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US4517253A Expired / Lapsed US ⏱️ 0.0 years remaining

Cryoelectrodeposition

Assignee: Individual
•
Filing: 1984-01-23
•
Granted: 1985-05-14
•
Expires: 2004-01-23
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Abstract

Abstract A process for electrodeposition of a material on a substrate that includes the steps of establishing a liquid halogenous electrolyte containing the material to be plated on the substrate and a solute, said electrolyte having an appropriate electrical conductance in a cryogenic environment; and establishing an electric field within the electrolyte to effect migration of ions of said material to the substrate where they deposit.

Inventors

  • 👤 Robert M. Rose
  • 👤 Donald R. Sadoway

Bibliographic Details

Application Number —
Jurisdiction US
Data Source google_patents
Last Synchronized 2026-10-28 17:39
CPC Classifications
C; C25; C25D; C25D3/00; C25D3/66; C25D3/665; C25D21/00; C25D21/02; C25D5/00; C25D5/003; C25D5/007; C25D5/60; C25D5/605; Y; Y10; Y10T; Y10T428/00; Y10T428/12; Y10T428/12493; Y10T428/12528; Y10T428/12639; Y10T428/12646; Y10T428/12653; Y10T428/12674; Y10T428/12681; Y10T428/12708; Y10T428/12736; Y10T428/1275; Y10T428/12757; Y10T428/12771; Y10T428/12861; Y10T428/12951; Y10T428/12972

