CN109055921A - A kind of electroless plated tin liquor and preparation method thereof - Google Patents
A kind of electroless plated tin liquor and preparation method thereof Download PDFInfo
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- CN109055921A CN109055921A CN201810981724.7A CN201810981724A CN109055921A CN 109055921 A CN109055921 A CN 109055921A CN 201810981724 A CN201810981724 A CN 201810981724A CN 109055921 A CN109055921 A CN 109055921A
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- electroless plated
- tin liquor
- plated tin
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- stabilizer
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/52—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating using reducing agents for coating with metallic material not provided for in a single one of groups C23C18/32 - C23C18/50
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- General Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
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- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
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- Chemically Coating (AREA)
Abstract
The present invention relates to a kind of electroless plated tin liquor and preparation method thereof, the electroless plated tin liquor is made of pink salt, promotor, wetting agent and stabilizer;Pink salt mass concentration is 5~20g/L, and promotor mass concentration is 30~200g/L, and wetting agent mass concentration is 0.1~0.5g/L, and stabilizer mass concentration is 50~170g/L;In reasonable concentration under the when synergistic effect of each component, electroless plated tin liquor of the invention is highly stable, and coating uniform compact is bright in half, and it is not high using operating temperature, at 35~45 DEG C, for 10~15min of plating thickness of coating up to 1.5~2 μm or so, plating weldability is good.
Description
Technical field
The invention belongs to field of surface treatment, and in particular to a kind of electroless plated tin liquor and preparation method thereof.
Background technique
Current electronics industry, with the fast development of SMD technology, thinner more complicated route is more and more appeared in
On pcb board, everything all requires that pcb board is uniform, flat, and can be by long-term storage and multiple temperature cycles
Still there is splendid solderability afterwards.In the past few years, PCB industry is seeking always a kind of ideal final coating side
Method.Although having several alternative techniques have passed through test, but without there is a kind of really ideal final coating
Process.In final panel processing problem, it is exactly hot air solder level technique that people, which discuss at most, but with regard to its technique sheet
For body, its process is complicated, with high costs, and the panel processed is also and unsatisfactory.Chemical nickel gold is due in Wire-
Advantage in terms of the connection surface that bonding and high-quality require, so also possessing certain occupation rate of market.But chemical nickel gold
Higher cost, technique controlling difficulty is larger.Organic coating (OSP) may is that a kind of method for solving the problems, such as this, but very much
In the case of, the coating only to metallize is just able to satisfy certain strict requirements.There is very good solution in the method for electroless plated tin
The problem, the process costs are moderate, and maintenance cost is low, technology difficulty is low, can in the hole of the pcb board of any size, even
The position for connecing disk uniformly covers one layer of tin.However that there are service lifes is short for electroless plated solution of tin, process stability difference
Problem needs to solve.
Summary of the invention
In view of this, the purpose of the present invention is to provide a kind of stable electroless plated tin liquor of performance and the chemistry
The preparation method of immersion plating tin liquor.
In order to achieve the above objectives, the invention provides the following technical scheme:
1. a kind of electroless plated tin liquor, consists of the following compositions: pink salt, promotor, wetting agent and stabilizer.
Further, the pink salt is one or more of stannous sulfate, stannous methanesulfonate, stannous chloride mixture.
Further, the pink salt mass concentration is 5~20g/L.
Further, the promotor is made of thiocarbamide and fluoride;
Or thiourea derivative and fluoride form.
Further, the promotor mass concentration is 30~200g/L.
Further, the thiourea derivative is methylthiourea, dimethyl sulfourea, tetramethyl thiourea, one in ethyl thiourea
Kind or several mixtures, the fluoride are sodium fluoride and/or ammonium acid fluoride.
Further, the thiocarbamide or thiourea derivative mass concentration are 30~200g/L, the mass concentration of the fluoride
For 0.01~1g/L.
Further, the wetting agent is polyethylene glycol, fatty alcohol polyoxyethylene ether, alkyl phenol polyoxyethylene ether one kind or several
The mixture of kind.
