US3663384A - Bath for electroplating tin-bismuth alloy - Google Patents

Bath for electroplating tin-bismuth alloy Download PDF

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Publication number
US3663384A
US3663384A US79272A US3663384DA US3663384A US 3663384 A US3663384 A US 3663384A US 79272 A US79272 A US 79272A US 3663384D A US3663384D A US 3663384DA US 3663384 A US3663384 A US 3663384A
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bismuth
tin
bath
acid
sulphate
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US79272A
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Jean P Lescure
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International Business Machines Corp
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International Business Machines Corp
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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

Definitions

  • ABSTRACT Bath for electroplating tin-bismuth alloy upon a metal object such as a frame of a computer, including fluoboric acid in order to maintain the pH acid, tin fluoborate and a bismuth oxide-bismuth sulphate mixture of low quantity.
  • the utilized method is of the soluble anode type and the cathode is formed of the object to be coated.
  • tin coatings have a drawback. Indeed, at temperatures near the room temperature, a temperature lower than 13 0, tin is submitted to an allotropic transformation: the deposited white tin is changed into a grey tin. This phenomenon is known as tin pest. This tin pest appears as a non-adherent powder which separates from the deposit, thereby exposing the underlying metal to corrosion.
  • the prior art has disclosed an electroplating method and bath for electroplating bismuth-tin-alloy.
  • the bath is basic and, therefore, bismuth must be introduced in the form of organic bismuthates which are not much soluble.
  • the operating temperature is near 90 C. This method is difficult as to its implementation and is relatively expensive and does not make it possible to obtain a sufficient bismuth concentration.
  • one object of this invention is to obtain an acid bath for electroplating tin-bismuth alloy.
  • Another object of the invention is the implementation of a tin-bismuth electroplating method with which it is possible to obtain a constant bismuth concentration in the tin.
  • Another object of the invention is the implementation of a method with which it is possible to obtain a uniform coating of the tin-bismuth alloy upon another metal and this in a simple and cheap manner.
  • the object to be coated is immersed into the bath where it acts as a cathode.
  • a tin anode is used which is wrapped in a polypropylene bag the texture of which is very close in order to prevent the non ionized metal particles from moving which are pulled out of the anode during dissolution of the anode used to regenerate the tin-contents in the bath.
  • the proportion of tin contained in the bath is within 2080 g. of metal tin per liter which is introduced in the form of tin salt, namely, tin fluoborate.
  • the concentration of the bismuth ions in the bath which is within 0.0l and 0.05 g. of bismuth per liter, is obtained in the bath by introducing therein from 0.1 to 0.5 g.
  • the bath contains also about lg. of formol per liter in order to avoid the anodic oxidation of the stannous ions (Sn* into stannic ions $11 Besides, this bath may include gelatine the proportions of which are 2 to 7 g. per liter and B-naphtol the proportions of which are 0.5 to 1.5 g. per liter in order to improve the quality of the deposit.
  • the bath may also contain brighteners in appropriate proportions.
  • the so-formed bath has an acid pI-l and its acidity corresponds to the acidity of a solution containing 100 g./liter of sulphuric acid.
  • the density is about 13 B.
  • the electroplating process is carried out at a temperature within 20-50 C.
  • the voltage is between 1 and 3 volts and the current density is between 0.8 and 3A/dm
  • the obtained deposit ratio is 0.5 M/mlllllte.
  • the anode-cathode surface ratio may be between 1 and 1.5.
  • tin fluoborate 30g/liter of metal tin fluoboric acid 130g/liter boric-acid 30g/liter mixture: bismuth sulphate 30% by weight bismuth oxide 70% by weight 0.3g/liter formol lg/liter equivalent acid H IOOg/liter The tests have been made at 25 C. and are gathered in the following table.
  • the preferred percentage of bismuth in tin is 0.4 percent.
  • An aqueous bath for electroplating tin-bismuth alloy characterized in that it includes acid ions in order to maintain pH acid, and characterized in that the bismuth is inserted in the form of a bismuth sulphate-bismuth oxide mixture, the concentration of which relative to the entire bath is between 0.1 and 0.5 grams per liter and in which the relative proportion of bismuth sulphate to bismuth oxide is in the range between 15/85 and 1.
  • tin fluoborate equivalent to 30g/liter of metal tin i oxide is in the range between 15/85 and l. I I 8/ of fluqbfllrif acid 4.
  • a tin plating bath according to claim 3 wherein said a bismuth mixture comprises bismuth sulphate and bismuth sulphatemismuth t fggzg the oxide in relative weight proportions of approximately 30 to 70 es tive on s b hts f wh' h 5 Pei-cam lrc 5%-75Z y s.
  • a tin plating bath according to claim 4 including approxi- 5.
  • lgll 0 f l mately 1 gram per liter of formal as additive to inhibit anodic oxidation of the stannous ions.

