CN106498453A - A kind of brightener of tin plating, tin alloy and its preparation method and application - Google Patents
A kind of brightener of tin plating, tin alloy and its preparation method and application Download PDFInfo
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- CN106498453A CN106498453A CN201610822767.1A CN201610822767A CN106498453A CN 106498453 A CN106498453 A CN 106498453A CN 201610822767 A CN201610822767 A CN 201610822767A CN 106498453 A CN106498453 A CN 106498453A
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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
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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
- C25D3/56—Electroplating: Baths therefor from solutions of alloys
- C25D3/60—Electroplating: Baths therefor from solutions of alloys containing more than 50% by weight of tin
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- Electroplating And Plating Baths Therefor (AREA)
Abstract
The invention discloses a kind of brightener of tin plating, tin alloy and its preparation method and application, per liter of component comprising following content：10～30g/L of polyethylene glycol, A 120～200g/L of agent, B 120～200g/L of agent, 2 2～4g/L of mercaptothiazoline, 100～180g/L of potassium hydroxide solution that mass concentration is 5%, and surplus distilled water；A agent is epoxy imidazoles amine aqueous solution；B agent is the mixed solution of PVP and Sodium Benzoate.Preparation method is 1) to add 200～500g of distilled water in a container；2) 10～30g polyethylene glycol, heating is added to stir to being completely dissolved to transparent, cool down；3) A 120～200g of agent are added while stirring；4) B 120～200g of agent are added while stirring；5) 2 2～4g of mercaptothiazoline are weighed, will be added in the 4) solution after the dissolving of 2 mercaptothiazolines with 100～180g of potassium hydroxide solution that mass concentration is 5%；6) distilled water is added to 1000ml constant volumes, stir.In application, 5～80g brighteners in every liter of plating solution, are added.Brightener of the present invention is added in plating solution, and plating solution can be made stable in properties, and coating performance is good.
Description
Technical field
The present invention relates to field of metal surface treatment, specially a kind of brightener of tin plating, tin alloy and preparation method thereof
And application.
Background technology
In the electronics industry, the requirement to bright tin plating and tin alloy is very strict, should not only meet conventional adhesion
Good, crystallize outside many requirements such as careful smooth, fragility is low, solderability is good, also require coating Wuxi palpus, without leak source, pin hole, fiber crops
Point；Plating solution is also answered that deposition velocity is fast, can be worked under higher temperature conditionss；Because then solution is easily muddy, heavy more than 30 DEG C
Shallow lake, Sn4+Easily produce, and produce Deposit appearance therewith and assume vaporific, greyness and have pin hole, pit, or even have whisker to produce.
This will bring greatly harm to microelectronic circuits.
Current tin plating and during tin alloy is industrial, mainly tin plating with stannous salt, and during Bivalent Tin is tin plating, by
In raw material bring into and anode on electrochemical anodic oxidation, cause plating solution extremely unstable, it is impossible to effectively suppress stannic
Produce, tetravalence tin ion accumulates more and more, after certain concentration is reached, will result in cathode efficiency decline, plating solution dispersion
Ability, coating is coarse and the problems such as have tin produce.
In the tin plating and tin alloy electric plating of microelectronics industry and information industry, to the bright property of coating, smooth type, dispersion
Property, corner without whisker require very harsh；This just has higher requirement to brightener used in plating solution.Can be used as light
The material of the brightener of plating Sn or Sn alloys is a lot, but nothing more than being and the ketone group containing containing aldehyde radical, such as benzaldehyde, cinnamic acid
Class material, such as benzene methylene acetone etc., then be aided with the sodium salt of one sodium salt of aryl or the double aryl of connection etc..The brightener of these composition compositions
There is good light effect, also there is to the dispersive property of plating solution preferably help, but significantly defect be not suitable for higher
Liquid temperature.During higher temperature, consumption is too fast, and causes coating fragility to increase, and solderability declines.
Content of the invention
The present invention is in place of the deficiencies in the prior art, there is provided a kind of brightener of tin plating, tin alloy and its preparation side
Method and application, the brightener cause tin plating electrolyte or plating Sn Alloy Plating Bath stable in properties, during tin plating or tin alloy, negative electrode
Current efficiency is stable, and plating solution is uniformly dispersed, and coating performance is good, and Wuxi must produce.