Further, the mass concentration of the wetting agent is 0.1~0.5g/L.
Further, the stabilizer is sulfuric acid, methane sulfonic acid, citric acid, tartaric acid one or more mixture, stabilizer
Mass concentration be 50~100g/L.
2. the preparation method of any of the above item electroless plated tin liquor, comprising the following steps: by stabilizer deionization
Water dissolution, is added promotor, stirring and dissolving;Add wetting agent, stirring and dissolving;It is eventually adding pink salt, stirring and dissolving, then constant volume
It can be prepared by the electroless plated tin liquor to required volume.
The beneficial effects of the present invention are: electroless plated tin liquor of the invention is highly stable, and coating uniform compact is in semi-gloss
Bright and not high using operating temperature, at 35~45 DEG C, 10~15min of plating thickness of coating is up to 1.5~2 μm or so, plating
Layer solderability is good.The stability of electroless plated tin liquor of the invention relies primarily on pink salt, promotor, wetting agent and stabilizer exist
Synergistic effect under certain matched proportion density, pink salt provide tin metal ion;Promotor is adjusted for surface, controls Sn2+Reduction
Rate makes the more uniform densification of coating, and univalent copper ion is also complexed in promotor, reduces Cu+The electrode potential of/Cu makes the electrode
Current potential is lower than Sn2+The electrode potential of/Sn realizes Sn2+Reduction displacement, to realize film forming;And fluorine ion also has promotion
The effect of film forming;Wetting agent reduces surface tension, and plating solution is made to be easier wetted workpieces surface, so that plating leakage is prevented, coating piebald
Etc. failures;Stabilizer further prevents Sn4+Generation;Prevent Sn2+Hydrolysis.Stabilizer is very crucial in electroless plated tin,
If not good stabilizer, 5~10h or so will occur muddy after plating solution is prepared, and plating solution is caused to scrap.Stabilizer can make simultaneously
It reacts softer, prevents uneven coating even;Sn2+, Sn4+Respectively have a common boundary acid and hard acid, they all with the affinity of hard base
It is relatively strong, more stable complex can be formed, electroless plated tin liquor formula of the invention is so as to preventing Sn2+It replaces and restores at interface
When, because of the coating floating failure that interface state variation causes, bath stability is greatly improved, the plating solution newly prepared is carrying out greatly
After area plating, it is still limpid to place 1 month or so plating solution.Electroless plated tin liquor of the invention solves existing chemical tin plating liquor
The technical problems such as operating temperature height has damage to substrate, and bath stability is poor, and coating is easy floating, and thickness of coating is thin.
Detailed description of the invention
In order to keep the purpose of the present invention, technical scheme and beneficial effects clearer, the present invention provides following attached drawing and carries out
Illustrate:
Fig. 1 is the test piece outside drawing of embodiment 1;
Fig. 2 is the state diagram after the consumption experiment of the electroless plated tin liquor of embodiment 1;
Fig. 3 is the test piece outside drawing of embodiment 2;
Fig. 4 is the state diagram after the consumption experiment of the electroless plated tin liquor of embodiment 2;
Fig. 5 is the test piece outside drawing of embodiment 3;
Fig. 6 is the state diagram after the consumption experiment of the electroless plated tin liquor of embodiment 3.
Specific embodiment
Below in conjunction with attached drawing, a preferred embodiment of the present invention will be described in detail.It is not specified in embodiment specific
The experimental method of condition, usually according to conventional conditions or according to the manufacturer's recommendations.
Embodiment 1
The electroless plated tin liquor of the present embodiment includes following component by concentration: pink salt 20g/L, promotor 80g/L, wetting agent
0.2g/L, stabilizer 170g/L;Wherein: the pink salt is stannous methanesulfonate 20g/L;The promotor is thiocarbamide 80g/L, fluorine
Change hydrogen ammonium 0.1g/L;The wetting agent is alkyl phenol polyoxyethylene ether 0.2g/L, and the stabilizer is methane sulfonic acid 150g/L, wine
Stone acid 20g/L.
