CN115522094B - Multi-doped silver alloy target material and preparation method and application thereof - Google Patents
Multi-doped silver alloy target material and preparation method and application thereof Download PDFInfo
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- CN115522094B CN115522094B CN202211155517.9A CN202211155517A CN115522094B CN 115522094 B CN115522094 B CN 115522094B CN 202211155517 A CN202211155517 A CN 202211155517A CN 115522094 B CN115522094 B CN 115522094B
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- 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
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- 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
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- 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
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/14—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of noble metals or alloys based thereon
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—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
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/3407—Cathode assembly for sputtering apparatus, e.g. Target
Abstract
The invention discloses a multielement doped silver alloy target, and a preparation method and application thereof, wherein the target comprises the following preparation raw materials in parts by weight: 97.24-99.944 parts of silver; 0.05 to 2.5 portions of copper; 0.005-0.25 part of manganous oxide; 0.001 to 0.01 part of tin. The silver alloy target material has good oxidation resistance, corrosion resistance and high reflectivity, and can be applied to reflective films, conductive films and organic light-emitting diodes.
Description
Technical Field
The invention relates to the technical field of metal targets, in particular to a multi-doped silver alloy target, and a preparation method and application thereof.
Background
The coating target is a sputtering source for forming various functional films on the substrate by magnetron sputtering, multi-arc ion plating or other types of coating systems under proper process conditions. Silver has the excellent performances of high reflectivity, low extinction coefficient, high thermal conductivity, low resistivity, good surface smoothing effect and the like, and is plated on a substrate by a common magnetron sputtering technology to prepare a silver-based film which is used for producing an electrode film or a reflecting layer film of a liquid crystal display, an optical recording medium and low-radiation glass.
Because the silver film is easy to oxidize and vulcanize when exposed to the air for a long time, the pure silver target material also has the defects of low heat resistance and low environmental resistance, so that the film formed by the pure silver target material is easy to oxidize when exposed to the air for a long time, the conductivity and the reflectivity of the film are greatly reduced, the adhesiveness with a glass substrate is poor, and the final use performance of the product is affected.
Therefore, it is necessary to provide a new multi-doped silver alloy target material capable of improving the oxidation resistance and corrosion resistance of the silver alloy thin film.
Disclosure of Invention
The present invention aims to solve at least one of the technical problems existing in the prior art. Therefore, the first aspect of the invention provides a multi-doped silver alloy target material, which can effectively improve oxidation resistance and corrosion resistance.
The multielement doped silver alloy target provided by the embodiment of the first aspect of the invention comprises the following preparation raw materials in parts by weight:
in the invention, the standard potential of Ag is 0.799V, the standard electrode potential of Cu is 0.337V, the standard potential of Mn is-1.18V, the standard potential of Sn is-0.136V, and the electrochemical principle of metals is as follows: in case of a large difference in the standard potentials of the two metals M1 and M2, a battery couple will be established. If EM1< EM2, the metal M2 will be protected as cathode to accept electrons, and M1 will be corroded, so adding trace Cu element with standard potential lower than Ag into silver target material can improve corrosion resistance of silver target material, and adding standard potential Cu > Mn > Sn, mn, sn can further increase corrosion resistance of silver target material.
In addition, cu is dissolved in Ag, has the effects of improving the strength of crystal grains and preventing recrystallization, and also has the effect of inhibiting the increase of the roughness of the surface of a coating film caused by the coarseness of the crystal grains due to heat in the subsequent plasma sputtering treatment, so that the adverse effect of reflectivity reduction caused by rapid corrosion generated by the roughness of the surface of the coating film can be avoided; after adding the manganous oxide and the tin, copper-manganese and copper-tin compounds can be formed in the alloy, the compounds have face-centered cubic lattices, the face-centered cubic lattices are stable, and the hardness of a target material can be improved, so that the warping degree in the machining process can be reduced, and the corrosion resistance and the oxidation resistance of the silver alloy film can be improved; meanwhile, the chemical property of the manganous oxide is stable, and the micro oxygen element is contained, so that the reaction of the metal component in the silver alloy film with oxygen in the atmospheric environment can be inhibited, and the oxidation resistance of the silver alloy film is further improved.
According to some embodiments of the invention, the multi-doped silver alloy target comprises the following preparation raw materials in parts by weight:
according to some embodiments of the invention, the multi-doped silver alloy target comprises the following preparation raw materials in parts by weight:
according to some embodiments of the invention, the silver has a purity of at least 99.99%.
An embodiment of the second aspect of the present invention provides a method for preparing a multi-doped silver alloy target, including the steps of:
and mixing and smelting silver, copper, manganous oxide and tin, sequentially casting and forming, hot forging, rolling, annealing, machining and binding to obtain the multi-element doped silver alloy target.