The present invention is adopted the following technical scheme that：
A kind of brightener of tin plating, tin alloy, it is characterised in that per liter of component comprising following content：Polyethylene glycol 10
～30g/L, A 120～200g/L of agent, B 120～200g/L of agent, 2～4g/L of 2-mercaptothiazoline, the hydrogen-oxygen that mass concentration is 5%
Change 100～180g/L of potassium solution, and surplus distilled water；
The A agent is epoxy imidazoles amine aqueous solution；
The B agent is the mixed solution of PVP and Sodium Benzoate.
The preferred version is, a kind of brightener of tin plating, tin alloy, it is characterised in that per liter comprising following content
Component：Polyethylene glycol 20g/L, A agent 160g/L, B agent 160g/L, 2-mercaptothiazoline 3g/L, the hydroxide that mass concentration is 5%
Potassium solution 150g/L；And surplus distilled water.
The molecular weight of the polyethylene glycol is 6000～12000.
A kind of method of the brightener for preparing tin plating, tin alloy, it is characterised in that complete as follows：
1) add 200～500g of distilled water in a container；
2) 10～30g polyethylene glycol, heating is added to stir to being completely dissolved to transparent, cool down；
3) A 120～200g of agent are added while stirring；
4) B 120～200g of agent are added while stirring；
5) 2～4g of 2-mercaptothiazoline is weighed, with 100～180g of potassium hydroxide solution that mass concentration is 5% by 2- mercaptos
It is added in the 4) solution after the dissolving of base thiazoline；
6) distilled water is added to 1000ml constant volumes, stir, the brightener of tin plating, tin alloy.
The A agent is prepared as follows：
1) dimethylamine agueous solution, 20～40g imidazoles that 200～400g mass concentrations are 33% are taken successively and is added to reaction bulb
In；
2) mixer is started, uses heating in water bath for reaction bottle；
3) when temperature of charge is at 55-65 DEG C in reaction bulb, stop heating, be added dropwise 180-200g's with dropping funel
Epoxychloropropane, under stirring, at the uniform velocity time for adding is more than 60 minutes；
4), after dripping, stir 20～40 minutes at remaining at 55-65 DEG C；
5) solution temperature in reaction bulb is risen to 85-95 DEG C, BFEE 1 is injected into reaction bulb with syringe
～3g, continues stirring 45-60 minutes；
6) stop stirring and heat, naturally cool to room temperature, extraction product, as A agent.
The B agent is prepared as follows：
1) 5～15g PVPs are weighed to be placed in a container, 200-250g, 55-65 DEG C distillation is added
Water, is placed on slightly hot on electric furnace, stirring, until PVP is completely dissolved, cools down；
2) 80～120g Sodium Benzoates are put in another container, add 300～500g, 55-65 DEG C of distilled water, plus
Heat of solution Sodium Benzoate is until fully transparent, cooling；
3) 1) mix described with 2) solution, distilled water is added to 1000ml constant volumes, stirred, as B agent.
The brightener of the tin plating, tin alloy is in electroplating bright Sn plating solutions and Sn-Pb, Sn-Zn, Sn-Co-Zn, Sn-
Application in Ni, Si-Bi alloy electroplating bath, it is characterised in that add brightener described in 5～80g in every liter of plating solution.
Beneficial effects of the present invention are：The brightener of tin plating, tin alloy of the present invention, not only suppresses tin plating solution, plating
Sn in Sn Alloy Plating Bath2+Oxidation, to Sn2+There is good stabilization, also to Sn4+There is stronger reduction, can will be molten
Already present Sn in liquid4+Sn is effectively reduced to2+；And can to solution in floating outstanding thing have coagulative precipitation function, it is ensured that solution
Long-time transparent；Organic matter also to being harmful in plating solution has masking action.Brightener component is polyethylene glycol, epoxy imidazoles
Amine, PVP, Sodium Benzoate, 2-mercaptothiazoline, potassium hydroxide, without poisonous aldehydes matter, in brightener
When component substance is used alone, it is impossible to reach the effect of stable plating solution, be only used in combination, i.e., depositing jointly when side in the plating solution makes
Plating solution is highly stable, during tin plating or tin alloy, cathode efficiency is stable for the plating solution added with brightener, plating solution point
Dissipate uniformly, coating bright property, uniformity, mildness are good, and Wuxi must produce.
