CN103014787B - A kind of copper electroplating liquid and electroplating technology thereof - Google Patents
A kind of copper electroplating liquid and electroplating technology thereof Download PDFInfo
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Abstract
The invention provides a kind of copper electroplating liquid and electroplating technology thereof, belong to electroplating technology field.Described electroplate liquid mainly comprises complexing agent, main salt, conducting salt, brightening agent, and its pH value is 9.0 ~ 11.0.For existing alkaline copper plating technique, plating solution causes the problem of environmental pollution usually containing prussiate, the present invention, by a kind of Alkali CyanideFree Copper Electroplating Technology, provides a kind of environment-protective process of electro-coppering.This electroplate liquid containing the advantage that prussiate, copper plate and basal body binding force are strong, can not be widely used in field of electroplating.
Description
Technical field
The present invention relates to a kind of electroplating technology, more particularly relate to a kind of cyanide-free alkaline copper plating technology.
Background technology
Industrialized development, problem of environmental pollution is more and more serious, and for protection of the environment, clean, environmental protection, energy-conservation production are more and more subject to the attention of industry.In electroplating industry cyanide copper plating process, production process must use prussiate cyanide copper plating process, there is the prussiate of hypertoxicity, and its environmental pollution is extremely serious, causes serious threat to workman is healthy; Along with the enhancing of the environmental consciousness of people, the copper-plating technique of an urgent demand development environment-protecting clean, substitutes traditional cyanide copper plating technique.Therefore, develop new environmental protection copper-plating technique, solve the health problem of problem of environmental pollution and direct labor, have positive social effect.In fact, the research and development to cyanideless electro-plating is carried out all the time in electroplating technology field in countries in the world, and along with the progress of correlation technique, and new electroplating additive comes into the market, the level of cyanogenless electroplating technology is progressively improving.
Summary of the invention
In view of this, the present invention proposes a kind of copper electroplating liquid and electroplating technology thereof, for a kind of Alkali CyanideFree Copper Electroplating Technology, be applied in electro-coppering production, layers of copper and basal body binding force well can reach that production technique cleans, the requirement of environmental protection, traditional cyanide copper plating technique can be substituted, solve prior art environmental pollution and the health threat problem to direct labor.
Technical scheme of the present invention is achieved in that a kind of copper electroplating liquid, and described electroplate liquid mainly comprises complexing agent, main salt, conducting salt, brightening agent, wherein:
Complexing agent content is 100 ~ 200 grams per liters;
Main salts contg is 30 ~ 100 grams per liters;
Conducting salt content is 20 ~ 50 grams per liters;
Brightening agent content is 10 ~ 100 mg/litre;
The pH value of electroplate liquid is 9.0 ~ 11.0; Solvent is water.
Described complexing agent is by one or more the combination in Trisodium Citrate, thionamic acid sodium, Sunmorl N 60S, disodium ethylene diamine tetraacetate.
Described complexing agent is disodium ethylene diamine tetraacetate and Trisodium Citrate.
Described main salt is by one or both in copper sulfate, ventilation breather.
Described main salt is ventilation breather, and its content is 50 ~ 80 grams per liters.
Described conducting salt is one or both in potassium sulfate, saltpetre.
Described brightening agent is one or more the combination in Sulfothiorine, potassium sulfocyanate, furans.
Described pH value ammoniacal liquor or sulfuric acid adjustment.
The electroplating technology of a kind of copper electroplating liquid of the present invention, is characterized in that: comprise the following steps:
(1) metallic copper is put into above-mentioned copper electroplating solution, as anode;
(2) workpiece is put into above-mentioned copper electroplating solution, as negative electrode;
(3) direct supply is passed into, cathode current density 0.5 ~ 3 ampere/square decimeter, temperature of electroplating solution 40 ~ 55 DEG C, electroplating time 2 ~ 8 minutes.
In described step (3), cathode current density is 1.0 ~ 2.0 amperes/square decimeter; Temperature of electroplating solution is 45 ~ 50 DEG C; Electroplating time is 4 ~ 6 minutes.
Compared with prior art, electroplate liquid of the present invention adopts New Chelating Agents to replace cyanide complex agent, and the beneficial effect had is:
1) electroplate liquid is not containing prussiate, reaches the requirement of environment-protecting clean production technique, can not threaten to the health problem of direct labor.
2) coating and basal body binding force well, reach the technical requirements of electrolytic coating bonding force.
Embodiment
Below in conjunction with specific embodiment, the present invention is described in further detail, but any limitation of the invention do not formed.
Embodiment 1
A kind of copper electroplating liquid, described electroplate liquid mainly comprises complexing agent, main salt, conducting salt, brightening agent, wherein:
PH value is 10.0, with ammoniacal liquor or sulfuric acid adjustment.
