CN113564543A - Silver palladium indium target material and preparation method thereof - Google Patents
Silver palladium indium target material and preparation method thereof Download PDFInfo
- Publication number
- CN113564543A CN113564543A CN202110818657.9A CN202110818657A CN113564543A CN 113564543 A CN113564543 A CN 113564543A CN 202110818657 A CN202110818657 A CN 202110818657A CN 113564543 A CN113564543 A CN 113564543A
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- silver
- palladium
- target material
- indium
- indium target
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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
- 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
- C22C5/00—Alloys based on noble metals
- C22C5/06—Alloys based on silver
-
- 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 silver palladium indium target material and a preparation method thereof, wherein the preparation method comprises the following steps: putting silver, indium and palladium gold into the intermediate frequency furnace for smelting; casting when the raw materials are completely molten and the liquid level is a mirror surface, and cooling to obtain a cast ingot; rolling the cast ingot to obtain a semi-finished product; carrying out heat treatment on the semi-finished product; and carrying out post-treatment to obtain a finished product of the silver-palladium-indium target material. The silver-palladium-indium target material and the preparation method thereof provided by the invention have the advantages that the operation is simple, the prepared silver-palladium-indium target material has strong salt spray resistance and oxidation resistance, and the grain refinement degree of the material is high.
Description
Technical Field
The invention belongs to the technical field of targets, and particularly relates to a silver-palladium-indium target and a preparation method thereof.
Background
With the rapid development of the electronic industry, the silver-palladium material has very high use value and economic value in the field of electronic components due to the excellent performance of the silver-palladium material. However, the existing silver-palladium material has poor salt spray resistance, easy oxidation and large grain size, and influences the service life and the use effect of the target material.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provide the silver-palladium-indium target material and the preparation method thereof, the operation is simple, the prepared silver-palladium-indium target material has strong oxidation resistance and high grain refinement degree.
The invention provides the following technical scheme:
a preparation method of a silver palladium indium target material comprises the following steps:
putting silver, indium and palladium gold into the intermediate frequency furnace for smelting;
casting when the raw materials are completely molten and the liquid level is a mirror surface, and cooling to obtain a cast ingot;
rolling the cast ingot to obtain a semi-finished product;
carrying out heat treatment on the semi-finished product;
and carrying out post-treatment to obtain a finished product of the silver-palladium-indium target material.
Further, the content of the silver is more than 99.99%, and the content of the indium and the content of the palladium gold are both more than 99.95%.
Further, the feeding mass ratio of the silver, the indium and the palladium-gold is (80.5-99.4): (0.1-9.5): (0.5-10).
Further, during smelting, half of the mass of silver is added firstly, indium is added after the silver is molten, palladium and gold are rapidly added after the indium is molten, the rest silver is added after the palladium and gold are molten, graphite is adopted for stirring until the alloy is completely molten, and charcoal is added for heat preservation for 10 minutes.
Furthermore, a graphite casting mold is adopted during casting, and the graphite casting mold is preheated for 15 minutes at a constant temperature of 280 ℃ before casting.
Further, during rolling, the cast ingot is placed on a cold rolling mill platform, the opening of the roller is reduced by 3mm after the thickness of the cast ingot is reached, the rolling direction of each rolling is consistent, the rolling is reduced by 3mm-4mm each time, and 2-3mm is reserved as the processing allowance on the basis of rolling to the thickness of a finished product.
Further, during heat treatment, the semi-finished product is placed in a heating furnace, the temperature is adjusted to 400 ℃, and the heat preservation time is 1 h.
Further, the post-processing comprises: removing head and tail, milling, cleaning and drying.
Furthermore, sampling is needed to perform sample quality detection after smelting and rolling.
The silver palladium indium target material is prepared by the preparation method of the silver palladium indium target material.
