CN114411104A - High-purity silver target and preparation method and application thereof - Google Patents
High-purity silver target and preparation method and application thereof Download PDFInfo
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- CN114411104A CN114411104A CN202210059031.9A CN202210059031A CN114411104A CN 114411104 A CN114411104 A CN 114411104A CN 202210059031 A CN202210059031 A CN 202210059031A CN 114411104 A CN114411104 A CN 114411104A
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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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
- B21J—FORGING; HAMMERING; PRESSING METAL; RIVETING; FORGE FURNACES
- B21J5/00—Methods for forging, hammering, or pressing; Special equipment or accessories therefor
- B21J5/002—Hybrid process, e.g. forging following casting
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23P—METAL-WORKING NOT OTHERWISE PROVIDED FOR; COMBINED OPERATIONS; UNIVERSAL MACHINE TOOLS
- B23P15/00—Making specific metal objects by operations not covered by a single other subclass or a group in this subclass
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- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- C21D1/00—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
- C21D1/26—Methods of annealing
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- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- C21D9/00—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor
- C21D9/0068—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor for particular articles not mentioned below
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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
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/3407—Cathode assembly for sputtering apparatus, e.g. Target
- C23C14/3414—Metallurgical or chemical aspects of target preparation, e.g. casting, powder metallurgy
Abstract
The invention provides a high-purity silver target and a preparation method and application thereof, wherein the purity of the high-purity silver target is 4N 5-5N, the microstructure of the high-purity silver target is fine and uniform grains, and the average grain size is less than or equal to 30 mu m; the preparation method mainly comprises the following steps: (1) carrying out first recrystallization annealing after the silver ingot is subjected to hot forging to obtain a first blank; (2) the first blank is subjected to static pressure deformation treatment and then is rolled to obtain a second blank; (3) and carrying out secondary recrystallization annealing on the second blank to obtain the high-purity silver target. The high-purity silver target is free of defects, the thickness of a film layer is uniform after the liquid crystal display is subjected to PVD coating, and the yield of the liquid crystal display is greatly improved.
Description
Technical Field
The invention relates to the technical field of sputtering target materials, in particular to a high-purity silver target and a preparation method and application thereof.
Background
The sputtering target material is an important key material necessary for manufacturing a semiconductor chip, and the principle of utilizing the sputtering target material to manufacture a device is to adopt a physical vapor deposition technology and bombard the target material by high-pressure accelerated gaseous ions so as to enable atoms of the target material to be sputtered out and deposited on a silicon wafer in a thin film mode, and finally a complex wiring structure in the semiconductor chip is formed.
The sputtering target has many advantages of uniformity, controllability and the like of metal coating, and is widely applied to the field of semiconductors. Silver is used in large quantities for the production of thin layers of electrodes or reflective layers, such as solar cells, liquid crystal displays, etc., due to its excellent properties of low electrical resistance and high reflectivity. With the rapid development of semiconductor technology, the technical requirements corresponding to solar cells and liquid crystal displays are higher and higher, so that the silver target material must meet the requirements of no defect inside, uniform structure, fine crystal grains and high purity, and the preparation process of the high-purity silver target has greater challenge.
CN103667768A discloses a method for manufacturing a silver target, which comprises the steps of selecting a silver raw material with the purity of more than 4N, melting the silver raw material by using an atmospheric smelting or vacuum smelting method, casting the molten liquid, cooling to form an ingot blank, immediately carrying out heat preservation and heat treatment on the ingot blank, carrying out heat preservation and homogenization at the temperature of 400-900 ℃, keeping the temperature for more than 0.5h, then carrying out hot rolling or air hammer forging to form a silver blank, carrying out cold rolling on the silver blank to form a cold rolled blank, carrying out annealing and heat treatment on the cold rolled blank, wherein the annealing and heat treatment temperature is 350-700 ℃, the annealing and heat treatment time is 0.5-3 h, obtaining the silver target blank, and finally obtaining the large-size silver target through machine tool processing.