Electro-plating method: adopt rectangle iron plate 70 × 100mm, in the Hull Cell of 267ml, carry out plating test, condition is: temperature 50 C, galvanic current are 1.0 amperes, electroplate 5 minutes, and anode uses copper coin, obtains test piece A1.
Electroplating effect is evaluated: observe test piece A1 outward appearance, and whether coating is bright evenly, crystallization is careful.
Coat binding strength is evaluated: according to ASTMB571(Usa Metals coating adhesive power qualitative test) standard, test piece A1 is heated to 240 ~ 260 DEG C in stove, then takes out the water putting into room temperature and cool, observe coating whether bubbling or come off.If layers of copper has bubbling or comes off, then layers of copper and substrate combinating strength defective; If layers of copper does not have bubbling or comes off, then layers of copper and substrate combinating strength qualified.
Embodiment 2
Electroplating bath components:
PH value is 10.0, with ammoniacal liquor or sulfuric acid adjustment.
Electro-plating method: adopt rectangle iron plate 70 × 100mm, in the Hull Cell of 267ml, carry out plating test, condition is: temperature 50 C, galvanic current are 1.0 amperes, electroplate 8 minutes, and anode uses copper coin, obtains test piece A2.
Electroplating effect is evaluated: observe test piece A2 outward appearance, and whether coating is bright evenly, crystallization is careful.
Coat binding strength is evaluated: according to ASTMB571 standard, test piece A2 is heated to 240 ~ 260 DEG C in stove, then takes out the water putting into room temperature and cools, and observes coating whether bubbling or come off.If layers of copper has bubbling or comes off, then layers of copper and substrate combinating strength defective; If layers of copper does not have bubbling or comes off, then layers of copper and substrate combinating strength qualified.
Embodiment 3
Electroplating bath components:
PH value is 11.0, with ammoniacal liquor or sulfuric acid adjustment.
Electro-plating method: adopt rectangle iron plate 70 × 100mm, in the Hull Cell of 267ml, carry out plating test, condition is: temperature 50 C, galvanic current are 1.0 amperes, electroplate 6 minutes, and anode uses copper coin, obtains test piece A3.
Electroplating effect is evaluated: observe test piece A3 outward appearance, and whether coating is bright evenly, crystallization is careful.
Coat binding strength is evaluated: according to ASTMB571 standard, test piece A3 is heated to 240 ~ 260 DEG C in stove, then takes out the water putting into room temperature and cools, and observes coating whether bubbling or come off.If layers of copper has bubbling or comes off, then layers of copper and substrate combinating strength defective; If layers of copper does not have bubbling or comes off, then layers of copper and substrate combinating strength qualified.
Embodiment 4
Electroplating bath components:
PH value is 9.0, with ammoniacal liquor or sulfuric acid adjustment.
Electro-plating method: adopt rectangle iron plate 70 × 100mm, in the Hull Cell of 267ml, carry out plating test, condition is: temperature 55 DEG C, galvanic current are 0.5 ampere, electroplate 8 minutes, and anode uses copper coin, obtains test piece A4.
Electroplating effect is evaluated: observe test piece A4 outward appearance, and whether coating is bright evenly, crystallization is careful.
Coat binding strength is evaluated: according to ASTMB571 standard, test piece A4 is heated to 240 ~ 260 DEG C in stove, then takes out the water putting into room temperature and cools, and observes coating whether bubbling or come off.If layers of copper has bubbling or comes off, then layers of copper and substrate combinating strength defective; If layers of copper does not have bubbling or comes off, then layers of copper and substrate combinating strength qualified.
Embodiment 5
Electroplating bath components:
PH value is 10.0, with ammoniacal liquor or sulfuric acid adjustment.
Electro-plating method: adopt rectangle iron plate 70 × 100mm, in the Hull Cell of 267ml, carry out plating test, condition is: temperature 40 DEG C, galvanic current are 0.5 ampere, electroplate 8 minutes, and anode uses copper coin, obtains test piece A5.
Electroplating effect is evaluated: observe test piece A5 outward appearance, and whether coating is bright evenly, crystallization is careful.
Coat binding strength is evaluated: according to ASTMB571 standard, test piece A5 is heated to 240 ~ 260 DEG C in stove, then takes out the water putting into room temperature and cools, and observes coating whether bubbling or come off.If layers of copper has bubbling or comes off, then layers of copper and substrate combinating strength defective; If layers of copper does not have bubbling or comes off, then layers of copper and substrate combinating strength qualified.
Embodiment 6
Electroplating bath components:
PH value is 10.0, with ammoniacal liquor or sulfuric acid adjustment.
Electro-plating method: adopt rectangle iron plate 70 × 100mm, in the Hull Cell of 267ml, carry out plating test, condition is: temperature 55 DEG C, galvanic current are 1.5 amperes, electroplate 4 minutes, and anode uses copper coin, obtains test piece A6.
