CN112779508A - Preparation method of high-purity vanadium target blank and high-purity vanadium target prepared by using same - Google Patents
Preparation method of high-purity vanadium target blank and high-purity vanadium target prepared by using same Download PDFInfo
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- CN112779508A CN112779508A CN202011580420.3A CN202011580420A CN112779508A CN 112779508 A CN112779508 A CN 112779508A CN 202011580420 A CN202011580420 A CN 202011580420A CN 112779508 A CN112779508 A CN 112779508A
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- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 title claims abstract description 111
- 229910052720 vanadium Inorganic materials 0.000 title claims abstract description 110
- 238000002360 preparation method Methods 0.000 title claims abstract description 25
- 238000000137 annealing Methods 0.000 claims abstract description 72
- 238000005242 forging Methods 0.000 claims abstract description 32
- 238000005096 rolling process Methods 0.000 claims abstract description 30
- 238000000034 method Methods 0.000 claims description 24
- 238000001816 cooling Methods 0.000 claims description 22
- 238000004321 preservation Methods 0.000 claims description 11
- 239000013077 target material Substances 0.000 claims description 9
- 238000005520 cutting process Methods 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 238000010894 electron beam technology Methods 0.000 claims description 6
- 238000004519 manufacturing process Methods 0.000 claims description 6
- 238000003723 Smelting Methods 0.000 claims description 5
- 238000003825 pressing Methods 0.000 claims description 5
- 238000003466 welding Methods 0.000 claims description 5
- 229910000838 Al alloy Inorganic materials 0.000 claims description 4
- 230000009467 reduction Effects 0.000 claims description 4
- 229910000881 Cu alloy Inorganic materials 0.000 claims description 3
- 239000012535 impurity Substances 0.000 claims description 2
- 230000006698 induction Effects 0.000 claims description 2
- 238000010313 vacuum arc remelting Methods 0.000 claims description 2
- 230000001808 coupling effect Effects 0.000 abstract description 5
- 230000002195 synergetic effect Effects 0.000 abstract description 5
- 230000000052 comparative effect Effects 0.000 description 12
- 230000008569 process Effects 0.000 description 12
- 238000001514 detection method Methods 0.000 description 9
- 229910052751 metal Inorganic materials 0.000 description 7
- 239000002184 metal Substances 0.000 description 7
- 230000037303 wrinkles Effects 0.000 description 7
- 239000013078 crystal Substances 0.000 description 6
- 238000002844 melting Methods 0.000 description 5
- 230000008018 melting Effects 0.000 description 5
- 239000007787 solid Substances 0.000 description 5
- 239000000155 melt Substances 0.000 description 4
- 238000005477 sputtering target Methods 0.000 description 4
- 230000009286 beneficial effect Effects 0.000 description 3
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 3
- 239000010931 gold Substances 0.000 description 3
- 229910052737 gold Inorganic materials 0.000 description 3
- 150000002500 ions Chemical class 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- 238000005266 casting Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000001125 extrusion Methods 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 238000010884 ion-beam technique Methods 0.000 description 2
- 238000001755 magnetron sputter deposition Methods 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 239000010409 thin film Substances 0.000 description 2
- 230000000007 visual effect Effects 0.000 description 2
- 229910000756 V alloy Inorganic materials 0.000 description 1
- PTXMVOUNAHFTFC-UHFFFAOYSA-N alumane;vanadium Chemical compound [AlH3].[V] PTXMVOUNAHFTFC-UHFFFAOYSA-N 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 238000005219 brazing Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000010892 electric spark Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 239000010408 film Substances 0.000 description 1
- 239000011888 foil Substances 0.000 description 1
- 238000007733 ion plating Methods 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 239000002932 luster Substances 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 238000001465 metallisation Methods 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 238000004080 punching Methods 0.000 description 1
- 238000001953 recrystallisation Methods 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 238000005204 segregation Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 229920001169 thermoplastic Polymers 0.000 description 1
- 239000004416 thermosoftening plastic Substances 0.000 description 1
- 235000012431 wafers Nutrition 0.000 description 1
- 239000002699 waste material Substances 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
