CN103866356A - Method for non-cyanide imitation gold plating of Cu-Zn binary alloy - Google Patents
Method for non-cyanide imitation gold plating of Cu-Zn binary alloy Download PDFInfo
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- CN103866356A CN103866356A CN201210533734.7A CN201210533734A CN103866356A CN 103866356 A CN103866356 A CN 103866356A CN 201210533734 A CN201210533734 A CN 201210533734A CN 103866356 A CN103866356 A CN 103866356A
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Abstract
The invention provides a plating solution for the non-cyanide imitation gold plating of a Cu-Zn binary alloy on low carbon steel, and its use method in order to improve the problems of severe toxicity, bad anode dissolvability and high treatment cost of three wastes of cyanide-containing plating solutions and the problems of complex composition, narrow range of technological parameters and unrealistic imitation gold color of non-cyanide plating solutions in present imitation gold plating technologies. The method is characterized in that the method comprises the following steps: an activated matrix can be directly plated without cleaning, so the operation is simple; the imitation gold plating solution is composed of potassium pyrophosphate, copper sulfate, zinc sulfate and glycerin, so the imitation gold plating solution has the advantages of green property, environmental protection, good dispersity, strong homogeneous plating ability, simple composition and easy maintenance; and the prepared gold imitation plating solution can meet the requirements of the cross cut test requirements of national standard GB9286-1998 paint and varnish film; and the obtained coating is passivated and seal-protected, and the protected coating meets the 5% brine neutral salt spray test indexes of the national standard GB5938-86 Corrosion Resistance Test Method of Metal Coating and Chemical Treatment Layer of Light Industrial Product, and can be used as a decorative coating.
Description
Technical field
The present invention relates to non-cyanide imitating gold electroplating field.
Background technology
Gold is very popular with its jewelly gorgeous color, therefore gold-platedly in decorative electroplating occupies larger proportion always, but proof gold electroplate again because price of gold costliness, hardness are low, wear no resistance, its application is restricted.The existing flavous color and luster of imitation gold deposit, can meet ornamental requirement, has improved again the mechanical property such as hardness, wear resistance of coating, has also saved gold, has obvious economic benefit and vast potential for future development.But current gold simulating electroplating process is mostly take cyaniding brass-plating as main, and this technological work electric current is little, allow electroplating time short, anode dissolution poor performance, and have severe toxicity containing cyanogen plating solution, three wastes processing cost is high, if deal with not only contaminate environment improperly, also endanger people's health.United nations environment development conference in 1992 has write " cleaner production " " 21st century Inter Action agenda ".China is the formal the Law of the People's Republic of China on Promoting Clean Production of implementing in 2003 also.So development cyanideless electro-plating is significant to socioeconomic Sustainable development.
The Cyanida free imitative electrogilding solution system that development in recent years is got up has pyrophosphate salt system, tartrate system, HEDP system, citric acid system etc.These systems have the advantages such as bath stability, covering power are strong, coating color and luster is more even, can obtain having to a certain extent the imitation gold deposit of decorative effect, but all have its limitation separately: as plating solution composition is complicated, current density is narrow, not easy care of plating solution; The impacts that coating and basal body binding force are poor, color and luster is wayward, coating bright property is subject to bottom bright coating etc., are difficult to realize commercial application, cannot fundamentally replace existing prussiate imitation gold plating.
Summary of the invention
Existing Cyanida free imitative electrogilding solution composition is complicated, narrow ranges of process parameters, and simulating golden colour pool is true to nature not; And prussiate electroplating technology has severe toxicity containing cyanogen plating solution, anode dissolution poor performance, three wastes processing cost is high.The present invention provides a kind of soft steel non-cyanide imitating gold electroplating Cu-Zn binary alloy electroplate liquid and using method thereof in order to overcome the above problems.