Compared with the prior art, the invention has the beneficial effects that:
(1) the preparation method of the silver-palladium-indium target material provided by the invention is simple to operate and high in preparation efficiency;
(2) according to the silver-palladium-indium target material finished product prepared by the invention, the inertia and the oxidation resistance are improved due to the addition of the palladium material, the material grain refinement is improved due to the addition of the indium material, and the defects of poor salt spray resistance and oxidation resistance of the existing silver target material are overcome.
Detailed Description
The following examples are only for illustrating the technical solutions of the present invention more clearly, and the protection scope of the present invention is not limited thereby.
Example 1
A preparation method of a silver palladium indium target material comprises the following steps:
preparing materials, namely preparing silver with the content of more than 99.99 percent and indium and palladium gold with the content of more than 99.95 percent.
Smelting, starting a water circulation cooling system, finishing front operation according to the operation specification of the 70KW intermediate frequency furnace, and according to silver: indium (b): palladium-gold (94.5): 5: feeding materials according to the mass ratio of 0.5; firstly, putting half mass of silver, putting indium after the silver is molten, quickly putting palladium-gold (easy to sink because of large specific gravity of palladium) after the indium is molten, putting the rest silver after the palladium-gold is molten, stirring by adopting graphite until the alloy is completely molten, adding charcoal and preserving heat for 10 minutes.
And step three, pouring, namely pouring when the molten liquid surface of the raw material is a mirror surface, and cooling to obtain a cast ingot. And (3) adopting a graphite casting mold during casting, and preheating the graphite casting mold at a constant temperature of 280 ℃ for 15 minutes before casting. In addition, when the molten liquid surface of the raw material is a mirror surface, a vacuum rod is taken to clamp and insert the molten liquid, and the molten liquid is taken out for quality detection and analysis.
And step four, rolling the cast ingot to obtain a semi-finished product, specifically, placing the cast ingot on a cold rolling mill platform, opening a roller to the thickness of the cast ingot, then reducing by 3mm, keeping the rolling direction consistent for each rolling, reducing by 3mm-4mm for each rolling, and reserving 2-3mm as a processing allowance on the basis of rolling to the thickness of the finished product. Care is taken to prevent cracking of the material during rolling.
And fifthly, placing the semi-finished product on an inspection bench, measuring the outer diameter and the inner diameter of the semi-finished product by using a vernier caliper, measuring the length by using a tape measure, and performing the next step after the semi-finished product is detected to be qualified.
And step six, heat treatment, namely placing the qualified semi-finished product in a heating furnace (a non-oxidation annealing furnace in the embodiment), adjusting the temperature to 400 ℃, and keeping the temperature for 1 h.
And seventhly, post-treatment, including removing the head and the tail, milling, cleaning and drying. Specifically, the extruded semi-finished product is placed on a band sawing machine, one end of the semi-finished product is sawn (sawn to a position where the wall thickness looks the same as much as possible), the required size is measured by a tape measure, the other end of the semi-finished product is removed, the wall thickness of two ends of the semi-finished product is ensured to be consistent as much as possible in the operation process, and the error is within 0.5 mm; clamping the sawed target semi-finished product on a milling machine table label, finishing cutting operation according to the milling machine operation specification, and then performing milling and drilling operation on a lathe and a drilling machine; then placing the target material in a cleaning basket, and finishing the cleaning operation according to the operation instruction of the ultrasonic cleaning machine; and finally, drying by using an oven to obtain the silver palladium indium target material.
And step eight, engraving the finished product of the silver-palladium-indium target material as required, packaging, performing selective inspection, and finally warehousing and storing.
Example 2
A preparation method of a silver palladium indium target material comprises the following steps:
preparing materials, namely preparing silver with the content of more than 99.99 percent and indium and palladium gold with the content of more than 99.95 percent.
Smelting, starting a water circulation cooling system, finishing front operation according to the operation specification of the 70KW intermediate frequency furnace, and according to silver: indium (b): palladium-gold 96.5: 3: feeding materials according to the mass ratio of 0.5; firstly, putting silver with half mass, putting indium after the silver is melted, quickly putting palladium-gold after the indium is melted, putting the rest silver after the palladium-gold is melted, stirring by adopting graphite until the alloy is completely melted, adding charcoal and preserving heat for 10 minutes.
