CN101328582A - Copper plating method of wirelike material and coppered wire - Google Patents
Copper plating method of wirelike material and coppered wire Download PDFInfo
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- CN101328582A CN101328582A CNA2008100818077A CN200810081807A CN101328582A CN 101328582 A CN101328582 A CN 101328582A CN A2008100818077 A CNA2008100818077 A CN A2008100818077A CN 200810081807 A CN200810081807 A CN 200810081807A CN 101328582 A CN101328582 A CN 101328582A
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- plating bath
- filamentary material
- displacement plating
- copper
- active agent
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Abstract
The invention provides a coppering method capable of forming filamentary material with even film of excellent sealing property, namely a coating method capable spraying and displacing the coating liquid on mobile filamentary material 3, wherein the displacement coating liquid contains more than 5g of CuSO4-5H2O, more than 5g and less than 400g of H2SO4, more than 5g and less than 400g of FeSO4-7H2O, more than 5mg and less than 10g of at least one kind of nonionic surfactant.
Description
Technical field
The present invention relates to the copper electroplating method and the coppered wire of filamentary materials such as a kind of welding wire or steel bead wire.
Background technology
In the past, as industrialized copper electroplating method, there was cupric cyanide to electroplate and the copper sulfate plating.Usually therefore the high-strength steels that use in filamentary material, particularly welding wire and bolt, PC steel wire and the line pipes etc., use the cupric cyanide of adaptation and even galvanic deposit excellence to electroplate more always.
In recent years, from viewpoints such as environmental problems, strong expectation adopts the copper sulfate that does not use cyanogen compound to electroplate.But, in copper sulfate is electroplated, have following problem: when carrying out galvanic deposit usually, cause Cu
2++ Fe → Cu+Fe
2+Reaction, the displacement copper of separating out the adaptation difference descends the quality of plating.
In order to prevent separating out of this displacement copper, use the galvanized bottoming of cupric cyanide (ス ト ラ ィ Network) plating in advance.In the method, owing to use 2 kinds of plating baths, therefore very numerous and diverse, nor can eliminate the very strong cyanogen waste liquid of toxicity fully.
In patent documentation 1, put down in writing following invention: by supplying with, also often cover the filamentary material surface, carry out the high plating of adaptation thus with fresh displacement plating bath thereby remove displacement copper with the specific displacement plating bath of nozzle ejection.In addition, in this method,, the crystallite dimension of copper is diminished, can carry out the density height by making the ground contact of displacement plating bath impact, the good plating of cohesiveness.But in the method for patent documentation 1, present practical situation are to obtain the adaptation that can fully withstand the Wire Drawing of carrying out in the manufacturing of filamentary material.
In addition, the concentration of known common displacement plating bath is high more, and plating speed is fast more, and it is higher that efficient becomes.But, in replacement copper plating, because of Cu
2+Reduction rate very big, so the speed of iron stripping plating the time also increases, at Fe
2+Just become precipitation (FeSO before being removed
4, Fe
2O
3) be enclosed in the coating, when having the excessive concentration of displacement plating bath thus, the adaptation variation.
Patent documentation 1: Japanese kokai publication hei 1-136974 communique
Summary of the invention
Point in view of the above problems, problem of the present invention be to provide a kind of even plated film that can form the adaptation excellence filamentary material copper electroplating method and do not need main equipment and productivity is high and high-quality coppered wire.
In order to solve above-mentioned problem,,, wherein, contain the above CuSO of 5g in the described displacement plating bath of every 1L on the filamentary material that moves, spraying the solution and coating method of displacement plating bath according to the solution and coating method of filamentary material of the present invention
45H
2The H that O, 5g are above and 400g is following
2SO
4, 5g is above and 400g is following FeSO
47H
2At least a kind of nonionic surface active agent that O and 5mg are above, this nonionic surface active agent preferably contains the tensio-active agent that is selected from sucrose fatty ester sorbitan-fatty acid ester, polyoxyethylene sorbitan fatty acid ester, fatty acid alkyl amide, Voranol EP 2001 and the polyoxyethylene alkyl phenyl ether.