Soft steel non-cyanide imitating gold electroplating Cu-Zn binary alloy electroplate liquid of the present invention and concrete using method thereof are carried out according to the following steps: one, according to the different requirements of effects on surface roughness, can adopt 150#, 800#, 1500#, 2000# sand papering 18AL surface of low-carbon steel, or it is carried out to polished finish, then 18AL soft steel is placed in acetone or alcohol and at room temperature processes 5min~10min with ultrasonic cleaning machine; Two, adopt concentrated hydrochloric acid to eliminate rust to 18AL soft steel, according to the difference of surface of low-carbon steel corrosion degree, the treatment time is generally 30 ~ 60s at ambient temperature; Then use deionized water rinsing; Three, be 200 ~ 350g/L by potassium pyrophosphate concentration, take potassium pyrophosphate and deionized water is mixed with activation solution, the lower treatment time of room temperature condition is 10 ~ 30s, after the activated processing of 18AL soft steel, need not clean and directly carry out luminance brightness copper; Four, press potassium pyrophosphate (K
4p
2o
7) 270g/L, cupric pyrophosphate (Cu
2p
2o
7-4H
2o) 70g/L, ammoniacal liquor 3mg/L, ultrapure water 700mg/L is mixed with the aqueous solution, and regulating pH by phosphoric acid and potassium hydroxide is 8.6 ~ 9.2, adds appropriate brightening agent and opens cylinder agent, obtains bright copper plating solution; Five, press potassium pyrophosphate (K
4p
2o
7-3H
2o) 200 ~ 300g/L, zinc sulfate (ZnSO
4-7H
2o) 40 ~ 50g/L, copper sulfate (CuSO
4-5H
2o) 2 ~ 5g/L, glycerol 10 ~ 30ml/L, 900ml ultrapure water, is mixed with the aqueous solution, and regulating pH by potassium pyrophosphate and potassium hydroxide is 8.0 ~ 8.6, obtains Cyanida free imitative electrogilding solution; Six, will in the Cyanida free imitative electrogilding solution obtaining through step 5, add H
2o
2(30%) aqueous solution 0.2 ~ 0.4m/L, it is carried out to preelectrolysis, and to remove foreign ion for subsequent use; Seven, the 18AL soft steel through step 3 processing is put in the burnt copper electrolyte of the light obtaining through step 4, at 50 ~ 55 ℃ of temperature, current density 0.8 ~ 1A/dm
2under condition, process 6 ~ 10min, 18AL soft steel is carried out to bright copper plating bottoming; Eight, the 18AL soft steel of the preplating bright copper bottoming obtaining through step 4 processing is put into through step 5 and step 6 and obtained in Cyanida free imitative electrogilding solution, at ambient temperature, current density is 0.5~1.25A/dm
2, process 90 ~ 360s, then 18AL soft steel is cleaned and dried up with distilled water, complete the non-cyanide imitating gold electroplating process to 18AL soft steel; Nine, by potassium bichromate (K
2cr
2o
4) 50g/L is mixed with the aqueous solution, is 3 ~ 4 by vinegar acid for adjusting pH, obtains cyanide-free imitation gold coating passivating solution; Ten, the 18AL soft steel with non-cyanide imitating gold electroplating layer obtaining through step 8 is put in the passivating solution obtaining through step 9, under 20 ~ 30 ℃ of conditions of temperature, Passivation Treatment 15min, with distilled water clean, dry up; 11, with shellac or acrylic acid or the like varnish coating protective film at 40 ~ 50 ℃, complete 18AL soft steel cyanide-free imitation gold technique whole process.
Soft steel non-cyanide imitating gold electroplating Cu-Zn binary alloy electroplate liquid of the present invention, the potassium pyrophosphate solution that employing concentration is 200 ~ 350g/L is to 18AL soft steel acid-wash activation, reactivation process is carried out at ambient temperature, treatment time is 10 ~ 30s, after the activated processing of 18AL soft steel, need not clean directly and electroplate.
Soft steel non-cyanide imitating gold electroplating Cu-Zn binary alloy electroplate liquid of the present invention, adopts potassium pyrophosphate (K
4p
2o
7-3H
2o) be main complexing agent, glycerol is auxiliary complex-former, copper sulfate (CuSO
4-5H
2o), zinc sulfate (ZnSO
4-7H
2o) be main salt, prepare with ultrapure water, utilize this aqueous solution to carry out non-cyanide imitating gold electroplating to 18AL soft steel, there is electroplate liquid good dispersity, degree of depth ability is strong, covering power good, specific conductivity is moderate, composition is simple, be convenient to the features such as maintenance, and to not using toxic substance, environmental protection in the imitation gold plating process of 18AL soft steel.
