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CN1354280A - Corrosion method of metal tin or tin alloy, and corrosion liquor of metal tin or tin alloy - Google Patents

Corrosion method of metal tin or tin alloy, and corrosion liquor of metal tin or tin alloy Download PDF

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Publication number
CN1354280A
CN1354280A CN 01135433 CN01135433A CN1354280A CN 1354280 A CN1354280 A CN 1354280A CN 01135433 CN01135433 CN 01135433 CN 01135433 A CN01135433 A CN 01135433A CN 1354280 A CN1354280 A CN 1354280A
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China
Prior art keywords
tin
etching
aqueous solution
alloy
corrosion
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CN 01135433
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Chinese (zh)
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CN1311099C (en
Inventor
齐藤知志
秋山大作
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Mitsuku K K
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Mitsuku K K
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Publication of CN1354280A publication Critical patent/CN1354280A/en
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  • Manufacturing Of Printed Circuit Boards (AREA)

Abstract

The present invention provides an etching solution for etching metallic tin or a tin alloy without eroding glass and generating nitrogen oxide, as well as for producing a little sludge and enabling its liquid waste to be easily treated. Etching metallic tin or a tin alloy by contacting a material to be treated with a water-soluble solution including tin (IV). A method for continuously etching them comprises converting tin (II) generated in the water-soluble solution to tin (IV), by adding an oxidizing agent to the solution, contacting it with oxygen and air, or oxidizing it at an anode side with electrolysis, and etching them.

