CN115976478A - Silver sulfide resistant alloy target material and preparation method thereof - Google Patents
Silver sulfide resistant alloy target material 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
- 239000013077 target material Substances 0.000 title claims abstract description 31
- 229910052946 acanthite Inorganic materials 0.000 title claims abstract description 18
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 229940056910 silver sulfide Drugs 0.000 title claims abstract description 18
- XUARKZBEFFVFRG-UHFFFAOYSA-N silver sulfide Chemical compound [S-2].[Ag+].[Ag+] XUARKZBEFFVFRG-UHFFFAOYSA-N 0.000 title claims description 15
- 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 28
- NPXOKRUENSOPAO-UHFFFAOYSA-N Raney nickel Chemical class [Al].[Ni] NPXOKRUENSOPAO-UHFFFAOYSA-N 0.000 claims abstract description 23
- 229910052738 indium Inorganic materials 0.000 claims abstract description 15
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 claims abstract description 15
- 229910052763 palladium Inorganic materials 0.000 claims abstract description 14
- 229910052706 scandium Inorganic materials 0.000 claims abstract description 11
- SIXSYDAISGFNSX-UHFFFAOYSA-N scandium atom Chemical compound [Sc] SIXSYDAISGFNSX-UHFFFAOYSA-N 0.000 claims abstract description 11
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-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
- 239000002202 Polyethylene glycol Substances 0.000 claims description 16
- 229920001223 polyethylene glycol Polymers 0.000 claims description 16
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 15
- 239000011230 binding agent Substances 0.000 claims description 12
- 238000000034 method Methods 0.000 claims description 11
- 239000000203 mixture Substances 0.000 claims description 10
- 239000000463 material Substances 0.000 claims description 9
- 238000005242 forging Methods 0.000 claims description 8
- 238000005098 hot rolling Methods 0.000 claims description 8
- 239000011812 mixed powder Substances 0.000 claims description 8
- 238000002156 mixing Methods 0.000 claims description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 7
- 229910052782 aluminium Inorganic materials 0.000 claims description 7
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 7
- 229910052759 nickel Inorganic materials 0.000 claims description 7
- 239000002994 raw material Substances 0.000 claims description 7
- 238000003723 Smelting Methods 0.000 claims description 6
- 238000000137 annealing Methods 0.000 claims description 6
- 230000008569 process Effects 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 4
- 238000002844 melting Methods 0.000 claims description 4
- 230000008018 melting Effects 0.000 claims description 4
- 239000004973 liquid crystal related substance Substances 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims description 3
- 238000002310 reflectometry Methods 0.000 abstract description 14
- 238000004073 vulcanization Methods 0.000 abstract description 7
- 230000000694 effects Effects 0.000 abstract description 6
- 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 27
- 239000010408 film Substances 0.000 description 26
- 230000000052 comparative effect Effects 0.000 description 21
- 229910052751 metal Inorganic materials 0.000 description 8
- 239000000654 additive Substances 0.000 description 6
- 230000000996 additive effect Effects 0.000 description 6
- 229910000828 alnico Inorganic materials 0.000 description 6
- 238000004321 preservation Methods 0.000 description 5
- 238000005486 sulfidation Methods 0.000 description 5
- 238000005987 sulfurization reaction Methods 0.000 description 5
- 239000000853 adhesive Substances 0.000 description 4
- 230000001070 adhesive effect Effects 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- 229910052761 rare earth metal Inorganic materials 0.000 description 4
- 238000004544 sputter deposition Methods 0.000 description 4
- 239000000758 substrate Substances 0.000 description 4
- 239000010409 thin film Substances 0.000 description 4
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 3
- 230000009286 beneficial effect Effects 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
- 238000007747 plating Methods 0.000 description 3
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 238000005096 rolling process Methods 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 239000011593 sulfur Substances 0.000 description 2
- 229910052717 sulfur Inorganic materials 0.000 description 2
- 230000002195 synergetic effect Effects 0.000 description 2
- 229910018507 Al—Ni Inorganic materials 0.000 description 1
- 229910000861 Mg 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
- 239000002390 adhesive tape Substances 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation 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
- 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
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 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
- 229910000510 noble metal Inorganic materials 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
- MUJIDPITZJWBSW-UHFFFAOYSA-N palladium(2+) Chemical compound [Pd+2] MUJIDPITZJWBSW-UHFFFAOYSA-N 0.000 description 1
- 229910052697 platinum Inorganic materials 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
- 238000005477 sputtering target Methods 0.000 description 1
- 238000006467 substitution reaction Methods 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
Abstract
The invention relates to the technical field of metal material processing, in particular to an anti-silver sulfide alloy target material and a preparation method thereof, wherein the anti-silver sulfide alloy target material comprises the following components in parts by weight: 90 to 99 parts of silver, 1 to 3 parts of indium, 1 to 3 parts of aluminum-nickel alloy, 0.01 to 0.15 part of scandium, 0.01 to 0.1 part of magnesium and 0.01 to 0.08 part of palladium, and has excellent effects in terms of vulcanization resistance and reflectivity.
