CN105506680A - Preparation method of electroplating liquid for reducing growth of plating layer tin whisker - Google Patents
Preparation method of electroplating liquid for reducing growth of plating layer tin whisker Download PDFInfo
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- CN105506680A CN105506680A CN201510981821.2A CN201510981821A CN105506680A CN 105506680 A CN105506680 A CN 105506680A CN 201510981821 A CN201510981821 A CN 201510981821A CN 105506680 A CN105506680 A CN 105506680A
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- acid
- electroplate liquid
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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
- C25D3/30—Electroplating: Baths therefor from solutions of tin
Abstract
The invention discloses a preparation method of electroplating liquid for reducing growth of a plating layer tin whisker. Acid plating liquid adopts mixed solution of methanesulfonic acid, acetic acid and hydrochloric acid; tin salt adopts mixed solution of soluble tin tetrathiomolybdate and dodecyl sulfate; such components as a curing agent, a dispersing agent, a brightening agent, an impurity removal masking agent and a surface active agent are added; and the substances are prepared to the electroplating liquid according to an optimized electroplating liquid preparation method. Compared with traditional electroplating liquid, the inhibition effect on growth of the tin whisker is obvious, the growth speed of the tin whisker is largely reduced, and the growth of the tin whisker on the surface of an electroplated part is reduced; and after the preparation method is used for electroplating, the plated layer is excellent in flexibility and ductility, has an excellent relief effect on appearance of cracks, is higher in temperature bearing capacity, and is high in practical value.
Description
Technical field
The present invention relates to metal plating galvanic deposit preparation field, particularly relate to a kind of preparation method reducing the long electroplate liquid of coating tin one of the main divisions of the male role in traditional opera.
Background technology
In electronic industry is produced, component's feet electroplates one deck tin-lead (Sn-Pb) alloy on the surface usually to improve the wettability of its welding, but lead element is the metallic element that a kind of bio-toxicity is very large, huge harm is had to human body and environment, after forbidding there are the objectionable impuritiess such as plumbous Pb, cadmium Cd, mercury Hg and sexavalent chrome Cr (VI) in waste after the electron device gurry regulations case passed through since European Commission is defined in 2004, exploitation Lead-Free Soldering Technology and corresponding Pure Tin Plating Process technology have become the Main Means substituting plating Sn-Pb alloy.Existing Pb-free wave soldering alloy, it is higher that ubiquity welding temperature, and crystallization is comparatively thick, the problems such as easy long Sn palpus.
How to seek a kind of effective electroplate liquid must inquire into the occurrence value avoided or reduce above-mentioned phenomenon.
Summary of the invention
Goal of the invention: the welding temperature existed in order to the Lead-free Pure Tin Plating Process alloy solved existing for prior art is higher, crystallization thick and Yi Changxi palpus problem, the invention provides a kind of surface finish of rear coating that uses good, flawless and stable chemical nature own, to tin must the preparation method of the long electroplate liquid of the inhibited reduction coating tin one of the main divisions of the male role in traditional opera of growth.
Technical scheme: for achieving the above object, the present invention adopts following technical scheme: a kind of preparation method reducing the long electroplate liquid of coating tin one of the main divisions of the male role in traditional opera, comprises the following steps:
(1) following raw materials is prepared according to Mass Calculation: volume ratio is the methylsulphonic acid of 5:1:2, acetic acid, mixing solutions 20-40 part of hydrochloric acid, solubility tetrathio molybdic acid tin 8-12 part, dodecyl sulfate 12-15 part, laking agent 2-6 part, dispersion agent 3-8 part, brightening agent 3-5 part, impurity elimination sequestering agent 4-6 part, tensio-active agent 1-3 part, water 20-30 part.
(2) water of 1/3rd amounts is got, slowly add the mixing solutions of the methylsulphonic acid of aequum, acetic acid, hydrochloric acid while stirring, the laking agent of aequum is added when solution temperature is down to room temperature, stir the brightening agent and the dispersion agent that add aequum after leaving standstill 10min, mixing and stirring becomes mixed solution A stand-by;
(3) before plating, mixed solution A prepared by step (2) is put into plating tank, regulate pH to 5.0-6.0, add the water of 1/3rd amounts again, then solubility tetrathio molybdic acid tin and the dodecyl sulfate of aequum is added, add the impurity elimination sequestering agent of aequum and the water of tensio-active agent and surplus after mixing and stirring deposition 20min, be stirred into required electroplate liquid stand-by.
More preferred, described dodecyl sulfate is the one in ammonium salt, sodium salt, sylvite, barium salt.
More preferred, described laking agent for epoxy chloropropane and ammonium chloride chitosan mass ratio be the mixture of 2:3.
