CN108677029B - Preparation method of high-purity gold regular particles for integrated circuit - Google Patents
Preparation method of high-purity gold regular particles for integrated circuit Download PDFInfo
- Publication number
- CN108677029B CN108677029B CN201810264365.3A CN201810264365A CN108677029B CN 108677029 B CN108677029 B CN 108677029B CN 201810264365 A CN201810264365 A CN 201810264365A CN 108677029 B CN108677029 B CN 108677029B
- Authority
- CN
- China
- Prior art keywords
- gold
- purity
- evaporation
- solution
- electrolytic
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
- 239000010931 gold Substances 0.000 title claims abstract description 113
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 title claims abstract description 110
- 229910052737 gold Inorganic materials 0.000 title claims abstract description 110
- 239000002245 particle Substances 0.000 title claims abstract description 25
- 238000002360 preparation method Methods 0.000 title abstract description 7
- 238000001704 evaporation Methods 0.000 claims abstract description 34
- 230000008020 evaporation Effects 0.000 claims abstract description 34
- 239000002994 raw material Substances 0.000 claims abstract description 25
- 238000000034 method Methods 0.000 claims abstract description 23
- 239000000463 material Substances 0.000 claims abstract description 18
- 238000000746 purification Methods 0.000 claims abstract description 16
- 238000003723 Smelting Methods 0.000 claims abstract description 12
- 238000005096 rolling process Methods 0.000 claims abstract description 9
- 238000005495 investment casting Methods 0.000 claims abstract description 7
- 229910052742 iron Inorganic materials 0.000 claims abstract description 7
- 239000000126 substance Substances 0.000 claims abstract description 7
- 238000005520 cutting process Methods 0.000 claims abstract description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 18
- GEHJYWRUCIMESM-UHFFFAOYSA-L sodium sulfite Chemical compound [Na+].[Na+].[O-]S([O-])=O GEHJYWRUCIMESM-UHFFFAOYSA-L 0.000 claims description 18
- 238000010438 heat treatment Methods 0.000 claims description 15
- 239000000047 product Substances 0.000 claims description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 9
- 238000004140 cleaning Methods 0.000 claims description 9
- 238000011068 loading method Methods 0.000 claims description 9
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 6
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 6
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 6
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 6
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 6
- 239000012153 distilled water Substances 0.000 claims description 6
- 229910017604 nitric acid Inorganic materials 0.000 claims description 6
- 238000007789 sealing Methods 0.000 claims description 6
- 235000010265 sodium sulphite Nutrition 0.000 claims description 6
- 238000000465 moulding Methods 0.000 claims description 5
- 229910004042 HAuCl4 Inorganic materials 0.000 claims description 3
- 239000012141 concentrate Substances 0.000 claims description 3
- 230000001276 controlling effect Effects 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 3
- 238000007865 diluting Methods 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- 239000000706 filtrate Substances 0.000 claims description 3
- 238000001914 filtration Methods 0.000 claims description 3
- 150000002500 ions Chemical group 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 238000004806 packaging method and process Methods 0.000 claims description 3
- 230000001105 regulatory effect Effects 0.000 claims description 3
- 238000010008 shearing Methods 0.000 claims description 3
- 239000011780 sodium chloride Substances 0.000 claims description 3
- 238000007711 solidification Methods 0.000 claims description 3
- 230000008023 solidification Effects 0.000 claims description 3
- 239000010936 titanium Substances 0.000 claims description 3
- 229910052719 titanium Inorganic materials 0.000 claims description 3
- 238000005303 weighing Methods 0.000 claims description 3
- 239000012535 impurity Substances 0.000 abstract description 9
- 229910052787 antimony Inorganic materials 0.000 abstract description 4
- 229910052797 bismuth Inorganic materials 0.000 abstract description 4
- 229910052799 carbon Inorganic materials 0.000 abstract description 4
- 229910052745 lead Inorganic materials 0.000 abstract description 4
- 238000005266 casting Methods 0.000 abstract description 3
- 229910052757 nitrogen Inorganic materials 0.000 abstract description 3
- 229910052755 nonmetal Inorganic materials 0.000 abstract description 3
- 229910052760 oxygen Inorganic materials 0.000 abstract description 3
- 229910052717 sulfur Inorganic materials 0.000 abstract description 3
- 238000005491 wire drawing Methods 0.000 abstract description 3
- 229910052751 metal Inorganic materials 0.000 abstract description 2
- 239000002184 metal Substances 0.000 abstract description 2
- 238000004519 manufacturing process Methods 0.000 description 5
- 239000000956 alloy Substances 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 229910045601 alloy Inorganic materials 0.000 description 2
