CN114959271B - Recovery method of sputtering silver residual target - Google Patents
Recovery method of sputtering silver residual target Download PDFInfo
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- CN114959271B CN114959271B CN202210537490.3A CN202210537490A CN114959271B CN 114959271 B CN114959271 B CN 114959271B CN 202210537490 A CN202210537490 A CN 202210537490A CN 114959271 B CN114959271 B CN 114959271B
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- silver
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- oxygen
- melt
- scum
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- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 title claims abstract description 57
- 229910052709 silver Inorganic materials 0.000 title claims abstract description 56
- 239000004332 silver Substances 0.000 title claims abstract description 56
- 238000004544 sputter deposition Methods 0.000 title claims abstract description 26
- 238000000034 method Methods 0.000 title claims abstract description 25
- 238000011084 recovery Methods 0.000 title claims description 16
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 35
- 239000001301 oxygen Substances 0.000 claims abstract description 35
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 35
- 238000010438 heat treatment Methods 0.000 claims abstract description 31
- 239000002994 raw material Substances 0.000 claims abstract description 18
- 238000003723 Smelting Methods 0.000 claims abstract description 14
- 239000003610 charcoal Substances 0.000 claims abstract description 13
- 238000004321 preservation Methods 0.000 claims abstract description 12
- 238000003756 stirring Methods 0.000 claims abstract description 12
- 229910021538 borax Inorganic materials 0.000 claims abstract description 10
- 239000004328 sodium tetraborate Substances 0.000 claims abstract description 10
- 235000010339 sodium tetraborate Nutrition 0.000 claims abstract description 10
- 239000007788 liquid Substances 0.000 claims abstract description 9
- 239000000463 material Substances 0.000 claims abstract description 9
- 238000004519 manufacturing process Methods 0.000 claims abstract description 8
- 238000002844 melting Methods 0.000 claims abstract description 8
- 230000008018 melting Effects 0.000 claims abstract description 8
- 238000001816 cooling Methods 0.000 claims abstract description 6
- 239000000155 melt Substances 0.000 claims description 10
- 238000002791 soaking Methods 0.000 claims 1
- 238000004064 recycling Methods 0.000 abstract description 2
- 238000002156 mixing Methods 0.000 abstract 1
- 239000012535 impurity Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 238000005266 casting Methods 0.000 description 2
- 238000000151 deposition Methods 0.000 description 2
- 230000008021 deposition Effects 0.000 description 2
- 238000005868 electrolysis reaction Methods 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 238000000465 moulding Methods 0.000 description 2
- 238000007747 plating Methods 0.000 description 2
- 229910000838 Al alloy Inorganic materials 0.000 description 1
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 1
- CSDREXVUYHZDNP-UHFFFAOYSA-N alumanylidynesilicon Chemical compound [Al].[Si] CSDREXVUYHZDNP-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 239000011651 chromium Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 229910001882 dioxygen Inorganic materials 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- 238000010309 melting process Methods 0.000 description 1
- 229910000623 nickel–chromium alloy Inorganic materials 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 238000005477 sputtering target Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 239000013077 target material Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/001—Dry processes
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B11/00—Obtaining noble metals
- C22B11/02—Obtaining noble metals by dry processes
- C22B11/021—Recovery of noble metals from waste materials
- C22B11/025—Recovery of noble metals from waste materials from manufactured products, e.g. from printed circuit boards, from photographic films, paper, or baths
-
- 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
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Metallurgy (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Organic Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Geology (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Manufacture And Refinement Of Metals (AREA)
- Physical Vapour Deposition (AREA)
Abstract
The invention discloses a method for recycling a sputtering silver residual target. Mixing and proportioning standard silver ingots and silver residual targets, putting the obtained mixed materials into an atmospheric smelting furnace for heating and melting, and introducing oxygen into the molten liquid obtained after melting; closing heating after oxygen stops flowing in, reducing oxygen flowing amount, and covering a heat preservation cover for standing; stopping introducing oxygen after standing, adding plant ash or borax into the obtained melt, stirring, and removing scum; and (3) continuously heating the obtained molten liquid after the scum is removed, immersing charcoal in the molten liquid in the heating process, adding plant ash or borax for stirring after heating and preserving heat, taking out the scum, pouring the obtained molten liquid into a mould for cooling and forming to obtain the raw material for manufacturing the sputtering silver target. The method has the advantages of short operation flow, low cost and high production efficiency, and the recovered product meets the raw material requirements for silver target production.
