EP0050343B1 - Molybdène enduit de métal précieux et son procédé de fabrication - Google Patents

Molybdène enduit de métal précieux et son procédé de fabrication Download PDF

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Publication number
EP0050343B1
EP0050343B1 EP81108457A EP81108457A EP0050343B1 EP 0050343 B1 EP0050343 B1 EP 0050343B1 EP 81108457 A EP81108457 A EP 81108457A EP 81108457 A EP81108457 A EP 81108457A EP 0050343 B1 EP0050343 B1 EP 0050343B1
Authority
EP
European Patent Office
Prior art keywords
duration
molybdenum
temperature
seconds
process 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.)
Expired
Application number
EP81108457A
Other languages
German (de)
English (en)
Other versions
EP0050343A1 (fr
Inventor
Wolfgang Ing.-Grad. Pikorz
Alois Dipl.-Phys. Sonntag
Hans Ing.-Grad. Scheuermann
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Licentia Patent Verwaltungs GmbH
Original Assignee
Licentia Patent Verwaltungs GmbH
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 Licentia Patent Verwaltungs GmbH filed Critical Licentia Patent Verwaltungs GmbH
Publication of EP0050343A1 publication Critical patent/EP0050343A1/fr
Application granted granted Critical
Publication of EP0050343B1 publication Critical patent/EP0050343B1/fr
Expired legal-status Critical Current

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Classifications

    • 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
    • C23G—CLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
    • C23G1/00—Cleaning or pickling metallic material with solutions or molten salts
    • C23G1/02—Cleaning or pickling metallic material with solutions or molten salts with acid solutions
    • C23G1/10—Other heavy metals
    • C23G1/106—Other heavy metals refractory metals
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
    • C25D5/10—Electroplating with more than one layer of the same or of different metals
    • C25D5/12—Electroplating with more than one layer of the same or of different metals at least one layer being of nickel or chromium
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
    • C25D5/34—Pretreatment of metallic surfaces to be electroplated
    • C25D5/38—Pretreatment of metallic surfaces to be electroplated of refractory metals or nickel
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
    • C25D5/48—After-treatment of electroplated surfaces
    • C25D5/50—After-treatment of electroplated surfaces by heat-treatment
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25F—PROCESSES FOR THE ELECTROLYTIC REMOVAL OF MATERIALS FROM OBJECTS; APPARATUS THEREFOR
    • C25F3/00—Electrolytic etching or polishing
    • C25F3/02—Etching
    • C25F3/08—Etching of refractory metals
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10S428/00—Stock material or miscellaneous articles
    • Y10S428/922—Static electricity metal bleed-off metallic stock
    • Y10S428/923—Physical dimension
    • Y10S428/924—Composite
    • Y10S428/926—Thickness of individual layer specified
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/12—All metal or with adjacent metals
    • Y10T428/12229—Intermediate article [e.g., blank, etc.]
    • Y10T428/12236—Panel having nonrectangular perimeter
    • Y10T428/12243—Disk
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/12—All metal or with adjacent metals
    • Y10T428/12493—Composite; i.e., plural, adjacent, spatially distinct metal components [e.g., layers, joint, etc.]
    • Y10T428/12771—Transition metal-base component
    • Y10T428/12806—Refractory [Group IVB, VB, or VIB] metal-base component
    • Y10T428/12826—Group VIB metal-base component
    • Y10T428/12833—Alternative to or next to each other
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/12—All metal or with adjacent metals
    • Y10T428/12493—Composite; i.e., plural, adjacent, spatially distinct metal components [e.g., layers, joint, etc.]
    • Y10T428/12771—Transition metal-base component
    • Y10T428/12806—Refractory [Group IVB, VB, or VIB] metal-base component
    • Y10T428/12826—Group VIB metal-base component
    • Y10T428/12847—Cr-base component
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/12—All metal or with adjacent metals
    • Y10T428/12493—Composite; i.e., plural, adjacent, spatially distinct metal components [e.g., layers, joint, etc.]
    • Y10T428/12771—Transition metal-base component
    • Y10T428/12861—Group VIII or IB metal-base component
    • Y10T428/12875—Platinum group metal-base component
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/12—All metal or with adjacent metals
    • Y10T428/12493—Composite; i.e., plural, adjacent, spatially distinct metal components [e.g., layers, joint, etc.]
    • Y10T428/12771—Transition metal-base component
    • Y10T428/12861—Group VIII or IB metal-base component
    • Y10T428/12889—Au-base component
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/12—All metal or with adjacent metals
    • Y10T428/12493—Composite; i.e., plural, adjacent, spatially distinct metal components [e.g., layers, joint, etc.]
    • Y10T428/12771—Transition metal-base component
    • Y10T428/12861—Group VIII or IB metal-base component
    • Y10T428/12896—Ag-base component

