CN101575720A - Nickel-free ferrous tin-cobalt alloy plating solution and process for utilizing plating solution for electroplating - Google Patents
Nickel-free ferrous tin-cobalt alloy plating solution and process for utilizing plating solution for electroplating Download PDFInfo
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- CN101575720A CN101575720A CNA2009100402403A CN200910040240A CN101575720A CN 101575720 A CN101575720 A CN 101575720A CN A2009100402403 A CNA2009100402403 A CN A2009100402403A CN 200910040240 A CN200910040240 A CN 200910040240A CN 101575720 A CN101575720 A CN 101575720A
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Abstract
The invention relates to a nickel-free ferrous tin-cobalt alloy plating solution and a process for utilizing the plating solution for electroplating. The plating solution comprises the following compositions: 0.2 to 6 g/L of tin, 0.6 to 4 g/L of cobalt, 8 to 180 g/L of complexant, 2 to 20 g/L of melanizing agent and 50 to 320 g/L of pH buffer. The parameters of the plating solution are as follows: the Baume of the plating solution is between 10 and 25 baume degrees; the temperature is between 28 and 48 DEG C; and the pH is between 10 and 13. The coating of the nickel-free ferrous tin-cobalt alloy plating solution is an alloy layer taking the tin as a main material, and a small amount of cobalt is added into the coating to form a binary alloy system; the cobalt content in a general ferrous tin-cobalt alloy plating solution exceeds 8 g/L, but the novel electroplating process can reduce the cobalt content to 0.8 g/L; and due to adoption of the special biodegradable stable complexant and the special biodegradable pH buffer, the production cost can be reduced, novel EU standards can be reached simultaneously, and various problems of the prior ferrous tin-cobalt alloy plating solution and the prior process can be solved.
Description
Technical field
The present invention relates to the alloy plating technical field, refer in particular to a kind of nickel-free ferrous tin-cobalt alloy plating solution and utilize this plating bath to carry out electroplating technique.This technology is applicable to the various article that contact closely with human body such as hardware, electronic product, personal digital product, dress accessory, toy for children, jewellery, furniture, food utensil.
Background technology
At present, the tin-cobalt alloy electroplating technology has been widely used in the plating of article accessories such as hardware, electronic product, personal digital product, dress accessory, toy for children, jewellery, furniture, food utensil, having implemented to electroplate environmental-friendly lead-free does not have tin-cobalt alloy coating that nickel do not have cyanogen to obtain black bright alloy environmental protection layer, satisfies on the market demand to black electroplated decoration product.Present stage, there was following problem in ubiquitous tin-cobalt alloy electroplating technology: 1, cobalt contents surpasses 5g/L, generally at 8g/L, and plating bath cost height.2, cobalt contents height in the plating bath more easily makes the coating carrying magnetic, does not cross rag trade needle checking machine commonly used, is commonly called as " ringing machine ".3, use potassium pyrophosphate or sodium to be complexing agent and conducting salt, between the PH 7～10, the plating bath instability, the very easy precipitation of cobalt and tin, cylinder bottom often had thick throw out after the production neutralization stopped production several days.4, the plating bath Baume is up to more than 24 °, and plating bath viscosity is big, and band water is serious, loses a large amount of cobalts, tin metal ion and potassium pyrophosphate, and being not intended to the free burial ground for the destitute increases cost; The electroplating temperature height wastes energy.5, cobalt has certain radioactivity, shows great attention to the requirement that comprises in the material cobalt chloride for 15 in the formally effective REACH of the European Union instruction in (are nuclear radiation materials as cobalt 60) on June 1st, 2007, requires the consumption of restriction cobalt.6, the difficult control of plating bath, low current district effect is bad, and often plating leakage, jaundice even if workman's state of the art height also needs often to adjust plating bath, cause wastage of material.7, solution composition is adjusted in the difficult control of coating depth color fully by rule of thumb.8, because coating low current district effect is bad, when producing the black and white mandarin duck chromatic effect of no nickel black nickel, electroplating time is long, and high Current Zone coating is very thick, and wire drawing, wiping look chronic requires the plated underlayer layer thickness very thick, wastes very big.
Though the black tin-cobalt alloy electroplating technology of present use can reach in European Union and the U.S. food standard about forbidding containing in the electrolytic coating regulation of described heavy metal, but cobalt contents is too high in the plating bath, may not necessarily satisfy the requirement of following environment-protection electroplating, and whole electroplating system cost height.
