CN111850485A - Preparation method of molybdenum alloy target - Google Patents
Preparation method of molybdenum alloy target Download PDFInfo
- Publication number
- CN111850485A CN111850485A CN201910360325.3A CN201910360325A CN111850485A CN 111850485 A CN111850485 A CN 111850485A CN 201910360325 A CN201910360325 A CN 201910360325A CN 111850485 A CN111850485 A CN 111850485A
- Authority
- CN
- China
- Prior art keywords
- isostatic pressing
- powder
- sheath
- molybdenum
- alloy target
- 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
- 229910001182 Mo alloy Inorganic materials 0.000 title claims abstract description 31
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 238000001513 hot isostatic pressing Methods 0.000 claims abstract description 60
- 238000009694 cold isostatic pressing Methods 0.000 claims abstract description 58
- 239000000843 powder Substances 0.000 claims abstract description 56
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims abstract description 40
- 238000000034 method Methods 0.000 claims abstract description 38
- 239000013077 target material Substances 0.000 claims abstract description 34
- 238000002156 mixing Methods 0.000 claims abstract description 28
- 150000001339 alkali metal compounds Chemical class 0.000 claims abstract description 23
- 238000011068 loading method Methods 0.000 claims abstract description 22
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 18
- 229910052708 sodium Inorganic materials 0.000 claims description 18
- 239000011734 sodium Substances 0.000 claims description 18
- PUZPDOWCWNUUKD-UHFFFAOYSA-M sodium fluoride Chemical compound [F-].[Na+] PUZPDOWCWNUUKD-UHFFFAOYSA-M 0.000 claims description 12
- 235000015393 sodium molybdate Nutrition 0.000 claims description 12
- 239000011684 sodium molybdate Substances 0.000 claims description 12
- TVXXNOYZHKPKGW-UHFFFAOYSA-N sodium molybdate (anhydrous) Chemical compound [Na+].[Na+].[O-][Mo]([O-])(=O)=O TVXXNOYZHKPKGW-UHFFFAOYSA-N 0.000 claims description 12
- 239000011261 inert gas Substances 0.000 claims description 10
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 7
- 229910002804 graphite Inorganic materials 0.000 claims description 7
- 239000010439 graphite Substances 0.000 claims description 7
- 239000000463 material Substances 0.000 claims description 7
- 150000003388 sodium compounds Chemical class 0.000 claims description 7
- 235000013024 sodium fluoride Nutrition 0.000 claims description 6
- 239000011775 sodium fluoride Substances 0.000 claims description 6
- 238000002844 melting Methods 0.000 claims description 5
- 230000008018 melting Effects 0.000 claims description 5
- 229910052750 molybdenum Inorganic materials 0.000 claims description 5
- 239000011733 molybdenum Substances 0.000 claims description 5
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims description 3
- 229910052721 tungsten Inorganic materials 0.000 claims description 3
- 239000010937 tungsten Substances 0.000 claims description 3
- 229910052783 alkali metal Inorganic materials 0.000 abstract description 11
- 238000005245 sintering Methods 0.000 description 15
- 229910000528 Na alloy Inorganic materials 0.000 description 12
- QMXBEONRRWKBHZ-UHFFFAOYSA-N [Na][Mo] Chemical compound [Na][Mo] QMXBEONRRWKBHZ-UHFFFAOYSA-N 0.000 description 12
- 239000011230 binding agent Substances 0.000 description 12
- 239000002270 dispersing agent Substances 0.000 description 11
- 238000000465 moulding Methods 0.000 description 10
- 239000002002 slurry Substances 0.000 description 10
- 239000010935 stainless steel Substances 0.000 description 10
- 229910001220 stainless steel Inorganic materials 0.000 description 10
- 238000004321 preservation Methods 0.000 description 8
- 150000001340 alkali metals Chemical class 0.000 description 6
- 239000002775 capsule Substances 0.000 description 6
- 238000010438 heat treatment Methods 0.000 description 6
- PQXKHYXIUOZZFA-UHFFFAOYSA-M lithium fluoride Chemical compound [Li+].[F-] PQXKHYXIUOZZFA-UHFFFAOYSA-M 0.000 description 6
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 5
- 230000007797 corrosion Effects 0.000 description 5
- 238000005260 corrosion Methods 0.000 description 5
- 239000007788 liquid Substances 0.000 description 5
- 229910052700 potassium Inorganic materials 0.000 description 5
- 239000011591 potassium Substances 0.000 description 5
- 238000007789 sealing Methods 0.000 description 5
- 238000004544 sputter deposition Methods 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- 238000003466 welding Methods 0.000 description 5
- 238000000280 densification Methods 0.000 description 4
- 238000003754 machining Methods 0.000 description 4
- KTSFMFGEAAANTF-UHFFFAOYSA-N [Cu].[Se].[Se].[In] Chemical compound [Cu].[Se].[Se].[In] KTSFMFGEAAANTF-UHFFFAOYSA-N 0.000 description 3
- 238000011049 filling Methods 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- MEFBJEMVZONFCJ-UHFFFAOYSA-N molybdate Chemical compound [O-][Mo]([O-])(=O)=O MEFBJEMVZONFCJ-UHFFFAOYSA-N 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- 239000012798 spherical particle Substances 0.000 description 3
- 238000005477 sputtering target Methods 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 229910000799 K alloy Inorganic materials 0.000 description 2
- 229910000733 Li alloy Inorganic materials 0.000 description 2
- 239000002202 Polyethylene glycol Substances 0.000 description 2
- MOOYSSSIVSFZQA-UHFFFAOYSA-N [Li].[Mo] Chemical compound [Li].[Mo] MOOYSSSIVSFZQA-UHFFFAOYSA-N 0.000 description 2
- VYKYLQRTMKIQFY-UHFFFAOYSA-N [Mo].[K] Chemical compound [Mo].[K] VYKYLQRTMKIQFY-UHFFFAOYSA-N 0.000 description 2
- 238000000498 ball milling Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 239000008367 deionised water Substances 0.000 description 2
- 229910021641 deionized water Inorganic materials 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000005242 forging Methods 0.000 description 2
- 239000001989 lithium alloy Substances 0.000 description 2
- 150000002642 lithium compounds Chemical class 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000011812 mixed powder Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 229920001223 polyethylene glycol Polymers 0.000 description 2