The preparation method of the electroless plated tin liquor of the present embodiment, includes the following steps:
(1) methane sulfonic acid and 20g tartaric acid for using 500ml deionized water dissolving 150g, are stirred well to dissolution;
(2) 80g thiocarbamide and 0.1g ammonium acid fluoride are added into above-mentioned solution, is stirred well to dissolution;
(3) 0.2g alkyl phenol polyoxyethylene ether is added, dissolution is stirred well to;
(4) electroless plated tin liquor: using 200ml deionized water dissolving 20g stannous methanesulfonate, after stirring to clarify, to
Mixed liquor made from (1) (2) (3) step is wherein added, stirs evenly, then can be prepared by institute using deionized water constant volume to 1L
State electroless plated tin liquor.
Wherein step (1) (2) (3) can respectively with being remixed after deionized water dissolving, can also be added sequentially to from
It is dissolved in sub- water, is eventually adding pink salt;Pink salt can be first with being added, before can also being directly added into after deionized water dissolving
Mixed liquor in.
The electroless plated tin liquor requirement of the present embodiment: operating temperature is 40 DEG C, plating time 10min.
The electroless plated tin liquor of the present embodiment is tested:
1, the appearance of coating, thickness and solderability detection:
Test method: the electroless plated tin liquor that 250mL the present embodiment is obtained is put into beaker, and constant temperature is to 40 DEG C, with purple
Copper test piece examination plating 10min, observes Deposit appearance, detects thickness of coating and solderability;
Test result: as shown in Figure 1, uniform half bright coating is obtained, no floating, plating leakage sign;Plating 10min plates thickness
Degree and solderability are as shown in table 1:
1 embodiment of table, 1 test piece performance
The chemical tin plating liquor operating temperature is 35~45 DEG C;It is preferred that operating temperature is 40 DEG C;Temperature it is excessive or too small
Significant impact can be generated to quality of coating and treatment effeciency.
2, bath stability:
Test method: the electroless plated tin liquor that 1000mL the present embodiment is obtained is put into beaker, and constant temperature is carried out to 40 DEG C
Consumption experiment, consumes the foundation of experiment: 1, coating is qualified;2, solution system is stablized.I.e. on the basis for meeting both the above condition
Upper plating test piece, with the consumption of plating solution, when reaching to greatest extent, coating performance and solution system will change, and disappear at this time
Consumption terminates, and solution is scrapped.Processing experiment test piece 1m2Afterwards, the stability state of plating solution is being handled as shown in Fig. 2, bath stability is good
After large area test piece, and during plating a large amount of water is brought in test piece into, plating solution is still limpid, and no turbidity and precipitation generates.
Embodiment 2
The electroless plated tin liquor of the present embodiment includes following component by concentration: pink salt 10g/L, promotor 80g/L, wetting agent
0.2g/L, stabilizer 170g/L;
Wherein: the pink salt is stannous sulfate 10g/L;The promotor is methylthiourea 80g/L, sodium fluoride 0.1g/L;
The wetting agent is polyethylene glycol (M=600) 0.2g/L, and the stabilizer is methane sulfonic acid 150g/L, tartaric acid 20g/L;This
The preparation method of the electroless plated tin liquor of embodiment, includes the following steps:
(1) methane sulfonic acid quantitative using deionized water dissolving, is stirred well to dissolution;
(2) quantitative methylthiourea and sodium fluoride are added into above-mentioned solution, is stirred well to dissolution;
(3) quantitative polyethylene glycol is added, dissolution is stirred well to;
(4) electroless plated tin liquor: finally stannous sulfate is added in mixed liquor made from (1) (2) (3) step, stirring makes
It is dissolved, and then can be prepared by the electroless plated tin liquor using deionized water constant volume.