According to this method, because nonionic surface active agent reduces the surface tension of displacement plating bath, the hydrogen eutectoid (the plain eutectoid of water) or the pit that suppress the formation of obstruction homogeneous coating produce, therefore think to form fine and close coating layer and can suppress sneaking into of impurity, thereby prevent peeling off of coating layer.In addition, carrying capacity of environment reduces owing to use cyanogen compound, and is constituted and made plating simple by single operation.
In addition, in the solution and coating method of filamentary material of the present invention, the above-mentioned nonionic surface active agent in the above-mentioned displacement plating bath among every 1L and organic class cathodic corrosion inhibitor can be for below the 10g.
Above-mentioned nonionic surface active agent and organic class cathodic corrosion inhibitor, among every 1L during about 10g its effect saturated.If particularly organic class cathodic corrosion inhibitor is too much, then coating is formed reaction and produce detrimentally affect, therefore preferably do not contain the above more amount that is necessary.
In addition, in the solution and coating method of filamentary material of the present invention, above-mentioned displacement plating bath can also contain at least a kind of halide ions that 0.1mmol is above and 1mol is following.
Can think halide ions generate CuX and make coating separate out nuclear produce a lot, thereby promote the formation of the coating layer that adaptation and homogeneity are high.
In addition, in the solution and coating method of filamentary material of the present invention, above-mentioned displacement plating bath can also contain at least a kind of above organic class cathodic corrosion inhibitor of 5mg, and described organic class cathodic corrosion inhibitor has for being adsorbed on needed polar group in metallic surface and the non-polar group that prevents that corrosives from contacting with the metallic surface.
Can think organic class cathodic corrosion inhibitor, promptly adsorb the corrosion inhibitor of tunicle formation type, be adsorbed and suppress small part and separate out at the reactive behavior point, thereby integrally form evenly and the high coating layer of adaptation.
In addition, coppered wire of the present invention forms for carry out wire drawing after spraying displacement plating bath copper coating on the filamentary material that moves, and wherein, the every 1L of above-mentioned displacement plating bath contains the above CuSO of 5g
45H
2The H that O, 5g are above and 400g is following
2SO
4, 5g is above and 400g is following FeSO
47H
2At least a kind of nonionic surface active agent that O, 5mg are above, the crystallite dimension of above-mentioned copper plate is
More than and
Below, the above-mentioned copper-plated thickness after the above-mentioned wire drawing is more than the 50nm.
Constitute according to this, can provide a kind of and do not need complex apparatus, do not use cyanogen compound, low-costly have the high and high-quality coppered wire of coating layer uniformly of adaptation simultaneously.
According to the present invention, suppress separating out of impurity with nonionic surface active agent, suppress the uneven growth of coating layer with organic class cathodic corrosion inhibitor, so can on filamentary material, carry out highly dense closing property and uniform plating.
Description of drawings
Fig. 1 is the sketch chart of the plater that uses in the solution and coating method of the present invention.
Fig. 2 is the photo of N/R sample wire example in the expression coating.
Fig. 3 is the photo of another example of N/R sample wire in the expression coating.
Fig. 4 is the photo that occurs fold or fissured sample wire example in the expression coating.
Fig. 5 is the photo of the sample wire example that appearance is peeled off on a small quantity in the expression coating.
Fig. 6 is the photo of the sample wire example that appearance is much peeled off in the expression coating.
Label declaration
1. coating bath
2. rinse bath
3. line (filamentary material)
4. plating nozzle
5. Washing spray nozzle
Embodiment
Thus, with reference to accompanying drawing embodiments of the present invention are described.
Fig. 1 represents an example of the displacement plater that uses among the present invention.The displacement plater constitutes in the following manner: described displacement plater has coating bath 1 and rinse bath 2, spray the displacement plating baths at the fresh displacement plating bath of supply on the coating bath 1 inner line (filamentary material) 3 that moves and on online 3 the surface by plating nozzle 4, carry out copper facing simultaneously, in rinse bath 2 by Washing spray nozzle 5 jet washing liquid water to line 3 and the washing line 3.