Abstract

Bath for electroplating tin-bismuth alloy upon a metal object such as a frame of a computer, including fluoboric acid in order to maintain the pH acid, tin fluoborate and a bismuth oxidebismuth sulphate mixture of low quantity. The utilized method is of the soluble anode type and the cathode is formed of the object to be coated.

Description

United States Patent Lescure [72] Inventor:
[73] Assignee: International Business Machines Corporation, Armonk, NY.
[22] Filed: Oct. 8, 1970 [21] Appl.No.: 79,272
Jean P. Lescure, Montpellier, France [30] Foreign Application Priority Data Dec. 19, 1969 France ..6944284 [5 2] [1.8. CI ..204/43 [5 l Int. Cl. C23b 5/38 [58] Field of Search ..204/43 [5 6] References Cited UNITED STATES PATENTS 3,360,446 12/1967 Jongkind ..204/43 3,522,155 7/1970 Dow ..204/43 [15] 3,663,384 [451 May 16, 1972 FORElGN PATENTS OR APPLICATIONS 526,037 9/1940 Great Britain ..204/43 OTHER PUBLICATlONS N. T. Kudryavtsev et al., Trudy MKHTI imenl D. l. Mendeleeva, No. 266, pp. 113- 119,(1959) Frederick A. Lowenheim, Modern Electroplating," p. 373, 1968) Primary Examiner-G. L. Kaplan Attorneyl'lanifin and Jancin and Robert Lieber [5 7] ABSTRACT Bath for electroplating tin-bismuth alloy upon a metal object such as a frame of a computer, including fluoboric acid in order to maintain the pH acid, tin fluoborate and a bismuth oxide-bismuth sulphate mixture of low quantity. The utilized method is of the soluble anode type and the cathode is formed of the object to be coated.
6 Claims, No Drawings BACKGROUND OF THE INVENTION 1. Field of the Invention tration of bismuth ions in the bath, is inserted into close texture polypropylene bags which prevent non dissolved molecules from being drawn into the bath while making it possible to obtain a concentration of bismuth ions which is This invention concerns an electroplating method and bath. 5 constant and near saturation More particularly, it concerns a method for depositing, through an electroplating process, a tin-bismuth alloy as well as the bath used for its implementation.
2. Description of the Prior Art It is well known for the man skilled in the art that it is possi- 1 ble to electrodeposit (or electroplate) metal tin upon various metal surfaces. For instance, it can be deposited upon aluminum, nickel, etc... The use of tin as a coating is preferred when casings, frames, etc., must be built which must show a high compatibility and a time-constant and frequency-independent contact impedance lower than 1 ohm. These properties are due to the fact that the tin oxide has the same impedance as the metal tin.
Unfortunately, tin coatings have a drawback. Indeed, at temperatures near the room temperature, a temperature lower than 13 0, tin is submitted to an allotropic transformation: the deposited white tin is changed into a grey tin. This phenomenon is known as tin pest. This tin pest appears as a non-adherent powder which separates from the deposit, thereby exposing the underlying metal to corrosion.
In order to avoid tin pest, it has been proposed to add bismuth or antimony to tin.
The prior art has disclosed an electroplating method and bath for electroplating bismuth-tin-alloy. The bath is basic and, therefore, bismuth must be introduced in the form of organic bismuthates which are not much soluble. In addition, the operating temperature is near 90 C. This method is difficult as to its implementation and is relatively expensive and does not make it possible to obtain a sufficient bismuth concentration.
SUMMARY OF THE INVENTION Therefore, one object of this invention is to obtain an acid bath for electroplating tin-bismuth alloy.
Another object of the invention is the implementation of a tin-bismuth electroplating method with which it is possible to obtain a constant bismuth concentration in the tin.
Another object of the invention is the implementation of a method with which it is possible to obtain a uniform coating of the tin-bismuth alloy upon another metal and this in a simple and cheap manner.
This invention will be further explained with reference to the following preferred embodiments of the invention.
DETAILED DESCRIPTION OF PREFERRED EMBODIMENTS In each embodiment of the invention, the object to be coated is immersed into the bath where it acts as a cathode. A tin anode is used which is wrapped in a polypropylene bag the texture of which is very close in order to prevent the non ionized metal particles from moving which are pulled out of the anode during dissolution of the anode used to regenerate the tin-contents in the bath.