Description

Method for corroding metallic tin or tin alloy and corrosive liquid of metallic tin or tin alloy
Technical Field
The present invention relates to a method for etching metallic tin or a tin alloy, which is useful for stripping tin plating used as a copper resist in the production of printed wiring boards, and an etching solution used for the method.
Background
As the etching liquid for metallic tin, conventionally, there have been used a solution containing a fluorine compound as a main component (Japanese patent laid-open publication No. Sho 59-74281), a solution containing nitrobenzenesulfonic acid as a main component (Japanese patent laid-open publication No. Hei 1-129491), a solution containing nitric acid as a main component (Japanese patent laid-open publication No. Hei 7-278846), and the like.
However, when a solution containing a fluorine compound as a main component is used, if a printed wiring board having an insulating layer containing glass fibers is treated, there is a problem that glass is corroded. Further, when a solution containing nitrobenzenesulfonic acid as a main component is used, there is a problem that sludge is easily generated in the etching solution. When a solution containing nitric acid as a main component is used, nitrogen oxide is generated when metal tin is corroded, which causes a problem of deterioration of working environment.
Disclosure of the invention
The invention aims to provide a corrosion method and a corrosion liquid which can corrode metal tin or tin alloy without corroding glass and generating nitrogen oxide, and has the advantages of less sludge generation and easy waste liquid treatment.
The present invention relates to a method for etching metallic tin or a tin alloy by bringing an aqueous solution containing tin having a valence of 4 into contact with a material to be treated containing metallic tin or a tin alloy, and an etching solution for metallic tin or a tin alloy composed of an aqueous solution containing tin having a valence of 4.
Detailed Description
Hereinafter, embodiments of the present invention will be described in detail.
The etching method of the present invention uses an aqueous solution containing tin having a valence of 4. The above-mentioned 4-valent tin includes tin compounds such as tin tetrachloride, tin dioxide, tin sulfate, sodium stannate, potassium stannate, etc. These may be used alone or in combination of 2 or more. The 4-valent tin may be in the form of a 4-valent tin in an aqueous solution, and for example, an aqueous solution of tin dichloride is prepared and then oxidized to have a 4-valent tin in an aqueous solution.
The concentration of the 4-valent tin in the aqueous solution is preferably 1 to 25% (by weight, the same applies hereinafter) in terms of 4-valent tin ions, more preferably 5 to 20%. If the concentration is less than 1%, the corrosion of tin is slowed down; if it exceeds 20%, the effect is not more pronounced by an increase in the amount added (e.g., an increase in the corrosion rate).
By bringing the aqueous solution into contact with a material to be treated having metallic tin or a tin alloy, the following formula (1):
(1) the reaction shown can achieve the purpose of corroding tin.
As a method of bringing the aqueous solution into contact with the material to be treated, there are a method of immersing the material to be treated in the aqueous solution, a method of spraying the aqueous solution on the material to be treated, and the like.
However, since 2-valent tin does not have the ability to corrode metallic tin or tin alloy, it is preferable to perform corrosion treatment while oxidizing the reduced tin to 4-valent tin in order to continuously perform corrosion, and the oxidation method includes a method of ① adding an oxidizing agent to the aqueous solution, a method of ② contacting the aqueous solution with oxygen or air, a method of ③ oxidizing tin on the anode side by electrolysis, and the like.
First, a method of ① in which an oxidizing agent is added to the aqueous solution to oxidize 2-valent tin to 4-valent tin and simultaneously perform etching will be described.
The oxidizing agent includes hydrogen peroxide, chlorine gas, sodium chlorate, sodium hypochlorite, nitric acid, a compound containing iron (3) in valence (e.g., ferric trichloride), a compound containing copper (2) in valence (e.g., cupric dichloride), and nitrobenzenesulfonic acid. The oxidizing agents may be used alone or in combination of 2 or more. Among them, hydrogen peroxide is preferably used because water is generated after the reaction, and the corrosion rate is not affected.
The method of adding the additive includes a method of calculating the amount of 2-valent tin generated by etching and then adding an oxidizing agent necessary for oxidizing the tin to 4-valent tin in advance, a method of sequentially adding an oxidizing agent in accordance with the amount of 2-valent tin generated by etching, and the like. The presence or absence of tin having a valence of 2 in the aqueous solution can be easily determined by measurement of an oxidation-reduction potential or the like. Of the foregoing methods, the first 1 method has an advantage in that the concentration of the oxidizing agent in the etching does not need to be monitored, and the latter 1 method has an advantage in that the oxidizing ability of the etching solution is relatively stable.
The amount of the oxidizing agent to be added can be adjusted depending on the kind of the material to be treated. For example, in the case of etching tin plating formed on copper, the amount of the oxidizing agent added is only required to be capable of oxidizing 2-valent tin generated by the etching to 4-valent tin, so that only tin plating is etched without etching copper as a base material. In addition, when not only tin is to be etched but also copper as a base material and a copper-tin alloy formed in the middle are to be etched at the same time,an oxidizing agent may be added in an excessive amount to improve the oxidizing ability of the etching solution. Therefore, although the oxidizing agent can be added in a stepwise manner in the case of dissolving only tin plating on copper, it is preferable to control the oxidizing ability to prevent the oxidizing ability of the etching solution from becoming too strong.
In order to accelerate the etching rate, it is preferable that chlorine ions are present in the aqueous solution. Sources of chloride ions include the aforementioned tin tetrachloride, tin dichloride, hydrochloric acid, ammonium chloride, sodium chloride, potassium chloride, and the like. The concentration of the chloride ion in the aqueous solution is preferably 1 to 35% (by weight, the same applies hereinafter), more preferably 3 to 30%. If the chloride ion concentration is less than 1%, the effect of accelerating the corrosion rate of tin is not sufficiently significant, and if the chloride ion concentration exceeds 35%, the effect is not more significant with an increase in the amount of addition. When hydrochloric acid is used as a chloride ion source, hydrogen chloride gas generates an offensive odor, which causes a pollution to the working environment.
The aqueous solution may contain other components as necessary, and for example, inorganic acids such as nitric acid and sulfuric acid, organic acids such as citric acid and malic acid, and the like may be added to increase the amount of dissolved tin.