Summary of the invention:
The objective of the invention is on conscientious and sufficient investigation, understanding, analysis, the above-mentioned existing black tin-cobalt alloy electroplating technology of summary basis, for overcoming and solve the deficiency of its existence, providing a kind of environmental-friendly lead-free not have nickel does not have cyanogen, reduces production costs, can reach simultaneously European Union new standard nickel-free ferrous tin-cobalt alloy plating solution and utilize this plating bath to carry out electroplating technique.
For achieving the above object, technical scheme provided by the invention is: a kind of nickel-free ferrous tin-cobalt alloy plating solution is characterized in that the parameter of this plating bath and each component content as follows:
Tin 0.2-6 gram/L
Cobalt 0.6-4 gram/L
Complexing agent 8-180 gram/L
Blackening agent 2-20 gram/L
PH buffer reagent 50-320 gram/L
10-25Be ° of plating bath Baume
Temperature 28-48 ℃
PH 10-13
Described complexing agent is one or more the combination in ETDA complexone, tartrate and salt thereof, citric acid and salt thereof, acetic acid and salt thereof, phosphoric acid and salt thereof, trolamine, lactic acid, each seed amino acid and salt, quadrol, sodium hydroxide, potassium hydroxide, oxysuccinic acid and salt thereof, tartaric acid and salt thereof, carbonate, the thiocyanate-.
Described blackening agent is a kind of in amino acid and salt, thiocyanic acid and salt thereof, cobalt salt and the pink salt.
Described cobalt salt is one or more the combination in the cobalt salt of cobaltous carbonate, cobalt chloride, rose vitriol and complexing agent.
Described pink salt is one or more the combination in the pink salt of tin protochloride, stannous sulfate, stannous pyrophosphate, tin methane sulfonate and complexing agent.
Described PH buffer reagent is one or more the combination in acetic acid and salt, tartrate and salt thereof, carbonic acid and salt thereof, phosphoric acid and salt thereof, ammoniacal liquor, trolamine, sodium tetraborate, potassium tetroxalate, citric acid and salt thereof, the quadrol.
A kind ofly utilize above-mentioned plating bath to carry out electroplating technique: with metallic copper, brass, with electro-coppering and copper alloy, nickel, a kind of in the Cu-Sn-Zn ternary alloy is basic unit, directly use this no nickel-tin alloy plating bath, under 28～48 ℃ of temperature, use sulfuric acid, hydrochloric acid or potassium hydroxide, sodium hydroxide is regulated between PH to 11～12, this moment, metallic tin content was between 0.5～4g/L, cobalt contents is between 0.4～4g/L, between complexing agent 5～300g/L, between PH buffer reagent 5～300g/L, between blackening agent 0.1～50g/L, the plating bath degree Beaume is 10～22 °, voltage control is 3～10 volts of barrel platings, 2～6 volts of rack platings with cathode current density are being rack plating 20～200 seconds or barrel plating 3～140 minutes under 0.1～3.5 ampere/square decimeter the situation; Plating finishes, and it is clean take out to electroplate the body and function flushing with clean water, can obtain the black of light and near black coating after drying up.
Coating of the present invention mainly is the alloy layer based on tin, add a spot of cobalt and form the binary alloy system, cobalt contents surpasses 8g/L in the general black tin-cobalt alloy electroplate liquid, and our new electroplating technology can be reduced to the content of cobalt 0.8g/L, use special biodegradable stable complexation agent and PH buffer reagent, thereby reduce production costs, can reach the new standard of European Union simultaneously, solve existing black tin-cobalt alloy electroplate liquid and all drawbacks of technology.
In sum, the present invention has the following advantages: 1, coating is nonmagnetic, is difficult for " ringing machine ".2, the coating cobalt contents is few, does not have radioactivity, can reach the new standard of European Union.3, plating bath normal-temperature operation (30 ℃) reduces cost.4, unleaded, the no nickel of plating bath, no cyanogen, all complexing agents can biological degradations, and the simple cost of wastewater treatment is low.5, the plating bath cobalt contents is low, and degree Beaume is low, and viscosity is low, and plating bath band water loss is few, saves a large amount of cobalts, tin metal ion, and cost reduces significantly.6, add materials in kiloampere hour ratio and chemical examination, easy to operate simple, labor strength is low.7, bath stability is middle strong basicity, and pH changes little (11～12), and tin, cobalt metal ion are difficult for decomposing precipitation.8, the high Current Zone of coating is effective, and when producing the black and white mandarin duck chromatic effect of no nickel black nickel, electroplating time is short, and high Current Zone coating is thin, and the time of wire drawing, wiping look very short, low to the requirement of plated underlayer layer thickness, saves cost in a large number.
