CN104480501A - High-tin copper-tin alloy electroplating solution and process for barrel plating - Google Patents
High-tin copper-tin alloy electroplating solution and process for barrel plating Download PDFInfo
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- CN104480501A CN104480501A CN201410712640.5A CN201410712640A CN104480501A CN 104480501 A CN104480501 A CN 104480501A CN 201410712640 A CN201410712640 A CN 201410712640A CN 104480501 A CN104480501 A CN 104480501A
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- tin
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- barrel plating
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D3/00—Electroplating: Baths therefor
- C25D3/02—Electroplating: Baths therefor from solutions
- C25D3/56—Electroplating: Baths therefor from solutions of alloys
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D3/00—Electroplating: Baths therefor
- C25D3/02—Electroplating: Baths therefor from solutions
- C25D3/56—Electroplating: Baths therefor from solutions of alloys
- C25D3/58—Electroplating: Baths therefor from solutions of alloys containing more than 50% by weight of copper
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D3/00—Electroplating: Baths therefor
- C25D3/02—Electroplating: Baths therefor from solutions
- C25D3/56—Electroplating: Baths therefor from solutions of alloys
- C25D3/60—Electroplating: Baths therefor from solutions of alloys containing more than 50% by weight of tin
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
Abstract
The invention discloses a high-tin copper-tin alloy electroplating solution for barrel plating. The solution is characterized by comprising pyrophosphate which is used as a complexing agent, monopotassium phosphate which is used as conducting salt, soluble copper salt and soluble tin salt which are used as main salts, phosphoric acid and potassium hydroxide which are used as a pH regulator of the electroplating solution, a stabilizer of the electroplating solution, and an appropriate amount of compound additives, wherein the concentration of pyrophosphate is 100-350g/L, the concentration of monopotassium phosphate is 40-120g/L, the concentration of the copper salt is 3-20g/L, the concentration of the tin salt is 3-20g/L, the concentration of the stabilizer is 1-12g/L, and the concentration of the compound additives is 1-20ml/L. The electroplating solution disclosed by the invention is simple in component, easy to maintain and applicable to a wide current density range; a plating is bright; a bright high-tin copper-tin alloy plating with a good matrix bonding force can be obtained in a manner of barrel plating.
Description
Technical field
The present invention relates to electroplating technology field, especially relate to a kind of high tin gunmetal electroplate liquid and the technique that are specifically designed to barrel plating.
Background technology
Cu-sn alloy coating, because of low, the good non-proliferation performance of its electroplating cost, is the optimal selection for nickel, joint nickel coating in numerous plating Application Areass.Traditional electroplating copper tin alloy technique is cyanide solution system, has huge damaging effect to human body and environment, and for meeting the Sustainable development requirement of Future Society, the concern that cyanideless electro-plating gunmetal technique is just more and more subject to people is held in both hands with heat.The stanniferous amount of high tin gunmetal is comparatively large, easy polishing, and polishing back reflection rate is high, and hardness is between nickel, chromium; In air, oxidation resistance is strong, and along with the increase of Theil indices in coating, the anti-corrosion capability of coating also increases thereupon.
In addition, different from rack plating, barrel plating is used for light and thin type miniature workpiece, and workpiece is complicated, often occurs that current efficiency is low, and the coating obtaining equal thickness needs the time long, and the problem such as bonding force is bad.Body series uses complex additive effectively to improve these problems, and is weakly alkaline plating system, and little to equipment corrosion, waste water easily processes, and greatly reduces the harm of environment.
Summary of the invention
The one that object of the present invention is exactly deficiency in order to solve prior art and provides is crossed liquid and is stablized, and waste liquid easy to handle height tin gunmetal electroplate liquid.
Another object of the present invention is to provide a kind of basic solution and is specifically designed to barrel plating height tin gunmetal electroplating technology.
The present invention adopts following technical solution to realize above-mentioned purpose: a kind of high tin gunmetal electroplate liquid for barrel plating, it is characterized in that, described solution comprises the pyrophosphate salt as complexing agent, as the potassium primary phosphate of conducting salt, as soluble copper salt, the solubility pink salt of main salt, as phosphoric acid and the potassium hydroxide of plating solution PH adjusting agent, bath stability agent and appropriate complex additive;
Described pyrophosphate salt concentration is 100-350g/L, potassium primary phosphate 40-120g/L, and mantoquita concentration is 3-20g/L, and pink salt concentration is 3-20g/L, and stabilizer concentration is 1-12g/L, and described complex additive concentration is 1-20ml/L.
