CN105063664A - Additive for producing electrolytic copper powder of uniform particle diameter - Google Patents

Additive for producing electrolytic copper powder of uniform particle diameter Download PDF

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Publication number
CN105063664A
CN105063664A CN201510443349.7A CN201510443349A CN105063664A CN 105063664 A CN105063664 A CN 105063664A CN 201510443349 A CN201510443349 A CN 201510443349A CN 105063664 A CN105063664 A CN 105063664A
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China
Prior art keywords
copper powder
additive
electrolytic copper
concentration
particle diameter
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CN201510443349.7A
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Chinese (zh)
Inventor
胡旭日
徐策
王海振
赵东
王天堂
孙云飞
朱琪琪
谢锋
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SHANDONG JINBAO ELECTRONIC CO Ltd
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SHANDONG JINBAO ELECTRONIC CO Ltd
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Priority to CN201510443349.7A priority Critical patent/CN105063664A/en
Publication of CN105063664A publication Critical patent/CN105063664A/en
Pending legal-status Critical Current

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Abstract

The invention relates to an additive for producing electrolytic copper powder of a uniform particle diameter. The additive comprises the following components of polyethylene (PE), polyvinyl pyrrolidone (PVP), cetyl trimethyl ammonium bromide (CTAB), multi-alkyl sulfonate, citrate, phosphite and pyrophosphate. According to the additive, the components are simple, raw materials are easy to obtain, and control can be performed easily during actual production; the obtained electrolytic copper powder is regular in shape and uniform in particle diameter, and the particle diameter ranges from 6 <mu>m to 15 <mu>m; the mobility is good, the current efficiency can reach 90%, and the copper powder purity reaches up to 99.7%.

