CN1837414A - Addictive for tin-electroplating solution of tin methane sulphonate series - Google Patents

Addictive for tin-electroplating solution of tin methane sulphonate series Download PDF

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Publication number
CN1837414A
CN1837414A CN 200510033691 CN200510033691A CN1837414A CN 1837414 A CN1837414 A CN 1837414A CN 200510033691 CN200510033691 CN 200510033691 CN 200510033691 A CN200510033691 A CN 200510033691A CN 1837414 A CN1837414 A CN 1837414A
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additive
tin
active agent
surface active
nonionic surface
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CN100595342C (en
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李基森
陈玫
娄红涛
冯辉
杨卫花
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Zhaoqing Lingguang new material technology development Co.,Ltd.
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Guangdong Fenghua High New Science & Technology Group Co Ltd
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Abstract

This invention discloses an additive for pure-tin plating solution of tin methanesulfonic sulfate series and the solution added this additive, which comprises the following components: (1) non-ionic surfactants; (2) aminated compound; (3) ampholytic surfactant. There isn't toxin such as lead and fluorin, and it is current density of wider rang, high current efficiency and shorter electroplating time. And it is homogeneous surface of coating after electroplating, good film thickness uniformity and surface wettable effect, good durability of weld,strong and tight cohesion of the coating and

