CN108677029A - A kind of integrated circuit High Purity Gold rule particle preparation method - Google Patents

A kind of integrated circuit High Purity Gold rule particle preparation method Download PDF

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Publication number
CN108677029A
CN108677029A CN201810264365.3A CN201810264365A CN108677029A CN 108677029 A CN108677029 A CN 108677029A CN 201810264365 A CN201810264365 A CN 201810264365A CN 108677029 A CN108677029 A CN 108677029A
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gold
purity
integrated circuit
raw material
added
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CN108677029B (en
Inventor
阳岸恒
裴洪营
朱勇
张济祥
谢宏潮
张国全
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Yunnan Precious Metal New Materials Holding Group Co ltd
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Sino Platinum Metals Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B11/00Obtaining noble metals
    • C22B11/04Obtaining noble metals by wet processes
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00Making metallic powder or suspensions thereof
    • B22F9/02Making metallic powder or suspensions thereof using physical processes
    • B22F9/06Making metallic powder or suspensions thereof using physical processes starting from liquid material
    • B22F9/08Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25CPROCESSES FOR THE ELECTROLYTIC PRODUCTION, RECOVERY OR REFINING OF METALS; APPARATUS THEREFOR
    • C25C1/00Electrolytic production, recovery or refining of metals by electrolysis of solutions
    • C25C1/20Electrolytic production, recovery or refining of metals by electrolysis of solutions of noble metals
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00Making metallic powder or suspensions thereof
    • B22F9/02Making metallic powder or suspensions thereof using physical processes
    • B22F9/06Making metallic powder or suspensions thereof using physical processes starting from liquid material
    • B22F9/08Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
    • B22F2009/0804Dispersion in or on liquid, other than with sieves
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00Technologies related to metal processing
    • Y02P10/20Recycling

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Manufacturing & Machinery (AREA)
  • Mechanical Engineering (AREA)
  • Electrolytic Production Of Metals (AREA)
  • Manufacture And Refinement Of Metals (AREA)

Abstract

The invention discloses a kind of integrated circuit High Purity Gold rule particle preparation methods, it proposes to be different from traditional melting, the technique that ingot casting, rolling, wire drawing, pelletizing technique pollute high-purity gold evaporation material strips in preparation process, completely newly prepares the new method of the high-purity gold evaporation rule particle of integrated circuit.Concrete technology is to carry out primary purification using electrolysis, removes most of metal and nonmetallic inclusion in 4N gold, secondary purification is carried out by chemical method again, High Purity Gold material purity is more than 99.999% or more, and can effectively control specific impurities Elements C, N, O, S, Fe, Pb, Sb, Bi etc. cast straight forming by controllable accurate and produce high-purity gold evaporation rule particle.Product purity proposed by the present invention reaches 99.999% or more, and C content is less than 1ppm;0.3 3mm of product cut size, error ± 0.2mm, weight error ± 0.1g, spatter property reach 1 grade of standard of electronics industry.