And step three, pouring, namely pouring when the molten liquid surface of the raw material is a mirror surface, and cooling to obtain a cast ingot. And (3) adopting a graphite casting mold during casting, and preheating the graphite casting mold at a constant temperature of 280 ℃ for 15 minutes before casting. In addition, when the molten liquid surface of the raw material is a mirror surface, a vacuum rod is taken to clamp and insert the molten liquid, and the molten liquid is taken out for quality detection and analysis.
And step four, rolling the cast ingot to obtain a semi-finished product, specifically, placing the cast ingot on a cold rolling mill platform, opening a roller to the thickness of the cast ingot, then reducing by 3mm, keeping the rolling direction consistent for each rolling, reducing by 3mm-4mm for each rolling, and reserving 2-3mm as a processing allowance on the basis of rolling to the thickness of the finished product. Care is taken to prevent cracking of the material during rolling.
And fifthly, placing the semi-finished product on an inspection bench, measuring the outer diameter and the inner diameter of the semi-finished product by using a vernier caliper, measuring the length by using a tape measure, and performing the next step after the semi-finished product is detected to be qualified.
And step six, heat treatment, namely placing the qualified semi-finished product in a heating furnace (a non-oxidation annealing furnace in the embodiment), adjusting the temperature to 400 ℃, and keeping the temperature for 1 h.
And seventhly, post-treatment, including removing the head and the tail, milling, cleaning and drying. Specifically, the extruded semi-finished product is placed on a band sawing machine, one end of the semi-finished product is sawn (sawn to a position where the wall thickness looks the same as much as possible), the required size is measured by a tape measure, the other end of the semi-finished product is removed, the wall thickness of two ends of the semi-finished product is ensured to be consistent as much as possible in the operation process, and the error is within 0.5 mm; clamping the sawed target semi-finished product on a milling machine table label, finishing cutting operation according to the milling machine operation specification, and then performing milling and drilling operation on a lathe and a drilling machine; then placing the target material in a cleaning basket, and finishing the cleaning operation according to the operation instruction of the ultrasonic cleaning machine; and finally, drying by using an oven to obtain the silver palladium indium target material.
And step eight, engraving the finished product of the silver-palladium-indium target material as required, packaging, performing selective inspection, and finally warehousing and storing.
Example 3
A preparation method of a silver palladium indium target material comprises the following steps:
preparing materials, namely preparing silver with the content of more than 99.99 percent and indium and palladium gold with the content of more than 99.95 percent.
Smelting, starting a water circulation cooling system, finishing front operation according to the operation specification of the 70KW intermediate frequency furnace, and according to silver: indium (b): palladium-gold is 90: 9.5: feeding materials according to the mass ratio of 0.5; firstly, putting silver with half mass, putting indium after the silver is melted, quickly putting palladium-gold after the indium is melted, putting the rest silver after the palladium-gold is melted, stirring by adopting graphite until the alloy is completely melted, adding charcoal and preserving heat for 10 minutes.
And step three, pouring, namely pouring when the molten liquid surface of the raw material is a mirror surface, and cooling to obtain a cast ingot. And (3) adopting a graphite casting mold during casting, and preheating the graphite casting mold at a constant temperature of 280 ℃ for 15 minutes before casting. In addition, when the molten liquid surface of the raw material is a mirror surface, a vacuum rod is taken to clamp and insert the molten liquid, and the molten liquid is taken out for quality detection and analysis.
And step four, rolling the cast ingot to obtain a semi-finished product, specifically, placing the cast ingot on a cold rolling mill platform, opening a roller to the thickness of the cast ingot, then reducing by 3mm, keeping the rolling direction consistent for each rolling, reducing by 3mm-4mm for each rolling, and reserving 2-3mm as a processing allowance on the basis of rolling to the thickness of the finished product. Care is taken to prevent cracking of the material during rolling.