Description

The additive that is used for tin-electroplating solution of tin methane sulphonate series
Technical field
The present invention relates to a kind of plating pure tin electroplate liquid that plates the additive of pure tin electroplate liquid and adopt this additive, specifically, the present invention relates to a kind of tin-electroplating solution of tin methane sulphonate series that is used for the additive of tin-electroplating solution of tin methane sulphonate series and adopts this additive.
Background technology
In electroplating process, additive plays important effect.Additive is to realize by the adsorption on metal/solution interface to the influence in the electrolytic etching of metal precipitation process.Because additive types is various, they are many-sided to the influence of electrolytic etching of metal precipitation process, and are very complicated.
Additive has certain effect to the internal stress of plated film.The stress of plated film is subjected to the influence of the weave construction of the condition of surface of material and plated film.The former influence custom is referred to as external stress, and the latter's influence is called inherent strain, is called for short internal stress.Internal stress is divided into two kinds of tension stress and stress.Tension stress is meant that some factor causes the stress that plated film shrinks, and stress then is to make plated film trend expansible stress.When the stress of plated film during greater than the sticking power of plated film and material, plated film president scar or decortication.If the tension stress of plated film is during greater than the tensile strength of plated film, plated film can crack, thereby reduces its corrosion resistance.When the internal stress skewness in the plated film, plated film can produce stress corrosion.In addition, tin must generation also with stress relevant, mainly be stress excessive due to.In addition, internal stress also may increase the pore rate and the fragility of plated film.Therefore, we must use additive in electroplating process, thereby reduce stress, improve coating quality.In order to obtain the plated film of compact crystallization, the polarized action of negative electrode in the time of must increasing metal ion and separate out.But, will occur owing to additive mixes the problems such as physical and mechanical properties that influence plated film if additive is selected words improperly.
Additive can have the leveling effect, and factors such as coating film thickness homogeneity are played significant effects.The leveling effect just be divided into flatten, three kinds of how much levelings and negative levelings.The mechanism of action for additive can be interpreted as: on the surface of micro-rough, if the net thickness of paddy place diffusion layer is greater than the place, peak, make additive (molecule or ion) enter the speed of the speed at paddy place less than the place, peak, the concentration of place, peak additive is then located greater than paddy, cause the resistance at place, peak to turn into to use greater than the paddy place, thereby reached the leveling effect; Otherwise, if the net thickness of paddy place diffusion layer is less than the place, peak, make additive (molecule or ion) enter the speed of the speed at paddy place greater than the place, peak, then the concentration of place, peak additive is then located less than paddy, cause the resistance at place, peak to turn into to use less than the paddy place, the deeper and deeper situation of paddy will occur, the perpendicular type striped of a rule just may appear in the surface.For example, such situation will appear in the both sexes organic compound with propionic ester structure, and the nicking of a rule appears in coating, and the leveling effect that it play is the effect of negative leveling.Under the surface of plating piece is not very smooth situation, just seem particularly outstanding of leveling effect just.
At present, the zinc-plated additive on the market all is the additive with sulfuric acid system basically, only has seldom partly to be used for the methylsulphonic acid system, and all can not electroplate with the end electrode of nickel electrode type electronic devices and components.Once there was patent documentation to put down in writing the zinc-plated additive of methylsulphonic acid system that contains heavy metal elements such as lead.For example, Chinese patent CN 98111714.7 discloses a kind of brightener that is used to contain the zinc-plated electroplate liquid of methylsulfonic acid lead, and it is made up of solvent, major-minor brightening agent and tensio-active agent; Solvent is water and water-soluble alcohol, main brightener is an aldehyde compound, auxiliary brightener is a phenol, tensio-active agent is an alkylphenol polyoxyethylene, earlier be dissolved in main and auxiliary brightening agent in the alcohol in proportion during preparation, simultaneously soluble in water tensio-active agent in proportion, the aqueous solution and alcoholic solution are mixed in proportion promptly get the brightening and leveling additive then.The tin plating electrolyte that adopts this brightener is by after electroplating for a long time, and coating is comparatively fine and close, even, and bonding force is stronger.But this brightener only is applicable to plumbiferous methylsulphonic acid tin bath solution.
