CN104087983A - Sulfate bright tin-electroplating solution - Google Patents
Sulfate bright tin-electroplating solution Download PDFInfo
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- CN104087983A CN104087983A CN201410305060.4A CN201410305060A CN104087983A CN 104087983 A CN104087983 A CN 104087983A CN 201410305060 A CN201410305060 A CN 201410305060A CN 104087983 A CN104087983 A CN 104087983A
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- tin
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- sulfate
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Abstract
The invention relates to a sulfate bright tin-electroplating solution capable of obviously enhancing the properties of the plating solution and coating in the bright tin-electroplating process. The additives comprise benzalacetone, formaldehyde and ascorbic acid. The solution is composed of 35-55 g/L stannous sulfate, 90-110 g/L 98% sulfuric acid, 0.2-0.4 g/L benzalacetone, 4-7 mL/L formaldehyde, 7-10 g/L ascorbic acid, 3-4 granules/L tin granules and the balance of deionized water. The sulfate tin-electroplating solution has the advantages of no toxicity, no harm and low price; the special additives contained in the sulfate tin-electroplating solution can improve the stability of the tin-electroplating solution, enhance the quality of the tin coating and prolong the service life of the electroplating solution; and the tin coating has the advantages of bright and smooth surface, very flat crystal grains and ordered arrangement.
Description
Technical field
The present invention relates to a kind of solution of vitriol bright plating tin, can significantly improve plating solution and coating performance in bright plating process of tin.
Background technology
Because it can suppress, tin one of the main divisions of the male role in traditional opera is long to be used as the solderable coating of high-quality for a long time tinsel, (ROHS) pass through because of " about being limited in the instruction that uses some objectionable constituent in electronic and electrical equipment " at present, the use of metallic lead is subject to strict restriction, this will affect the use range of tinsel, therefore unleaded pure tin coating is come into one's own gradually, it is also a kind of high-quality solderable coating, is widely used in electronics and foodstuffs industry.In acid tin plating technique with being most widely used of vitriol eleetrotinplate, its advantage is that composition is simple, easy to maintenance, sedimentation velocity is fast, coating is bright, leveling property and weldability good; Its shortcoming is that plating solution is unstable, easily oxidized, and coating easily long tin must and make electronic product produce potential safety hazard.
Though have many eleetrotinplate specialist additives at present domestic, eleetrotinplate performance is made moderate progress, not only price is high, and heat resistance and antioxidant property ideal not enough, also easily causes environmental pollution.
Summary of the invention
The problem existing for existing eleetrotinplate technology, the object of the present invention is to provide a kind of solution of vitriol bright plating tin, wherein contain special additive, this additive can effectively improve plating solution performance, extends bath life, improve quality of coating, for the fast development of eleetrotinplate technique provides important technical guarantee.
Technical scheme of the present invention: a kind of solution of vitriol bright plating tin, the additive containing is benzylideneacetone, formaldehyde and xitix; Composition and content are as follows: stannous sulfate is 35-55g/L, and 98% sulfuric acid is 90-110g/L, and benzylideneacetone is 0.2-0.4g/L, and formaldehyde is 4-7mL/L, and xitix is 7-10g/L, and tin grain is 3-4 grain/L, and all the other are deionized water.
A solution for vitriol bright plating tin, its working temperature is 15-40 DEG C, working current density is 1.5-2.5A/dm
2.
The collocation method of plating solution: to the deionized water that adds 500ml in 1 liter of plating tank, then add successively the weigh vitriol oil (98%) and stannous sulfate accurately, stirring and dissolving, to join in electroplate liquid with the benzylideneacetone that OP emulsifying agent was processed, add the formaldehyde of accurate weighing, add the xitix of accurate weighing, add some tin grains; Finally be settled to 1L with deionized water.
Because the main salt of plating solution of the present invention is stannous sulfate, stannous ion is easy to oxidized, and especially under high-temperature condition, Bivalent Tin is easy to be oxidized to tetravalent tin.
