CN110697756A - Production process of high-purity copper oxide powder for integrated circuit - Google Patents
Production process of high-purity copper oxide powder for integrated circuit Download PDFInfo
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- CN110697756A CN110697756A CN201911026369.9A CN201911026369A CN110697756A CN 110697756 A CN110697756 A CN 110697756A CN 201911026369 A CN201911026369 A CN 201911026369A CN 110697756 A CN110697756 A CN 110697756A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G3/00—Compounds of copper
- C01G3/02—Oxides; Hydroxides
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- 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
- C25C1/12—Electrolytic production, recovery or refining of metals by electrolysis of solutions of copper
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- 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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- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Electrolytic Production Of Metals (AREA)
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
Abstract
The invention discloses a production process of high-purity copper oxide powder for integrated circuits, which comprises the following steps: (1) collecting copper wires with skins; (2) peeling the copper wire to obtain a copper wire; (3) putting the copper wire into a pressing machine for pressing to form a copper block; (4) putting the copper block formed by pressing into a cutting machine for cutting, so that the copper block is divided into a plurality of small copper sections; (5) preparing copper powder to be oxidized from the copper section by an electrolytic method; (6) conveying the copper powder to be oxidized to a copper powder oxidation device for oxidation to obtain copper oxide powder; wherein the step of preparing the copper powder by adopting an electrolytic method further comprises the following steps: a. preparing copper sulfate; b. inserting the copper section as a cathode plate and the Pb-Sn-Ca alloy as an anode plate into an electrolytic cell for electrifying and electrolysis; c. scraping copper powder from the surface of the copper section serving as the cathode, and collecting the copper powder; d. washing, saponifying and dehydrating the copper powder; e. drying and reducing copper powder; f. and sieving to obtain the copper powder to be oxidized.
Description
Technical Field
The invention relates to the field of copper powder production, in particular to a production process of high-purity copper oxide powder for a copper powder integrated circuit.
Background
Copper oxide powder is an important inorganic chemical raw material, is mainly used for integrated circuits, magnetic industries, fireworks and the like in the electronic industry, along with the development of the society, the technology of the integrated circuits in the electronic industry is continuously promoted, the demand of high-purity copper oxide powder is not continuously increased, but the existing copper oxide powder is generally prepared in an atomization mode, namely, a solution is atomized after electrolysis in copper sulfate and then directly roasted and oxidized to obtain the copper oxide powder.
Disclosure of Invention
The invention aims to provide a production process of high-purity copper oxide powder for integrated circuits, which aims to solve the problems in the background technology.
The technical scheme of the invention is realized as follows: a production process of high-purity copper oxide powder for integrated circuits comprises the following steps:
(1) collecting copper wires with skins;
(2) peeling the copper wire to obtain a copper wire;
(3) putting the copper wire into a pressing machine for pressing to form a copper block;
(4) putting the copper block formed by pressing into a cutting machine for cutting, so that the copper block is divided into a plurality of small copper sections;
(5) preparing copper powder to be oxidized from the copper section by an electrolytic method;
(6) and conveying the copper powder to be oxidized to a copper powder oxidation device for oxidation to obtain the copper oxide powder.
In the above process for producing high-purity copper oxide powder for integrated circuits, the step (5) of preparing copper powder by electrolysis further comprises:
a. preparing copper sulfate;
b. inserting the copper section as a cathode plate and the Pb-Sn-Ca alloy as an anode plate into an electrolytic cell for electrifying and electrolysis;
c. scraping copper powder from the surface of the copper section serving as the cathode, and collecting the copper powder;
d. washing, saponifying and dehydrating the copper powder;
e. drying and reducing copper powder;
f. and sieving to obtain the copper powder to be oxidized.
In the production process of the high-purity copper oxide powder for the integrated circuit, the step a comprises the steps of mixing and reacting part of copper sections with dilute sulfuric acid added with 10% of hydrogen peroxide to form copper sulfate, and placing the copper sulfate on a high-level pool of an electrolytic tank, wherein the electrolytic tank is also provided with a low-level pool.
