CN106947879B - Silver-based alloy target blank for vacuum magnetron sputtering, preparation method and application thereof - Google Patents
Silver-based alloy target blank for vacuum magnetron sputtering, preparation method and application thereof Download PDFInfo
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- CN106947879B CN106947879B CN201710233551.6A CN201710233551A CN106947879B CN 106947879 B CN106947879 B CN 106947879B CN 201710233551 A CN201710233551 A CN 201710233551A CN 106947879 B CN106947879 B CN 106947879B
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- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 105
- 239000000956 alloy Substances 0.000 title claims abstract description 105
- 229910052709 silver Inorganic materials 0.000 title claims abstract description 29
- 239000004332 silver Substances 0.000 title claims abstract description 29
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 title description 26
- 238000001755 magnetron sputter deposition Methods 0.000 title description 2
- 238000004544 sputter deposition Methods 0.000 claims abstract description 17
- 239000010949 copper Substances 0.000 claims abstract description 16
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 15
- 229910052802 copper Inorganic materials 0.000 claims abstract description 14
- 239000011701 zinc Substances 0.000 claims abstract description 13
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 12
- 229910052779 Neodymium Inorganic materials 0.000 claims abstract description 12
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 12
- 229910052727 yttrium Inorganic materials 0.000 claims abstract description 12
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 claims abstract description 12
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 10
- 229910052749 magnesium Inorganic materials 0.000 claims abstract description 10
- 239000011777 magnesium Substances 0.000 claims abstract description 10
- 229910052725 zinc Inorganic materials 0.000 claims abstract description 10
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000004411 aluminium Substances 0.000 claims abstract description 8
- 238000000034 method Methods 0.000 claims abstract description 8
- 229910052684 Cerium Inorganic materials 0.000 claims abstract description 6
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims abstract description 6
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 6
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims abstract description 6
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 claims abstract description 6
- QEFYFXOXNSNQGX-UHFFFAOYSA-N neodymium atom Chemical compound [Nd] QEFYFXOXNSNQGX-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000010703 silicon Substances 0.000 claims abstract description 6
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 4
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 36
- 239000000654 additive Substances 0.000 claims description 26
- 230000000996 additive effect Effects 0.000 claims description 26
- 238000002844 melting Methods 0.000 claims description 26
- 230000008018 melting Effects 0.000 claims description 26
- 229910052786 argon Inorganic materials 0.000 claims description 18
- 239000007789 gas Substances 0.000 claims description 16
- 238000005266 casting Methods 0.000 claims description 15
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 12
- 229910002804 graphite Inorganic materials 0.000 claims description 12
- 239000010439 graphite Substances 0.000 claims description 12
- 238000001816 cooling Methods 0.000 claims description 11
- 238000005275 alloying Methods 0.000 claims description 9
- TVZPLCNGKSPOJA-UHFFFAOYSA-N copper zinc Chemical compound [Cu].[Zn] TVZPLCNGKSPOJA-UHFFFAOYSA-N 0.000 claims description 6
- 239000004615 ingredient Substances 0.000 claims description 6
- 238000003760 magnetic stirring Methods 0.000 claims description 6
- 230000002035 prolonged effect Effects 0.000 claims description 6
- 238000010792 warming Methods 0.000 claims description 6
- 229910052751 metal Inorganic materials 0.000 claims description 4
- 238000003723 Smelting Methods 0.000 claims description 3
- 230000006698 induction Effects 0.000 claims description 3
- 230000001681 protective effect Effects 0.000 claims description 3
- 238000007670 refining Methods 0.000 claims description 3
- 229910000906 Bronze Inorganic materials 0.000 claims description 2
- 239000010974 bronze Substances 0.000 claims description 2
- KUNSUQLRTQLHQQ-UHFFFAOYSA-N copper tin Chemical compound [Cu].[Sn] KUNSUQLRTQLHQQ-UHFFFAOYSA-N 0.000 claims description 2
- 239000000843 powder Substances 0.000 claims description 2
- 238000007710 freezing Methods 0.000 claims 1
- 230000008014 freezing Effects 0.000 claims 1
- 238000005303 weighing Methods 0.000 claims 1
- 238000004073 vulcanization Methods 0.000 abstract description 6
- 239000007769 metal material Substances 0.000 abstract description 2
- 238000002310 reflectometry Methods 0.000 description 11
- 239000013078 crystal Substances 0.000 description 7
- 239000000126 substance Substances 0.000 description 7