And fifthly, placing the semi-finished product on an inspection bench, measuring the outer diameter and the inner diameter of the semi-finished product by using a vernier caliper, measuring the length by using a tape measure, and performing the next step after the semi-finished product is detected to be qualified.
And step six, heat treatment, namely placing the qualified semi-finished product in a heating furnace (a non-oxidation annealing furnace in the embodiment), adjusting the temperature to 400 ℃, and keeping the temperature for 1 h.
And seventhly, post-treatment, including removing the head and the tail, milling, cleaning and drying. Specifically, the extruded semi-finished product is placed on a band sawing machine, one end of the semi-finished product is sawn (sawn to a position where the wall thickness looks the same as much as possible), the required size is measured by a tape measure, the other end of the semi-finished product is removed, the wall thickness of two ends of the semi-finished product is ensured to be consistent as much as possible in the operation process, and the error is within 0.5 mm; clamping the sawed target semi-finished product on a milling machine table label, finishing cutting operation according to the milling machine operation specification, and then performing milling and drilling operation on a lathe and a drilling machine; then placing the target material in a cleaning basket, and finishing the cleaning operation according to the operation instruction of the ultrasonic cleaning machine; and finally, drying by using an oven to obtain the silver palladium indium target material.
And step eight, engraving the finished product of the silver-palladium-indium target material as required, packaging, performing selective inspection, and finally warehousing and storing.
The silver-palladium-indium target material prepared in the embodiment 1 to 3 is subjected to neutral salt water spraying test, the test temperature is 35 +/-2 ℃, and the spraying pressure is 0.7-1.7Kgf/cm2The amount of spray precipitation is 1-2ml/80cm2and/H, spraying for 24H (H), observing the surface topography change of the sample and judging the corrosion grade (9.9 grades represent that the corrosion area rate is less than 0.01 percent, and 9.8 grades represent that the corrosion area rate is 0.01-0.02 percent), and the results are shown in the following table 1:
TABLE 1
As can be seen from table 1, in the silver palladium indium target material prepared in examples 1 to 3, when the neutral salt water spray test is performed for 8H, the surface of the sample is unchanged, and after the neutral salt water spray test is performed for 24H, the corrosion level is above 9.8, that is, the neutral salt water spray test result is excellent (the judgment standard is QB/T3832-1999), which proves that the silver palladium indium target material prepared by the present invention has excellent salt spray resistance and oxidation resistance.
The above description is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, several modifications and variations can be made without departing from the technical principle of the present invention, and these modifications and variations should also be regarded as the protection scope of the present invention.
Claims (10)
1. The preparation method of the silver-palladium-indium target material is characterized by comprising the following steps:
putting silver, indium and palladium gold into the intermediate frequency furnace for smelting;
casting when the raw materials are completely molten and the liquid level is a mirror surface, and cooling to obtain a cast ingot;
rolling the cast ingot to obtain a semi-finished product;
carrying out heat treatment on the semi-finished product;
and carrying out post-treatment to obtain a finished product of the silver-palladium-indium target material.
2. The method for preparing the silver-palladium-indium target material according to claim 1, wherein the silver content is more than 99.99%, and the indium content and the palladium-gold content are both more than 99.95%.
3. The method for preparing the silver-palladium-indium target material according to claim 1, wherein the feeding mass ratio of the silver, the indium and the palladium-gold is (80.5-99.4): (0.1-9.5): (0.5-10).
4. The method for preparing the silver-palladium-indium target material according to claim 1, wherein during smelting, half mass of silver is added, indium is added after the silver is melted, palladium and gold are rapidly added after the indium is melted, the rest silver is added after the palladium and gold are melted, graphite is adopted for stirring until the alloy is completely melted, and charcoal is added for heat preservation for 10 minutes.
5. The method for preparing the silver-palladium-indium target material according to claim 1, wherein a graphite casting mold is adopted during casting, and the graphite casting mold is preheated at a constant temperature of 280 ℃ for 15 minutes before casting.
