CN117070905A - Oversized silver alloy target and preparation method thereof - Google Patents
Oversized silver alloy target and preparation method thereof Download PDFInfo
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- CN117070905A CN117070905A CN202311210455.1A CN202311210455A CN117070905A CN 117070905 A CN117070905 A CN 117070905A CN 202311210455 A CN202311210455 A CN 202311210455A CN 117070905 A CN117070905 A CN 117070905A
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- silver alloy
- alloy target
- oversized
- silver
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- 229910001316 Ag alloy Inorganic materials 0.000 title claims abstract description 72
- 238000002360 preparation method Methods 0.000 title claims abstract description 27
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims abstract description 24
- 229910052709 silver Inorganic materials 0.000 claims abstract description 24
- 239000004332 silver Substances 0.000 claims abstract description 24
- 229910052738 indium Inorganic materials 0.000 claims abstract description 19
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 claims abstract description 19
- 238000005098 hot rolling Methods 0.000 claims abstract description 17
- 238000003723 Smelting Methods 0.000 claims abstract description 14
- 238000005097 cold rolling Methods 0.000 claims abstract description 13
- 238000005242 forging Methods 0.000 claims abstract description 13
- 238000010438 heat treatment Methods 0.000 claims abstract description 11
- 229910052751 metal Inorganic materials 0.000 claims abstract description 11
- 239000002184 metal Substances 0.000 claims abstract description 11
- 239000013077 target material Substances 0.000 claims abstract description 10
- 238000005266 casting Methods 0.000 claims abstract description 7
- 238000002310 reflectometry Methods 0.000 claims abstract description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 8
- 238000000137 annealing Methods 0.000 claims description 8
- 229910045601 alloy Inorganic materials 0.000 claims description 7
- 239000000956 alloy Substances 0.000 claims description 7
- 229910052786 argon Inorganic materials 0.000 claims description 4
- 238000000034 method Methods 0.000 claims description 4
- 238000005096 rolling process Methods 0.000 claims description 4
- 238000004321 preservation Methods 0.000 claims description 3
- 230000008569 process Effects 0.000 claims description 3
- 238000004544 sputter deposition Methods 0.000 abstract description 11
- 238000000576 coating method Methods 0.000 abstract description 4
- 239000011248 coating agent Substances 0.000 abstract description 2
- 239000013078 crystal Substances 0.000 abstract 1
- 239000007769 metal material Substances 0.000 abstract 1
- 238000010583 slow cooling Methods 0.000 abstract 1
- 238000011161 development Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000000758 substrate Substances 0.000 description 3
- 230000002159 abnormal effect Effects 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 238000000151 deposition Methods 0.000 description 2
- 230000008021 deposition Effects 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 230000003746 surface roughness Effects 0.000 description 2
- 229920001621 AMOLED Polymers 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 230000008676 import Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000010884 ion-beam technique Methods 0.000 description 1
- 239000004973 liquid crystal related substance Substances 0.000 description 1
- 238000001755 magnetron sputter deposition Methods 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000006104 solid solution Substances 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 238000005477 sputtering target Methods 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
Classifications
-
- 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
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C5/00—Alloys based on noble metals
- C22C5/06—Alloys based on silver
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Crystallography & Structural Chemistry (AREA)
- Physical Vapour Deposition (AREA)
Abstract
The invention relates to the technical field of metal targets, in particular to an oversized silver alloy target and a preparation method thereof. The silver alloy target consists of silver and indium, wherein the mass percentage of the indium is 0.3-0.6%, and the balance is silver. The size of the silver alloy target is 2300×1800×14mm. The invention discloses a preparation method of an oversized silver alloy target, which comprises the following steps: smelting silver and indium metal material in vacuum furnace at 1100-1200 deg.c and vacuum degree less than or equal to 6 x 10 ‑2 mmH, when in casting, the temperature of a casting chamber is 700-1000 ℃, and the silver alloy spindle is obtained by slow cooling, and the obtained silver alloy spindle is subjected to hot forging, hot rolling, cold rolling and heat treatment to obtain the silver alloy target with oversized size and average grain size10-40 μm. According to the invention, the crystal grains of the silver alloy target material are fine and uniform by adding the indium with a specific proportion into the pure silver. The oversized silver alloy target is suitable for sputtering coating and can be used for preparing silver alloy films with good conductivity and reflectivity. The invention has very important significance for the application of the oversized silver alloy target material.