In the production process of the high-purity copper oxide powder for the integrated circuit, in the step c, the copper powder is scraped by the powder brushing machine to be mixed with the copper sulfate, and the powder brushing time of the powder brushing machine on the negative plate is 10 seconds every cycle and is brushed once every 30 seconds.
In the production process of the high-purity copper oxide powder for the integrated circuit, the mixture of the copper powder and the copper sulfate is filtered, the residual copper powder is washed and filtered by the dilute solution after the copper sulfate is filtered, then the copper powder is washed and filtered by the purified water, the dilute solution is washed and filtered firstly, then the purified water is washed and filtered, and the process is repeated for 4-5 times.
In the production process of the high-purity copper oxide powder for the integrated circuit, the residual copper powder is washed and filtered by the dilute solution and the purified water, then saponified by the saponification solution, and finally washed and filtered by the purified water to obtain the clean copper powder.
In the above production process of the high-purity copper oxide powder for integrated circuits, in the step e, a drying and reducing furnace is used to perform drying and reducing processes at the same time, wherein the drying temperature is 450 ℃ and the reducing temperature is 410 ℃.
In the production process of the high-purity copper oxide powder for the integrated circuit, nitrogen is introduced in the drying and reducing processes, and ammonia is introduced in the reducing process.
In the above production process of high-purity copper oxide powder for integrated circuits, the temperature of the combustion chamber for oxidizing and roasting in the copper powder oxidizing device in step (6) is 550 ℃.
In the production process of the high-purity copper oxide powder for the integrated circuit, the oxidation roasting frequency of the copper powder in the step (6) is at least twice.
The invention has the beneficial effects that: the copper wire is made into a copper block, copper powder is separated out of the copper block in an electrolytic mode, the copper powder is separated from copper sulfate, clean copper powder is obtained through multiple times of washing and filtering, the copper powder is further purified before oxidation, and then oxidation is carried out through a copper powder oxidation device, so that high-purity copper oxide powder is obtained, and the copper oxide powder is suitable for being applied to integrated circuits.
Detailed Description
The claimed solution will now be described in further detail with reference to specific embodiments.
The invention relates to a production process of high-purity copper oxide powder for integrated circuits, which comprises the following steps:
(1) collecting copper wires with skins;
(2) peeling the copper wire by a copper wire peeling machine to obtain a copper wire;
(3) putting the copper wire into a pressing machine for pressing to form a copper block;
(4) putting the copper block formed by pressing into a cutting machine for cutting, so that the copper block is divided into a plurality of small copper sections;
(5) and preparing copper powder to be oxidized from the copper section by an electrolytic method: the preparation method comprises the following steps:
a. preparing copper sulfate: mixing and reacting part of the copper section with dilute sulfuric acid added with 10% of hydrogen peroxide to form copper sulfate, and placing the copper sulfate on a high-level pool of an electrolytic cell, wherein the electrolytic cell is simultaneously provided with a low-level pool, so that the flow of the copper sulfate can be increased in the electrolytic process, and the electrolytic efficiency is improved.
b. Inserting the copper section as a cathode plate and the Pb-Sn-Ca alloy as an anode plate into an electrolytic cell for electrifying and electrolysis;
c. scraping copper powder from the surface of the copper section serving as the cathode, and collecting the copper powder, wherein the copper powder can be scraped by a powder brushing machine to mix the copper powder with copper sulfate, and the powder brushing time of the powder brushing machine on the cathode plate is 10 seconds every cycle, and the powder brushing is carried out once every 30 seconds.
d. Washing, saponifying and dehydrating copper powder: and (2) filtering the mixture of the copper powder and the copper sulfate, washing and filtering the residual copper powder through a dilute solution, then washing and filtering through purified water, washing and filtering the dilute solution firstly, then washing and filtering through purified water, repeating the process for 4-5 times in a circulating manner, washing and filtering the residual copper powder through the dilute solution and the purified water, then saponifying the residual copper powder through a saponification solution, and finally washing and filtering through the purified water to obtain the clean copper powder.
e. Drying and reducing copper powder: and simultaneously carrying out drying and reducing processes by using a drying and reducing furnace, wherein the drying temperature is 450 ℃, the reducing temperature is 410 ℃, nitrogen is introduced in the drying and reducing processes, and ammonia is introduced in the reducing process.
f. And screening to obtain the copper powder to be oxidized, and using layered screening in the screening process, wherein the screen holes of each layer are different, so that the sizes of the particles separated from each layer can be similar as much as possible.
