US3835007A - Process for bonding copper or iron to titanium or tantalum - Google Patents

Process for bonding copper or iron to titanium or tantalum Download PDF

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Publication number
US3835007A
US3835007A US00314858A US31485872A US3835007A US 3835007 A US3835007 A US 3835007A US 00314858 A US00314858 A US 00314858A US 31485872 A US31485872 A US 31485872A US 3835007 A US3835007 A US 3835007A
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United States
Prior art keywords
copper
titanium
iron
metal
tantalum
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Expired - Lifetime
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US00314858A
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English (en)
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A Ferat
R Masotti
H Chavanel
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Rhone Progil SA
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Rhone Progil SA
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    • 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
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
    • C23C28/02—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D only coatings only including layers of metallic material
    • C23C28/023—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D only coatings only including layers of metallic material only coatings of metal elements only
    • 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
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/02—Pretreatment of the material to be coated
    • C23C14/021—Cleaning or etching treatments

Definitions

  • the present invention relates to a new process of bond ing copper or iron to titanium or tantalum and to the new industirial products resulting from it.
  • Bonding of these metals has been known for many years and has employed such processes as rolling, plating, hammering, co-drawing, classical or ultra-sonic soldering. Those techniques are intended to permit one to bring together as closely as possible sheets or plates of titanium or tantalum and of another metal. This prior art bonding has also been achieved by electro-deposition of a metal on a sheet or plate of titanium 'or tantalum.
  • the present invention contemplates, by using the process according to invention, to provide an important solution of the problem of bonding titanium or tantalum to copper or iron.
  • an object of the invention to provide a superior bonding of copper or iron to titanium or tantalum.
  • FIG. 1 is a plan view of bonded sheets of copper (Cu) and titanium (Ti) in accordance with the invention, which are employed to conduct a conductivity test, to be described hereinbelow, showing one of the important advantages of the bonded products of the invention.
  • FIG. 2 is an elevation of the bonded sheets of FIG. 1.
  • the present invention comprises first depositing on titanium or tantalum, in accordance with certain conditions, a thin adhering layer of the contemplated metal, copper or iron, the layer having a very strong adherence or bond with the support metal, titanium or tantalum, then of increasing this adhering layer by adding additional copper or iron by any known means.
  • the present process consists of in a first stage, depositing a thin adhering layer of copper or iron on the support metal, then in a second stage, adding by any known way additional amounts of deposited metal layer.
  • This process is characterized in that the supporting metal (titanium or tantalum) is first subjected to a mechanical and/or chemical cleaning treatment, then to an ionic bombardment in a residual atmosphere of rare gas and receives afterwards a copper or iron deposit by cathodic sputtering of one of these metals in a residual atmosphere of rare gas at a temperature of less than 500 C., the resulting adhering layer of copper or iron being subsequently supplemented in any known way.
  • cathodic sputtering are characterized by depositing a metal by electrical discharge in a low pressure of inert gas.
  • the apparatus for cathodic sputtering consists of a vacuum enclosure, a pumping system, a high voltage electrical feed and an inert gas introduction system.
  • the supporting metal titanium or tantalum
  • the supporting metal before being introduced in the vacuum enclosure is subjected to a thermal and/or chemical treatment of sanding and/0r degreasing.
  • This supporting metal and the metal to be pulverized are put in electrode position in enclosure containing a rare gas residual atmosphere (such as argon).
  • a rare gas residual atmosphere such as argon
  • the supporting metal In the first stage of ionic bombardment the supporting metal is positioned cat'hodically in applying negative high voltage. It becomes the cathode for some time and a small portion of the surface is pulverized.
  • the other metal to be bonded is protected during this operation, by means of a moving mask, against becoming contaminated with particles eminating from the support metal.