Claims Analysis

Total Claims: 55
Claim 1
Independent Claim 96 words
A method of electrodeposition of a reactive metal, an elemental semiconductor, a noble or precious metal and compounds and alloys thereof onto a subtrate, that comprises: establishing an anhydrous ion solution of the material to be deposited in a liquid electrolyte consisting of a mixture taken from the group consisting of liquid halides and halogens having an appropriate electrical conductance and said material; immersing electrodes in the ion solution; and establishing an electrical potential between the electrodes to attract material ions in the solution to one of the electrodes which serves as a substrate for deposition.
Claim 2
Independent Claim 96 words
A method of electrodeposition of a reactive metal, an elemental semiconductor, a noble or precious metal and compounds and alloys thereof onto a subtrate, that comprises: establishing an anhydrous ion solution of the material to be deposited in a liquid electrolyte consisting of a mixture taken from the group consisting of liquid halides and halogens having an appropriate electrical conductance and said material; immersing electrodes in the ion solution; and establishing an electrical potential between the electrodes to attract material ions in the solution to one of the electrodes which serves as a substrate for deposition.
Claim 3
Dependent Claim 47 words
A method of electrodeposition according to claim 1 in which the liquid electrolyte is the liquid halide anhydrous hydrogen chloride to which is added tetramethyl ammonium and potassium chlorides to enhance the electrical conductivity of the solution and a soluble salt of the material to be electrodeposited.
Claim 4
Dependent Claim 31 words
A method according to claim 2 in which the material to be deposited is the reactive metal Nb and the salt of the material to be electrodeposted is KNbCl 6 .
Claim 5
Dependent Claim 27 words
A method according to claim 2 in which the solution is maintained at a temperature in the range between about 150 degrees K and 200 degrees K.
Claim 6
Dependent Claim 24 words
A method according to claim 2 in which said electric potential is maintained with respect to a reference electrode immersed in the ion solution.
Claim 7
Dependent Claim 16 words
A method according to claim 2 in which material is electrodeposited under conditions of controlled current.
Claim 8
Dependent Claim 22 words
A method according to claim 2 in which the substrate is taken from the group consisting of tantalum, copper, nickel and platinum.
Claim 9
Dependent Claim 34 words
A method according to claim 2 in which the material to be electrodeposited is the reactive metal Zr and the soluble salt of the material to be electrodeposited is K 2 ZrCl 6 .
Claim 10
Dependent Claim 34 words
A method according to claim 2 in which the material to be electrodeposited is the elemental semiconductor Si and the soluble salt of the material to be electrodeposited is K 2 SiCl 6 .
Claim 11
Dependent Claim 18 words
A method of electrodeposition according to claim 1 in which the electrolyte is the liquid interhalogen chlorine monofluoride.
Claim 12
Dependent Claim 19 words
A method according to claim 10 in which the substrate is the same material as the material electrodeposited thereon.
Claim 13
Dependent Claim 18 words
A method of electrodeposition according to claim 1 in which the electrolyte is the liquid halide boron trifluoride.
Claim 14
Dependent Claim 36 words
A method of electrodeposition according to claim 1 in which the reactive material to be electrodeposited is a metal taken from the group consisting of Ti, Zr, Hf, V, Nb, Ta, Cr, Re, Mo and W.
Claim 15
Dependent Claim 21 words
A method of electrodeposition according to claim 13 in which a plurality of reactive metals is simultaneously deposited onto the substrate.
Claim 16
Dependent Claim 28 words
A method of electrodeposition according to claim 13 in which the substrate consists of the same metal or metals as the reactive metal or metals respectively deposited thereon.
Claim 17
Dependent Claim 32 words
A method of electrodeposition according to claim 1 in which the material to be electrodeposited is an elemental semiconductor taken from the group Si, Ge, B, P, Ga, As and gray Sn.
Claim 18
Dependent Claim 32 words
A method of electrodeposition according to claim 16 in which a plurality of elemental semiconductors, with or without their principal dopants, B, P, Ga, As, Ae, is simultaneously electrodeposited onto the substrate.
Claim 19
Dependent Claim 26 words
A method of electrodeposition according to claim 1 in which the substrate is composed of graphite, vitreous carbon or any other electrically conductive form of carbon.
Claim 20
Dependent Claim 34 words
A method of electrodeposition according to claim 1 in which the material to be electrodeposited is a noble or precious metal taken from the group consisting of ruthenium, osmium, rhodium, iridium, palladium, and platinum.
Claim 21
Dependent Claim 23 words
A method of electrodeposition according to claim 19 in which the material to be deposited includes a plurality of the elements therein listed.
Claim 22
Dependent Claim 58 words
A method of electrodeposition according to claim 1 wherein the material to be electrodeposited is the reactive metal niobium, the cathode substrate is niobium, the electrolyte is liquid chlorine monofluoride containing niobium halide and other halide salts, the anode is niobium, and the solution is maintained at a temperature between about 110 degrees K. and 180 degrees K.
Claim 23
Dependent Claim 43 words
A method of electrodeposition according to claim 1 in which the material to be electrodeposited is taken from the group of reactive metals consisting of molybdenum (MO), tungsten (W) and titanium (Ti) and in which the liquid electrolyte is liquid chlorine monofluoride (ClF).
Claim 24
Dependent Claim 26 words
A method according to claim 22 in which the temperature during electrodeposition is maintained in the range between about 110 degrees K. and 180 degrees K.
Claim 25
Dependent Claim 16 words
A method according to claim 1 in which the material to be electrodeposited is a silicide.
Claim 26
Dependent Claim 30 words
A method according to claim 24 in which the silicide is taken from the group consisting of MoSi 2 and WSi 2 to achieve a wear-resistant surface on the substrate.
Claim 27
Dependent Claim 81 words
A process for electrodeposition of a material on a substrate that comprises: establishing an electrolyte taken from the group consisting of anhydrous liquid halogens and anhydrous liquid halides and having an appropriate electrical conductance in a cryogenic environment; immersing the substrate in the liquid halogen electrolyte, said electrolyte including ions of the material to be deposited and a solute; and establishing an electric field within the electrolyte to effect migration of ions of said material to the substrate where they deposit.
