more than or equal to 1.0 multiplied by 10
-3Pa, and keeping the temperature for 1 hour.
Example 6
A preparation method of a molybdenum planar sputtering target comprises the following steps:
(1) selecting molybdenum powder with the purity of more than or equal to 99.95 percent and the granularity of 3.6 mu m as a raw material, pressing the molybdenum powder into a molybdenum green body by cold isostatic pressing, wherein the content of K in the molybdenum powder is less than or equal to 20ppm, and the content of O in the molybdenum powder is less than or equal to 800ppm, and the pressing pressure is 188Pa, and the pressure maintaining time is 12.5 min;
(2) rapidly heating the molybdenum green body to 1570 ℃ in a microwave sintering furnace under the vacuum condition, preserving heat for 18min, and sintering into a molybdenum plate blank with the density of more than or equal to 95%;
(3) purifying the molybdenum plate blank sintered in the step (2) by using an electron beam melting method, so that the purity of the molybdenum plate blank is improved to more than 99.999% from 99.95%, and the content of gas impurities C, N, O is reduced to less than 5 ppm;
(4) finally, the molybdenum plate blank is processed into the molybdenum target material by adopting the processing mode of forging and cogging firstly and then cross rolling, the total deformation is 78 percent, and the molybdenum target material is processed into the finished molybdenum sputtering target material according to a specified specification machine after vacuum annealing, wherein the annealing temperature is 1090 ℃, and the vacuum degree is more than or equal to 1.0 multiplied by 10
-3Pa, and keeping the temperature for 1 hour.
Claims (6)
1. A preparation method of a molybdenum plane sputtering target is characterized by comprising the following steps: the method comprises the following steps:
(1) molybdenum powder with the purity of more than or equal to 99.95 percent is selected as a raw material, and the molybdenum powder is pressed into a molybdenum green body through cold isostatic pressing;
(2) sintering the molybdenum green compact pressed in the step (1) into a molybdenum plate blank in a microwave sintering furnace under a vacuum condition;
(3) purifying the molybdenum plate blank sintered in the step (2) by using an electron beam melting method, so that the purity of the molybdenum plate blank is improved to more than 99.999% from 99.95%, and the content of gas impurities C, N, O is reduced to less than 5 ppm;
(4) and finally, machining the molybdenum plate blank into a molybdenum target material by adopting a machining mode of forging and cogging firstly and then cross rolling, and machining the molybdenum target material into a finished molybdenum sputtering target material according to a specified specification after vacuum annealing.
2. The method for preparing a molybdenum planar sputtering target according to claim 1, wherein the method comprises the following steps: the granularity of the raw material molybdenum powder selected in the step (1) is 3-4 microns, the content of K in the molybdenum powder is less than or equal to 20ppm, and the content of O in the molybdenum powder is less than or equal to 800 ppm.
3. The method for preparing a molybdenum planar sputtering target according to claim 1, wherein the method comprises the following steps: and (2) when the molybdenum powder is subjected to cold isostatic pressing to form a molybdenum green body in the step (1), the pressing pressure is 180-200 Pa, and the pressure maintaining time is 10-13 min.
4. The method for preparing a molybdenum planar sputtering target according to claim 1, wherein the method comprises the following steps: the conditions for sintering the molybdenum green compact into the molybdenum plate blank in the step (2) under the vacuum condition of the microwave sintering furnace are as follows: and rapidly heating the molybdenum green body to 1500-1600 ℃, preserving heat for 10-30 min, and sintering to obtain the molybdenum plate blank with the density of more than or equal to 95%.
5. The method for preparing a molybdenum planar sputtering target according to claim 1, wherein the method comprises the following steps: and (4) crushing coarse columnar crystals in the initial molybdenum ingot by using a forging cogging mode for the molybdenum plate blank subjected to impurity removal and purification by electron beam smelting, and then performing pressure processing by using a cross rolling method, wherein the total deformation is 70-90%.
6. The method for preparing a molybdenum planar sputtering target according to claim 1, wherein the method comprises the following steps: carrying out vacuum annealing on the molybdenum plate blank processed in the step (4), wherein the vacuum annealing temperature is 1050-1150 ℃, and the vacuum degree is more than or equal to 1.0 multiplied by 10
-3Pa, and keeping the temperature for 1 hour.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111560590A (en) * | 2020-05-25 | 2020-08-21 | 北京工业大学 | Preparation method of target material for microwave sintering cathode coating |
| CN114395700A (en) * | 2022-01-14 | 2022-04-26 | 宁波江丰钨钼材料有限公司 | Molybdenum blank and preparation method and application thereof |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101956159A (en) * | 2010-09-30 | 2011-01-26 | 金堆城钼业股份有限公司 | Method for preparing high-purity molybdenum titanium sputtering target |
| CN103132033A (en) * | 2013-03-26 | 2013-06-05 | 金堆城钼业股份有限公司 | Method for preparing molybdenum target |
| US20130224422A1 (en) * | 2010-06-30 | 2013-08-29 | H.C. Starck, Inc. | Molybdenum containing targets |
| US20150136584A1 (en) * | 2004-08-31 | 2015-05-21 | Brad Lemon | Methods of depositing thin films using molybdenum sputtering targets |
| CN109940158A (en) * | 2019-04-03 | 2019-06-28 | 中南大学 | A kind of quick preparation process of fine grain molybdenum plate |
-
2019
- 2019-11-05 CN CN201911072981.XA patent/CN110777343A/en not_active Withdrawn
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20150136584A1 (en) * | 2004-08-31 | 2015-05-21 | Brad Lemon | Methods of depositing thin films using molybdenum sputtering targets |
| US20130224422A1 (en) * | 2010-06-30 | 2013-08-29 | H.C. Starck, Inc. | Molybdenum containing targets |
| CN101956159A (en) * | 2010-09-30 | 2011-01-26 | 金堆城钼业股份有限公司 | Method for preparing high-purity molybdenum titanium sputtering target |
| CN103132033A (en) * | 2013-03-26 | 2013-06-05 | 金堆城钼业股份有限公司 | Method for preparing molybdenum target |
| CN109940158A (en) * | 2019-04-03 | 2019-06-28 | 中南大学 | A kind of quick preparation process of fine grain molybdenum plate |
Non-Patent Citations (1)
| Title |
|---|
| BACK-KYU LEE,ET AL: "preparation of ultra-high purity cylindrical Mo ingot by Electron Beam drip melting", 《MATERIALS TRANSACTIONS》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111560590A (en) * | 2020-05-25 | 2020-08-21 | 北京工业大学 | Preparation method of target material for microwave sintering cathode coating |
| CN114395700A (en) * | 2022-01-14 | 2022-04-26 | 宁波江丰钨钼材料有限公司 | Molybdenum blank and preparation method and application thereof |
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