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23P—METAL-WORKING NOT OTHERWISE PROVIDED FOR; COMBINED OPERATIONS; UNIVERSAL MACHINE TOOLS
- B23P15/00—Making specific metal objects by operations not covered by a single other subclass or a group in this subclass
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/16—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of other metals or alloys based thereon
- C22F1/18—High-melting or refractory metals or alloys based thereon
-
- 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
-
- 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
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Crystallography & Structural Chemistry (AREA)
- Physical Vapour Deposition (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
The invention relates to a preparation method of a high-purity vanadium target blank and a high-purity vanadium target prepared by using the same, wherein the preparation method comprises the following steps: sequentially forging, annealing, rolling and re-annealing the vanadium ingot to obtain a high-purity vanadium target blank; wherein the temperature of the secondary annealing is 450-550 ℃. The preparation method utilizes the synergistic coupling effect of forging, annealing, rolling and secondary annealing, and strictly limits the temperature of the secondary annealing to be 450-550 ℃, the prepared vanadium target blank has the advantages of uniform internal structure and fine grains, the grain size is less than or equal to 50 mu m and can be basically controlled within the range of 20-40 mu m, and the yield is up to more than 90%.
Description
Technical Field
The invention relates to the technical field of sputtering target materials, in particular to a preparation method of a high-purity vanadium target blank and a high-purity vanadium target material prepared by using the same.
Background
Magnetron sputtering is one of the main techniques for preparing thin film materials, ions generated by an ion source are accelerated and gathered in vacuum to form ion beam flow with high speed energy, the ion beam flow bombards the surface of a solid, kinetic energy exchange is carried out between the ions and atoms on the surface of the solid, the atoms on the surface of the solid leave the solid and are deposited on the surface of a substrate, and a thin film with the thickness of nanometer or micrometer level is formed. The bombarded solid is a raw material for preparing a magnetron sputtering deposition film, is generally called a sputtering target material, and is intensively applied to industries such as information storage, integrated circuits, displays, automobile rearview mirrors and the like.
The sputtering target material can be obtained by thermoplastic deformation Processing (TMP), and the process improves the structure and the performance of a metal material and obtains the required shape and size by the processes of forging, rolling, heat treatment annealing and the like of an ingot obtained by smelting and casting, and is a core key technology for manufacturing the sputtering target material.
In the fabrication of integrated circuits, pure gold is generally used as the surface conductive layer, but gold and silicon wafers tend to generate AuSi low-melting-point compounds, which results in weak bonding between gold and silicon interfaces. The barrier layer needs to be made of metal with high melting point and also needs to bear larger current density, and high-purity metal vanadium can meet the requirement. Vanadium is a silver-grey metal with a density of 6.11g/cm3The melting point is 1919 + -2 ℃, which belongs to the high melting point rare metals. Pure vanadium has good plasticity, and can be rolled into sheets, foils and drawn into wires at normal temperature. Although vanadium alloy targets have been used in the fields of solar energy, flat panel displays, electronics, semiconductors, and the like, such as integrated circuits, back plate metallization, photoelectrons, and the like, few reports have been made on methods for preparing high-purity vanadium targets.
For example, CN104894388A discloses a method for preparing a vanadium target by electron beam melting, which uses argon arc welding to connect irregular metal vanadium leftover materials, or uses a vanadium-aluminum alloy containing 90% of vanadium to be placed in a bin of an electromagnetic focusing electron beam melting furnace as a melt electrode, bombards, melts and melts the melt electrode by a high-energy electron beam, and obtains a high-purity vanadium target by evaporation under the condition of continuous vacuum pumping. Although the preparation method can prepare the vanadium target with the purity of more than 99.95 percent and the density of 6.11g/cm, meets the requirements of ion plating on the target, and can also recycle and re-melt the waste vanadium target, the preparation method has higher requirements on equipment and is not suitable for large-scale popularization and application.