The injection direction of plating nozzle 4 can be set arbitrarily in 0 ° to 180 ° scope with respect to the travel direction of line 3, and a plurality of plating nozzles 4 can be to be surrounded the shape configuration by line 3, preferably with the equal angles arranged spaced.
In addition, can fold line 3 in the coating bath 1, or make its in the shape of a spiral shape move, thereby make the plating time lengthening.
In order to make displacement plating bath impact ground collision line 3,, wish that the spraying pressure of displacement plating bath is set at 0.05kg/cm so that the crystallization of coating diminishes
2More than.
The translational speed of line 3 can be set at for example 50～500m/min, but is not limited thereto scope.
The displacement plating bath that uses in the present embodiment, every 1L contain the above CuSO of 5g
45H
2The H that O, 5g are above and 400g is following
2SO
4, 5g is above and 400g is following FeSO
47H
2At least a kind of nonionic surface active agent that O, 5mg are above.
Nonionic surface active agent can use the tensio-active agent of low minute subclass such as alkyl glycoside or polymer classes such as polyoxyethylene glycol, gelatine, gelatin and polyvinyl alcohol, can use alkylbenzene phenols tensio-active agents such as senior alcohols (nonionic) tensio-active agents such as fatty acids such as sucrose fatty ester sorbitan-fatty acid ester, polyoxyethylene sorbitan fatty acid ester, fatty acid alkyl amide (nonionic) tensio-active agent, Voranol EP 2001 and polyoxyethylene alkyl phenyl ether.They can be categorized as: glycerine, Sorbitol Powder, the ester type that polyvalent alcohols such as sucrose and lipid acid form through ester linkage, have on the raw material of hydroxyls such as higher alcohols or alkylphenol and mainly ethylene oxide (oxyethane) is carried out the ether type that load aggregation forms, the ether that the addition ethylene oxide forms on lipid acid or polyhydric alcohol fatty acid ester/ester type, and comprise the compound that the lipophilic group of fatty acid alkyl amide etc. and hydrophilic radical form through amide linkage or contain APG etc. to be other nonionic surface active agent of the compound of raw material with the carbohydrate.
In addition, the displacement plating bath of present embodiment preferably also contains at least a kind of halide ions that 0.1mmol is above and 1mol is following and at least a kind of organic class cathodic corrosion inhibitor that 5mg is above and 10g is following.
Halide ions uses for example Cl
-, Br
-And I
-In more than a kind.In order to contain these halide ionss, can in the displacement plating bath, add for example NaCl, NaBr, NaI, KCl, CaCl
2, MgCl
2, HCl or 8-hydroxyl-7-iodo-5-quinoline sulfonic acid etc.
Organic class cathodic corrosion inhibitor is a kind of corrosion inhibitor that adsorbs tunicle formation type, and it has for being adsorbed on the needed polar group in metallic surface and preventing the non-polar group that contact of corrosives to the metallic surface.Comprise in the polar group of organic class cathodic corrosion inhibitor that electricity seal precision (Electricity prints precision) big N, O, P, S etc. are original (original) at center, for example ,-NH
2,＞NH ,-N ,-OH,＞O etc.Compound with these polar groups in aqueous acid with proton (H
+) combination, form ion.
In water, have anode part and cathode portion in the corrosive metal.Cathode portion becomes electronegative state, attracts the ion (physical adsorption) that exists in acid owing to gravitation.Physical adsorption the ion of organic class cathodic corrosion inhibitor of the metal after the corrosion, suppress hydrionic reduction reaction (cathodic reaction) and make fine and close tunicle.When the alkyl R of organic class cathodic corrosion inhibitor is alkyl, favourable to suppressing corrosion.In addition, the alkyl R of organic class cathodic corrosion inhibitor can be quaternary ammonium salt, SH
-, CNS
-Deng.