- 238000005498 polishing Methods 0.000 description 6
- 238000005987 sulfurization reaction Methods 0.000 description 6
- 239000000203 mixture Substances 0.000 description 4
- 239000011248 coating agent Substances 0.000 description 3
- 238000000576 coating method Methods 0.000 description 3
- 238000005260 corrosion Methods 0.000 description 3
- 230000007797 corrosion Effects 0.000 description 3
- 230000007423 decrease Effects 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000013077 target material Substances 0.000 description 3
- 229910001316 Ag alloy Inorganic materials 0.000 description 2
- 229910000838 Al alloy Inorganic materials 0.000 description 2
- 230000008033 biological extinction Effects 0.000 description 2
- 230000002708 enhancing effect Effects 0.000 description 2
- 238000003754 machining Methods 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 238000005477 sputtering target Methods 0.000 description 2
- 238000002834 transmittance Methods 0.000 description 2
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- 235000000177 Indigofera tinctoria Nutrition 0.000 description 1
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 1
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 1
- 229910052946 acanthite Inorganic materials 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 239000011651 chromium Substances 0.000 description 1
- 210000001787 dendrite Anatomy 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 229940097275 indigo Drugs 0.000 description 1
- COHYTHOBJLSHDF-UHFFFAOYSA-N indigo powder Natural products N1C2=CC=CC=C2C(=O)C1=C1C(=O)C2=CC=CC=C2N1 COHYTHOBJLSHDF-UHFFFAOYSA-N 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 239000011733 molybdenum Substances 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 229940056910 silver sulfide Drugs 0.000 description 1
- XUARKZBEFFVFRG-UHFFFAOYSA-N silver sulfide Chemical compound [S-2].[Ag+].[Ag+] XUARKZBEFFVFRG-UHFFFAOYSA-N 0.000 description 1
- 238000005494 tarnishing Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C5/00—Alloys based on noble metals
- C22C5/06—Alloys based on silver
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/02—Making non-ferrous alloys by melting
- C22C1/03—Making non-ferrous alloys by melting using master alloys
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C5/00—Alloys based on noble metals
- C22C5/06—Alloys based on silver
- C22C5/08—Alloys based on silver with copper as the next major constituent
-
- 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
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Physical Vapour Deposition (AREA)
Abstract
The invention belongs to metal material processing technical fields, and in particular to one kind is for vacuum magnetic-control sputtering silver-base alloy target blank and its preparation method and application.By weight percentage, other alloy elements of metallic silver and 0.535wt%~1.74wt% in the alloy comprising 98.26wt%~99.465wt%, other alloy elements at least one element selected from the following: copper, yttrium, nickel, cerium, zinc, aluminium, magnesium, neodymium, silicon etc..The present invention is made the silver-base alloy target produced have the excellent performances such as good resistance to vulcanization and lower resistivity, is applied in vacuum magnetic-control sputtering after working process by different alloy proportion and preparation method.
Description
Technical field
The invention belongs to metal material processing technical fields, and in particular to one kind is used for vacuum magnetic-control sputtering silver-base alloy target
Material blank and its preparation method and application.
Background technique
Silver-based film made of silver or silver-base alloy has some excellent performances, such as: reflectivity is high, transmittance is high,
Extinction coefficient is low, heating conduction is high, resistivity is low, also has excellent smooth surface effect etc..Therefore, silver-base alloy is extensive
It is thin applied to the reflectance coating of optical record medium, Transflective film, thermal diffusion film, the reflecting electrode of flat-panel monitor
Film, preparation of electromagnetic shielded film etc..If organic electroluminescent (organic EL) display is a kind of emissive type FPD
Device, thus it need the reflection-types metal film such as silver, aluminium, chromium, molybdenum composition reflection anode film reach the light of organic EL radiation into
The purpose of row reflection.Common silver, silver-base alloy, aluminum or aluminum alloy film as reflection anode film, using their high reflectances with
The characteristics of low-resistivity, to reach the requirement of reflection anode mould.Wherein, though the cost of aluminium and aluminium alloy is lower, they can only
There is 80% or more reflectivity in specific visible wavelength region, but silver and its alloy can be visible in 400nm~800nm
Reach 80% or more high reflectance in optical wavelength section.Thus, often select the reflection anode of silver or its alloy as display
Film.