CN105039920A discloses a preparation method of a high-density high-purity sputtering rotary silver target. Firstly, processing stainless steel according to the requirements of customers, then carrying out sand blasting by using brown corundum and priming by using Cu-Al wires, wherein the thickness of the priming layer is 0.5 mm. And spraying the silver powder by using a Laval nozzle made of tungsten carbide alloy, wherein the structure of the nozzle designed by the tungsten carbide alloy is shown in figure 1, the silver powder is spherical powder, the granularity is 5-45 micrometers, the nitrogen pressure is 3-5 Mpa, the nitrogen heating temperature is 400-500 ℃, and the powder feeding rotating speed is 6 RPM. The particles are accelerated for 2 times through the Laval nozzle, and the particle speed is increased to 600-800 m/s. The silver target material prepared by cold spraying has the advantages of simple process and compact structure, the relative density of the target material can reach more than 99.8 percent, and the grain structure inside the target material is uniform, fine and free from defect. And the deposition efficiency is high, and the production cost is reduced.
However, the silver target blank prepared by the method has large and uneven grain size distribution, and the sputtering rate is easily uncontrollable and the film thickness is uneven when the physical vapor deposition technology is adopted for coating, so that the liquid crystal display is scrapped due to uneven resistivity.
Therefore, the development of a preparation method of the high-purity silver target with fine grains and uniform distribution is of great significance.
Disclosure of Invention
In order to solve the technical problems, the invention provides a high-purity silver target and a preparation method and application thereof, and the steps of static pressure deformation treatment and recrystallization annealing are added in the existing silver target preparation method, so that crystal grains in the silver target become fine and are uniformly distributed; the preparation method has the advantages of simple process and low cost, and is suitable for industrial popularization.
In order to achieve the purpose, the invention adopts the following technical scheme:
in a first aspect, the invention provides a high-purity silver target, wherein the purity of the high-purity silver target is 4N 5-5N, the microstructure of the high-purity silver target is fine and uniform grains, and the average grain size is less than or equal to 30 microns.
The high-purity silver target has high purity, fine and uniform internal crystal grains, the average crystal grain size is less than or equal to 30 mu m, the thickness of a film layer is uniform after the high-purity silver target is used for PVD coating of a liquid crystal display, and the yield of the liquid crystal display is greatly improved to more than 98% from the original 90%.
In a second aspect, the present invention also provides a method for preparing a high purity silver target as described in the first aspect, the method comprising the steps of:
(1) carrying out first recrystallization annealing after the silver ingot is subjected to hot forging to obtain a first blank; the heat preservation time of the hot forging is 30-60 min; the temperature of the first recrystallization annealing is 200-300 ℃;
(2) the first blank is subjected to static pressure deformation treatment and then is rolled to obtain a second blank;
(3) and carrying out secondary recrystallization annealing on the second blank to obtain the high-purity silver target.
According to the preparation method of the high-purity silver target, the heat preservation time of hot forging is 30-60 min, when the heat preservation time of hot forging is short, the heating of the cast ingot is uneven, the final crystal grains are uneven, and the cast ingot is cracked during forging; when the hot forging heat preservation time is longer, the ingot casting crystal grains further grow and coarsen; the temperature of the first recrystallization annealing is 200-300 ℃, and when the temperature of the first recrystallization annealing is lower, the recrystallization of crystal grains is insufficient, so that the size of the crystal grains is not uniform; when the first recrystallization annealing temperature is higher, the grains are further grown and coarsened after the recrystallization of the grains is completed. Compared with the existing method which only sequentially adopts high-temperature forging, rolling deformation and recrystallization annealing, the preparation method of the high-purity silver target disclosed by the invention carries out twice recrystallization annealing, so that the crystal grains in the silver target are more uniformly distributed; the step of static pressure deformation is added, so that the crystal grains in the silver target can be finer, and the high-purity silver target with uniformly distributed crystal grains and the average crystal grain size of less than or equal to 30 mu m is finally obtained.
The heat preservation time of the hot forging is 30-60 min, for example, 30min, 32min, 35min, 40min, 45min, 50min, 55min or 60 min.
The first recrystallization annealing temperature of the present invention is 200 to 300 ℃, and may be, for example, 200 ℃, 210 ℃, 220 ℃, 230 ℃, 250 ℃, 260 ℃, 280 ℃ or 300 ℃.
Preferably, the purity of the silver ingot in the step (1) is 4N 5-5N, and the silver ingot can be 4N5, 4N6, 4N7, 4N8, 4N9 or 5N.
Preferably, the hot forging temperature is 300 to 350 ℃, for example, 300 ℃, 302 ℃, 305 ℃, 308 ℃, 310 ℃, 315 ℃, 320 ℃, 330 ℃ or 350 ℃.