Soft steel non-cyanide imitating gold electroplating Cu-Zn binary alloy electroplate liquid of the present invention, electroplate liquid consists of: potassium pyrophosphate concentration is 200 ~ 300g/L, and zinc sulfate concentration is 40 ~ 50g/L, and concentration of copper sulfate is 2 ~ 5g/L, glycerol concentration is 5 ~ 20ml/L, and ultrapure water content is 900ml.When potassium pyrophosphate content is too low, coating is yellow-green colour; When zinc sulfate content is too low, coating color and luster is inhomogeneous, and the place that current density is little is golden red.When copper too high levels, coating is golden red.
Soft steel non-cyanide imitating gold electroplating Cu-Zn binary alloy electroplate liquid of the present invention, must remain on certain pH value scope could stably manufactured.Adopting phosphoric acid, potassium hydroxide is plating solution pH adjusting agent, makes pH remain on 8.0 ~ 8.6.When pH is too low, coating is golden red; When pH is too high, Deposit appearance color and luster is yellow-green colour.
Soft steel non-cyanide imitating gold electroplating Cu-Zn binary alloy electroplate liquid of the present invention, must add 0.2 ~ 0.4m/L H before use
2o
2(30%), Cyanida free imitative electrogilding solution is carried out to preelectrolysis and remove foreign ion, otherwise coating blackout.
Soft steel non-cyanide imitating gold electroplating Cu-Zn binary alloy electrolytic solution of the present invention, concrete compound method is as follows: (1) is dissolved in potassium pyrophosphate in 900mL ultrapure water; (2) in continuous whipping process, zinc sulfate is joined in batches in the potassium pyrophosphate solution having prepared, until it dissolves completely; (3), constantly stirring, under heated condition, copper sulfate is joined in the solution that step 2 prepares, bath temperature is controlled at 40 ~ 60 ℃, until it dissolves completely; (4), under the state constantly stirring, glycerol is joined in the solution that step 3 prepares, until it is uniformly dispersed; (5) pass through phosphoric acid, the potassium hydroxide regulating step 4 electrolytic solution pH for preparing 8.0 ~ 8.6; (6) in step 5 obtain solution, add 0.2 ~ 0.4m/L H
2o
2(30%), under low current density, electrolysis 4 ~ 6h removes the laggard electroplating of foreign ion.
Soft steel non-cyanide imitating gold electroplating Cu-Zn binary alloy electroplate liquid of the present invention must just can obtain color and luster true to nature in certain processing range, has the imitation gold deposit of decorative effect.Processing condition are: at ambient temperature, current density is 0.5 ~ 1.25A/dm
2, process 90 ~ 360s.
Soft steel non-cyanide imitating gold electroplating Cu-Zn binary alloy electroplate liquid of the present invention just can carry out ornamental imitation gold plating after 18AL surface of low-carbon steel carries out the processing of preplating bright copper; Imitation gold plating process adopts pneumatic blending or movable cathode, to guarantee that electroplate liquid is uniformly dispersed and eliminates concentration polarization.
Soft steel non-cyanide imitating gold electroplating Cu-Zn binary alloy electroplate liquid of the present invention, does not carry out can obtaining equally the golden yellow imitation gold deposit of class under the processing of preplating bright copper at 18AL surface of low-carbon steel, sees accompanying drawing 1.
Soft steel non-cyanide imitating gold electroplating Cu-Zn binary alloy electroplate liquid of the present invention, by soft steel is carried out after gold simulating electroplating process processing, can obtain the golden yellow coating of one deck class 18 ~ 24K gold at 18AL surface of low-carbon steel, imitative golden effect is true to nature, alternative prussiate imitation gold deposit, see accompanying drawing 2, and this imitation gold deposit comes off without coating through pliability test; The requirement of the cross cut test that meets standard GB/T 9286-1998 paint and varnish paint film to decorative metals coating.
