CN103695976A - Treatment method for copper product before electronickelling - Google Patents

Treatment method for copper product before electronickelling Download PDF

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Publication number
CN103695976A
CN103695976A CN201310695709.3A CN201310695709A CN103695976A CN 103695976 A CN103695976 A CN 103695976A CN 201310695709 A CN201310695709 A CN 201310695709A CN 103695976 A CN103695976 A CN 103695976A
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polishing
time
electronickelling
copper products
treatment process
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CN201310695709.3A
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CN103695976B (en
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方丁玉
王秋旭
薛明峰
居文娟
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Yangzhou Hy Technology Development Co Ltd
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Yangzhou Hy Technology Development Co Ltd
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Abstract

The invention relates to a treatment method for a copper product before electronickelling. The method comprises the following steps: firstly, polishing the copper product to be electroplated for the first time, and then washing; polishing for the second time, and then washing for three times; pickling, wherein a pickling solution for pickling is sulfuric acid of which the volume fraction is 30%; finally, activating to finish treatment, wherein the activating solution for activation is sulfuric acid of which the volume fraction is 3-5%. By adopting the treatment method, only oxide and greasy dirt on the surface of the copper product can be processed, and the copper layer is not corroded, so that the integrity of the product is greatly protected; meanwhile, the electroplated appearance is good in consistence, consistent in surface color and luster, and good in uniformity after electronickelling is carried out, and the brightness is improved.

