CN115976478B - Silver sulfide resistant alloy target and preparation method thereof - Google Patents
Silver sulfide resistant alloy target and preparation method thereof Download PDFInfo
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- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 32
- 239000000956 alloy Substances 0.000 title claims abstract description 32
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 229910052946 acanthite Inorganic materials 0.000 title claims abstract description 17
- 229940056910 silver sulfide Drugs 0.000 title claims abstract description 17
- XUARKZBEFFVFRG-UHFFFAOYSA-N silver sulfide Chemical compound [S-2].[Ag+].[Ag+] XUARKZBEFFVFRG-UHFFFAOYSA-N 0.000 title claims description 14
- 229910052709 silver Inorganic materials 0.000 claims abstract description 32
- 239000004332 silver Substances 0.000 claims abstract description 31
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 claims abstract description 30
- NPXOKRUENSOPAO-UHFFFAOYSA-N Raney nickel Chemical class [Al].[Ni] NPXOKRUENSOPAO-UHFFFAOYSA-N 0.000 claims abstract description 25
- 229910052763 palladium Inorganic materials 0.000 claims abstract description 15
- 229910052738 indium Inorganic materials 0.000 claims abstract description 14
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000011777 magnesium Substances 0.000 claims abstract description 12
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims abstract description 11
- 229910052749 magnesium Inorganic materials 0.000 claims abstract description 11
- 229910052706 scandium Inorganic materials 0.000 claims abstract description 10
- SIXSYDAISGFNSX-UHFFFAOYSA-N scandium atom Chemical compound [Sc] SIXSYDAISGFNSX-UHFFFAOYSA-N 0.000 claims abstract 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 18
- 239000013077 target material Substances 0.000 claims description 17
- 239000002202 Polyethylene glycol Substances 0.000 claims description 16
- 229920001223 polyethylene glycol Polymers 0.000 claims description 16
- 238000000034 method Methods 0.000 claims description 12
- 239000011230 binding agent Substances 0.000 claims description 11
- 238000003723 Smelting Methods 0.000 claims description 10
- 229910052759 nickel Inorganic materials 0.000 claims description 9
- 229910052782 aluminium Inorganic materials 0.000 claims description 8
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 8
- 238000005242 forging Methods 0.000 claims description 8
- 238000005098 hot rolling Methods 0.000 claims description 8
- 238000002156 mixing Methods 0.000 claims description 8
- 239000002994 raw material Substances 0.000 claims description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 7
- 239000000463 material Substances 0.000 claims description 7
- 238000000137 annealing Methods 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 6
- 230000008569 process Effects 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 4
- 239000011812 mixed powder Substances 0.000 claims description 4
- 239000004973 liquid crystal related substance Substances 0.000 claims description 3
- 238000002310 reflectometry Methods 0.000 abstract description 12
- 230000000694 effects Effects 0.000 abstract description 7
- 238000005987 sulfurization reaction Methods 0.000 abstract description 4
- 239000007769 metal material Substances 0.000 abstract description 2
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 29
- 229910001316 Ag alloy Inorganic materials 0.000 description 26
- 239000010408 film Substances 0.000 description 25
- 230000000052 comparative effect Effects 0.000 description 21
- 229910052751 metal Inorganic materials 0.000 description 11
- 239000002184 metal Substances 0.000 description 9
- ZCNBOEGXFWYXEO-UHFFFAOYSA-N scandium Chemical compound [Sc].[Sc] ZCNBOEGXFWYXEO-UHFFFAOYSA-N 0.000 description 9
- 238000004073 vulcanization Methods 0.000 description 8
- 239000000654 additive Substances 0.000 description 6
- 230000000996 additive effect Effects 0.000 description 6
- 238000005486 sulfidation Methods 0.000 description 6
- 229910000828 alnico Inorganic materials 0.000 description 5
- 238000004321 preservation Methods 0.000 description 5
- 239000000853 adhesive Substances 0.000 description 4
- 230000001070 adhesive effect Effects 0.000 description 4
- 229910052761 rare earth metal Inorganic materials 0.000 description 4
- 239000000758 substrate Substances 0.000 description 4
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 3
- 239000002390 adhesive tape Substances 0.000 description 3
- 229910052802 copper Inorganic materials 0.000 description 3
- 239000010949 copper Substances 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 230000009467 reduction Effects 0.000 description 3
