CN105369302A - Preparation method for electroplating solution for inhibiting copper exposure of tinned copper wire - Google Patents
Preparation method for electroplating solution for inhibiting copper exposure of tinned copper wire Download PDFInfo
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- CN105369302A CN105369302A CN201510981575.0A CN201510981575A CN105369302A CN 105369302 A CN105369302 A CN 105369302A CN 201510981575 A CN201510981575 A CN 201510981575A CN 105369302 A CN105369302 A CN 105369302A
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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
- C25D3/32—Electroplating: Baths therefor from solutions of tin characterised by the organic bath constituents used
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- Electroplating Methods And Accessories (AREA)
- Electroplating And Plating Baths Therefor (AREA)
Abstract
The invention discloses a preparation method for an electroplating solution for inhibiting copper exposure of a tinned copper wire. According to the prepared method, an acidic plating solution adopting a mixed solution comprising chlorosulfonic acid, acetic acid and chromic acid, a tin salt adopting a mixed solution comprising stannous monosulphate and dodecyl sulfate, a fixing agent, a reducing agent, a brightening agent, a masking agent, a surfactant and the like are mixed in an optimized manner to be prepared into the electroplating solution; compared with application of the conventional electroplating solution, the electroplating solution is obvious in inhibition effect on copper exposure phenomenon; a plating layer subjected to electroplating through the electroplating solution is high in flexibility and ductility, and good in the plating solution flowing performance; the electroplating solution has an excellent relaxation effect on appearing of plating layer cracks, is relatively flexible in temperature tolerance, and has a very high practical value.
Description
Technical field
The present invention relates to metal plating galvanic deposit preparation field, particularly relate to a kind of preparation method suppressing tinned wird to reveal the electroplate liquid of copper.
Background technology
In wires and cables industry, rubber insulation mine cable, retardant cable of locomotives, shipboard cable and aircraft lac cable, and the shield braid etc. of electric wire generally uses tinned wird.Copper cash effectively can be prevented after copper wire tin-plating to be oxidized blackening, and to be clamminess problem with the rubber that rubber contacts causes, improve the work-ing life of cable and the weldability of conductor wire core.At present, the mode of production of China's line cable industry tinned wird, mainly contains hot tinning and eleetrotinplate two kinds.Hot tinning technique is simple, and equipment cost is low, but the main characteristic of tin-plated product quality: tack and continuity are all difficult to ensure, are not suitable for the product that specification of quality is high, and production small dimension tinned wird easily breaks, and joint is many, is difficult to ensure production with fixed lengths.Eleetrotinplate technique is more complicated, and quality product is better, and material usage is few, is more suitable for producing small dimension and the high product of quality requirements.But copper cash due to the impact of electroplate liquid and other related factors, easily causes dew copper when electrolytic tinning, produce scrap wire, waste starting material, make the manufacturing cost of product increase.
Therefore, how to prepare a kind of suitable electroplate liquid and just seem of crucial importance with the generation avoided or suppress tinned wird to reveal copper phenomenon.
Summary of the invention
Goal of the invention: in order to solve in the copper cash eleetrotinplate technique existing for prior art the problem revealed copper phenomenon and occur, the invention provides the preparation method that a kind of electroplating effect is good, dew copper phenomenon is had to the electroplate liquid of detailed inhibiting suppression tinned wird dew copper.
Technical scheme: for achieving the above object, the present invention adopts following technical scheme: a kind of preparation method suppressing tinned wird to reveal the electroplate liquid of copper, comprises the following steps:
(1) following raw materials is prepared according to Mass Calculation: volume ratio is the chlorsulfonic acid of 6:1:2, acetic acid, mixing solutions 30-50 part of chromic acid, stannous sulfate 10-16 part, dodecyl sulfate 10-14 part, laking agent 4-8 part, reductive agent 1-3 part, brightening agent 6-8 part, sequestering agent 5-9 part, tensio-active agent 1-3 part, water 30-40 part;
(2) water of 1/3rd amounts is got, slowly add the mixing solutions of the chlorsulfonic acid of aequum, acetic acid, chromic acid while stirring, the laking agent of aequum is added when solution temperature is down to room temperature, stir the brightening agent and the reductive agent that add aequum after leaving standstill 20min, 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 4.0-5.5, add the water of 1/3rd amounts again, then stannous sulfate and the dodecyl sulfate of aequum is added, add the sequestering agent of aequum and the water of tensio-active agent and surplus after mixing and stirring deposition 30min, 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 1:3.