According to some embodiments of the invention, the method comprises the steps of: and smelting the manganous oxide, copper, silver and tin in sequence, casting and forming in sequence, hot forging, rolling, machining and binding to obtain the multi-element doped silver alloy target.
Three preparation raw materials are sequentially added according to the sequence from high melting point to low melting point, and the former preparation raw material is smelted for a period of time and then added into the latter preparation raw material, so that when the latter preparation raw material with a slightly lower melting point is added, the former preparation raw material with a high melting point is smelted for a period of time, the whole smelting time can be saved, the smelting effect can be improved, and the four preparation raw materials are fully mixed.
According to some embodiments of the invention, the smelting temperature is 1100-1200 ℃. Thus, silver, copper, manganous oxide and tin can be sufficiently melted.
According to some embodiments of the invention, the temperature of the hot forging is 480-550 ℃, and the heat preservation time of the hot forging is 2-4 h.
According to some embodiments of the invention, the total deformation of the hot forging is 30-50%.
According to some embodiments of the invention, the rolling single pass reduction is 10-15%.
According to some embodiments of the invention, the rolling has a total reduction of 70%.
According to some embodiments of the invention, machining refers to machining a cast-formed blank to a finished size.
According to some embodiments of the invention, binding refers to binding the machined semifinished product with the support. The support may be plate-like or tubular. For example, the machined semi-finished product is plate-shaped, a copper backboard is used as a back support piece and is attached to the back of the machined semi-finished product, and solder binding is adopted between the backboard and the target material.
According to some embodiments of the invention, the bound solder comprises silver tin alloy solder.
A third aspect of the present invention provides a silver alloy thin film prepared using the multi-doped silver alloy target described above.
A fourth aspect of the present invention provides the use of the silver alloy thin film described above in a reflective film, a conductive film, an organic light emitting diode.
Additional features and advantages of the invention will be set forth in the description which follows, and in part will be obvious from the description, or may be learned by practice of the invention.
Drawings
The foregoing and/or additional aspects and advantages of the invention will become apparent and may be better understood from the following description of embodiments taken in conjunction with the accompanying drawings in which:
FIG. 1 is a schematic diagram of the basic principle of electrochemical corrosion of metals according to examples 1-3 of the present invention;
FIG. 2 is a sample schematic and a mosaic schematic of the target performance test of the present invention.
Detailed Description
The following are specific embodiments of the present invention, and the technical solutions of the present invention will be further described with reference to the embodiments, but the present invention is not limited to these embodiments.
The reagents, methods and apparatus employed in the present invention, unless otherwise specified, are all conventional in the art.
Example 1
Example 1 provides a silver alloy target, the content of the preparation raw materials is shown in table 1, and the preparation method is as follows:
s1, weighing manganous-manganic oxide, copper, silver and tin according to mass, placing the manganous-manganic oxide, copper, silver and tin in a low-frequency magnetic induction smelting furnace, pumping the graphite crucible to 0.001Pa in vacuum degree, introducing nitrogen gas for atmosphere protection, gradually raising the temperature to 1200 ℃, controlling the temperature raising rate to 30 ℃/min, and fully smelting to obtain an ingot;
s2, smelting, casting and forming the cast ingot by using an electron beam smelting furnace, and pumping the vacuum degree of the electron beam smelting furnace to be below 0.001; in the smelting process, the feeding speed is controlled to be 140Kg/h, the smelting speed is consistent with the feeding speed, the ingot pulling speed is controlled to be matched with the smelting speed, so that the liquid level of a molten pool is kept stable, and finally, an ingot with the diameter of 100-500 mm is formed, and an alloy ingot is subjected to hot forging, rolling, machining and binding to obtain the silver alloy target. The method comprises the steps of hot forging at 480 ℃, cooling to room temperature after hot forging, rolling, wherein the single rolling reduction is 10%, and the total reduction is 50%, so as to obtain the silver alloy target with phi 76.2 multiplied by 6.35 mm.
The basic schematic diagram of the metal electrochemical corrosion of this embodiment is shown in fig. 1.