Description
1. Technical field:
the invention relates to a treatment method of a sputtering target, in particular to a recovery method of a sputtering silver residual target.
2. The background technology is as follows:
the sputtering silver target is mainly used in glass industry and electronic industry, and during the sputtering process, before the silver plating layer is sputtered, chromium plating, nickel-chromium alloy, silicon-aluminum alloy and other materials are firstly plated. Since reverse deposition occurs during sputtering, the front material and various substrates (glass, quartz, etc.) are deposited on the silver target, resulting in an increase in the impurity element content in the silver target.
At present, the recovery process of the sputtering silver residual target caused by deposition mainly comprises the steps of melting the sputtering silver residual target into a cast plate, putting the cast plate into an electrolytic tank for electrolysis, and adding the electrolyzed silver powder into an atmosphere smelting furnace for melting and casting ingots to prepare raw materials meeting the requirements. The process flow is long, the cost is high, the middle of the noble metal is occupied greatly, the silver loss is high in the recovery process, and meanwhile, the environment pollution caused by electrolysis and twice ingot casting is serious, so that the environment protection is not facilitated.
3. The invention comprises the following steps:
the invention aims to solve the technical problems that: aiming at the defects of the prior art in recovering the sputtering silver residual target, the invention provides the recovery method of the sputtering silver residual target, which has the advantages of short flow, low cost and high production efficiency.
In order to solve the problems, the invention adopts the following technical scheme:
the invention provides a recovery method of a sputtering silver residual target, which comprises the following steps:
a. the standard silver ingot and the silver residual target are used as raw materials for proportioning, and the weight ratio of the raw materials to the silver residual target is 1-4: 1, a step of;
b. c, putting the mixed material prepared in the step a into an atmospheric smelting furnace for heating and melting, and introducing oxygen into the molten liquid obtained after melting; closing heating after oxygen stops flowing in, reducing oxygen flowing amount, and covering a heat preservation cover for standing;
c. stopping introducing oxygen after standing, adding plant ash or borax into the obtained melt, stirring, and removing scum;
d. and c, continuously heating the solution obtained after the scum is removed, immersing charcoal in the solution in the heating process, heating to 1120-1180 ℃ for heat preservation for 3-5 min, adding plant ash or borax for stirring after heat preservation, taking out the scum, pouring the obtained solution into a mould for cooling and forming, and obtaining the raw material for manufacturing the sputtering silver target.
According to the method for recovering the sputtering silver residual target, the temperature in the heating and melting process in the step b is controlled to be 1030-1080 ℃.
According to the method for recovering the sputtering silver residual target, the oxygen gas in the step b is introduced into the reactor for 1-3 min at an amount of 2-20L/min.
According to the method for recovering the sputtering silver residual target, in the step b, the oxygen inlet amount is reduced, and the oxygen inlet amount is controlled to be 0.5-2L/min.
According to the method for recovering the sputtering silver residual target, the standing time in the step b is 2-5 min.
According to the above recovery method of the sputtered silver residual target, the weight ratio of the addition amount of the plant ash or borax to the melt in the step c is 1:300 to 500.
According to the above method for recovering a sputtered silver residual target, when the charcoal is immersed in the melt in the step d, the ratio of the surface area of the charcoal immersed in the melt to the volume of the melt is 1cm 2 ：10～30cm 3 The immersion time is 2-5 min.
According to the above recovery method of the sputtered silver residual target, the weight ratio of the addition amount of the plant ash or borax to the melt in the step d is 1: 500-1000.
The invention has the positive beneficial effects that:
1. in the method for recycling the sputtering silver residual target material, the silver material is obtained by adopting methods of oxidation impurity removal, closed deoxidization, high-temperature impurity removal and the like in the smelting process, and meets the raw material requirements required by silver target production.
2. The invention shortens the recovery process flow, reduces the operation difficulty, improves the recovery rate of silver and effectively reduces the environmental pollution in the recovery process.
Therefore, the invention has remarkable social and economic benefits.