Description
Technical Field
The invention relates to the technical field of metal targets, in particular to an oversized silver alloy target and a preparation method thereof.
Background
Along with the continuous development of semiconductor chip preparation research and development industry, a sputtering film material occupies an important position in the semiconductor field, wherein magnetron sputtering is one of important technologies for preparing film materials, and based on a phase deposition technology, a high-energy ion beam is utilized to bombard a target material, so that target atoms escape and deposit on the surface of a substrate to form a layer of compact film, the product performance of the sputtering film is determined by the performance of the sputtering film, namely, the product performance is closely related to factors such as grain size, tissue uniformity and impurity content of the target material, the finer and more uniform grain size is, the better the sputtering speed and thickness uniformity of a deposition layer are, and high-quality sputtering film products can be ensured. On the other hand, the quality of the film formed on the substrate can be influenced by the surface roughness of the silver target, the thickness of the film material prepared by sputtering the target with lines or coarser surface is uneven, the local electric field is easy to be uneven during working, abnormal discharge is generated at the convex position, and components are damaged, so that the process for preparing the silver target needs to be changed, the product requirement is improved, and the microstructure, the morphology and the like of the silver target are improved.
With the continuous development of display technology, the performance requirements of the fields such as liquid crystal televisions and touch screens on organic light emitting diode devices are higher and higher, particularly, the requirements of the development of AMOLED devices cannot be met by the domestic existing targets due to the import of Mitsubishi corporation in the manufacture of large-size and multiple devices of the large-size silver alloy targets, and high energy is generated at the joints of the targets due to the fact that the non-uniformity of spraying is easily caused when the large-area planar targets are sprayed, so that the requirements on the large-area covered single-chip sputtering targets are increased increasingly, and therefore, the silver alloy targets with the ultra-large size and better performance are required to be obtained, and the sputtered silver plating films with the large area, high coverage rate, smooth surface and excellent photoelectric property can be deposited on a flexible substrate.
Disclosure of Invention
In view of the above, the invention aims to provide an oversized silver alloy target and a preparation method thereof, so as to solve the problems of large preparation difficulty and coarse and uneven grains of the oversized silver alloy target.
Based on the above purpose, the invention provides an oversized silver alloy target and a preparation method thereof, and the specific operation steps are as follows:
the invention provides an oversized silver alloy target and a preparation method thereof, wherein the silver alloy target consists of silver and indium; wherein the mass percentage of indium is 0.3-0.6%, and the balance is silver.
Preferably, the length of the oversized silver alloy target is more than or equal to 2m, the width is more than or equal to 1.5m, and the thickness is more than or equal to 0.01m.
Preferably, the length of the oversized silver alloy target is 2.3m, the width is 1.8m, and the thickness is 0.014m.
Preferably, the oversized silver alloy target and the preparation method thereof comprise the following steps: smelting, hot forging, hot rolling, cold rolling and annealing.
Preferably, the maximum temperature of the smelting chamber is 1100-1200 ℃.
Preferably, when the metal is melted, argon is introduced for protection, and the vacuum degree is less than or equal to 6 multiplied by 10 -2 mmH。
Preferably, the spout temperature of the smelting furnace is 950-1150 ℃.
Preferably, the mould chamber temperature is 700-1000 ℃.
Preferably, the heating temperature in the hot forging process is 600-800 ℃.
Preferably, the forging ratio is 3.5 to 4.5.
Preferably, the hot rolling heating temperature is 500-700 ℃.
Preferably, the hot rolling is performed for a total of 6 passes, the first 5 passes being all reversing rolling.
Preferably, the deformation of each pass of hot rolling is 25% -25% -25% -25% -20% -3%.
Preferably, the total deformation of the hot rolling is 86%.
Preferably, the total deformation of the cold rolling is 71%, and then the reversing leveling is performed.
Preferably, the maximum temperature at the time of annealing is 300-400 ℃.
Preferably, the holding time at the highest temperature during the annealing is 1-2h.
Preferably, the average grain size of the oversized silver alloy target is 20-80 μm.
Preferably, the oversized silver alloy target can be used for preparing a silver alloy film with good conductivity and reflectivity.