- 150000003112 potassium compounds Chemical class 0.000 description 2
- NROKBHXJSPEDAR-UHFFFAOYSA-M potassium fluoride Chemical compound [F-].[K+] NROKBHXJSPEDAR-UHFFFAOYSA-M 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- ZTQSAGDEMFDKMZ-UHFFFAOYSA-N Butyraldehyde Chemical compound CCCC=O ZTQSAGDEMFDKMZ-UHFFFAOYSA-N 0.000 description 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
- 239000004372 Polyvinyl alcohol Substances 0.000 description 1
- 229920002125 Sokalan® Polymers 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 229910000573 alkali metal alloy Inorganic materials 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000005056 compaction Methods 0.000 description 1
- 238000007596 consolidation process Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000005429 filling process Methods 0.000 description 1
- 239000010408 film Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000005469 granulation Methods 0.000 description 1
- 230000003179 granulation Effects 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 238000001192 hot extrusion Methods 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 229920003063 hydroxymethyl cellulose Polymers 0.000 description 1
- 229940031574 hydroxymethyl cellulose Drugs 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 238000000462 isostatic pressing Methods 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- NMHMDUCCVHOJQI-UHFFFAOYSA-N lithium molybdate Chemical compound [Li+].[Li+].[O-][Mo]([O-])(=O)=O NMHMDUCCVHOJQI-UHFFFAOYSA-N 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 239000004584 polyacrylic acid Substances 0.000 description 1
- 229920002451 polyvinyl alcohol Polymers 0.000 description 1
- 235000003270 potassium fluoride Nutrition 0.000 description 1
- 239000011698 potassium fluoride Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 230000003746 surface roughness Effects 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/3407—Cathode assembly for sputtering apparatus, e.g. Target
- C23C14/3414—Metallurgical or chemical aspects of target preparation, e.g. casting, powder metallurgy
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/02—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
-
- 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
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/14—Metallic material, boron or silicon
-
- 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
- B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
- B22F2998/10—Processes characterised by the sequence of their steps
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Fluid Mechanics (AREA)
- Powder Metallurgy (AREA)
Abstract
The invention discloses a preparation method of a molybdenum alloy target, which comprises the following steps: mixing molybdenum powder and alkali metal compound powder in proportion; loading the uniformly mixed molybdenum powder and alkali metal compound powder into a cold isostatic pressing die, and carrying out cold isostatic pressing to obtain a target blank; putting the target blank into a sheath, vacuumizing the sheath, and performing hot isostatic pressing; removing the sheath to obtain the molybdenum alloy target material. Compared with the prior art, the preparation method of the molybdenum alloy target provided by the invention has the following advantages: the sheath is used for avoiding the loss of alkali metal elements during hot isostatic pressing, and the combination of the cold isostatic pressing process and the hot isostatic pressing process improves the compactness and the shrinkage uniformity of the target material to the maximum extent.
Description
Technical Field
The invention relates to the field of target preparation, in particular to a molybdenum alloy target preparation method.
Background
In recent years, with the increasing development of sputtering targets and sputtering technologies, the sputtering targets play an increasingly important role in the sputtering technology, and the quality of the sputtering targets directly affects the film formation quality after sputtering. The molybdenum-based alkali metal alloy target material (hereinafter, referred to as molybdenum alloy target material) formed by molybdenum and alkali metal source is used as an important raw material in the sputtering process route of the copper indium gallium selenide solar cell, and is mainly used for providing the alkali metal source for improving the efficiency of the copper indium gallium selenide solar cell. Therefore, the photoelectric conversion efficiency of the solar cell is directly influenced by the quality of the performance of the molybdenum alloy target material.
The existing preparation method of the molybdenum alloy target mainly comprises the steps of adding an alkali metal compound into a molybdenum-based target, and sintering at a high temperature to realize doping of a sodium element, but the alkali metal compound is easy to volatilize during high-temperature sintering in the preparation process, so that the alkali metal element is lost. In addition, doping of the alkali metal compound generally results in poor target compactness and affects the performance of the molybdenum alloy target.
Disclosure of Invention
In order to solve the problems of alkali metal element loss and poor compactness of the molybdenum alloy target material in the preparation process of the molybdenum alloy target material, the invention provides a preparation method of the molybdenum alloy target material.
The preparation method of the molybdenum alloy target material provided by the invention comprises the following steps:
mixing molybdenum powder and alkali metal compound powder in proportion;
loading the uniformly mixed molybdenum powder and alkali metal compound powder into a cold isostatic pressing die, and carrying out cold isostatic pressing to obtain a target blank;
putting the target blank into a sheath, vacuumizing the sheath, and performing hot isostatic pressing;
removing the sheath to obtain the molybdenum alloy target material.