Description

A kind of integrated circuit High Purity Gold rule particle preparation method
Technical field
The present invention relates to integrated circuit High Purity Gold feedstock purification and with prepare High Purity Gold rule particle method, the conjunction Golden material is mainly used as the electrode material of manufacture IC chip.
Background technology
High Purity Gold has contact resistance low and stablize, and electric conductivity and thermal conductivity are good, easily bonding, easily form film and with half The characteristics such as conductor matrix adhesion is good, are the important structural evaporation coating film materials in integrated circuit device.With extensive Integrated circuit just develops towards high speed, small size, thin space direction, puts forward higher requirements, to the quality of gold evaporation material 99.999% or more golden purity is sought, the geometry and size to gold evaporation material also have special requirement, just adapt to integrate The high speed development of circuit industry.Integrated circuit is mainly monopolized by Ji Jia international corporations with high-purity gold evaporation material, including Zhuan Xinwan Rich, Honeywell, Umicore, he Li Shi etc..The shadow of material performance, processing technology etc. during by gold evaporation material preparation It rings, China cannot still prepare integrated circuit industry with high-purity gold evaporation material in batches at present.China's integrated circuit is steamed with High Purity Gold Hair material relies primarily on import, expensive, seriously restricts the development of China's IC industry.
Currently, the production of high-purity gold evaporation material is related to raw material preparation, melting, ingot casting, rolling, wire drawing, pelletizing (according to visitor Family require) etc. all too many levels, either will for the control of links spatter property in the purity of raw material or process Ask high.High-end integrated circuit is more than 99.999% or more with high-purity gold evaporation material requirements gold purity, and can effectively control spy To determine impurity element C, Fe, Pb, Sb, Bi etc., and ensures raw material cleanliness factor, no organic pollution, gas nonmetalloid content is low, Geometry and size also have special requirement pair simultaneously, just adapt to the high speed development of integrated circuit industry.Due to working as previous existence Production. art flow is longer, contacts various process equipments, and product is highly prone to pollute, and the limitation of technological process itself determines production The quality of product is difficult to have further promotion.
Invention content
The purpose of the present invention proposes completely newly to prepare the new method of the high-purity gold evaporation rule particle of integrated circuit.This method has Body technology is to carry out primary purification using electrolysis, removes most of metal and nonmetallic inclusion in 4N gold, then pass through chemical method Secondary purification is carried out, High Purity Gold material purity is more than 99.999% or more, and can effectively control specific impurities Elements C, N, O, S, Then Fe, Pb, Sb, Bi etc. cast straight forming by controllable accurate and produce integrated circuit with high-purity gold evaporation rule particle.
High Purity Gold rule particle proposed by the present invention, product purity reach 99.999% or more, and C content is less than 1ppm;Production Product grain size 0.3-3mm, error ± 0.2mm, weight error ± 0.1g, spatter property reach 1 grade of standard of electronics industry.
The present invention proposes one kind and using electrorefining-chemical purification-controllable accurate casting and forming, prepares integrated circuit With the new method of High Purity Gold rule particle.Grain size 0.3-3mm rule particles are prepared with this method, and purity reaches 99.999%, miscellaneous Matter content≤10ppm, C content≤1ppm.This method prepares High Purity Gold rule particle, and purity is high, and impurity content is low, in the same size Property it is good, production efficiency is high, and spatter property is good, can be used as the evaporation material for manufacturing IC chip.
Innovative point of the present invention is:High Purity Gold raw material is prepared using electrorefining-chemical purification technology.It effectively controls specific Impurity element C, N, O, S, Fe, Pb, Sb, Bi etc..
Innovative point of the present invention also resides in:High Purity Gold rule particle is prepared using controllable accurate cast molding technology, is shortened Technique short route does not introduce impurity, and spatter property is good, improves the quality of high-purity gold evaporation material.Be different from completely traditional melting, Ingot casting, rolling, wire drawing, pelletizing technique pollute high-purity gold evaporation material strips in preparation process.
High Purity Gold rule particle evaporation material preparation method of the present invention is as follows:
1, golden raw material:Au purity >=99.99%.
2, chemical purification:
(1) raw material ingot is then rolled into the thin slice of thickness≤0.5mm, is cut into the gold plaque of length and width≤100mm;
(2) stock is put into 5L beakers, each beaker fills gold 1-3kg, and hydrochloric acid is added, then adds nitric acid.Rate of charge Example is hydrochloric acid (ml):Nitric acid (ml):Golden (g)=2:0.5:2;
(3) it is 80V~120V, heated solution, until gold all dissolvings to adjust pressure regulator voltage;
(4) pressure regulator voltage is set to 200~205V, heating makes gold solution be concentrated into gold content 800g/L~1000g/ L。
(5) hydrochloric acid is added, until solution is emerged without yellow gas;
(6) solution cooled to room temperature, it is 80g/L~100g/L that first water, which is added, and is diluted to gold content;
(7) quantitative filter paper filtering solution is used;
(8) sodium sulfite (g) is pressed:Golden (g)=1.2~2.0:1 sodium sulfite is added into filtrate;
(9) it is heated with heater, temperature is controlled at 80 DEG C~100 DEG C, keeps 20h~25h;