Compared with the prior art, the invention has the beneficial effects that:
(1) The invention provides a silver alloy target material, which consists of silver and indium, wherein the mass percent of the indium is 0.3-0.6%, and the balance is silver. Because the solid solubility of indium in silver is higher, the addition of indium can form solid solution strengthening, and the effect of refining grains is generated, so that the strength of the silver alloy is improved. The oversized silver alloy target is prepared through smelting, hot forging, hot rolling, cold rolling, annealing and other steps. According to customer feedback, on the basis of maintaining good conductivity and reflectivity of the silver alloy film, the adhesiveness of the silver alloy film can be greatly improved, and the surface roughness of the silver alloy film can be improved.
(2) In the silver alloy target material, the average grain size of the oversized silver alloy target material is 20-80 mu m, and fine grains can ensure the high-quality sputtering coating process, so that the problems of arc abnormal discharge and sputtering in the sputtering coating process are reduced.
(4) The invention provides an oversized silver alloy target and a preparation method thereof, which have the advantages of simple process, convenient operation, low cost and the like, and are suitable for large-scale industrialized preparation and subsequent application.
Drawings
In order to more clearly illustrate the invention or the technical solutions of the prior art, the drawings which are used in the description of the embodiments or the prior art will be briefly described, it being obvious that the drawings in the description below are only of the invention and that other drawings can be obtained from them without inventive effort for a person skilled in the art.
FIG. 1 is a photograph of an oversized silver alloy target of example 1;
FIG. 2 is a metallographic photograph of an oversized silver alloy target of example 1;
fig. 3 is a metallographic photograph of an oversized silver alloy target in example 2.
Detailed Description
The present invention will be further described in detail with reference to specific embodiments in order to make the objects, technical solutions and advantages of the present invention more apparent.
Example 1
An oversized silver alloy target and a preparation method thereof, comprising the following steps:
the silver alloy target consists of silver and indium, wherein the mass percentage of the indium is 0.6 percent, and the balance is silver.
And (3) taking a metal silver block with purity more than 99.99%, and putting the metal silver block into a vacuum smelting furnace, wherein the highest temperature of a smelting chamber is 1200 ℃. When the metal is melted, adding indium blocks with purity more than 99.999%, then introducing argon for protection, and the vacuum degree is less than or equal to 6 multiplied by 10 -2 mmH. During casting, the temperature of the nozzle of the smelting furnace is 1150 ℃ and the temperature of the casting chamber is 1000 ℃. And finally, slowly cooling to obtain the silver alloy spindle.
The obtained silver alloy spindle was hot forged at a heating temperature of 800 ℃ and a forging ratio of 4.5. And hot rolling the alloy blank after hot forging, wherein the heating temperature is 700 ℃. The total hot rolling is 6 times, the reversing rolling is carried out in the first 5 times, the deformation of each time is 25% -25% -25% -20% -3%, and the total deformation is 86%. And (3) performing cold rolling deformation on the alloy blank after hot rolling, wherein the cold rolling deformation is 71%, and then reversing and leveling. And annealing the alloy blank after cold rolling, wherein the highest temperature is 300 ℃ and the heat preservation time is 2 hours. After the processing and the heat treatment, the oversized silver alloy target with the length of 2.3m, the width of 1.8m, the thickness of 0.014m and the average grain size of 13 mu m is finally obtained.
Example 2
An oversized silver alloy target and a preparation method thereof, comprising the following steps:
the silver alloy target consists of silver and indium, wherein the mass percentage of the indium is 0.3 percent, and the balance is silver.
Taking a metal silver block with purity more than 99.99%, and putting the metal silver block into a vacuum smelting furnace, wherein the highest temperature of a smelting chamber is 1000 ℃; when the metal is melted, adding indium blocks with purity more than 99.999%, then introducing argon for protection, and the vacuum degree is less than or equal to 6 multiplied by 10 -2 mmH; during casting, the temperature of a nozzle of the smelting furnace is 950 ℃ and the temperature of a casting chamber is 700 ℃; and finally, slowly cooling to obtain the silver alloy spindle.
Carrying out hot forging on the obtained silver alloy spindle, wherein the heating temperature is 600 ℃, and the forging ratio is 3.5; hot rolling the alloy blank after hot forging, wherein the heating temperature is 500 ℃; the total hot rolling is 6 times, the reversing rolling is carried out in the first 5 times, the deformation of each time is 25% -25% -25% -20% -3%, and the total deformation is 86%; cold rolling deformation is carried out on the alloy blank after hot rolling, the cold rolling deformation is 71%, and then reversing and leveling are carried out; annealing the alloy blank after cold rolling, wherein the highest temperature is 400 ℃ and the heat preservation time is 1h; after the processing and the heat treatment, the oversized silver alloy target with the length of 2.3m, the width of 1.8m, the thickness of 0.014m and the average grain size of 38 mu m is finally obtained.