Compared with the prior art, the preparation method of the molybdenum alloy target material has the following advantages: by using the sheath during hot isostatic pressing, the hot isostatic pressing process can be carried out in a closed environment, so that the loss of alkali metal elements is avoided, the combination of the cold isostatic pressing process and the hot isostatic pressing process is realized, firstly, the target blank is preliminarily molded and densified through the cold isostatic pressing process, and the densification of the target is further improved through the hot isostatic pressing process, so that the compactness of the target is improved to the maximum extent.
Drawings
The accompanying drawings are included to provide a further understanding of the embodiments of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the example serve to explain the principles of the invention and not to limit the invention.
Fig. 1 is a flow chart illustrating a method for preparing a molybdenum alloy target according to an embodiment of the present invention;
FIG. 2 is a schematic view of a support member inside a jacket according to an embodiment of the present invention;
FIG. 3 is a cross-sectional view of a support member according to an embodiment of the present invention;
fig. 4 is a cross-sectional structural view of a support member according to an embodiment of the present invention.
Reference numerals: 10-support, 20-capsule, 30-target blank.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the drawings of the embodiments of the present invention. It is to be understood that the embodiments described are only a few embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the described embodiments of the invention without any inventive step, are within the scope of protection of the invention.
As shown in fig. 1, a method for preparing a molybdenum alloy target provided by an embodiment of the present invention includes:
step S01: mixing molybdenum powder and alkali metal compound powder in certain proportion.
According to the specification requirements of the target product, molybdenum powder with corresponding purity and granularity is selected, the purity of the molybdenum powder is usually more than or equal to 99.95%, and the Fisher granularity of the molybdenum powder is 1.0-20 μm.
The melting point of the alkali metal compound is higher than 600 ℃, so that the local melting and precipitation of the alkali metal compound possibly caused by the condition of preparing the (copper indium gallium selenide) thin-film solar cell or the heat treatment in the sputtering link can be effectively avoided, and the performance of the chip is further influenced. The alkali metal compound with the melting point higher than 600 ℃ can be any one of a potassium compound, a lithium compound or a sodium compound, or a mixture of two of the three compounds, or a mixture of the three compounds. Wherein, the potassium compound can be potassium fluoride or potassium molybdate, the lithium compound can be lithium fluoride or lithium molybdate, and the sodium compound can be sodium molybdate or sodium fluoride. Wherein, the mass fraction of the sodium element is 0.5-5.0% of the sodium compound, namely the mass of the sodium element accounts for 0.5-5.0% of the total mass of the molybdenum powder and the sodium compound powder. Preferably, the mass fraction of the sodium element is 1.0-3.0%.
Molybdenum powder and alkali metal compound powder with corresponding mass are weighed, the two powders are mixed uniformly by a way of directly and mechanically mixing in a powder mixer, and in order to avoid the increase of the oxygen content of the molybdenum powder and the formation of crystals of part of the alkali metal compound powder in the powder mixing process, inert gas can be filled in the powder mixer for protection. The powder mixing time can be adjusted according to different powder treatment amounts and different powder mixing powers.
The two kinds of powder can be mixed by adopting a slurry preparation mode, namely, the two kinds of powder and a liquid medium are prepared into slurry under the condition that a dispersing agent and a binder exist, and the liquid medium can be selected from deionized water, ethanol, acetone and the like; then adding the prepared slurry into a high-speed ball mill for ball milling for a certain time, thereby ensuring the uniformity of a sodium source, a dispersing agent and a binder in the slurry; further, the slurry after ball milling treatment can be prepared into spherical particles with the particle size of 50-500 μm by adopting a spray granulation process, wherein the spherical particles are formed by uniformly mixing alkali metal compound powder and molybdenum powder.
In the process of preparing the mixed powder in the slurry mode, the dispersing agent is beneficial to improving the solid solubility of the mixed powder in liquid, and the binding agent is beneficial to improving the strength of a blank in the subsequent forming operation. Because a proper amount of dispersant and binder are added in the slurry preparation process, and the dispersant and the binder need to be removed before the hot isostatic pressing treatment after the cold isostatic pressing treatment step, the dispersant and the binder are C, H, O organics which can be removed by heating to a certain temperature (such as the temperature of hot isostatic pressing) and keeping the temperature for a certain time (such as the holding time of hot isostatic pressing), wherein the dispersant can be polyacrylic acid and salts thereof, hydroxymethyl cellulose salt and the like, and the binder can be polyvinyl alcohol, polyethylene glycol butyral.
Step S02: and (3) loading the uniformly mixed molybdenum powder and alkali metal compound powder into a cold isostatic pressing die, and carrying out cold isostatic pressing to obtain a target blank.
The isostatic pressing technique is a technique for molding a product in a closed container under an ultrahigh pressure state having a uniform pressure. Cold isostatic pressing and hot isostatic pressing can be classified according to the temperature during forming and consolidation. Wherein, the cold isostatic pressing refers to that at normal temperature, liquid is used as a pressure medium, the cold isostatic pressing is mainly used for powder material forming, and a target blank is provided for further sintering, forging or hot isostatic pressing procedures. Specifically, the cold isostatic pressing treatment pressure is 100MPa to 240MPa, and may be, for example, 100MPa, 140MPa, 180MPa, 200MPa, or 240 MPa. The temperature is normal temperature, and the pressure holding time is 0.5h-1 h. For example, it may be 0.5h, 0.6h, 0.7h, 0.8h, 0.9h, 1 h.