Electroplating effect is evaluated: observe test piece A6 outward appearance, and whether coating is bright evenly, crystallization is careful.
Coat binding strength is evaluated: according to ASTMB571 standard, test piece A6 is heated to 240 ~ 260 DEG C in stove, then takes out the water putting into room temperature and cools, and observes coating whether bubbling or come off.If layers of copper has bubbling or comes off, then layers of copper and substrate combinating strength defective; If layers of copper does not have bubbling or comes off, then layers of copper and substrate combinating strength qualified.
Embodiment 7
Electroplating bath components:
PH value is 10.5, with ammoniacal liquor or sulfuric acid adjustment.
Electro-plating method: adopt rectangle iron plate 70 × 100mm, in the Hull Cell of 267ml, carry out plating test, condition is: temperature 50 C, galvanic current are 1.0 amperes, electroplate 5 minutes, and anode uses copper coin, obtains test piece A7.
Electroplating effect is evaluated: observe test piece A7 outward appearance, and whether coating is bright evenly, crystallization is careful.
Coat binding strength is evaluated: according to ASTMB571 standard, test piece A7 is heated to 240 ~ 260 DEG C in stove, then takes out the water putting into room temperature and cools, and observes coating whether bubbling or come off.If layers of copper has bubbling or comes off, then layers of copper and substrate combinating strength defective; If layers of copper does not have bubbling or comes off, then layers of copper and substrate combinating strength qualified.
Embodiment 8
Electroplating bath components:
PH value is 11.0, with ammoniacal liquor or sulfuric acid adjustment.
Electro-plating method: adopt rectangle iron plate 70 × 100mm, in the Hull Cell of 267ml, carry out plating test, condition is: temperature 45 C, galvanic current are 0.5 ampere, electroplate 3 minutes, and anode uses copper coin, obtains test piece A8.
Electroplating effect is evaluated: observe test piece A8 outward appearance, and whether coating is bright evenly, crystallization is careful.
Coat binding strength is evaluated: according to ASTMB571 standard, test piece A8 is heated to 240 ~ 260 DEG C in stove, then takes out the water putting into room temperature and cools, and observes coating whether bubbling or come off.If layers of copper has bubbling or comes off, then layers of copper and substrate combinating strength defective; If layers of copper does not have bubbling or comes off, then layers of copper and substrate combinating strength qualified.
Comparative example 1
Electroplating bath components: do not add inferior sodium phosphate;
Electro-plating method: adopt rectangle iron plate 70 × 100mm, in the Hull Cell of 267ml, carry out plating test, condition is: temperature 50 C, galvanic current are 1.0 amperes, electroplate 5 minutes, and anode uses copper coin, obtains test piece B1.
Electroplating effect is evaluated: observe test piece B1 outward appearance, and whether coating is bright evenly, crystallization is careful.
Coat binding strength is evaluated: according to ASTMB571 standard, test piece B1 is heated to 240 ~ 260 DEG C in stove, then takes out the water putting into room temperature and cools, and observes coating whether bubbling or come off.If layers of copper has bubbling or comes off, then layers of copper and substrate combinating strength defective; If layers of copper does not have bubbling or comes off, then layers of copper and substrate combinating strength qualified.
Copper facing test piece obtained above, Deposit appearance effect and bonding strength are as table 1.
Table 1: electroplating effect evaluation table
| Numbering | Plating solution is numbered | Deposit appearance | Coat binding strength |
| Embodiment 1 | A1 | Light is even, crystallization is careful | Qualified |
| Embodiment 2 | A2 | Light is even, crystallization is careful | Qualified |
| Embodiment 3 | A3 | Light is even, crystallization is careful | Qualified |
| Embodiment 4 | A4 | Light is even, crystallization is careful | Qualified |
| Embodiment 5 | A5 | Light is even, crystallization is careful | Qualified |
| Embodiment 6 | A6 | Light is even, crystallization is careful | Qualified |
| Embodiment 7 | A7 | Light is even, crystallization is careful | Qualified |
| Embodiment 8 | A8 | Light is even, crystallization is careful | Qualified |
| Comparative example 1 | B1 | Light is even, crystallization is careful | Qualified |
Not containing prussiate in embodiment 1-8 plating solution, the plating solution of comparative example 1 contains prussiate, and the test piece outward appearance layers of copper light of embodiment 1-8 and comparative example 1 is even, crystallization is careful, good with substrate combinating strength.In sum, a kind of Alkali CyanideFree Copper Electroplating Technology provided by the invention, electroplate liquid is not containing prussiate, and copper electroplating layer light is even, crystallization is careful, the advantage good with substrate combinating strength.
The above embodiments are only the preferred embodiments of the present invention, can not limit interest field of the present invention with this, and therefore, the equivalent variations done according to the present patent application the scope of the claims, still belongs to the scope that the present invention is contained.