Definitions

  • the invention relates to molybdenum, which is coated with a noble metal, and a method for producing such a layer sequence.
  • Such layer sequences are widely used in semiconductor technology as contact material, because the thermal expansion coefficient of the silicon used as the semiconductor material and the thermal expansion coefficient of the molybdenum used as the contact material are similar to each other and therefore no or only low thermal stresses occur even at changing operating temperatures.
  • the molybdenum which is used in the form of disks with a disk thickness of approximately 0.5 to a few mm, is coated with a noble metal, whereby a favorable electrical contact resistance is achieved.
  • the noble metal protects the molybdenum contact against oxidation of the surface and against the attack of aggressive chemicals, which act on the semiconductor body in the course of further process steps during an etching treatment, the shape and properties of which develop, but must not damage the molybdenum contact during this etching treatment.
  • the thinnest possible coating is desirable; however, a certain minimum layer thickness of the precious metal must not be undercut, because otherwise sufficient etch resistance is no longer guaranteed.
  • gold as the coating material, for example, there is sufficient etching resistance only if the layer thickness is at least 1.5 to 3 ⁇ m. With layer thicknesses of less than 1.5 ⁇ m, pores occur, which means that attacks of the base material molybdenum cannot be avoided during etching. Therefore, in practice it has not been possible to do without a thicker gold layer.
  • thinner layer thicknesses of the coating material result in higher costs for the base material, because this has to be prepared better and more uniformly.
  • the high mechanical sensitivity of such thin layers is disadvantageous.
  • layer thicknesses of the noble metal are required. In the case of smaller disk diameters, for example diameters of approximately 6 mm, the noble metal layer thicknesses must be up to 10 ⁇ m.
  • a disadvantage of a coating with chromium is that poor and, above all, fluctuating contact resistances are then recorded, which preclude general use. These fluctuating transition resistances of chromium are probably due to surface oxidation processes that occur randomly and irregularly and cannot be influenced in a targeted manner.
  • temperatures of over 100 ° C occur during several work steps from the alloying of the diffused silicon body to the chromium-coated molybdenum wafer to the installation in a hermetically sealed housing, as a result of which the above-mentioned are evident Oxidation processes are promoted.
  • the object of the invention is to reduce the high need for noble metal in the coating of molybdenum, while maintaining the favorable contact resistance, the good adhesive strength and the known other advantages of the noble metals, but also the above-mentioned disadvantages of other materials and processes, such as lack Avoid etch resistance, more effort in preparing the base material, mechanical sensitivity, fluctuating contact resistance or inefficiency.
  • this object is achieved according to the invention in that the noble metal in a layer thickness of 0.02 ... 1.0 ⁇ m, preferably 0.1 wm, via an intermediate layer of chromium with a layer thickness of 0.5 ... 10.0 ⁇ m, preferably 1.5 ⁇ m, is applied to the molybdenum.
  • the layer sequence has excellent etching resistance despite the lower proportion of noble metal compared to the known etching solution mixtures of nitric acid, hydrofluoric acid, acetic acid and optionally phosphoric acid and shows surprisingly good and uniform contact resistances.
  • Another advantage of the chrome-gold layer sequence compared to pure precious metal coatings, for example gold coatings, is achieved by their better wear resistance.
  • the use of the layer sequence according to the invention is extremely economical and suitable for precious metals such as gold, silver, platinum, palladium, rhodium, ruthenium.
  • the excellent properties of the layer sequence according to the invention are based on a diffusion of the noble metal into the chromium surface, which is thereby stabilized against undesired oxidation processes.
  • the contact resistance is also reduced accordingly.
  • step c) It has proven advantageous to carry out process step c) in a solution of 1 part by volume of concentrated sulfuric acid, 1 part by volume of concentrated nitric acid and 3 parts by volume of concentrated phosphoric acid at room temperature for a period of 15 and the step g) at a current density of about 20 A / allow dm 2 to run at room temperature for a period of 30 s.
  • the applied coatings at a temperature of 500 ... 1 100 ° C, preferably for gold, platinum, palladium, rhodium and ruthenium at a temperature of about 750 ° C, preferably for silver at a temperature of about 950 ° C to anneal for a period of 10 min.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Mechanical Engineering (AREA)
  • Electroplating Methods And Accessories (AREA)
  • Other Surface Treatments For Metallic Materials (AREA)
  • Electrodes Of Semiconductors (AREA)
  • Electroplating And Plating Baths Therefor (AREA)