The target includes a planar target and a tubular target. Generally, in the preparation process of the tubular target material, the cold isostatic pressing adopts a mode of directly filling powder in a tubular mold containing a rigid target core, and the compaction treatment is continuously carried out in the filling process, so that the uniformity of powder filling is ensured, and gaps among powder materials are avoided. Wherein, the material of the mould can be selected from rubber or plastic.
After the cold isostatic pressing treatment is finished, the tubular target blank with the relative density of 60-75% can be obtained. Therefore, the target blank can be subjected to preliminary molding and densification treatment, and the tubular target blank is provided for the subsequent hot isostatic pressing process.
Step S03: and (3) loading the target blank into a sheath, vacuumizing the sheath, and performing hot isostatic pressing.
The hot isostatic pressing process places the product in a closed container, and generally, high-pressure gas is introduced into the container to apply equal pressure to the product and high temperature, so that the product is sintered and densified under the action of high temperature and high pressure. Specifically, the pressure of the hot isostatic pressing treatment is 100MPa to 240MPa, and may be, for example, 100MPa, 140MPa, 180MPa, 200MPa, or 240 MPa. The temperature may be 1000 ℃ to 1550 ℃, for example, 1000 ℃, 1100 ℃, 1200 ℃, 1300 ℃, 1400 ℃ and 1550 ℃. The temperature holding time is 2h-10 h. For example, the reaction time can be 2h, 4h, 5h, 8h, 9h and 10 h.
Specifically, the operation flow of hot isostatic pressing is as follows:
(1) and (4) charging. And manufacturing a target sheath meeting the conditions according to the shrinkage condition of the target blank obtained by cold isostatic pressing, and loading the target blank obtained by cold isostatic pressing into the sheath.
The jacket material is generally stainless steel or titanium, depending on the sintering temperature, and the wall thickness of the jacket is 1.0mm to 3.0mm, for example 1.0mm, 1.5mm, 2.0mm, 2.5mm, 3.0 mm. The inside and outside of the sheath are required to be smooth and have no burrs and bulges.
(2) And (7) welding and sealing. And (4) performing welding sealing operation on the welding sealing opening reserved in the sheath to ensure that the sealing is completely welded and sealed. The thin tube channel for vacuum pumping does not need to be sealed by welding.
(3) Heating and vacuumizing. And (3) placing the sheath with the target blank in a box body or a hearth for heating, and connecting a reserved vacuum thin tube into a vacuum pump for vacuumizing operation. Starting a heating program and carrying out vacuumizing operation until a preset temperature is reached and the vacuum degree reaches 10-3And when the Pa is not fluctuated any more, performing welding and sealing operation on the reserved vacuum thin tube. The predetermined temperature is generally required to be higher than 200 ℃ and lower than the melting point of the alkali metal compound. If sodium molybdate is selected as the alkali metal compound, the predetermined temperature may be in the range of 200 ℃ to 687 ℃.
(4) And (4) performing hot isostatic pressing operation. And (3) placing the sealed target blank sheath on a working platform of hot isostatic pressing equipment, and heating and filling inert gas such as argon according to a set heating program. The hot isostatic pressing temperature is 1000-1550 ℃, the pressure in the cavity is 100-200 MPa, and the heat preservation time is controlled to be 2-10 h according to the size of the workpiece. And after the heat preservation is finished, cooling according to the set temperature, and finishing the hot isostatic pressing operation process.
After the hot isostatic pressing equipment reaches a set temperature, the mechanical strength of a sheath material is reduced, the sheath is rapidly shrunk by the pressure difference between the inside and the outside of the wall of the sheath, and pressure is transmitted to an internal target blank, so that the rapid densification of the target blank is realized, the compactness of the target material is improved, for the target material, the relative density of the target blank is improved from 60-75% after cold isostatic pressing to more than 98% after hot isostatic pressing sintering, and the target blank sintering process can be obviously shrunk. Meanwhile, the sheath is a closed container, so that volatilization of alkali metal elements in the liquid phase alkali metal source is limited to the maximum extent, and the content of the alkali metal elements is effectively controlled. In addition, the hot isostatic pressing can also avoid the defects of mechanical cracks and the like in the target blank caused by improving the relative density of the target blank by adopting the traditional hot extrusion or forging and pressing and the like.
For the preparation of the tubular target, the target blank obtained by cold isostatic pressing is a tubular target blank, and then the tubular target blank is put into a tubular jacket. The hot isostatic pressing sintering process of the tubular target blank is generally vertical. Due to the influence of the rigid sheath structure and the gravity of the target blank, the conditions of large middle shrinkage and small upper and lower shrinkage of the tubular target blank after sintering are generally shown, irregular deformation increases the machining loss of the target blank and influences the size of the target blank, so how to control the shrinkage uniformity of the tubular target blank in the sintering process is a difficult point of the hot isostatic pressing process.
Optionally, as shown in fig. 2, the interior of the wrap 20 has a support 10. I.e. when the hot isostatic pressing is performed, the support 10 is inserted inside the capsule 20.
As shown in fig. 2-4, a rigid support 10 is inserted into the jacket 20, the support 10 being a column having a longitudinal length greater than or equal to the length of the jacket 20. The lateral dimension of the support 10 should be smaller than the lateral dimension of the capsule 20 so as to leave a gap for shrinkage after sintering of the target blank 30. The addition of the support member 10 can effectively reduce the problem of uneven shrinkage of the target blank 30 during sintering process caused by the structural influence of the rigid capsule 20 and the self-gravity of the target blank 30. Meanwhile, considering that the target blank 30 wraps the rigid support member 10 after sintering is completed, the difficulty of separating the target blank 30 from the support member 10 is increased.