Specific embodiment
Again the present invention is described further with reference to embodiments：
Embodiment 1
Prepare brightener：
(1) A agent, the i.e. agent of epoxy aminoimidazole are first prepared, and step is as follows：
1) take the dimethylamine agueous solution of 300g 33%, 30g imidazoles successively to be added in reaction bulb；
2) mixer is started, is heated with water-bath at leisure；
3) when temperature of charge is at 60 DEG C in reaction bulb, heating, the epoxy that 190g is slowly added dropwise with dropping funel are stopped
Chloropropane, under stirring, at the uniform velocity time for adding is more than 60 minutes；
4), after dripping, remain at；
5) solution temperature in reaction bulb is risen to 90 DEG C, BFEE 2g is injected into reaction bulb with syringe, after
Continuous stirring 50 minutes；
6) stop stirring and heat, naturally cool to room temperature, extraction product obtains light yellow, viscous liquid,
As A agent.
(2) mixed solution of B agent, i.e. PVP and Sodium Benzoate is prepared again, and step is as follows：
1) 10g PVPs are weighed to be placed in a container, 200g, 60 DEG C distilled water is added, is placed on electric furnace
On slightly hot, stirring, until PVP is completely dissolved, cool down；
2) 100g Sodium Benzoates are put in another container, 400g, 60 DEG C distilled water are added, and heating for dissolving is until complete
All-transparent, cooling；
3) 1) mixed with 2) solution, distilled water is added to 1000ml, stirred, as B agent.
(3) A agent and B agent are configured to brightener according to the following steps finally：
1) add distilled water 300g in a container；
2) 20g polyethylene glycol (M=12000) is added, slightly hot, stir transparent to being completely dissolved, be cooled to transparent；
3) 160gA agent is added while stirring；
4) 160gB agent is added while stirring；
5) 3g2- mercaptothiazolines are weighed, is added in above-mentioned liquid after being dissolved with the potassium hydroxide solution of 150g5%；
6) distilled water is added to 1000ml, stirred, that is, obtain brightener of the present invention.
The component of per liter of gained brightener is：Polyethylene glycol 20g/L, A agent 160g/L, B agent 160g/L, 2-mercaptothiazoline
3g/L, mass concentration are 5% potassium hydroxide solution 150g/L；And surplus distilled water.
Embodiment 2
Prepare brightener：
(1) A agent, the i.e. agent of epoxy aminoimidazole are first prepared, and step is as follows：
1) take the dimethylamine agueous solution of 200g 33%, 20g imidazoles successively to be added in reaction bulb；
2) mixer is started, is heated with water-bath at leisure；
3) when temperature of charge is at 55 DEG C in reaction bulb, heating, the epoxy that 180g is slowly added dropwise with dropping funel are stopped
Chloropropane, under stirring, at the uniform velocity time for adding is more than 60 minutes；
4), after dripping, remain at；
5) solution temperature in reaction bulb is risen to 85 DEG C, BFEE 1g is injected into reaction bulb with syringe, after
Continuous stirring 45 minutes；
6) stop stirring and heat, naturally cool to room temperature, extraction product obtains light yellow, viscous liquid,
As A agent.
(2) mixed solution of B agent, i.e. PVP and Sodium Benzoate is prepared again, and step is as follows：
1) 5g PVPs are weighed to be placed in a container, 250g, 55 DEG C distilled water is added, is placed on electric furnace
Slightly hot, stirring, until PVP is completely dissolved, is cooled down；
2) 80g Sodium Benzoates are put in another container, 300g, 55 DEG C distilled water are added, and heating for dissolving is until complete
All-transparent, cooling；
3) 1) mixed with 2) solution, distilled water is added to 1000ml, stirred, as B agent.
(3) A agent and B agent are configured to brightener according to the following steps finally：
1) add distilled water 400g in a container；
2) 10g polyethylene glycol (M=8000) is added, slightly hot, stir transparent to being completely dissolved, be cooled to transparent；
3) 120gA agent is added while stirring；
4) 120gB agent is added while stirring；
5) 2g2- mercaptothiazolines are weighed, is added in above-mentioned liquid after being dissolved with the potassium hydroxide solution of 100g5%；
6) distilled water is added to 1000ml, stirred, that is, obtain brightener of the present invention.
The component of per liter of gained brightener is：Polyethylene glycol 10g/L, A agent 120g/L, B agent 120g/L, 2-mercaptothiazoline
2g/L, mass concentration are 5% potassium hydroxide solution 100g/L；And surplus distilled water.