Further illustrating as such scheme, described pyrophosphate salt is the one in potassium pyrophosphate, trisodium phosphate.
Described soluble copper salt adopts at least one to be selected from following material: cupric pyrophosphate, copper sulfate, cupric chloride, copper methane sulfonate, neutralized verdigris, thionamic acid copper, 2-hydroxy-propanesulfonic acid copper.
Described solubility pink salt adopts at least one to be selected from following material: the sub-tin of stannous pyrophosphate, stannous sulfate, tin protochloride, stannous fluoboric acid, 2-hydroxy-propanesulfonic acid, the sub-tin of alkylsulphonic acid.
Described additive is following three kinds of additive compound: first kind A is amine, comprise a kind of, the two kinds or more of material being selected from following material or condensation and obtaining: ammonia, dimethylamine, quadrol, dimethylaminopropylamine, diethylenetriamine, Tri N-Propyl Amine, α-amino isopropyl alcohol, trolamine, tetraethylene pentamine, hexamethylene-diamine, vulkacit H, piperazine, imidazoles; Equations of The Second Kind B is sulfur-bearing compounds, comprises a kind of, the two kinds or more of material being selected from following material or condensation and obtaining: between thiosalicylic acid, butyl or isopropyl xanthan hydrochlorate, 2-[4-morpholinodithio sulfonic acid, thiosinamine, bismuth ketone, dimethylamino phenmethyl rhodamine, methylthiourea, two pyridines, rubeanic acid, sulfo-malonyl-are for urea; 3rd class C is the condenses of amine and epoxy compounds, and amine is the material that the first additive may comprise, and epoxy compounds is oxyethane, propylene oxide, epoxy chloropropane, epoxy resin.
Described stablizer is the compound containing two hydroxyls, comprises the one in Resorcinol, pyrocatechol, Resorcinol, 2-Naphthol, xitix, citric acid, hydroxy benzenesulfonic acid.
An electroplating technology for barrel plating height tin gunmetal, is characterized in that, described ultrasonic oil removal adopts HN-E10 electrolytic degreasing powder 50-70g/L, and temperature remains on 65-85 DEG C; Electrochemical deoiling adopts the powerful degreasing powder 40-60g/L of HN-132, and temperature remains on 50-80 DEG C; Acid pickling and rust removing process is carry out in the solution environmental of φ (HCl)=15-25% in concentration; Weak acid reactivation process is carried out under the solution environmental of φ (HCl)=3-8%; Passivation adopts 25-35g/L K
2crO
4carry out in solution, temperature is 55-65 DEG C, passivation time 15-30s;
In described electroplate liquid, cathode current density is 0.2-3A/dm
2, the temperature of electroplate liquid controls to control at 8.0-9.0 at 15-35 DEG C, PH, drum rotational speed 15r/min, circulating filtration, and plating 1min-3h all can obtain the high tin cu-sn alloy coating of light.
The beneficial effect that the present invention adopts above-mentioned technical solution to reach is:
Electroplating solution component of the present invention is simple, is easy to safeguard, is applicable to wider current density range, and coating light, can obtain the high tin cu-sn alloy coating of the light good with basal body binding force.
Accompanying drawing explanation
Fig. 1 is high tin cu-sn alloy coating scanning electron microscope (SEM) figure of the present invention;
Fig. 2 is the EDS collection of illustrative plates of high tin cu-sn alloy coating;
Fig. 3 is the product schematic diagram before barrel plating;
Fig. 4 is the product schematic diagram after barrel plating.