Description

A kind of additive for the production of uniform particle size electrolytic copper powder
Technical field
The present invention relates to a kind of additive, particularly relate to a kind of additive for the production of uniform particle size electrolytic copper powder, belong to electrolytic copper powder processing technique field.
Background technology
Copper powder is one of basic raw material of powder metallurgy industry, is widely used in the industries such as friction materials, oil bearing, electrical contact material, electro-conductive material, and plays an important role in fields such as automobile, household electrical appliances, electronics, communications.The preparation method of copper powder mainly contains electrolytic process, atomization, oxidation reduction process etc.
Wherein, the general production process of electrolytic copper powder is: molten copper liquid making, and---------cleaning---dries---reduction---screening to electrolytic copper powder to scrape powder.Usually, the copper powder that electrolytic process obtains is generally dendroid, not of uniform size and to each other cross winding mobility is reduced, add post-processing difficulty.
Summary of the invention
The present invention is directed to the deficiency that above-mentioned prior art exists, a kind of additive for the production of uniform particle size electrolytic copper powder is provided.
The technical scheme that the present invention solves the problems of the technologies described above is as follows: a kind of additive for the production of uniform particle size electrolytic copper powder, containing following component in often liter of electrolytic solution:
Wherein, Cu in described electrolytic solution 2+concentration is 10-15g/L, H 2sO 4concentration is 100-130g/L, and liquid temperature is 25-35 DEG C.
By above-mentioned additive application in the method for producing electrolytic copper powder, step is as follows: at Cu 2+10-15g/L, H 2sO 4110-130g/L, electrolytic current density 1500-2500A/m 2, temperature 25-35 DEG C solution in, add additive of the present invention by said components content, use stainless steel plate to make negative electrode, electrolytic copper plate makes anode, galvanic deposit, once peels off every 60min and scrapes powder, by obtained copper powder through cleaning, oven dry, reduction and screening process.
The invention has the beneficial effects as follows: binder component of the present invention is simple, and raw material is easy to get, and easily controls in actual production, gained electrolytic copper powder regular shape, uniform particle sizes, particle size range is 6-15 μm, good fluidity, current efficiency can reach 90%, copper powder high purity 99.7%.
On the basis of technique scheme, the present invention can also do following improvement.
Preferably, the described additive for the production of uniform particle size electrolytic copper powder, containing following component in often liter of electrolytic solution:
Further, described many alkylsulfonates are the many alkylsulfonates of solubility, are preferably many alkyl sodium sulfonates or many alkylsulphonic acids potassium.
Further, described Citrate trianion is soluble citrate, is preferably Trisodium Citrate or Tripotassium Citrate.
Further, described phosphite is solubility phosphite, is preferably sodium phosphite or potassium phosphite.
Further, described pyrophosphate salt is soluble pyrophosphate, is preferably trisodium phosphate or potassium pyrophosphate.
Accompanying drawing explanation
Fig. 1 is the copper powder metallograph that the embodiment of the present invention 1 obtains.
Embodiment
Be described principle of the present invention and feature below in conjunction with example, example, only for explaining the present invention, is not intended to limit scope of the present invention.
Embodiment 1
At Cu 2+10g/L, H 2sO 4110g/L, electrolytic current density 1500A/m 2, temperature 25 ± 2 DEG C solution in, add polythene PE, Polyvinylpyrolidone (PVP) PVP, many alkylsulphonic acids potassium, Tripotassium Citrate, potassium phosphite and potassium pyrophosphate as additive, control that the concentration of polythene PE is 20mg/L, the concentration of Polyvinylpyrolidone (PVP) PVP is 10mg/L, the concentration of many alkylsulphonic acids potassium is 90mg/L, the concentration of Tripotassium Citrate is 50mg/L, the concentration of potassium phosphite is 50mg/L, the concentration of potassium pyrophosphate is 20mg/L.
Use stainless steel plate to make negative electrode, electrolytic copper plate makes anode, galvanic deposit, once peel off every 60min and scrape powder, by obtained copper powder through cleaning, drying, reduce and screening process, Fig. 1 is the copper powder metallograph that the present embodiment obtains, and its properties data are in table 1.
Embodiment 2
At Cu 2+12g/L, H 2sO 4120g/L, electrolytic current density 2000A/m 2, temperature 30 ± 2 DEG C solution in, add polythene PE, Polyvinylpyrolidone (PVP) PVP, cetyl trimethylammonium bromide CTAB, many alkyl sodium sulfonates, sodium phosphite and trisodium phosphate as additive, control that the concentration of polythene PE is 30mg/L, the concentration of Polyvinylpyrolidone (PVP) PVP is 20mg/L, the concentration of cetyl trimethylammonium bromide CTAB is 8mg/L, the concentration of many alkyl sodium sulfonates is 100mg/L, the concentration of sodium phosphite is 10mg/L, the concentration of trisodium phosphate is 30mg/L.
Use stainless steel plate to make negative electrode, electrolytic copper plate makes anode, galvanic deposit, once peels off scrape powder every 60min, and by obtained copper powder through cleaning, oven dry, reduction and screening process, its properties data are in table 1.
Embodiment 3
At Cu 2+15g/L, H 2sO 4130g/L, electrolytic current density 2500A/m 2, temperature 35 ± 2 DEG C solution in, add polythene PE, Polyvinylpyrolidone (PVP) PVP, cetyl trimethylammonium bromide CTAB, many alkyl sodium sulfonates, Trisodium Citrate and trisodium phosphate as additive, control that the concentration of polythene PE is 10mg/L, the concentration of Polyvinylpyrolidone (PVP) PVP is 30mg/L, the concentration of cetyl trimethylammonium bromide CTAB is 15mg/L, the concentration of many alkyl sodium sulfonates is 70mg/L, the concentration of Trisodium Citrate is 25mg/L, the concentration of trisodium phosphate is 40mg/L.
Use stainless steel plate to make negative electrode, electrolytic copper plate makes anode, galvanic deposit, once peels off scrape powder every 60min, and by obtained copper powder through cleaning, oven dry, reduction and screening process, its properties data are in table 1.
Embodiment 4
At Cu 2+10g/L, H 2sO 4130g/L, electrolytic current density 2000A/m 2, temperature 28 ± 2 DEG C solution in, add Polyvinylpyrolidone (PVP) PVP, cetyl trimethylammonium bromide CTAB, many alkyl sodium sulfonates, Trisodium Citrate, sodium phosphite and trisodium phosphate as additive, the concentration controlling Polyvinylpyrolidone (PVP) PVP is 40mg/L, the concentration of cetyl trimethylammonium bromide CTAB is 20mg/L, the concentration of many alkyl sodium sulfonates is 50mg/L, the concentration of Trisodium Citrate is 10mg/L, the concentration of sodium phosphite is 20mg/L, the concentration of trisodium phosphate is 50mg/L.
Use stainless steel plate to make negative electrode, electrolytic copper plate makes anode, galvanic deposit, once peels off scrape powder every 60min, and by obtained copper powder through cleaning, oven dry, reduction and screening process, its properties data are in table 1.
Comparative example
At Cu 2+10g/L, H 2sO 4110g/L, electrolytic current density 1500A/m 2, temperature 25 ± 2 DEG C solution in, use stainless steel plate make negative electrode, electrolytic copper plate makes anode, galvanic deposit, once peels off scrape powder every 60min, by obtained copper powder through cleaning, dry, reduction and screening process, its properties data are in table 1.
The copper powder detection perform data contrast of table 1 embodiment 1-4 and comparative example
As can be seen from Table 1, add additive of the present invention in the electrolytic solution, can effectively suppress copper powder to be dendritic growth, change the better bar-shaped growth of mobility into; Comparatively comparative example is more regular for the electrolytic copper powder shape obtained, and copper powder size is little and evenly, good fluidity, significantly can reduce post-processing difficulty.
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, within the spirit and principles in the present invention all, any amendment done, equivalent replacement, improvement etc., all should be included within protection scope of the present invention.