Soft steel non-cyanide imitating gold electroplating Cu-Zn binary alloy electroplate liquid of the present invention; make cyanide-free imitation gold coating through passivation; after shellac, acrylic acid or the like, epoxy resin varnish closed protective, corrosion resisting property is good, meets the 5% salt solution neutral salt spray test index of standard GB/T 5938-86 " the Kesternich test method of light industrial goods metal plating and chemical treatment layer ".
Accompanying drawing explanation
Fig. 1: directly carry out non-cyanide imitating gold electroplating design sketch at 18AL surface of low-carbon steel.
Fig. 2: 18AL soft steel is first carried out to the bottoming of preplating bright copper, then carry out non-cyanide imitating gold electroplating design sketch.
Embodiment
Embodiment mono-
The soft steel non-cyanide imitating gold electroplating Cu-Zn binary alloy electroplate liquid of present embodiment and concrete using method thereof are carried out according to the following steps: one, according to the different requirements of effects on surface roughness, can adopt 150#, 800#, 1500#, 2000# sand papering 18AL surface of low-carbon steel, or it is carried out to polished finish, then 18AL soft steel is placed in acetone or alcohol and at room temperature processes 5min ~ 10min with ultrasonic cleaning machine; Two, adopt concentrated hydrochloric acid to eliminate rust to 18AL soft steel, according to the difference of surface of low-carbon steel corrosion degree, the treatment time is generally 30 ~ 60s at ambient temperature; Then use deionized water rinsing; Three, be 250g/L by potassium pyrophosphate concentration, take potassium pyrophosphate and deionized water is mixed with activation solution, the lower treatment time of room temperature condition is 20s, after the activated processing of 18AL soft steel, need not clean and directly carry out luminance brightness copper; Four, press potassium pyrophosphate (K
4p
2o
7) 270g/L, cupric pyrophosphate (Cu
2p
2o
7-4H
2o) 70g/L, ammoniacal liquor 3mg/L, ultrapure water 700mg/L is mixed with the aqueous solution, and regulating pH by phosphoric acid and potassium hydroxide is 8.6, adds appropriate brightening agent and opens cylinder agent, obtains bright copper plating solution; Five, press potassium pyrophosphate (K
4p
2o
7-3H
2o) 200g/L, zinc sulfate (ZnSO
4-7H
2o) 42g/L, copper sulfate (CuSO
4-5H
2o) 2.6g/L, glycerol 8ml/L, 900ml ultrapure water, is mixed with the aqueous solution, and regulating pH by potassium pyrophosphate and potassium hydroxide is 8.2, obtains Cyanida free imitative electrogilding solution; Six, will in the cyanide-free imitation gold electrolytic solution obtaining through step 5, add H
2o
2(30%) aqueous solution 0.2m/L, it is carried out to preelectrolysis, and to remove foreign ion for subsequent use; Seven, the 18AL soft steel through step 3 processing is put in the burnt copper electrolyte of the light obtaining through step 4, at temperature 50 C, current density 0.8A/dm
2under condition, process 6 ~ 10min, 18AL soft steel is carried out to bright copper plating bottoming; Eight, the 18AL soft steel of the preplating bright copper bottoming obtaining through step 7 processing is put into through step 5 and step 6 and obtained in Cyanida free imitative electrogilding solution, at ambient temperature, current density is 0.8A/dm
2, process 180s, then 18AL soft steel is cleaned and dried up with distilled water, complete the non-cyanide imitating gold electroplating process to 18AL soft steel; Nine, by potassium bichromate (K
2cr
2o
4) 50g/L is mixed with the aqueous solution, is 3 ~ 4 by vinegar acid for adjusting pH, obtains cyanide-free imitation gold coating passivating solution; Ten, the 18AL soft steel with non-cyanide imitating gold electroplating layer obtaining through step 8 is put in the passivating solution obtaining through step 9, under 20 ~ 30 ℃ of conditions of temperature, Passivation Treatment 15min, with distilled water clean, dry up; 11, with shellac or acrylic acid or the like varnish coating protective film at 40 ℃, complete 18AL soft steel cyanide-free imitation gold technique whole process.
Embodiment bis-
The present embodiment is different from embodiment mono-: in step 3, potassium pyrophosphate concentration is 200g/L, and reactivation process is carried out at ambient temperature, and the treatment time is 30s.Other are identical with embodiment mono-.
