CN101665964A - Environment-friendly imitation gold plating production technology - Google Patents
Environment-friendly imitation gold plating production technology Download PDFInfo
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- CN101665964A CN101665964A CN200910187608A CN200910187608A CN101665964A CN 101665964 A CN101665964 A CN 101665964A CN 200910187608 A CN200910187608 A CN 200910187608A CN 200910187608 A CN200910187608 A CN 200910187608A CN 101665964 A CN101665964 A CN 101665964A
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- pyrophosphate
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Abstract
Environment-friendly imitation gold plating production technology aims at solving the technical problems that the stability of plating solution is poor and the range of controllable color parameters is narrow in the present imitation gold plating technology. Potassium pyrophosphate is used as a main complexing agent, and copper sulfate and zinc sulfate are used as main salt, while nitrilotriaceticacid and seignette salt are used as auxiliary complexing agent for performing Cu-Zn-Sn ternary non-cyanide imitation gold plating. Imitation gold coating similar to real gold can be obtained in the technology. Experiments show that, compared with the previous imitation gold plating technology, the novel imitation gold plating technology is easier to control, the stability is greatly improved, theconcentration of main salt is lower, the technology is simpler and cyanide is not used as the complexing agent anymore. Therefore, compared with the conventional technology, toxicity and pollution ofthe novel technology are reduced significantly, thus benefiting popularization of green production.
Description
Technical field
The present invention relates to the many complex copper-zinc of a kind of environment-friendly type-tin alloy imitation gold plating complete processing, is a kind of means that metal or non-metal material surface are decorated plating technic.
Background technology
The research of environment-friendly imitation gold plating technology becomes the focus of current domestic and international research to improving day by day of environment protection control because of its huge processing market and country.
The non-cyanide imitating gold electroplating technology that research is both at home and abroad at present intended being applied to produce comprises binary (Cu-Zn, Cu-Sn) alloy, ternary (Cu-Zn-Sn, Cu-Sn-In) alloy and quaternary (Cu-Zn-Sn-In, Cu-Sn-In-Ni) alloy.System comprises pyrophosphate salt, Citrate trianion, tartrate, HEDP system etc.According to current data record, must add suitable additive if will obtain the imitation gold deposit of light, as some alcamines or thionamic acid class and derivative thereof etc., when especially above-mentioned brightening agent being mixed use, can be at 3-4A/dm
2Obtain complete bright imitation gold deposit in the current density range.At present, the research of domestic relevant non-cyanide imitating gold electroplating mainly concentrates on the laboratory condition exploratory stage, because there is unstable in its plating bath, be difficult to realize industrialization, simultaneously, it is narrow that the coating color and luster can be controlled processing range, causes the disunity of product batches color and luster, this is the key point of its cyaniding imitation gold plating of can not comparing, thereby its technology is not used widely as yet.
Summary of the invention
Bath stability at present gold simulating electroplating process existence is poor, the technical problem of color and luster controllable parameter narrow range, the present invention optimizes by experiment, a kind of environment-friendly imitation gold plating production technology has been proposed, in the pyrophosphate salt system, adopt potassium pyrophosphate as main complexing agent, with copper sulfate and zinc sulfate as main salt, Seignette salt and glycerine that introducing has hydroxyl structure are that auxiliary ligand is made additive, its hydroxyl participates in coordination, to change coordination ion structure and electrode surface state, finally reach the purpose of codeposition.This production technique realizes by following step:
At first prepare plating bath, the potassium pyrophosphate with 270-290g/L is dissolved in the distilled water of 1/2 prewired liquor capacity earlier, and water temperature will be controlled between 30-40 ℃, uses the copper sulfate CuSO of the distilled water of small amount of thermal with 7-9g/L then
45H
2The zinc sulfate ZnSO of O, 18-22g/L
47H
2O dissolves respectively, while stirring above-mentioned solution is slowly joined in the potassium pyrophosphate solution, makes it to become cupric pyrophosphate and zinc pyrophosphate precipitation; Continue to add potassium pyrophosphate solution to resolution of precipitate, generate cupric pyrophosphate potassium and zinc pyrophosphate potassium solution; Then cupric pyrophosphate potassium and zinc pyrophosphate potassium solution are mixed, stir; Next the Seignette salt of 30-35g/L and the nitrilotriacetic acid(NTA) of 33-38g/L are dissolved respectively with distilled water, join in cupric pyrophosphate potassium and the zinc pyrophosphate potassium solution, and with yellow soda ash and lemon acid for adjusting pH value to 8.5-9.3; With joining in cupric pyrophosphate potassium and the zinc pyrophosphate potassium solution after the dissolving of the sodium stannate of 4.2-4.6g/L, use yellow soda ash and lemon acid for adjusting pH value to 9.0 then again at last, it is stand-by to leave standstill 24 hours after-filtration;
Add the glycerine of 10ml/L and the hydrogen peroxide of 1ml/L in plating forward direction cupric pyrophosphate potassium and the zinc pyrophosphate potassium solution, to sample polish in order, pickling, oil removing, nickel preplating, bright nickel plating, imitative gold plating.