(6) Conveying the copper powder to be oxidized to a copper powder oxidizing device for oxidation to obtain copper oxide powder: the temperature of a combustion chamber for oxidizing roasting in the copper powder oxidizing device is 550 ℃, wherein the oxidizing roasting frequency of the copper powder is at least twice, so that the copper powder is oxidized more thoroughly, and the quality of the copper oxide powder is improved.
According to the invention, copper wires are made into copper blocks, copper powder is separated out from the copper blocks in an electrolytic mode, and after the copper powder is separated from copper sulfate, clean copper powder is obtained through multiple times of washing and filtering, so that the copper powder is further purified before oxidation, and then is oxidized through a copper powder oxidation device, thus obtaining high-purity copper oxide powder, and the copper oxide powder is suitable for being applied to integrated circuits.
Furthermore, it should be understood that although the present description refers to embodiments, not every embodiment may contain only a single embodiment, and such description is for clarity only, and those skilled in the art should integrate the description, and the embodiments may be combined as appropriate to form other embodiments understood by those skilled in the art.
Claims (10)
1. A production process of high-purity copper oxide powder for integrated circuits is characterized by comprising the following steps:
(1) collecting copper wires with skins;
(2) peeling the copper wire to obtain a copper wire;
(3) putting the copper wire into a pressing machine for pressing to form a copper block;
(4) putting the copper block formed by pressing into a cutting machine for cutting, so that the copper block is divided into a plurality of small copper sections;
(5) preparing copper powder to be oxidized from the copper section by an electrolytic method;
(6) and conveying the copper powder to be oxidized to a copper powder oxidation device for oxidation to obtain the copper oxide powder.
2. The process for producing high-purity copper powder for integrated circuits as claimed in claim 1, wherein the step (5) of preparing copper powder by electrolysis further comprises:
a. preparing copper sulfate;
b. inserting the copper section as a cathode plate and the Pb-Sn-Ca alloy as an anode plate into an electrolytic cell for electrifying and electrolysis;
c. scraping copper powder from the surface of the copper section serving as the cathode, and collecting the copper powder;
d. washing, saponifying and dehydrating the copper powder;
e. drying and reducing copper powder;
f. and sieving to obtain the copper powder to be oxidized.
3. The process for producing high-purity copper oxide powder for integrated circuits as claimed in claim 2, wherein the step a comprises mixing part of the copper segments with dilute sulfuric acid containing 10% hydrogen peroxide to react to form copper sulfate, and placing the copper sulfate on the upper tank of the electrolytic cell, which is also provided with the lower tank.
4. The process for producing high-purity copper oxide powder for integrated circuits as claimed in claim 2, wherein in the step c, the copper powder is scraped off by a powder brushing machine to be mixed with copper sulfate, and the powder brushing machine brushes the cathode plate for 10 seconds every 30 seconds every cycle.
5. The process for producing high-purity copper powder oxide for integrated circuits as claimed in claim 4, wherein the copper powder and copper sulfate mixture are filtered to remove copper sulfate, the remaining copper powder is washed and filtered by dilute solution, and then washed and filtered by purified water, wherein the dilute solution is washed and filtered and then purified water is washed and filtered, and the cycle is repeated 4-5 times.
6. The process for producing high-purity copper powder for integrated circuits as claimed in claim 5, wherein the residual copper powder is washed and filtered by dilute solution and purified water, then saponified by saponification solution, and finally washed and filtered by purified water to obtain clean copper powder.