Description
Technical Field
The invention relates to the technical field of metal material processing, in particular to an anti-silver sulfide alloy target material and a preparation method thereof.
Background
The target material is also called sputtering target material, and is named as target material bombarded by high-speed metal plasma flow in the sputtering process. The target material is a core raw material for preparing functional films in the fields of semiconductors, display panels, photovoltaics and the like, and the process cannot be replaced. Different film systems can be obtained by replacing different targets, thereby realizing the functions of conduction or blocking and the like.
At present, most of the target materials for display are metal targets, silver is the cheapest of noble metals, and has excellent characteristics such as low resistance and high reflectivity,the film is widely applied to the fields of semiconductors, displays, electronic device reflecting films, radiation-proof glass and the like. However, pure silver has a disadvantage that when the silver-based thin film is exposed to air or a high-temperature and high-humidity environment for a long time, the surface of the thin film is easily oxidized and easily reacts with H in the air 2 And reacting S gas to generate tarnished silver sulfide. The generated sulfide or oxide absorbs blue light, so that the reflectivity of a blue light wave band in the reflecting layer is reduced, the reflectivity of the film is further reduced, and phenomena such as silver crystal grain growth or silver atom agglomeration are easy to generate. Therefore, the silver-based thin film has problems such as a decrease in conductivity and reflectance, and a deterioration in adhesion to the substrate, and these disadvantages of pure silver can be improved by doping with 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 components in parts by mass are: 90-99 parts of metallic silver, 1-3 parts of a metallic element additive and 0.001-0.1 part of a rare earth element additive, wherein the purity of the metallic silver is at least 99.99%, and the silver alloy target material is obtained by smelting the metallic silver, the metallic element additive and the rare earth element additive according to a certain proportion, so that the prepared silver alloy target material has more excellent performance compared with the traditional silver alloy target material, the adhesion capacity of the silver alloy target material and a base material is greatly improved, and the silver alloy target material 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 Ag x In y M z Q n Wherein, the proportion of the indium is more than or equal to 8 percent and less than or equal to 40 percent (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 percent (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 percent (atomic ratio), and the content of the silver x is more than or equal to 60 percent (atomic ratio). The silver alloy target can be prepared into a silver alloy film with excellent heat resistance, adhesive force, conductivity, corrosion resistance and sulfidization resistance by magnetron sputtering plating, ion sputtering plating, vacuum evaporation plating or electron beam evaporation, and is suitable for a reflective electrode film, a liquid crystal display and an optical recording mediumOrganic light emitting diode and electrochromism.
Chinese patent application CN105316630a discloses a silver alloy target material, a manufacturing method thereof and an organic light emitting diode using the same, wherein the silver alloy target material is substantially composed of silver and indium or silver, indium, palladium and copper. The average grain size is between 33 μm and 126 μm. 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 ratio and controlling the average grain size to be between 33 μm and 126 μm, the silver alloy target can be used for preparing a silver alloy thin film with good heat resistance, sulfidation resistance, adhesion, high reflectivity and high fineness through sputtering, but the effects of the silver alloy target in various aspects are to be further improved.
However, the film obtained from the silver alloy target cannot simultaneously achieve 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 and a method for preparing the same, which can solve the above-mentioned problems.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a silver alloy target material with excellent effects in the aspects of sulfuration resistance and reflectivity and a preparation method thereof.
The invention 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 invention also relates to a preparation method of the silver sulfide resistant alloy target, which comprises the following steps:
(1) Preparing materials according to a ratio, mixing the raw materials, and smelting to obtain an alloy cast ingot;
(2) Forging the alloy ingot obtained in the step (1) to obtain a blank;
(3) And carrying out hot rolling and annealing treatment on the blank in sequence to obtain the product.
Preferably, the temperature of melting in step (1) is 1150-1350 ℃.
More preferably, step (1) is at 1X 10 -2 To 1X 10 -4 Heating to 1150-1350 ℃ under the vacuum degree of a torr, and preserving heat for 0.5-1 h for smelting.