- 238000004544 sputter deposition Methods 0.000 description 3
- 239000010409 thin film Substances 0.000 description 3
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 238000007747 plating Methods 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 238000005096 rolling process Methods 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 238000006467 substitution reaction Methods 0.000 description 2
- 230000002195 synergetic effect Effects 0.000 description 2
- 229910000990 Ni alloy Inorganic materials 0.000 description 1
- KJTLSVCANCCWHF-UHFFFAOYSA-N Ruthenium Chemical compound [Ru] KJTLSVCANCCWHF-UHFFFAOYSA-N 0.000 description 1
- 241001062472 Stokellia anisodon Species 0.000 description 1
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- 229910000756 V alloy Inorganic materials 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 230000001627 detrimental effect Effects 0.000 description 1
- QYHNIMDZIYANJH-UHFFFAOYSA-N diindium Chemical compound [In]#[In] QYHNIMDZIYANJH-UHFFFAOYSA-N 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000005566 electron beam evaporation Methods 0.000 description 1
- 235000019441 ethanol Nutrition 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000001755 magnetron sputter deposition Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- HBVFXTAPOLSOPB-UHFFFAOYSA-N nickel vanadium Chemical compound [V].[Ni] HBVFXTAPOLSOPB-UHFFFAOYSA-N 0.000 description 1
- 229910052758 niobium Inorganic materials 0.000 description 1
- 239000010955 niobium Substances 0.000 description 1
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 239000010970 precious metal Substances 0.000 description 1
- 229910052703 rhodium Inorganic materials 0.000 description 1
- 239000010948 rhodium Substances 0.000 description 1
- MHOVAHRLVXNVSD-UHFFFAOYSA-N rhodium atom Chemical compound [Rh] MHOVAHRLVXNVSD-UHFFFAOYSA-N 0.000 description 1
- 229910052707 ruthenium Inorganic materials 0.000 description 1
- 150000003378 silver Chemical group 0.000 description 1
- 229910052718 tin Inorganic materials 0.000 description 1
- 239000011135 tin Substances 0.000 description 1
- 238000007738 vacuum evaporation Methods 0.000 description 1
- 229910052720 vanadium Inorganic materials 0.000 description 1
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 description 1
Abstract
The application relates to the technical field of metal material processing, in particular to an anti-silver sulfide alloy target and a preparation method thereof, wherein the anti-silver sulfide alloy target comprises the following components in parts by weight: 90-99 parts of silver, 1-3 parts of indium, 1-3 parts of aluminum-nickel alloy, 0.01-0.15 part of scandium, 0.01-0.1 part of magnesium and 0.01-0.08 part of palladium, and has excellent effect on the aspects of sulfuration resistance and reflectivity.
Description
Technical Field
The application relates to the technical field of metal material processing, in particular to an anti-silver sulfide alloy target and a preparation method thereof.
Background
Targets are also known as "sputter targets" and are named for the target material that is bombarded by a high-velocity metal plasma stream during sputtering. The target material is a core raw material for preparing functional films in the fields of semiconductors, display panels, photovoltaics and the like, and has irreplaceability in process. Different film systems can be obtained by changing different targets, thereby realizing the functions of electric conduction or blocking and the like.
At present, most of display targets are metal targets, silver is the cheapest precious metal, has excellent characteristics of low resistance, high reflectivity and the like, and is widely applied to the fields of semiconductors, displays, electronic device reflection films, radiation-proof glass and the like. However, pure silver has the disadvantage that when the silver-based film is exposed to air or high temperature and high humidity environment for a long period of time, the surface of the film is easily oxidized and easily reacts with H in the air 2 S gas reacts to generate silver sulfide with a tarnish color. The sulfide or oxide produced absorbs blue light, and the reflectance of the reflective layer in the blue light band is reduced, and the reflectance of the thin film is reduced, and further, the phenomena such as silver crystal grain growth and silver atom aggregation are easily generated. Therefore, the silver-based film has problems such as a decrease in conductivity and reflectance, a deterioration in adhesion to the base plate, and the like, and the disadvantages of pure silver can be improved by doping other metal elements.