Embodiment tri-
The present embodiment is different from embodiment mono-or two: in step 3, potassium pyrophosphate concentration is 300g/L, and reactivation process is carried out at ambient temperature, and the treatment time is 10s.Other are identical with embodiment mono-or two.
Embodiment tetra-
The present embodiment is different from one of embodiment mono-to three: in step 5, potassium pyrophosphate concentration is 200g/L, and zinc sulfate concentration is 42g/L, and concentration of copper sulfate is 3.0g/L, and glycerol concentration is 10ml/L, and ultrapure water content is 900ml.Other are identical with one of embodiment mono-to three.
Embodiment five
The present embodiment is different from one of embodiment mono-to four: in step 5, potassium pyrophosphate concentration is 250g/L, and zinc sulfate concentration is 42g/L, and concentration of copper sulfate is 2.4g/L, and glycerol concentration is 10ml/L, and ultrapure water content is 900ml.Other are identical with one of embodiment mono-to four.
Embodiment six
The present embodiment is different from one of embodiment mono-to five: in step 5, electrolytic solution pH remains on 8.0.Other are identical with embodiment mono-to five.
Embodiment seven
The present embodiment is different from one of embodiment mono-to six: H in step 6
2o
2(30%) concentration is 0.3m/L, and other are identical with one of embodiment mono-to six.
Embodiment eight
The present embodiment is different from one of embodiment mono-to seven: in step 8, non-cyanide imitating gold electroplating processing condition are, at 20 ~ 50 ℃ of temperature, current density is 0.8A/dm
2, process 60 ~ 600s.Other are identical with one of specific embodiment one to seven.
Embodiment nine
The present embodiment is different from one of embodiment mono-to eight: non-cyanide imitating gold electroplating processing condition are, at 20 ~ 50 ℃ of temperature, current density is 1.2A/dm
2, process 120s.Other are identical with one of embodiment mono-to eight.
Embodiment ten
The present embodiment is different from one of embodiment mono-to nine: non-cyanide imitating gold electroplating can directly apply to surface of low-carbon steel without bottoming coating.Other are identical with one of embodiment mono-to nine.
Claims (7)
1. the method for non-cyanide imitating gold electroplating Cu-Zn binary alloy on soft steel, is characterized in that adopting potassium pyrophosphate solution to carry out activation treatment to 18AL soft steel, need not clean and directly carry out imitation gold plating after processing; In Cyanida free imitative electrogilding solution system, adopting potassium pyrophosphate is main complexing agent, and glycerol is auxiliary complex-former, and copper sulfate, zinc sulfate are main salt, and phosphoric acid, potassium hydroxide are pH adjusting agent; Non-cyanide imitating gold electroplating process is: 18AL soft steel sanding and polishing → degreasing and rust removal → activation treatment → bright copper plating → imitation gold plating → Passivation Treatment → coating protective, and concrete operations are as follows:
(1) sanding and polishing: according to the different requirements of effects on surface roughness, can adopt 150#, 800#, 1500#, 2000# sand papering 18AL surface of low-carbon steel, or it is carried out to polished finish;
(2) degreasing and rust removal: 18AL soft steel is placed in acetone or alcohol and at room temperature processes 5min ~ 10min with ultrasonic cleaning machine; Then adopt concentrated hydrochloric acid to eliminate rust to 18AL soft steel, according to the difference of surface of low-carbon steel corrosion degree, the treatment time is generally 30 ~ 60s at ambient temperature; Then use deionized water rinsing;
(3) activation treatment: be 200 ~ 350g/L by potassium pyrophosphate concentration, take potassium pyrophosphate, be mixed with activation solution with deionized water, under room temperature condition, soak time is 10 ~ 30s, need not clean and directly carry out bright copper plating after the activated processing of 18AL soft steel;
(4) bright copper plating: press potassium pyrophosphate (K
4p
2o
7) 270g/L, cupric pyrophosphate (Cu
2p
2o
7-4H
