CN108517543A - A kind of cyanogen-free silver-plating solution, simplicity rapid detection method and quantitative detecting method that can dynamically monitor copper ion pollution content - Google Patents
A kind of cyanogen-free silver-plating solution, simplicity rapid detection method and quantitative detecting method that can dynamically monitor copper ion pollution content Download PDFInfo
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Abstract
The invention belongs to non-cyanide silver coating fields, and in particular to copper ion concentration indicator is added in a kind of cyanogen-free silver-plating solution, simplicity rapid detection method and quantitative detecting method that can dynamically monitor copper ion pollution content predominantly in cyanogen-free silver-plating solution.Copper ion concentration indicator is added in the present invention in cyanogen-free silver-plating solution, under the conditions of not influencing the basic performance of plating solution, the variation of content of copper ion can be monitored in real time by way of colour developing, it is easy rapidly to detect content of copper ion and realize quantitative analysis in the cyanogen-free silver-plating solution of low concentration content of copper ion.Can be more than a certain concentration in content of copper ion by monitoring content of copper ion in real time（It is recommended that 2 g/L）When cyanogen-free silver-plating solution is handled, reduce content of copper ion, prevent from having an impact the quality of coating of plating piece.In addition, if cyanogen-free silver-plating solution quickly becomes blue, illustrates there are the production accidents such as very big probability is not powered on or plating piece is fallen, be convenient for the management to plating solution and the control to product quality.
Description
Technical field
The invention belongs to non-cyanide silver coating fields, and in particular to a kind of non-cyanide silver coating that can dynamically monitor copper ion pollution content
Electroplate liquid, easy rapid detection method and quantitative detecting method.
Background technology
Silver has extensive purposes in industry and daily life, is a kind of high-tech metal, at the same be also a kind of army,
The dual-purpose metal of the people.Plating silver layer has unique silvery white gloss, chemical property to stablize.Plating silver layer has high conduction, leads
It is hot, there is good welding performance.Electrosilvering printed wiring board in the electronics industry, electronic component in instrument and meter, fly
The significant points of the Communication Equipments such as machine, optical instrument and high-frequency component and waveguide and equipment, which are obtained for, to be widely applied, with
Ensure good electric conductivity and brazing property.In addition, electrosilvering has beautiful silvery white gloss, in household implements, tableware
And it is also widely used as decorative layer in various craftworks.
So far, plating silver process both domestic and external is mostly or using cyaniding plant of silver technique, mainly due to the plating solution
Stability is good, and covering power and depth capability are preferable, and coating crystallization is more careful, and appearance is silvery white.But cyanide severe toxicity, it is right
Human body and environment it is very harmful, when production, requires have good exhaust equipment and wastewater treatment condition.With countries in the world
The reinforcement of environmental protection consciousness and the appearance of relevant policies, have cyanogen plating be increasingly becoming restricted industry, become limitation declare,
The superseded technique of principle." being electroplated containing cyanogen " ranks " out of category " the 182nd, and therefore, galvanizer authors have been devoted to be free of
CN-Non-cyanide silver coating research, successively propose that thiosulfate is silver-plated, sulphite is silver-plated, sulfosalicylic acid is silver-plated and sub-
The silver-plated equal cyanide-free silver plating process of amidodisulfonic acid salt, while also having applied for some patents, such as United States Patent (USP) USP4247372,
USP4478691, USP4246077, USP4126524 etc.；Japan Patent JP7039945；In addition there is European patent
EP0705919, EP1416065, EP1418251 etc..It is compared with cyaniding plant of silver, there are still many disadvantages for non-cyanide silver coating, main
Problem is wanted to have：(1) bath stability sex chromosome mosaicism.The stability of many non-cyanide plating silvering solutions is bad, either alkali plating solution or acidity
All there is bath stability in plating solution, make troubles to management and operation, while cost being made to increase to some extent.
(2) plating solution cost is higher.Therefore, less using the enterprise of cyanide-free silver plating process at present.In the case, a kind of toxicity it is low or
The development and application of the cyanide-free silver plating process nontoxic, cost is relatively suitable are a major subjects as field of electroplating.