Preferably, the smelting process in step (1) is carried out 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 the hot rolling in the step (3) is 550-700 ℃, the heat preservation is carried out for 1-3h, 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 performed before each raw material is smelted in the step (1), and the specific pretreatment process comprises the following steps: 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 addition amount of the binder is 0.5 to 3% by mass of silver
More preferably, the preparation method comprises the following steps:
(1) Preparing materials according to a ratio, dissolving the other 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 the mixture and drying the mixture to obtain mixed powder, mixing the mixed powder with the aluminum-nickel alloy, heating the mixed powder to 1150-1350 ℃ under a vacuum condition, and preserving heat for 0.5-1 h to smelt to obtain an alloy ingot;
(2) Forging the alloy ingot obtained in the step (1) at the temperature of 550-700 ℃, and keeping the temperature for 1-3 hours, wherein the forging ratio is 2.5-3, so as to obtain a blank;
(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 1-3h, the total deformation is 60-70%, the reduction rate of each pass is controlled to be 10-12%, annealing treatment is carried out at the temperature of 550-700 ℃ once every two passes in the rolling process, and the heat preservation is carried out for 20-30min, so as to obtain the product.
The invention also relates to the 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 invention are:
according to the invention, the aluminum-nickel alloy is added into the silver-based target material, and compared with the way of independently adding aluminum and nickel or adding other alloys, the sulfuration resistance of the silver-based target material can be obviously improved.
Scandium, magnesium and palladium added in the silver-based target material have obvious synergistic effect, and the anti-sulfuration performance and reflectivity of the target material are improved.
According to the invention, a small amount of indium, aluminum-nickel alloy, scandium, magnesium and palladium are added into the silver-based target material, and the components act synergistically, so that the film formed after sputtering has excellent effects in the aspects of sulfuration resistance, oxidation resistance and reflectivity, and has high adhesive force with the base material.
In addition, the binder is added in the process of preparing the silver-based target material, the composition of the binder is optimized, the uniformity of the silver-based target material is improved, the components can fully play the roles, and the comprehensive performance of the silver-based target material is excellent.
Detailed Description
The invention is further described below in conjunction with specific embodiments, and the advantages and features of the invention will become more apparent as the description proceeds. These examples are illustrative only and do not limit the scope of the present invention in any way. It will be understood by those skilled in the art that various changes in form and details may be made therein without departing from the spirit and scope of the invention, and that such changes and substitutions are intended to be within the scope of the invention.
The purity of the silver and the indium adopted by the invention is more than 99.99 percent, and the purity of other elements is more than 99.9 percent.
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 ratio, dissolving the rest components except the aluminum-nickel alloy and 2% of a 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 the mixture and drying the mixture to obtain mixed powder, mixing the mixed powder with the aluminum-nickel alloy, heating the mixed powder to 1350 ℃ under a vacuum condition, and preserving heat for 1h for smelting to obtain an alloy cast ingot;
(2) Forging the alloy ingot obtained in the step (1), keeping the temperature at 650 ℃ for 2 hours, and obtaining a blank material, 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 time is 2h, the total deformation is 60%, the reduction rate of each pass is controlled to be 10% of the deformation, annealing treatment is carried out at the temperature of 650 ℃ every two passes in the rolling process, and the heat preservation time is 30min.
The following examples and comparative examples were prepared according to the same procedure 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 the example 3 is only that in the preparation process, the raw materials in the step (1) are directly mixed and smelted without adding a binder or being dissolved 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 changed in parts.
TABLE 1
| Comparative example 1/part | Comparative example 2/part | Comparative example 3/part | |
| Silver | 95 | 95 | 95 |
| Indium (In) | 2 | 2 | 2 |
| Aluminum-nickel alloy | 2 | 2 | 2 |
| Scandium (Sc) | 0 | 0.133 | 0.133 |
| Magnesium alloy | 0.1 | 0.067 | 0 |
| Palladium (II) | 0.1 | 0 | 0.067 |
Comparative example 4
The only difference from example 3 is that no Al-Ni alloy was added, 0.5 parts of Al and 1.5 parts of Ni were added separately, and the other conditions were the same as in example 3.
Comparative example 5
The difference from example 3 is only that the amount of the alnico alloy used is 2 parts to 5 parts, and the other conditions are the same as example 3.
Comparative example 6
Except for the difference from example 3 in that the amount of the alnico alloy was changed to 2 parts to 0.5 part, the other conditions were the same as example 3.
Comparative example 7
The only difference from example 3 is that the alnico was replaced with an equal mass ni-v alloy (mass ratio of ni and v 3:1). Test example 1 adhesion test (film thickness 150 nm)
The silver alloy films were placed in a high-temperature and high-humidity environment with a humidity of 85% and a temperature of 85 ℃ for 96 hours, and then a peel test was performed using Scotch 600 type Scotch tape from 3M company. The adhesive tape is torn off after being attached to the surface of each silver alloy film, and if the silver alloy films are not peeled off, the silver alloy films and the base material have good adhesive force. Specific results are shown in table 2.