Preferably, the hot forging comprises three-way forging, and the deformation in each direction is more than or equal to 55%, such as 55%, 56%, 58%, 60%, 65%, 68% or 70%.
The three-way forging of the invention refers to the forging in the x, y and z directions respectively.
Preferably, the holding time of the first recrystallization annealing is 60 to 90min, for example, 60min, 65min, 70min, 80min, 85min, 88min or 90 min.
Preferably, the pressure direction of the static pressure deformation treatment in the step (2) is parallel to the length direction of the silver ingot, and the deformation amount is more than or equal to 65%, such as 65%, 66%, 68%, 70%, 75% or 80%.
Preferably, the temperature of the static pressure deformation treatment is 20 to 30 ℃, and may be, for example, 20 ℃, 21 ℃, 23 ℃, 25 ℃, 28 ℃ or 30 ℃.
Preferably, the rolling reduction amount in the step (2) is 1-2 mm/pass, and may be, for example, 1 mm/pass, 1.1 mm/pass, 1.2 mm/pass, 1.4 mm/pass, 1.5 mm/pass, 1.8 mm/pass or 2 mm/pass.
Preferably, the rolling temperature is 20 to 30 ℃, for example, 20 ℃, 21 ℃, 23 ℃, 25 ℃, 28 ℃ or 30 ℃.
The thickness of the second blank obtained after rolling is not limited, and the thickness of the silver target can be actually required.
Preferably, the temperature of the second recrystallization annealing in the step (3) is 200 to 300 ℃, and may be, for example, 200 ℃, 210 ℃, 220 ℃, 230 ℃, 250 ℃, 260 ℃, 280 ℃ or 300 ℃.
Preferably, the holding time of the second recrystallization annealing is 60 to 90min, for example, 60min, 65min, 70min, 80min, 85min, 88min or 90 min.
Preferably, after the hot forging in the step (1), the first recrystallization and the second recrystallization in the step (3) are all performed with water cooling.
Preferably, the second recrystallization annealing of the step (3) is further followed by turning.
The recitation of numerical ranges herein includes not only the above-recited values, but also any values between any of the above-recited numerical ranges not recited, and for brevity and clarity, is not intended to be exhaustive of the specific values encompassed within the range.
As a preferred technical scheme of the invention, the preparation method comprises the following steps:
(1) carrying out hot forging on silver ingots with the purity of 4N 5-5N at the temperature of 300-350 ℃ for 30-60 min, and then carrying out first recrystallization annealing at the temperature of 200-300 ℃ for 60-90 min to obtain first blanks; the hot forging comprises three-way forging, and the deformation in each direction is more than or equal to 55 percent;
(2) after the first blank is subjected to static pressure deformation treatment at the temperature of 20-30 ℃, rolling at the temperature of 20-30 ℃ and with the pressing amount of 1-2 mm per pass is carried out to obtain a second blank; the pressure direction of the static pressure deformation treatment is parallel to the length direction of the silver ingot, and the deformation amount is more than or equal to 65 percent;
(3) carrying out secondary recrystallization annealing on the second blank at the temperature of 200-300 ℃ for 60-90 min, and turning to obtain the high-purity silver target;
and (3) performing water cooling treatment after the hot forging in the step (1), the first recrystallization and the second recrystallization in the step (3).
In a third aspect, the invention also provides the use of the high-purity silver target of the first aspect in sputter film formation in a liquid crystal display.
Compared with the prior art, the invention has at least the following beneficial effects:
the preparation method of the high-purity silver target provided by the invention has simple process, and the high-purity silver target with fine and uniformly distributed crystal grains can be prepared; the thickness of the film layer of the high-purity silver target is uniform after PVD coating of the liquid crystal display, and the yield of the liquid crystal display is greatly improved to more than 98% from 90%.
Detailed Description
For the purpose of facilitating an understanding of the present invention, the present invention will now be described by way of examples. It should be understood by those skilled in the art that the examples are only for the understanding of the present invention and should not be construed as the specific limitations of the present invention.
The present invention is described in further detail below. The following examples are merely illustrative of the present invention and do not represent or limit the scope of the claims, which are defined by the claims.