The supporting member 10 may adopt the structure shown in fig. 3, and the cross section of the supporting member 10 is circular with a protrusion, and the protrusion may be triangular, and may also be in other shapes, such as rectangular, semicircular, etc. The number of the protrusions is multiple, such as 10, 12, 15, 16, 20, 30, etc. The structure of the supporting member 10 can also be the structure shown in fig. 4, and the cross section of the supporting member 10 is a regular polygon, such as a regular pentagon, a regular hexagon, a regular heptagon, a regular octagon, a regular decagon, etc.
After the target blank 30 is sintered, the support 10 is in line-to-surface contact with the inner side wall of the capsule 20, and after the sintering is finished, the difficulty in separating the target blank 30 from the support 10 can be reduced. It is understood that other configurations of the support 10 are possible, other than a circular or regular polygon with protrusions in the cross-section of the support 10, as long as the line-to-plane contact between the support 10 and the inner sidewall of the capsule 20 after sintering of the target blank 30 is achieved.
Instead of the solid cylinder shown in fig. 3 and 4, the support 10 may be a tubular cylinder of a hollow structure, i.e., a cylinder having a cross-section of a ring-shaped structure. In particular, the solid support 10 may be selected from graphite supports 10. The support 10 with a hollow structure can be made of stainless steel, molybdenum or tungsten, and the thickness of the tube with the hollow structure is more than or equal to 2 mm.
Step S04: removing the sheath of the target blank formed by hot isostatic pressing to obtain the molybdenum alloy target material.
And removing the outer deformed metal sheath from the target blank subjected to hot isostatic pressing forming by adopting a mechanical processing or chemical corrosion method to obtain the target blank for mechanical processing. And then machining the target blank into a corresponding specification and surface roughness by adopting a numerical control lathe according to actual production requirements.
The preparation method of the molybdenum alloy target has the following advantages:
(1) the introduction of the metal sheath material solves the problem of serious volatilization of alkali metal elements in the densification process of the target blank, and the content of the alkali metal after the target blank is sintered is stably maintained in a reasonable range.
(2) In the technical scheme, cold isostatic pressing is firstly adopted to obtain a target blank with the relative density of 60-75%, and then hot isostatic pressing operation is carried out, so that the compactness and the shrinkage uniformity of the target material are improved. If the powder is directly filled into a metal sheath for hot isostatic pressing operation, the designed sheath size is required to be far larger than the size required by the cold isostatic pressing target blank, which means that the sheath deforms more in the hot isostatic pressing process. Although the sheath can deform under the action of high temperature and high pressure in the hot isostatic pressing cavity so as to compact the target blank, the larger deformation of the sheath can influence the improvement of the compactness of the target blank and the uniformity of shrinkage, and the mechanical processing loss and the processing difficulty of the target blank in the subsequent process are increased.
(3) The uniformity of sintering shrinkage of the target blank is improved by adding the rigid supporting piece with a special section shape in the sheath, and the processing loss and the processing difficulty are reduced.
Example 1
(1) Molybdenum powder and sodium molybdate powder are uniformly mixed according to the proportion, and the mass fraction of sodium element is 0.5%. The mixing mode adopts mechanical mixing in a powder mixer, and inert gas is filled into the powder mixer for protection.
(2) And (3) loading the uniformly mixed molybdenum powder and sodium molybdate powder into a cold isostatic pressing die, and carrying out cold isostatic pressing to obtain a tubular target blank, wherein the pressure of cold isostatic pressing is 100MPa, and the pressure maintaining time is 1 h.
(3) And (3) loading the tubular target blank obtained by cold isostatic pressing into a sheath, vacuumizing the sheath, and carrying out hot isostatic pressing, wherein the sheath is made of stainless steel, the hot isostatic pressing is carried out at the pressure of 240MPa and the temperature of 1000 ℃ for 2 h.
(4) And removing the sheath of the target blank subjected to hot isostatic pressing forming by adopting a mechanical processing mode to obtain the molybdenum-sodium alloy target material.
The mass content of sodium in the obtained molybdenum-sodium alloy target material is 0.4%, and the relative density of the target material is 93%.
Example 2
(1) Molybdenum powder and sodium molybdate are uniformly mixed according to the proportion, and the mass fraction of sodium element is 5.0%. The mixing mode adopts mechanical mixing in a powder mixer, and inert gas is filled into the powder mixer for protection.
(2) And (3) loading the uniformly mixed molybdenum powder and sodium molybdate powder into a cold isostatic pressing die, and carrying out cold isostatic pressing to obtain a tubular target blank, wherein the pressure of cold isostatic pressing is 240MPa, and the pressure maintaining time is 0.5 h.
(3) And (2) loading the tubular target blank obtained by cold isostatic pressing into a sheath, vacuumizing the sheath, and carrying out hot isostatic pressing molding, wherein the sheath is made of stainless steel, meanwhile, a support piece is inserted into the sheath, the support piece is made of graphite, the support piece is a cylinder with the length being greater than that of the sheath in the longitudinal direction, and the cross section of the support piece is circular with burrs on the periphery. The pressure of hot isostatic pressing treatment is 100MPa, the temperature is 1100 ℃, and the heat preservation time is 5 h.
(4) And removing the support from the target blank subjected to hot isostatic pressing forming, and then removing the sheath by adopting a chemical corrosion mode to obtain the molybdenum-sodium alloy target.
The mass content of sodium in the obtained molybdenum-sodium alloy target material is 4.5%, and the relative density of the target material is 85%.