(10) after restoring, gold is taken out to evaporating dish, each evaporating dish fills gold 1-4kg, and capping is placed in electric dry oven, if Constant temperature degree 150-200 degree keeps the temperature natural cooling after 15-20h.
3, electrorefining:
(1) primary purification raw material is smelting, rolling processing factory Jinyang pole plate, every piece of anode plate weight 1000-3000g, sun Plate dimensions are:It is wide:120mm~150mm, length:250mm~300mm;
(2) it after using high pure raw material to prepare the HAuCl4 solution that 3-6 rises 1000g/L, adds 5-8 and rises 3000g/L's NaCl solution mixes, and is added after distilled water is diluted to 20-50L and is put into electrolytic cell;
(3) each electrolytic cell puts into 4 pieces of Jinyang pole plates, and Jinyang pole plate is hooked on gold in stud, gold anode connect anode, Cathode titanium plates connect cathode, are placed on electrolytic cell, and distance is 70 ± 5mm between anode and cathode;
(4) electrolyzer temperature is set as 50-70 degree, is cut off the power after keeping 20-24h;
(5) it is dispensed to beaker after taking out cathode gold, secondary ion water is used to clean to Ph values as 6.5-7.5;
(6) gold is taken out to evaporating dish, each evaporating dish fills gold 1-4kg, and capping is placed in electric dry oven, set temperature 150-200 degree keeps the temperature natural cooling after 15-20h.
4, controllable accurate casting and forming:Using intermediate frequency (IF) smelting equipment, high-purity sea is added after assembling high purity aluminium oxide crucible Continuous gold raw material is warming up to 1100-1200 degree, and gold is continuously added raw material supplement after being molten into liquid, and every batch of ingot casting feeds 2000 grams, With being taken out after stove natural cooling, using chloroazotic acid corrosion surface 10-20S, dried after being cleaned with secondary deionized water;By fritting ingot casting It is packed into high purity aluminium oxide bottom and leaks crucible, so that golden melt is leak into secondary ion sink coagulation forming after being warming up to 1250 degree, melting is complete High-purity gold particle is taken out at rear.
5, purged and packed:AuSn15-25% alloying pellets are carried out in ultrasonic cleaner to clean and dry, examine with acetone It after testing qualified weighing products, is sealed in polybag, is reloaded into can or plastic casing with sealing machine, Product labelling is sent out on note Goods.
Description of the drawings
Fig. 1 and Fig. 2 is integrated circuit High Purity Gold rule particle product and high-purity cake of gold.
Specific implementation mode
1 integrated circuit of embodiment is prepared with High Purity Gold ¢ 1mm rule particle products;
1, golden raw material:Au purity >=99.99%.
2, chemical purification:
(1) raw material ingot is then rolled into the thin slice of thickness≤0.5mm, is cut into the gold plaque of length and width≤100mm;
(2) stock is put into 5L beakers, each beaker fills gold 1-3kg, and hydrochloric acid is added, then adds nitric acid.Rate of charge Example is hydrochloric acid (ml):Nitric acid (ml):Golden (g)=2:0.5:2;
(3) it is 80V~120V, heated solution, until gold all dissolvings to adjust pressure regulator voltage;
(4) pressure regulator voltage is set to 200~205V, heating makes gold solution be concentrated into gold content 800g/L~1000g/ L。
(5) hydrochloric acid is added, until solution is emerged without yellow gas;
(6) solution cooled to room temperature, it is 80g/L~100g/L that first water, which is added, and is diluted to gold content;
(7) quantitative filter paper filtering solution is used;
(8) sodium sulfite (g) is pressed:Golden (g)=1.2~2.0:1 sodium sulfite is added into filtrate;
(9) it is heated with heater, temperature is controlled at 80 DEG C~100 DEG C, keeps 20h~25h;
(10) after restoring, gold is taken out to evaporating dish, each evaporating dish fills gold 1-4kg, and capping is placed in electric dry oven, if Constant temperature degree 150-200 degree keeps the temperature natural cooling after 15-20h.
3, electrorefining:
(1) primary purification raw material is smelting, rolling processing factory Jinyang pole plate, every piece of anode plate weight 1000-3000g, sun Plate dimensions are:It is wide:120mm~150mm, length:250mm~300mm;
(2) it after using high pure raw material to prepare the HAuCl4 solution that 3-6 rises 1000g/L, adds 5-8 and rises 3000g/L's NaCl solution mixes, and is added after distilled water is diluted to 20-50L and is put into electrolytic cell;
(3) each electrolytic cell puts into 4 pieces of Jinyang pole plates, and Jinyang pole plate is hooked on gold in stud, gold anode connect anode, Cathode titanium plates connect cathode, are placed on electrolytic cell, and distance is 70 ± 5mm between anode and cathode;
(4) electrolyzer temperature is set as 50-70 degree, is cut off the power after keeping 20-24h;
(5) it is dispensed to beaker after taking out cathode gold, secondary ion water is used to clean to Ph values as 6.5-7.5;
(6) gold is taken out to evaporating dish, each evaporating dish fills gold 1-4kg, and capping is placed in electric dry oven, set temperature 150-200 degree keeps the temperature natural cooling after 15-20h.
4, controllable accurate casting and forming:Using intermediate frequency (IF) smelting equipment, high-purity sea is added after assembling high purity aluminium oxide crucible Continuous gold raw material is warming up to 1100-1200 degree, and gold is continuously added raw material supplement after being molten into liquid, and every batch of ingot casting feeds 2000 grams, With being taken out after stove natural cooling, using chloroazotic acid corrosion surface 10-20S, dried after being cleaned with secondary deionized water;By fritting ingot casting It is packed into high purity aluminium oxide bottom and leaks crucible, so that golden melt is leak into secondary ion sink coagulation forming after being warming up to 1250 degree, melting is complete High-purity gold particle is taken out at rear.
5, purged and packed:AuSn15-25% alloying pellets are carried out in ultrasonic cleaner to clean and dry, examine with acetone It after testing qualified weighing products, is sealed in polybag, is reloaded into can or plastic casing with sealing machine, Product labelling is sent out on note Goods.Raw material and product are shown in Fig. 1.