More preferred, described reductive agent is metallic reducing agent.
More preferred, described brightening agent is the mixture of citric acid, tartaric acid, silicone oil, dodecyl poly glucoside, and the mass ratio of four kinds of materials should be 2:1:1:2 mutually.
More preferred, described sequestering agent is halfcystine, Padil, tartrate three mass ratio are the mixture of 2:1:2.
More preferred, described tensio-active agent is nonionic surface active agent.
More preferred, the storing temp of described mixed solution A is not higher than 40 degrees Celsius.
Beneficial effect: a kind of preparation method suppressing tinned wird to reveal the electroplate liquid of copper provided by the present invention, acidic bath adopts chlorsulfonic acid, acetic acid, the mixing solutions of chromic acid, pink salt adopts the mixing solutions of stannous sulfate and dodecyl sulfate, and with the addition of laking agent, reductive agent, brightening agent, sequestering agent, the compositions such as tensio-active agent, above-mentioned each composition is prepared into electroplate liquid according to the electroplate liquid preparation method optimized, compared with the application of traditional electrical plating solution, obvious to dew copper phenomenon inhibition, and use the present invention to carry out electroplating rear coating to there is snappiness and ductility is good, the effect that plating solution go-bit performance 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:
Suppress tinned wird to reveal a preparation method for the electroplate liquid of copper, comprise the following steps:
(1) following raw materials is prepared according to Mass Calculation: volume ratio is chlorsulfonic acid, acetic acid, the mixing solutions 30 parts of chromic acid, stannous sulfate 10 parts, sodium lauryl sulphate 10 parts, 4 parts, laking agent, reductive agent 1 part, brightening agent 6 parts, sequestering agent 5 parts, 1 part, the tensio-active agent of 6:1:2,30 parts, water;
(2) water of 1/3rd amounts is got, slowly add the mixing solutions of the chlorsulfonic acid of aequum, acetic acid, chromic acid while stirring, the laking agent of aequum is added when solution temperature is down to room temperature, stir the brightening agent and the reductive agent that add aequum after leaving standstill 20min, mixing and stirring becomes mixed solution A stand-by, and 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 4.0-5.5, add the water of 1/3rd amounts again, then add aequum stannous sulfate and, sodium lauryl sulphate, add the sequestering agent of aequum and the water of tensio-active agent and surplus after mixing and stirring deposition 30min, be stirred into required electroplate liquid stand-by.
Wherein, described laking agent for epoxy chloropropane and ammonium chloride chitosan mass ratio be the mixture of 1:3; Described reductive agent is metallic reducing agent; Described brightening agent is the mixture of citric acid, tartaric acid, silicone oil, dodecyl poly glucoside, and the mass ratio of four kinds of materials should be 2:1:1:2 mutually; Described sequestering agent is halfcystine, Padil, tartrate three mass ratio are the mixture of 2:1:2; Described tensio-active agent is nonionic surface active agent.