Example 3
(1) Molybdenum powder and sodium fluoride are uniformly mixed according to the proportion, and the mass fraction of sodium element is 1.0%. The mixing mode adopts slurry mixing, the liquid medium selects deionized water, the binder selects polyethylene glycol, and finally spherical particles with the granularity of about 100 mu m and uniformly mixed molybdenum powder and sodium molybdate powder are prepared.
(2) And (3) loading the uniformly mixed molybdenum powder and sodium fluoride powder into a cold isostatic pressing die, and carrying out cold isostatic pressing to obtain a tubular target blank, wherein the pressure of the cold isostatic pressing treatment is 150MPa, and the pressure maintaining time is 0.6 h.
(3) Because the slurry mixing method adds the dispersing agent and the binding agent in the slurry preparation process, the dispersing agent and the binding agent need to be removed from the tubular target blank obtained by cold isostatic pressing before heat treatment and the like. Specifically, the mixture may be slowly heated to 500 ℃ for 24 hours to remove the dispersant and binder.
(4) And (2) loading the tubular target blank subjected to cold isostatic pressing and binder and dispersant removal into a sheath, vacuumizing the sheath, and performing hot isostatic pressing molding, wherein the sheath is made of stainless steel, meanwhile, a support piece is inserted into the sheath, the support piece is made of tungsten, the support piece is a cylinder with the length being equal to the length of the sheath in the longitudinal direction, and the cross section of the support piece is in a ring shape with burrs on the outer periphery, namely the support piece is in a tubular hollow structure. The hot isostatic pressing treatment pressure is 150MPa, the temperature is 1200 ℃, and the heat preservation time is 7 h.
(5) And removing the support from the target blank subjected to hot isostatic pressing forming, and then removing the sheath by adopting a machining mode to obtain the molybdenum-sodium alloy target.
The mass content of sodium in the obtained molybdenum-sodium alloy target material is 0.8%, and the relative density of the target material is 90%.
Example 4
(1) Molybdenum powder and sodium molybdate are uniformly mixed according to the proportion, and the mass fraction of sodium element is 2.0%. The mixing mode adopts mechanical mixing in a powder mixer, and inert gas is filled into the powder mixer for protection.
(2) And (3) loading the uniformly mixed molybdenum powder and sodium molybdate powder into a cold isostatic pressing die, and carrying out cold isostatic pressing to obtain a tubular target blank, wherein the pressure of the cold isostatic pressing is 200MPa, and the pressure maintaining time is 0.7 h.
(3) And (2) loading the tubular target blank obtained by cold isostatic pressing into a sheath, vacuumizing the sheath, and carrying out hot isostatic pressing molding, wherein the sheath is made of stainless steel, meanwhile, a support piece is inserted into the sheath, the support piece is made of graphite, the support piece is a column with the length being greater than that of the sheath in the longitudinal direction, and the cross section of the support piece is a hexagon with central symmetry. The pressure of hot isostatic pressing treatment is 180MPa, the temperature is 1300 ℃, and the heat preservation time is 8 h.
(4) And removing the support from the target blank subjected to hot isostatic pressing forming, and then removing the sheath by adopting a chemical corrosion mode to obtain the molybdenum-sodium alloy target.
The mass content of sodium in the obtained molybdenum-sodium alloy target material is 1.8%, and the relative density of the target material is 95%.
Example 5
(1) Molybdenum powder and sodium fluoride are uniformly mixed according to the proportion, and the mass fraction of sodium element is 3.0%. The mixing mode adopts mechanical mixing in a powder mixer, and inert gas is filled into the powder mixer for protection.
(2) And (3) loading the uniformly mixed molybdenum powder and sodium fluoride powder into a cold isostatic pressing die, and carrying out cold isostatic pressing to obtain a tubular target blank, wherein the pressure of the cold isostatic pressing treatment is 180MPa, and the pressure maintaining time is 0.8 h.
(3) And (2) loading the tubular target blank obtained by cold isostatic pressing into a sheath, vacuumizing the sheath, and carrying out hot isostatic pressing treatment, wherein the sheath is made of stainless steel, meanwhile, a support piece is inserted into the sheath, the support piece is made of graphite and is a cylinder with the length being greater than that of the sheath in the longitudinal direction, and the cross section of the support piece is circular with burrs on the periphery. The pressure of hot isostatic pressing molding is 200MPa, the temperature is 1550 ℃, and the heat preservation time is 10 h.
(4) And removing the support from the target blank subjected to hot isostatic pressing forming, and then removing the sheath by adopting a chemical corrosion mode to obtain the molybdenum-sodium alloy target.
The mass content of sodium in the obtained molybdenum-sodium alloy target material is 2.7%, and the relative density of the target material is 92%.
Example 6
(1) Molybdenum powder and potassium molybdate are uniformly mixed according to the proportion, and the mass fraction of potassium element is 3.0%. The mixing mode adopts mechanical mixing in a powder mixer, and inert gas is filled into the powder mixer for protection.
(2) And (3) loading the uniformly mixed molybdenum powder and potassium molybdate powder into a cold isostatic pressing die, and carrying out cold isostatic pressing to obtain a tubular target blank, wherein the pressure of cold isostatic pressing is 240MPa, and the pressure maintaining time is 0.5 h.
(3) And (2) loading the tubular target blank obtained by cold isostatic pressing into a sheath, vacuumizing the sheath, and carrying out hot isostatic pressing molding, wherein the sheath is made of stainless steel, meanwhile, a support piece is inserted into the sheath, the support piece is made of graphite, the support piece is a cylinder with the length being greater than that of the sheath in the longitudinal direction, and the cross section of the support piece is circular with burrs on the periphery. The pressure of hot isostatic pressing molding is 100MPa, the temperature is 1100 ℃, and the heat preservation time is 5 h.