6. The preparation method of the silver, palladium and indium target material according to claim 1, wherein during rolling, the ingot is placed on a platform of a cold rolling mill, the opening of a roller is reduced by 3mm after the ingot is rolled to the thickness, the rolling direction of each rolling is consistent, the rolling direction of each rolling is reduced by 3mm-4mm, and 2-3mm is reserved as the processing allowance on the basis of rolling to the thickness of a finished product.
7. The method for preparing the silver-palladium-indium target material according to claim 1, wherein during the heat treatment, the semi-finished product is placed in a heating furnace, the temperature is adjusted to 400 ℃, and the heat preservation time is 1 h.
8. The method for preparing the silver-palladium-indium target material according to claim 1, wherein the post-treatment comprises: removing head and tail, milling, cleaning and drying.
9. The method for preparing the silver-palladium-indium target material according to claim 1, wherein sampling is required for sample quality detection after melting and rolling.
10. The silver-palladium-indium target material is characterized by being prepared by the preparation method of the silver-palladium-indium target material according to any one of claims 1 to 9.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202110818657.9A CN113564543A (en) | 2021-07-20 | 2021-07-20 | Silver palladium indium target material and preparation method thereof |
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| CN202110818657.9A CN113564543A (en) | 2021-07-20 | 2021-07-20 | Silver palladium indium target material and preparation method thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115415534A (en) * | 2022-09-30 | 2022-12-02 | 先导薄膜材料（广东）有限公司 | Silver palladium indium target material and preparation method thereof |
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| JP2004002929A (en) * | 2001-08-03 | 2004-01-08 | Furuya Kinzoku:Kk | Silver alloy, sputtering target, reflector for reflection lcd, reflection wiring electrode, thin film, manufacturing method therefor, optical recording medium, electro magnetic wave shield, metal material for electronic part, wiring material, electronic part, electronic appliance, processing method of metal film, electron optical part, laminate, and glass of building material |
| US20040055882A1 (en) * | 2001-03-16 | 2004-03-25 | Koichi Hasegawa | Sputtering target material |
| WO2012140928A1 (en) * | 2011-04-15 | 2012-10-18 | 三井金属鉱業株式会社 | Sputtering target for solar cell |
| WO2017195929A1 (en) * | 2016-05-12 | 2017-11-16 | 희성금속 주식회사 | Silver alloy composition for forming conductive film, and preparation method therefor |
| CN112746173A (en) * | 2020-12-29 | 2021-05-04 | 广东先导稀材股份有限公司 | Method for purifying and regenerating silver palladium from silver palladium indium target material waste |
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2021
- 2021-07-20 CN CN202110818657.9A patent/CN113564543A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20040055882A1 (en) * | 2001-03-16 | 2004-03-25 | Koichi Hasegawa | Sputtering target material |
| JP2004002929A (en) * | 2001-08-03 | 2004-01-08 | Furuya Kinzoku:Kk | Silver alloy, sputtering target, reflector for reflection lcd, reflection wiring electrode, thin film, manufacturing method therefor, optical recording medium, electro magnetic wave shield, metal material for electronic part, wiring material, electronic part, electronic appliance, processing method of metal film, electron optical part, laminate, and glass of building material |
| WO2012140928A1 (en) * | 2011-04-15 | 2012-10-18 | 三井金属鉱業株式会社 | Sputtering target for solar cell |
| WO2017195929A1 (en) * | 2016-05-12 | 2017-11-16 | 희성금속 주식회사 | Silver alloy composition for forming conductive film, and preparation method therefor |
| CN112746173A (en) * | 2020-12-29 | 2021-05-04 | 广东先导稀材股份有限公司 | Method for purifying and regenerating silver palladium from silver palladium indium target material waste |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115415534A (en) * | 2022-09-30 | 2022-12-02 | 先导薄膜材料（广东）有限公司 | Silver palladium indium target material and preparation method thereof |
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