Embodiment:
Embodiment 1:
Tin 0.3 gram/L
Cobalt 0.6 gram/L
Complexing agent 8 gram/L
Blackening agent 2 gram/L
PH buffer reagent 50 gram/L
10Be ° of plating bath Baume
28 ℃ of temperature
PH 12
Experiment effect: test piece walks more than 95%, and coating is thin slightly, and it is coffee-like that color is, and color and luster is even.
Embodiment 2:
Tin 4 gram/L
Cobalt 2 gram/L
Complexing agent 80 gram/L
Blackening agent 10 gram/L
PH buffer reagent 100 gram/L
15Be ° of plating bath Baume
35 ℃ of temperature
PH 11
Experiment effect: test piece walks 99%, and coating is shiny black evenly.
Embodiment 3:
Tin 6 gram/L
Cobalt 4 gram/L
Complexing agent 120 gram/L
Blackening agent 20 gram/L
PH buffer reagent 320 gram/L
25Be ° of plating bath Baume
40 ℃ of temperature
PH 12
Experiment effect: test piece walks 99%, and coating is abundant, and color and luster is shiny black evenly.
The concrete selection of the employed additive of the various embodiments described above is as follows:
1) complexing agent: complexing Sn
2+, Co
2+, guarantee that it is stable in the plating bath equably to electroplate.Complexing agent can be ammonia hydroxyl complexing agent, tartrate and salt, citric acid and salt thereof, acetic acid and salt thereof, phosphoric acid and salt thereof, trolamine, lactic acid, each seed amino acid and salt, quadrol, sodium hydroxide, potassium hydroxide, oxysuccinic acid and salt thereof, tartaric acid and salt thereof, carbonate, thiocyanate-s etc. such as ETDA.
2) blackening agent: daily use can keep and increase blackness, once adds coating is hazed, and jaundice, coating turns white very little.Blackout salt can be each seed amino acid, thiocyanic acid and salt thereof etc.
3) PH buffer reagent: the buffering pH value, make it stable, reduce the plating bath pH value and change.The PH buffer reagent can be acetic acid and salt, tartrate and salt thereof, carbonic acid and salt thereof, phosphoric acid and salt thereof, ammoniacal liquor, trolamine, sodium tetraborate, potassium tetroxalate, citric acid and salt, quadrol etc.
Also can use following metal-salt in the electroplate liquid of nickel-free ferrous tin-cobalt alloy:
1) cobalt salt: daily additional Co
2+, increasing black and can eliminating excessive pink salt influences, and can make the coating jaundice too much.Cobalt salt can be the cobalt salt of cobaltous carbonate, cobalt chloride, cobaltous phosphate, rose vitriol and complexing agent.
2) pink salt: daily additional Sn
2+, enhancing walks, and too many coating is white partially, and influence walks and coating hazes very little; This pink salt has that the complexing salt of eliminating cobalt is excessive to haze and the influence of the excessive jaundice of cobalt.Pink salt can be the pink salt of tin protochloride, stannous sulfate, stannous pyrophosphate, tin methane sulfonate and complexing agent.
The solution additive each component is best to be formed:
Complexing agent: tartrate or salt, citric acid or salt, acetic acid and salt thereof, each seed amino acid and salt, carbonate, phosphoric acid and salt thereof.
Blackening agent: sulfur-containing amino acid.
PH buffer reagent: tartrate or salt, carbonate, phosphoric acid and salt thereof, ammoniacal liquor, quadrol, acetic acid and salt thereof.