Silver-based film is chronically exposed in air or when under hot and humid environment, and film surface is oxidized easily, and holds
Easily with the H in air2S gas reacts, and generates the silver sulfide of dark and gloomy color.The sulfide or oxide of generation can absorb indigo plant
Light declines the blue wave band reflectivity in reflecting layer, and then declines the reflectivity of film, is additionally easy to produce silver-colored crystal grain
Phenomena such as growth or silver atoms agglomerate.Thus silver-based film will appear electric conductivity and reflectivity decline, bad with the adaptation of bottom plate
The problems such as change.Therefore, while can maintain silver-colored high reflectance itself, low-resistivity, pass through addition alloying elements enhancing
The sulfidation-resistance energy and machining property of silver, to develop a kind of new silver-base alloy.
Summary of the invention
For some shortcomings existing for silver-base alloy target, the purpose of the present invention is to provide one kind to be used for Vacuum Magnetic
Control sputtering silver-base alloy target blank and its preparation method and application, the means of alloying are carried out by addition alloying elements
Carry out sulfidation-resistance energy, the machining property etc. of enhancing silver-base alloy sputtering target material.
The technical scheme is that
One kind being used for vacuum magnetic-control sputtering silver-base alloy target blank, by weight percentage, the silver-base alloy target base
Other alloy elements of metallic silver and 0.535wt%~1.74wt% in material comprising 98.26wt%~99.465wt%, institute
Other alloy elements stated include the combination of following one or more kinds of elements: Cu, Y, Ni, Ce, Zn, Al, Mg, Nd, Si.
Described is used for vacuum magnetic-control sputtering silver-base alloy target blank, by weight percentage, copper content 0.5wt%
~1.5wt%, yttrium content is 0wt%~1.0wt%, and contains one or more of following additional alloy element:
Ni, Ce, Zn, Al, Mg, Nd, Si, additional alloy element additive amount add up to 0.035wt%~0.14wt%, and surplus is silver.
The preparation method for vacuum magnetic-control sputtering silver-base alloy target blank, comprises the following steps that:
(1) according to the ratio with 10-5Accurate balance accurately weighs the weight of the required metallic element of each alloy, is protected using band argon gas
The Efco-Northrup furnace of protection unit carries out alloy melting；It is warming up to fusing in graphite crucible firstly, metallic copper is put into, then exists
Zinc is added at 1120 DEG C ± 50 DEG C and carries out alloying smelting, drops to graphite crucible on cooling platform after melting, in Re Ding
Protection, permanent magnetic stirring and orientation force to carry out casting and forming under conditions of cooling, and the ormolu blank of acquisition is cooled to room temperature
It taking out afterwards and is rolled and sheared, obtained copper zinc binary intermediate alloy is spare, high-purity argon gas prolonged enough is passed through before melting,
Melting furnace air is drained, and keep logical high-purity argon gas to ingot casting to be cooled to room temperature to terminate；
(2) silver is put into graphite crucible, fusing is warming up to using the Efco-Northrup furnace with argon protective device, according to need
It is molten that yttrium, nickel, copper zinc intermediate alloy, cerium, aluminium, magnesium, neodymium, element silicon progress alloying are successively separately added at 1500 DEG C ± 50 DEG C
Refining carries out ingredient using spectrometer and quickly detects simultaneously adjusting component, is ready for casting and forming after ingredient is qualified；It is passed through before melting
High-purity argon gas prolonged enough, it is ensured that drain induction melting furnace air；
(3) graphite crucible is dropped on cooling platform after silver-base alloy melting, in the protection of heat top, permanent magnetic stirring and is determined
Casting and forming is carried out under conditions of to pressure cooling, silver-base alloy target blank is made, logical high-purity argon gas to ingot blank is cooled to room
Temperature；
(4) it is cooled to room temperature to ingot blank, takes out silver-base alloy target blank, riser position is cut off, cut as needed
Silver-base alloy target blank at certain size and shape is stand-by.