Claims (15)

1. Molybdène enduit de métal précieux, caractérisé en ce que le métal précieux est appliqué en couche de 0,02 1,0 µm, de préférence de 0,1 µm d'épaisseur, sur une couche intermédiaire de chrome de 0,5 à 10,0 µm, de préférence de 1,5 µm d'épaisseur, appliquée sur le molybdène.
2. Molybdène enduit de métal précieux selon la revendication 1, caractérisé en ce que le métal précieux utilisé est l'or, l'argent, le platine, le palladium, le rhodium ou le ruthénium.
3. Procédé pour le recouvrement de molybdène par une série de couches selon l'une des revendications 1 ou 2, caractérisé par la succession des opérations suivantes :
a) Dégraissage préalable de molybdène dans un solvant organique
b) rinçage à l'eau
c) attaque chimique pour le nettoyage du molybdène
d) rinçage à l'eau
e) nouvelle attaque chimique pour le nettoyage du molybdène selon c)
f) rinçage à l'eau
g) traitement dans un bain de dégraissage alcalin
h) rinçage à l'eau
i) activation de la surface du molybdène
j) application du chrome par galvanisation
k) rinçage à l'eau
I) activation cathodique de la couche de chrome
m) rinçage à l'eau
n) application du métal précieux par galvanisation
o) rinçage à l'eau
p) recuit des couches appliquées sous atmosphère protectrice d'hydrogène.
4. Procédé selon la revendication 3, caractérisé en ce que, pour l'opération c), l'attaque chimique est effectuée, au moyen d'une solution composée d'un volume d'acide sulfurique concentré, d'un volume d'acide nitrique concentré et de trois volumes d'acide sulfurique concentré, à la température ambiante pendant une durée de 15 sec.
5. Procédé selon la revendication 3, caractérisé en ce que, pour l'opération g), le traitement s'effectue avec une densité de courant de l'ordre de 20 A/dm2 à la température ambiante pendant une durée de 30 sec.
6. Procédé selon la revendication 3, caractérisé en ce que, pour l'opération i), la surface de molybdène est activée dans de l'acide chlorhydrique concentré à la température ambiante pendant une durée de 15 sec. environ.
7. Procédé selon la revendication 3, caractérisé en ce, pour l'opération j), le molybdène est recouvert de chrome dans un bain composé de 400 g de Cr203 et de 4 g de H2SO4 par litre, avec une densité de courant de 15 A/dm2 à une température de 50 ± 5 °C pendant une durée de 8 min.
8. Procédé selon la revendication 3, caractérisé en ce que, pour l'opération I), la couche de chrome est soumise à une activation cathodique dans de l'acide sulfurique de 1 à 15 %, de préférence à 8 %, avec une densité de courant de 2 à 40 A/dm2, de préférence de 20 A/dm2 à la température ambiante pendant une durée de 2 à 60 sec., de préférence de 20 sec.
9. Procédé selon la revendication 3, caractérisé en ce que, pour l'opération n), la couche de chrome est recouverte d'or dans un bain d'or usuel d'acidité allant de faiblement acide à neutre avec une densité de courant de l'ordre de 3 Aldm2 à une température de 50 ± 5 °C pendant une durée de 10 sec.
10. Procédé selon la revendication 3, caractérisé en ce que, pour l'opération n), la couche de chrome est recouverte d'argent dans un bain d'argent, préalable au cyanure avec une densité de courant de l'ordre de 2 A/dm2 à une température de 20 ± 3 °C pendant une durée de 20 sec.
11. Procédé selon la revendication 3, caractérisé en ce que, pour l'opération n), la couche de chrome est recouverte de platine dans un bain acide avec une densité de courant de l'ordre de 3 Aldm2 à une température de 50 ± 5 °C pendant une durée de 15 sec.
12. Procédé selon la revendication 3, caractérisé en ce que, pour l'opération n), la couche de chrome est recouverte de palladium dans un bain neutre avec une densité de courant de l'ordre de 3 Aldm2 à une température de 45 ± 5 °C pendant une durée de 15 sec.
13. Procédé selon la revendication 3, caractérisé en ce que, pour l'opération n), la couche de chrome est recouverte de rhodium dans un bain acide avec une densité de courant de l'ordre de 3 Aldm2 à une température de 50 ± 5 °C pendant une durée de 25 sec.
14. Procédé selon la revendication 3, caractérisé en ce que, pour l'opération n), la couche de chrome est recouverte de ruthénium dans un bain acide avec une densité de courant de l'ordre de 3 Aldm2 à une température de 70 ± 5 °C pendant une durée de 20 sec.
15. Procédé selon la revendication 3, caractérisé en ce que, pour l'opération p), les couches appliquées sont soumises pendant une durée de 10 min, à un recuit effectué de préférence à une température de 500 à 1 100 °C, de préférence de 750 °C pour l'or, le platine, le palladium, le rhodium et le ruthénium et à une température de 950 °C de préférence pour l'argent.
EP81108457A 1980-10-21 1981-10-17 Molybdène enduit de métal précieux et son procédé de fabrication Expired EP0050343B1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE3039658 1980-10-21
DE19803039658 DE3039658A1 (de) 1980-10-21 1980-10-21 Mit edelmetall beschichtetes molybdaen und verfahren zu seiner herstellung