7. The process for producing high-purity copper oxide powder for integrated circuits as claimed in claim 2, wherein in step e, the drying and reducing processes are simultaneously performed by using a drying and reducing furnace, wherein the drying temperature is 450 ℃ and the reducing temperature is 410 ℃.
8. The process for producing high-purity copper oxide powder for integrated circuits as claimed in claim 7, wherein nitrogen is introduced during the drying and the reduction, and ammonia is introduced during the reduction.
9. The process for producing high-purity copper powder oxide for integrated circuits as claimed in claim 1, wherein the temperature of the combustion chamber for oxidizing and baking in the copper powder oxidizing apparatus in step (6) is 550 ℃.
10. The process for producing high-purity copper oxide powder for integrated circuits as claimed in claim 9, wherein the copper powder is oxidized and roasted at least twice in the step (6).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201911026369.9A CN110697756A (en) | 2019-10-26 | 2019-10-26 | Production process of high-purity copper oxide powder for integrated circuit |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201911026369.9A CN110697756A (en) | 2019-10-26 | 2019-10-26 | Production process of high-purity copper oxide powder for integrated circuit |
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| CN110697756A true CN110697756A (en) | 2020-01-17 |
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| CN201911026369.9A Pending CN110697756A (en) | 2019-10-26 | 2019-10-26 | Production process of high-purity copper oxide powder for integrated circuit |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111593373A (en) * | 2020-07-13 | 2020-08-28 | 重庆有研重冶新材料有限公司 | Production method of electrolytic copper powder for perforating charge |
| CN112499663A (en) * | 2020-12-21 | 2021-03-16 | 泰兴冶炼厂有限公司 | Preparation method of heavy high-purity copper oxide for magnetic material |
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| CN102531028A (en) * | 2012-01-04 | 2012-07-04 | 金川集团有限公司 | Method for preparing cupric oxide powder |
| CN202337842U (en) * | 2011-11-28 | 2012-07-18 | 重庆华浩冶炼有限公司 | Electrolytic copper powder integrated production system |
| CN103128272A (en) * | 2011-11-28 | 2013-06-05 | 重庆华浩冶炼有限公司 | Electrolytic copper-powder-processing technique |
| CN103862029A (en) * | 2012-12-18 | 2014-06-18 | 重庆华浩冶炼有限公司 | Copper powder composition and production method thereof |
| CN104724749A (en) * | 2015-03-17 | 2015-06-24 | 深圳市中冠环保科技有限公司 | Method for producing superfine copper oxide powder |
| CN106854768A (en) * | 2016-11-21 | 2017-06-16 | 西北矿冶研究院 | electrodeposition preparation method of superfine copper powder |
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2019
- 2019-10-26 CN CN201911026369.9A patent/CN110697756A/en active Pending
Patent Citations (6)
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| CN202337842U (en) * | 2011-11-28 | 2012-07-18 | 重庆华浩冶炼有限公司 | Electrolytic copper powder integrated production system |
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| CN102531028A (en) * | 2012-01-04 | 2012-07-04 | 金川集团有限公司 | Method for preparing cupric oxide powder |
| CN103862029A (en) * | 2012-12-18 | 2014-06-18 | 重庆华浩冶炼有限公司 | Copper powder composition and production method thereof |
| CN104724749A (en) * | 2015-03-17 | 2015-06-24 | 深圳市中冠环保科技有限公司 | Method for producing superfine copper oxide powder |
| CN106854768A (en) * | 2016-11-21 | 2017-06-16 | 西北矿冶研究院 | electrodeposition preparation method of superfine copper powder |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111593373A (en) * | 2020-07-13 | 2020-08-28 | 重庆有研重冶新材料有限公司 | Production method of electrolytic copper powder for perforating charge |
| CN111593373B (en) * | 2020-07-13 | 2022-06-17 | 重庆有研重冶新材料有限公司 | Production method of electrolytic copper powder for perforating charge |
| CN112499663A (en) * | 2020-12-21 | 2021-03-16 | 泰兴冶炼厂有限公司 | Preparation method of heavy high-purity copper oxide for magnetic material |
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Application publication date: 20200117 |
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