The preparation method for vacuum magnetic-control sputtering silver-base alloy target blank, metallic silver, copper used in this method,
Yttrium powder, bronze, zinc powder, aluminium powder, magnesium powder purity by weight >=99.99%, nickel powder, cerium used in this method, neodymium, silicon purity by weight
>=99.95%.
The application for vacuum magnetic-control sputtering silver-base alloy target blank, silver-base alloy target blank, by adding
It is applied in vacuum magnetic-control sputtering after work processing.
Design philosophy of the invention is:
In the present invention, it is excellent that silver has that reflectivity and transmittance are high, extinction coefficient is low, good heat conductivity, resistivity are low etc.
Performance, but Yin Yinnai vulcanization and discoloration-resisting it is poor, it is easy to change, cause the reflectivity of film to reduce.It therefore, need to be to the greatest extent
On the basis of amount keeps silver-colored excellent performance, by adding alloying elements, the sulfuration resistant and anti-tarnishing ability of silver are improved.Copper coin
Element is dissolved in silver, can prevent recrystallizing for crystal grain, and reflectivity is inhibited to reduce.Yttrium can improve silver sulfuration resistant and
Discoloration-resisting.
In the present invention, Cu is dissolved in Ag, is had the intensity for improving crystal grain, is prevented from recrystallizing, and reflectivity decline is inhibited
Effect.When the additive amount of Cu is more than 3wt%, the reflectivity of silver alloy be can decrease, and when being lower than 0.5wt%, cannot be prevented
Crystal grain recrystallizes, so cannot inhibit the reduction of reflectivity.In addition, Y can improve the sulfuration resistant and fastness of silver alloy
Ability.Therefore, the present invention selects Cu0.5wt%~1.5wt%, Y 0wt%~1.0wt%.
The invention has the advantages and beneficial effects that:
1, the present invention has the silver-base alloy target produced good by different alloy proportion and preparation method
The excellent performances such as resistance to vulcanization and lower resistivity.
2, silver-base alloy sputtering target material of the invention, is mainly used for the reflectance coating of electronic product display.Using the present invention
Silver-base alloy target can obtain that sulfidation-resistance is preferable, resistivity is low, adhesion using vacuum magnetron sputtering coating film technology
Good silver-base alloy film.The indices of silver-base alloy target of the present invention meet international standard, can apply in the market.
Detailed description of the invention
Fig. 1 is the Ag0.5Cu silver-base alloy target blank micro-organization chart of different Y additive amounts；Wherein, a:1#；B:2#；C:
3#；D:4#.
Fig. 2 is that color at any time is tested in the resistance to vulcanization of Ag0.5Cu silver-base alloy target blank surface ingot casting of different Y additive amounts
Variation.
Fig. 3 is the Ag1.0Cu silver-base alloy target blank micro-organization chart of different Y additive amounts；Wherein, a:5#；B:6#；C:
7#；D:8#.
Fig. 4 is that color at any time is tested in the resistance to vulcanization of Ag1.0Cu silver-base alloy target blank surface ingot casting of different Y additive amounts
Variation.
Fig. 5 is the Ag1.5Cu silver-base alloy target blank micro-organization chart of different Y additive amounts；Wherein, a:9#；B:10#；
C:11#；D:12#.
Fig. 6 is that color at any time is tested in the resistance to vulcanization of Ag1.5Cu silver-base alloy target blank surface ingot casting of different Y additive amounts
Variation.