Claim 28
Dependent Claim 81 words
A process for electrodeposition of a material on a substrate that comprises: establishing an electrolyte taken from the group consisting of anhydrous liquid halogens and anhydrous liquid halides and having an appropriate electrical conductance in a cryogenic environment; immersing the substrate in the liquid halogen electrolyte, said electrolyte including ions of the material to be deposited and a solute; and establishing an electric field within the electrolyte to effect migration of ions of said material to the substrate where they deposit.
Claim 29
Dependent Claim 14 words
A process according to claim 26 in which the electrolyte is a liquid interhalogen.
Claim 30
Dependent Claim 14 words
A process according to claim 27 in which the material is a reactive metal.
Claim 31
Dependent Claim 14 words
A process according to claim 26 in which the material is an elemental semiconductor.
Claim 32
Dependent Claim 17 words
A process according to claim 26 in which the electrolyte is a mixture of halogen and interhalogen.
Claim 33
Dependent Claim 36 words
A process according to claim 26 in which the electrolyte is a halogenous compound, a hydrogen halide, or a halide of a group VB element, or a halide of a group IIIB element, or an interhalogen.
Claim 34
Dependent Claim 28 words
A process according to claim 26 in which the temperature is held between 50 degrees K. and 500 degrees K., the precise temperature depending on the elecrolyte used.
Claim 35
Dependent Claim 21 words
A process according to claim 26 in which the electrolyte is a mixture such as HCl and BF 3 and HF.
Claim 36
Dependent Claim 11 words
A product produced in accordance with the process of claim 26.
Claim 37
Dependent Claim 36 words
A product that comprises: a layer of a reactive material electrolytically deposited from an anhydrous inorganic ion solution on a substrate that is totally free of thermal damage due to the depositing of the material thereon.
Claim 38
Dependent Claim 36 words
A product that comprises: a layer of a reactive material electrolytically deposited from an anhydrous inorganic ion solution on a substrate that is totally free of thermal damage due to the depositing of the material thereon.
Claim 39
Dependent Claim 68 words
A product according to claim 35 wherein the electrolytically deposited reactive material is a metal taken from the group of reactive metals consisting of Ti, Zr, Hf, V, Nb, Cr, Mo, Ta, W and Re or from the group of elemental semiconductors consisting of Si and gray Sn, or from the group of noble or precious metals consisting of Ru, Os, Rh, Ir, Pd, Pt, Ag and Au.
Claim 40
Dependent Claim 12 words
A product according to claim 36 in which the substrate is steel.
Claim 41
Dependent Claim 21 words
A product according to claim 35 in which the layer of material is electrodeposited onto the substrate at below room temperature.
Claim 42
Dependent Claim 21 words
A product according to claim 35 wherein the reactive material is taken from groups IVA through VIA of the periodic table.
Claim 43
Dependent Claim 15 words
A product according to claim 39 wherein the layer is greater than about ten micrometers.
Claim 44
Dependent Claim 13 words
A product according to claim 35 wherein the material is an elemental semiconductor.
Claim 45
Dependent Claim 12 words
A product according to claim 35 wherein the material is a silicide.
Claim 46
Dependent Claim 27 words
A process according to claim 31 wherein the halide of the group VB element is taken from the group consisting of PF 3 and SbF 3 .
Claim 47
Dependent Claim 21 words
A process according to claim 33 wherein said mixture is taken from the group consisting of HCl, BF 3 and HF.
Claim 48
Dependent Claim 11 words
A product produced in accordance with the process of claim 1.
Claim 49
Dependent Claim 20 words
A process according to claim 31 wherein the hydrogen halide is taken from the group consisting of HF and HCl.
Claim 50
Dependent Claim 20 words
A process according to claim 31 wherein the interhalogen is taken from the group consisting of BrF 3 and ClF.
Claim 51
Independent Claim 120 words
A method of electrodeposition of a material onto a substrate, that comprises: establishing an anhydrous ion solution of the material in a liquid electrolyte consisting of a mixture taken from the group consisting of liquid halides and halogens having an appropriate electrical conductance and said material, said material being taken from the group consisting of Zr, Si, Ti, Hf, V, Nb, Ta, Cr, Mo, W, GeB, Re, gray Sn, P, Ga, As, Al, osmium, rhodium, iridium, palladium, platinum, silver, gold and their silicide compounds; immersing electrodes in the ion solution; and establishing an electrical potential between the electrodes to attract material ions of said material in the solution to one of the electrodes which serves as a substrate for deposition.
Claim 52
Independent Claim 120 words
A method of electrodeposition of a material onto a substrate, that comprises: establishing an anhydrous ion solution of the material in a liquid electrolyte consisting of a mixture taken from the group consisting of liquid halides and halogens having an appropriate electrical conductance and said material, said material being taken from the group consisting of Zr, Si, Ti, Hf, V, Nb, Ta, Cr, Mo, W, GeB, Re, gray Sn, P, Ga, As, Al, osmium, rhodium, iridium, palladium, platinum, silver, gold and their silicide compounds; immersing electrodes in the ion solution; and establishing an electrical potential between the electrodes to attract material ions of said material in the solution to one of the electrodes which serves as a substrate for deposition.
Claim 53
Dependent Claim 20 words
A method of electrodeposition according to claim 48 in which ion solution is maintained at cryogenic temperature during said electrodeposition.
Claim 54
Dependent Claim 18 words
A process according to claim 31 wherein the halide of the group IIIB element is BF 3 .
Claim 55
Dependent Claim 16 words
A process according to claim 27 in which the material is a noble or precious metal.

References Cited (Backward Citations)

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DE237014C Cited
GB189517190A Cited
GB320818A Cited
US3778360A Cited
US3990953A Cited
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US4227291A Cited
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USPTO Annuity & Maintenance Windows

Annuity Stage Window Opens Payment Deadline Surcharge Period Until Estimated Fee Status
3.5 Years (Year 4) 1988-05-13 1988-11-12 1989-05-14 $2000.00 Window Closed / Lapsed
7.5 Years (Year 8) 1992-05-13 1992-11-12 1993-05-14 $3760.00 Window Closed / Lapsed
11.5 Years (Year 12) 1996-05-13 1996-11-12 1997-05-14 $7700.00 Window Closed / Lapsed

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