4. Detailed description of the preferred embodiments
The present invention will be described in more detail by the following specific embodiments, but is not intended to limit the scope of the technical solution of the present invention.
Example 1:
the invention relates to a recovery method of a sputtering silver residual target, which comprises the following detailed steps:
a. the standard silver ingot and the silver residual target are used as raw materials for proportioning, and the weight ratio of the raw materials to the silver residual target is 3:1, the total weight of the obtained mixture is 30kg;
b. c, putting the mixed material prepared in the step a into an atmospheric smelting furnace, heating to 1030 ℃ for smelting, and introducing oxygen into the molten liquid obtained after smelting, wherein the oxygen introducing amount is 5L/min, and the introducing time is 2min; after stopping introducing oxygen, closing heating, reducing the oxygen introducing amount to 2L/min, and covering a heat preservation cover for standing for 2min;
c. stopping introducing oxygen after standing, adding 80g of plant ash into the obtained melt, stirring on the surface, and removing scum;
d. continuously heating the solution obtained after removing the scum in the step c to raise the temperature, immersing charcoal in the solution for 3min in the heating process, wherein the ratio of the surface area of the charcoal immersed in the solution to the volume of the solution is 1cm 2 ：10cm 3 Heating to 1120 ℃ for heat preservation for 5min, adding 50g of plant ash for stirring after heat preservation, taking out scum, pouring the obtained melt into a mould for cooling and molding to obtain the raw material for manufacturing the sputtering silver target.
The product recovered in the embodiment is detected and analyzed, the component quality accords with national standard No. 1 silver standard, and the content of each pollution element is Ni 0.015ppm, cr 0.005ppm, al 0.005ppm, si 0.035ppm and oxygen content is 8ppm.
Example 2:
the invention relates to a recovery method of a sputtering silver residual target, which comprises the following detailed steps:
a. the standard silver ingot and the silver residual target are used as raw materials for proportioning, and the weight ratio of the raw materials to the silver residual target is 2:1, the total weight of the obtained mixture is 60kg;
b. c, putting the mixed material prepared in the step a into an atmospheric smelting furnace, heating to 1080 ℃ for smelting, and introducing oxygen into the molten liquid obtained after smelting, wherein the oxygen introducing amount is 10L/min, and the introducing time is 3min; after stopping oxygen introduction, closing heating, reducing oxygen introduction amount to 1L/min, and covering a heat preservation cover for standing for 5min;
c. after standing, stopping introducing oxygen, adding 200g of plant ash into the obtained melt, stirring on the surface, and removing scum;
d. c, continuously heating the solution obtained after the scum is removed in the step c,immersing charcoal in the molten solution for 5min in the heating process, wherein the ratio of the surface area of charcoal immersed in the molten solution to the volume of molten solution is 1cm 2 ：30cm 3 Heating to 1180deg.C for 5min, adding 60g plant ash, stirring, taking out scum, pouring the obtained melt into a mold, cooling, and molding to obtain the raw material for preparing the sputtering silver target.
The product recovered in the embodiment is detected and analyzed, the component quality accords with national standard No. 1 silver standard, and the content of each pollution element is Ni 0.02ppm, cr 0.005ppm, al 0.008ppm, si 0.031ppm and oxygen content is 7ppm.
Example 3:
the invention relates to a recovery method of a sputtering silver residual target, which comprises the following detailed steps:
a. the standard silver ingot and the silver residual target are used as raw materials for proportioning, and the weight ratio of the raw materials to the silver residual target is 4:1, the total weight of the obtained mixture is 30kg;
b. c, putting the mixed material prepared in the step a into an atmospheric smelting furnace, heating to 1050 ℃ for smelting, and introducing oxygen into the molten liquid obtained after smelting, wherein the oxygen introducing amount is 20L/min, and the introducing time is 1min; after stopping oxygen introduction, closing heating, reducing oxygen introduction amount to 0.5L/min, and covering a heat preservation cover for standing for 2min;
c. stopping introducing oxygen after standing, adding 50g of plant ash into the obtained melt, stirring on the surface, and removing scum;
d. continuously heating the solution obtained after removing the scum in the step c to raise the temperature, immersing charcoal in the solution for 3min in the heating process, wherein the ratio of the surface area of the charcoal immersed in the solution to the volume of the solution is 1cm 2 ：15cm 3 Heating to 1150 deg.c for 4min, adding plant ash 30g, stirring, taking out scum, cooling to form, and final product.