- 241000270465 Eumeces Species 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000003749 cleanliness Effects 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 230000008676 import Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
Images
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
- C22B11/00—Obtaining noble metals
- C22B11/04—Obtaining noble metals by wet processes
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
- B22F9/08—Making 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
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25C—PROCESSES FOR THE ELECTROLYTIC PRODUCTION, RECOVERY OR REFINING OF METALS; APPARATUS THEREFOR
- C25C1/00—Electrolytic production, recovery or refining of metals by electrolysis of solutions
- C25C1/20—Electrolytic production, recovery or refining of metals by electrolysis of solutions of noble metals
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
- B22F9/08—Making 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
- B22F2009/0804—Dispersion in or on liquid, other than with sieves
-
- 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
Landscapes
- 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 method for preparing high-purity gold evaporation regular particles for integrated circuits, and provides a novel method for preparing the high-purity gold evaporation regular particles for the integrated circuits, which is different from the traditional processes of smelting, ingot casting, rolling, wire drawing and grain cutting, wherein the process causes pollution to high-purity gold evaporation materials in the preparation process. The specific process comprises the steps of carrying out primary purification by adopting an electrolytic method, removing most of metal and nonmetal impurities in 4N gold, and then carrying out secondary purification by adopting a chemical method, wherein the purity of a high-purity gold raw material is more than 99.999%, specific impurity elements such as C, N, O, S, Fe, Pb, Sb, Bi and the like can be effectively controlled, and the high-purity gold evaporation regular particles are directly produced by controllable precision casting and direct forming. The purity of the product provided by the invention reaches more than 99.999 percent, and the content of C is lower than 1 ppm; the particle size of the product is 0.3-3mm, the error is +/-0.2 mm, the weight error is +/-0.1 g, and the cleanness reaches the grade 1 standard of the electronic industry.
Description
Technical Field
The invention relates to a method for purifying high-purity gold raw materials for integrated circuits and preparing high-purity gold regular particles, wherein the alloy materials are mainly used as electrode materials for manufacturing integrated circuit chips.
Background
High purity gold has the characteristics of low and stable contact resistance, good electrical and thermal conductivity, easy bonding, easy film formation, good adhesion to semiconductor substrates, and the like, and is an important evaporation coating material in integrated circuit devices. With the development of large-scale integrated circuits towards high speed, small size and narrow pitch, the quality of the gold evaporation material is required to be higher, the purity of gold is required to be more than 99.999%, and the geometric shape and size of the gold evaporation material are also required to meet the high-speed development of the integrated circuit industry. High purity gold evaporation materials for integrated circuits are mainly monopolized by several international companies, including zhuangyifung, honeywell, eumeces, heili, etc. Under the influence of the properties of raw materials, processing technology and the like in the preparation process of the gold evaporation material, the high-purity gold evaporation material for the integrated circuit industry cannot be prepared in batches in China at present. The high-purity gold evaporation material for the integrated circuit in China mainly depends on import and is high in price, and the development of the integrated circuit industry in China is severely restricted.
At present, the production of high-purity gold evaporation materials involves many links such as raw material preparation, smelting, ingot casting, rolling, wire drawing, grain cutting (according to customer requirements), and the control of cleanness of all links in the process of raw material purity and processing is extremely high. The high-purity gold evaporation material for the high-end integrated circuit requires that the gold purity is more than 99.999 percent, can effectively control specific impurity elements such as C, Fe, Pb, Sb, Bi and the like, ensures the cleanliness of raw materials, has no organic pollution, has low content of gas non-metal elements, has special requirements on the geometric shape and the size at the same time, and can only adapt to the high-speed development of the integrated circuit industry. The current production process flow is long, and the product is very easy to be polluted due to contact with various processing equipment, and the quality of the product is difficult to be further improved due to the limitation of the process flow.