  • This ionic bombardment of the support has for its purpose to degas and scour the surface which is to receive the deposit of other metal, by removing oxide layers, traces of hydrocarbons, fats, etc. As a result, the surface of the support metal is converted as closely as possible to the pure metallic state.
  • the supporting metal is next disconnected from the high voltage source and placedin the anode position ready to receive the deposit resulting from sputtering of the metal to be bonded (copper or iron), which is placed in the cathode position.
  • the copper or iron metal is cleared of its mask and then connected to the high voltage source. Cathode sputtering on the anode is then conducted in a residual atmosphere of pure rare gas, such as argon, radon, etc.
  • the process of the invention provides a very strongly bonded layer or coating of copper or iron on titanium or tantalum. Finally, after supplementing the bonded layer of copper or iron by conventional means, there is obtained a product which has mechanical and electrical characteristics high- 1y desirable for the contemplated applications.
  • Example I A square titanium plate of 100 mm. on each side and 8/ mm. thick was scoured by subjecting it to a fluonitric attack by immersion for 2 minutes in a mixture of nitric and hydrofluoric acids, washed with water, then with acetone and finally dried.
  • the thickness of the thin copper coating is increased by electro-deposition of an additional copper layer of 1 mm.
  • the work iece was introduced as the cathode into an acid electrolysis bath of copper sulfate containing 250 grams per liter of cupric sulfate pentahydrate, 75 grams per liter of sulfuric acid (having a specific gravity of 1.66) in distilled Water.
  • the electrolysis bath was stirred while at room temperature.
  • the anode was of copper.
  • the density of the electrolysis current was 3 amperes per square decimeter.
  • Example 2 Example 1 was repeated but the titanium plate was treated by sanding with Fontainebleau sand (40-80 microns) before the fluonitric attack.
  • Example 3 Example 1 was repeated, except that the copper deposition was made on a titanium plate freshly scoured and cooled for 30 minutes, at a greater speed, namely, 600 angstroms per minute.
  • Example 4 Example 1 was repeated, except that the titanium sheet was treated by sanding before the fiuonitric attack and the copper deposition was made on titanium while at room temperature at a speed of 600 angstroms per minute.
  • Example 5 Example 1 was repeated, except that the titanium plate was not subjected to any fluonitric attack.
  • Example 6 Example 1 was repeated, except that the titanium plate was not subjected to fluoronitric attack, but instead to a sanding with corundum having a granule size of about 250 microns.
  • Example 1 was repeated, but copper was replaced by iron in producing the iron bonding on the titanium sheet and the iron coating was then coated with a copper deposit by electro-deposition under the following conditions.
  • the workpiece was introduced as the cathode in an electrolysis bath containing 100 grams per liter of cupric sulfate pentahydrate, cc. per liter of diethylenetriamine and 10 cc. per liter of ammonium sulfate, all in distilled water.
  • the deposition was conducted maintaining the bath at a temperature of about 60 C. with the electrolysis current density being about 4 amperes per square decimeter.
  • the anode was of copper.
  • Example 1 was repeated, except that the titanium plate was replaced by one of tantalum of the same dimensions.
  • Example 7 was repeated, except that the titanium plate was replaced by one of tantalum of the same dimensions.
  • the sample geometry was that shown in accordance with the appended drawings.
  • the difference in potential was measured at various points; 3 measures were made between points situated on titanium and copper, on copper alone, and on titanium alone.
  • the following results were obtained, with a titanium thickness of 8/ 10 millimeter and a copper thickness of ll/ 10 millimeters:
  • a process of bonding a substrate metal selected from the class consisting of titanium and tantalum with a coating metal selected from the class consisting of iron and copper comprising, in a first stage, depositing a thin bond ing layer of coating metal on said substrate metal, and, in a second stage, of thickening the deposited layer in any known method with additional metal, characterized in that said substrate metal is first subjected to a preliminary cleaning treatment, then to an ionic bombardment in a residual atmosphere of rare gas and afterwards a bonded layer of said coating metal is deposited by cathodic sputtering on said substrate metal in residual atmosphere of rare gas at a temperature lower than 500 C, said bonded layer of said coating metal being thickened by addition of more metal.