Since silver ion has oxidability more higher than copper ion, even across complexing, copper can also be in silver plating liquid
Displacement reaction occurs.Other metals are not contained in cyanide-free silver plating process, but the silver ion content of its plating solution is higher（10~20 g/
L）, and the complexing power of main complexing agent and silver ion is weaker than cyanide, therefore careless manipulation, especially without by pre- silver-plated
When, plating piece metal can occur displacement with the silver ion in plating solution and react.Numerous studies show the presence due to displacement, without
The nickel-plated substrates for crossing preplating cannot the directly plating in non-cyanide silver coating plating solution.Even Copper base material, the overlong time for entering slot also may be used
Binding force is caused to decline the pollution with plating solution to cause surface that displacement reaction occurs.Studies have shown that at 40 DEG C when Copper base material is silver-plated
Under the conditions of, it can replace within 3 minutes.For the especially complex plating piece of structure, especially there is a plating piece of tiny deep hole, in deep hole
The generation for also tending to have displacement, the contact because of the copper lead of careless manipulation with plating solution can also lead to dirt of the copper ion to plating solution
Dye.It is not complicated into slot or plating piece using charging, fail that the displacements such as plating piece removal also will produce copper ion in time after plating
Pollution.It is discovered by experiment that when plating solution contains 0.5 g/L copper ions, the hardness of coating slightly has compared to more pollution-free plating solution
It is a little to reduce.Copper ion pollutes the component that will not change coating, but certain influence is still produced to processing range, bright
Current density range reduces.When the concentration of copper ion further rises to 1.0 g/L, low current density leads to sample surfaces
There is more fine particle protrusion.Therefore, industrial production, especially with being needed in plating solution in the production process of cyanideless electro-plating
The content dynamic of copper ion monitors, and ensures the quality of the reliable and coating of plating solution.
Invention content
The present invention in view of the above-mentioned problems, provide it is a kind of can dynamically monitor copper ion pollution content cyanogen-free silver-plating solution,
Monitoring method and quantitative detecting method.
The technical solution used in the present invention is as follows：A kind of non-cyanide silver coating plating that can dynamically monitor copper ion pollution content
Liquid, including copper ion concentration indicator.Wherein cyanogen-free silver-plating solution includes main complexing agent, additional conductive salt, compound additive
And pH adjusting agent, it can be as disclosed in patent CN201610587832.7, CN201110219268.0, CN201110226274.9
Cyanogen-free silver-plating solution or other existing disclosed cyanogen-free silver-plating solutions, it is all applicable.
The copper ion concentration indicator is aminotrimethylenephosphonic acid（ATMP）, 1-hydroxy ethylidene-1,1-diphosphonic acid（HEDP）, second
Ethylenediamine tetraacetic acid (EDTA)（EDTA）, it is ethylenediamine, one or more in potassium citrate.
The copper ion concentration indicator is ethylenediamine tetra-acetic acid（EDTA）.
The ethylenediamine tetra-acetic acid（EDTA）Content be 1-8 g/L.
The copper ion concentration indicator is aminotrimethylenephosphonic acid, 1-hydroxy ethylidene-1,1-diphosphonic acid.
The content of the aminotrimethylenephosphonic acid is 1-8 g/L, and the content of the 1-hydroxy ethylidene-1,1-diphosphonic acid is 1-8 g/
L。
A method of easy quickly detection copper ion pollutes content, including following procedure during non-cyanide silver coating：
（1）Using the above-mentioned cyanogen-free silver-plating solution that can dynamically monitor copper ion and pollute content, configuration several groups contain difference
The copper ion indicator color contrast sample of content of copper ion；
（2）Using the above-mentioned cyanogen-free silver-plating solution progress non-cyanide silver coating that can dynamically monitor copper ion and pollute content, in no cyanogen
The color of silver plating process, cyanogen-free silver-plating solution changes with the increase of content of copper ion in electroplate liquid, by by non-cyanide silver coating
Electroplate liquid is compared with copper ion indicator color contrast sample, determines the content interval of copper ion in cyanogen-free silver-plating solution.
Step（2）In, the mode of comparison is the judgement of naked eyes shade or ultraviolet-visible spectrometer.
Pass through ultraviolet-visible spectrometer, spy of 600 ~ 700 sections the nm maximum absorption peaks as copper ions plating solution
Absorption peak is levied, the content interval of copper ion is determined by the comparison size of the absorbance value of characteristic absorption peak.