Disclosure of Invention
The invention aims to provide a novel method for preparing high-purity gold evaporation regular particles for integrated circuits. The specific process of the method comprises the steps of carrying out primary purification by adopting an electrolytic method, removing most of metal and non-metal impurities in 4N gold, carrying out secondary purification by adopting a chemical method, wherein the purity of a high-purity gold raw material is more than 99.999 percent, and specific impurity elements such as C, N, O, S, Fe, Pb, Sb, Bi and the like can be effectively controlled, and then directly forming by controllable precision casting to produce the high-purity gold evaporation regular particles for the integrated circuit.
The purity of the high-purity gold regular particles provided by the invention reaches over 99.999 percent, and the content of C is lower than 1 ppm; the particle size of the product is 0.3-3mm, the error is +/-0.2 mm, the weight error is +/-0.1 g, and the cleanness reaches the grade 1 standard of the electronic industry.
The invention provides a novel method for preparing high-purity gold regular particles for integrated circuits by adopting electrolytic purification, chemical purification and controllable precision casting molding. The method is used for preparing regular particles with the particle size of 0.3-3mm, the purity reaches 99.999 percent, the impurity content is less than or equal to 10ppm, and the C content is less than or equal to 1 ppm. The method for preparing the high-purity gold regular particles has the advantages of high purity, low impurity content, good size consistency, high production efficiency and good cleanness, and can be used as an evaporation material for manufacturing integrated circuit chips.
The innovation points of the invention are as follows: preparing high-purity gold raw material by adopting an electrolytic purification-chemical purification technology. Effectively control specific impurity elements such as C, N, O, S, Fe, Pb, Sb, Bi and the like.
The innovation points of the invention are as follows: the controllable precision casting molding technology is adopted to prepare the high-purity gold regular particles, so that the process is shortened, the flow is short, no impurity is introduced, the cleanness is good, and the quality of the high-purity gold evaporation material is improved. Completely different from the traditional smelting, ingot casting, rolling, wire drawing and grain cutting processes, the preparation process of the high-purity gold evaporation material causes pollution.
The preparation method of the high-purity gold regular particle evaporation material comprises the following steps:
1. gold raw material: the purity of Au is more than or equal to 99.99 percent.
2. Chemical purification:
(1) rolling the raw material gold ingot into a sheet with the thickness less than or equal to 0.5mm, and shearing the sheet into gold sheets with the length and width less than or equal to 100 mm;
(2) the prepared materials are put into 5L beakers, 1-3kg of gold is filled in each beaker, hydrochloric acid is added, and then nitric acid is added. The feeding proportion is hydrochloric acid (ml): nitric acid (ml): gold (g) ═ 2: 0.5: 2;
(3) regulating the voltage of a voltage regulator to 80-120V, and heating the solution until the gold is completely dissolved;
(4) setting the voltage of a voltage regulator to 200-205V, and heating to concentrate the gold solution until the gold content is 800-1000 g/L.
(5) Adding hydrochloric acid until no yellow gas emerges from the solution;
(6) naturally cooling the solution to room temperature, and adding primary distilled water to dilute the solution until the gold content is 80-100 g/L;
(7) filtering the solution by using quantitative filter paper;
(8) sodium sulfite (g): 1.2-2.0% of gold (g): 1 adding sodium sulfite into the filtrate;
(9) heating by a heater, controlling the temperature at 80-100 ℃, and keeping for 20-25 h;
(10) after reduction, the gold is taken out to evaporation dishes, 1-4kg of gold is loaded in each evaporation dish, the evaporation dishes are covered and placed in an electric oven, the temperature is set to be 150-.