Specific embodiment
In the specific implementation process, the present invention is used for the preparation method of vacuum magnetic-control sputtering silver-base alloy target blank, packet
Include following processing step:
(1) according to the ratio with 10-5Accurate balance accurately weighs the weight of the required metallic element of each alloy, is protected using band argon gas
The Efco-Northrup furnace of protection unit carries out alloy melting；It is warming up to fusing in graphite crucible firstly, metallic copper is put into, then exists
Zinc is added at 1120 DEG C ± 50 DEG C or so and carries out alloying smelting, drops to graphite crucible on cooling platform after melting,
Hot top protection, permanent magnetic stirring and orientation force to carry out casting and forming under conditions of cooling, and the ormolu blank of acquisition is cooled to
It is taken out after room temperature and is rolled and sheared, obtained copper zinc binary intermediate alloy is spare, is passed through before melting prolonged high-purity enough
Argon gas, draining melting furnace air and logical high-purity argon gas to ingot casting is kept to be cooled to room temperature terminates；
(2) silver is put into graphite crucible, fusing is warming up to using the Efco-Northrup furnace with argon protective device, according to need
It wants, the elements such as yttrium, nickel, copper zinc intermediate alloy, cerium, aluminium, magnesium, neodymium, silicon is successively separately added at 1500 DEG C ± 50 DEG C and carry out alloy
Change melting, melting carries out ingredient using spectrometer after a certain period of time and quickly detects simultaneously adjusting component, is ready for after ingredient is qualified
Casting and forming；High-purity argon gas prolonged enough is passed through before melting, it is ensured that drain induction melting furnace air；
(3) graphite crucible is dropped on cooling platform after silver-base alloy melting, in the protection of heat top, permanent magnetic stirring and is determined
Casting and forming is carried out under conditions of to pressure cooling, silver-base alloy target blank is made, logical high-purity argon gas to ingot blank is cooled to room
Temperature；
(4) it is cooled to room temperature to ingot blank, takes out silver-base alloy target blank, riser position is cut off, cut as needed
Silver-base alloy target blank at certain size and shape is stand-by.
In the following, being further elaborated on by embodiment and attached drawing to the present invention.
Embodiment 1
After melting, count by weight percentage, the specific chemical composition of the present embodiment silver-base alloy target blank is such as
Under: copper content 0.5wt%；Yttrium content is 0wt%~1.0wt%；Additional alloy element is selected from one of following element
Or two or more: Ni, Ce, Zn, Al, Mg, Nd, Si, additive amount add up to 0.035wt%~0.14wt%；Surplus is silver.
| Cu | Y | Ni | Ce | Zn | Al | Mg | Nd | Si | Ag | |
| 1# | 0.5 | 0 | 0.005~0.02 | 0.005~0.02 | 0.005~0.02 | 0.005~0.02 | 0.005~0.02 | 0.005~0.02 | 0.005~0.02 | Surplus |
| 2# | 0.5 | 0.1 | 0.005~0.02 | 0.005~0.02 | 0.005~0.02 | 0.005~0.02 | 0.005~0.02 | 0.005~0.02 | 0.005~0.02 | Surplus |
| 3# | 0.5 | 0.5 | 0.005~0.02 | 0.005~0.02 | 0.005~0.02 | 0.005~0.02 | 0.005~0.02 | 0.005~0.02 | 0.005~0.02 | Surplus |
| 4# | 0.5 | 1.0 | 0.005~0.02 | 0.005~0.02 | 0.005~0.02 | 0.005~0.02 | 0.005~0.02 | 0.005~0.02 | 0.005~0.02 | Surplus |
Note: alloy content is mass percent (wt%)
After polishing, polishing, corrosion, alloy blank performance is detected and tested, silver-base alloy in the embodiment
The microscopic structure of target blank is shown in attached drawing 1, and the sample crystallite dimension that increases with the additive amount of element Y becomes smaller；The addition of element Y
The crystal grain for measuring the 4# sample of 1.0wt% obviously refines, but has the precipitation of black granulated substance.Each silver-base alloy target blank surface face
Color, which changes over time, sees attached list 1 and attached drawing 2, and the silver-based that can find out that the additive amount of element Y is 0.1wt% in this embodiment closes
The sulfidation-resistance of golden target blank can be good compared with other samples.