In summary, according to the oversized silver alloy target and the preparation method thereof provided by the invention, the grains of the silver alloy target are fine and uniform by adding the indium with a specific proportion into the pure silver. The size of the oversized silver alloy target material prepared by the method is 2300 multiplied by 1800 multiplied by 14mm, and the average grain size is 10-40 mu m. The oversized silver alloy target is suitable for sputtering coating and can be used for preparing silver alloy films with good conductivity and reflectivity. The invention has very important significance for the application of the oversized silver alloy target material.
Those of ordinary skill in the art will appreciate that: the discussion of any of the embodiments above is merely exemplary and is not intended to suggest that the scope of the invention (including the claims) is limited to these examples; the technical features of the above embodiments or in the different embodiments may also be combined within the idea of the invention, the steps may be implemented in any order and there are many other variations of the different aspects of the invention as described above, which are not provided in detail for the sake of brevity.
The present invention is intended to embrace all such alternatives, modifications and variances which fall within the broad scope of the appended claims. Therefore, any omission, modification, equivalent replacement, improvement, etc. of the present invention should be included in the scope of the present invention.
Claims (10)
1. An oversized silver alloy target and a preparation method thereof are characterized in that the silver alloy target consists of silver and indium; wherein the mass percentage of indium is 0.3-0.6%, and the balance is silver;
the length of the silver alloy target material is more than or equal to 2m, the width is more than or equal to 1.5m, and the thickness is more than or equal to 0.01m.
2. The oversized silver alloy target and the preparation method thereof according to claim 1, wherein the silver alloy target has a length of 2.3m, a width of 1.8m and a thickness of 0.014m.
3. The oversized silver alloy target and the preparation method thereof according to claim 1, wherein the preparation method of the silver alloy target comprises the following steps: (1) smelting; (2) hot forging; (3) hot rolling; (4) cold rolling; and (5) annealing.
4. The oversized silver alloy target and the preparation method thereof according to claim 3, wherein the highest temperature of the smelting chamber in the step (1) is 1100-1200 ℃; and argon is introduced to protect the metal when the metal is melted, and the vacuum degree is less than or equal to 6 multiplied by 10 -2 mmH; the temperature of the nozzle of the smelting furnace is 950-1150 ℃; the temperature of the casting chamber is 700-1000 DEG C。
5. The oversized silver alloy target and the preparation method thereof according to claim 3, wherein the heating temperature in the hot forging process in the step (2) is 600-800 ℃, and the forging ratio is 3.5-4.5.
6. The oversized silver alloy target and the preparation method thereof according to claim 3, wherein the hot rolling in the step (3) is performed for 6 times in total, the reversing rolling is performed for the first 5 times, the deformation of each pass is 25% -25% -25% -20% -3%, the total deformation is 86%, and the hot rolling heating temperature is 500-700 ℃.
7. The oversized silver alloy target and the preparation method thereof according to claim 1, wherein the alloy blank after hot rolling is subjected to cold rolling deformation, the cold rolling deformation amount is 71%, and then the reversing leveling is performed.
8. The oversized silver alloy target and the preparation method thereof according to claim 1, wherein the highest temperature during annealing is 300-400 ℃ and the heat preservation time is 1-2h.
9. The oversized silver alloy target and the preparation method thereof according to claim 1, wherein the average grain size of the silver alloy target is 20-80 μm.
10. The oversized silver alloy target and the preparation method thereof according to any one of claims 1 to 9, wherein the oversized silver alloy target can be used for preparing a silver alloy film with good conductivity and reflectivity.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311210455.1A CN117070905A (en) | 2023-09-19 | 2023-09-19 | Oversized silver alloy target and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311210455.1A CN117070905A (en) | 2023-09-19 | 2023-09-19 | Oversized silver alloy target and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN117070905A true CN117070905A (en) | 2023-11-17 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202311210455.1A Pending CN117070905A (en) | 2023-09-19 | 2023-09-19 | Oversized silver alloy target and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN117070905A (en) |
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2023
- 2023-09-19 CN CN202311210455.1A patent/CN117070905A/en active Pending
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