CN107385399A discloses an extrusion method of a vanadium tube target, which comprises the steps of smelting a metal vanadium block by a vacuum electron beam to obtain a high-purity vanadium ingot with the diameter of phi 150-phi 215mm, and polishing the outer surface of the vanadium ingot; then, digging out a vanadium rod with the diameter of phi 50-phi 125mm by means of electric spark punching and linear cutting; coating the inner wall, the outer wall and the end faces of the vanadium tube blank by using a sheath material, and welding and sealing; heating to 750-1000 ℃, preserving heat for 1-2 hrs, extruding the vanadium tube blank with the sheath to obtain a vanadium tube with an intermediate size, and finally performing straightening treatment and machining to obtain the required finished vanadium tube target. The density of the finished vanadium tube target is lower, and the extrusion method of the vanadium tube target is greatly different from the preparation method of the planar target.
In summary, there is a need to develop an effective method for preparing a high-purity vanadium target blank, so as to prepare a vanadium target material with a uniform internal structure and fine crystal grains, which meets the quality requirements of the industries such as semiconductors and sensors.
Disclosure of Invention
In order to solve the technical problems, the invention provides a preparation method of a high-purity vanadium target blank and a high-purity vanadium target prepared by using the same, wherein the preparation method utilizes the synergistic coupling effect of forging, annealing, rolling and re-annealing, the temperature of the re-annealing is strictly limited to 450-550 ℃, the prepared vanadium target blank has the advantages of uniform internal structure and fine grains, the grain size is less than or equal to 50 mu m and can be basically controlled within the range of 20-40 mu m, and the yield is up to more than 90%.
In order to achieve the purpose, the invention adopts the following technical scheme:
one of the purposes of the invention is to provide a preparation method of a high-purity vanadium target blank, which comprises the following steps: sequentially forging, annealing, rolling and re-annealing the vanadium ingot to obtain a high-purity vanadium target blank; wherein the temperature of the secondary annealing is 450-550 ℃.
The preparation method utilizes the synergistic coupling effect of forging, annealing, rolling and secondary annealing, strictly limits the temperature of the secondary annealing to be 450-.
The re-annealing temperature in the present invention is 450-550 ℃, such as 450 ℃, 460 ℃, 480 ℃, 500 ℃, 520 ℃, 530 ℃, 540 ℃ or 550 ℃, but not limited to the recited values, and other values not recited in the range of the values are also applicable.
In a preferred embodiment of the present invention, the vanadium content of the vanadium ingot is 99 to 99.99% by mass, and the balance is unavoidable impurities, for example, 99%, 99.1%, 99.2%, 99.3%, 99.4%, 99.5%, 99.6%, 99.8%, or 99.99%, but the present invention is not limited to the above-mentioned values, and other values not listed in the above-mentioned range are also applicable.
As the preferable technical scheme of the invention, the vanadium ingot is smelted by adopting any one of electron beam, vacuum arc remelting or vacuum induction smelting, and then is poured to obtain the vanadium ingot.
Preferably, the vanadium ingot is cut according to a target size, and then forged.
Preferably, the cutting is performed using a horizontal sawing machine.
In a preferred embodiment of the present invention, the forging process further comprises a preheating process, wherein the temperature of the preheating process is 450 ℃ or 500 ℃, for example, 450 ℃, 460 ℃, 470 ℃, 480 ℃, 490 ℃ or 500 ℃, but not limited to the recited values, and other values not recited in the range of the recited values are also applicable.
In a preferred embodiment of the present invention, the total deformation rate of the forging is 70 to 80%, for example, 70%, 72%, 74%, 75%, 78%, or 80%, but the total deformation rate is not limited to the above-mentioned values, and other values not shown in the above-mentioned value range are also applicable.
The forging treatment of the invention can further eliminate casting defects such as loose structure and the like in the cast ingot, optimize the microstructure in the cast ingot and crush the columnar crystal of the cast ingot into fine crystal grains, thereby playing a role in grain refinement.
The preheating treatment before forging can effectively prevent the cracking problem of the cast ingot in the forging process and is more beneficial to the subsequent forging.