The method of content of copper ion, wherein content of copper ion are less than or equal in a kind of quantitative analysis cyanogen-free silver-plating solution
0.1 g/L, includes the following steps：
（1）The cyanogen-free silver-plating solution that copper ion pollutes content can dynamically be monitored using claim 1-6 any one of them, matched
Set the copper ion indicator color contrast sample for the different content of copper ion that several groups contain the sections 0-0.10 g/L；
（2）Pass through the ultraviolet-visible absorption spectroscopy of ultraviolet-visible spectrometer copper ion indicator color contrast sample；
（3）The absorbance value at 600 ~ 700 sections nm maximum absorption peaks is read, absorbance-concentration curve is drawn, utilizes Linear Quasi
It closes, obtains fit equation；
（4）By tested sample by ultraviolet-visible spectrometer ultraviolet-visible absorption spectroscopy, 600 ~ 700 sections nm are read
The absorbance value at maximum absorption peak；
（5）By step（4）In absorbance value substitute into step（3）In fit equation in, obtain concentration value；
Wherein, tested sample is step（1）Described in can dynamically monitor copper ion pollution content cyanogen-free silver-plating solution.
Beneficial effects of the present invention are as follows：Copper ion concentration indicator is added in the present invention in cyanogen-free silver-plating solution, with
The variation of copper ion concentration can develop the color, and can monitor the variation of content of copper ion, easy quickly inspection in real time by way of colour developing
The size of content of copper ion and the cyanogen-free silver-plating solution in low concentration content of copper ion are surveyed, it can be with its content of quantitative analysis.
Can be more than a certain amount of in content of copper ion by monitoring content of copper ion in real time（It is recommended that 2 g/L）When to non-cyanide silver coating
Electroplate liquid is handled, and is reduced content of copper ion, is prevented from having an impact the silver-plated effect of plating piece.In addition, if non-cyanide silver coating
Electroplate liquid quickly becomes blue, illustrates there are the production accidents such as very big probability is not powered on or plating piece is fallen, can be with timely processing.This hair
Colour stable after the bright cyanogen-free silver-plating solution colour developing that can dynamically monitor copper ion pollution content, meanwhile, the copper being added from
Sub- indicator plating solution is without influence, on quality of coating without influence.
Description of the drawings
Fig. 1 is the result of embodiment one.
Fig. 2 is the result of embodiment two.
Fig. 3 is the result of embodiment three.
Fig. 4 is the result of example IV.
Fig. 5 is to contain different Cu2+The ultraviolet-visible absorption spectroscopy of the plating silver plating solution of concentration.
Fig. 6 is the standard working curve of absorbance-concentration.
Specific implementation mode
Below in conjunction with the accompanying drawings and specific embodiment, the present invention can be better described.
Embodiment one：
（1）Configuration contains ethylenediamine tetra-acetic acid（EDTA）The cyanogen-free silver-plating solution of the copper ion indicator of 8 g/L；
（2）Experiment weighs 4.88 g CuSO4•5H2O is configured to the solution of 50.00 mL, 25.0 g/L with a deionized water；
（3）Then utilize cyanogen-free silver-plating solution to dilute, be configured to 0.001 successively, 0.002,0.004,0.01,0.02,0.05,
0.1, the Cu of 0.2,0.3,0.5,1.0,1.5,2.0,3.0 g/L concentration2+Solution；
（4）The random plating fluid samples taken out during non-cyanide silver coating, with step（3）Compare
The results are shown in Figure 1, step（3）The solution of configuration is with Cu2+The increase of concentration and color gradually deepens, in 0.1-1
The color aberration in the sections g/L is apparent, excessively shallow or too deep in the part less than 0.1 g/L and the part colours more than 1 g/L, color
It is poor little, judged by naked eyes, has large error.Step（4）In plating fluid samples color between 0.02 g/L, 0.05
Between g/L two.It is accurately detected by ICP, step（4）In plating fluid samples concentration in 0.045 g/L.
Embodiment two：
（1）Configuration contains 1-hydroxy ethylidene-1,1-diphosphonic acid（HEDP）The non-cyanide plating of the copper ion indicator of 4 g/L, 7 g/L of potassium citrate
Plating solution for silver-plating；
（2）Experiment weighs 4.88 g CuSO4•5H2O is configured to the solution of 50.00 mL, 25.0 g/L with a deionized water；
（3）Then utilize cyanogen-free silver-plating solution to dilute, be configured to 0.01 successively, 0.02,0.04,0.1,0.2,0.5,1.0,
2.0, the Cu of 3.0 g/L concentration2+Solution；
（4）The random plating fluid samples taken out during non-cyanide silver coating, with step（3）Compare
The results are shown in Figure 1, step（3）The solution of configuration is with Cu2+The increase of concentration and color gradually deepens, step（4）In
Plating fluid samples color between 0.1 g/L, 0.2 g/L two.It is accurately detected by ICP, step（4）In plating solution examination
The concentration of sample is in 0.109 g/L.