Claims (6)

1. for the production of an additive for uniform particle size electrolytic copper powder, it is characterized in that, containing following component in often liter of electrolytic solution:
Wherein, Cu in described electrolytic solution 2+concentration is 10-15g/L, H 2sO 4concentration is 100-130g/L, and liquid temperature is 25-35 DEG C.
2. additive according to claim 1, is characterized in that, containing following component in often liter of electrolytic solution:
3. additive according to claim 1 and 2, is characterized in that, described many alkylsulfonates are the many alkylsulfonates of solubility.
4. additive according to claim 1 and 2, is characterized in that, described Citrate trianion is soluble citrate.
5. additive according to claim 1 and 2, is characterized in that, described phosphite is solubility phosphite.
6. additive according to claim 1 and 2, is characterized in that, described pyrophosphate salt is soluble pyrophosphate.
CN201510443349.7A 2015-07-24 2015-07-24 Additive for producing electrolytic copper powder of uniform particle diameter Pending CN105063664A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106987869A (en) * 2017-04-06 2017-07-28 山东金宝电子股份有限公司 The method for being electrolysed the additive package of alkaline etching waste liquid for producing and copper powder being prepared with it
CN107059065A (en) * 2017-04-06 2017-08-18 山东金宝电子股份有限公司 The additive package of electrolytic acid etching waste liquor and the method that copper powder is prepared with it
CN110938846A (en) * 2018-09-21 2020-03-31 中国科学院大连化学物理研究所 CO (carbon monoxide)2Electrode for electrochemical reduction, preparation and application thereof

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1686645A (en) * 2005-04-26 2005-10-26 黄德欢 Method of preparing nano-bronze powder using electric deposition
CN102978667A (en) * 2012-10-25 2013-03-20 烟台大学 Preparation method for nanometer copper powder through electro-deposition
CN103388160A (en) * 2013-07-19 2013-11-13 北京科技大学 Method for preparation of ultrafine copper powder by waste circuit board copper dissolution-electrodeposition combined method

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1686645A (en) * 2005-04-26 2005-10-26 黄德欢 Method of preparing nano-bronze powder using electric deposition
CN102978667A (en) * 2012-10-25 2013-03-20 烟台大学 Preparation method for nanometer copper powder through electro-deposition
CN103388160A (en) * 2013-07-19 2013-11-13 北京科技大学 Method for preparation of ultrafine copper powder by waste circuit board copper dissolution-electrodeposition combined method

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106987869A (en) * 2017-04-06 2017-07-28 山东金宝电子股份有限公司 The method for being electrolysed the additive package of alkaline etching waste liquid for producing and copper powder being prepared with it
CN107059065A (en) * 2017-04-06 2017-08-18 山东金宝电子股份有限公司 The additive package of electrolytic acid etching waste liquor and the method that copper powder is prepared with it
CN110938846A (en) * 2018-09-21 2020-03-31 中国科学院大连化学物理研究所 CO (carbon monoxide)2Electrode for electrochemical reduction, preparation and application thereof
CN110938846B (en) * 2018-09-21 2021-09-07 中国科学院大连化学物理研究所 CO (carbon monoxide)2Electrode for electrochemical reduction, preparation and application thereof

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