Characteristics of the present invention and beneficial effect: compare with existing gold simulating electroplating process and to have the advantages that toxicity is littler, wider, performance is more stable, just can obtain imitation gold deposit bright in colour, full, that outward appearance is true to nature at metal or nonmetallic surface according to processing step of the present invention and processing condition.Thereby has a higher utility.Be embodied in:
(1) color and luster has controllability
By processing condition, comprise copper, zinc, tin ion concentration ratio, current density, pH, variation of temperature definite control color intervals such as influence to the simulating golden colour pool.
(2) plating bath has stability
Selection by auxiliary complex-former guarantees copper, zinc, the whole complexings of tin ion, also guaranteed the free amount of complexing agent in the plating bath, selection by oxygenant can prevent that positive quaternary tin ion is reduced into the tin ion of positive divalence, also can reach the pin hole effect of eliminating coating, and then the stability of plating bath, the life cycle that prolongs plating bath have been increased.
Embodiment:
A kind of environment-friendly imitation gold plating production technology, in the pyrophosphate salt system, adopt potassium pyrophosphate as main complexing agent, with copper sulfate and zinc sulfate as main salt, Seignette salt and glycerine that introducing has hydroxyl structure are that auxiliary ligand is made additive, its hydroxyl participates in coordination, to change coordination ion structure and electrode surface state, finally reach the purpose of codeposition, this production technique realizes by following step:
At first prepare plating bath, the potassium pyrophosphate with 270-290g/L is dissolved in the distilled water of 1/2 prewired liquor capacity earlier, and water temperature will be controlled between 30-40 ℃, uses the copper sulfate CuSO of the distilled water of small amount of thermal with 7-9g/L then
45H
2The zinc sulfate ZnSO of O, 18-22g/L
47H
2O dissolves respectively, while stirring above-mentioned solution is slowly joined in the potassium pyrophosphate solution, makes it to become cupric pyrophosphate and zinc pyrophosphate precipitation; Continue to add potassium phosphate solution to resolution of precipitate, generate cupric pyrophosphate potassium and zinc pyrophosphate potassium solution; Then cupric pyrophosphate potassium and zinc pyrophosphate potassium solution are mixed, stir; Next the Seignette salt of 30-35g/L and the nitrilotriacetic acid(NTA) of 33-38g/L are dissolved respectively with distilled water, join in cupric pyrophosphate potassium and the zinc pyrophosphate potassium solution, and with yellow soda ash and lemon acid for adjusting pH value to 8.5-9.3; With joining in cupric pyrophosphate potassium and the zinc pyrophosphate potassium solution after the dissolving of the sodium stannate of 4.2-4.6g/L, use yellow soda ash and lemon acid for adjusting pH value to 9.0 then again at last, it is stand-by to leave standstill 24 hours after-filtration;
Add the glycerine of 10ml/L and the hydrogen peroxide of 1ml/L in plating forward direction cupric pyrophosphate potassium and the zinc pyrophosphate potassium solution; To sample polish in order, pickling, oil removing, nickel preplating, bright nickel plating, imitative gold plating.
Described additive is the Seignette salt by 30-35g/L, and the nitrilotriacetic acid(NTA) of 33-38g/L, the yellow soda ash of 10g/L, the glycerine of 10ml/L and the hydrogen peroxide of 1ml/L dissolve the back respectively and mix formation.