Example 1
The embodiment provides a preparation method of a high-purity silver target, which comprises the following steps:
(1) carrying out hot forging on a silver ingot with the purity of 4N8 at the temperature of 330 ℃ for 40min, and then carrying out first recrystallization annealing at the temperature of 270 ℃ for 80min to obtain a first blank; the hot forging comprises three-way forging, and the deformation in each direction is more than or equal to 55 percent;
(2) after the first blank is subjected to static pressure deformation treatment at the temperature of 26 ℃, rolling at the temperature of 25 ℃ and with the pressing amount of 1.2mm per pass is carried out to obtain a second blank; the pressure direction of the static pressure deformation treatment is parallel to the length direction of the silver ingot, and the deformation amount is 68%;
(3) carrying out second recrystallization annealing on the second blank at the temperature of 230 ℃ for 70min, and turning to obtain the high-purity silver target;
and (3) performing water cooling treatment after the hot forging in the step (1), the first recrystallization and the second recrystallization in the step (3).
Example 2
The embodiment provides a preparation method of a high-purity silver target, which comprises the following steps:
(1) carrying out hot forging on a silver ingot with the purity of 4N5 at the temperature of 350 ℃ for 60min, and then carrying out first recrystallization annealing at the temperature of 300 ℃ for 60min to obtain a first blank; the hot forging comprises three-way forging, and the deformation in each direction is more than or equal to 55 percent;
(2) after the first blank is subjected to static pressure deformation treatment at the temperature of 30 ℃, rolling at the temperature of 30 ℃ and with the pressing amount of 1mm per pass is carried out to obtain a second blank; the pressure direction of the static pressure deformation treatment is parallel to the length direction of the silver ingot, and the deformation amount is 65%;
(3) carrying out second recrystallization annealing on the second blank at the temperature of 200 ℃ for 60min, and turning to obtain the high-purity silver target;
and (3) performing water cooling treatment after the hot forging in the step (1), the first recrystallization and the second recrystallization in the step (3).
Example 3
The embodiment provides a preparation method of a high-purity silver target, which comprises the following steps:
(1) carrying out hot forging on a silver ingot with the purity of 5N at the temperature of 300 ℃ for 30min, and then carrying out first recrystallization annealing at the temperature of 200 ℃ for 90min to obtain a first blank; the hot forging comprises three-way forging, and the deformation in each direction is more than or equal to 55 percent;
(2) carrying out static pressure deformation treatment on the first blank at the temperature of 20 ℃, and then carrying out rolling with the temperature of 20-30 ℃ and the pressing amount of 2mm per pass to obtain a second blank; the pressure direction of the static pressure deformation treatment is parallel to the length direction of the silver ingot, and the deformation amount is more than or equal to 65 percent;
(3) carrying out second recrystallization annealing on the second blank at the temperature of 300 ℃ for 90min, and turning to obtain the high-purity silver target;
and (3) performing water cooling treatment after the hot forging in the step (1), the first recrystallization and the second recrystallization in the step (3).
Comparative example 1
This comparative example provides a method of manufacturing a high purity silver target, which is the same as example 1 except that the holding time for hot forging in step (1) was changed from 40min to 20 min.
Comparative example 2
This comparative example provides a method of manufacturing a high purity silver target, which is the same as example 1, except that the heat-retaining time for the hot forging in step (1) was changed from 40min to 80 min.
Comparative example 3
This comparative example provides a method of manufacturing a high purity silver target, which is the same as example 1 except that the temperature of the first recrystallization annealing in step (1) was changed from 270 ℃ to 180 ℃.
Comparative example 4
This comparative example provides a method of manufacturing a high purity silver target, which is the same as example 1 except that the temperature of the first recrystallization annealing in step (1) was changed from 270 ℃ to 330 ℃.
Comparative example 5
This comparative example provides a method of manufacturing a high purity silver target, which is the same as example 1 except that the first recrystallization annealing in step (1) is omitted.
Comparative example 6
This comparative example provides a method of manufacturing a high purity silver target, which is the same as example 1 except that the static pressure deformation treatment in step (2) is omitted.
The average grain size and grain distribution of the high purity silver targets prepared in the above examples and comparative examples are shown in table 1.