Example 2
Example 2 provides a silver alloy target, the content of the preparation raw materials is shown in table 1, and the preparation method is as follows:
s1, weighing manganous-manganic oxide, copper, silver and tin according to mass, placing the manganous-manganic oxide, copper, silver and tin in a low-frequency magnetic induction smelting furnace, pumping the graphite crucible to 0.001Pa in vacuum degree, introducing nitrogen gas for atmosphere protection, gradually raising the temperature to 1200 ℃, controlling the temperature raising rate to 30 ℃/min, and fully smelting to obtain an ingot;
s2, smelting, casting and forming the cast ingot by using an electron beam smelting furnace, and pumping the vacuum degree of the electron beam smelting furnace to be below 0.001; in the smelting process, the feeding speed is controlled to be 140Kg/h, the smelting speed is consistent with the feeding speed, the ingot pulling speed is controlled to be matched with the smelting speed, so that the liquid level of a molten pool is kept stable, and finally, an ingot with the diameter of 100-500 mm is formed, and an alloy ingot is subjected to hot forging, rolling, machining and binding to obtain the silver alloy target. The method comprises the steps of hot forging at 480 ℃, cooling to room temperature after hot forging, rolling, wherein the single rolling reduction is 10%, and the total reduction is 50%, so as to obtain the silver alloy target with phi 76.2 multiplied by 6.35 mm.
Example 3
Example 3 provides a silver alloy target, the content of the preparation raw materials is shown in table 1, and the preparation method is as follows:
s1, weighing manganous-manganic oxide, copper, silver and tin according to mass, placing the manganous-manganic oxide, copper, silver and tin in a low-frequency magnetic induction smelting furnace, pumping the graphite crucible to 0.001Pa in vacuum degree, introducing nitrogen gas for atmosphere protection, gradually raising the temperature to 1200 ℃, controlling the temperature raising rate to 30 ℃/min, and fully smelting to obtain an ingot;
s2, smelting, casting and forming the cast ingot by using an electron beam smelting furnace, and pumping the vacuum degree of the electron beam smelting furnace to below 0.001 Pa; in the smelting process, the feeding speed is controlled to be 140Kg/h, the smelting speed is consistent with the feeding speed, the ingot pulling speed is controlled to be matched with the smelting speed, so that the liquid level of a molten pool is kept stable, and finally, an ingot with the diameter of 100-500 mm is formed, and an alloy ingot is subjected to hot forging, rolling, machining and binding to obtain the silver alloy target. The method comprises the steps of hot forging at 480 ℃, cooling to room temperature after hot forging, rolling, wherein the single rolling reduction is 10%, and the total reduction is 50%, so as to obtain the silver alloy target with phi 76.2 multiplied by 6.35 mm.
Comparative example 1
Comparative example 1 provides a silver alloy target, the preparation method and preparation raw material of which are the same as those of example 1, except that copper element is not included in this example.
Comparative example 2
Comparative example 2 provides a silver alloy target, the preparation method and preparation raw materials of which are the same as those of example 1, except that trimanganese tetroxide is not included in this example.
Comparative example 3
Comparative example 3 provides a silver alloy target, the preparation method and preparation raw materials of which are the same as those of example 1, except that tin is not included in this example.
Comparative example 4
Comparative example 4 provides a silver target, which is prepared by a method and raw materials similar to those of example 1, except that copper, trimanganese tetroxide, and tin are not included in this example.
Table 1 the contents (parts) of the raw materials for preparation of examples 1 to 3 and comparative examples 1 to 4
| Example 1 | Example 2 | Example 3 | Comparative example 1 | Comparative example 2 | Comparative example 3 | Comparative example 4 | |
| Silver (Ag) | 98.494 | 98.739 | 98.4845 | 99.994 | 98.499 | 98.495 | 100 |
| Copper (Cu) | 1.5 | 1.25 | 1.5 | - | 1.5 | 1.5 | - |
| Manganous oxide of manganese | 0.005 | 0.006 | 0.0065 | 0.005 | - | 0.005 | - |
| Tin (Sn) | 0.001 | 0.005 | 0.009 | 0.001 | 0.001 | - | - |
Test example 1:
target performance test
Metallographic samples prepared from the silver alloy targets of examples 1-3 and comparative examples 1-4 are used for measuring grain size and hardness, and a sampling schematic diagram and a mosaic schematic diagram of the target performance test are shown in fig. 2.
The grain size test method comprises the following steps: three points are taken at an angle of 90 degrees, each point is taken to be two samples, 10 x 2mm, transparent resin is adopted for thermal mosaic, abrasive paper with 180-240-400-800-1200 meshes is adopted for grinding in sequence, flannelette is adopted for polishing until a mirror surface is prepared into a metallographic sample with the diameter phi of 30 x 10mm, finally acid liquor is adopted for corrosion for 10-20 seconds, and a metallographic microscope is adopted for measuring the grain size.
Hardness: the surface and side hardness of the metallographic samples were measured with a vickers hardness tester.
The test results are shown in Table 2.
Table 2 data for testing target properties of examples 1 to 3 and comparative examples 1 to 4
From the doping components of examples and comparative examples in Table 1, examples 1 to 3 were doped with 3 components, comparative examples 1 to 3 were doped with 2 components, and comparative example 4 was undoped.