The proportion of tin contained in the bath is within 2080 g. of metal tin per liter which is introduced in the form of tin salt, namely, tin fluoborate.
It contains from 100 to 200 g. of free fluoboric acid; it may also contain in appropriate proportions a buffer solution such as boric acid. The concentration of the bismuth ions in the bath, which is within 0.0l and 0.05 g. of bismuth per liter, is obtained in the bath by introducing therein from 0.1 to 0.5 g. per liter of a mixture formed of bismuth sulphate, Bi (S0,) and of bismuth oxide (Bi- 0 the composition of which may vary from 15 to 50 percent by weight of bismuth sulphate and from 85 to 50 percent by weight of bismuth oxide, the preferred ratio of the mixture being, 30 percent by weight of Bi (So )B3, 70 percent of Bi 0 This soluble mixture, but with The bath contains also about lg. of formol per liter in order to avoid the anodic oxidation of the stannous ions (Sn* into stannic ions $11 Besides, this bath may include gelatine the proportions of which are 2 to 7 g. per liter and B-naphtol the proportions of which are 0.5 to 1.5 g. per liter in order to improve the quality of the deposit.
The bath may also contain brighteners in appropriate proportions.
The so-formed bath has an acid pI-l and its acidity corresponds to the acidity of a solution containing 100 g./liter of sulphuric acid. The density is about 13 B.
The electroplating process is carried out at a temperature within 20-50 C. The voltage is between 1 and 3 volts and the current density is between 0.8 and 3A/dm For a current density of lA/dm, the obtained deposit ratio is 0.5 M/mlllllte. The anode-cathode surface ratio may be between 1 and 1.5. The following examples are only given by way of a non limitative example. Six deposit tests have been made upon a steel sheet coated with a nickel layer which is of the Watt type and 15 p. thick, by varying the potential. The bath had the following composition:
tin fluoborate 30g/liter of metal tin fluoboric acid 130g/liter boric-acid 30g/liter mixture: bismuth sulphate 30% by weight bismuth oxide 70% by weight 0.3g/liter formol lg/liter equivalent acid H IOOg/liter The tests have been made at 25 C. and are gathered in the following table.
Percent by Current weight of Voltage, density, Time, B1 in the Tests No. v. a./dm. hours deposit The so-prepared plates, after a stay of days at 0 C showed no trace of tin pest or oxidation.
The preferred percentage of bismuth in tin is 0.4 percent.
When performing the electroplating operation, it should be advisable to empty the container every 24 hours in order to prevent tin from getting enriched with tin at rest, to check the bags containing bismuth and to clean the container.
Though the description makes use of tin fluoborate, it is obvious for the man skilled in the art that another tin salt can be used. The man skilled in the art will also recognize that bismuth can be inserted in forms different from that used in the invention.
It is clear that the previous description has only been given as an unrestrictive example and that numerous alternatives may be considered without departing from the spirit and scope of the invention.
What is claimed is:
1. An aqueous bath for electroplating tin-bismuth alloy, characterized in that it includes acid ions in order to maintain pH acid, and characterized in that the bismuth is inserted in the form of a bismuth sulphate-bismuth oxide mixture, the concentration of which relative to the entire bath is between 0.1 and 0.5 grams per liter and in which the relative proportion of bismuth sulphate to bismuth oxide is in the range between 15/85 and 1.
2. An aqueous electroplating bath characterized in that it includes:
1. tin fluoborate equivalent to 30g/liter of metal tin i oxide is in the range between 15/85 and l. I I 8/ of fluqbfllrif acid 4. A tin plating bath according to claim 3 wherein said a bismuth mixture comprises bismuth sulphate and bismuth sulphatemismuth t fggzg the oxide in relative weight proportions of approximately 30 to 70 es tive on s b hts f wh' h 5 Pei-cam lrc 5%-75Z y s. A tin plating bath according to claim 4 including approxi- 5. lgll 0 f l mately 1 gram per liter of formal as additive to inhibit anodic oxidation of the stannous ions.
3. An aqueous acid fluoborate tin-bismuth alloy electroplat- 6. A tin plating bath according to claim 4 wherein the coning bath containing stannous ions, free fluoboric acid and an ceml'ation of said liiismulh tu In p op tion t fh lOtal acid soluble mixture of bismuth sulphate and bismuth oxide in volume of the bath between and grams P which the relative proportion of bismuth sulphate to bismuth