Embodiment
A kind of high tin gunmetal electroplate liquid for barrel plating of the present invention, described solution comprises the pyrophosphate salt as complexing agent, as the potassium primary phosphate of conducting salt, as soluble copper salt, the solubility pink salt of main salt, as phosphoric acid and potassium hydroxide, bath stability agent and the appropriate complex additive of plating solution PH adjusting agent.In plating solution, phosphoric acid salt is the one in potassium pyrophosphate, trisodium phosphate.Soluble copper salt adopts at least one to be selected from following material: cupric pyrophosphate, copper sulfate, cupric chloride, copper methanesulfonate, neutralized verdigris, thionamic acid copper, 2-hydroxy-propanesulfonic acid copper.Solubility pink salt adopts at least one to be selected from following material: the sub-tin of stannous pyrophosphate, stannous sulfate, tin protochloride, stannous fluoboric acid, 2-hydroxy-propanesulfonic acid, the sub-tin of alkylsulphonic acid.Additive is three kinds of additive compound: first kind A is amine, comprise a kind of, the two kinds or more of material being selected from following material or condensation and obtaining: ammonia, dimethylamine, quadrol, dimethylaminopropylamine, diethylenetriamine, Tri N-Propyl Amine, α-amino isopropyl alcohol, trolamine, tetraethylene pentamine, hexamethylene-diamine, vulkacit H, piperazine, imidazoles; Equations of The Second Kind B is sulfur-bearing compounds, comprises a kind of, the two kinds or more of material being selected from following material or condensation and obtaining: between thiosalicylic acid, butyl or isopropyl xanthan hydrochlorate, 2-[4-morpholinodithio sulfonic acid, thiosinamine, bismuth ketone, dimethylamino phenmethyl rhodamine, methylthiourea, two pyridines, rubeanic acid, sulfo-malonyl-are for urea; 3rd class C is the condenses of amine and epoxy compounds, and amine is the material that the first additive may comprise, and epoxy compounds is oxyethane, propylene oxide, epoxy chloropropane, epoxy resin.Stablizer is the compound containing two hydroxyls, comprises the one in Resorcinol, pyrocatechol, Resorcinol, 2-Naphthol, xitix, citric acid, hydroxy benzenesulfonic acid.
Below in conjunction with specific embodiment, technical scheme of the present invention is explained in detail.
Embodiment 1
In the present embodiment, for the high tin gunmetal electroplate liquid of barrel plating, the system component of this solution is as follows:
| Potassium pyrophosphate | 200g/L |
| Neutralized verdigris | 10g/L |
| Stannous sulfate | 14g/L |
| Stablizer | 1.0g/L |
| Conducting salt | 40g/L |
| Additive A | 1mL/L |
| Additive B | 2.4mL/L |
| Addition of C | 1.2mL/L |
Wherein, the electroplating technology of barrel plating height tin gunmetal, below anticathode metal base treating processes: base material-ultrasonic oil removal (HN-E10 electrolytic degreasing powder 50 ~ 70g/L, 65 ~ 85 DEG C)--acid pickling and rust removing [φ (HCl)=20%]-rinses--washing-weak acid activation [φ (HCl)=5%]-washing-barrel plating height tin gunmetal-washing-passivation (30g/L K to-flushing-electrochemical deoiling (the powerful degreasing powder 40 ~ 60g/L of HN-132,50 ~ 80 DEG C) in flushing
2crO
4, temperature 60 C, passivation time 15 ~ 30s) and-washing-oven dry-finished product.In described electroplate liquid, cathode current density is 0.2-3A/dm
2, the temperature of electroplate liquid controls to control at 8.0-9.0 at 15-35 DEG C, PH, drum rotational speed 15r/min, circulating filtration, and plating 1min-3h all can obtain the high tin cu-sn alloy coating of light.