Next, a method of ② in which the aqueous solution is brought into contact with oxygen or air to oxidize tin having a valence of 2 to tin having a valence of 4 will be described.
The aqueous solution may be brought into contact with oxygen or air by introducing oxygen or air into the aqueous solution, spraying the aqueous solution into the aqueous solution while the aqueous solution is brought into contact with the material to be treated, passing the aqueous solution through a gas absorption apparatus such as a packed column or a bubble column, or the like.
In order to accelerate the etching rate, it is preferable to use this method in which chloride ions are present in the aqueous solution. The concentration of the chloride ion is preferably 1 to 25%, more preferably 3 to 20%. If the chloride ion concentration is less than 1%, the action of accelerating the corrosion rate of metallic tin or tin alloy is insufficient, and if the chloride ion concentration exceeds 25%, the 2-valent tin cannot be effectively oxidized, and the corrosion rate will be reduced during continuous corrosion.
The method of contacting the aqueous solution with oxygen or air may further contain other components as necessary. For example, inorganic acids such as nitric acid and sulfuric acid, and organic acids such as citric acid and malic acid may be added to increase the maximum amount of tin dissolved. In addition, in order to increase the etching rate, an oxidizing agent such as hydrogen peroxide, sodium chlorate, or nitrobenzene sulfonic acid may be added to the copper or tin during etching.
The amount of oxygen and the amount of air used for contacting the aqueous solution with oxygen or air may be set so as to correspond to the amount of tin (2) valent formed in the aqueous solution. Since the amount of the 2 nd valent tin formed in the aqueous solution is proportional to the amount of corrosion, the corrosion can be continuously performed by using oxidation conditions according to the amount of corrosion, that is, the amount of the 2 nd valent tin formed.
Finally, a method of ③ electrolytically oxidizing the 2 nd valent tin generated by the etching to oxidize the tin to 4 th valent tin and simultaneously etching the tin will be described.
For example, an electrolytic layer is prepared, which is partitioned between an anode and a cathode by an anion exchange membrane, and an etchant containing tin having a valence of 2 for etching is introduced on the anode side, and hydrochloric acid containing the same anionic acid as the etchant is introduced on the cathode side, followed by electrolysis. This oxidizes the tin having a valence of 2 to tin having a valence of 4 on the anode side, and the solution on the anode side is regenerated as an etching solution. Hydrochloric acid, water and the like are preferably added to the regenerated etching solution to adjust the chloride ion concentration.
The present invention is applicable to stripping of tin plating used as a copper resist in the production of printed wiring boards. In this case, the tin-copper alloy layer formed between tin and copper must be peeled off. Therefore, in order to peel off the tin layer and the tin-copper alloy in the same step, it is preferable to improve the oxidizing ability of the etching solution of the present invention. Alternatively, after only the tin layer is peeled off by the etching solution of the present invention, the tin-copper alloy is peeled off by a stripping solution for tin-copper alloy (S-651B manufactured by Meige corporation, etc.).
The etching solution of the present invention is useful for etching metallic tin and tin alloys in various members such as lead frames, electrodes of electronic components, and accessories.
Example 1
1000g of an etching solution composed of 280g of stannic chloride 5 hydrate, 106g of 35% hydrochloric acid and 614g of deionized water was prepared, and a pure tin plate (1.0mm thick) was used as a material to be treated.
The material to be treated was immersed in the etching solution (35 ℃ C.), and the tin was etched by shaking and shaking. Further, in order to oxidize the2-valent tin generated by the etching to 4-valent tin, the etching was performed while introducing air into the etching solution, and the etching rate was 8.1 μm/min.
After 10g of tin was dissolved, the etching rate was reduced to 6.5 μm/min, and 92.8g of dilute hydrochloric acid (17.5% concentration) was added to return the chloride ion concentration and the 4-valent tin ion concentration to substantially the same values as the initial concentrations, so that the etching rate was also returned to the initial levels.
The operation described above, i.e., ① dissolving 10g of tin in 1000g of etching solution, ② supplementing 92.8g of dilute hydrochloric acid, ③ taking out 1000g of etching solution, was repeated for 5 cycles, whereby the etching ability (etching rate) was maintained.
94.8g of tin was dissolved in 1kg of the etching solution, and the etching solution was continuously used by merely adding hydrochloric acid.
Example 2
1000g of an etching solution composed of 432g of stannic chloride-5 hydrate, 100g of 35% hydrochloric acid and 468g of deionized water was prepared, and a pure tin plate (1.0mm thick) was used as a material to be treated.
The material to be treated was immersed in the etching solution (35 ℃ C.), shaken and oscillated to etch the tin. The etching rate was 11.9 μm/min. Further, since the oxidation-reduction potential is greatly lowered by the 2-valent tin generated by the corrosion, the oxidation-reduction potential is monitored and the oxidation-reduction potential is returned to the initial value by adding hydrogen peroxide at a concentration of 35% as needed.
After 10g of tin was dissolved, hydrogen peroxide was added to restore the oxidation-reduction potential to the original state, but the corrosion rate was restored to 10.3 μm/min. The total amount of hydrogen peroxide (35%) added was 16.4 g. Then, by adding 42.0g of hydrochloric acid (35%), the chlorine ion concentration and the concentration of the 4-valent tin ion can be returned to substantially the same values as the initial concentrations, and the etching rate can be returned to the initial level.
The above operation, ①, was carried out to dissolve 10g of tin in 1000g of etching solution while maintaining the redox potential, ② was supplemented with 42.0g of hydrochloric acid, ③ was carried out to take out 1000g of etching solution, and this was repeated for 5 cycles, whereby the etching capacity (etching rate) was maintained.
146.2g of tin can be dissolved in 1kg of the etching solution, and the etching solution can be continuously used only by supplementing hydrogen peroxide and hydrochloric acid.
The corrosion method and the corrosion liquid of the present invention can recover the corrosion performance decreased by the dissolution of tin without using an expensive reagent, and can continuously corrode metallic tin or tin alloy at an extremely low cost as compared with the conventional corrosion method and the corrosion liquid.
In addition, the etching method and the etching solution of the invention can etch metal tin or tin alloy without etching glass and generating nitrogen oxide.
The corrosion method and the corrosion liquid of the invention hardly produce slurry, and the waste liquid is convenient to treat.