For example, chinese patent application CN112323030a discloses a silver alloy target and a preparation method thereof, the silver alloy target comprises metallic silver, a metallic element additive and a rare earth element additive, wherein the mass portions of the components are: 90-99 parts of metal silver, 1-3 parts of metal element additive and 0.001-0.1 part of rare earth element additive, wherein the purity of the metal silver is at least 99.99%, and the silver alloy target is obtained by smelting the metal silver, the metal element additive and the rare earth element additive according to a certain proportion, so that the prepared silver alloy target has more excellent performance compared with the traditional silver alloy target, the adhesion capability of the silver alloy target with a base material is greatly improved, and the silver alloy target is more reliable in use.
Chinese patent application CN109306414A discloses a silver alloy target material, a film and a preparation method thereof, wherein the silver alloy target material is formed by Ag x In y M z Q n Wherein the proportion of indium is more than or equal to 8% and less than or equal to 40% (atomic ratio), M is at least one element of tin, gold, platinum, palladium, niobium, rhodium and ruthenium, z is more than or equal to 0 and less than or equal to 8% (atomic ratio), Q is at least one element of rare earth elements, n is more than or equal to 0 and less than or equal to 3% (atomic ratio), and the content x of silver is more than or equal to 60% (atomic ratio). The silver alloy target material can be prepared into a silver alloy film with excellent heat resistance, adhesive force, conductivity, corrosion resistance and sulfuration resistance by magnetron sputtering plating, ion sputtering plating, vacuum evaporation or electron beam evaporation, and is suitable for the fields of reflective electrode films, liquid crystal displays, optical recording media, organic light emitting diodes, electrochromic and the like.
Chinese patent application CN105316630a discloses a silver alloy target, a method for manufacturing the same, and an organic light emitting diode using the target, wherein the silver alloy target is substantially composed of silver and indium or silver, indium, palladium and copper. The average grain size is between 33 μm and 126. Mu.m. Based on the total weight of the silver alloy target, the content of indium is more than or equal to 0.25wt% and less than or equal to 5wt%, the content of palladium is more than or equal to 0.25wt% and less than or equal to 3.5wt%, and the content of copper is more than or equal to 0.25wt% and less than or equal to 3wt%. By adding indium or indium, palladium and copper in a predetermined proportion and controlling the average grain size to be between 33 and 126 μm, the silver alloy target can be sputtered to obtain a silver alloy film with good heat resistance, sulfidation resistance, adhesion, high reflectivity and high fineness, but the effects of the silver alloy target are to be further improved.
However, the thin film produced by the silver alloy target cannot simultaneously have excellent effects in various aspects such as adhesion to a substrate, sulfidation resistance, heat resistance, and reflectance.
Therefore, it is necessary to develop a silver alloy target material capable of solving the above technical problems and a method for preparing the same.
Disclosure of Invention
The application aims to overcome the defects of the prior art and provide a silver alloy target with excellent effects on sulfuration resistance and reflectivity and a preparation method thereof.
The application is realized by the following technical scheme:
the silver sulfide resistant alloy target comprises the following components in parts by weight: 90-99 parts of silver, 1-3 parts of indium, 1-3 parts of aluminum-nickel alloy, 0.01-0.15 part of scandium, 0.01-0.1 part of magnesium and 0.01-0.08 part of palladium.
Preferably, the mass ratio of aluminum to nickel in the aluminum-nickel alloy is 1:2-4.
The application also relates to a preparation method of the silver sulfide resistant alloy target, which comprises the following steps:
(1) Preparing materials according to a proportion, and mixing and smelting the raw materials to obtain an alloy cast ingot;
(2) Forging the alloy cast ingot obtained in the step (1) to obtain a blank;
(3) And (5) carrying out hot rolling and annealing treatment on the blank in sequence to obtain the finished product.
Preferably, the smelting temperature in step (1) is 1150-1350 ℃.
More preferably, step (1) is performed at 1X 10 -2 Up to 1X 10 -4 Heating to 1150-1350 ℃ under the vacuum degree of torr, and preserving the heat for 0.5-1 h for smelting.
Preferably, the smelting process in step (1) is performed under vacuum conditions or in an inert gas atmosphere.
Preferably, the forging ratio in step (2) is 2.5 to 3.
Preferably, the temperature of hot rolling in the step (3) is 550-700 ℃, the heat preservation is carried out for 1-3 hours, and the total deformation is 60-70%.
Preferably, the annealing temperature in the step (3) is 550-700 ℃, and the temperature is kept for 20-30min.
Preferably, pretreatment is carried out before smelting the raw materials in the step (1), and the specific pretreatment process is as follows: and dissolving the rest components except the aluminum-nickel alloy and the binder in absolute ethyl alcohol, drying to obtain mixed powder, and mixing with the aluminum-nickel alloy.