The electroless plated tin liquor requirement of the present embodiment:
The operating temperature of the electroplate liquid of the present embodiment is 40 DEG C, plating time 10min.
The electroless plated tin liquor of the present embodiment is tested:
1, the appearance of coating, thickness and solderability detection:
Test method: the electroless plated tin liquor that 250mL the present embodiment is obtained is put into beaker, and constant temperature is to 40 DEG C, with purple
Copper test piece examination plating 10min, observes Deposit appearance, detects thickness of coating and solderability;
Test result: as shown in figure 3, uniform half bright coating is obtained, no floating, plating leakage sign;Plating 10min plates thickness
Degree and solderability are as shown in table 2:
2 embodiment of table, 2 test piece performance
2, bath stability:
Test method: the electroless plated tin liquor that 1000mL the present embodiment is obtained is put into beaker, and constant temperature is carried out to 40 DEG C
Consumption experiment, processing experiment test piece 1m2The stability state of plating solution is as shown in figure 4, bath stability is good, in processing large area examination afterwards
After piece, and during plating a large amount of water is brought in test piece into, plating solution is still limpid, and no turbidity and precipitation generates.
Embodiment 3
The electroless plated tin liquor of the present embodiment includes following component by concentration: pink salt 15g/L, promotor 80g/L, wetting agent
0.2g/L, stabilizer 120g/L;
Wherein: the pink salt is stannous chloride 15g/;The promotor is thiocarbamide 80g/L, ammonium acid fluoride 0.1g/L.It is described
Wetting agent is alkyl phenol polyoxyethylene ether 0.2g/L, and the stabilizer is sulfuric acid 100g/L, citric acid 20g/L;The present embodiment
The preparation method of electroless plated tin liquor, includes the following steps:
(1) sulfuric acid quantitative using deionized water dissolving, is stirred well to dissolution;
(2) quantitative thiocarbamide and ammonium acid fluoride are added into above-mentioned solution, is stirred well to dissolution;
(3) quantitative alkyl phenol polyoxyethylene ether is added, dissolution is stirred well to;
(4) electroless plated tin liquor: quantitative stannous chloride is added in mixed liquor made from (1) (2) (3) step, sufficiently
It stirs to dissolve, then can be prepared by the electroless plated tin liquor using deionized water constant volume.
The electroless plated tin liquor requirement of the present embodiment:
The operating temperature of the electroplate liquid of the present embodiment is 40 DEG C, plating time 10min.
The electroless plated tin liquor of the present embodiment is tested:
1, the appearance of coating, thickness and solderability detection:
Test method: the electroless plated tin liquor that 250mL the present embodiment is obtained is placed in a beaker, and constant temperature is to 40 DEG C, with purple
Copper test piece examination plating 10min, observes Deposit appearance, detects thickness of coating and solderability;
Test result: as shown in figure 5, uniform half bright coating is obtained, no floating, plating leakage sign;Plating 10min plates thickness
Degree and solderability are as shown in table 3:
3 embodiment of table, 3 test piece performance
2, bath stability:
Test method: the electroless plated tin liquor that 1000mL the present embodiment is obtained is placed in a beaker, and constant temperature is carried out to 40 DEG C
Consumption experiment, processing experiment test piece 1m2The stability state of plating solution is as shown in fig. 6, bath stability is good, in processing large area examination afterwards
After piece, and during plating a large amount of water is brought in test piece into, plating solution is still limpid, and no turbidity and precipitation generates.
Finally, it is stated that preferred embodiment above is only used to illustrate the technical scheme of the present invention and not to limit it, although logical
It crosses above preferred embodiment the present invention is described in detail, however, those skilled in the art should understand that, can be
Various changes are made to it in form and in details, without departing from claims of the present invention limited range.
Claims (10)
1. a kind of electroless plated tin liquor, which is characterized in that consist of the following compositions: pink salt, promotor, wetting agent and stabilizer.