For satisfying environmental protection requirement, plumbous at present application has been subjected to increasing restriction, and zinc-plated electroplate liquid is also to unleaded development.Thereby be necessary to develop a kind of additive that is applicable to unleaded tin-electroplating solution of tin methane sulphonate series.
Summary of the invention
One of purpose of the present invention provide a kind of can be used for common chip electronic component and nickel electrode type electronic devices and components plating pure tin, the tin-electroplating solution of tin methane sulphonate series additive, this additive is applicable to unleaded, floride-free electroplate liquid system, poisonous element and compounds thereof such as itself is not leaded yet, fluorine are the environment-friendly additives.
The tin methane sulfonate that is used for of the present invention is that the additive of zinc-plated electroplate liquid comprises following composition:
(1) one or more nonionic surface active agent;
(2) one or more nitrogenous compound;
(3) one or more amphoterics;
Above-mentioned additive both can have been made and do the agent form, also can make aqua, for example aforesaid combination was dissolved in the pure water, made aqua.The preferred form that adopts aqua.
Wherein, nonionic surface active agent act as hydrotropy, both can improve the amphoterics solvability, also can improve the stability of electroplate liquid.Say in principle, the kind of nonionic surface active agent is unrestricted among the present invention, can be secondary octyl phenol polyethylene ether (OP) class, alkylphenol polyethylene ether (NPE) class or hydroxybenzene polyoxydivinyl ether (TX) class etc., and promptly can be independent a kind of nonionic surface active agent, also can be the mixture of several nonionic surface active agent.For example, can be secondary octyl phenol polyethenoxy (10) ether, secondary octyl phenol polyethenoxy (15) ether, Nonyl pheno (10) ether, Nonyl pheno (18) ether, alkylphenol-polyethenoxy (8) polyoxypropylene (5) ether.Owing to only adopt hydroxybenzene polyoxydivinyl ether class nonionic surface active agent can reach good effect, therefore, can adopt hydroxybenzene polyoxydivinyl ether class nonionic surface active agent separately.
Because nitrogenous compound has the inhomogeneity effect that increases thickness of coating and thickness, therefore, additive of the present invention has adopted nitrogenous compound, for example aminated compounds.Aminated compounds can be selected from alcamine compound, alkylamide compound, amides etc.Wherein, alcamine compound can be thanomin, Propanolamine, diethanolamine, trolamine; Alkylamide compound can be an ethamine, propylamine; Amides can be alkylamide or niacinamide.
Among the present invention, the effect of amphoterics is to improve the galvanized current efficiency of tin and electroplating velocity, optimization coating structure.Amphoterics can be selected from imidazoline type amphoterics, amino acid type amphoteric surface active agent, betaine type amphoteric surfac-tant or its combination.Owing to only adopt the betaine type amphoteric surfac-tant can reach good effect, therefore, can adopt the betaine type amphoteric surfac-tant separately, for example, AMONYL 380LC, the single acetic acid imidazoline type of cocounut oil both sexes trimethyl-glycine, cocamidopropyl propyl amide hydroxyl sulphonic acid betaine, dodecyl methyl trimethyl-glycine etc. or its combination.
Among the present invention, the concentration of nonionic surface active agent generally is controlled between the 5-50g/L, is preferably 10-40g/L, more preferably 20-30g/L.
Among the present invention, the concentration of nitrogenous compound generally is controlled between the 5-50g/L, is preferably 10-40g/L, more preferably 20-30g/L.
Among the present invention, the concentration of amphoterics generally is controlled between the 1-60g/L, is preferably 5-40g/L, more preferably 15-30g/L.
The use temperature of additive of the present invention generally between 10-35 ℃, is preferably 18-28 ℃, more preferably 22-24 ℃; The pH value of applied environment is generally 2-6, is preferably pH3-5, more preferably pH3.5 ± 0.5.
Another object of the present invention provides a kind of tin-electroplating solution of tin methane sulphonate series that adds additive of the present invention.