More preferred, described dispersion agent is polyacrylic acid and EDTA mass ratio is the mixture of 2:1-5:1.
More preferred, described brightening agent is the mixture of citric acid, cocinic acid, silicone oil, dodecyl poly glucoside, and the mass ratio of four kinds of materials should be 2:2:1:3 mutually.
More preferred, described impurity elimination sequestering agent is acidic cpd.
More preferred, described tensio-active agent is aniorfic surfactant.
Further, the storing temp of described mixed solution A is not higher than 40 degrees Celsius.
Beneficial effect: a kind of preparation method reducing the long electroplate liquid of coating tin one of the main divisions of the male role in traditional opera provided by the present invention, acidic bath adopts methylsulphonic acid, acetic acid, the mixing solutions of hydrochloric acid, pink salt adopts the mixing solutions of solubility tetrathio molybdic acid tin and dodecyl sulfate, and with the addition of laking agent, dispersion agent, brightening agent, impurity elimination sequestering agent, the compositions such as tensio-active agent, above-mentioned substance is prepared from according to the electroplate liquid preparation method optimized, compared with traditional electrical plating solution, obvious to the growth inhibitory effect of tin palpus, greatly reduce the growth velocity of tin palpus, reduce the growth of plated item surface tin palpus, and use the present invention to carry out electroplating rear coating to there is snappiness and ductility is good, to the appearance of coating crackle, there is good mitigation, more flexible to temperature capacity, there is very strong practical value.
Embodiment
Below in conjunction with embodiment, the present invention is described in further detail:
Embodiment 1:
Reduce a preparation method for the long electroplate liquid of coating tin one of the main divisions of the male role in traditional opera, comprise the following steps:
(1) following raw materials is prepared according to Mass Calculation: volume ratio is methylsulphonic acid, acetic acid, the mixing solutions 20 parts of hydrochloric acid, 8 parts, solubility tetrathio molybdic acid tin, ammonium lauryl sulfate 12 parts, 2 parts, laking agent, dispersion agent 3 parts, brightening agent 3 parts, impurity elimination sequestering agent 4 parts, 1 part, the tensio-active agent of 5:1:2,20 parts, water;
(2) water of 1/3rd amounts is got, slowly add the mixing solutions of the methylsulphonic acid of aequum, acetic acid, hydrochloric acid while stirring, the laking agent of aequum is added when solution temperature is down to room temperature, stir the brightening agent and the dispersion agent that add aequum after leaving standstill 10min, mixing and stirring becomes mixed solution A stand-by; The storing temp of mixed solution A is not higher than 40 degrees Celsius;
(3) before plating, mixed solution A prepared by step (2) is put into plating tank, regulate pH to 5.0-6.0, add the water of 1/3rd amounts again, then solubility tetrathio molybdic acid tin and the ammonium lauryl sulfate of aequum is added, add the impurity elimination sequestering agent of aequum and the water of tensio-active agent and surplus after mixing and stirring deposition 20min, be stirred into required electroplate liquid stand-by.
Described laking agent for epoxy chloropropane and ammonium chloride chitosan mass ratio be the mixture of 2:3; Described dispersion agent is polyacrylic acid and EDTA mass ratio is the mixture of 2:1; Described brightening agent is the mixture of citric acid, cocinic acid, silicone oil, dodecyl poly glucoside, and the mass ratio of four kinds of materials should be 2:2:1:3 mutually; Described impurity elimination sequestering agent is acidic cpd; Described tensio-active agent is aniorfic surfactant.
Embodiment 2:
Reduce a preparation method for the long electroplate liquid of coating tin one of the main divisions of the male role in traditional opera, comprise the following steps:
(1) following raw materials is prepared according to Mass Calculation: volume ratio is methylsulphonic acid, acetic acid, the mixing solutions 40 parts of hydrochloric acid, 12 parts, solubility tetrathio molybdic acid tin, 15 parts, dodecyl sulphate potassium, 6 parts, laking agent, dispersion agent 8 parts, brightening agent 5 parts, impurity elimination sequestering agent 6 parts, 3 parts, the tensio-active agent of 5:1:2,30 parts, water;
(2) water of 1/3rd amounts is got, slowly add the mixing solutions of the methylsulphonic acid of aequum, acetic acid, hydrochloric acid while stirring, the laking agent of aequum is added when solution temperature is down to room temperature, stir the brightening agent and the dispersion agent that add aequum after leaving standstill 10min, mixing and stirring becomes mixed solution A stand-by; The storing temp of mixed solution A is not higher than 40 degrees Celsius;
(3) before plating, mixed solution A prepared by step (2) is put into plating tank, regulate pH to 5.0-6.0, add the water of 1/3rd amounts again, then solubility tetrathio molybdic acid tin and the dodecyl sulphate potassium of aequum is added, add the impurity elimination sequestering agent of aequum and the water of tensio-active agent and surplus after mixing and stirring deposition 20min, be stirred into required electroplate liquid stand-by.
