EP1378590A1 - Bath for gold electro deposition - Google Patents

Bath for gold electro deposition Download PDF

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Publication number
EP1378590A1
EP1378590A1 EP02405558A EP02405558A EP1378590A1 EP 1378590 A1 EP1378590 A1 EP 1378590A1 EP 02405558 A EP02405558 A EP 02405558A EP 02405558 A EP02405558 A EP 02405558A EP 1378590 A1 EP1378590 A1 EP 1378590A1
Authority
EP
European Patent Office
Prior art keywords
gold
bismuth
bath
sulfite
bath according
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Withdrawn
Application number
EP02405558A
Other languages
German (de)
French (fr)
Inventor
Pierre Laude
Pierre-André Aeby
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Metalor Technologies International SA
Original Assignee
Metalor Technologies International SA
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Metalor Technologies International SA filed Critical Metalor Technologies International SA
Priority to EP02405558A priority Critical patent/EP1378590A1/en
Priority to EP03729763A priority patent/EP1520063B1/en
Priority to ES03729763T priority patent/ES2252673T3/en
Priority to AU2003240347A priority patent/AU2003240347A1/en
Priority to PCT/CH2003/000400 priority patent/WO2004005589A1/en
Priority to AT03729763T priority patent/ATE307918T1/en
Priority to DE60302074T priority patent/DE60302074T2/en
Publication of EP1378590A1 publication Critical patent/EP1378590A1/en
Withdrawn legal-status Critical Current

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Classifications

    • 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
    • C25D3/48—Electroplating: Baths therefor from solutions of gold

Definitions

  • the present invention relates to the field of baths for deposits Electrolytic. It relates, more particularly, to a sulphite gold bath of type of those used to deposit layers of gold both ductile and thick, ie typically more than 200 ⁇ m. These deposits are particularly well suited, in particular, to the production of protuberances conductors, known as "bumps", used to connect electronic chips.
  • toxicity being a very relative notion, we will define as toxic a harmful substance in the quantities used for the intended application and as non-toxic a substance which does not harm this application.
  • metal layer be particularly ductile, regular, fine grains with very low hardness.
  • the sulphite gold baths currently known provide too much deposits. hard, which requires additional heat treatment to soften them. Of more, they use toxic grain refiners, containing arsenic or thallium. Furthermore, the solutions obtained are aggressive and attack the substrates, especially when it comes to photoresists.
  • the main object of the present invention is to provide a sulphite gold bath free of toxic compounds and allowing a deposit particularly tender, without having to use a subsequent heat treatment.
  • the pH of the bath obtained is neutral and the solution does not attack the photoresists commonly used.
  • the bath according to the invention is of the type comprising, in solution in water, gold sulfite, a grain refiner, a complexing agent and a conductive salt.
  • This bath is characterized in that its grain refiner, not toxic, is chosen from soluble compounds of bismuth, tin, tellurium and selenium.
  • the bath also comprises amidosulfonic acid.
  • the bath obtained uses neither toxic gold salt, nor toxic grain refiner.
  • it makes it possible to obtain tender deposits, typically having a hardness between 50 and 70 Vickers, without the need to perform a any heat treatment.
  • the solution obtained does not attack substrates on which bumps are commonly deposited and its pH is typically between 6.7 and 7.5.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Electroplating And Plating Baths Therefor (AREA)
  • Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)

Abstract

A bath for the electrolytic deposition of gold comprises, in solution in water, a gold sulfite, a grain refiner, an inhibitor and a conducting salt. The grain refiner is chosen from soluble compounds of bismuth, tin, tellurium and selenium. Preferred Features: The soluble bismuth compound is a soluble complex of ammonium citrate and bismuth. The inhibitor contains a derivative of phosphonic acid. The conducting salt is ammonium sulfite. The bath may also contain 20-100 g/liter, preferably 50 g/liter, of amidosulphonic acid.