Additive of the present invention can be that zinc-plated electroplate liquid matches with existing tin methane sulfonate both, also can match with three layers of bath system of chip components and parts provided by the present invention.Additive current density range broad of the present invention, current efficiency height, to electroplate required time shorter, can shorten about 20% electroplating time.The surperficial uniform and delicate of zinc-plated back coating, thickness evenness and moistened surface are effective, but soldering resistance can be good, and binding force of cladding material is strong and combination is tight.The covering power of tin-electroplating solution of tin methane sulphonate series that has added additive of the present invention is strong, the coating surface uniform and delicate that obtains after the plating.
Embodiment
Embodiment 1
Mix the following additive preparation that becomes to assign to: 7g/L secondary octyl phenol polyethenoxy (10) ether, 30g/L thanomin, 5g/L AMONYL 380LC TB-L7.Prepared additive outward appearance is light yellow stream malleability better fluid, and density is 1.019g/ml, and the pH value is 9.30, and chemical property is stable.
Above-mentioned additive is added in the tin plating electrolyte, cooperate other composition to do Hull groove experiment, with 0.4A strength of current brass-plating sheet, thickness of coating can reach 9.2um.
Embodiment 2
Mix the following additive preparation that becomes to assign to: 15g/L Nonyl pheno (10) ether, 18g/L niacinamide, the single acetic acid imidazoline type of 20g/L cocounut oil both sexes trimethyl-glycine RAM-C.
Above-mentioned additive is added in the tin plating electrolyte, cooperate other composition to do Hull groove experiment, with 0.4A strength of current brass-plating sheet, thickness of coating can reach 13.4um.
Embodiment 3
Mix the following additive preparation that becomes to assign to: 30g/L Nonyl pheno (18) ether, 6g/L ethamine, 50g/L cocamidopropyl propyl amide hydroxyl sulphonic acid betaine RAM-CAS.
Above-mentioned additive is added in the tin plating electrolyte, cooperate other composition to do Hull groove experiment, with 0.4A strength of current brass-plating sheet, thickness of coating can reach 12.6um.
Embodiment 4
Mix the following additive preparation that becomes to assign to: 45g/L secondary octyl phenol polyethenoxy (15) ether, 25g/L diethanolamine, 12g/L dodecyl methyl trimethyl-glycine B-12.
Above-mentioned additive is added in the tin plating electrolyte, cooperate other composition to do Hull groove experiment, with 0.4A strength of current brass-plating sheet, thickness of coating can reach 11.2um.
Embodiment 5
Mix the following additive preparation that becomes to assign to: 20g/L secondary octyl phenol polyethenoxy (10) ether, 40g/L trolamine, the single acetic acid imidazoline type of 30g/L cocounut oil both sexes trimethyl-glycine RAM-C.
Above-mentioned additive is added in the tin plating electrolyte, cooperate other composition to do Hull groove experiment, with 0.4A strength of current brass-plating sheet, thickness of coating can reach 14.5um.
Embodiment 6
Mix the following additive preparation that becomes to assign to: 25g/L alkylphenol-polyethenoxy (8) polyoxypropylene (5) ether, 20g/L niacinamide, 28g/L cocamidopropyl propyl amide hydroxyl sulphonic acid betaine RAM-CAS.
Above-mentioned additive is added in the diethanolamine tin plating electrolyte, cooperate other composition to do Hull groove experiment, with 0.5A strength of current brass-plating sheet, thickness of coating can reach 15.2um.
Embodiment 7
Assign to prepare additive of the present invention by the one-tenth shown in the table 3, and it joined in the tin plating bath, carry out Hull groove experiment then, come the brass-plating sheet with 0.4A strength of current, thickness of coating following (seeing Table 1):
Table 1 result shows that under 0.4A strength of current, with the tin plating bath brass-plating sheet that has added above-mentioned prescription, the thickness of coating that obtains generally can reach 2.96-4.68um.
Table 1
The test sequence number Nonionic surface active agent (g/L) Nitrogenous compound (g/L) Amphoterics (g/L) Thickness (um)
01 6 8 10 3.72
02 15 45 10 2.96
03 25 25 50 3.47
04 35 16 50 3.91
05 25 35 10 3.24
06 45 35 30 4.54
07 35 35 20 4.37
08 45 45 40 4.68
The contrast experiment
We have carried out the groove experiment of contrast Hull with additive of the present invention and import additive and certain homemade additive, and real to give used electric current is 0.4A, and electroplating time is that the 5min. experimental result is as shown in table 2 below:
Table 2
Figure A20051003369100121
We have also contrasted the electrochemical parameter (seeing Table 3) of relevant above three kinds of additives:
Table 3
Additive Can allow strength of current scope (A) Can allow current density range (A/dm 2) Electroplating time (min) Current efficiency (%) Sedimentation velocity (um/h)
Import 0-42 0-1.2 90 40-50 10
Domestic 0-55 0-1.2 60 40-50 10
The present invention 0-70 0-2 30 70-80 20
Experimental result shows that additive of the present invention has following advantage:
1. improve the cathodic polarization ability, enlarged current density range, improved dispersive ability and covering power;
2. the current efficiency height can plate out thicker coating in the identical time.
3. the coating surface uniform and delicate that obtains after electroplating, the plating bath covering power is strong.