Embodiment 1
The present invention optimizes by experiment, has proposed the many complex copper-zinc of a kind of environment-friendly type-tin alloy imitation gold plating novel process.Cu
2+, Zn
2+Be d
10Electronic configuration, the electrochemical reaction overvoltage of hydration coordination ion is very little, and is single during with a kind of part, the overvoltage of plating bath be not too low be exactly too high, even the concentration of change complexing agent, pH also difficulty reach requirement.In order to improve the overvoltage of reaction, the present invention introduces Seignette salt and glycerine with hydroxyl structure in the pyrophosphate salt system be that auxiliary ligand is made additive, its hydroxyl can participate in coordination, to change coordination ion structure and electrode surface state, finally reaches the purpose of codeposition.In addition, poly-hydroxy has chela shape structure, can be used as bridging group while and two metal ion-chelants, can be used as the stablizer of metal ion in the scope of pH8.5-9.3.Consider from the cleaner production angle, this technology nontoxic pollution-free, stable performance, controllability is good.
Present embodiment is with through the carbon steel (composition: C:0.004-0.012 after the oil removing, processing of rust removing; Si :≤0.03; Mn :≤0.20; P :≤0.030; S :≤0.030; Al :≤0.050) be sample, at its coating surface 18K imitation gold deposit, optimize stability non-cyanide imitating gold electroplating system preferably by exploitative experiment, with this system complexing agent of deciding, by add Seignette salt and glycerine auxiliary complex-former and stablizer hydrogen peroxide obtain dispersive ability and covering power better and operating restraint at 0.2-0.4A/dm
2Processing parameter; Test on the perfect basis at laboratory condition, determine the production technique typing.
The technical scheme that present embodiment adopts is:
CuSO
4.5H
2O 7-9g/L
ZnSO
4.7H
2O 18-22g/L
NaSnO
3.3H
2O 4.2-4.6g/L
K
4P
2O
7.3H
2O 270-290g/L
Seignette salt 30-35g/L
Nitrilotriacetic acid(NTA) 33-38g/L
Yellow soda ash 10g/L
Glycerine 10ml/L
Hydrogen peroxide 1ml/L
Temperature 25-35 ℃
Current density (Dk) 0.2-0.4A/dm
2
pH 8.5-9.3
7: 3 sheet brasses of positive plate
The plating bath compound method:
At first, load weighted potassium pyrophosphate is dissolved in the distilled water of 1/2 prewired liquor capacity, water temperature will be controlled between 30-40 ℃, distilled water with small amount of thermal dissolves required copper sulfate, zinc sulfate respectively then, under agitation above-mentioned solution is slowly joined in the potassium pyrophosphate solution, make it to become cupric pyrophosphate and zinc pyrophosphate precipitation; Continue to add potassium pyrophosphate solution to resolution of precipitate, generate cupric pyrophosphate potassium and zinc pyrophosphate potassium solution, then cupric pyrophosphate potassium and zinc pyrophosphate potassium are mixed, stir.
Next Seignette salt and nitrilotriacetic acid(NTA) are dissolved respectively, join in the solution, and with yellow soda ash and lemon acid for adjusting pH value to 8.5-9.3.
At last sodium stannate dissolving is added in the solution, use yellow soda ash and lemon acid for adjusting pH value to 9.0 then again, it is stand-by to leave standstill 24 hours after-filtration.
The glycerine and the 1ml/L hydrogen peroxide that add 10ml/L before the plating are at 30 ℃ of temperature, pH8.9, current density 0.3A/dm
2Following examination plating.
Imitation gold plating layer processing technological flow:
To sample carbon steel pickling (HCl) → clear water wash → oil removing → clear water washes → nickel preplating → clear water washes → mechanical polishing → clear water washes → oil removing → clear water washes → imitation gold plating layer → clear water washes → sealing treatment → clear water washes → dry.
Show that by the experimental data of listing below in preparation plating bath process, the variation of processing condition (as copper, zinc, tin ion concentration ratio, current density, pH, temperature etc.) is to the influence in simulating golden colour pool.