Embodiment 2
In the present embodiment, for the high tin gunmetal electroplate liquid of barrel plating, the system component of this solution is as follows:
| Potassium pyrophosphate | 200g/L |
| Cupric pyrophosphate | 10g/L |
| Tin protochloride | 14g/L |
| Stablizer | 2.0g/L |
| Conducting salt | 75g/L |
| Additive A | 3.2mL/L |
| Additive B | 1.0mL/L |
| Addition of C | 2.8mL/L |
Embodiment 3
In the present embodiment, for the high tin gunmetal electroplate liquid of barrel plating, the system component of this solution is as follows:
| Potassium pyrophosphate | 100g/L |
| Copper sulfate | 10g/L |
| Stannous pyrophosphate | 18g/L |
| Stablizer | 6g/L |
| Conducting salt | 100g/L |
| Additive A | 4.0mL/L |
| Additive B | 0.8mL/L |
| Addition of C | 0.6mL/L |
Embodiment 4
In the present embodiment, for the high tin gunmetal electroplate liquid of barrel plating, the system component of this solution is as follows:
| Potassium pyrophosphate | 250g/L |
| Cupric chloride | 15g/L |
| Stannous pyrophosphate | 13g/L |
| Stablizer | 10g/L |
| Conducting salt | 60g/L |
| Additive A | 0.4mL/L |
| Additive B | 4.8mL/L |
| Addition of C | 1.6mL/L |
Embodiment 5
In the present embodiment, for the high tin gunmetal electroplate liquid of barrel plating, the system component of this solution is as follows:
| Potassium pyrophosphate | 180g/L |
| Neutralized verdigris | 15g/L |
| Stannous pyrophosphate | 8g/L |
| Stablizer | 8g/L |
| Conducting salt | 120g/L |
| Additive A | 0.6mL/L |
| Additive B | 0.4mL/L |
| Addition of C | 1.2mL/L |
As Figure 1-Figure 2, to be thickness the be high tin cu-sn alloy coating of 5 μm, its EDS collection of illustrative plates shows that in coating, each element weight percent is: C 0.34%, O 1.87%, Fe 1.24%, Cu48.01%, Sn 48.54%; Composition graphs 3 and 4, the product coating adopting plating solution of the present invention and electroplating technology to obtain light, can obtain the high tin cu-sn alloy coating of the light good with basal body binding force.
Above-described is only the preferred embodiment of the present invention, it should be pointed out that for the person of ordinary skill of the art, and without departing from the concept of the premise of the invention, can also make some distortion and improvement, these all belong to protection scope of the present invention.
Claims (7)
1. the high tin gunmetal electroplate liquid for barrel plating, it is characterized in that, described solution comprises the pyrophosphate salt as complexing agent, as the potassium primary phosphate of conducting salt, as soluble copper salt, the solubility pink salt of main salt, as phosphoric acid and the potassium hydroxide of plating solution PH adjusting agent, bath stability agent and appropriate complex additive;
Described pyrophosphate salt concentration is 100-350g/L, potassium primary phosphate 40-120g/L, and mantoquita concentration is 3-20g/L, and pink salt concentration is 3-20g/L, and stabilizer concentration is 1-12g/L, and described complex additive concentration is 1-20ml/L.
2. the high tin gunmetal electroplate liquid for barrel plating according to claim 1, it is characterized in that, described pyrophosphate salt is the one in potassium pyrophosphate, trisodium phosphate.
3. the high tin gunmetal electroplate liquid for barrel plating according to claim 1, it is characterized in that, described soluble copper salt adopts at least one to be selected from following material: cupric pyrophosphate, copper sulfate, cupric chloride, copper methane sulfonate, neutralized verdigris, thionamic acid copper, 2-hydroxy-propanesulfonic acid copper.
4. the high tin gunmetal electroplate liquid for barrel plating according to claim 1, it is characterized in that, described solubility pink salt adopts at least one to be selected from following material: the sub-tin of stannous pyrophosphate, stannous sulfate, tin protochloride, stannous fluoboric acid, 2-hydroxy-propanesulfonic acid, the sub-tin of alkylsulphonic acid.
5. the high tin gunmetal electroplate liquid for barrel plating according to claim 1, it is characterized in that, described additive is following three kinds of additive compound: first kind A is amine, comprise a kind of, the two kinds or more of material being selected from following material or condensation and obtaining: ammonia, dimethylamine, quadrol, dimethylaminopropylamine, diethylenetriamine, Tri N-Propyl Amine, α-amino isopropyl alcohol, trolamine, tetraethylene pentamine, hexamethylene-diamine, vulkacit H, piperazine, imidazoles; Equations of The Second Kind B is sulfur-bearing compounds, comprises a kind of, the two kinds or more of material being selected from following material or condensation and obtaining: between thiosalicylic acid, butyl or isopropyl xanthan hydrochlorate, 2-[4-morpholinodithio sulfonic acid, thiosinamine, bismuth ketone, dimethylamino phenmethyl rhodamine, methylthiourea, two pyridines, rubeanic acid, sulfo-malonyl-are for urea; 3rd class C is the condenses of amine and epoxy compounds, and amine is the material that the first additive may comprise, and epoxy compounds is oxyethane, propylene oxide, epoxy chloropropane, epoxy resin.