Description

Treatment process before a kind of copper products electronickelling
Technical field
The present invention relates to the treatment process before a kind of copper products electronickelling, belong to copper products electronickelling technology field.
Background technology
Fast-developing with electronic circuit, the importance of nickel plating technology obviously improves, and pre-treatment mostly in the market is directly carries out chemical corrosion (sulfuric acid and Sulfothiorine) to copper material, very easily injures copper products surface.In the composition of former chemical corrosion, contain a large amount of sulfuric acid, itself and nitric acid are strong oxidizer (oxidisability: the concentrated nitric acid > vitriol oil), with copper, vigorous oxidation all can occur reacts, main and the sulfuric acid reaction (during proportioning, sulfuric acid content is much larger than nitric acid) of copper when polishing, and reaction is violent, polishing time is short, easily causes the polishing of copper products regional area not thorough, causes jaundice or blackout during plating.
Summary of the invention
Technical problem to be solved by this invention is to provide the treatment process before a kind of copper products electronickelling, solves deficiency of the prior art, meets the simplicity of copper products electronickelling pre-treatment, guarantees the quality of copper products.
The technical scheme that the present invention solves the problems of the technologies described above is as follows: the treatment process before a kind of copper products electronickelling, comprises the following steps:
(1) copper products of preparing electronickelling is first carried out to polishing for the first time, wash subsequently; Wherein, the polishing fluid I that described polishing for the first time adopts is grouped into by the one-tenth of following volume ratio: nitric acid: sulfuric acid: hydrochloric acid: water: degreasing agent=1:12:0.05:28:2.5;
(2) copper products after polishing for the first time and washing is carried out to polishing for the second time, carry out subsequently three road washings; The polishing fluid II that wherein said polishing for the second time adopts is grouped into by the one-tenth of following volume ratio: nitric acid: polishing fluid I: water: degreasing agent=1:1:7:1;
(3) copper products after polishing for the second time and washing is carried out to pickling, the pickle solution that described pickling adopts is that volume fraction is 30% sulfuric acid;
(4) copper products after overpickling is activated again, complete processing, the activation solution that described activation adopts is that volume fraction is 3~5% sulfuric acid.
Complete after above-mentioned processing copper products can directly carry out the step of electronickelling operation.
On the basis of technique scheme, the present invention can also do following improvement.
Further, in described step (1), the temperature of polishing is for the first time room temperature, and the time is 5~10 seconds.
Further, the washing concrete operations of described step (2) Zhong San road are washed for entering successively three washing baths, and the water wherein using in three road washings is deionized water.
Further, in described step (2), the temperature of polishing is for the second time room temperature, and the time is 2~3 minutes.
Further, in described step (3), the temperature of pickling is room temperature, and the time is 4~6 seconds.
Further, in described step (4), the temperature of activation is room temperature, and the time is 1~3 minute.
Above-mentioned room temperature refers to 15~25 ℃.
Further, in described step (1) and step (2), degreasing agent is the dimethylbenzene that adds scouring agent, and the amount that wherein scouring agent adds is 0.1L/kg.
Further, the main component of described scouring agent is poly--(oxo-1,2-second dimethylene)-ɑ-nonyl phenyl-ω-hydroxyl.
Sulfuric acid content die-off (a small amount of sulfuric acid be that old polishing fluid is brought into) in polishing fluid, copper and nitric acid and sulfuric acid all become diluted acid, oxidisability reduces immediately, main aobvious acid, be responsible for removing terminal surfaces cupric oxide and oil mark, during polishing reaction temperature and, polishing time lengthens, and can eliminate thorough phenomenon of pre-treatment.
Due to existing polishing fluid reaction temperature and (substantially not contacting internal layer copper), so plate out product surface, be vaporific, can before existing polishing, add according to demand former polishing flow process (approximately 5 seconds time) together, can guarantee that the copper products brightness plating out increases.
The invention has the beneficial effects as follows: the present invention only processes copper products oxide on surface and greasy dirt, does not corrode copper layer, has protected greatly the integrity of product; carry out after electronickelling, the outward appearance of electroplating out is unanimously better simultaneously, and surface color is consistent; good uniformity, and brightness is improved.
Embodiment
Below principle of the present invention and feature are described, example, only for explaining the present invention, is not intended to limit scope of the present invention.
Embodiment 1
(1) copper products of preparing electronickelling is first at room temperature carried out to polishing for the first time 5 seconds, wash subsequently; Wherein, the polishing fluid I that described polishing for the first time adopts is grouped into by the one-tenth of following volume ratio: nitric acid: sulfuric acid: hydrochloric acid: water: degreasing agent=1:12:0.05:28:2.5.
(2) copper products after polishing for the first time and washing is at room temperature carried out to polishing for the second time 2 minutes, enter respectively subsequently in three washing baths and utilize deionized water to wash; The polishing fluid II that wherein said polishing for the second time adopts is grouped into by the one-tenth of following volume ratio: nitric acid: polishing fluid I: water: degreasing agent=1:1:7:1.
In described step (1) and step (2), degreasing agent is the dimethylbenzene that adds scouring agent, and the amount that wherein scouring agent adds is 0.1L/kg, adopts and adds 1.5L scouring agent to make in 15 kilograms of dimethylbenzene.
(3) copper products after polishing for the second time and washing is at room temperature carried out to pickling, the pickle solution that described pickling adopts is that volume fraction is 30% sulfuric acid, pickling 4 seconds.
(4) copper products after overpickling is activated again, complete processing, the activation solution that described activation adopts is that volume fraction is 3% sulfuric acid, activates 1 minute.
Copper products surface color homogeneous after activation, good uniformity, presents the original yellow of copper.
Complete after above-mentioned processing copper products can directly carry out the step of electronickelling operation.
Copper products surface color is consistent after electronickelling, good uniformity, and brightness is improved, and presents glittering silver color.
Embodiment 2
(1) copper products of preparing electronickelling is first at room temperature carried out to polishing for the first time 8 seconds, wash subsequently; Wherein, the polishing fluid I that described polishing for the first time adopts is grouped into by the one-tenth of following volume ratio: nitric acid: sulfuric acid: hydrochloric acid: water: degreasing agent=1:12:0.05:28:2.5.
(2) copper products after polishing for the first time and washing is at room temperature carried out to polishing for the second time 2.5 minutes, enter respectively subsequently in three washing baths and utilize deionized water to wash; The polishing fluid II that wherein said polishing for the second time adopts is grouped into by the one-tenth of following volume ratio: nitric acid: polishing fluid I: water: degreasing agent=1:1:7:1.
In described step (1) and step (2), degreasing agent is the dimethylbenzene that adds scouring agent, and the amount that wherein scouring agent adds is 0.1L/kg, adopts and adds 1.5L scouring agent to make in 15 kilograms of dimethylbenzene.
(3) copper products after polishing for the second time and washing is at room temperature carried out to pickling, the pickle solution that described pickling adopts is that volume fraction is 30% sulfuric acid, pickling 5 seconds.
(4) copper products after overpickling is activated again, complete processing, the activation solution that described activation adopts is that volume fraction is 5% sulfuric acid, activates 2 minutes.
Copper products surface color homogeneous after activation, good uniformity, presents the original yellow of copper.
Complete after above-mentioned processing copper products can directly carry out the step of electronickelling operation.
Copper products surface color is consistent after electronickelling, good uniformity, and brightness is improved, and presents glittering silver color.
Embodiment 3
(1) copper products of preparing electronickelling is first at room temperature carried out to polishing for the first time 10 seconds, wash subsequently; Wherein, the polishing fluid I that described polishing for the first time adopts is grouped into by the one-tenth of following volume ratio: nitric acid: sulfuric acid: hydrochloric acid: water: degreasing agent=1:12:0.05:28:2.5.
(2) copper products after polishing for the first time and washing is at room temperature carried out to polishing for the second time 3 minutes, enter respectively subsequently in three washing baths and utilize deionized water to wash; The polishing fluid II that wherein said polishing for the second time adopts is grouped into by the one-tenth of following volume ratio: nitric acid: polishing fluid I: water: degreasing agent=1:1:7:1.
In described step (1) and step (2), degreasing agent is the dimethylbenzene that adds scouring agent, and the amount that wherein scouring agent adds is 0.1L/kg, adopts and adds 1.5L scouring agent to make in 15 kilograms of dimethylbenzene.
(3) copper products after polishing for the second time and washing is at room temperature carried out to pickling, the pickle solution that described pickling adopts is that volume fraction is 30% sulfuric acid, pickling 6 seconds.
(4) copper products after overpickling is activated again, complete processing, the activation solution that described activation adopts is that volume fraction is 5% sulfuric acid, activates 3 minutes.
Copper products surface color homogeneous after activation, good uniformity, presents the original yellow of copper.
Complete after above-mentioned processing copper products can directly carry out the step of electronickelling operation.
Copper products surface color is consistent after electronickelling, good uniformity, and brightness is improved, and presents glittering silver color.
Comparative example
The mode of a large amount of sulfuric acid in employing background technology and the chemical corrosion of nitric acid, carries out electronickelling pre-treatment to copper products, and the copper products surface obtaining exists aberration, lack of homogeneity, and surface brightness is not as above-described embodiment.
After electronickelling there is aberration in copper products surface, and lack of homogeneity, has the generation of white mist, and color and luster is not glittering.
This shows; embodiments of the invention are only processed copper products oxide on surface and greasy dirt; do not corrode copper layer; protected greatly the integrity of product, carried out after electronickelling simultaneously, the outward appearance of electroplating out is unanimously better; with respect to comparative example; surface color is consistent, good uniformity, and brightness is improved.
The foregoing is only preferred embodiment of the present invention, in order to limit the present invention, within the spirit and principles in the present invention not all, any modification of doing, be equal to replacement, improvement etc., within all should being included in protection scope of the present invention.