Description

La présente invention se rapporte au domaine des bains pour dépôts électrolytiques. Elle concerne, plus particulièrement, un bain d'or sulfitique du type de ceux employés pour déposer des couches d'or à la fois ductiles et épaisses, c'est à dire typiquement de plus de 200 µm. Ces dépôts sont particulièrement bien adaptés, notamment, à la réalisation de protubérances conductrices, connues sous le nom de "bumps", utilisées pour connecter des puces électroniques.The present invention relates to the field of baths for deposits Electrolytic. It relates, more particularly, to a sulphite gold bath of type of those used to deposit layers of gold both ductile and thick, ie typically more than 200 µm. These deposits are particularly well suited, in particular, to the production of protuberances conductors, known as "bumps", used to connect electronic chips.

Pendant longtemps, l'or a été présent dans les bains sous la forme de complexes cyanurés, comme (Au(CN)2)-. Cependant, malgré la qualité des dépôts obtenus, la toxicité des cyanures a conduit à la recherche d'autres produits et des solutions de complexes solubles de sulfites d'or y ont été substituées.For a long time, gold has been present in baths in the form of cyanide complexes, such as (Au (CN) 2 ) - . However, despite the quality of the deposits obtained, the toxicity of cyanides led to the search for other products and solutions of soluble complexes of gold sulfites were substituted.

On notera que, la toxicité étant une notion très relative, on définira comme toxique une substance nocive dans les quantités utilisées pour l'application visée et comme non-toxique une substance ne présentant pas de nocivité pour cette application.Note that, toxicity being a very relative notion, we will define as toxic a harmful substance in the quantities used for the intended application and as non-toxic a substance which does not harm this application.

Certaines utilisations de dépôts d'or, notamment pour la réalisation de bumps, nécessitent que la couche de métal soit particulièrement ductile, régulière, à grains fins et présentant une très faible dureté.Certain uses of gold deposits, in particular for making bumps, require that the metal layer be particularly ductile, regular, fine grains with very low hardness.

Or, les bains d'or sulfitiques connus actuellement fournissent des dépôts trop durs, ce qui impose un traitement thermique supplémentaire pour les ramollir. De plus, ils utilisent des affineurs de grains toxiques, contenant de l'arsenic ou du thallium. Par ailleurs, les solutions obtenues sont agressives et attaquent les substrats, notamment lorsqu'il s'agit de photorésistes. Now, the sulphite gold baths currently known provide too much deposits. hard, which requires additional heat treatment to soften them. Of more, they use toxic grain refiners, containing arsenic or thallium. Furthermore, the solutions obtained are aggressive and attack the substrates, especially when it comes to photoresists.

La présente invention a principalement pour but de fournir un bain d'or sulfitique exempt de composés toxiques et permettant de réaliser un dépôt particulièrement tendre, sans avoir recours à un traitement thermique ultérieur. Le pH du bain obtenu est neutre et la solution n'attaque pas les photorésistes couramment utilisés.The main object of the present invention is to provide a sulphite gold bath free of toxic compounds and allowing a deposit particularly tender, without having to use a subsequent heat treatment. The pH of the bath obtained is neutral and the solution does not attack the photoresists commonly used.

De façon plus précise, le bain selon l'invention est du type comportant, en solution dans de l'eau, du sulfite d'or, un affineur de grain, un complexant et un sel conducteur. Ce bain est caractérisé en ce que son affineur de grain, non toxique, est choisi parmi des composés solubles de bismuth, d'étain, de tellure et de sélénium.More precisely, the bath according to the invention is of the type comprising, in solution in water, gold sulfite, a grain refiner, a complexing agent and a conductive salt. This bath is characterized in that its grain refiner, not toxic, is chosen from soluble compounds of bismuth, tin, tellurium and selenium.

De façon avantageuse, le bain comporte, en outre, de l'acide amidosulfonique.Advantageously, the bath also comprises amidosulfonic acid.

D'autres caractéristiques de l'invention ressortiront de la description qui va suivre, non accompagnée de dessin.Other characteristics of the invention will emerge from the description which follows follow, not accompanied by a drawing.