In the present embodiment, the resistivity of silver-base alloy target blank respectively is 1.79 × 10-8Ω·m、1.97×10-8Ω·m、3.05×10-8Ω·m、2.42×10-8Ω m, alloy rigidity respectively be 43.23HV, 52.43HV,
64.36HV、58.27HV。
Embodiment 2
After melting, count by weight percentage, the specific chemical composition of the present embodiment silver-base alloy target blank is such as
Under: copper content 1.0wt%；Yttrium content is 0wt%~1.0wt%；Additional alloy element is selected from one of following element
Or two or more: Ni, Ce, Zn, Al, Mg, Nd, Si, additive amount add up to 0.035wt%~0.14wt%；Surplus is silver.
| Cu | Y | Ni | Ce | Zn | Al | Mg | Nd | Si | Ag | |
| 5# | 1.0 | 0 | 0.005~0.02 | 0.005~0.02 | 0.005~0.02 | 0.005~0.02 | 0.005~0.02 | 0.005~0.02 | 0.005~0.02 | Surplus |
| 6# | 1.0 | 0.1 | 0.005~0.02 | 0.005~0.02 | 0.005~0.02 | 0.005~0.02 | 0.005~0.02 | 0.005~0.02 | 0.005~0.02 | Surplus |
| 7# | 1.0 | 0.5 | 0.005~0.02 | 0.005~0.02 | 0.005~0.02 | 0.005~0.02 | 0.005~0.02 | 0.005~0.02 | 0.005~0.02 | Surplus |
| 8# | 1.0 | 1.0 | 0.005~0.02 | 0.005~0.02 | 0.005~0.02 | 0.005~0.02 | 0.005~0.02 | 0.005~0.02 | 0.005~0.02 | Surplus |
Note: alloy content is mass percent (wt%)
After polishing, polishing, corrosion, alloy blank performance is detected and tested, silver-base alloy in the embodiment
The microscopic structure of target blank is shown in attached drawing 3, as the additive amount of element Y increases the sample crystallite dimension that silver-based adds up to target blank
Become smaller；The 8# sample of the additive amount 1.0wt% of element Y have black granulated substance cast sturcture dendrite near border be precipitated and
It is distributed more uniform.Each silver-base alloy target blank surface color, which changes over time, sees attached list 2 and attached drawing 4, it can be seen that element Y
Additive amount be 0.1wt% the sulfidation-resistance of silver-base alloy target blank can be good compared with other samples.
In the present embodiment, the resistivity of silver-base alloy target blank respectively is 1.73 × 10-8Ω·m、2.53×10-8Ω·m、2.96×10-8Ω·m、2.32×10-8Ω m, alloy rigidity respectively be 48.16HV, 55.68HV,
70.16HV、69.76HV。
Embodiment 3
After melting, count by weight percentage, the specific chemical composition of the present embodiment silver-base alloy target blank is such as
Under: copper content 1.5wt%；Yttrium content is 0wt%~1.0wt%；Additional alloy element is selected from one of following element
Or two or more: Ni, Ce, Zn, Al, Mg, Nd, Si, additive amount add up to 0.035wt%~0.14wt%；Surplus is silver.
| Cu | Y | Ni | Ce | Zn | Al | Mg | Nd | Si | Ag | |
| 9# | 1.5 | 0 | 0.005~0.02 | 0.005~0.02 | 0.005~0.02 | 0.005~0.02 | 0.005~0.02 | 0.005~0.02 | 0.005~0.02 | Surplus |
| 10# | 1.5 | 0.1 | 0.005~0.02 | 0.005~0.02 | 0.005~0.02 | 0.005~0.02 | 0.005~0.02 | 0.005~0.02 | 0.005~0.02 | Surplus |
| 11# | 1.5 | 0.5 | 0.005~0.02 | 0.005~0.02 | 0.005~0.02 | 0.005~0.02 | 0.005~0.02 | 0.005~0.02 | 0.005~0.02 | Surplus |
| 12# | 1.5 | 1.0 | 0.005~0.02 | 0.005~0.02 | 0.005~0.02 | 0.005~0.02 | 0.005~0.02 | 0.005~0.02 | 0.005~0.02 | Surplus |
Note: alloy content is mass percent (wt%)
After polishing, polishing, corrosion, alloy blank performance is detected and tested, silver-base alloy in the embodiment
The microscopic structure of target blank is shown in attached drawing 5, and the 10# sample crystallite dimension of the additive amount 0.1wt% of element Y becomes smaller, no precipitated phase
Occur；The crystal grain of the 11# sample of the additive amount 0.1wt% of element Y obviously refines, and has black granulated substance in the branch of cast sturcture
Brilliant near border is precipitated and distribution is more uniform；The grain refining effect of the 12# sample of the additive amount 0.1wt% of element Y is very
Obviously, equally there is the precipitation of black granulated substance and quantity is increased.Each silver-base alloy target blank surface color becomes at any time
Change sees attached list 3 and attached drawing 6, it can be seen that the additive amount of element Y is that the sulfidation-resistance of 0.1wt% can be good compared with other samples.