In plating solution, there are following 2 reaction process:
O
2+4H
++2Sn
2+→2Sn
4++2H
2O (1)
Sn+Sn
4+→2Sn
2+ (2)
Reaction formula (1) makes plating solution oxidation, and reaction formula (2) makes plating solution protected.Two reactions all belong to heterogeneous reaction, plating solution contacts with air and makes dissolved oxygen in plating solution, or in plating solution, there are other oxidizing substances, capital makes the speed of reaction formula (1) be greater than reaction formula (2), although there is tin anode plate to exist, but along with time lapse, plating solution still can be by slow oxidation, is also Sn
2+be oxidized to Sn
4+, Sn
4+after concentration accumulation rises to a certain degree, due to Sn
4+hydrolytic action is greater than Sn
2+, hydrolysis then produces hydrolysis dregs (β-stannic acid that alpha tin acid is transformed into).Hydrolytic process is as shown in the formula shown in (3):
Sn
4++4H
2O→Sn(OH)
4+4H
+ (3)
Sn (OH)
4β-the stannic acid being finally converted into by alpha tin acid, β-stannic acid is a kind of material that is insoluble to acid or alkali, thereby makes Bath mudding.
Therefore can in solution, place a little tin grain oxidized to prevent divalent tin ion.
The present invention is a kind of nontoxic, harmless, cheap vitriol the solution of electrotinning, the special additive containing, can improve the stability of eleetrotinplate plating solution and the quality of raising tin coating, has extended bath life, the surface-brightening of tin coating is level and smooth, and crystal grain is very smooth, arrangement is orderly.For the development of eleetrotinplate technique provides powerful technical support, this is a great advantage to be restricted the solderable coating being affected because of lead.
Brief description of the drawings
Fig. 1 is the effect photo of the tin coating after the embodiment of the present invention 1 is electroplated.
Fig. 2 is the electromicroscopic photograph of the tin coating after the embodiment of the present invention 1 is electroplated.
Fig. 3 is the cathodic polarization curve figure of the embodiment of the present invention 1 plating solution;
In Fig. 3: the non-additive plating tin liquor of A-; The plating tin liquor that B-contains additive.
Fig. 4 is the effect photo of the tin coating after the embodiment of the present invention 5 is electroplated.
Fig. 5 is the electromicroscopic photograph of the tin coating after the embodiment of the present invention 5 is electroplated.
Embodiment
The present invention is intended to explore the additive of wide material sources, with low cost, environmentally safe, to obtain a kind of vitriol eleetrotinplate plating solution of uniqueness, to improve plating solution performance and to improve quality of coating.
The overall craft flow process of acid electroplating tin is as follows:
Oil removing → washing → rust cleaning → washing → plating → washing → water seal → dry up → inspection → product, the present invention is applied in electroplating work procedure.
Below by embodiment, the present invention is elaborated.
Embodiment 1
First prepare electroplate liquid, to the deionized water that adds 500ml in 1 liter of plating tank, then add successively the accurate concentration of weighing and be 98% vitriol oil 100g, stannous sulfate 40g, the benzylideneacetone 0.3g processing with OP emulsifying agent, formaldehyde 6mL, xitix 8g, is finally settled to 1L with deionized water.
After placing some tin grains (3-4 grain/L) in the above-mentioned electroplate liquid preparing, can utilize this plating solution to carry out eleetrotinplate.Sheet tin is made anode, and iron plate is made negative electrode, and temperature is that 20 DEG C, current density are 2A/dm
2, the treatment time is 30 seconds.
Fig. 1, Fig. 2 are pictorial diagram and the electron-microscope scanning figure that obtains eleetrotinplate, from this two figure, can find out that the surface-brightening of tin coating is level and smooth, and crystal grain is very smooth, arrangement is orderly.As can be seen from Figure 3, this special additive can effectively improve the polarized action of negative electrode, makes coating careful, thereby can obtain tin coating careful, bright and that dispersive ability is strong.
The stability of plating solution is good, places at normal temperatures and pressures and within 30 days, does not become muddy, still can carry out eleetrotinplate at the temperature of 40 DEG C, and current efficiency reaches 98.5%.
Embodiment 2
First to the deionized water that adds 500ml in 1 liter of plating tank, then adding successively the accurate concentration of weighing is 98% vitriol oil 100g, stannous sulfate 40g, after processing benzylideneacetone with OP emulsifying agent, join in electroplate liquid, benzylideneacetone 0.2g, formaldehyde 4mL, xitix 7g, is finally settled to 1L with deionized water.
After placing some tin grains (3-4 grain/L) in the above-mentioned electroplate liquid preparing, can utilize this plating solution to carry out eleetrotinplate.Sheet tin is made anode, and iron plate is made negative electrode, and temperature is that 20 DEG C, current density are 2A/dm
2, the treatment time is 30 seconds.