Embodiment three：
（1）Configuration contains 1-hydroxy ethylidene-1,1-diphosphonic acid（HEDP）2 g/L, aminotrimethylenephosphonic acid（ATMP）5 g/L, ethylenediamine tetraacetic
Acetic acid（EDTA）The cyanogen-free silver-plating solution of the copper ion indicator of 1 g/L；
（2）Experiment weighs 4.88 g CuSO4•5H2O is configured to the solution of 50.00 mL, 25.0 g/L with a deionized water；
（3）Then utilize cyanogen-free silver-plating solution to dilute, be configured to 0.01 successively, 0.02,0.04,0.1,0.2,0.5,1.0,
The Cu2+ solution of 2.0 g/L concentration；
（4）The random plating fluid samples taken out during non-cyanide silver coating, with step（3）It compares.
The results are shown in Figure 1, step（3）The solution of configuration is with Cu2+The increase of concentration and color gradually deepens, but it is whole
Color is relatively shallower, the Cu of low concentration2+It is difficult to which naked eyes discover concentration variation, step（4）In plating fluid samples color between
Between 0.04 g/L, 0.1 g/L two.It is accurately detected by ICP, step（4）In plating fluid samples concentration in 0. 073 g/
L。
Example IV：
（1）Configuration contains 1-hydroxy ethylidene-1,1-diphosphonic acid（HEDP）3g/L, aminotrimethylenephosphonic acid（ATMP）The copper ion of 4 g/L refers to
Show the cyanogen-free silver-plating solution of agent；
（2）Experiment weighs 4.88 g CuSO4•5H2O is configured to the solution of 50.00 mL, 25.0 g/L with a deionized water；
（3）Then utilize cyanogen-free silver-plating solution to dilute, be configured to 0.01 successively, 0.02,0.04,0.1,0.2,0.5,1.0,
2.0, the Cu2+ solution of 3.0 g/L concentration；
（4）The random plating fluid samples taken out during non-cyanide silver coating, with step（3）It compares.
The results are shown in Figure 1, step（3）The solution of configuration is with Cu2+The increase of concentration and color gradually deepens, in 0.2-
The section aberration of 3 g/L is big, and especially 2.0,3.0 g/L, it is used for the monitoring of content of copper ion limit, when content of copper ion is more than
When 3 g/L, color obviously deepens, it is necessary to handle plating solution, prevent silver-plated, step（4）In plating fluid samples color between
Between 0.10 g/L, 0.20 g/L two.It is accurately detected by ICP, step（4）In plating fluid samples concentration in 0.189 g/
L。
Embodiment five：
To containing 0.500,0.250,0.125,0.050,0.0375,0.025,0.020,0.010 and 0.005 g/L Cu2+It is dense
The cyanogen-free silver-plating solution of degree makees reference using with blank plating solution, carries out the measurement of uv-vis spectra.We intercept 400 ~
The spectrogram of 800 nm is overlapped, and is provided in Fig. 5.Copper ion indicator uses ethylenediamine tetraacetic wherein in cyanogen-free silver-plating solution
Acetic acid（EDTA）8 g/L.
As can be seen from the figure absorption spectrum is gradually increased with the raising of copper ion concentration, is maximum absorption at 647 nm
Peak, in order to draw the standard curve of absorbance and concentration, we read the absorbance value at 647 nm, are summarized in table 1.
Absorbance-concentration curve is drawn in Fig. 6 with this.It can be seen from the figure that when copper ion concentration is less than 0.1 g/L
When, absorbance has preferable linear relationship with concentration.When concentration is more than 0.1 g/L, due to change of ionic activity etc.
The growth of absorbance deviates linear.In order to obtain can be with result of the comparison, we are using cyanogen-free silver-plating solution as solvent.Its
Concentration is higher, and total ionic strength is more than 4 mol/L, and conductivity is 40 ~ 50 mS/cm, 1.05 ~ 1.07 g/L of density.Therefore
Higher copper ion concentration is tested unsuitable using ultraviolet-visible absorption spectroscopy.Low concentration data are utilized into linear fit, are obtained
To fit equation（ConcentrationCUnit be g/L）, R2=0.993, substantially conform to quantitative analysis requirement.
By detecting the copper ion concentration in multigroup unknown cyanogen-free silver-plating solution, with the copper that is accurately detected by ICP from
Sub- concentration results compare, and the sample of 0.1 g/L is less than for copper ion concentration, and error 0.3-1.9% is dense for copper ion
Degree is more than 0.1 g/L samples, error 2.4-9.2%.
ICP, that is, inductively coupled plasma spectrum generator, can accurately detect content of copper ion.