Embodiment 3
Prepare brightener：
(1) A agent, the i.e. agent of epoxy aminoimidazole are first prepared, and step is as follows：
1) take the dimethylamine agueous solution of 400g 33%, 40g imidazoles successively to be added in reaction bulb；
2) mixer is started, is heated with water-bath at leisure；
3) when temperature of charge is at 65 DEG C in reaction bulb, heating, the epoxy that 200g is slowly added dropwise with dropping funel are stopped
Chloropropane, under stirring, at the uniform velocity time for adding is more than 60 minutes；
4), after dripping, remain at；
5) solution temperature in reaction bulb is risen to 95 DEG C, BFEE 3g is injected into reaction bulb with syringe, after
Continuous stirring 60 minutes；
6) stop stirring and heat, naturally cool to room temperature, extraction product obtains light yellow, viscous liquid,
As A agent.
(2) mixed solution of B agent, i.e. PVP and Sodium Benzoate is prepared again, and step is as follows：
1) 15g PVPs are weighed to be placed in a container, 250g, 65 DEG C distilled water is added, is placed on electric furnace
On slightly hot, stirring, until PVP is completely dissolved, cool down；
2) 120g Sodium Benzoates are put in another container, 500g, 65 DEG C distilled water are added, and heating for dissolving is until complete
All-transparent, cooling；
3) 1) mixed with 2) solution, distilled water is added to 1000ml, stirred, as B agent.
(3) A agent and B agent are configured to brightener according to the following steps finally：
1) add distilled water 500g in a container；
2) 30g polyethylene glycol (M=6000) is added, slightly hot, stir transparent to being completely dissolved, be cooled to transparent；
3) 200gA agent is added while stirring；
4) 200gB agent is added while stirring；
5) 4g2- mercaptothiazolines are weighed, is added in above-mentioned liquid after being dissolved with the potassium hydroxide solution of 180g5%；
6) distilled water is added to 1000ml, stirred, that is, obtain brightener of the present invention.
The component of per liter of gained brightener is：Polyethylene glycol 30g/L, A agent 200g/L, B agent 200g/L, 2-mercaptothiazoline
4g/L, mass concentration are 5% potassium hydroxide solution 180g/L；And surplus distilled water.
The application of brightener：
Brightener is added to the amount in different plating solutions：
A. electroplating bright tin plating solution (Sn) solution (pH：5～6；T：Room temperature；Dk(A/dm2)：0.2～30)：Stannous sulfate
30g/L；Sulfuric acid (d=1.84,96%) 70g/L；Stabilizer 80-100g/L；Brightener 50-80g/L.
B. electroplating bright tin-lead (Sn-Pb) alloy solution (pH：5～6；T room temperatures；Dk(A/dm2)：2～10)：Sodium citrate
90-110g/L；Ethylenediamine tetra-acetic acid 30-35g/L；Ammonium acetate 40-60g/L；Boric acid 25-35g/L；Lead acetate 10-15g/L；Chlorine
Change stannous 40-60g/L；Stabilizer 80-100g/L；Brightener 50-80g/L；
C. electroplating bright tin zinc (Sn-Zn) alloy solution (pH：5～6；T：5～35 DEG C；Dk(A/dm2)：1～3.5)：Lemon
Lemon acid trisodium 80-100g/L；Ammonium acetate 45-55g/L；Ethylenediamine tetra-acetic acid 25-35g/L；Stannous chloride 40-50g/L；Zinc chloride
60-80g/L；Stabilizer 80-100g/L；Brightener 50-80g/L.
D. electroplating bright tin cobalt zinc (Sn-Co-Zn) alloy solution (pH：4～6；T：5～35 DEG C；Dk(A/dm2)：0.5～
5.0)：Trisodium citrate 100-150g/L；Disodium ethylene diamine tetraacetate 20-30g/L；Stannous chloride 15-20g/L；Cobaltous sulfate 25-
35g/L；Zinc chloride 15-20g/L；Stabilizer 60-100g/L；Brightener 5-20g/L.
E. electroplating bright tin nickel (Sn-Ni) alloy solution (pH：3～4；T：30～40 DEG C；Dk(A/dm2)：1～3)：Lemon
Sour trisodium 90-110g/L；Disodium ethylene diamine tetraacetate 30-40g/L；Stannous chloride 20-30g/L；Nickel sulfate 250-300g/L；Sugar
Smart 2g/L；Lauryl sodium sulfate 0.2g/L；Stabilizer 50-80g/L；Brightener：40-60g/L.
F. electroplating bright tin (Sn-Bi) alloy solution (pH：4.0～4.5；T：10～30 DEG C；Dk(A/dm2)：0.5～
1.5)：Trisodium citrate 100-120g/L；Ethylenediamine tetra-acetic acid 30-40g/L；Stannous sulfate 25-30g/L；Boric acid 30-40g/L；
Polyethylene glycol (6000) 2-3g/L；Sour sodium 3-5g/L；Stabilizer 20-30g/L；Brightener：20-30g/L.