Claims (10)

1, a kind of additive that is used for tin-electroplating solution of tin methane sulphonate series, this additive comprises following composition:
(1) one or more nonionic surface active agent;
(2) one or more nitrogenous compound;
(3) one or more amphoterics.
2, additive as claimed in claim 1, it is characterized in that described nonionic surface active agent is secondary octyl phenol glymes nonionic surface active agent, polyoxyethylene nonylphenol ether class nonionic surface active agent and other alkylphenol glymes nonionic surface active agent or its composition.
3, additive as claimed in claim 1 is characterized in that, described nitrogenous compound is an aminated compounds.
4, additive as claimed in claim 3 is characterized in that, described aminated compounds is alcamine compound, alkylamide compound, amides or its composition.
5, additive as claimed in claim 1 is characterized in that, described amphoterics is imidazoline type amphoterics, amino acid type amphoteric surface active agent, betaine type amphoteric surfac-tant or its composition.
6, additive as claimed in claim 1 is characterized in that, described nonionic surface active agent is a hydroxybenzene polyoxydivinyl ether class nonionic surface active agent, and described amphoterics is the betaine type amphoteric surfac-tant.
7, additive as claimed in claim 6, it is characterized in that described betaine type amphoteric surfac-tant is AMONYL 380LC, the single acetic acid imidazoline type of cocounut oil both sexes trimethyl-glycine, cocamidopropyl propyl amide hydroxyl sulphonic acid betaine, dodecyl methyl trimethyl-glycine or its composition.
8, additive as claimed in claim 4 is characterized in that, described aminated compounds is ethamine, thanomin, Propanolamine, diethanolamine, trolamine, niacinamide or its composition.
As the described additive of one of claim 1-6, it is characterized in that 9, various component concentrations are as follows in the described additive:
(1) nonionic surface active agent 5-50g/L;
(2) aminated compounds 5-50g/L;
(3) amphoterics 1-60g/L.
10, a kind of tin-electroplating solution of tin methane sulphonate series that has added as additive as described in one of claim 1-9.
CN200510033691A 2005-03-24 2005-03-24 Addictive for tin-electroplating solution of tin methane sulphonate series Active CN100595342C (en)

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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101922026A (en) * 2010-08-18 2010-12-22 济南德锡科技有限公司 Methanesulfonic acid-based matte pure tin electroplating solution and additive thereof
CN102660760A (en) * 2010-10-22 2012-09-12 罗门哈斯电子材料有限公司 Tin plating solution
CN102953096A (en) * 2011-08-17 2013-03-06 上海申和热磁电子有限公司 Additive for weak acid methanesulfonic acid dark tin solution
CN104593835A (en) * 2015-02-04 2015-05-06 广东羚光新材料股份有限公司 Neutral tin plating solution used in electroplating terminal electrodes of chip component
CN105316711A (en) * 2014-07-31 2016-02-10 Apct株式会社 Tin-based electroplating solution for solder bumps including perfluoroalkyl surfactant
CN110106535A (en) * 2019-06-10 2019-08-09 广东比格莱科技有限公司 A kind of tin plating additive of neutrality
CN113430592A (en) * 2021-06-30 2021-09-24 广东德浩化工新材料有限公司 Neutral tin plating stabilizer and preparation method thereof

Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101922026A (en) * 2010-08-18 2010-12-22 济南德锡科技有限公司 Methanesulfonic acid-based matte pure tin electroplating solution and additive thereof
CN101922026B (en) * 2010-08-18 2012-02-01 济南德锡科技有限公司 Methanesulfonic acid-based matte pure tin electroplating solution and additive thereof
CN102660760A (en) * 2010-10-22 2012-09-12 罗门哈斯电子材料有限公司 Tin plating solution
CN102660760B (en) * 2010-10-22 2015-09-23 罗门哈斯电子材料有限公司 Tin plating electrolyte
CN102953096A (en) * 2011-08-17 2013-03-06 上海申和热磁电子有限公司 Additive for weak acid methanesulfonic acid dark tin solution
CN105316711A (en) * 2014-07-31 2016-02-10 Apct株式会社 Tin-based electroplating solution for solder bumps including perfluoroalkyl surfactant
CN105316711B (en) * 2014-07-31 2018-01-05 Apct株式会社 Solder bump comprising perfluoralkyl surfactant tin alloy electric plating liquid
CN104593835A (en) * 2015-02-04 2015-05-06 广东羚光新材料股份有限公司 Neutral tin plating solution used in electroplating terminal electrodes of chip component
CN110106535A (en) * 2019-06-10 2019-08-09 广东比格莱科技有限公司 A kind of tin plating additive of neutrality
CN113430592A (en) * 2021-06-30 2021-09-24 广东德浩化工新材料有限公司 Neutral tin plating stabilizer and preparation method thereof

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