(4) And removing the support from the target blank subjected to hot isostatic pressing forming, and then removing the sheath by adopting a chemical corrosion mode to obtain the molybdenum-potassium alloy target.
The mass content of potassium in the obtained molybdenum-potassium alloy target is 2.7%, and the relative density of the target is 93%.
Example 7
(1) Molybdenum powder and lithium fluoride are uniformly mixed according to the proportion, and the mass fraction of lithium element is 2.0%. The mixing mode adopts mechanical mixing in a powder mixer, and inert gas is filled into the powder mixer for protection.
(2) And (3) loading the uniformly mixed molybdenum powder and lithium fluoride powder into a cold isostatic pressing die, and carrying out cold isostatic pressing to obtain a tubular target blank, wherein the pressure of the cold isostatic pressing treatment is 150MPa, and the pressure maintaining time is 0.5 h.
(3) And (2) loading the tubular target blank obtained by cold isostatic pressing into a sheath, vacuumizing the sheath, and carrying out hot isostatic pressing molding, wherein the sheath is made of stainless steel, meanwhile, a support piece is inserted into the sheath, the support piece is made of graphite, the support piece is a cylinder with the length being greater than that of the sheath in the longitudinal direction, and the cross section of the support piece is circular with burrs on the periphery. The pressure of hot isostatic pressing molding is 120MPa, the temperature is 1200 ℃, and the heat preservation time is 8 h.
(4) And removing the support from the target blank subjected to hot isostatic pressing forming, and then removing the sheath by adopting a machining mode to obtain the molybdenum-lithium alloy target material.
The mass content of lithium in the obtained molybdenum-lithium alloy target material is 1.7%, and the relative density of the target material is 94%.
Example 8
(1) Molybdenum powder and sodium molybdate powder are uniformly mixed according to the proportion, and the mass fraction of sodium element is 0.5%. The mixing mode adopts mechanical mixing in a powder mixer, and inert gas is filled into the powder mixer for protection.
(2) And (3) loading the uniformly mixed molybdenum powder and sodium molybdate powder into a cold isostatic pressing die, and carrying out cold isostatic pressing to obtain a planar target blank, wherein the pressure of the cold isostatic pressing treatment is 100MPa, and the pressure maintaining time is 1 h.
(3) And (3) loading the planar target blank obtained by cold isostatic pressing into a sheath, vacuumizing the sheath, and carrying out hot isostatic pressing, wherein the sheath is made of stainless steel, the hot isostatic pressing is carried out at the pressure of 240MPa and the temperature of 1000 ℃ for 2 h.
(4) And removing the sheath of the target blank subjected to hot isostatic pressing forming by adopting a mechanical processing mode to obtain the molybdenum-sodium alloy target material.
The mass content of sodium in the obtained molybdenum-sodium alloy target material is 0.4%, and the relative density of the target material is 96%.
It is to be understood that the terms "cross-section," "transverse," "longitudinal," and the like are used herein for convenience in describing the invention and to simplify the description, and are not intended to indicate or imply that the referenced device or element must have a particular orientation, be constructed and operated in a particular orientation, and are not to be construed as limiting the invention.
Although the embodiments of the present invention have been described above, the above description is only for the convenience of understanding the present invention, and is not intended to limit the present invention. It will be understood by those skilled in the art that various changes in form and details may be made therein without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (10)
1. A preparation method of a molybdenum alloy target is characterized by comprising the following steps:
mixing molybdenum powder and alkali metal compound powder in proportion;
loading the uniformly mixed molybdenum powder and alkali metal compound powder into a cold isostatic pressing die, and carrying out cold isostatic pressing to obtain a target blank;
putting the target blank into a sheath, vacuumizing the sheath, and performing hot isostatic pressing;
removing the sheath to obtain the molybdenum alloy target material.
2. The method for preparing the molybdenum alloy target according to claim 1, wherein the alkali metal compound is a sodium compound, and the mass of the sodium element accounts for 0.5-5.0% of the total mass of the molybdenum powder and the sodium compound powder.
3. The method for preparing a molybdenum alloy target according to claim 2, wherein the sodium compound is sodium fluoride or sodium molybdate.
4. The method for preparing a molybdenum alloy target according to claim 1, wherein the melting point of the alkali metal compound is greater than 600 ℃.
5. The method for preparing the molybdenum alloy target according to claim 1, wherein the step of uniformly mixing the molybdenum powder and the alkali metal compound powder in proportion comprises:
and mechanically mixing the molybdenum powder and the alkali metal compound powder in a powder mixer, wherein the powder mixer is filled with inert gas.
6. The method for preparing the molybdenum alloy target according to claim 1, wherein the pressure of the cold isostatic pressing is 100MPa-240MPa, and the dwell time is 0.5h-1 h.
7. The method for preparing a molybdenum alloy target according to claim 1, wherein the target blank is a tubular target blank, a support is arranged inside the sheath, and the support is a cylinder with a length greater than or equal to the length of the sheath.
8. The method for preparing a molybdenum alloy target according to claim 7, wherein the cross section of the support is a regular polygon or a circle with protrusions.
9. The method for preparing a molybdenum alloy target according to claim 7, wherein the material of the support is one of graphite, molybdenum and tungsten.