De préférence, le bain pour dépôt électrolytique d'or selon l'invention comporte :

  • de 7 à 20 g/L d'or, sous la forme de sulfite d'or choisi parmi d'autres sels solubles d'or pour la qualité du dépôt obtenu,
  • de 5 à 50 mg/L de bismuth, sous la forme d'un sel soluble de citrate d'ammonium et de bismuth, utilisé comme affineur de grain non-toxique,
  • de 10 à 50 mL/L d'un dérivé d'acide phosphonique, par exemple, le produit connu sous le nom de Dequest 2010, utilisé comme complexant,
  • de 20 à 100 g/L de sulfite d'ammonium, utilisé comme sel conducteur pour l'électrodéposition, et
  • de 20 à 100 g/L d'acide amidosulfonique, également utilisé comme sel conducteur.
Preferably, the bath for electrolytic deposition of gold according to the invention comprises:
  • from 7 to 20 g / L of gold, in the form of gold sulphite chosen from other soluble gold salts for the quality of the deposit obtained,
  • 5 to 50 mg / L of bismuth, in the form of a soluble salt of ammonium citrate and bismuth, used as a non-toxic grain refiner,
  • 10 to 50 mL / L of a phosphonic acid derivative, for example, the product known as Dequest 2010, used as a complexing agent,
  • from 20 to 100 g / L of ammonium sulfite, used as a conductive salt for electroplating, and
  • from 20 to 100 g / L of amidosulfonic acid, also used as a conductive salt.

Selon un mode de réalisation particulièrement avantageux, le bain comporte :

  • 10 g/L d'or, sous la forme de sulfite d'or,
  • 15 mg/L de bismuth, sous la forme d'un sel soluble de citrate d'ammonium et de bismuth,
  • 25 mL/L de Dequest 2010,
  • 50 g/L de sulfite d'ammonium, et
  • 50 g/L d'acide amidosulfonique.
According to a particularly advantageous embodiment, the bath comprises:
  • 10 g / L of gold, in the form of gold sulfite,
  • 15 mg / L of bismuth, in the form of a soluble salt of ammonium citrate and bismuth,
  • 25 mL / L of Dequest 2010,
  • 50 g / L of ammonium sulfite, and
  • 50 g / L of amidosulfonic acid.

Ainsi, le bain obtenu n'utilise ni de sel d'or toxique, ni d'affineur de grains toxique. De plus, il permet d'obtenir des dépôts tendres, présentant typiquement une dureté comprise entre 50 et 70 Vickers, sans qu'il soit nécessaire d'effectuer un quelconque traitement thermique. La solution obtenue n'attaque pas les substrats sur lesquelles des bumps sont couramment déposés et son pH est typiquement compris entre 6,7 et 7,5.Thus, the bath obtained uses neither toxic gold salt, nor toxic grain refiner. In addition, it makes it possible to obtain tender deposits, typically having a hardness between 50 and 70 Vickers, without the need to perform a any heat treatment. The solution obtained does not attack substrates on which bumps are commonly deposited and its pH is typically between 6.7 and 7.5.

La description qui vient d'être faite n'est qu'un exemple particulier d'un bain pour dépôt d'or électrolytique selon l'invention. Il est aussi possible d'utiliser, comme affineur de grain, tout composé soluble d'étain, de tellure ou de sélénium.The description which has just been made is only a particular example of a bath for electrolytic gold deposition according to the invention. It is also possible to use, like grain refiner, any soluble compound of tin, tellurium or selenium.

Claims (8)