Organic class cathodic corrosion inhibitor is specifically as follows vulkacit H, urea, thiocarbamide, thiourea derivative, Thiovanic acid, acrylamide etc.Can enumerate vulkacit H, urea, thiocarbamide, thiourea derivative, Thiovanic acid, acrylamide, alkylamine, hexahydroaniline, aniline, anils, cyanobenzene, aromatic aldehyde, furan derivatives, dicyanobenzenes formic acid, indoles, thymus pyrimidine, mercaptobenzoxazole and phenylbenzene o-phenanthroline etc., but be not limited to these, so long as have for being adsorbed on the needed polar group in metallic surface and preventing that organic class cathodic corrosion inhibitor of corrosives to the non-polar group that contacts of metallic surface from getting final product.
Because nonionic surface active agent reduces surface tension, therefore suppress the hydrogen eutectoid of the formation of obstruction homogeneous coating, promote the multipolarization of plating, prevent that pit from producing.Add 0.005g/L in the displacement plating bath and tell on when above, but effect is saturated during 10g/L, even it is add more volume, also nonsensical.
If halide ions is made as X
-, then form Cu
+Absorption intermediate CuX
AdThereby, promote separating out of copper.That is, on online 3 the surface, the Cu in the displacement plating bath
+At Cu
++ X
-→ CuX
AdAfter the reaction, by reduction CuX
AdBe generated as metal Cu.This centre adsorbent CuX
AdTherefore become copper and separate out the nuclear of (plating), produce the multipolarization of separating out, crystalline particle is fine and become fine and close, improves for the adaptation of the coating layer of line 3.
Do not have effect when halide ions is lower than 0.1mmol/L, effect is saturated when surpassing 1000mmol/L, owing to also can cause corrosion, therefore is preferably set to the addition that 0.1mmol/L is above and 1000mmol/L is following.
Add gelatine, gelatin, polyoxyethylene glycol, VITAMIN B4, guanine, thiocarbamide, phenol, and organic compound such as amino acid during as polymeric sorbent, in this reaction owing to suppress CuX
AdReduction, therefore can promote the multinucleation of separating out the adaptation of coating layer to be improved.
Organic class cathodic corrosion inhibitor is adsorbed at the reactive behavior point, therefore suppresses partial copper and separates out, thereby make the speed of separating out stdn and integrally form uniform coating.Organic class cathodic corrosion inhibitor is at first to the reactive behavior point place absorption that coating is separated out easily, and therefore remaining reaction becomes slightly active.Thus, the multinucleation that nonionic surface active agent is caused is whole and carry out the very even fine coating of generation equably.Its as a result adaptation increase substantially.
Organic class cathodic corrosion inhibitor adds 0.005g/L and obtains effect when above in the displacement plating bath, but effect is saturated during 10g/L.In addition, the excessive interpolation of organic class cathodic corrosion inhibitor is because the necessary coating reactive behavior point that covers abovely, be difficult to generate the coating of expectation, coating quality/adaptation descends, and formation efficiency is variation also, therefore, the addition of organic class cathodic corrosion inhibitor should be controlled at below the 10g/L.
Embodiment
In the device of Fig. 1, use and contain 70g CuSO at every 1L
45H
2O, 90g H
2SO
4, 100gFeSO
47H
2Having added the plating bath that nonionic surface active agent, halide ions and organic class cathodic corrosion inhibitor of different amounts obtain in the displacement plating bath of O, is the enterprising line replacement copper facing experiment of line of 2.3mm or 2.6mm at diameter.
This is plated under 25 ℃ of the temperature and carries out, and is after the diameter 1.2mm with the further Wire Drawing of the line behind the plating, and perhaps further Wire Drawing is after diameter 0.8mm or the 1.0mm, estimates for the adaptation of coating layer, measures the crystallite dimension of coating layer simultaneously.
With sample wire after being wound into spirrillum on the pole, with multiplying power is that 30 times microscopic visual measurement is observed its surface, adaptation is estimated in the following manner: fully unusual situation unconfirmed is ◎ (with Fig. 2 and Fig. 3 as an example), do not occur peeling off but concavo-convex, fold occurs or fissured situation is zero (with Fig. 4 as an example), the situation that occurs peeling off on a small quantity is △ (with Fig. 5 as an example), peels off a lot of situation of appearance to be * (with Fig. 6 as an example).In addition, crystallite dimension uses the unrelieved stress device to calculate according to Schrrer method (integral breadth method).