Claims (4)

1. a kind of high-purity gold evaporation rule particle of integrated circuit, it is characterised in that:In the High Purity Gold component content, the purity of Au >=99.999%, impurity content≤10ppm, C content≤1ppm;Product cut size 0.3-3mm, error ± 0.2mm, weight error ± 0.1g, spatter property reach 1 grade of standard of electronics industry.
2. a kind of high-purity gold evaporation rule particle preparation method of integrated circuit, it is characterised in that contain following processing step:
1), golden raw material:Au purity >=99.99%;
2), chemical purification:
(1) raw material ingot is then rolled into the thin slice of thickness≤0.5mm, is cut into the gold plaque of length and width≤100mm;
(2) stock is put into 5L beakers, each beaker fills gold 1-3kg, and hydrochloric acid is added, then adds nitric acid.Ingredient proportion is Hydrochloric acid (ml):Nitric acid (ml):Golden (g)=2:0.5:2;
(3) it is 80V~120V, heated solution, until gold all dissolvings to adjust pressure regulator voltage;
(4) pressure regulator voltage is set to 200~205V, heating makes gold solution be concentrated into gold content 800g/L~1000g/L;
(5) hydrochloric acid is added, until solution is emerged without yellow gas;
(6) solution cooled to room temperature, it is 80g/L~100g/L that first water, which is added, and is diluted to gold content;
(7) quantitative filter paper filtering solution is used;
(8) sodium sulfite (g) is pressed:Golden (g)=1.2~2.0:1 sodium sulfite is added into filtrate;
(9) it is heated with heater, temperature is controlled at 80 DEG C~100 DEG C, keeps 20h~25h;
(10) after restoring, gold is taken out to evaporating dish, each evaporating dish fills gold 1-4kg, and capping is placed in electric dry oven, setting temperature 150-200 degree is spent, natural cooling after 15-20h is kept the temperature,
3), electrorefining:
(1) primary purification raw material is smelting, rolling processing factory Jinyang pole plate, every piece of anode plate weight 1000-3000g, anode plate Size is:It is wide:120mm~150mm, length:250mm~300mm;
(2) after using high pure raw material to prepare the HAuCl4 solution that 3-6 rises 1000g/L, the NaCl for adding 5-8 liters 3000g/L is molten Liquid mixes, and is added after distilled water is diluted to 20-50L and is put into electrolytic cell;
(3) each electrolytic cell puts into 4 pieces of Jinyang pole plates, and Jinyang pole plate is hooked on gold in stud, and gold anode connects anode, cathode Titanium plate connects cathode, is placed on electrolytic cell, and distance is 70 ± 5mm between anode and cathode;
(4) electrolyzer temperature is set as 50-70 degree, is cut off the power after keeping 20-24h;
(5) it is dispensed to beaker after taking out cathode gold, secondary ion water is used to clean to Ph values as 6.5-7.5;
(6) gold is taken out to evaporating dish, each evaporating dish fills gold 1-4kg, and capping is placed in electric dry oven, set temperature 150- 200 degree, natural cooling after 15-20h is kept the temperature,
4), controllable accurate casting and forming:Using intermediate frequency (IF) smelting equipment, high-purity cake of gold is added after assembling high purity aluminium oxide crucible Raw material is warming up to 1100-1200 degree, and gold is continuously added raw material supplement after being molten into liquid, and every batch of ingot casting feeds 2000 grams, with stove It takes out after natural cooling, using chloroazotic acid corrosion surface 10-20S, is dried after being cleaned with secondary deionized water;Fritting ingot casting is packed into Crucible is leaked at high purity aluminium oxide bottom, so that golden melt is leak into secondary ion sink coagulation forming after being warming up to 1250 degree, after the completion of melting Take out high-purity gold particle;
5), purged and packed:AuSn15-25% alloying pellets are carried out in ultrasonic cleaner to clean and dry, examine with acetone It after qualified weighing products, is sealed in polybag, is reloaded into can or plastic casing with sealing machine, Product labelling is sent out on note Goods.
3. the integrated circuit according to claim 2 preparation method of high-purity gold evaporation rule particle, it is characterised in that:Institute Raw material used in step (3) is stated to be prepared by step (1), (2) chemistry-electrolytic method.
4. integrated circuit described in claim 1 is applied to the evaporation material of IC chip with high-purity gold evaporation rule particle Material.
CN201810264365.3A 2018-03-28 2018-03-28 Preparation method of high-purity gold regular particles for integrated circuit Active CN108677029B (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110280780A (en) * 2019-07-28 2019-09-27 长春黄金研究院烟台贵金属材料研究所有限公司 A kind of nano gold sol preparation method based on molten gold
CN110842158A (en) * 2019-11-12 2020-02-28 珠海格力绿色再生资源有限公司 Smelting and casting method of sponge gold and application thereof
CN110863215A (en) * 2019-12-27 2020-03-06 有研亿金新材料有限公司 Method for preparing gold electrolyte by using gold electrolysis anode mud
CN115090884A (en) * 2022-06-08 2022-09-23 江西兆驰半导体有限公司 Preparation method of platinum particles