Carried out the practicality examination after the new electroplating technology that the present invention produces is finished, examination shows the coating black bright under this technology, and multiple black, black-and-blue, yellow black, coffee color, brownish black, grey black, rifle black effect can be provided; Anti-variable color ability is better, and anti-neutral salt spray test is effective; Precipitation can not appear in bath stability; And answer European Union and the U.S. about forbidding that containing relevant described heavy metal specified requirement in the electrolytic coating detects, and the content of European Union and U.S. food standard weight metal is: Pb≤0.010MG/DM, Cr≤0.050MG/DM, Ni≤0.020MG/DM, Cd≤0.050MG/DM.After testing, this technology meets European Union and the U.S. fully and contains the requirement of described heavy metal regulation about forbidding electrolytic coating.Containing metal cobalt and tin in the coating, the ratio between them is 1～2: change between 2～1.
Emphasis of the present invention is used in environmental-friendly lead-free not to be had nickel and does not have in the black tin-cobalt alloy electroplating bath solution of cyanogen and add special complexing agent, blackening agent, PH buffer reagent, and use by a certain percentage, reaching the promising change of above argumentation plating solution performance, is a revolution concerning relevant the plating!
The great economic benefit that the new electroplating technology that the present invention produces can produce: 1, save in a large number than the precious metal cobalt salt, the most of innovation of single Delta of the Pearl River garment accessories specialty Electroplate Factory just can be saved 300 tons in 1 year, about 5,000 ten thousand yuan (valuation in 2007).2, save a large amount of metal pink salts, the most of innovation of single clothes Delta of the Pearl River auxiliary material specialty Electroplate Factory just can be saved 80 tons in 1 year, about 1,500 ten thousand yuan (valuation in 2007).3, a large amount of potassium pyrophosphates of saving are 2000 tons, the oxygen enrichmentization and the wastewater treatment expense of anti-sealing, the most of innovation of single clothes Delta of the Pearl River auxiliary material specialty Electroplate Factory, 5,000 ten thousand yuan of saving in a year (valuation in 2007).4, stop to return goods and incur loss through delay delivery date because of " ring machine ".5, when producing the black and white mandarin duck chromatic effect of no nickel black nickel, saving plating underlayer cost, with the used bottom copper-nickel alloy of the garment accessories tin coating of outlet, the most of innovation of Delta of the Pearl River auxiliary material specialty Electroplate Factory, 20,000 ten thousand yuan of saving in a year (valuation in 2007).
The above only is this neoteric preferred embodiment, is not that patent of the present invention is done any pro forma restriction.The those of ordinary skill of all industry, but all shown in the by specification and the above, and implement this new invention patent glibly.But all those skilled in the art in not breaking away from this new invention patent scheme scope, when can utilizing the above technology contents that discloses, change, modify equal variation with differentiation and make a little, are the equivalent embodiment of patent of the present invention.Simultaneously, all substantial process according to patent of the present invention to the change of any equivalent variations that above embodiment did, modify with differentiation etc., all belong in the scope of patent scheme of the present invention.
Claims (7)
1, a kind of nickel-free ferrous tin-cobalt alloy plating solution is characterized in that, the parameter of this plating bath and each component content as follows:
Tin 0.2-6 gram/L
Cobalt 0.6-4 gram/L
Complexing agent 8-180 gram/L
Blackening agent 2-20 gram/L
PH buffer reagent 50-320 gram/L
10-25Be ° of plating bath Baume
Temperature 28-48 ℃
PH 10-13
Particularly point out and do not contain potassium pyrophosphate or sodium in this prescription.
2, a kind of nickel-free ferrous tin-cobalt alloy plating solution according to claim 1 is characterized in that: complexing agent is one or more the combination in complexone, tartrate and salt thereof, citric acid and salt thereof, acetic acid and salt thereof, phosphoric acid and salt thereof, trolamine, lactic acid, each seed amino acid and salt, quadrol, sodium hydroxide, potassium hydroxide, oxysuccinic acid and salt thereof, tartaric acid and salt thereof, carbonate, the thiocyanate-s such as ETDA.
3, a kind of nickel-free ferrous tin-cobalt alloy plating solution according to claim 1 is characterized in that: described blackening agent is a kind of in amino acid and salt, thiocyanic acid and the salt thereof.
4, a kind of nickel-free ferrous tin-cobalt alloy plating solution according to claim 3 is characterized in that: cobalt salt is one or more the combination in the cobalt salt of cobaltous carbonate, cobalt chloride, rose vitriol and complexing agent.