In a preferred embodiment of the present invention, the annealing temperature is 400-500 ℃, for example, 400 ℃, 420 ℃, 440 ℃, 450 ℃, 470 ℃, 490 ℃ or 500 ℃, but the annealing temperature is not limited to the values listed, and other values not listed in the numerical range are also applicable.
Preferably, the annealing is carried out for a holding time of 60-120min, such as 60min, 70min, 80min, 90min, 100min, 110min or 120min, but not limited to the recited values, and other values not recited in the range of values are also applicable.
The annealing treatment of the invention can eliminate residual stress and internal structure defects in the forged vanadium ingot and is beneficial to smooth subsequent rolling.
Preferably, after the annealing, cooling is performed by air cooling, and then the rolling is performed.
In a preferred embodiment of the present invention, the rolling is controlled to a rolling reduction of 0.5 to 1mm per pass, for example, 0.5mm, 0.6mm, 0.7mm, 0.8mm, 0.9mm or 1mm, but the rolling is not limited to the above-mentioned values, and other values not listed in the above-mentioned numerical range are also applicable.
Preferably, the rolling has a total deformation of 70-80%, such as 70%, 72%, 74%, 75%, 78%, or 80%, but not limited to the recited values, and other values not recited within this range are equally applicable.
The rolling of the invention not only can further refine grains and homogenize the structure, but also can mold the vanadium target blank to obtain the target blank with target diameter and target thickness; the rolling reduction amount of each pass is further controlled to ensure that the vanadium target blank does not crack, when the reduction amount is too large, the vanadium target blank cracks, the total number of rolling passes is reduced, the number of times of grain refining is reduced, and the final structure size is not uniform.
In a preferred embodiment of the present invention, the holding time for the re-annealing is 90 to 150min, for example, 90min, 100min, 110min, 120min, 130min, 140min, or 150min, but is not limited to the above-mentioned values, and other values not shown in the above-mentioned range are also applicable.
Preferably, water cooling is carried out after the secondary annealing, so as to obtain the high-purity vanadium target blank.
The water cooling of the invention can stop the growth of crystal grains in the vanadium target blank and ensure that the crystal grains are fine.
As a preferred technical scheme of the invention, the preparation method comprises the following steps:
(1) cutting a vanadium ingot with 99-99.99% of vanadium by mass by using a horizontal sawing machine according to a target size, preheating at the temperature of 450-500 ℃, then forging, and controlling the total deformation rate of the forging to be 70-80%;
(2) annealing the vanadium ingot obtained by forging in the step (1), wherein the annealing temperature is 400-500 ℃, the heat preservation time is 60-120min, and then cooling by air cooling;
(3) rolling the vanadium cast ingot obtained by annealing in the step (2), controlling the pressing amount of each pass to be 0.5-1mm, and controlling the total deformation amount to be 70-80% until a vanadium target blank with a target diameter and a target thickness is obtained;
(4) and (4) carrying out secondary annealing treatment on the vanadium target blank obtained by rolling in the step (3), wherein the temperature of the secondary annealing is 450-550 ℃, the heat preservation time is 90-150min, and carrying out water cooling after the secondary annealing to obtain the high-purity vanadium target blank.
The second purpose of the invention is to provide a high-purity vanadium target material, which is obtained by welding a high-purity vanadium target blank prepared by the preparation method of the first purpose and a back plate.
Preferably, the backing sheet comprises an aluminum alloy backing sheet and/or a copper alloy backing sheet.
The high-purity vanadium target blank prepared by the method is subjected to size detection and performance detection, the qualified vanadium target blank is combined with an aluminum alloy back plate or a copper alloy back plate through brazing or diffusion welding, and then the high-purity vanadium target blank is precisely processed according to a drawing to obtain a final finished product vanadium target; the size detection comprises diameter detection and thickness detection, and the performance detection comprises surface state detection and grain size detection.
The surface state detection is used for judging whether the surface of the prepared high-purity vanadium target blank has wrinkles and cracks.