3. Electrolytic purification:
(1) the primary purification raw materials are processed into gold anode plates by a smelting and rolling processing factory, each anode plate weighs 1000-: width: 120 mm-150 mm, length: 250 mm-300 mm;
(2) preparing 3-6 liters of 1000g/L HAuCl4 solution by adopting high-purity raw materials, then adding 5-8 liters of 3000g/L NaCl solution for mixing, adding distilled water for diluting to 20-50L, and then putting into an electrolytic bath;
(3) putting 4 gold anode plates into each electrolytic cell, hanging the gold anode plates on a titanium rod by using a gold hook, connecting a gold anode with a positive electrode, connecting a cathode titanium plate with a negative electrode, and placing the electrolytic cells on which the distance between the anode and the cathode is 70 +/-5 mm;
(4) setting the temperature of the electrolytic bath to be 50-70 ℃, and cutting off the power supply after keeping for 20-24 h;
(5) taking out cathode gold, subpackaging the cathode gold into a beaker, and cleaning the beaker by using secondary ionized water until the pH value is 6.5-7.5;
(6) taking out the gold into evaporation dishes, loading 1-4kg of gold into each evaporation dish, covering and placing in an electric oven, setting the temperature at 150-.
4. Controllable precision casting molding: adopting intermediate frequency smelting equipment, assembling a high-purity alumina crucible, adding a high-purity sponge gold raw material, heating to 1100-; and (3) putting the pre-melted cast ingot into a high-purity alumina bottom leakage crucible, heating to 1250 ℃, enabling the molten gold to leak into a secondary ion water tank for solidification and forming, and taking out high-purity gold particles after smelting is finished.
5. Cleaning and packaging: cleaning AuSn 15-25% alloy particles in an ultrasonic cleaner by using acetone, drying, weighing qualified products, sealing in a plastic bag by using a sealing machine, then loading into an iron box or a plastic box, and attaching product labels for shipment.
Drawings
FIGS. 1 and 2 show regular granular products of high purity gold and high purity sponge gold for integrated circuits.
Detailed Description
Example 1 integrated circuits were prepared using a high purity phi 1mm regular granular product;
1. gold raw material: the purity of Au is more than or equal to 99.99 percent.
2. Chemical purification:
(1) rolling the raw material gold ingot into a sheet with the thickness less than or equal to 0.5mm, and shearing the sheet into gold sheets with the length and width less than or equal to 100 mm;
(2) the prepared materials are put into 5L beakers, 1-3kg of gold is filled in each beaker, hydrochloric acid is added, and then nitric acid is added. The feeding proportion is hydrochloric acid (ml): nitric acid (ml): gold (g) ═ 2: 0.5: 2;
(3) regulating the voltage of a voltage regulator to 80-120V, and heating the solution until the gold is completely dissolved;
(4) setting the voltage of a voltage regulator to 200-205V, and heating to concentrate the gold solution until the gold content is 800-1000 g/L.
(5) Adding hydrochloric acid until no yellow gas emerges from the solution;
(6) naturally cooling the solution to room temperature, and adding primary distilled water to dilute the solution until the gold content is 80-100 g/L;
(7) filtering the solution by using quantitative filter paper;
(8) sodium sulfite (g): 1.2-2.0% of gold (g): 1 adding sodium sulfite into the filtrate;
(9) heating by a heater, controlling the temperature at 80-100 ℃, and keeping for 20-25 h;
(10) after reduction, the gold is taken out to evaporation dishes, 1-4kg of gold is loaded in each evaporation dish, the evaporation dishes are covered and placed in an electric oven, the temperature is set to be 150-.
3. Electrolytic purification:
(1) the primary purification raw materials are processed into gold anode plates by a smelting and rolling processing factory, each anode plate weighs 1000-: width: 120 mm-150 mm, length: 250 mm-300 mm;
(2) preparing 3-6 liters of 1000g/L HAuCl4 solution by adopting high-purity raw materials, then adding 5-8 liters of 3000g/L NaCl solution for mixing, adding distilled water for diluting to 20-50L, and then putting into an electrolytic bath;
(3) putting 4 gold anode plates into each electrolytic cell, hanging the gold anode plates on a titanium rod by using a gold hook, connecting a gold anode with a positive electrode, connecting a cathode titanium plate with a negative electrode, and placing the electrolytic cells on which the distance between the anode and the cathode is 70 +/-5 mm;
(4) setting the temperature of the electrolytic bath to be 50-70 ℃, and cutting off the power supply after keeping for 20-24 h;
(5) taking out cathode gold, subpackaging the cathode gold into a beaker, and cleaning the beaker by using secondary ionized water until the pH value is 6.5-7.5;
(6) taking out the gold into evaporation dishes, loading 1-4kg of gold into each evaporation dish, covering and placing in an electric oven, setting the temperature at 150-.