Claims (8)

1. the treatment process before copper products electronickelling, is characterized in that, comprises the following steps:
(1) copper products of preparing electronickelling is first carried out to polishing for the first time, wash subsequently; Wherein, the polishing fluid I that described polishing for the first time adopts is comprised of the composition of following volume ratio: nitric acid: sulfuric acid: hydrochloric acid: water: degreasing agent=1:12:0.05:28:2.5;
(2) copper products after polishing for the first time and washing is carried out to polishing for the second time, carry out subsequently three road washings; The polishing fluid II that wherein said polishing for the second time adopts is comprised of the composition of following volume ratio: nitric acid: polishing fluid I: water: degreasing agent=1:1:7:1;
(3) copper products after polishing for the second time and washing is carried out to pickling, the pickle solution that described pickling adopts is that volume fraction is 30% sulfuric acid;
(4) copper products after overpickling is activated again, complete processing, the activation solution that described activation adopts is that volume fraction is 3~5% sulfuric acid.
2. the treatment process before copper products electronickelling according to claim 1, is characterized in that, in described step (1), the temperature of polishing is for the first time room temperature, and the time is 5~10 seconds.
3. the treatment process before copper products electronickelling according to claim 1, is characterized in that, the washing concrete operations of described step (2) Zhong San road are washed for entering successively three washing baths, and wherein in three roads washings, the water of use is deionized water.
4. the treatment process before copper products electronickelling according to claim 1, is characterized in that, in described step (2), the temperature of polishing is for the second time room temperature, and the time is 2~3 minutes.
5. the treatment process before copper products electronickelling according to claim 1, is characterized in that, in described step (3), the temperature of pickling is room temperature, and the time is 4~6 seconds.
6. the treatment process before copper products electronickelling according to claim 1, is characterized in that, in described step (4), the temperature of activation is room temperature, and the time is 1~3 minute.
7. according to the treatment process before copper products electronickelling described in claim 1 to 6 any one, it is characterized in that, in described step (1) and step (2), degreasing agent is the dimethylbenzene that adds scouring agent, and the amount that wherein scouring agent adds is 0.1L/kg.
8. the treatment process before copper products electronickelling according to claim 7, is characterized in that, the main component of described scouring agent is poly--(oxo-1,2-second dimethylene)-ɑ-nonyl phenyl-ω-hydroxyl.
CN201310695709.3A 2013-12-17 2013-12-17 A kind of processing method before copper products electronickelling Active CN103695976B (en)