Bain pour dépôt électrolytique d'or, comportant, en solution dans de l'eau, du sulfite d'or, un affineur de grain, un complexant et un sel conducteur, caractérisé en ce que ledit affineur de grain est choisi parmi des composés solubles de bismuth, d'étain, de tellure et de sélénium.Bath for the electrolytic deposition of gold, comprising, in solution in water, gold sulfite, a grain refiner, a complexing agent and a conductive salt, characterized in that said grain refiner is chosen from soluble compounds bismuth, tin, tellurium and selenium. Bain selon la revendication 1, caractérisé en ce que ledit composé de bismuth est un complexe soluble de citrate d'ammonium et de bismuth.Bath according to claim 1, characterized in that said bismuth compound is a soluble complex of ammonium citrate and bismuth. Bain selon l'une des revendications 1 et 2, caractérisé en ce que ledit complexant contient un dérivé d'acide phosphonique.Bath according to either of Claims 1 and 2, characterized in that the said complexing agent contains a phosphonic acid derivative. Bain selon l'une des revendications 1 à 3, caractérisé en ce que ledit sel conducteur est du sulfite d'ammonium.Bath according to one of claims 1 to 3, characterized in that said conductive salt is ammonium sulfite. Bain selon l'une des revendications 2 à 4, caractérisé en ce qu'il comporte: de 7 à 20 g/L d'or, de 5 à 50 mg/L de bismuth, de 10 à 50 mL/L d'un dérivé d'acide phosphonique, et de 20 à 100 g/L de sulfite d'ammonium. Bath according to one of Claims 2 to 4, characterized in that it comprises: from 7 to 20 g / L of gold, from 5 to 50 mg / L of bismuth, from 10 to 50 mL / L of a phosphonic acid derivative, and from 20 to 100 g / L of ammonium sulfite. Bain selon la revendication 5, caractérisé en ce qu'il comporte : 10 g/L d'or, 15 mg/L de bismuth, 25 mL/L d'un dérivé d'acide phosphonique, et 50 g/L de sulfite d'ammonium. Bath according to claim 5, characterized in that it comprises: 10 g / L of gold, 15 mg / L of bismuth, 25 mL / L of a phosphonic acid derivative, and 50 g / L of ammonium sulfite. Bain selon l'une des revendications 1 à 6, caractérisé en ce qu'il comporte, en outre, de 20 à 100 g/L d'acide amidosulfonique.Bath according to one of Claims 1 to 6, characterized in that it additionally comprises from 20 to 100 g / L of amidosulfonic acid. Bain selon la revendication 7, caractérisé en ce qu'il comporte 50 g/L d'acide amidosulfonique.Bath according to claim 7, characterized in that it comprises 50 g / L of amidosulfonic acid.
EP02405558A 2002-07-04 2002-07-04 Bath for gold electro deposition Withdrawn EP1378590A1 (en)

Priority Applications (7)

Application Number Priority Date Filing Date Title
EP02405558A EP1378590A1 (en) 2002-07-04 2002-07-04 Bath for gold electro deposition
EP03729763A EP1520063B1 (en) 2002-07-04 2003-06-20 Bath for gold electrodeposition
ES03729763T ES2252673T3 (en) 2002-07-04 2003-06-20 BATHROOM FOR GOLD ELECTROLYTIC DEPOSIT.
AU2003240347A AU2003240347A1 (en) 2002-07-04 2003-06-20 Bath for gold electrodeposition
PCT/CH2003/000400 WO2004005589A1 (en) 2002-07-04 2003-06-20 Bath for gold electrodeposition
AT03729763T ATE307918T1 (en) 2002-07-04 2003-06-20 BATH FOR GALVANIC GOLD DEPOSITION
DE60302074T DE60302074T2 (en) 2002-07-04 2003-06-20 BATHROOM FOR GALVANIC GOLD BUST

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
EP02405558A EP1378590A1 (en) 2002-07-04 2002-07-04 Bath for gold electro deposition

Publications (1)

Publication Number Publication Date
EP1378590A1 true EP1378590A1 (en) 2004-01-07

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EP02405558A Withdrawn EP1378590A1 (en) 2002-07-04 2002-07-04 Bath for gold electro deposition
EP03729763A Expired - Lifetime EP1520063B1 (en) 2002-07-04 2003-06-20 Bath for gold electrodeposition

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Application Number Title Priority Date Filing Date
EP03729763A Expired - Lifetime EP1520063B1 (en) 2002-07-04 2003-06-20 Bath for gold electrodeposition

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EP (2) EP1378590A1 (en)
AT (1) ATE307918T1 (en)
AU (1) AU2003240347A1 (en)
DE (1) DE60302074T2 (en)
ES (1) ES2252673T3 (en)
WO (1) WO2004005589A1 (en)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE102005036133B4 (en) 2005-07-26 2013-09-12 Wieland Dental + Technik Gmbh & Co. Kg Bath for the electrodeposition of gold and gold alloys and additive mixture for such a bath
CN103741180A (en) * 2014-01-10 2014-04-23 哈尔滨工业大学 Cyanide-free bright electrogilding additive and application thereof