Publications (2)

Publication Number Publication Date
EP0050343A1 EP0050343A1 (fr) 1982-04-28
EP0050343B1 true EP0050343B1 (fr) 1984-01-18

Family

ID=6114850

Family Applications (1)

Application Number Title Priority Date Filing Date
EP81108457A Expired EP0050343B1 (fr) 1980-10-21 1981-10-17 Molybdène enduit de métal précieux et son procédé de fabrication

Country Status (4)

Country Link
US (1) US4464441A (fr)
EP (1) EP0050343B1 (fr)
JP (1) JPS5794594A (fr)
DE (1) DE3039658A1 (fr)

Families Citing this family (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE3214989A1 (de) * 1982-04-22 1983-11-10 Doduco KG Dr. Eugen Dürrwächter, 7530 Pforzheim Mit edelmetall oder einer edelmetallegierung beschichtetes elektrisches kontaktstueck
GB2130602B (en) * 1982-11-24 1986-04-16 Stc Plc Electroplating electrical contacts
GB2168381B (en) * 1984-12-12 1988-03-09 Stc Plc Gold plated electrical contacts
US5093280A (en) * 1987-10-13 1992-03-03 Northrop Corporation Refractory metal ohmic contacts and method
GB9107364D0 (en) * 1991-04-08 1991-05-22 Skw Metals Uk Ltd Coated molybdenum parts and process for their production
US5367195A (en) * 1993-01-08 1994-11-22 International Business Machines Corporation Structure and method for a superbarrier to prevent diffusion between a noble and a non-noble metal

Family Cites Families (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2697130A (en) * 1950-12-30 1954-12-14 Westinghouse Electric Corp Protection of metal against oxidation
US2928169A (en) * 1957-01-07 1960-03-15 John G Beach Electroplated articles having molybdenum base metal
US2886499A (en) * 1957-01-07 1959-05-12 Glenn R Schaer Protective metal coatings for molybdenum
GB959748A (en) * 1961-07-20 1964-06-03 Westinghouse Electric Corp Semiconductor device
DE1283970B (de) * 1966-03-19 1968-11-28 Siemens Ag Metallischer Kontakt an einem Halbleiterbauelement
FR2120037B1 (fr) * 1970-12-29 1977-08-05 Licentia Gmbh
JPS5525619B2 (fr) * 1974-02-13 1980-07-07
US4082622A (en) * 1977-04-20 1978-04-04 Gte Automatic Electric Laboratories Incorporated Electrodeposition of ruthenium
US4071417A (en) * 1977-06-29 1978-01-31 Bell Telephone Laboratories, Incorporated Process for decreasing the porosity of gold
US4212907A (en) * 1979-03-22 1980-07-15 The United States Of America As Represented By The United States Department Of Energy Pre-treatment for molybdenum or molybdenum-rich alloy articles to be plated

Also Published As

Publication number Publication date
DE3039658A1 (de) 1982-05-06
DE3039658C2 (fr) 1988-07-14
EP0050343A1 (fr) 1982-04-28
US4464441A (en) 1984-08-07
JPH0365438B2 (fr) 1991-10-11
JPS5794594A (en) 1982-06-12

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