Embodiment 2:
Suppress tinned wird to reveal a preparation method for the electroplate liquid of copper, comprise the following steps:
(1) following raw materials is prepared according to Mass Calculation: volume ratio is chlorsulfonic acid, acetic acid, the mixing solutions 50 parts of chromic acid, stannous sulfate 16 parts, dodecyl sulphate barium 14 parts, 8 parts, laking agent, reductive agent 3 parts, brightening agent 8 parts, sequestering agent 9 parts, 3 parts, the tensio-active agent of 6:1:2,40 parts, water;
(2) water of 1/3rd amounts is got, slowly add the mixing solutions of the chlorsulfonic acid of aequum, acetic acid, chromic acid while stirring, the laking agent of aequum is added when solution temperature is down to room temperature, stir the brightening agent and the reductive agent that add aequum after leaving standstill 20min, mixing and stirring becomes mixed solution A stand-by, and 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 4.0-5.5, add the water of 1/3rd amounts again, then stannous sulfate and the dodecyl sulphate barium of aequum is added, add the sequestering agent of aequum and the water of tensio-active agent and surplus after mixing and stirring deposition 30min, be stirred into required electroplate liquid stand-by.
Wherein, described laking agent for epoxy chloropropane and ammonium chloride chitosan mass ratio be the mixture of 1:3; Described reductive agent is metallic reducing agent; Described brightening agent is the mixture of citric acid, tartaric acid, silicone oil, dodecyl poly glucoside, and the mass ratio of four kinds of materials should be 2:1:1:2 mutually; Described sequestering agent is halfcystine, Padil, tartrate three mass ratio are the mixture of 2:1:2; Described tensio-active agent is nonionic surface active agent.
Embodiment 3:
Suppress tinned wird to reveal a preparation method for the electroplate liquid of copper, comprise the following steps:
(1) following raw materials is prepared according to Mass Calculation: volume ratio is chlorsulfonic acid, acetic acid, the mixing solutions 40 parts of chromic acid, stannous sulfate 13 parts, 12 parts, dodecyl sulphate potassium, 6 parts, laking agent, reductive agent 2 parts, brightening agent 7 parts, sequestering agent 7 parts, 2 parts, the tensio-active agent of 6:1:2,35 parts, water;
(2) water of 1/3rd amounts is got, slowly add the mixing solutions of the chlorsulfonic acid of aequum, acetic acid, chromic acid while stirring, the laking agent of aequum is added when solution temperature is down to room temperature, stir the brightening agent and the reductive agent that add aequum after leaving standstill 20min, mixing and stirring becomes mixed solution A stand-by, and 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 4.0-5.5, add the water of 1/3rd amounts again, then stannous sulfate and the dodecyl sulphate potassium of aequum is added, add the sequestering agent of aequum and the water of tensio-active agent and surplus after mixing and stirring deposition 30min, be stirred into required electroplate liquid stand-by.
Wherein, described laking agent for epoxy chloropropane and ammonium chloride chitosan mass ratio be the mixture of 1:3; Described reductive agent is metallic reducing agent; Described brightening agent is the mixture of citric acid, tartaric acid, silicone oil, dodecyl poly glucoside, and the mass ratio of four kinds of materials should be 2:1:1:2 mutually; Described sequestering agent is halfcystine, Padil, tartrate three mass ratio are the mixture of 2:1:2; Described tensio-active agent is nonionic surface active agent.
Embodiment 4:
Choose the bare copper wire of four groups of identical materials and specification, adopt following electroplating technology flow process: unwrapping wire → alkali cleaning → clear water flushing → pickling → plating → clear water rinses → dry up → take-up → wire drawing, annealing → take-up (finished product); Wherein electroplating process take embodiment 1-3 to prepare electroplate liquid test, another group adopts traditional electroplate liquid to carry out electroplating processes, concrete electroplating processes process is, first electroplate liquid is prepared, copper cash leaching after front and continued art breading is embedded in electroplate liquid, and applies certain voltage at negative electrode and anode and carry out electroplating processes.
After above-mentioned process, the copper cash finished product of embodiment 1-3 test group and traditional electrical plating solution process control group is carried out an acceptance inspection, result shows, and the plating finished product dew copper phenomenon incidence of embodiment 1-3 is 1%-4%, and coating surface is smooth, ductility and snappiness better, plating solution go-bit performance is good, and traditional control group dew copper phenomenon is up to more than 30%, and coating crystallization is coarse, embrittlement, produces striped and true hole.