4. Controllable precision casting molding: adopting intermediate frequency smelting equipment, assembling a high-purity alumina crucible, adding a high-purity sponge gold raw material, heating to 1100-; and (3) putting the pre-melted cast ingot into a high-purity alumina bottom leakage crucible, heating to 1250 ℃, enabling the molten gold to leak into a secondary ion water tank for solidification and forming, and taking out high-purity gold particles after smelting is finished.
5. Cleaning and packaging: cleaning AuSn 15-25% alloy particles in an ultrasonic cleaner by using acetone, drying, weighing qualified products, sealing in a plastic bag by using a sealing machine, then loading into an iron box or a plastic box, and attaching product labels for shipment. The raw materials and products are shown in figure 1.
Claims (2)
1. A method for preparing high-purity gold evaporation regular particles for integrated circuits is characterized by comprising the following process steps:
1) and gold raw material: the purity of Au is more than or equal to 99.99 percent;
2) and chemical purification:
(1) rolling the raw material gold ingot into a sheet with the thickness less than or equal to 0.5mm, and shearing the sheet into gold sheets with the length and width less than or equal to 100 mm;
(2) putting the prepared materials into 5L beakers, loading 1-3kg of gold in each beaker, adding hydrochloric acid, then adding nitric acid, and feeding the materials according to the proportion of hydrochloric acid (ml): nitric acid (ml): gold (g) ═ 2: 0.5: 2;
(3) regulating the voltage of a voltage regulator to 80-120V, and heating the solution until the gold is completely dissolved;
(4) setting the voltage of a voltage regulator to 200-205V, and heating to concentrate the gold solution to the gold content of 800-1000 g/L;
(5) adding hydrochloric acid until no yellow gas emerges from the solution;
(6) naturally cooling the solution to room temperature, and adding primary distilled water to dilute the solution until the gold content is 80-100 g/L;
(7) filtering the solution by using quantitative filter paper;
(8) sodium sulfite (g): 1.2-2.0% of gold (g): 1 adding sodium sulfite into the filtrate;
(9) heating by a heater, controlling the temperature at 80-100 ℃, and keeping for 20-25 h;
(10) after reduction, taking out the gold into evaporation dishes, loading 1-4kg of gold into each evaporation dish, covering and placing in an electric oven, setting the temperature at 150-,
3) and electrolytic purification:
(1) the primary purification raw materials are processed into gold anode plates by a smelting and rolling processing factory, each anode plate weighs 1000-: width: 120 mm-150 mm, length: 250 mm-300 mm;
(2) preparing 3-6 liters of 1000g/L HAuCl4 solution by adopting high-purity raw materials, then adding 5-8 liters of 3000g/L NaCl solution for mixing, adding distilled water for diluting to 20-50L, and then putting into an electrolytic bath;
(3) putting 4 gold anode plates into each electrolytic cell, hanging the gold anode plates on a titanium rod by using a gold hook, connecting a gold anode with a positive electrode, connecting a cathode titanium plate with a negative electrode, and placing the electrolytic cells on which the distance between the anode and the cathode is 70 +/-5 mm;
(4) setting the temperature of the electrolytic bath to be 50-70 ℃, and cutting off the power supply after keeping for 20-24 h;
(5) taking out cathode gold, subpackaging the cathode gold into a beaker, and cleaning the beaker by using secondary ionized water until the pH value is 6.5-7.5;
(6) taking out the gold into evaporation dishes, loading 1-4kg of gold into each evaporation dish, covering and placing in an electric oven, setting the temperature at 150-,
4) and controllable precision casting molding: adopting intermediate frequency smelting equipment, assembling a high-purity alumina crucible, adding a high-purity sponge gold raw material, heating to 1100-; loading the pre-melted cast ingot into a high-purity alumina bottom leakage crucible, heating to 1250 ℃, enabling molten gold to leak into a secondary ion water tank for solidification and forming, and taking out high-purity gold particles after smelting is finished;
5) and cleaning and packaging: cleaning and drying high-purity gold particles in an ultrasonic cleaner by using acetone, weighing qualified products, sealing the qualified products in a plastic bag by using a sealing machine, then loading the plastic bag into an iron box or a plastic box, and attaching product labels for delivery.