Claims (5)

  1. 2. An aqueous electroplating bath characterized in that it includes:
  2. 3. An aqueous acid fluoborate tin-bismuth alloy electroplating bath containing stannous ions, free fluoboric acid and an acid soluble mixture of bismuth sulphate and bismuth oxide in which the relative proportion of bismuth sulphate to bismuth oxide is in the range between 15/85 and 1.
  3. 4. A tin plating bath according to claim 3 wherein said bismuth mixture comprises bismuth sulphate and bismuth oxide in relative weight proportions of approximately 30 to 70 percent.
  4. 5. A tin plating bath according to claim 4 including approximately 1 gram per liter of formol as additive to inhibit anodic oxidation of the stannous ions.
  5. 6. A tin plating bath according to claim 4 wherein the concentration of said bismuth mixture in proportion to the total volume of the bath is between 0.1 and 0.5 grams per liter.
US79272A 1969-12-19 1970-10-08 Bath for electroplating tin-bismuth alloy Expired - Lifetime US3663384A (en)

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Cited By (22)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4162205A (en) * 1978-10-19 1979-07-24 Vulcan Materials Company Method of electroplating tin and alkaline electroplating bath therefor
US4331518A (en) * 1981-01-09 1982-05-25 Vulcan Materials Company Bismuth composition, method of electroplating a tin-bismuth alloy and electroplating bath therefor
US4565610A (en) * 1983-12-22 1986-01-21 Learonal, Inc. Bath and process for plating lead and lead/tin alloys
US4565609A (en) * 1983-12-22 1986-01-21 Learonal, Inc. Bath and process for plating tin, lead and tin-lead alloys
US4599149A (en) * 1981-09-11 1986-07-08 Learonal, Inc. Process for electroplating tin, lead and tin-lead alloys and baths therefor
US4617097A (en) * 1983-12-22 1986-10-14 Learonal, Inc. Process and electrolyte for electroplating tin, lead or tin-lead alloys
US4701244A (en) * 1983-12-22 1987-10-20 Learonal, Inc. Bath and process for electroplating tin, lead and tin/alloys
US4717460A (en) * 1983-12-22 1988-01-05 Learonal, Inc. Tin lead electroplating solutions
US4749626A (en) * 1985-08-05 1988-06-07 Olin Corporation Whisker resistant tin coatings and baths and methods for making such coatings
US4871429A (en) * 1981-09-11 1989-10-03 Learonal, Inc Limiting tin sludge formation in tin or tin/lead electroplating solutions
WO1990004048A1 (en) * 1988-10-14 1990-04-19 Atochem North America, Inc. A method, bath and cell for the electrodeposition of tin-bismuth alloys
US5039576A (en) * 1989-05-22 1991-08-13 Atochem North America, Inc. Electrodeposited eutectic tin-bismuth alloy on a conductive substrate