2. electroless plated tin liquor according to claim 1, it is characterised in that: the pink salt is stannous sulfate, methane sulfonic acid
One or more of stannous, stannous chloride mixture.
3. electroless plated tin liquor according to claim 1, it is characterised in that: the pink salt mass concentration is 5~20g/L.
4. electroless plated tin liquor according to claim 1, it is characterised in that: the promotor is by thiocarbamide and fluoride group
At;
Or thiourea derivative and fluoride form.
5. electroless plated tin liquor according to claim 4, it is characterised in that: the thiourea derivative is methylthiourea, two
One or more of methylthiourea, tetramethyl thiourea, ethyl thiourea mixture, the fluoride are sodium fluoride and/or fluorination
Hydrogen ammonium.
6. electroless plated tin liquor according to claim 4, it is characterised in that: the thiocarbamide or thiourea derivative mass concentration
For 30~200g/L, the mass concentration of the fluoride is 0.01~1g/L.
7. electroless plated tin liquor according to claim 1, it is characterised in that: the wetting agent is polyethylene glycol, fatty alcohol
The mixture of polyoxyethylene ether, alkyl phenol polyoxyethylene ether one or more.
8. electroless plated tin liquor according to claim 1, it is characterised in that: the mass concentration of the wetting agent be 0.1~
0.5g/L。
9. electroless plated tin liquor according to claim 1, it is characterised in that: the stabilizer is sulfuric acid, methane sulfonic acid, lemon
Lemon acid, tartaric acid one or more mixture, the mass concentration of stabilizer are 50~170g/L.
10. the preparation method of any one of the claim 1~9 electroless plated tin liquor, which comprises the following steps:
By stabilizer deionized water dissolving, promotor, stirring and dissolving is added;Add wetting agent, stirring and dissolving;It is eventually adding tin
Salt, stirring and dissolving, then be settled to required volume and can be prepared by the electroless plated tin liquor.
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CN110306213B (en) * | 2019-07-08 | 2020-08-04 | 广州三孚新材料科技股份有限公司 | Tin plating solution for solar cell and preparation method thereof |
CN111690918A (en) * | 2020-07-29 | 2020-09-22 | 昆山汇荣电子材料有限公司 | Tinning method for copper wire for producing tinned copper stranded wire |
CN112144048A (en) * | 2020-09-21 | 2020-12-29 | 广州三孚新材料科技股份有限公司 | Chemical tin plating solution for heterojunction solar battery and preparation method thereof |
CN114561633A (en) * | 2022-02-23 | 2022-05-31 | 吉安宏达秋科技有限公司 | Tin plating solution, preparation method thereof and tin plating method for printed circuit board |
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Cited By (7)
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CN110129776A (en) * | 2019-04-09 | 2019-08-16 | 江苏驰马拉链科技股份有限公司 | A kind of chemical plating fluid producing light gold brass teeth zipper and preparation method and application |
CN110306213B (en) * | 2019-07-08 | 2020-08-04 | 广州三孚新材料科技股份有限公司 | Tin plating solution for solar cell and preparation method thereof |
CN111690918A (en) * | 2020-07-29 | 2020-09-22 | 昆山汇荣电子材料有限公司 | Tinning method for copper wire for producing tinned copper stranded wire |
CN112144048A (en) * | 2020-09-21 | 2020-12-29 | 广州三孚新材料科技股份有限公司 | Chemical tin plating solution for heterojunction solar battery and preparation method thereof |
CN112144048B (en) * | 2020-09-21 | 2021-11-12 | 广州三孚新材料科技股份有限公司 | Chemical tin plating solution for heterojunction solar battery and preparation method thereof |
CN114561633A (en) * | 2022-02-23 | 2022-05-31 | 吉安宏达秋科技有限公司 | Tin plating solution, preparation method thereof and tin plating method for printed circuit board |
CN114561633B (en) * | 2022-02-23 | 2023-11-14 | 吉安宏达秋科技有限公司 | Tinning liquid, preparation method thereof and tinning method for printed circuit board |
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