Experimental result is as shown in table 1.In addition, the kind of nonionic surface active agent is 1: polyoxyethylene glycol, 2: alkyl glycoside, 3: gelatine, 4: gelatin, 5: polyvinyl alcohol, 6: polyoxyethylene alkyl phenyl ether, 7: glycerine.In addition, the material that adds in order to generate halide ions is 1:NaCl, 2:KCl, 3:CaCl
2, 4:MgCl
2, 5:HCl, 6:NaBr.In addition, the kind of organic class cathodic corrosion inhibitor is 1: vulkacit H, 2: thiocarbamide, 3: acrylamide, 4: Thiovanic acid.In addition, the stringy classification is 1) be line footpath 1.2mm, 2 with line footpath 2.3mm Wire Drawing) be line footpath 1.2mm, 3 with line footpath 2.6mm Wire Drawing) with 1) further chase after be processed as line footpath 0.8mm, 4) with 2) further chase after and be processed as line footpath 1.0mm.
Table 1
Shown in this result,, can improve the adaptation and the crystallite dimension of coating by in plating bath, adding more than the nonionic surface active agent 5mg/L.
Except nonionic surface active agent,, can become preferred plating by adding planting at least arbitrarily in halide ions and the organic class cathodic corrosion inhibitor.
In addition, shown in this experimental result, crystallite dimension diminished when wire drawing degree as can be known was big.Crystallite dimension less than
The time, grain boundary area increases, and easily heating oxidation during Wire Drawing may cause that the adaptation reduction of coating layer or the energising stability of line reduce.Crystallite dimension surpasses
The time, can not the draw line surface during Wire Drawing, the result produces and peels off.
Thickness of coating is preferably 50～500 μ m.50 μ m are easy to generate the thin place of part or defective and can be corroded on copper plating film when following.And cause during because of wire drawing to peel off etc. in the online manufacturing and may become serious problems.In addition, when being applicable to welding wire, in the release in when welding, also occur inhomogeneous, thereby the weldability variation.On the other hand, when 500 μ m were above, because the tunicle thickening, even very little machining stress, the coating tunicle was also peeled off easily.Its result causes that erosion resistance worsens, the stringiness variation.Also be disadvantageous in addition economically.
In addition, in order to keep unremitting copper plate, wish that also making the thickness of coating after the Wire Drawing is more than the 50nm.
In addition, when having confirmed to improve the temperature of plating bath, even identical plating bath is formed, it is big that copper-plated mould also becomes.
Claims (7)
1. the copper electroplating method of a filamentary material wherein sprays the displacement plating bath to the filamentary material that moves, and it is characterized in that, the every 1L of described displacement plating bath contains the above CuSO of 5g
45H
2The H that O, 5g are above and 400g is following
2SO
4, 5g is above and 400g is following FeSO
47H
2At least a kind of nonionic surface active agent that O and 5mg are above.
2. the copper electroplating method of filamentary material according to claim 1, wherein, described nonionic surface active agent is below the 10g in the described displacement plating bath of every 1L.
3. the copper electroplating method of filamentary material according to claim 2, wherein, described nonionic surface active agent is selected from sucrose fatty ester sorbitan-fatty acid ester, polyoxyethylene sorbitan fatty acid ester, fatty acid alkyl amide, Voranol EP 2001 and polyoxyethylene alkyl phenyl ether.
4. the copper electroplating method of filamentary material according to claim 3, wherein, described displacement plating bath also contains at least a kind of halide ions that 0.1mmol is above and 1mol is following.
5. the copper electroplating method of filamentary material according to claim 4, wherein, described displacement plating bath also contains at least a kind of above organic class cathodic corrosion inhibitor of 5mg, and this organic class cathodic corrosion inhibitor has the polar group and the non-polar group that prevents that corrosives from contacting with the metallic surface that is used to be adsorbed on the metallic surface.
6. the copper electroplating method of filamentary material according to claim 5, wherein, in the described displacement plating bath of every 1L, described organic class cathodic corrosion inhibitor is below the 10g.