Claims (5)
1. an electroplating technology for copper electroplating liquid, is characterized in that: described copper electroplating liquid mainly comprises complexing agent, main salt, conducting salt, brightening agent, wherein:
Complexing agent content is 100 ~ 200 grams per liters;
Main salts contg is 50 ~ 100 grams per liters;
Conducting salt content is 20 ~ 50 grams per liters;
Brightening agent content is 10 ~ 100 mg/litre;
The pH value of electroplate liquid is 9.0 ~ 11.0; Solvent is water;
Described complexing agent is Trisodium Citrate and disodium ethylene diamine tetraacetate;
Described main salt is ventilation breather;
Described brightening agent is one or more the combination in Sulfothiorine, potassium sulfocyanate, furans;
Described electroplate liquid is used for direct current electrode position;
Electroplating technology comprises the following steps:
(1) metallic copper is put into above-mentioned copper electroplating solution, as anode;
(2) workpiece is put into above-mentioned copper electroplating solution, as negative electrode;
(3) direct supply is passed into, cathode current density 0.5 ~ 3 ampere/square decimeter, temperature of electroplating solution 40 ~ 55 DEG C, electroplating time 2 ~ 8 minutes.
2. the electroplating technology of a kind of copper electroplating liquid as claimed in claim 1, is characterized in that: in described step (3), cathode current density is 1.0 ~ 2.0 amperes/square decimeter; Temperature of electroplating solution is 45 ~ 50 DEG C; Electroplating time is 4 ~ 6 minutes.
3. the electroplating technology of a kind of copper electroplating liquid as claimed in claim 1, is characterized in that: described main salt is ventilation breather, and its content is 50 ~ 80 grams per liters.
4. the electroplating technology of a kind of copper electroplating liquid as claimed in claim 1, is characterized in that: described conducting salt is one or both in potassium sulfate, saltpetre.
5. the electroplating technology of a kind of copper electroplating liquid as claimed in claim 1, is characterized in that: bath pH values ammoniacal liquor or sulfuric acid adjustment.
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Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104388991A (en) * | 2014-11-14 | 2015-03-04 | 无锡信大气象传感网科技有限公司 | Copper electroplate liquid and preparation method thereof |
| CN107604392A (en) * | 2017-09-29 | 2018-01-19 | 佛山市春暖花开科技有限公司 | A kind of electroplate liquid of copper |
| CN107740146A (en) * | 2017-10-27 | 2018-02-27 | 桐城运城制版有限公司 | A kind of intaglio plate copper plating additive |
| CN109868492A (en) * | 2018-05-18 | 2019-06-11 | 临海市伟星电镀有限公司 | A kind of no cyanogen alkali copper electroplating liquid and preparation method thereof |
| CN109825861A (en) * | 2019-03-18 | 2019-05-31 | 辽宁科技大学 | A kind of pure iron base basic plating copper coating technique |
| CN110760905A (en) * | 2019-11-28 | 2020-02-07 | 汕头市铠嘉模具有限公司 | Application of alkaline cyanide-free copper plating process in gravure industry |
| CN110923757B (en) * | 2019-12-27 | 2021-04-06 | 广州三孚新材料科技股份有限公司 | Cyanide-free alkali copper electroplating solution and use method thereof |
| CN114657611B (en) * | 2022-04-20 | 2024-03-12 | 佛山市诺诚科技有限公司 | Alkaline copper electroplating solution and electroplating method thereof |
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| US5750018A (en) * | 1997-03-18 | 1998-05-12 | Learonal, Inc. | Cyanide-free monovalent copper electroplating solutions |
| CN102234825A (en) * | 2010-05-01 | 2011-11-09 | 湖北恒鑫金属表面处理有限公司 | Industrial method for citrate alkaline non-cyanide copper plating on steel substrate |
| CN102677116A (en) * | 2012-06-12 | 2012-09-19 | 山东建筑大学 | Method for dipulse preplating non-cyanide alkaline copper on ferro matrix |
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| US20060231409A1 (en) * | 2005-03-31 | 2006-10-19 | Tdk Corporation | Plating solution, conductive material, and surface treatment method of conductive material |
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Patent Citations (3)
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|---|---|---|---|---|
| US5750018A (en) * | 1997-03-18 | 1998-05-12 | Learonal, Inc. | Cyanide-free monovalent copper electroplating solutions |
| CN102234825A (en) * | 2010-05-01 | 2011-11-09 | 湖北恒鑫金属表面处理有限公司 | Industrial method for citrate alkaline non-cyanide copper plating on steel substrate |
| CN102677116A (en) * | 2012-06-12 | 2012-09-19 | 山东建筑大学 | Method for dipulse preplating non-cyanide alkaline copper on ferro matrix |
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