Compared with the prior art, the invention has at least the following beneficial effects:
the preparation method utilizes the synergistic coupling effect of forging, annealing, rolling and secondary annealing, strictly limits the temperature of the secondary annealing to be 450-.
Detailed Description
For the purpose of facilitating an understanding of the present invention, the present invention will now be described by way of examples. It should be understood by those skilled in the art that the examples are only for the understanding of the present invention and should not be construed as the specific limitations of the present invention.
Example 1
The embodiment provides a preparation method of a high-purity vanadium target blank, which comprises the following steps:
(1) cutting a vanadium ingot with 99.5 percent of vanadium by mass according to a target size by using a horizontal sawing machine, preheating at 480 ℃, then forging, and controlling the total deformation rate of the forging to be 75 percent;
(2) annealing the vanadium ingot obtained by forging in the step (1), wherein the annealing temperature is 450 ℃, the heat preservation time is 100min, and then cooling by air cooling;
(3) rolling the vanadium cast ingot obtained by annealing in the step (2), controlling the pressing amount of each pass to be 0.7mm, and controlling the total deformation amount to be 75% until a vanadium target blank with the target diameter and the target thickness is obtained;
(4) and (4) carrying out secondary annealing treatment on the vanadium target blank obtained by rolling in the step (3), wherein the temperature of the secondary annealing is 500 ℃, the heat preservation time is 120min, and carrying out water cooling after the secondary annealing to obtain the high-purity vanadium target blank.
Example 2
The embodiment provides a preparation method of a high-purity vanadium target blank, which comprises the following steps:
(1) cutting a vanadium ingot with 99.99% of vanadium by mass by using a horizontal sawing machine according to a target size, preheating at 500 ℃, forging, and controlling the total deformation rate of the forging to be 80%;
(2) annealing the vanadium ingot obtained by forging in the step (1), wherein the annealing temperature is 500 ℃, the heat preservation time is 120min, and then cooling by air cooling;
(3) rolling the vanadium cast ingot obtained by annealing in the step (2), controlling the pressing amount of each pass to be 1mm, and controlling the total deformation amount to be 80% until a vanadium target blank with the target diameter and the target thickness is obtained;
(4) and (4) carrying out secondary annealing treatment on the vanadium target blank rolled in the step (3), wherein the temperature of the secondary annealing is 550 ℃, the heat preservation time is 150min, and carrying out water cooling after the secondary annealing to obtain the high-purity vanadium target blank.
Example 3
The embodiment provides a preparation method of a high-purity vanadium target blank, which comprises the following steps:
(1) cutting a vanadium ingot with 99.99% of vanadium by mass by using a horizontal sawing machine according to a target size, preheating at 450 ℃, forging, and controlling the total deformation rate of the forging to be 70%;
(2) annealing the vanadium ingot obtained by forging in the step (1), wherein the annealing temperature is 400 ℃, the heat preservation time is 60min, and then cooling by air cooling;
(3) rolling the vanadium cast ingot obtained by annealing in the step (2), controlling the pressing amount of each pass to be 0.5mm, and controlling the total deformation amount to be 70% until a vanadium target blank with a target diameter and a target thickness is obtained;
(4) and (4) carrying out secondary annealing treatment on the vanadium target blank obtained by rolling in the step (3), wherein the temperature of the secondary annealing is 450 ℃, the heat preservation time is 90min, and carrying out water cooling after the secondary annealing to obtain the high-purity vanadium target blank.
Comparative example 1
This comparative example provides a method for preparing a high purity vanadium target blank, except that the re-annealing temperature in step (4) was changed from "500 ℃ to" 400 ℃, and the other conditions were exactly the same as in example 1.
Comparative example 2
This comparative example provides a method for preparing a high purity vanadium target blank, except that the re-annealing temperature in step (4) was changed from "500 ℃ to" 600 ℃, and the other conditions were exactly the same as in example 1.