Main salt concentration is to the influence of coating outward appearance in table one plating bath
(T=30 ℃, current density=0.3A/dm, pH=9.2, t=30s, cathode-anode plate area are than=2: 1)
Main salt ionic concentration is than (Cu: cupric ion is separated out easily when Zn) increasing, and coating is red partially; Zinc is separated out easily when ratio reduces, and coating is white partially.So it is 1 that the main salt concentration ratio is controlled at: 2-1: be the best in the time of 2.5.
Main complexing agent is to the influence of coating outward appearance in table two plating bath
(T=30 ℃, current density=0.3A/dm, pH=9.2, t=30s, cathode-anode plate area are than=2: 1)
Complexing agent concentration is too low, the solution instability, and the solution muddiness is easily separated out copper powder, and coating also can be rubescent; When complexing agent concentration was too high, plating bath was relatively stable, but coating color is too shallow.So the potassium pyrophosphate consumption generally is controlled at 270-290g/L.
The hydrogen peroxide consumption is to the influence of coating outward appearance in table three plating bath.
(T=30 ℃, current density=0.3A/dm, pH=9.2, t=30s, cathode-anode plate area are than=2: 1)
The too high levels of hydrogen peroxide can cause the whole oxidisability of plating bath too high, can make coating send out crow even burn when too high levels.So in the configuration electroplate liquid, hydrogen peroxide should not add too much, only need to add on a small quantity, about 1ml/L gets final product.
The glycerine consumption is to the influence of coating outward appearance in table four plating bath.
(T=30 ℃, current density=0.3A/dm, pH=9.2, t=30s, cathode-anode plate area are than=2: 1)
Glycerine as outside the additive, can improve the quality of coating in plating.So, when its content is crossed when low, coating can seem burnt hair, turn white, coating can be smooth not careful yet; Coating can seem smooth careful in the time of too high levels, but coating color can be rubescent.So the glycerine consumption should be controlled at 10ml/L for best.
Table five bath temperature is to the influence of coating outward appearance.
(current density=0.3A/dm, pH=9.2, t=30s, cathode-anode plate area are than=2: 1)
When temperature was low, current density reduced, and cathode efficiency also reduces, so sedimentation velocity also can slow down, and burnt phenomenon but can cause, along with temperature reduces empyreumatic part also can be along with increase; When temperature is higher, can make pyrophosphate salt be hydrolyzed into speeding up of orthophosphoric acid salt, along with temperature raises, the outward appearance of coating also can shoal, even blackout.So temperature is controlled at about 30 ℃ to best.
Table six current density is to the influence of coating outward appearance
(T=30 ℃, pH=9.2, t=30s, cathode-anode plate area are than=2: 1)
When current density was on the low side, separating out of zinc and tin can reduce, and opposite separating out of copper can increase to some extent, and therefore along with the reduction of current density, the color of coating can be more and more darker, and it is blue to redden; On the contrary, when current density was higher, what zinc and tin can become separated out easily, and copper separate out minimizing, therefore along with the increase of current density, the color of coating can be more and more shallow, even turn white.So the optimum range of current density should be controlled between the 0.2-0.3.
Table seven pH value is to the influence of coating outward appearance
(T=30 ℃, current density=0.3A/dm, t=30s, cathode-anode plate area are than=2: 1)
As can be seen from the above table, coating can obtain golden yellow when the pH of plating bath value is between 8.6-9.2.After the pH value diminished, coating was rubescent thereupon, was rendered as bronze colour fully after arriving about 7.4; After the pH value became greatly, coating turned white thereupon, and after the pH value surpassed 10.4, coating was rendered as white substantially.So best pH value scope is between the 8.6-9.2.