More preferably, the binder is a mixture of polyethylene glycol and polyethylene glycol, and the mass ratio of the polyethylene glycol to the polyethylene glycol is 3-5:1.
More preferably, the binder is added in an amount of 0.5 to 3% by mass of silver
More preferably, the preparation method comprises the steps of:
(1) Preparing materials according to a proportion, dissolving the rest components except the aluminum-nickel alloy and 0.5-3% of binder (the addition amount is calculated by the mass of silver) in absolute ethyl alcohol, wherein the binder is a mixture of polyethylene glycol and polyethylene glycol, the mass ratio of the polyethylene glycol to the polyethylene glycol is 3-5:1, uniformly mixing, drying to obtain mixed powder, mixing with the aluminum-nickel alloy, heating to 1150-1350 ℃ under vacuum condition, and preserving heat for 0.5-1 h for smelting to obtain alloy cast ingots;
(2) Forging the alloy ingot obtained in the step (1) at 550-700 ℃, preserving heat for 1-3h, and obtaining a blank, wherein the forging ratio is 2.5-3;
(3) And (3) sequentially carrying out hot rolling on the blank, wherein the hot rolling temperature is 550-700 ℃, the heat preservation is carried out for 1-3 hours, the total deformation is 60-70%, the reduction rate of each pass is controlled to be 10-12%, the annealing treatment is carried out at 550-700 ℃ every two passes in the rolling process, and the heat preservation is carried out for 20-30 minutes, so that the product is obtained.
The application also relates to application of the silver sulfide resistant alloy target material or the silver sulfide resistant alloy target material prepared by the preparation method in a liquid crystal display or an organic light-emitting diode.
The beneficial effects of the application are as follows:
according to the application, the aluminum-nickel alloy is added into the silver-based target, and compared with the single addition of aluminum and nickel or the addition of other alloys, the anti-vulcanization performance of the silver-based target can be remarkably improved.
Scandium, magnesium and palladium added into the silver-based target material have remarkable synergistic effect, and the anti-vulcanization performance and reflectivity of the target material are improved.
According to the application, a small amount of indium, aluminum-nickel alloy, scandium, magnesium and palladium are added into the silver-based target material, all the components act synergistically, and the thin film formed after sputtering has excellent effects on the aspects of sulfuration resistance, oxidation resistance and reflectivity, and meanwhile, the adhesion force with a base material is higher.
In addition, the adhesive is added in the process of preparing the silver-based target material, the composition of the adhesive is optimized, the uniformity of the silver-based target material is improved, the components can fully play the roles, and the silver-based target material has excellent comprehensive performance.
Detailed Description
The application will be further described with reference to specific embodiments, and advantages and features of the application will become apparent from the description. These examples are merely exemplary and do not limit the scope of the application in any way. It will be understood by those skilled in the art that various changes and substitutions of details and forms of the technical solution of the present application may be made without departing from the spirit and scope of the present application, but these changes and substitutions fall within the scope of the present application.
The purity of silver and indium adopted by the application is more than 99.99%, and the purity of other elements is more than 99.9%.
Example 1
The silver sulfide resistant alloy target comprises the following components in parts by weight: 90 parts of silver, 1 part of indium, 1 part of aluminum-nickel alloy, 0.01 part of scandium, 0.01 part of magnesium and 0.01 part of palladium; the mass ratio of aluminum to nickel in the aluminum-nickel alloy is 1:2.
The preparation process comprises the following steps:
(1) Preparing materials according to a proportion, dissolving the rest components except the aluminum-nickel alloy and 2% of binder (the addition amount is calculated by the mass of silver) in absolute ethyl alcohol, wherein the binder is a mixture of polyethylene glycol and polyethylene glycol, the mass ratio of the polyethylene glycol to the polyethylene glycol is 4:1, uniformly mixing, drying to obtain mixed powder, mixing with the aluminum-nickel alloy, heating to 1350 ℃ under vacuum condition, and preserving heat for 1h to smelt to obtain alloy cast ingots;
(2) Forging the alloy ingot obtained in the step (1) at 650 ℃, preserving heat for 2 hours, and obtaining a blank, wherein the forging ratio is 2.5;
(3) And (3) sequentially carrying out hot rolling on the blank, wherein the hot rolling temperature is 650 ℃, the heat preservation is carried out for 2 hours, the total deformation is 60%, the reduction rate of each pass is controlled to be 10%, the annealing treatment is carried out at the temperature of 650 ℃ every two passes in the rolling process, and the heat preservation is carried out for 30 minutes, so that the product is obtained.