In the present embodiment, the resistivity of silver-base alloy target blank respectively is 1.69 × 10-8Ω·m、2.01×10-8Ω·m、2.93×10-8Ω·m、2.01×10-8Ω m, alloy rigidity respectively be 48.16HV, 55.68HV,
70.16HV、69.76HV。
The Ag0.5Cu silver-base alloy surface sulfuration resistant of 1 difference Y additive amount of subordinate list tests color change result at any time
| Sample | 0h | 0.5h | 1h | 2h | 4h | 6h | 8h |
| 1# | It is non-discolouring | It is non-discolouring | It is non-discolouring | It is yellowish | Yellow | Brown | Dark brown |
| 2# | It is non-discolouring | It is non-discolouring | It is non-discolouring | It is non-discolouring | It is yellowish | It is yellowish | Yellow |
| 3# | It is non-discolouring | It is non-discolouring | It is yellowish | It is light yellow | Yellow | Puce | Puce |
| 4# | It is non-discolouring | It is non-discolouring | It is yellowish | Yellow | Brown | Puce | Dark brown |
The Ag1.0Cu silver-base alloy surface sulfuration resistant of 2 difference Y additive amount of subordinate list tests color change result at any time
| Sample | 0h | 0.5h | 1h | 2h | 4h | 6h | 8h |
| 5# | It is non-discolouring | It is non-discolouring | It is non-discolouring | It is non-discolouring | It is yellowish | Brown | Dark brown |
| 6# | It is non-discolouring | It is non-discolouring | It is non-discolouring | It is non-discolouring | It is non-discolouring | It is yellowish | It is yellowish |
| 7# | It is non-discolouring | It is non-discolouring | It is non-discolouring | It is non-discolouring | It is yellowish | Yellow | Puce |
| 8# | It is non-discolouring | It is non-discolouring | It is non-discolouring | It is yellowish | It is yellowish | Puce | Dark brown |
The Ag1.5Cu silver-base alloy surface sulfuration resistant of 3 difference Y additive amount of subordinate list tests color change result at any time
| Sample | 0h | 0.5h | 1h | 2h | 4h | 6h | 8h |
| 9# | It is non-discolouring | It is non-discolouring | It is non-discolouring | It is non-discolouring | It is yellowish | It is yellowish | Yellow |
| 10# | It is non-discolouring | It is non-discolouring | It is non-discolouring | It is non-discolouring | It is non-discolouring | It is non-discolouring | It is yellowish |
| 11# | It is non-discolouring | It is non-discolouring | It is non-discolouring | It is non-discolouring | It is yellowish | It is light yellow | It is light yellow |
| 12# | It is non-discolouring | It is non-discolouring | It is non-discolouring | It is non-discolouring | It is yellowish | Yellow | Puce |
Embodiment the result shows that, the present invention passes through every detection and test, it can be seen that the additive amount of Y is 0.1wt%, Cu
Additive amount be 1.5wt% when, the existing preferable sulfidation-resistance energy of the silver-base alloy target blank, but maintain silver low resistance
Rate, while crystal grain has been refined, it can satisfy the required performance requirement of silver-base alloy target, production can be promoted.