Described laking agent for epoxy chloropropane and ammonium chloride chitosan mass ratio be the mixture of 2:3; Described dispersion agent is polyacrylic acid and EDTA mass ratio is the mixture of 5:1; Described brightening agent is the mixture of citric acid, cocinic acid, silicone oil, dodecyl poly glucoside, and the mass ratio of four kinds of materials should be 2:2:1:3 mutually; Described impurity elimination sequestering agent is acidic cpd; Described tensio-active agent is aniorfic surfactant.
Embodiment 3:
Reduce a preparation method for the long electroplate liquid of coating tin one of the main divisions of the male role in traditional opera, comprise the following steps:
(1) following raw materials is prepared according to Mass Calculation: volume ratio is methylsulphonic acid, acetic acid, the mixing solutions 30 parts of hydrochloric acid, 10 parts, solubility tetrathio molybdic acid tin, dodecyl sulphate barium 14 parts, 4 parts, laking agent, dispersion agent 6 parts, brightening agent 4 parts, impurity elimination sequestering agent 5 parts, 2 parts, the tensio-active agent of 5:1:2,25 parts, water;
(2) water of 1/3rd amounts is got, slowly add the mixing solutions of the methylsulphonic acid of aequum, acetic acid, hydrochloric acid while stirring, the laking agent of aequum is added when solution temperature is down to room temperature, stir the brightening agent and the dispersion agent that add aequum after leaving standstill 10min, mixing and stirring becomes mixed solution A stand-by; The storing temp of mixed solution A is not higher than 40 degrees Celsius;
(3) before plating, mixed solution A prepared by step (2) is put into plating tank, regulate pH to 5.0-6.0, add the water of 1/3rd amounts again, then solubility tetrathio molybdic acid tin and the dodecyl sulphate barium of aequum is added, add the impurity elimination sequestering agent of aequum and the water of tensio-active agent and surplus after mixing and stirring deposition 20min, be stirred into required electroplate liquid stand-by.
Described laking agent for epoxy chloropropane and ammonium chloride chitosan mass ratio be the mixture of 2:3; Described dispersion agent is polyacrylic acid and EDTA mass ratio is the mixture of 3:1; Described brightening agent is the mixture of citric acid, cocinic acid, silicone oil, dodecyl poly glucoside, and the mass ratio of four kinds of materials should be 2:2:1:3 mutually; Described impurity elimination sequestering agent is acidic cpd; Described tensio-active agent is aniorfic surfactant.
Embodiment 4:
The industrial Tin plating technique of employing standard carries out the preparation of sample: plating substrate is the Cu lead frame of C19210, and temperature of electroplating solution is 30 ~ 55 DEG C, and electroplating efficiency is 600/h, and plating, without stirring, then carries out 150 DEG C, the high temperature anneal of 1h; Test is divided into four groups, electroplate liquid prepared by the electroplate liquid adopting the preparation method of above-described embodiment 1-3 to be prepared into and traditional Pure Tin Plating Process liquid and preparation method thereof is electroplated respectively, the coating mean thickness that after plating, x-ray fluorescence analyzer is measured is 10 ~ 12 microns, tin palpus growth experiment under Thermal cycling conditions have employed the accelerated test method of JEDEC201, its parameter is :-55 DEG C (+0/-10 DEG C) ~+85 DEG C (+10/-0 DEG C), atmospheric environment, in 3 circulation/h. experimentations, often after experience 500 circulations, just observe the growth of tin palpus; Carry out 1500 circulations altogether, observe the growth conditions of three tin palpuses.
Result is as shown in the table:
Can find out from upper table, use the electroplate liquid that a kind of preparation method reducing the long electroplate liquid of coating tin one of the main divisions of the male role in traditional opera of embodiment of the present invention 1-3 is prepared from, compared with traditional electrical plating solution service condition, obvious to the growth inhibitory effect of tin palpus, greatly reduce the growth velocity of tin palpus, reduce the growth of plated item surface tin palpus, and use the electroplate liquid that is prepared from of the present invention to carry out electroplating rear coating to there is snappiness and ductility is good, to the appearance of coating crackle, there is good mitigation, comparatively flexible to temperature capacity, there is very strong practical value.