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CN101508016A (en) * 2009-03-13 2009-08-19 贵研铂业股份有限公司 New preparation method of intermediate alloy for bonding gold wire
CN104404569A (en) * 2014-11-04 2015-03-11 常州钇金环保科技有限公司 Preparation technology of high purity gold
CN104789794A (en) * 2015-04-01 2015-07-22 山东招金金银精炼有限公司 Refinement technology of high-purity gold

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CN101508016A (en) * 2009-03-13 2009-08-19 贵研铂业股份有限公司 New preparation method of intermediate alloy for bonding gold wire
CN104404569A (en) * 2014-11-04 2015-03-11 常州钇金环保科技有限公司 Preparation technology of high purity gold
CN104789794A (en) * 2015-04-01 2015-07-22 山东招金金银精炼有限公司 Refinement technology of high-purity gold

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110280780A (en) * 2019-07-28 2019-09-27 长春黄金研究院烟台贵金属材料研究所有限公司 A kind of nano gold sol preparation method based on molten gold
CN110842158A (en) * 2019-11-12 2020-02-28 珠海格力绿色再生资源有限公司 Smelting and casting method of sponge gold and application thereof
CN110863215A (en) * 2019-12-27 2020-03-06 有研亿金新材料有限公司 Method for preparing gold electrolyte by using gold electrolysis anode mud
CN115090884A (en) * 2022-06-08 2022-09-23 江西兆驰半导体有限公司 Preparation method of platinum particles

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Address after: No. 988, Keji Road, high tech Development Zone, Wuhua District, Kunming, Yunnan 650000 (Kunming Precious Metals Research Institute)

Patentee after: Yunnan Precious Metal New Materials Holding Group Co.,Ltd.

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Address before: No. 988, Keji Road, high tech Development Zone, Wuhua District, Kunming, Yunnan 650000 (Kunming Precious Metals Research Institute)

Patentee before: Sino-Platinum Metals Co.,Ltd.

Country or region before: China