TABLE 1
As can be seen from table 1:
(1) the comprehensive examples 1-3 show that the average grain size of the high-purity silver target obtained by the preparation method of the high-purity silver target is less than or equal to 30 microns, and the grains are uniformly distributed;
(2) it can be seen from the combination of the example 1 and the comparative examples 1-2 that the heat preservation time of the hot forging in the step (1) of the example 1 is 40min, compared with the heat preservation time of the hot forging in the step (1) of the comparative examples 1 and 2 which is 20min and 80min respectively, the average grain size of the high-purity silver target obtained in the example 1 is 23 μm, and the grain distribution is uniform, while the average grain size of the high-purity silver target obtained in the comparative example 1 is 32 μm due to the shorter heat preservation time of the hot forging, but the grain distribution is not uniform, and the forging treatment is carried out during the use, so that the cracking sometimes occurs; comparative example 2 because the heat preservation time of hot forging is longer, the crystal grains of the cast ingot can further grow and coarsen, and the obtained high-purity silver target has uniform crystal grain distribution, but the average crystal grain size is larger and is 52 mu m; therefore, the invention limits the heat preservation time of hot forging to 30-60 min, and can obtain the high-purity silver target with fine crystal grains which uniformly meet the use requirement of the liquid crystal display;
(3) it can be seen from the combination of example 1 and comparative examples 3 to 4 that the first recrystallization annealing temperature in step (1) of example 1 is 270 ℃, compared with the first recrystallization annealing temperatures of 180 ℃ and 330 ℃ in step (1) of comparative examples 3 and 4, respectively, the average grain size of the high-purity silver target obtained in example 1 is 23 μm, and the grain distribution is uniform, while in comparative example 3, the first recrystallization annealing temperature is lower, so that the grain recrystallization is insufficient, and the grain size is not uniform; comparative example 4 since the first recrystallization annealing temperature was higher, the grains further grew and coarsened after the completion of the recrystallization of the grains, and the average grain size was 56 μm; therefore, the temperature of the first recrystallization annealing is limited to 200-300 ℃, and the high-purity silver target with fine and uniform crystal grains meeting the use requirement of the liquid crystal display can be obtained;
(4) it can be seen from the combination of example 1 and comparative examples 5-6 that, in the step (1) of example 1, the silver ingot is subjected to hot forging and then subjected to first recrystallization annealing, and in the step (2), the static pressure deformation treatment is performed, so that compared with the case that the first recrystallization annealing in the step (1) is omitted in the step (5) of comparative example and the static pressure deformation treatment in the step (2) is omitted in the comparative example 6, the high-purity silver target prepared in the example 1 has fine crystal grains and uniform and consistent crystal grain distribution, and in the comparative example 5 and the comparative example 6, the necessary treatment process is omitted, so that the average crystal grain sizes of the obtained high-purity silver target are 65 μm and 71 μm respectively, which are far larger than those in the example 1, and the crystal grains are distributed unevenly; therefore, the method for preparing the high-purity silver target can obtain the high-purity silver target with fine and uniform crystal grains which meet the use requirement of the liquid crystal display by sequentially carrying out hot forging, first recrystallization annealing, static pressure deformation treatment and second recrystallization annealing on the silver ingot.
In conclusion, the preparation method of the high-purity silver target provided by the invention has simple process, can prepare the high-purity silver target with fine and uniformly distributed crystal grains, and is suitable for the liquid crystal display.
The applicant declares that the above description is only a specific embodiment of the present invention, but the scope of the present invention is not limited thereto, and it should be understood by those skilled in the art that any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention are within the scope and disclosure of the present invention.
Claims (10)
1. The high-purity silver target is characterized in that the purity of the high-purity silver target is 4N 5-5N, the microstructure of the high-purity silver target is fine and uniform grains, and the average grain size is less than or equal to 30 mu m.
2. A method for preparing a high purity silver target according to claim 1, comprising the steps of:
(1) carrying out first recrystallization annealing after the silver ingot is subjected to hot forging to obtain a first blank; the heat preservation time of the hot forging is 30-60 min; the temperature of the first recrystallization annealing is 200-300 ℃;
(2) the first blank is subjected to static pressure deformation treatment and then is rolled to obtain a second blank;
(3) and carrying out secondary recrystallization annealing on the second blank to obtain the high-purity silver target.
3. The preparation method according to claim 2, wherein the purity of the silver ingot in the step (1) is 4N 5-5N;
preferably, the temperature of the hot forging is 300-350 ℃;
preferably, the hot forging comprises three-way forging, and the deformation amount in each direction is more than or equal to 55 percent.