The high-purity vanadium target blanks obtained in the above examples and comparative examples were subjected to the following performance tests:
(1) surface state: judging whether wrinkles and cracks exist or not by a visual method;
(2) grain size: measuring according to a cross-section method disclosed in the national standard GB/T6394-2017 method for measuring average grain size of metal;
(3) the internal structure uniformity of the target material is as follows: firstly, a visual standard sample is taken as a standard, and then the surface is clean and uniform in color and luster after precision processing, and no bunch-shaped or dot-shaped specks appear, so that the segregation phenomenon does not appear when the internal structure is uniform;
(4) yield: and calculating the yield of the preparation method according to the ratio of the number of finished products with qualified quality of the high-purity vanadium target blank to the total number of the prepared finished products.
The results of the tests relating to the high purity vanadium target blanks obtained in the above examples and comparative examples are shown in table 1.
TABLE 1
| Group of | Surface state | Grain size | Uniformity of internal structure of target | Yield of finished products |
| Example 1 | Without wrinkles and cracks | 31.8μm | Clean surface and uniform color | 96.8％ |
| Example 2 | Without wrinkles and cracks | 35.7μm | Clean surface and uniform color | 96.6％ |
| Example 3 | Without wrinkles and cracks | 25.5μm | Clean surface and uniform color | 97.7％ |
| Comparative example 1 | Without wrinkles and cracks | Not completely recrystallized | Clean surface and uniform color | 5.1％ |
| Comparative example 2 | Without wrinkles and cracks | 67.9μm | Clean surface and uniform color | 67.8％ |
From table 1, the following points can be seen:
(1) the preparation method utilizes the synergistic coupling effect of forging, annealing, rolling and secondary annealing, and strictly limits the temperature of the secondary annealing to be 450-;
(2) comparing the example 1 with the comparative example 1, the re-annealing temperature of the comparative example 1 is only 400 ℃ which is lower than the range of 550 ℃ of 450 ℃ in the invention, so that the temperature can not reach the recrystallization temperature, no crystal grains are generated, and the yield is only 5.1%;
(3) comparing the example 1 with the comparative example 2, the re-annealing temperature of the comparative example 1 is as high as 600 ℃ and higher than the range of 550 ℃ of 450-.
The applicant states that the present invention is illustrated by the above examples to show the detailed process equipment and process flow of the present invention, but the present invention is not limited to the above detailed process equipment and process flow, i.e. it does not mean that the present invention must rely on the above detailed process equipment and process flow to be implemented. It should be understood by those skilled in the art that any modification of the present invention, equivalent substitutions of the raw materials of the product of the present invention, addition of auxiliary components, selection of specific modes, etc., are within the scope and disclosure of the present invention.
Claims (10)
1. The preparation method of the high-purity vanadium target blank is characterized by comprising the following steps of: sequentially forging, annealing, rolling and re-annealing the vanadium ingot to obtain a high-purity vanadium target blank; wherein the temperature of the secondary annealing is 450-550 ℃.
2. The preparation method of claim 1, wherein the mass percent of vanadium in the vanadium ingot is 99-99.99%, and the balance is inevitable impurities.
3. The preparation method according to claim 1 or 2, characterized in that the vanadium ingot is obtained by smelting in any one of electron beam, vacuum arc remelting or vacuum induction smelting and then pouring;
preferably, the vanadium ingot is cut according to a target size, and then forged;
preferably, the cutting is performed using a horizontal sawing machine.
4. The method as claimed in any one of claims 1 to 3, further comprising a preheating treatment before the forging, wherein the temperature of the preheating treatment is 450-500 ℃.
5. The production method according to any one of claims 1 to 4, wherein the total deformation ratio of the forging is 70 to 80%.
6. The method according to any one of claims 1 to 5, wherein the annealing temperature is 400-500 ℃;
preferably, the heat preservation time of the annealing is 60-120 min;
preferably, after the annealing, cooling is performed by air cooling, and then the rolling is performed.
7. The production method according to any one of claims 1 to 6, wherein the rolling controls the amount of reduction per pass to be 0.5 to 1 mm;
preferably, the total deformation of the rolling is 70-80%.