Claims (3)
1. a kind of preparation method for vacuum magnetic-control sputtering silver-base alloy target blank, it is characterised in that: by weight percentage
It counts, includes the metallic silver of the wt% of 98.26 wt% ~ 99.465 in the silver-base alloy target blank, copper content is 0.5 wt% ~ 1.5
One or more of wt%, yttrium content are the wt% of 0.1 wt% ~ 1.0, and contain following additional alloy element: Ni, Ce,
Zn, Al, Mg, Nd, Si, additional alloy element additive amount add up to the wt% of 0.035 wt% ~ 0.14；
The preparation method for vacuum magnetic-control sputtering silver-base alloy target blank, comprises the following steps that:
(1) weight for accurately weighing the required metallic element of each alloy with the accurate balance of 10-5 according to the ratio is protected using band argon gas
The Efco-Northrup furnace of device carries out alloy melting；Fusing is warming up in graphite crucible firstly, metallic copper is put into, then 1120
Zinc is added at DEG C ± 50 DEG C and carries out alloying smelting, drops to graphite crucible on cooling platform after melting, is protected on heat top
Shield, permanent magnetic stirring and orientation force to carry out casting and forming under conditions of cooling, after the ormolu blank of acquisition is cooled to room temperature
Taking-up is rolled and is sheared, and obtained copper zinc binary intermediate alloy is spare, and high-purity argon gas prolonged enough is passed through before melting, is arranged
Melting furnace air to the greatest extent, and logical high-purity argon gas to the ingot casting of holding is cooled to room temperature and terminates；
(2) silver is put into graphite crucible, is warming up to fusing using the Efco-Northrup furnace with argon protective device, exists as needed
1500 DEG C ± 50 DEG C are successively separately added into yttrium, nickel, copper zinc intermediate alloy, cerium, aluminium, magnesium, neodymium, element silicon progress alloying and melt
Refining carries out ingredient using spectrometer and quickly detects simultaneously adjusting component, is ready for casting and forming after ingredient is qualified；It is passed through before melting
High-purity argon gas prolonged enough, it is ensured that drain induction melting furnace air；
(3) graphite crucible is dropped on cooling platform after silver-base alloy melting, it is strong in the protection of heat top, permanent magnetic stirring and orientation
Casting and forming is carried out under conditions of freezing but, silver-base alloy target blank is made, logical high-purity argon gas to ingot blank is cooled to room temperature；
(4) it is cooled to room temperature to ingot blank, takes out silver-base alloy target blank, riser position is cut off, is cut into one as needed
The silver-base alloy target blank for determining size and shape is stand-by.
2. the preparation method described in accordance with the claim 1 for vacuum magnetic-control sputtering silver-base alloy target blank, feature exist
In: metallic silver, copper used in this method, yttrium powder, bronze, zinc powder, aluminium powder, magnesium powder purity by weight >=99.99%, used in this method
Nickel powder, cerium, neodymium, silicon purity by weight >=99.95%.
3. according to the application for being used for vacuum magnetic-control sputtering silver-base alloy target blank described in claim 1 ~ 2 any one,
It is characterized in that, silver-base alloy target blank, is applied in vacuum magnetic-control sputtering after working process.
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| CN113444914A (en) * | 2021-07-19 | 2021-09-28 | 福建阿石创新材料股份有限公司 | Silver-based alloy and preparation method thereof, silver alloy composite film and application thereof |
| CN113913761B (en) * | 2021-10-11 | 2022-08-12 | 芜湖映日科技股份有限公司 | Ag-based alloy target material and preparation method thereof |
| CN116334548A (en) * | 2022-12-28 | 2023-06-27 | 济源豫金靶材科技有限公司 | A kind of silver-copper-zinc alloy sputtering target material and preparation method thereof |
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| CN1361525A (en) * | 2000-12-26 | 2002-07-31 | 株式会社神户制钢所 | Reflective layer or semi-transparent reflective layer for optical informatino recording media, optical information recording media and sputtering target for optical information recording media |
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| JP3803864B2 (en) * | 2001-11-19 | 2006-08-02 | 三菱マテリアル株式会社 | Silver alloy sputtering target for reflection layer formation of optical recording media |
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| CN1361525A (en) * | 2000-12-26 | 2002-07-31 | 株式会社神户制钢所 | Reflective layer or semi-transparent reflective layer for optical informatino recording media, optical information recording media and sputtering target for optical information recording media |
| CN1458986A (en) * | 2001-03-16 | 2003-11-26 | 石福金属兴业株式会社 | Sputtering target material |
| CN1751345A (en) * | 2003-03-13 | 2006-03-22 | 三菱麻铁里亚尔株式会社 | Silver alloy sputterig target for forming reflective layer of optical recording medium |
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