Test example 2 anti-vulcanization test (film thickness 150 nm)
And (3) placing each silver alloy film in a closed environment in which sulfur steam is introduced, observing the condition that each silver alloy film is blackened when contacting with the sulfur steam, and recording the time required for blackening. As shown in Table 2, the better the vulcanization resistance, the longer the time required for the surface to become black in the vulcanization treatment.
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. Specific results are shown in table 2.
TABLE 2
As can be seen from the data in Table 2:
compared with the example 3, the preparation process of the example 4 has no adhesive, the uniformity of the film is poor, the functions of all components are influenced, and the adhesion between the film and the base material is poor. And the differences between the vulcanization resistance and the reflectivity at different positions of the film are large, so table 2 shows the range values.
Comparative examples 1-3 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 simultaneously, and comparative examples 1-3 and example 3 have the same addition of the three elements. As a result, the vulcanization resistance and the reflectance of comparative examples 1 to 3 were not as good as those of example 3, indicating that the three elements had a significant synergistic effect in improving the vulcanization resistance and the reflectance. In comparative example 1, although slight peeling occurred, 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 did not add an aluminum-nickel alloy, but added aluminum and nickel alone, and as a result, comparative example 4 was significantly less effective in adhesion to the substrate, anti-sulfidation performance, and reflectivity, indicating that the alloy is more beneficial to improving the above performance than the metal element alone, probably because the metal element alone has a higher melting point and a higher melting difficulty, which is not beneficial to uniform dispersion.
Comparing the comparative examples 5-6 with example 3, it is demonstrated that too high or too low amount of the alnico is not good for improving the anti-sulfuration property and reflectivity of the film, and must be within the proper amount range to have better effect.
Comparative example 7 compared with example 3, it shows that the sulfidation resistance and reflectivity are reduced by replacing the alnico with other types of alloys, and the alnico of the present invention is more advantageous to improve the sulfidation resistance and reflectivity of the film.
The above detailed description is specific to one possible embodiment of the present invention, and the embodiment is not intended to limit the scope of the present invention, and all equivalent implementations or modifications without departing from the scope of the present invention should be included in the technical scope of the present invention.
Claims (10)
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.
2. The silver sulfide resistant alloy target according to claim 1, wherein the mass ratio of aluminum to nickel in the aluminum-nickel alloy is 1:2-4.
3. The method for preparing the silver sulfide resistant alloy target material of any one of claims 1-2, which is characterized by comprising the following steps:
(1) Preparing materials according to a ratio, mixing the raw materials, and smelting to obtain an alloy ingot;
(2) Forging the alloy ingot obtained in the step (1) to obtain a blank;
(3) And (4) carrying out hot rolling and annealing treatment on the blank in sequence to obtain the product.
4. The production method according to claim 3, wherein the temperature of melting in the step (1) is 1150-1350 ℃.
5. The production method according to claim 3, wherein the forging ratio in the step (2) is 2.5 to 3.
6. The method according to claim 3, wherein the hot rolling in the step (3) is carried out at a temperature of 550-700 ℃ for 1-3 hours and a total deformation of 60-70%.
7. The method according to claim 3, wherein the annealing in step (3) is carried out at a temperature of 550 to 700 ℃ for 20 to 30min.
8. The preparation method according to claim 3, wherein each raw material is pretreated before being smelted in the step (1), and the specific pretreatment process comprises the following steps: 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.
9. The preparation method of claim 8, 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.
10. Use of the silver sulfide resistant alloy target according to any one of claims 1 to 2 or the silver sulfide resistant alloy target prepared by the preparation method according to any one of claims 3 to 9 in a liquid crystal display or an organic light emitting diode.
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| CN202211610110.0A CN115976478B (en) | 2022-12-13 | 2022-12-13 | Silver sulfide resistant alloy target and preparation method thereof |
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| CN202211610110.0A CN115976478B (en) | 2022-12-13 | 2022-12-13 | Silver sulfide resistant alloy target and preparation method thereof |
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| Publication Number | Publication Date |
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| CN115976478A true CN115976478A (en) | 2023-04-18 |
| CN115976478B CN115976478B (en) | 2023-11-28 |
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| CN117247273A (en) * | 2023-11-17 | 2023-12-19 | 江苏迪纳科精细材料股份有限公司 | Preparation method and device of X-IZO magnetron sputtering target material with high mobility |
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