The following examples and comparative examples were prepared in the same manner as in example 1.
Example 2
The silver sulfide resistant alloy target comprises the following components in parts by weight: 99 parts of silver, 3 parts of indium, 3 parts of aluminum-nickel alloy, 0.15 part of scandium, 0.1 part of magnesium and 0.08 part of palladium; the mass ratio of aluminum to nickel in the aluminum-nickel alloy is 1:4.
The preparation process is the same as in example 1.
Example 3
The silver sulfide resistant alloy target comprises the following components in parts by weight: 95 parts of silver, 2 parts of indium, 2 parts of aluminum-nickel alloy, 0.1 part of scandium, 0.05 part of magnesium and 0.05 part of palladium; the mass ratio of aluminum to nickel in the aluminum-nickel alloy is 1:3.
The preparation process is the same as in example 1.
Example 4
The difference from example 3 is only that in the preparation process, the raw materials in step (1) are directly mixed and smelted, no binder is added, and the raw materials are insoluble in ethanol, and the rest conditions are the same.
The formulations of comparative examples 1 to 3 are shown in Table 1, and the conditions were the same as in example 3 except that the amounts of the raw materials were different.
TABLE 1
| Comparative example 1/part | Comparative example 2/part | Comparative example 3/part | |
| Silver (Ag) | 95 | 95 | 95 |
| Indium (indium) | 2 | 2 | 2 |
| Aluminium nickel alloy | 2 | 2 | 2 |
| Scandium (scandium) | 0 | 0.133 | 0.133 |
| Magnesium (Mg) | 0.1 | 0.067 | 0 |
| Palladium | 0.1 | 0 | 0.067 |
Comparative example 4
The difference from example 3 is that no aluminum-nickel alloy was added, 0.5 part of aluminum and 1.5 parts of nickel were added alone, and the other conditions were the same as in example 3.
Comparative example 5
The difference from example 3 was that the amount of the aluminum-nickel alloy used was changed to 5 parts by 2 parts, and the other conditions were the same as those of example 3.
Comparative example 6
The difference from example 3 was that the amount of the aluminum-nickel alloy used was changed to 0.5 part by 2 parts, and the other conditions were the same as those in example 3.
Comparative example 7
The only difference from example 3 is that the alnico alloy is replaced by an equal mass of nickel-vanadium alloy (mass ratio of nickel to vanadium 3:1). Test example 1 adhesion test (film thickness 150 nm)
The silver alloy films were first placed in a high temperature and high humidity environment at 85% humidity and 85 ℃ for 96 hours, and then subjected to a peeling test using 3M Scotch 600 type transparent adhesive tape. And (3) adhering the adhesive tape to the surface of each silver alloy film, and tearing off the adhesive tape, wherein if the silver alloy films are not peeled off, the silver alloy films and the base material have good adhesive force. The specific results are shown in Table 2.
Test example 2 anti-vulcanization test (film thickness 150 nm)
Each silver alloy film was placed in a closed environment to which sulfur vapor was introduced, and the state of blackening by contact with sulfur vapor was observed, and the time required for blackening was recorded. The specific results are shown in Table 2, and the better the vulcanization resistance, the longer the time required for blackening the vulcanization treated surface.
Test example 3 reflectance (film thickness 90 nm)
And measuring the reflectivity of each silver alloy film by adopting an ultraviolet-visible light spectrometer, wherein the wavelength range is 430-470nm. The specific results are shown in Table 2.
TABLE 2
As can be seen from the data in table 2:
example 4 compared to example 3, the film had poor uniformity and affected the action of the components without the addition of the binder during the preparation process, so the adhesion between the film and the substrate was poor. And the difference between the anti-vulcanization performance and the reflectivity at different positions of the film is large, so the values in the range of table 2 are obtained.
Comparative examples 1 to 3 differ from example 3 only in that: comparative example 1 contains no scandium, comparative example 2 contains no palladium, comparative example 3 contains no magnesium, example 3 contains scandium, palladium and magnesium at the same time, and the amounts of the three elements added in comparative examples 1 to 3 and example 3 are the same. The results of comparative examples 1 to 3 are not as good in both the anti-vulcanization property and the reflectance as those of example 3, indicating that the synergistic effect of the three elements in improving the anti-vulcanization property and the reflectance is remarkable. Further, although comparative example 1 was slightly peeled off, the film of example 3 of the present application had good adhesion to the substrate.