From the above results, a kind of preparation method suppressing tinned wird to reveal the electroplate liquid of copper of the present invention is obvious to dew copper phenomenon inhibition, and use the present invention to carry out electroplating rear coating to there is snappiness and ductility is good, the effect that plating solution go-bit performance 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. suppress tinned wird to reveal a preparation method for the electroplate liquid of copper, it is characterized in that comprising the following steps:
(1) following raw materials is prepared according to Mass Calculation: volume ratio is the chlorsulfonic acid of 6:1:2, acetic acid, mixing solutions 30-50 part of chromic acid, stannous sulfate 10-16 part, dodecyl sulfate 10-14 part, laking agent 4-8 part, reductive agent 1-3 part, brightening agent 6-8 part, sequestering agent 5-9 part, tensio-active agent 1-3 part, water 30-40 part;
(2) water of 1/3rd amounts is got, slowly add the mixing solutions of the chlorsulfonic acid of aequum, acetic acid, chromic acid while stirring, the laking agent of aequum is added when solution temperature is down to room temperature, stir the brightening agent and the reductive agent that add aequum after leaving standstill 20min, 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 4.0-5.5, add the water of 1/3rd amounts again, then stannous sulfate and the dodecyl sulfate of aequum is added, add the sequestering agent of aequum and the water of tensio-active agent and surplus after mixing and stirring deposition 30min, be stirred into required electroplate liquid stand-by.
2. the preparation method of the electroplate liquid of suppression tinned wird dew copper according to claim 1, 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 of suppression tinned wird according to claim 1 dew copper, is characterized in that: described laking agent for epoxy chloropropane and ammonium chloride chitosan mass ratio be the mixture of 1:3.
4. the preparation method of the electroplate liquid of suppression tinned wird dew copper according to claim 1, is characterized in that: described reductive agent is metallic reducing agent.
5. the preparation method of the electroplate liquid of suppression tinned wird dew copper according to claim 1, is characterized in that: described brightening agent is the mixture of citric acid, tartaric acid, silicone oil, dodecyl poly glucoside, and the mass ratio of four kinds of materials should be 2:1:1:2 mutually.
6. the preparation method of the electroplate liquid of suppression tinned wird dew copper according to claim 1, is characterized in that: described sequestering agent is halfcystine, Padil, tartrate three mass ratio are the mixture of 2:1:2.
7. the preparation method of the electroplate liquid of suppression tinned wird dew copper according to claim 1, is characterized in that: described tensio-active agent is nonionic surface active agent.
8. the preparation method of the electroplate liquid of suppression tinned wird dew copper according to claim 1, 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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| CN201510981575.0A CN105369302A (en) | 2015-12-23 | 2015-12-23 | Preparation method for electroplating solution for inhibiting copper exposure of tinned copper wire |
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| CN201510981575.0A CN105369302A (en) | 2015-12-23 | 2015-12-23 | Preparation method for electroplating solution for inhibiting copper exposure of tinned copper wire |
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| CN201510981575.0A Pending CN105369302A (en) | 2015-12-23 | 2015-12-23 | Preparation method for electroplating solution for inhibiting copper exposure of tinned copper wire |
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Cited By (2)
| 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 |
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| CN104060307A (en) * | 2014-06-30 | 2014-09-24 | 句容市博远电子有限公司 | Pure tin electroplating solution for inhibiting growth of tin whiskers and application thereof |
| CN104894617A (en) * | 2015-06-19 | 2015-09-09 | 司徒建辉 | Electroplating solution for bright silver plating |
| CN104911640A (en) * | 2015-06-17 | 2015-09-16 | 黄惠娟 | Electroplating liquid for electroplating treatment |
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2015
- 2015-12-23 CN CN201510981575.0A patent/CN105369302A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103422130A (en) * | 2012-05-14 | 2013-12-04 | 中国科学院金属研究所 | Plating solution and method for electroplating bright tin plating layer |
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| CN104894617A (en) * | 2015-06-19 | 2015-09-09 | 司徒建辉 | Electroplating solution for bright silver plating |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| 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 |
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Application publication date: 20160302 |