US5066367A (en) * 1981-09-11 1991-11-19 Learonal Inc. Limiting tin sludge formation in tin or tin/lead electroplating solutions
US5094726A (en) * 1981-09-11 1992-03-10 Learonal, Inc. Limiting tin sludge formation in tin or tin-lead electroplating solutions
US5391402A (en) * 1993-12-03 1995-02-21 Motorola Immersion plating of tin-bismuth solder
US5393573A (en) * 1991-07-16 1995-02-28 Microelectronics And Computer Technology Corporation Method of inhibiting tin whisker growth
US5450784A (en) * 1993-09-28 1995-09-19 Detroit Diesel Corporation Electroplated piston skirt for improved scuff resistance
WO2003021008A1 (en) * 2000-02-29 2003-03-13 Learonal Japan Inc. Tin electroplating solution and method for plating
US20090145765A1 (en) * 2007-12-11 2009-06-11 Enthone Inc. Composite coatings for whisker reduction
US20090145764A1 (en) * 2007-12-11 2009-06-11 Enthone Inc. Composite coatings for whisker reduction
US20140332393A1 (en) * 2013-05-09 2014-11-13 Ebara Corporation Sn ALLOY PLATING APPARATUS AND Sn ALLOY PLATING METHOD
US9850588B2 (en) 2015-09-09 2017-12-26 Rohm And Haas Electronic Materials Llc Bismuth electroplating baths and methods of electroplating bismuth on a substrate

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KR102579360B1 (en) * 2018-12-04 2023-09-18 현대자동차주식회사 Auxiliary brake control system of vehicle
CN111188069A (en) * 2019-12-31 2020-05-22 大连长丰实业总公司 Tin-plated bismuth alloy solution and preparation method thereof

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB526037A (en) * 1938-03-07 1940-09-10 Remy Van Der Zypen & Co A method for producing an electroplated tin coating on other metals, particularly iron or steel sheets or strips
US3360446A (en) * 1964-05-08 1967-12-26 M & T Chemicals Inc Electrodepositing a tin-bismuth alloy and additives therefor
US3522155A (en) * 1964-07-10 1970-07-28 M & T Chemicals Inc Method of electrodepositing a tinbismuth alloy and compositions therefor

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB526037A (en) * 1938-03-07 1940-09-10 Remy Van Der Zypen & Co A method for producing an electroplated tin coating on other metals, particularly iron or steel sheets or strips
US3360446A (en) * 1964-05-08 1967-12-26 M & T Chemicals Inc Electrodepositing a tin-bismuth alloy and additives therefor
US3522155A (en) * 1964-07-10 1970-07-28 M & T Chemicals Inc Method of electrodepositing a tinbismuth alloy and compositions therefor

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
Frederick A. Lowenheim, Modern Electroplating, p. 373, (1968) *
N. T. Kudryavtsev et al., Trudy MKHTI imenl D. I. Mendeleeva, No. 266, pp. 113 119, (1959) *