The coating surface light obtaining is level and smooth, and crystal grain is smooth, and the stability of plating solution is also better in order, places at normal temperatures and pressures and within 30 days, does not become muddy, still can carry out eleetrotinplate at the temperature of 40 DEG C, and current efficiency reaches 93.5%.
Embodiment 3
Prepare electroplate liquid by mode similarly to Example 1, wherein, the vitriol oil 100g/L that concentration is 98%, stannous sulfate 40g/L, does not add benzylideneacetone, formaldehyde and xitix.
After placing some tin grains (3-4 grain/L) in the above-mentioned electroplate liquid preparing, can utilize this plating solution to carry out eleetrotinplate.Sheet tin is anode, and iron plate is negative electrode, and temperature is that 20 DEG C, current density are 2A/dm
2, the treatment time is 30 seconds.
It is coarse, brightless that the tin coating obtaining by embodiment 3 shows, quality of coating is poor, and plating solution just had turbid phenomenon to occur after 24 hours.
Embodiment 4
First to the deionized water that adds 500ml in 1 liter of plating tank, then adding successively the accurate concentration of weighing is 98% vitriol oil 100g, stannous sulfate 40g, after processing benzylideneacetone with OP emulsifying agent, join in electroplate liquid, benzylideneacetone 0.5g, formaldehyde 8mL, xitix 11g, is finally settled to 1L with deionized water.
After placing some tin grains (3-4 grain/L) in the above-mentioned electroplate liquid preparing, can utilize this plating solution to carry out eleetrotinplate.Sheet tin is made anode, and iron plate is made negative electrode, and temperature is that 20 DEG C, current density are 2A/dm
2, the treatment time is 30 seconds.
The most of light of coating surface obtaining is level and smooth, but brightless in some place of part, the corner of coating, most of crystal grain is smooth, and the stability of plating solution is also better in order, places at normal temperatures and pressures and within 30 days, does not become muddy, and current efficiency reaches 96.3%.
Embodiment 5
Prepare electroplate liquid by mode similarly to Example 1, wherein, the vitriol oil 100g/L that concentration is 98%, stannous sulfate 40g/L, benzylideneacetone 0.4g/L, formaldehyde 6mL/L, xitix 8g/L.
After placing some tin grains (3-4 grain/L) in the above-mentioned electroplate liquid preparing, can utilize this plating solution to carry out eleetrotinplate.Sheet tin is anode, and iron plate is negative electrode, and temperature is that 35 DEG C, current density are 2A/dm
2, the time is 30 seconds.
On the basis of embodiment 1, after increasing benzylideneacetone content and increasing temperature to 35 DEG C, the tin coating of acquisition as shown in Figure 4, Figure 5, can find out that the surface-brightening of tin coating is level and smooth from pictorial diagram and electron-microscope scanning figure, and crystal grain is very smooth, arrange in order.The stability of plating solution is also better, can continuous electroplating 14 days, and current efficiency reaches 95.3%.
Embodiment 6
Prepare electroplate liquid by mode similarly to Example 1, wherein, the vitriol oil 120g/L that concentration is 98%, stannous sulfate 60g/L, benzylideneacetone 0.4g/L, formaldehyde 6mL/L, xitix 8g/L.
After placing some tin grains (3-4 grain/L) in the above-mentioned electroplate liquid preparing, can utilize this plating solution to carry out eleetrotinplate.Sheet tin is anode, and iron plate is negative electrode, and temperature is that 20 DEG C, current density are 2A/dm
2, the time is 30 seconds.
The coating surface light obtaining, but crystallization is thicker, and bath stability is also poor.
Embodiment 7
Prepare electroplate liquid by mode similarly to Example 1, wherein, the vitriol oil 80g/L that concentration is 98%, stannous sulfate 30g/L, benzylideneacetone 0.4g/L, formaldehyde 6mL/L, xitix 8g/L.
After placing some tin grains (3-4 grain/L) in the above-mentioned electroplate liquid preparing, can utilize this plating solution to carry out eleetrotinplate.Sheet tin is anode, and iron plate is negative electrode, and temperature is that 20 DEG C, current density are 2A/dm
2, the time is 30 seconds.
The coating surface part light obtaining, some place does not plate metallic tin.
Embodiment 8
Prepare electroplate liquid by mode similarly to Example 1, wherein, the vitriol oil 100g/L that concentration is 98%, stannous sulfate 40g/L, benzylideneacetone 0.3g/L, formaldehyde 6mL/L, xitix 8g/L.