Families Citing this family (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR101464343B1 (en) * 2013-04-02 2014-11-28 한밭대학교 산학협력단 Non cyanide gold plating bath for bump and preparation method of bump
CN103741181B (en) * 2014-01-10 2016-01-27 哈尔滨工业大学 A kind of many coordination agents cyanide-free gold electroplating plating solution and electrogilding technique
CN107299366A (en) * 2017-08-24 2017-10-27 重庆立道表面技术有限公司 Non-cyanide plating solution for copper-plating used

Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR2060106A1 (en) * 1969-08-19 1971-06-11 Sel Rex Corp Bath for electroplating gold
GB1325352A (en) * 1969-08-08 1973-08-01 Sel Rex Corp Electrodeposition of gold and gold alloys
DE3537283A1 (en) * 1984-10-25 1986-04-30 VEB Mikroelektronik "Friedrich Engels" Ilmenau, DDR 6300 Ilmenau Gold electroplating bath for fabricating functional gold layers at high deposition rates
US4795534A (en) * 1986-09-25 1989-01-03 Vanguard Research Associates, Inc. Electrolyte solution and process for gold electroplating
US5055173A (en) * 1989-02-24 1991-10-08 Degussa Aktiengesellschaft Bath for the electrolytic deposition of fine gold coatings
DE4226167A1 (en) * 1992-08-07 1994-02-10 Sel Alcatel Ag Device mounting on substrate by thermo:compression bonding - using electroplated gold@ contact bumps, esp. for chip on chip bonding
WO2002068728A1 (en) * 2001-02-28 2002-09-06 Wieland Dental + Technik Gmbh & Co. Kg Bath for the galvanic deposition of gold and gold alloys, and the use thereof

Family Cites Families (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE3805627A1 (en) * 1988-02-24 1989-09-07 Wieland Edelmetalle GOLD BATH
DE4425110C1 (en) * 1994-07-15 1995-10-26 Heraeus Gmbh W C Aq. plating bath for electrodeposition of palladium

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB1325352A (en) * 1969-08-08 1973-08-01 Sel Rex Corp Electrodeposition of gold and gold alloys
FR2060106A1 (en) * 1969-08-19 1971-06-11 Sel Rex Corp Bath for electroplating gold
DE3537283A1 (en) * 1984-10-25 1986-04-30 VEB Mikroelektronik "Friedrich Engels" Ilmenau, DDR 6300 Ilmenau Gold electroplating bath for fabricating functional gold layers at high deposition rates
US4795534A (en) * 1986-09-25 1989-01-03 Vanguard Research Associates, Inc. Electrolyte solution and process for gold electroplating
US5055173A (en) * 1989-02-24 1991-10-08 Degussa Aktiengesellschaft Bath for the electrolytic deposition of fine gold coatings
DE4226167A1 (en) * 1992-08-07 1994-02-10 Sel Alcatel Ag Device mounting on substrate by thermo:compression bonding - using electroplated gold@ contact bumps, esp. for chip on chip bonding
WO2002068728A1 (en) * 2001-02-28 2002-09-06 Wieland Dental + Technik Gmbh & Co. Kg Bath for the galvanic deposition of gold and gold alloys, and the use thereof

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE102005036133B4 (en) 2005-07-26 2013-09-12 Wieland Dental + Technik Gmbh & Co. Kg Bath for the electrodeposition of gold and gold alloys and additive mixture for such a bath
DE102005036133C5 (en) * 2005-07-26 2017-07-13 Ivoclar Vivadent Ag Bath for the electrodeposition of gold and gold alloys and additive mixture for such a bath
CN103741180A (en) * 2014-01-10 2014-04-23 哈尔滨工业大学 Cyanide-free bright electrogilding additive and application thereof
CN103741180B (en) * 2014-01-10 2015-11-25 哈尔滨工业大学 Non-cyanide bright electrogilding additive and application thereof

Also Published As

Publication number Publication date
EP1520063A1 (en) 2005-04-06
DE60302074D1 (en) 2005-12-01
ES2252673T3 (en) 2006-05-16
AU2003240347A1 (en) 2004-01-23
DE60302074T2 (en) 2006-07-13
ATE307918T1 (en) 2005-11-15
EP1520063B1 (en) 2005-10-26
WO2004005589A1 (en) 2004-01-15

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