8. The production method according to any one of claims 1 to 7, wherein the holding time for the re-annealing is 90 to 150 min;
preferably, water cooling is carried out after the secondary annealing, so as to obtain the high-purity vanadium target blank.
9. The production method according to any one of claims 1 to 8, characterized by comprising the steps of:
(1) cutting a vanadium ingot with 99-99.99% of vanadium by mass by using a horizontal sawing machine according to a target size, preheating at the temperature of 450-500 ℃, then forging, and controlling the total deformation rate of the forging to be 70-80%;
(2) annealing the vanadium ingot obtained by forging in the step (1), wherein the annealing temperature is 400-500 ℃, the heat preservation time is 60-120min, and then cooling by air cooling;
(3) rolling the vanadium cast ingot obtained by annealing in the step (2), controlling the pressing amount of each pass to be 0.5-1mm, and controlling the total deformation amount to be 70-80% until a vanadium target blank with a target diameter and a target thickness is obtained;
(4) and (4) carrying out secondary annealing treatment on the vanadium target blank obtained by rolling in the step (3), wherein the temperature of the secondary annealing is 450-550 ℃, the heat preservation time is 90-150min, and carrying out water cooling after the secondary annealing to obtain the high-purity vanadium target blank.
10. A high-purity vanadium target material, which is obtained by welding a high-purity vanadium target blank prepared by the preparation method of any one of claims 1 to 9 with a back plate;
preferably, the backing sheet comprises an aluminum alloy backing sheet and/or a copper alloy backing sheet.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113649771A (en) * | 2021-08-16 | 2021-11-16 | 宁波江丰电子材料股份有限公司 | Preparation method of copper evaporation material |
| CN113649773A (en) * | 2021-08-25 | 2021-11-16 | 宁波江丰电子材料股份有限公司 | Preparation method of large-size panel aluminum target |
| CN117026176A (en) * | 2023-08-14 | 2023-11-10 | 中色（宁夏）东方集团有限公司 | Preparation method of high-purity metal vanadium tube target material |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103898459A (en) * | 2014-04-16 | 2014-07-02 | 昆山海普电子材料有限公司 | Preparation method of high-purity cobalt target |
| CN111004985A (en) * | 2019-11-25 | 2020-04-14 | 有研亿金新材料有限公司 | Preparation method of nickel-vanadium sputtering target material |
| CN111088481A (en) * | 2018-10-23 | 2020-05-01 | 宁波江丰电子材料股份有限公司 | Nickel target blank and method for manufacturing target material |
| CN111304606A (en) * | 2020-03-30 | 2020-06-19 | 宁波江丰电子材料股份有限公司 | Preparation method of defect-free high-purity nickel-vanadium target blank and target prepared by using defect-free high-purity nickel-vanadium target blank |
-
2020
- 2020-12-28 CN CN202011580420.3A patent/CN112779508A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103898459A (en) * | 2014-04-16 | 2014-07-02 | 昆山海普电子材料有限公司 | Preparation method of high-purity cobalt target |
| CN111088481A (en) * | 2018-10-23 | 2020-05-01 | 宁波江丰电子材料股份有限公司 | Nickel target blank and method for manufacturing target material |
| CN111004985A (en) * | 2019-11-25 | 2020-04-14 | 有研亿金新材料有限公司 | Preparation method of nickel-vanadium sputtering target material |
| CN111304606A (en) * | 2020-03-30 | 2020-06-19 | 宁波江丰电子材料股份有限公司 | Preparation method of defect-free high-purity nickel-vanadium target blank and target prepared by using defect-free high-purity nickel-vanadium target blank |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113649771A (en) * | 2021-08-16 | 2021-11-16 | 宁波江丰电子材料股份有限公司 | Preparation method of copper evaporation material |
| CN113649773A (en) * | 2021-08-25 | 2021-11-16 | 宁波江丰电子材料股份有限公司 | Preparation method of large-size panel aluminum target |
| CN117026176A (en) * | 2023-08-14 | 2023-11-10 | 中色（宁夏）东方集团有限公司 | Preparation method of high-purity metal vanadium tube target material |
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