2. The method of claim 1, wherein the step of preparing high-purity gold evaporation-regular particles comprises: the raw materials used in the step 4) are prepared by the chemical-electrolytic method in the steps 2) and 3).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810264365.3A CN108677029B (en) | 2018-03-28 | 2018-03-28 | Preparation method of high-purity gold regular particles for integrated circuit |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810264365.3A CN108677029B (en) | 2018-03-28 | 2018-03-28 | Preparation method of high-purity gold regular particles for integrated circuit |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN108677029A CN108677029A (en) | 2018-10-19 |
| CN108677029B true CN108677029B (en) | 2020-07-07 |
Family
ID=63800589
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201810264365.3A Active CN108677029B (en) | 2018-03-28 | 2018-03-28 | Preparation method of high-purity gold regular particles for integrated circuit |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN108677029B (en) |
Families Citing this family (4)
| 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 |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
-
2018
- 2018-03-28 CN CN201810264365.3A patent/CN108677029B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
Non-Patent Citations (1)
| Title |
|---|
| 民转军技术;国家国防科技工业局;《中国军转民》;20130531;第77-78页 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN108677029A (en) | 2018-10-19 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN108677029B (en) | Preparation method of high-purity gold regular particles for integrated circuit | |
| CN1201036C (en) | Copper phosphide anode for electroplating | |
| CN104724758B (en) | A kind of WO3The preparation method of nanoscale twins material | |
| CN101555015A (en) | Purifying method and device for removing boron from polysilicon | |
| US9120674B2 (en) | Process for cleaning polycrystalline silicon chunks | |
| CN107974695A (en) | A kind of method of once electrolytic method production superelevation fine copper | |
| WO2017043837A1 (en) | Method for preparing silver powder using silver grains | |
| CN111850329A (en) | Production line equipment and process for preparing high-purity magnesium alloy through continuous vacuum melting | |
| CN103160854A (en) | Preparation method of high-purity copper | |
| CN101597040B (en) | Method for producing food grade phosphoric acid with refined wet phosphoric acid and product thereof | |
| CN103779309A (en) | Gold-plating gold and silver palladium alloy single-crystal bonding filament and manufacturing method thereof | |
| JPH0558048B2 (en) | ||
| CN101775650A (en) | Preparation method of solar polycrystalline silicon cast ingot and device thereof | |
| CN101580946B (en) | Method for preparing advanced tin by electrolyzing high-stibium crude-tin alloy in hydrochloric acid system | |
| CN107267774B (en) | A kind of method of lead-acid accumulator cast welding lead skim recycling | |
| JPS6247955B2 (en) | ||
| CN114293227A (en) | Processing technology of high-purity copper product for aerospace | |
| JPH05301731A (en) | Purification of quartz glass | |
| CN1222391C (en) | Smelting method for phosphorus-copper solder | |
| CN102554186A (en) | Method for preparing copper electrolysis anode plate | |
| CN102978429B (en) | Copper alloy for manufacturing frame | |
| CN107460501B (en) | A kind of preparation method of indium industry electrolysis sulfuric acid solution of indium used | |
| CN101935041A (en) | Method for extracting polysilicon through electron beams and acid washing | |
| CN112917644A (en) | Processing technology of high-corrosion-resistance crucible for gold smelting | |
| CN104022095A (en) | Gold-plated silver lanthanum calcium alloy bonding wire and manufacture method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| CP03 | Change of name, title or address |
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. Country or region after: China 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 |
|
| CP03 | Change of name, title or address |