The brightener of tin plating, tin alloy of the present invention so that plating solution during tin plating or tin alloy, cathode current
Stabilised efficiency, plating solution are uniformly dispersed, and coating bright property, uniformity, mildness are good, and Wuxi must produce.In addition, light of the present invention
Bright dose does not contain poisonous aldehydes matter, safety and environmental protection.
Claims (7)
1. a kind of brightener of tin plating, tin alloy, it is characterised in that per liter of component comprising following content：Polyethylene glycol 10～
30g/L, A 120～200g/L of agent, B 120～200g/L of agent, 2～4g/L of 2-mercaptothiazoline, the hydroxide that mass concentration is 5%
100～180g/L of potassium solution, and surplus distilled water；
The A agent is epoxy imidazoles amine aqueous solution；
The B agent is the mixed solution of PVP and Sodium Benzoate.
2. the brightener of a kind of tin plating, tin alloy according to claim 1, it is characterised in that per liter includes following content
Component：Polyethylene glycol 20g/L, A agent 160g/L, B agent 160g/L, 2-mercaptothiazoline 3g/L, the hydrogen-oxygen that mass concentration is 5%
Change potassium solution 150g/L；And surplus distilled water.
3. the brightener of tin plating, tin alloy according to claim 1 and 2, it is characterised in that the molecule of the polyethylene glycol
Measure as 6000～12000.
4. a kind of method of tin plating, tin alloy the brightener prepared described in claim 1, it is characterised in that by following step
Suddenly complete：
1) add 200～500g of distilled water in a container；
2) 10～30g polyethylene glycol, heating is added to stir to being completely dissolved to transparent, cool down；
3) A 120～200g of agent are added while stirring；
4) B 120～200g of agent are added while stirring；
5) 2～4g of 2-mercaptothiazoline is weighed, with 100～180g of potassium hydroxide solution that mass concentration is 5% by 2- sulfydryl thiophenes
It is added in the 4) solution after oxazoline dissolving；
6) distilled water is added to 1000ml constant volumes, stirred, obtain final product the brightener of tin plating, tin alloy.
5. the method for the brightener for preparing tin plating, tin alloy according to claim 4, it is characterised in that the A agent is by such as
Prepared by lower step：
1) take dimethylamine agueous solution, 20～40g imidazoles that 200～400g mass concentrations are 33% successively to be added in reaction bulb；
2) mixer is started, uses heating in water bath for reaction bottle；
3) when temperature of charge is at 55-65 DEG C in reaction bulb, stop heating, the epoxy that 180-200g is added dropwise with dropping funel
Chloropropane, under stirring, at the uniform velocity time for adding is more than 60 minutes；
4), after dripping, stir 20～40 minutes at remaining at 55-65 DEG C；
5) solution temperature in reaction bulb is risen to 85-95 DEG C, 1～3g of BFEE is injected with syringe into reaction bulb,
Continue stirring 45-60 minutes；
6) stop stirring and heat, naturally cool to room temperature, extraction product, as A agent.
6. according to the method for the brightener for preparing tin plating, tin alloy described in claim 4, it is characterised in that the B agent is pressed
Prepared by following steps：
1) 5～15g PVPs are weighed to be placed in a container, 200-250g, 55-65 DEG C distilled water is added,
Slightly hot on electric furnace, stirring is placed on, until PVP is completely dissolved, is cooled down；
2) 80～120g Sodium Benzoates are put in another container, 300～500g, 55-65 DEG C of distilled water is added, and are heated molten
Solution Sodium Benzoate is until fully transparent, cooling；
3) 1) mix described with 2) solution, distilled water is added to 1000ml constant volumes, stirred, as B agent.
7. the brightener of tin plating, tin alloy according to claim 1 electroplating bright Sn plating solutions and Sn-Pb, Sn-Zn,
Application in Sn-Co-Zn, Sn-Ni, Si-Bi alloy electroplating bath, it is characterised in that add described in 5～80g in every liter of plating solution
Brightener.
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Cited By (1)
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| CN112915911A (en) * | 2021-01-26 | 2021-06-08 | 浙江科宝新材料科技有限公司 | Brightener processing method |
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| CN112915911A (en) * | 2021-01-26 | 2021-06-08 | 浙江科宝新材料科技有限公司 | Brightener processing method |
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