5, a kind of nickel-free ferrous tin-cobalt alloy plating solution according to claim 3 is characterized in that: pink salt is one or more the combination in the pink salt of tin protochloride, stannous sulfate, stannous pyrophosphate, tin methane sulfonate and complexing agent.
6, a kind of nickel-free ferrous tin-cobalt alloy plating solution according to claim 1 is characterized in that: described PH buffer reagent is one or more the combination in acetic acid and salt, tartrate and salt thereof, carbonic acid and salt thereof, phosphoric acid and salt thereof, ammoniacal liquor, trolamine, sodium tetraborate, potassium tetroxalate, citric acid and salt thereof, the quadrol.
7, a kind ofly carry out electroplating technique according to the described plating bath of claim 1, it is characterized in that: with metallic copper, brass, with electro-coppering and copper alloy, nickel, a kind of in the Cu-Sn-Zn ternary alloy is basic unit, directly use this no nickel tin-cobalt alloy plating solution, under 28～48 ℃ of temperature, use sulfuric acid, hydrochloric acid or potassium hydroxide, sodium hydroxide is regulated between PH to 11～12, this moment, metallic tin content was between 0.5～4g/L, cobalt contents is between 0.4～4g/L, between complexing agent 5～300g/L, between PH buffer reagent 5～300g/L, between blackening agent 0.1～50g/L, the plating bath degree Beaume is 10～22 °, voltage control is 3～10 volts of barrel platings, and 2～6 volts of rack platings with cathode current density are being rack plating 20～200 seconds or barrel plating 3～140 minutes under 0.1～3.5 ampere/square decimeter the situation; Plating finishes, and it is clean take out to electroplate the body and function flushing with clean water, can obtain the black of light and near black coating after drying up.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102560577A (en) * | 2012-03-08 | 2012-07-11 | 杜强 | Nickel-free black tin cobalt alloy plating solution and electroplating technology by using same |
| CN104152956A (en) * | 2014-07-22 | 2014-11-19 | 广东达志环保科技股份有限公司 | Micro-cobalt gun-color electroplating liquid and electroplating method thereof |
| CN104562107A (en) * | 2014-12-23 | 2015-04-29 | 佛山科学技术学院 | Highly-corrosion-resistant environment-friendly black tin-cobalt alloy electroplating liquid and electroplating method thereof. |
| CN105297090A (en) * | 2015-12-01 | 2016-02-03 | 张颖 | Decorative electroplating liquid for forming black alloy plating layer |
| CN106435671A (en) * | 2016-12-25 | 2017-02-22 | 苏州锆钒电子科技有限公司 | Novel tin-cobalt alloy electroplating process |
| CN108315784A (en) * | 2017-09-22 | 2018-07-24 | 贵州振华群英电器有限公司（国营第八九厂） | A kind of electrotinning cerium nickel alloy plating solution and preparation method thereof |
| CN112095129A (en) * | 2020-09-23 | 2020-12-18 | 深圳市森泰金属技术有限公司 | Copper alloy surface retro process method |
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2009
- 2009-06-15 CN CN2009100402403A patent/CN101575720B/en active Active
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102560577A (en) * | 2012-03-08 | 2012-07-11 | 杜强 | Nickel-free black tin cobalt alloy plating solution and electroplating technology by using same |
| CN104152956A (en) * | 2014-07-22 | 2014-11-19 | 广东达志环保科技股份有限公司 | Micro-cobalt gun-color electroplating liquid and electroplating method thereof |
| CN104562107A (en) * | 2014-12-23 | 2015-04-29 | 佛山科学技术学院 | Highly-corrosion-resistant environment-friendly black tin-cobalt alloy electroplating liquid and electroplating method thereof. |
| CN105297090A (en) * | 2015-12-01 | 2016-02-03 | 张颖 | Decorative electroplating liquid for forming black alloy plating layer |
| CN106435671A (en) * | 2016-12-25 | 2017-02-22 | 苏州锆钒电子科技有限公司 | Novel tin-cobalt alloy electroplating process |
| CN108315784A (en) * | 2017-09-22 | 2018-07-24 | 贵州振华群英电器有限公司（国营第八九厂） | A kind of electrotinning cerium nickel alloy plating solution and preparation method thereof |
| CN112095129A (en) * | 2020-09-23 | 2020-12-18 | 深圳市森泰金属技术有限公司 | Copper alloy surface retro process method |
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