Claims (2)
1. environment-friendly imitation gold plating production technology, in the pyrophosphate salt system, adopt potassium pyrophosphate as main complexing agent, with copper sulfate and zinc sulfate as main salt, Seignette salt and glycerine that introducing has hydroxyl structure are that auxiliary ligand is made additive, its hydroxyl participates in coordination, to change coordination ion structure and electrode surface state, finally reach the purpose of codeposition, this production technique realizes by following step:
At first prepare plating bath, the potassium pyrophosphate with 270-290g/L is dissolved in the distilled water of 1/2 prewired liquor capacity earlier, and water temperature will be controlled between 30-40 ℃, uses the copper sulfate CuSO of the distilled water of small amount of thermal with 7-9g/L then
45H
2The zinc sulfate ZnSO of O, 18-22g/L
47H
2O dissolves respectively, while stirring above-mentioned solution is slowly joined in the potassium pyrophosphate solution, makes it to become cupric pyrophosphate and zinc pyrophosphate precipitation; Continue to add potassium pyrophosphate solution to resolution of precipitate, generate cupric pyrophosphate potassium and zinc pyrophosphate potassium solution; Then cupric pyrophosphate potassium and zinc pyrophosphate potassium solution are mixed, stir; Next the Seignette salt of 30-35g/L and the nitrilotriacetic acid(NTA) of 33-38g/L are dissolved respectively with distilled water, join in cupric pyrophosphate potassium and the zinc pyrophosphate potassium solution, and with yellow soda ash and lemon acid for adjusting pH value to 8.5-9.3; With joining in cupric pyrophosphate potassium and the zinc pyrophosphate potassium solution after the dissolving of the sodium stannate of 4.2-4.6g/L, use yellow soda ash and lemon acid for adjusting pH value to 9.0 then again at last, it is stand-by to leave standstill 24 hours after-filtration;
Add the glycerine of 10ml/L and the hydrogen peroxide of 1ml/L in plating forward direction cupric pyrophosphate potassium and the zinc pyrophosphate potassium solution; To sample polish in order, pickling, oil removing, nickel preplating, bright nickel plating, imitative gold plating.
2. environment-friendly imitation gold plating production technology according to claim 1, it is characterized in that: described additive is the Seignette salt by 30-35g/L, the nitrilotriacetic acid(NTA) of 33-38g/L, the yellow soda ash of 10g/L, the glycerine of 10ml/L and the hydrogen peroxide of 1ml/L dissolve the back respectively and mix formation.
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| CN105274593A (en) * | 2015-11-30 | 2016-01-27 | 苏州市金星工艺镀饰有限公司 | Imitation gold electroplate liquid and electroplating method thereof |
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| CN102568640B (en) * | 2010-12-13 | 2016-03-30 | 马羽宽 | The anti-sparking battery lead plate of fluorescent magnetic particle inspection machine seized part powered electrode or backing plate |
| CN105274593A (en) * | 2015-11-30 | 2016-01-27 | 苏州市金星工艺镀饰有限公司 | Imitation gold electroplate liquid and electroplating method thereof |
| CN105543914A (en) * | 2015-12-23 | 2016-05-04 | 苏州市金星工艺镀饰有限公司 | Electroplating method for decorative copper zinc alloy electroplating solution |
| CN106676594A (en) * | 2016-06-10 | 2017-05-17 | 太原工业学院 | Low-cost cyanide-free copper-zinc-tin alloy electroplating solution and copper-zinc-tin alloy electroplating technology thereof |
| JP2018119169A (en) * | 2017-01-23 | 2018-08-02 | 学校法人関東学院 | Electroplating solution, electroplating method and electroplating film |
| CN110702845A (en) * | 2019-10-12 | 2020-01-17 | 广州超邦化工有限公司 | Titration analysis method for copper and nickel in pyrophosphate-citrate copper-nickel alloy plating solution |
| CN110702845B (en) * | 2019-10-12 | 2022-03-04 | 广州超邦化工有限公司 | Titration analysis method for copper and nickel in pyrophosphate-citrate copper-nickel alloy plating solution |
| CN110592627A (en) * | 2019-10-31 | 2019-12-20 | 四川轻化工大学 | Cyanide-free imitation gold electroplating solution and magnesium alloy electroplating process thereof |
| CN113463147A (en) * | 2021-07-14 | 2021-10-01 | 四川轻化工大学 | Carbon steel surface cyanide-free gold-imitating copper-zinc-tin alloy electroplating process |
| CN114908388A (en) * | 2022-05-18 | 2022-08-16 | 湖南科技大学 | Cu-Sn-based alloy plating layer and preparation method thereof |
| CN114908388B (en) * | 2022-05-18 | 2024-02-02 | 湖南科技大学 | Cu-Sn-based alloy coating and preparation method thereof |
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Open date: 20100310 |