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Cited By (12)

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Publication number Priority date Publication date Assignee Title
CN104046989A (en) * 2014-06-06 2014-09-17 扬州虹扬科技发展有限公司 Novel method for preprocessing electrotinned glue-filled product
CN104846410A (en) * 2015-06-16 2015-08-19 沈阳飞机工业(集团)有限公司 Method for electroplating nickel on brass and red copper alloy
CN105002537A (en) * 2015-07-30 2015-10-28 柳州市旭平首饰有限公司 Deoiling method adopted before silver plating of copper accessories
CN105803463A (en) * 2016-05-03 2016-07-27 扬州虹扬科技发展有限公司 Pre-treatment method of copper particles for electrosilvering
CN105908158A (en) * 2016-05-03 2016-08-31 扬州虹扬科技发展有限公司 Method for plating tin on thin copper particles
CN106245048A (en) * 2016-08-05 2016-12-21 扬州虹扬科技发展有限公司 Pyrite tube core acid washing method
CN106544479A (en) * 2016-12-26 2017-03-29 广东长盈精密技术有限公司 Plate and preparation method thereof in a kind of mobile phone
CN106702448A (en) * 2017-03-16 2017-05-24 江苏金坤科技有限公司 Pretreatment method of nickel material electrogilding
CN107119291A (en) * 2017-05-24 2017-09-01 江苏金坤科技有限公司 A kind of nickel-plating liquid and the efficient nickel plating technology based on the nickel-plating liquid
CN108728841A (en) * 2018-05-04 2018-11-02 瑞声科技(新加坡)有限公司 Roll copper darkening ring piece preparation method and calendering copper darkening ring piece
CN109267127A (en) * 2018-08-30 2019-01-25 扬州虹扬科技发展有限公司 A kind of Copper base material treatment fluid and pretreating process
CN109898114A (en) * 2019-03-25 2019-06-18 扬州虹扬科技发展有限公司 A kind of production technology of hang plating production line

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Cited By (16)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104046989A (en) * 2014-06-06 2014-09-17 扬州虹扬科技发展有限公司 Novel method for preprocessing electrotinned glue-filled product
CN104846410A (en) * 2015-06-16 2015-08-19 沈阳飞机工业(集团)有限公司 Method for electroplating nickel on brass and red copper alloy
CN105002537A (en) * 2015-07-30 2015-10-28 柳州市旭平首饰有限公司 Deoiling method adopted before silver plating of copper accessories
CN105803463B (en) * 2016-05-03 2019-01-04 扬州虹扬科技发展有限公司 A kind of preprocess method of the copper particle for electrosilvering
CN105803463A (en) * 2016-05-03 2016-07-27 扬州虹扬科技发展有限公司 Pre-treatment method of copper particles for electrosilvering
CN105908158A (en) * 2016-05-03 2016-08-31 扬州虹扬科技发展有限公司 Method for plating tin on thin copper particles
CN105908158B (en) * 2016-05-03 2019-01-25 扬州虹扬科技发展有限公司 A method of it is tin plating on thin copper particle
CN106245048A (en) * 2016-08-05 2016-12-21 扬州虹扬科技发展有限公司 Pyrite tube core acid washing method
CN106245048B (en) * 2016-08-05 2018-07-03 扬州虹扬科技发展有限公司 Brass tube core acid washing method
CN106544479A (en) * 2016-12-26 2017-03-29 广东长盈精密技术有限公司 Plate and preparation method thereof in a kind of mobile phone
CN106702448A (en) * 2017-03-16 2017-05-24 江苏金坤科技有限公司 Pretreatment method of nickel material electrogilding
CN107119291A (en) * 2017-05-24 2017-09-01 江苏金坤科技有限公司 A kind of nickel-plating liquid and the efficient nickel plating technology based on the nickel-plating liquid
CN108728841A (en) * 2018-05-04 2018-11-02 瑞声科技(新加坡)有限公司 Roll copper darkening ring piece preparation method and calendering copper darkening ring piece
CN109267127A (en) * 2018-08-30 2019-01-25 扬州虹扬科技发展有限公司 A kind of Copper base material treatment fluid and pretreating process
CN109267127B (en) * 2018-08-30 2023-09-05 扬州虹扬科技发展有限公司 Copper substrate treatment fluid and pretreatment process
CN109898114A (en) * 2019-03-25 2019-06-18 扬州虹扬科技发展有限公司 A kind of production technology of hang plating production line

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