Cited By (26)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4162205A (en) * 1978-10-19 1979-07-24 Vulcan Materials Company Method of electroplating tin and alkaline electroplating bath therefor
US4331518A (en) * 1981-01-09 1982-05-25 Vulcan Materials Company Bismuth composition, method of electroplating a tin-bismuth alloy and electroplating bath therefor
US5094726A (en) * 1981-09-11 1992-03-10 Learonal, Inc. Limiting tin sludge formation in tin or tin-lead electroplating solutions
US5066367A (en) * 1981-09-11 1991-11-19 Learonal Inc. Limiting tin sludge formation in tin or tin/lead electroplating solutions
US4599149A (en) * 1981-09-11 1986-07-08 Learonal, Inc. Process for electroplating tin, lead and tin-lead alloys and baths therefor
US4871429A (en) * 1981-09-11 1989-10-03 Learonal, Inc Limiting tin sludge formation in tin or tin/lead electroplating solutions
US4701244A (en) * 1983-12-22 1987-10-20 Learonal, Inc. Bath and process for electroplating tin, lead and tin/alloys
US4717460A (en) * 1983-12-22 1988-01-05 Learonal, Inc. Tin lead electroplating solutions
US4617097A (en) * 1983-12-22 1986-10-14 Learonal, Inc. Process and electrolyte for electroplating tin, lead or tin-lead alloys
US4565609A (en) * 1983-12-22 1986-01-21 Learonal, Inc. Bath and process for plating tin, lead and tin-lead alloys
US4565610A (en) * 1983-12-22 1986-01-21 Learonal, Inc. Bath and process for plating lead and lead/tin alloys
US4749626A (en) * 1985-08-05 1988-06-07 Olin Corporation Whisker resistant tin coatings and baths and methods for making such coatings
WO1990004048A1 (en) * 1988-10-14 1990-04-19 Atochem North America, Inc. A method, bath and cell for the electrodeposition of tin-bismuth alloys
US5039576A (en) * 1989-05-22 1991-08-13 Atochem North America, Inc. Electrodeposited eutectic tin-bismuth alloy on a conductive substrate
US5393573A (en) * 1991-07-16 1995-02-28 Microelectronics And Computer Technology Corporation Method of inhibiting tin whisker growth
US5450784A (en) * 1993-09-28 1995-09-19 Detroit Diesel Corporation Electroplated piston skirt for improved scuff resistance
US5391402A (en) * 1993-12-03 1995-02-21 Motorola Immersion plating of tin-bismuth solder
US5435838A (en) * 1993-12-03 1995-07-25 Motorola, Inc. Immersion plating of tin-bismuth solder
WO2003021008A1 (en) * 2000-02-29 2003-03-13 Learonal Japan Inc. Tin electroplating solution and method for plating
US20090145765A1 (en) * 2007-12-11 2009-06-11 Enthone Inc. Composite coatings for whisker reduction
US20090145764A1 (en) * 2007-12-11 2009-06-11 Enthone Inc. Composite coatings for whisker reduction
US8226807B2 (en) 2007-12-11 2012-07-24 Enthone Inc. Composite coatings for whisker reduction
US8906217B2 (en) 2007-12-11 2014-12-09 Enthone Inc. Composite coatings for whisker reduction
US20140332393A1 (en) * 2013-05-09 2014-11-13 Ebara Corporation Sn ALLOY PLATING APPARATUS AND Sn ALLOY PLATING METHOD
US9816197B2 (en) * 2013-05-09 2017-11-14 Ebara Corporation Sn alloy plating apparatus and Sn alloy plating method
US9850588B2 (en) 2015-09-09 2017-12-26 Rohm And Haas Electronic Materials Llc Bismuth electroplating baths and methods of electroplating bismuth on a substrate

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DE2050145A1 (en) 1971-06-24
GB1299519A (en) 1972-12-13
FR2071199A5 (en) 1971-09-17
JPS4931606B1 (en) 1974-08-23

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