Comparative example 4 compared with example 3, comparative example 4 was not added with an alnico alloy, but with the addition of aluminum and nickel alone, and as a result, comparative example 4 was significantly reduced in the effect of all of adhesion to a substrate, anti-sulfidation property and reflectivity, indicating that the alloy was more advantageous for improving the above properties than the metal element alone, probably because the metal element alone had a higher melting point, a greater difficulty in melting, and was disadvantageous for uniform dispersion.
Comparative examples 5 to 6, compared with example 3, demonstrate that too high or too low an amount of the alnico alloy is detrimental to improving the anti-sulfidation properties and reflectivity of the film, and must be within a suitable range of amounts to have a good effect.
Comparative example 7 shows that the replacement of the alnico alloy with other types of alloys, the reduction in the anti-sulfidation performance and the reflectivity, compared with example 3, shows that the alnico alloy of the present application is more advantageous in improving the anti-sulfidation performance and the reflectivity of the film.
The foregoing detailed description is directed to one of the possible embodiments of the present application, which is not intended to limit the scope of the application, but is to be accorded the full scope of all such equivalents and modifications so as not to depart from the scope of the application.
Claims (9)
1. The silver sulfide resistant alloy target is characterized by comprising the following components in parts by weight: 90-99 parts of silver, 1-3 parts of indium, 1-3 parts of aluminum-nickel alloy, 0.01-0.15 part of scandium, 0.01-0.1 part of magnesium and 0.01-0.08 part of palladium;
the mass ratio of aluminum to nickel in the aluminum-nickel alloy is 1:2-4.
2. A method for preparing the silver sulfide resistant alloy target material according to claim 1, comprising the following steps:
(1) Preparing materials according to a proportion, and mixing and smelting the raw materials to obtain an alloy cast ingot;
(2) Forging the alloy cast ingot obtained in the step (1) to obtain a blank;
(3) And (5) carrying out hot rolling and annealing treatment on the blank in sequence to obtain the finished product.
3. The method according to claim 2, wherein the smelting temperature in step (1) is 1150-1350 ℃.
4. The method according to claim 2, wherein the forging ratio in step (2) is 2.5 to 3.
5. The method according to claim 2, wherein the hot rolling in the step (3) is carried out at 550 to 700 ℃ for 1 to 3 hours with a total deformation of 60 to 70%.
6. The method according to claim 2, wherein the annealing temperature in the step (3) is 550-700 ℃, and the temperature is kept for 20-30min.
7. The preparation method according to claim 2, wherein the pretreatment is performed before smelting each raw material in step (1), and the specific pretreatment process is as follows: and dissolving the rest components except the aluminum-nickel alloy and the binder in absolute ethyl alcohol, drying to obtain mixed powder, and mixing with the aluminum-nickel alloy.
8. The preparation method according to claim 7, wherein the binder is a mixture of polyethylene glycol and polyethylene glycol, and the mass ratio of the polyethylene glycol to the polyethylene glycol is 3-5:1.
9. The use of the silver sulfide resistant alloy target material according to claim 1 or the silver sulfide resistant alloy target material prepared by the preparation method according to any one of claims 2 to 8 in a liquid crystal display or an organic light emitting diode.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211610110.0A CN115976478B (en) | 2022-12-13 | 2022-12-13 | Silver sulfide resistant alloy target and preparation method thereof |
Applications Claiming Priority (1)
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| TW200530411A (en) * | 2003-12-10 | 2005-09-16 | Tanaka Precious Metal Ind | Silver alloy for reflective film |
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| CN115341187A (en) * | 2022-08-26 | 2022-11-15 | 中山智隆新材料科技有限公司 | Silver alloy target material and preparation method and application thereof |
| TW202246534A (en) * | 2021-01-22 | 2022-12-01 | 日商三菱綜合材料股份有限公司 | Ag alloy film, and Ag alloy sputtering target |
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| EP1734140A1 (en) * | 2003-12-10 | 2006-12-20 | Tanaka Kikinzoku Kogyo Kabushiki Kaisha | Silver alloy excelling in performance of reflectance maintenance |
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