10. The method for preparing a molybdenum alloy target according to any one of claims 1 to 9, wherein the hot isostatic pressing is performed at a pressure of 100MPa to 240MPa, a temperature of 1000 ℃ to 1550 ℃ and a holding time of 2h to 10 h.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910360325.3A CN111850485A (en) | 2019-04-29 | 2019-04-29 | Preparation method of molybdenum alloy target |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910360325.3A CN111850485A (en) | 2019-04-29 | 2019-04-29 | Preparation method of molybdenum alloy target |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN111850485A true CN111850485A (en) | 2020-10-30 |
Family
ID=72966477
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201910360325.3A Pending CN111850485A (en) | 2019-04-29 | 2019-04-29 | Preparation method of molybdenum alloy target |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN111850485A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114632933A (en) * | 2022-03-14 | 2022-06-17 | 郑州大学 | Porous molybdenum and method for preparing molybdenum-sodium alloy by using same |
| CN115383105A (en) * | 2022-08-10 | 2022-11-25 | 洛阳爱科麦钨钼科技股份有限公司 | High-density molybdenum-copper alloy material and preparation method thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104087903A (en) * | 2014-07-25 | 2014-10-08 | 安泰科技股份有限公司 | Molybdenum-sodium tube-type target material, manufacturing method of molybdenum-sodium tube-type target material and molybdenum-sodium target material |
-
2019
- 2019-04-29 CN CN201910360325.3A patent/CN111850485A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104087903A (en) * | 2014-07-25 | 2014-10-08 | 安泰科技股份有限公司 | Molybdenum-sodium tube-type target material, manufacturing method of molybdenum-sodium tube-type target material and molybdenum-sodium target material |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114632933A (en) * | 2022-03-14 | 2022-06-17 | 郑州大学 | Porous molybdenum and method for preparing molybdenum-sodium alloy by using same |
| CN115383105A (en) * | 2022-08-10 | 2022-11-25 | 洛阳爱科麦钨钼科技股份有限公司 | High-density molybdenum-copper alloy material and preparation method thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN110216277B (en) | Preparation method of refractory metal composite pipe | |
| JP2011225985A (en) | METHOD FOR MANUFACTURING CYLINDRICAL Mo ALLOY TARGET | |
| CN110379525B (en) | Rod-shaped nuclear fuel element resistant to accidents and preparation method thereof | |
| CN111850485A (en) | Preparation method of molybdenum alloy target | |
| CN110158042A (en) | A kind of molybdenum niobium alloy rotary target material and preparation method thereof | |
| CN108213440A (en) | A kind of preparation method of Mo Re alloys tubing | |
| CN110193601B (en) | Preparation method of double-layer or multi-layer refractory metal composite pipe | |
| CN115502403A (en) | Preparation method of large-size and high-density molybdenum target | |
| CN114990499B (en) | Preparation method of molybdenum alloy target | |
| LU502735B1 (en) | Preparation process of multi-component spherical alloy powder | |
| CN116571748A (en) | Powder hot isostatic pressing near-net forming method of titanium alloy workpiece | |
| CN210420134U (en) | Support for hot isostatic pressing preparation of tubular target | |
| CN105803406A (en) | Preparation method of rare earth transition alloy rotary target for film coating of magneto-optical recording medium and prepared target of rare earth transition alloy rotary target | |
| EP4169639A1 (en) | Electric current sintering method and electric current sintering device | |
| CN106222475B (en) | A kind of preparation method of Large scale alloy | |
| CN115722667A (en) | Horizontal continuous material-increasing spiral extrusion equipment for section bar and preparation method | |
| CN115896495A (en) | Method for rapidly sintering high-uranium-density high-thermal-conductivity composite core block | |
| US11919072B2 (en) | Preparation process of multi-component spherical alloy powder | |
| CN112427644A (en) | Preparation method of authigenic ceramic particle reinforced copper-based gradient spot welding electrode cap | |
| RU2818277C1 (en) | Tungsten electrode for electrolysis of salt melt for production of rare-earth metals and method of its production | |
| CN112996208B (en) | Plasma torch cathode and preparation method thereof | |
| RU2497211C1 (en) | Method to manufacture fuel rods with zirconium shell | |
| US20240309533A1 (en) | Tungsten Electrode for Molten Salt Electrolysis for Rare Earth Metals Preparation, and Preparation Method Thereof | |
| CN115894033B (en) | Preparation method of large-size magnesium fluoride moderated body | |
| CN114131026B (en) | Process for producing molybdenum tube blank by mould pressing method |
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 | ||
| TA01 | Transfer of patent application right | ||
| TA01 | Transfer of patent application right |
Effective date of registration: 20221117 Address after: 510670 room 229, annex building, No. 111, Kexue Avenue, Huangpu District, Guangzhou City, Guangdong Province (office only) Applicant after: Hanwa Technology Co.,Ltd. Address before: 101407 Yanqi Industrial Development Zone, Huairou District, Beijing Applicant before: HANERGY NEW MATERIAL TECHNOLOGY Co.,Ltd. |
|
| TA01 | Transfer of patent application right | ||
| TA01 | Transfer of patent application right |
Effective date of registration: 20221216 Address after: 510670 room 229, annex building, No. 111, Kexue Avenue, Huangpu District, Guangzhou City, Guangdong Province (office only) Applicant after: Hanwa Technology Co.,Ltd. Address before: 101407 Yanqi Industrial Development Zone, Huairou District, Beijing Applicant before: HANERGY NEW MATERIAL TECHNOLOGY Co.,Ltd. |
|
| WD01 | Invention patent application deemed withdrawn after publication | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20201030 |