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Physical Vapour Deposition (AREA)
  • Electrolytic Production Of Metals (AREA)
  • Laminated Bodies (AREA)
  • Fixed Capacitors And Capacitor Manufacturing Machines (AREA)
US00314858A 1971-12-24 1972-12-13 Process for bonding copper or iron to titanium or tantalum Expired - Lifetime US3835007A (en)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
FR7147874A FR2164546B1 (OSRAM) 1971-12-24 1971-12-24

Publications (1)

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US3835007A true US3835007A (en) 1974-09-10

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US00314858A Expired - Lifetime US3835007A (en) 1971-12-24 1972-12-13 Process for bonding copper or iron to titanium or tantalum

Country Status (14)

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US (1) US3835007A (OSRAM)
JP (1) JPS521697B2 (OSRAM)
AT (1) AT318344B (OSRAM)
BE (1) BE793268A (OSRAM)
BR (1) BR7209084D0 (OSRAM)
CA (1) CA991586A (OSRAM)
CH (1) CH567105A5 (OSRAM)
DE (1) DE2263013A1 (OSRAM)
ES (1) ES409995A1 (OSRAM)
FR (1) FR2164546B1 (OSRAM)
GB (1) GB1379830A (OSRAM)
IT (1) IT973575B (OSRAM)
NL (1) NL7215746A (OSRAM)
SE (1) SE374764B (OSRAM)

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3930975A (en) * 1973-10-27 1976-01-06 Robert Bosch G.M.B.H. Sputtering method for producing solder-fast copper layers
US3986944A (en) * 1975-06-27 1976-10-19 Honeywell Information Systems, Inc. Method for obtaining adhesion of multilayer thin films
US4328080A (en) * 1980-10-24 1982-05-04 General Electric Company Method of making a catalytic electrode
US4964962A (en) * 1988-10-08 1990-10-23 Matsushita Electric Works, Ltd. Method for forming conducting metal layer on inorganic substrate
US20050045469A1 (en) * 2003-08-29 2005-03-03 Northrop Grumman Corporation Titanium foil metallization product and process
EP1775752A3 (de) * 2005-10-15 2007-06-13 Burth, Dirk, Dr. Herstellung eines Elektronenaustrittsfensters mittels eines Ätzprozesses
US20110266504A1 (en) * 2007-08-06 2011-11-03 Katholieke Universiteit Leuven Deposition from ionic liquids

Families Citing this family (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4281235A (en) * 1979-10-09 1981-07-28 Tri Delta Industries, Inc. Method for welding ferrous alloys to aluminum and aluminum alloys or refractory metals
JPH03115560A (ja) * 1989-09-28 1991-05-16 Daido Metal Co Ltd すべり軸受の製造方法
US7968829B2 (en) * 2006-12-28 2011-06-28 United Technologies Corporation Electrical connection for titanium metal heater in jet turbine applications

Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3930975A (en) * 1973-10-27 1976-01-06 Robert Bosch G.M.B.H. Sputtering method for producing solder-fast copper layers
US3986944A (en) * 1975-06-27 1976-10-19 Honeywell Information Systems, Inc. Method for obtaining adhesion of multilayer thin films
US4328080A (en) * 1980-10-24 1982-05-04 General Electric Company Method of making a catalytic electrode
US4964962A (en) * 1988-10-08 1990-10-23 Matsushita Electric Works, Ltd. Method for forming conducting metal layer on inorganic substrate
US20050045469A1 (en) * 2003-08-29 2005-03-03 Northrop Grumman Corporation Titanium foil metallization product and process
WO2005021826A3 (en) * 2003-08-29 2005-12-01 Northrop Grumman Corp Titanium foil metallization product and process
EP1775752A3 (de) * 2005-10-15 2007-06-13 Burth, Dirk, Dr. Herstellung eines Elektronenaustrittsfensters mittels eines Ätzprozesses
US20090160309A1 (en) * 2005-10-15 2009-06-25 Dirk Burth Electron beam exit window
US20110266504A1 (en) * 2007-08-06 2011-11-03 Katholieke Universiteit Leuven Deposition from ionic liquids

Also Published As

Publication number Publication date
SE374764B (OSRAM) 1975-03-17
JPS521697B2 (OSRAM) 1977-01-17
CA991586A (fr) 1976-06-22
BR7209084D0 (pt) 1973-09-25
FR2164546A1 (OSRAM) 1973-08-03
DE2263013A1 (de) 1973-06-28
FR2164546B1 (OSRAM) 1974-06-07
JPS4872044A (OSRAM) 1973-09-28
IT973575B (it) 1974-06-10
AT318344B (de) 1974-10-10
CH567105A5 (OSRAM) 1975-09-30
ES409995A1 (es) 1975-12-01
NL7215746A (OSRAM) 1973-06-26
BE793268A (fr) 1973-06-22
GB1379830A (en) 1975-01-08

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