After placing some tin grains (3-4 grain/L) in the above-mentioned electroplate liquid preparing, can utilize this plating solution to carry out eleetrotinplate.Sheet tin is anode, and iron plate is negative electrode, and temperature is that 20 DEG C, current density are 1.0A/dm
2, the time is 30 seconds.
The coating surface part light obtaining, some place does not plate metallic tin.
Embodiment 9
Prepare electroplate liquid by mode similarly to Example 1, wherein, the vitriol oil 100g/L that concentration is 98%, stannous sulfate 40g/L, benzylideneacetone 0.3g/L, formaldehyde 6mL/L, xitix 8g/L.
After placing some tin grains (3-4 grain/L) in the above-mentioned electroplate liquid preparing, can utilize this plating solution to carry out eleetrotinplate.Sheet tin is anode, and iron plate is negative electrode, and temperature is that 20 DEG C, current density are 2.8A/dm
2, the time is 30 seconds.
The coating surface part light obtaining, has black splotch to occur at edge, and has fringe phenomena to produce.
Claims (3)
1. a solution for vitriol bright plating tin, is characterized in that: the additive containing is benzylideneacetone, formaldehyde and xitix; Composition and content are as follows: stannous sulfate is 35-55g/L, and 98% sulfuric acid is 90-110g/L, and benzylideneacetone is 0.2-0.4g/L, and formaldehyde is 4-7mL/L, and xitix is 7-10g/L, and tin grain is 3-4 grain/L, and all the other are deionized water.
2. the solution of a kind of vitriol bright plating tin according to claim 1, is characterized in that: its working temperature is 15-40 DEG C, and working current density is 1.5-2.5A/dm
2.
3. the solution of a kind of vitriol bright plating tin according to claim 1, it is characterized in that: optimum parameter is: adding by every 1 liter of the solution of electrotinning the accurate concentration of weighing is 98% vitriol oil 100g, stannous sulfate 40g, the benzylideneacetone 0.3g processing with OP emulsifying agent, formaldehyde 6mL, xitix 8g, all the other are deionized water, in the above-mentioned electroplate liquid preparing, place tin grain 3-4 grain/L.
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| CN201410305060.4A CN104087983A (en) | 2014-06-30 | 2014-06-30 | Sulfate bright tin-electroplating solution |
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|---|---|---|---|
| CN201410305060.4A CN104087983A (en) | 2014-06-30 | 2014-06-30 | Sulfate bright tin-electroplating solution |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105734620A (en) * | 2016-03-11 | 2016-07-06 | 深圳市松柏实业发展有限公司 | Tin stripping and tin plating liquid, preparing method of tin stripping and tin plating liquid and cyclic regeneration method for adopting tin stripping and tin plating liquid for recycling metal tin |
| CN106835210A (en) * | 2017-03-09 | 2017-06-13 | 昆明理工大学 | A kind of sulfate bright tin plating solution and preparation method thereof |
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| WO2006078549A1 (en) * | 2005-01-21 | 2006-07-27 | Technic, Inc. | Pulse plating process for deposition of gold-tin alloy |
| CN101962790A (en) * | 2010-08-20 | 2011-02-02 | 河南科技大学 | Electrolyte composition for half bright acid tinning |
| CN102995072A (en) * | 2012-10-30 | 2013-03-27 | 南通汇丰电子科技有限公司 | Tinning solution for copper-clad steel wire |
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2014
- 2014-06-30 CN CN201410305060.4A patent/CN104087983A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2006078549A1 (en) * | 2005-01-21 | 2006-07-27 | Technic, Inc. | Pulse plating process for deposition of gold-tin alloy |
| CN101962790A (en) * | 2010-08-20 | 2011-02-02 | 河南科技大学 | Electrolyte composition for half bright acid tinning |
| CN102995072A (en) * | 2012-10-30 | 2013-03-27 | 南通汇丰电子科技有限公司 | Tinning solution for copper-clad steel wire |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105734620A (en) * | 2016-03-11 | 2016-07-06 | 深圳市松柏实业发展有限公司 | Tin stripping and tin plating liquid, preparing method of tin stripping and tin plating liquid and cyclic regeneration method for adopting tin stripping and tin plating liquid for recycling metal tin |
| CN106835210A (en) * | 2017-03-09 | 2017-06-13 | 昆明理工大学 | A kind of sulfate bright tin plating solution and preparation method thereof |
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Application publication date: 20141008 |
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