4. The method according to claim 2 or 3, wherein the first recrystallization annealing in the step (1) is performed for 60 to 90 min.
5. The preparation method according to any one of claims 2 to 4, wherein the pressure direction of the static pressure deformation treatment in the step (2) is parallel to the length direction of the silver ingot, and the deformation amount is not less than 65%;
preferably, the temperature of the static pressure deformation treatment is 20-30 ℃;
preferably, the rolling reduction is 1-2 mm per pass;
preferably, the rolling temperature is 20-30 ℃.
6. The method according to any one of claims 2 to 5, wherein the temperature of the second recrystallization annealing in the step (3) is 200 to 300 ℃;
preferably, the heat preservation time of the second recrystallization annealing is 60-90 min.
7. The production method according to any one of claims 2 to 6, wherein water cooling treatment is performed after the hot forging in the step (1), after the first recrystallization and after the second recrystallization in the step (3) are completed.
8. The method according to any one of claims 2 to 7, wherein the second recrystallization annealing in the step (3) is further followed by turning.
9. The method according to any one of claims 2 to 8, characterized by comprising the steps of:
(1) carrying out hot forging on silver ingots with the purity of 4N 5-5N at the temperature of 300-350 ℃ for 30-60 min, and then carrying out first recrystallization annealing at the temperature of 200-300 ℃ for 60-90 min to obtain first blanks; the hot forging comprises three-way forging, and the deformation in each direction is more than or equal to 55 percent;
(2) after the first blank is subjected to static pressure deformation treatment at the temperature of 20-30 ℃, rolling at the temperature of 20-30 ℃ and with the pressing amount of 1-2 mm per pass is carried out to obtain a second blank; the pressure direction of the static pressure deformation treatment is parallel to the length direction of the silver ingot, and the deformation amount is more than or equal to 65 percent;
(3) carrying out secondary recrystallization annealing on the second blank at the temperature of 200-300 ℃ for 60-90 min, and turning to obtain the high-purity silver target;
and (3) performing water cooling treatment after the hot forging in the step (1), the first recrystallization and the second recrystallization in the step (3).
10. Use of the high purity silver target of claim 1 for sputter film formation in liquid crystal displays.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115141952A (en) * | 2022-07-05 | 2022-10-04 | 株洲火炬安泰新材料有限公司 | High-purity silver target material and processing method thereof |
| CN115233123A (en) * | 2022-07-20 | 2022-10-25 | 宁波江丰电子材料股份有限公司 | Aluminum-copper alloy target blank and preparation method thereof |
| CN115992342A (en) * | 2022-12-15 | 2023-04-21 | 先导薄膜材料（广东）有限公司 | High-purity silver sputtering target material and preparation method thereof |
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| CN104694862A (en) * | 2013-12-09 | 2015-06-10 | 有研亿金新材料股份有限公司 | Preparation method of silver sputtering target blank |
| CN112921287A (en) * | 2021-01-22 | 2021-06-08 | 宁波江丰电子材料股份有限公司 | Ultrahigh-purity copper target material and grain orientation control method thereof |
| CN113755801A (en) * | 2021-09-17 | 2021-12-07 | 福州大学 | Preparation method of high-purity aluminum target material with uniform orientation |
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| CN104694862A (en) * | 2013-12-09 | 2015-06-10 | 有研亿金新材料股份有限公司 | Preparation method of silver sputtering target blank |
| CN112921287A (en) * | 2021-01-22 | 2021-06-08 | 宁波江丰电子材料股份有限公司 | Ultrahigh-purity copper target material and grain orientation control method thereof |
| CN113755801A (en) * | 2021-09-17 | 2021-12-07 | 福州大学 | Preparation method of high-purity aluminum target material with uniform orientation |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115141952A (en) * | 2022-07-05 | 2022-10-04 | 株洲火炬安泰新材料有限公司 | High-purity silver target material and processing method thereof |
| CN115233123A (en) * | 2022-07-20 | 2022-10-25 | 宁波江丰电子材料股份有限公司 | Aluminum-copper alloy target blank and preparation method thereof |
| CN115992342A (en) * | 2022-12-15 | 2023-04-21 | 先导薄膜材料（广东）有限公司 | High-purity silver sputtering target material and preparation method thereof |
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