The product recovered in the embodiment is detected and analyzed, the component quality accords with national standard No. 1 silver standard, and the content of each pollution element is Ni 0.022ppm, cr 0.008ppm, al 0.01ppm, si 0.042ppm and oxygen content is 9ppm.
Claims (2)
1. The recovery method of the sputtering silver residual target is characterized by comprising the following steps of:
a. the standard silver ingot and the silver residual target are used as raw materials for proportioning, and the weight ratio of the raw materials to the silver residual target is 1-4: 1, a step of;
b. c, putting the mixed material prepared in the step a into an atmospheric smelting furnace for heating and melting, wherein the temperature is controlled to be 1030-1080 ℃; introducing oxygen into the molten liquid obtained after melting, wherein the oxygen introducing amount is 2-20L/min and the oxygen introducing time is 1-3 min; after stopping the oxygen introducing, closing the heating, reducing the oxygen introducing amount, controlling the oxygen introducing amount to be 0.5-2L/min, and covering a heat preservation cover for standing;
c. stopping introducing oxygen after standing, adding plant ash or borax into the obtained melt, stirring, and removing scum;
the weight ratio of the addition amount of the plant ash or borax to the melt is 1: 300-500 parts;
d. c, continuously heating the solution obtained after the scum is removed, immersing charcoal in the solution in the heating process, heating to 1120-1180 ℃ for heat preservation for 3-5 min, adding plant ash or borax for stirring after heat preservation, taking out the scum, pouring the obtained solution into a mould for cooling and forming to obtain the raw material for manufacturing the sputtering silver target;
when the charcoal is immersed in the melt, the ratio of the surface area of the charcoal immersed in the melt to the volume of the melt is 1cm 2 ：10～30cm 3 The soaking time is 2-5 min; the weight ratio of the addition amount of the plant ash or borax to the melt is 1: 500-1000.
2. The method for recovering a sputtered silver residual target according to claim 1, wherein: and b, standing for 2-5 min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210537490.3A CN114959271B (en) | 2022-05-18 | 2022-05-18 | Recovery method of sputtering silver residual target |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210537490.3A CN114959271B (en) | 2022-05-18 | 2022-05-18 | Recovery method of sputtering silver residual target |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN114959271A CN114959271A (en) | 2022-08-30 |
| CN114959271B true CN114959271B (en) | 2024-01-23 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN202210537490.3A Active CN114959271B (en) | 2022-05-18 | 2022-05-18 | Recovery method of sputtering silver residual target |
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Citations (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4029494A (en) * | 1973-08-24 | 1977-06-14 | Outokumpu Oy | Process for smelting and recovery of a material containing noble metals |
| US4564391A (en) * | 1985-03-05 | 1986-01-14 | The United States Of America As Represented By The United States Department Of Energy | Method for the recovery of silver from silver zeolite |
| RU2082784C1 (en) * | 1993-06-15 | 1997-06-27 | Геннадий Павлович Попов | Method of primary processing mixed scrap and mixed wastes of nonferrous metals and plant for its embodiment |
| JP2007224340A (en) * | 2006-02-22 | 2007-09-06 | Sumitomo Metal Mining Co Ltd | Production method of high purity silver ingot |
| JP2010506714A (en) * | 2006-10-20 | 2010-03-04 | テラ ノヴァ | Method for treating waste containing precious metals and apparatus for carrying out the method |
| WO2010071048A1 (en) * | 2008-12-17 | 2010-06-24 | Ｔａｎａｋａホールディングス株式会社 | Method for recovering metal from target and target manufacturing method |
| CN103667768A (en) * | 2013-12-24 | 2014-03-26 | 济源豫金靶材科技有限公司 | Silver target manufacturing method |
| CN107955881A (en) * | 2017-11-17 | 2018-04-24 | 宁波创润新材料有限公司 | A kind of method of smelting for recycling sputtering target material |
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| JP2020147811A (en) * | 2019-03-14 | 2020-09-17 | Ｊｘ金属株式会社 | Precious metal recovery method |
| 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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2022
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