Claims (6)

1. A method for etching metallic tin or a tin alloy, characterized by bringing an aqueous solution containing tin having a valence of 4 into contact with a material to be treated having metallic tin or a tin alloy.
2. A method for etching metallic tin or tin alloy, characterized in that an aqueous solution containing tin having a valence of 4 is brought into contact with a material to be treated having metallic tin or tin alloy, and the metallic tin or tin alloy is etched while oxidizing tin having a valence of 2 generated in the aqueous solution to tin having a valence of 4, thereby continuously etching the metallic tin or tin alloy.
3. The method according to claim 2, wherein the oxidation is performed by adding an oxidizing agent to the aqueous solution, by bringing the aqueous solution into contact with oxygen or air, or by oxidizing the aqueous solution on the anode side by electrolysis.
4. The method according to claim 1 or 2, wherein the tin having a valence of 4 is tin tetrachloride.
5. The corrosive liquid of metallic tin or tin alloy is characterized by comprising an aqueous solution containing tin having a valence of 4.
6. The etching solution according to claim 5, wherein the tin having a valence of 4 is tin tetrachloride.
CNB01135433XA 2000-10-26 2001-09-26 Corrosion method of metal tin or tin alloy, and corrosion liquor of metal tin or tin alloy Expired - Fee Related CN1311099C (en)

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JP2000327341A JP4580085B2 (en) 2000-10-26 2000-10-26 Method for etching metal tin or tin alloy and metal tin or tin alloy etchant

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CN1311099C CN1311099C (en) 2007-04-18

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103741142A (en) * 2014-01-10 2014-04-23 中南大学 Method for recycling tin from waste tin-stripping solution based on tin-stripping solution of hydrochloric acid-tin salt system
CN103866324A (en) * 2013-05-20 2014-06-18 昆山市板明电子科技有限公司 Selective tin etching solution
CN106216792A (en) * 2016-08-22 2016-12-14 中南大学 A kind of all kinds of components and parts of clean separation reclaim the method and device of stannum from discarded circuit board
CN110618009A (en) * 2019-10-30 2019-12-27 无锡隆达金属材料有限公司 Method for microcosmic metallographic corrosion of cupronickel alloy

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP2503029B1 (en) * 2011-03-22 2013-03-20 Atotech Deutschland GmbH Process for etching a recessed structure filled with tin or a tin alloy

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US4283248A (en) * 1979-02-01 1981-08-11 Nitto Electric Industrial Co., Ltd. Etching solution for tin-nickel alloy and process for etching the same
JPS59219475A (en) * 1983-05-30 1984-12-10 Metsuku Kk Tin or tin alloy stripper
JPS6263692A (en) * 1985-05-10 1987-03-20 C Uyemura & Co Ltd Method for removing tetravalent tin ions in surface treatment solution
US4944851A (en) * 1989-06-05 1990-07-31 Macdermid, Incorporated Electrolytic method for regenerating tin or tin-lead alloy stripping compositions
JP3382031B2 (en) * 1993-11-16 2003-03-04 株式会社東芝 Method for manufacturing semiconductor device
JPH08285993A (en) * 1995-04-17 1996-11-01 Toshiba Corp Chemical decontamination method and decontamination apparatus therefor
JPH09302480A (en) * 1996-05-14 1997-11-25 Nikko Metal Pureeteingu Kk Removing solution of tin or tin alloy and peeling method
CN1178260A (en) * 1996-08-30 1998-04-08 美克株式会社 Liquid for separating tin from tin alloy
GB9901586D0 (en) * 1999-01-25 1999-03-17 Alpha Fry Ltd Process for the recovery of lead and/or tin or alloys thereof from substrate surfaces

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103866324A (en) * 2013-05-20 2014-06-18 昆山市板明电子科技有限公司 Selective tin etching solution
CN103866324B (en) * 2013-05-20 2015-09-16 昆山市板明电子科技有限公司 Selectivity tin etching solution
CN103741142A (en) * 2014-01-10 2014-04-23 中南大学 Method for recycling tin from waste tin-stripping solution based on tin-stripping solution of hydrochloric acid-tin salt system
CN103741142B (en) * 2014-01-10 2016-06-29 中南大学 A kind of tin stripper based on hydrochloric acid-pink salt system and the method reclaiming stannum from waste tin stripper
CN106216792A (en) * 2016-08-22 2016-12-14 中南大学 A kind of all kinds of components and parts of clean separation reclaim the method and device of stannum from discarded circuit board
CN106216792B (en) * 2016-08-22 2018-12-21 中南大学 A method of all kinds of components of clean separation and tin is recycled from discarded circuit board
CN110618009A (en) * 2019-10-30 2019-12-27 无锡隆达金属材料有限公司 Method for microcosmic metallographic corrosion of cupronickel alloy

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CN1311099C (en) 2007-04-18
JP2002129359A (en) 2002-05-09
JP4580085B2 (en) 2010-11-10
TWI233454B (en) 2005-06-01

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Granted publication date: 20070418

Termination date: 20110926