6. the high tin gunmetal electroplate liquid for barrel plating according to claim 1, it is characterized in that, described stablizer is the compound containing two hydroxyls, comprises the one in Resorcinol, pyrocatechol, Resorcinol, 2-Naphthol, xitix, citric acid, hydroxy benzenesulfonic acid.
7. one kind utilizes the electroplating technology of the electroplate liquid barrel plating height tin gunmetal as described in claim 1-6 any one, it is characterized in that, its anticathode metal base treatment process process comprises: base material-ultrasonic oil removal-flushing-electrochemical deoiling-flushing-acid pickling and rust removing-flushing-washing-weak acid activation-washing-barrel plating height tin gunmetal-washing-passivation-washing-oven dry-finished product;
Described ultrasonic oil removal adopts HN-E10 electrolytic degreasing powder 50-70g/L, and temperature remains on 65-85 DEG C; Electrochemical deoiling adopts the powerful degreasing powder 40-60g/L of HN-132, and temperature remains on 50-80 DEG C; Acid pickling and rust removing process is carry out in the solution environmental of φ (HCl)=15-25% in concentration; Weak acid reactivation process is carried out under the solution environmental of φ (HCl)=3-8%; Passivation adopts 25-35g/L K
2crO
4carry out in solution, temperature is 55-65 DEG C, passivation time 15-30s;
In described electroplate liquid, cathode current density is 0.2-3A/dm
2, the temperature of electroplate liquid controls to control at 8.0-9.0 at 15-35 DEG C, PH, drum rotational speed 15r/min, circulating filtration, and plating 1min-3h all can obtain the high tin cu-sn alloy coating of light.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410712640.5A CN104480501A (en) | 2014-11-28 | 2014-11-28 | High-tin copper-tin alloy electroplating solution and process for barrel plating |
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|---|---|---|---|
| CN201410712640.5A CN104480501A (en) | 2014-11-28 | 2014-11-28 | High-tin copper-tin alloy electroplating solution and process for barrel plating |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107799291A (en) * | 2017-10-22 | 2018-03-13 | 苏州南尔材料科技有限公司 | A kind of preparation method of the manganese bismuth permanent-magnet material with electrodeposited coating |
| CN111893530A (en) * | 2020-08-07 | 2020-11-06 | 广州三孚新材料科技股份有限公司 | Cyanide-free cupronickel-tin electroplating solution and preparation method thereof |
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|---|---|---|---|---|
| EP1146148A2 (en) * | 2000-04-14 | 2001-10-17 | Nihon New Chrome Co. Ltd. | Cyanide-free pyrophosphoric acid bath for use in copper-tin alloy plating |
| US20020166774A1 (en) * | 1999-12-10 | 2002-11-14 | Shipley Company, L.L.C. | Alloy composition and plating method |
| CN102953098A (en) * | 2012-11-20 | 2013-03-06 | 广东致卓精密金属科技有限公司 | Electroplating solution and process for electroplating white copper tin by alkaline solution |
| CN104152955A (en) * | 2014-07-17 | 2014-11-19 | 广东致卓精密金属科技有限公司 | Plating solution and process for electroplating and brightening white copper-tin by using alkaline solution |
-
2014
- 2014-11-28 CN CN201410712640.5A patent/CN104480501A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20020166774A1 (en) * | 1999-12-10 | 2002-11-14 | Shipley Company, L.L.C. | Alloy composition and plating method |
| EP1146148A2 (en) * | 2000-04-14 | 2001-10-17 | Nihon New Chrome Co. Ltd. | Cyanide-free pyrophosphoric acid bath for use in copper-tin alloy plating |
| CN102953098A (en) * | 2012-11-20 | 2013-03-06 | 广东致卓精密金属科技有限公司 | Electroplating solution and process for electroplating white copper tin by alkaline solution |
| CN104152955A (en) * | 2014-07-17 | 2014-11-19 | 广东致卓精密金属科技有限公司 | Plating solution and process for electroplating and brightening white copper-tin by using alkaline solution |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107799291A (en) * | 2017-10-22 | 2018-03-13 | 苏州南尔材料科技有限公司 | A kind of preparation method of the manganese bismuth permanent-magnet material with electrodeposited coating |
| CN111893530A (en) * | 2020-08-07 | 2020-11-06 | 广州三孚新材料科技股份有限公司 | Cyanide-free cupronickel-tin electroplating solution and preparation method thereof |
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Application publication date: 20150401 |