As can be seen from the data in table 2, in the silver alloy targets of examples 1 to 3 of the present invention, the grain size was 108um or less, the grain size of the silver alloy targets of comparative examples 1 to 3 was 170um or less, and the grain size of the silver target of comparative example 4 was 180um or less; in examples 1 to 3 of the present invention, the hardness of the silver alloy targets was 124Hv or less, the hardness of the silver alloy targets of comparative examples 1 to 3 was 100Hv or less, and the hardness of the silver target of comparative example 4 was 90Hv or less. From the standpoint of grain size and hardness, examples 1 to 3 doped with 3 components are clearly superior to comparative examples 1 to 3 doped with 2 components, and comparative examples 1 to 3 doped with 2 components are superior to comparative example 4 undoped.
Test example 2:
film performance test: silver alloy targets of examples 1 to 3 and comparative examples 1 to 4 were prepared as silver alloy films: and (3) using a magnetron sputtering machine to prepare the film with the thickness of 100nm on the glass substrate with the thickness of 0.5mm at the sputtering pressure of 0.3Pa and the sputtering power of 500W.
The silver alloy targets of examples 1 to 3 and comparative examples 1 to 4 were tested for oxidation resistance, heat resistance, reflectance, and corrosion resistance:
oxidation resistance: the target material was placed in a water bath at 80 ℃ and observed for oxidation resistance.
Heat resistance: and (3) annealing each silver alloy film for 10min at four annealing temperatures of 150 ℃, 250 ℃, 350 ℃ and 450 ℃ to observe the surface morphology of each silver alloy film after annealing.
Reflectivity: and (3) carrying out reflectivity test on the silver alloy film by utilizing a spectrophotometer under the condition of 380-780 nm wavelength.
Corrosion resistance: corrosion resistance tests were carried out in examples and comparative examples using a corrosion test liquid dip. Corrosion test liquid composition: 20g/L of sodium chloride (NaCl) and ammonium chloride (NH) 4 Cl) 17.5g/L, urea (CH) 4 N 2 O) 5g/L acetic acid (CH) 3 COOH) 2.5g/L, lactic acid (C) 3 H 6 O 3 ) 15g/L and sodium hydroxide (NaOH), and the pH of the corrosion test liquid was adjusted to 4.7 by adjusting the sodium hydroxide content.
The test results are shown in Table 3.
TABLE 3 data for film Performance test of examples 1-3 and comparative examples 1-4
From the doping components of examples and comparative examples in Table 1, examples 1 to 3 were doped with 3 components, comparative examples 1 to 3 were doped with 2 components, and comparative example 4 was undoped. As is clear from the data in Table 3, the thin films prepared with the silver alloy targets of examples 1 to 3 of the present invention had oxidation resistance of 35 minutes or more, reflectance of 94.5% or more, corrosion resistance of 30 hours, and good heat resistance at high temperature. From the viewpoints of oxidation resistance, heat resistance, reflectance and corrosion resistance, examples 1 to 3 doped with 3 components are clearly superior to comparative examples 1 to 3 doped with 2 components, and comparative examples 1 to 3 doped with 2 components are superior to comparative example 4 undoped.
The present invention has been described in detail with reference to the above embodiments, but the present invention is not limited to the above embodiments, and various changes can be made within the knowledge of those skilled in the art without departing from the spirit of the present invention.
Claims (8)
1. A multi-element doped silver alloy target is characterized in that,
the preparation method comprises the following preparation raw materials in parts by weight:
98.4835 to 98.994 parts of silver;
1.0-1.5 parts of copper;
0.005-0.0065 parts of manganous oxide;
0.001 to 0.01 part of tin.
2. The multi-doped silver alloy target of claim 1, wherein the purity of the silver is at least 99.99%.
3. A method of preparing a multi-doped silver alloy target according to claim 1 or 2, comprising the steps of:
and sequentially smelting the silver, copper, manganous oxide and tin, sequentially carrying out casting molding, hot forging, rolling, machining and binding to obtain the multi-doped silver alloy target.
4. The method for preparing a multi-doped silver alloy target according to claim 3, wherein the smelting temperature is 1100-1200 ℃.
5. The method for preparing the multi-doped silver alloy target according to claim 3, wherein the hot forging condition is that the temperature is 480-550 ℃ and the heat preservation time is 2-4 hours.
6. The method of preparing a multi-doped silver alloy target according to claim 3, wherein the total deformation of the hot forging is 30-50%.
7. A silver alloy thin film prepared from the multi-doped silver alloy target of claim 1 or 2.
8. Use of the silver alloy thin film according to claim 7 in a reflective film, a conductive film, an organic light emitting diode.
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