2o) 70g/L, ammoniacal liquor 3mg/L, ultrapure water 700mg/L is mixed with the aqueous solution, and regulating pH by phosphoric acid and potassium hydroxide is 8.6 ~ 9.2, adds appropriate brightening agent and opens cylinder agent, obtains bright copper plating liquid; To put in the burnt copper electrolyte of this light, at 50 ~ 55 ℃ of temperature, current density 0.8 ~ 1A/dm through step (3) 18AL soft steel after treatment
2under condition, process 6 ~ 10min, 18AL soft steel is carried out to bright copper plating bottoming;
(5) imitation gold plating: press potassium pyrophosphate (K
4p
2o
7-3H
2o) 200 ~ 300g/L, zinc sulfate (ZnSO
4-7H
2o) 40 ~ 50g/L, copper sulfate (CuSO
4-5H
2o) 2 ~ 5g/L, glycerol 10 ~ 30ml/L, 900ml ultrapure water, is mixed with the aqueous solution, and regulating pH by potassium pyrophosphate and potassium hydroxide is 8.0 ~ 8.6, obtains Cyanida free imitative electrogilding solution; Then add H
2o
2(30%) aqueous solution 0.2 ~ 0.4m/L, it is carried out to preelectrolysis, and to remove foreign ion for subsequent use; The 18AL soft steel of processing the preplating bright copper bottoming obtaining through step (4) is put in the Cyanida free imitative electrogilding solution after preelectrolysis, and at ambient temperature, current density is 0.5 ~ 1.25A/dm
2, process 90 ~ 360s, then 18AL soft steel is cleaned and dried up with distilled water, complete the non-cyanide imitating gold electroplating process to 18AL soft steel;
(6) Passivation Treatment: by potassium bichromate (K
2cr
2o
4) 50g/L is mixed with the aqueous solution, is 3 ~ 4 by vinegar acid for adjusting pH, obtains cyanide-free imitation gold coating passivating solution; The 18AL soft steel with imitation gold deposit obtaining is put in this passivating solution, under 20 ~ 30 ℃ of conditions of temperature, Passivation Treatment 15min, with distilled water clean, dry up;
(7) coating protective: with shellac or acrylic acid or the like varnish coating protective film at 40 ~ 50 ℃, complete 18AL soft steel cyanide-free imitation gold technique whole process.
2. soft steel non-cyanide imitating gold electroplating Cu-Zn binary alloy method according to claim 1, it is characterized in that in step (3), potassium pyrophosphate concentration is 250g/L, reactivation process is carried out at ambient temperature, treatment time is 10 ~ 30s, after the activated processing of 18AL soft steel, need not clean and directly carry out bright copper plating.
3. soft steel non-cyanide imitating gold electroplating Cu-Zn binary alloy method according to claim 1, it is characterized in that in Cyanida free imitative electrogilding solution, adopting potassium pyrophosphate is main complexing agent, glycerol is auxiliary complex-former, and copper sulfate, zinc sulfate are main salt, and phosphoric acid, potassium hydroxide are pH adjusting agent.
4. soft steel non-cyanide imitating gold electroplating Cu-Zn binary alloy method according to claim 1, is characterized in that step (4) bright copper plating is to operate at ambient temperature, and current density is 0.8 ~ 1A/dm
2, the treatment time is 360s.
5. soft steel non-cyanide imitating gold electroplating Cu-Zn binary alloy method according to claim 1, it is characterized in that in step (5), potassium pyrophosphate concentration is 200 ~ 300g/L, zinc sulfate concentration is 40 ~ 50g/L, concentration of copper sulfate is 2 ~ 5g/L, glycerol concentration is 5 ~ 20ml/L, ultrapure water content is 900ml, and regulating Cyanida free imitative electrogilding solution pH by potassium pyrophosphate and potassium hydroxide is 8.0 ~ 8.6.
6. soft steel non-cyanide imitating gold electroplating Cu-Zn binary alloy method according to claim 1, is characterized in that needing to carry out the processing of electroplating bright copper substrate before ornamental non-cyanide imitating gold electroplating.
7. soft steel non-cyanide imitating gold electroplating Cu-Zn binary alloy method according to claim 1, is characterized in that non-cyanide imitating gold electroplating can directly apply to surface of low-carbon steel without bottoming processing.
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JP2018119169A (en) * | 2017-01-23 | 2018-08-02 | 学校法人関東学院 | Electroplating solution, electroplating method and electroplating film |
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