7. coppered wire, it is that the filamentary material that moves is sprayed the displacement plating bath and forms carrying out wire drawing behind the copper coating, it is characterized in that the every 1L of described displacement plating bath contains the above CuSO of 5g
45H
2The H that O, 5g are above and 400g is following
2SO
4, 5g is above and 400g is following FeSO
47H
2At least a kind of nonionic surface active agent that O and 5mg are above, the crystallite dimension of described copper plate is 50
More than and 250
Below, and the thickness of the described copper plate after the described wire drawing is more than the 50nm.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2007164711A JP2009001872A (en) | 2007-06-22 | 2007-06-22 | Copper-plating method of wire-like material, and copper-plated wire |
| JP2007164711 | 2007-06-22 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN101328582A true CN101328582A (en) | 2008-12-24 |
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ID=40204584
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNA2008100818077A Pending CN101328582A (en) | 2007-06-22 | 2008-04-02 | Copper plating method of wirelike material and coppered wire |
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|---|---|
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| CN (1) | CN101328582A (en) |
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| CN102154634A (en) * | 2011-02-21 | 2011-08-17 | 山东大学 | Preparation method for copper clad aluminum composite conductive material |
| CN104372315A (en) * | 2013-07-19 | 2015-02-25 | 罗门哈斯电子材料有限公司 | Electroless copper plating solution |
| CN104593602A (en) * | 2014-12-31 | 2015-05-06 | 上海第二工业大学 | Method for extracting metallic lead from alkaline leaching solution of waste lead-containing glass |
| CN107460455A (en) * | 2017-07-25 | 2017-12-12 | 东莞聚顺环保科技有限公司 | The tin plating water-based process material of copper ecology and its tin plating method |
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|---|---|---|---|---|
| BE759316A (en) * | 1969-12-30 | 1971-04-30 | Parker Ste Continentale | COMPOSITION AND METHOD FOR FORMING A COPPER DEPOSIT ON FERROUS METAL SURFACES |
| BE793376A (en) * | 1972-03-13 | 1973-04-16 | Parker Ste Continentale | COMPOSITION AND PROCESS FOR COPING METAL SURFACES |
| JPS544329B2 (en) * | 1973-03-20 | 1979-03-06 | ||
| US4563216A (en) * | 1984-06-15 | 1986-01-07 | Amchem Products, Inc. | Compositions and processes for coating ferrous surfaces with copper |
| JPH01129977A (en) * | 1987-11-13 | 1989-05-23 | Hitachi Ltd | Copper plating solution |
| JPH01136974A (en) * | 1987-11-20 | 1989-05-30 | Kobe Steel Ltd | Surface treatment of filament material |
| JP2003249405A (en) * | 2002-02-25 | 2003-09-05 | Hitachi Metals Ltd | Rare-earth permanent magnet and surface treatment method thereof |
-
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- 2007-06-22 JP JP2007164711A patent/JP2009001872A/en active Pending
-
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- 2008-04-02 CN CNA2008100818077A patent/CN101328582A/en active Pending
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| CN102154634A (en) * | 2011-02-21 | 2011-08-17 | 山东大学 | Preparation method for copper clad aluminum composite conductive material |
| CN102154634B (en) * | 2011-02-21 | 2012-08-22 | 山东大学 | Preparation method for copper clad aluminum composite conductive material |
| CN104372315A (en) * | 2013-07-19 | 2015-02-25 | 罗门哈斯电子材料有限公司 | Electroless copper plating solution |
| CN104593602A (en) * | 2014-12-31 | 2015-05-06 | 上海第二工业大学 | Method for extracting metallic lead from alkaline leaching solution of waste lead-containing glass |
| CN107460455A (en) * | 2017-07-25 | 2017-12-12 | 东莞聚顺环保科技有限公司 | The tin plating water-based process material of copper ecology and its tin plating method |
| CN107557767A (en) * | 2017-07-25 | 2018-01-09 | 东莞聚顺环保科技有限公司 | Nickel ecology copper facing water-based process material and its copper electroplating method |
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|---|---|
| JP2009001872A (en) | 2009-01-08 |
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