Should be understood that, above embodiment is only not used in for illustration of the present invention and limits the scope of the invention, after having read the present invention, the amendment of those skilled in the art to the various equivalent form of value of the present invention has all fallen within the application's claims limited range.
Claims (8)
1. reduce a preparation method for the long electroplate liquid of coating tin one of the main divisions of the male role in traditional opera, it is characterized in that comprising the following steps:
(1) following raw materials is prepared according to Mass Calculation: volume ratio is the methylsulphonic acid of 5:1:2, acetic acid, mixing solutions 20-40 part of hydrochloric acid, solubility tetrathio molybdic acid tin 8-12 part, dodecyl sulfate 12-15 part, laking agent 2-6 part, dispersion agent 3-8 part, brightening agent 3-5 part, impurity elimination sequestering agent 4-6 part, tensio-active agent 1-3 part, water 20-30 part.
(2) water of 1/3rd amounts is got, slowly add the mixing solutions of the methylsulphonic acid of aequum, acetic acid, hydrochloric acid while stirring, the laking agent of aequum is added when solution temperature is down to room temperature, stir the brightening agent and the dispersion agent that add aequum after leaving standstill 10min, mixing and stirring becomes mixed solution A stand-by;
(3) before plating, mixed solution A prepared by step (2) is put into plating tank, regulate pH to 5.0-6.0, add the water of 1/3rd amounts again, then solubility tetrathio molybdic acid tin and the dodecyl sulfate of aequum is added, add the impurity elimination sequestering agent of aequum and the water of tensio-active agent and surplus after mixing and stirring deposition 20min, be stirred into required electroplate liquid stand-by.
2. the preparation method of the electroplate liquid that reduction coating tin one of the main divisions of the male role in traditional opera according to claim 1 is long, is characterized in that: described dodecyl sulfate is the one in ammonium salt, sodium salt, sylvite, barium salt.
3. the preparation method of the electroplate liquid that reduction coating tin one of the main divisions of the male role in traditional opera according to claim 1 is long, is characterized in that: described laking agent for epoxy chloropropane and ammonium chloride chitosan mass ratio be the mixture of 2:3.
4. the preparation method of the electroplate liquid that reduction coating tin one of the main divisions of the male role in traditional opera according to claim 1 is long, is characterized in that: described dispersion agent is polyacrylic acid and EDTA mass ratio is the mixture of 2:1-5:1.
5. the preparation method of the electroplate liquid that reduction coating tin one of the main divisions of the male role in traditional opera according to claim 1 is long, it is characterized in that: described brightening agent is the mixture of citric acid, cocinic acid, silicone oil, dodecyl poly glucoside, and the mass ratio of four kinds of materials should be 2:2:1:3 mutually.
6. the preparation method of the electroplate liquid that reduction coating tin one of the main divisions of the male role in traditional opera according to claim 1 is long, is characterized in that: described impurity elimination sequestering agent is acidic cpd.
7. the preparation method of the electroplate liquid that reduction coating tin one of the main divisions of the male role in traditional opera according to claim 1 is long, is characterized in that: described tensio-active agent is aniorfic surfactant.
8. the preparation method of the electroplate liquid that reduction coating tin one of the main divisions of the male role in traditional opera according to claim 1 is long, is characterized in that: the storing temp of described mixed solution A is not higher than 40 degrees Celsius.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201510981821.2A CN105506680A (en) | 2015-12-23 | 2015-12-23 | Preparation method of electroplating liquid for reducing growth of plating layer tin whisker |
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| CN201510981821.2A CN105506680A (en) | 2015-12-23 | 2015-12-23 | Preparation method of electroplating liquid for reducing growth of plating layer tin whisker |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106835208A (en) * | 2016-12-15 | 2017-06-13 | 中国航空工业集团公司北京航空材料研究院 | A kind of high-efficiency environment friendly without cyanogen sulfate zinc plating solution |
| CN108103540A (en) * | 2018-01-24 | 2018-06-01 | 永星化工(上海)有限公司 | Tin alloy electric plating liquid |
| CN112064069A (en) * | 2020-08-17 | 2020-12-11 | 云南春城档案用品有限公司 | Environment-friendly bright tin plating treatment process method |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106835208A (en) * | 2016-12-15 | 2017-06-13 | 中国航空工业集团公司北京航空材料研究院 | A kind of high-efficiency environment friendly without cyanogen sulfate zinc plating solution |
| CN108103540A (en) * | 2018-01-24 | 2018-06-01 | 永星化工(上海)有限公司 | Tin alloy electric plating liquid |
| CN112064069A (en) * | 2020-08-17 | 2020-12-11 | 云南春城档案用品有限公司 | Environment-friendly bright tin plating treatment process method |
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