Example the above is only the implementation of the present invention is not used for limiting the scope of the invention；The protection of the present invention
Range is limited by the claim in claims, and every according to equivalence changes made by invention and modification, all in this hair
Within the protection domain of bright patent.
Claims (10)
1. a kind of cyanogen-free silver-plating solution that can dynamically monitor copper ion pollution content, which is characterized in that include copper ion concentration
Indicator.
2. the cyanogen-free silver-plating solution according to claim 1 that can dynamically monitor copper ion pollution content, it is characterised in that：
The copper ion concentration indicator is aminotrimethylenephosphonic acid, 1-hydroxy ethylidene-1,1-diphosphonic acid, ethylenediamine tetra-acetic acid, ethylenediamine, lemon
It is one or more in lemon acid potassium.
3. the cyanogen-free silver-plating solution according to claim 2 that can dynamically monitor copper ion pollution content, it is characterised in that：
The copper ion concentration indicator is ethylenediamine tetra-acetic acid.
4. the cyanogen-free silver-plating solution according to claim 3 that can dynamically monitor copper ion pollution content, feature exist
In：The content of the ethylenediamine tetra-acetic acid is 1-8 g/L.
5. the cyanogen-free silver-plating solution according to claim 2 that can dynamically monitor copper ion pollution content, it is characterised in that：
The copper ion concentration indicator is aminotrimethylenephosphonic acid, 1-hydroxy ethylidene-1,1-diphosphonic acid.
6. the cyanogen-free silver-plating solution according to claim 5 that can dynamically monitor copper ion pollution content, feature exist
In：The content of the aminotrimethylenephosphonic acid is 1-8 g/L, and the content of the 1-hydroxy ethylidene-1,1-diphosphonic acid is 1-8 g/L.
7. a kind of method of quickly detection copper ion pollution content easy during non-cyanide silver coating, which is characterized in that including with
Lower process：
（1）The cyanogen-free silver-plating solution that copper ion pollutes content can dynamically be monitored using claim 1-6 any one of them, matched
Set the copper ion indicator color contrast sample that several groups contain different content of copper ion；
（2）Using claim 1-6 any one of them can dynamically monitor copper ion pollute content cyanogen-free silver-plating solution into
Row non-cyanide silver coating becomes in the color of non-cyanide silver coating process, cyanogen-free silver-plating solution with the increase of content of copper ion in electroplate liquid
Change, by comparing cyanogen-free silver-plating solution and copper ion indicator color contrast sample, determines in cyanogen-free silver-plating solution
The content interval of copper ion.
8. the method for quickly detection copper ion pollution content easy during non-cyanide silver coating according to claim 7,
It is characterized in that：Step（2）In, the mode of comparison is the judgement of naked eyes shade or ultraviolet-visible spectrometer.
9. the method for quickly detection copper ion pollution content easy during non-cyanide silver coating according to claim 8,
It is characterized in that：By ultraviolet-visible spectrometer, 600 ~ 700 sections nm maximum absorption peaks are as copper ions plating solution
Characteristic absorption peak determines the content interval of copper ion by the comparison size of the absorbance value of characteristic absorption peak.
10. the method for content of copper ion, wherein content of copper ion are less than or equal in a kind of quantitative analysis cyanogen-free silver-plating solution
0.1 g/L, which is characterized in that include the following steps：
（1）The cyanogen-free silver-plating solution that copper ion pollutes content can dynamically be monitored using claim 1-6 any one of them, matched
Set the copper ion indicator color contrast sample for the different content of copper ion that several groups contain the sections 0-0.10 g/L；
（2）Pass through the ultraviolet-visible absorption spectroscopy of ultraviolet-visible spectrometer copper ion indicator color contrast sample；
（3）The absorbance value at 600 ~ 700 sections nm maximum absorption peaks is read, absorbance-concentration curve is drawn, utilizes Linear Quasi
It closes, obtains fit equation；
（4）By tested sample by ultraviolet-visible spectrometer ultraviolet-visible absorption spectroscopy, 600 ~ 700 sections nm are read
The absorbance value at maximum absorption peak；
（5）By step（4）In absorbance value substitute into step（3）In fit equation in, obtain concentration value；
Wherein, tested sample is step（1）Described in can dynamically monitor copper ion pollution content cyanogen-free silver-plating solution.
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| CN112180884A (en) * | 2020-10-27 | 2021-01-05 | 张家港扬子江冷轧板有限公司 | Method for visually evaluating quality of electrotinning solution on line |
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