US4065600A
Expired / Lapsed
US
⏱️ 0.0 years remaining
Metal oxide films
Assignee: Pilkington Automotive Ltd
•
Filing: 1971-05-18
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Granted: 1977-12-27
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Expires: 1991-05-18
Abstract
Abstract In a method of depositing a transparent electrically conductive metal oxide coating by reactive sputtering onto the surface of a substrate, the substrate is supported, in spaced relationship with a cathode which is to be sputtered, in a vacuum chamber containing an atmosphere comprising an inert gas and a controlled oxygen concentration at a selected total pressure. The substrate is heated prior to sputtering to a selected elevated temperature, and reactive sputtering is caused by applying a selected negative potential relative to the substrate. The oxygen in the atmosphere is provided and maintained at a selected concentration, and the heating of said substrate is controlled during sputtering to maintain the substrate temperature substantially constant at the selected temperature during substrate heating caused by sputtering. The selected values of the oxygen concentration substrate temperature, vacuum chamber pressure, and cathode potential are so chosen that the deposited coating is haze-free, and its specific electrical resistivity lies at or close to the minimum of the curve which is obtained by plotting specific electrical resistivity against oxygen concentration while maintaining the substrate temperature, vacuum chamber pressure and cathode potential all constant at the selected values. Glass articles with stable, transparent and haze-free coatings having acceptable resistance are produced by the method.
Inventors
- 👤 Robert David King
- 👤 Robert Hiscutt
- 👤 Peter Molineux
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-10-23 15:05
CPC Classifications
C; C23; C23C; C23C14/00; C23C14/0021; C23C14/0036; H; H01; H01B; H01B1/00
Claims Analysis
Total Claims: 44
Claim 1
Independent Claim
197 words
A method of depositing a transparent electrically conductive metal oxide coating by reactive sputtering onto the surface of a substrate, wherein: the substrate is supported, in spaced relationship with a cathode which is to be sputtered, in a vacuum chamber containing an atmosphere comprising an inert gas and a controlled oxygen concentration at a selected reduced total pressure, the substrate is heated prior to sputtering to a selected elevated temperature, and reactive sputtering is caused by applying a selected negative potential to the cathode relative to the substrate, the oxygen in the atmosphere being provided and maintained at a selected concentration, and the heating of said substrate being controlled during sputtering to maintain said substrate temperature substantially constant at said selected temperature during heating of said substrate caused by sputtering, the selected values of the oxygen concentration, substrate temperature, vacuum chamber pressure, and cathode potential being so chosen that the deposited coating is haze-free, and its specific electrical resistivity lies at or close to the minimum of the curve which is obtained by plotting specific electrical resistivity against oxygen concentration while maintaining the substrate temperature, vacuum chamber pressure and cathode potential all constant at said selected values.
Claim 2
Independent Claim
197 words
A method of depositing a transparent electrically conductive metal oxide coating by reactive sputtering onto the surface of a substrate, wherein: the substrate is supported, in spaced relationship with a cathode which is to be sputtered, in a vacuum chamber containing an atmosphere comprising an inert gas and a controlled oxygen concentration at a selected reduced total pressure, the substrate is heated prior to sputtering to a selected elevated temperature, and reactive sputtering is caused by applying a selected negative potential to the cathode relative to the substrate, the oxygen in the atmosphere being provided and maintained at a selected concentration, and the heating of said substrate being controlled during sputtering to maintain said substrate temperature substantially constant at said selected temperature during heating of said substrate caused by sputtering, the selected values of the oxygen concentration, substrate temperature, vacuum chamber pressure, and cathode potential being so chosen that the deposited coating is haze-free, and its specific electrical resistivity lies at or close to the minimum of the curve which is obtained by plotting specific electrical resistivity against oxygen concentration while maintaining the substrate temperature, vacuum chamber pressure and cathode potential all constant at said selected values.
Claim 3
Dependent Claim
15 words
The method according to claim 1 wherein the substrate is a sheet of soda-lime-silica glass.
Claim 4
Dependent Claim
17 words
The method according to claim 2 wherein the glass is toughened before having said coating sputtered therein.
Claim 5
Dependent Claim
28 words
The method of claim 1 wherein the cathode is an alloy of a base metal having an atomic number of from 48 to 52 and another compatible metal.
Claim 6
Dependent Claim
42 words
The method of claim 1 wherein the cathode is an alloy of a base metal having an atomic number of from 48 to 52 and another compatible metal having a valency difference of 1 or 2 with respect to the base metal.
Claim 7
Dependent Claim
24 words
The method of claim 1 wherein the cathode is an indium/tin alloy comprising between 50 and 98% indium and between 2 and 50% tin.
Claim 8
Dependent Claim
24 words
The method of claim 1 wherein the cathode is an indium/tin alloy comprising between 80 and 90% indium and between 10 and 20% tin.
Claim 9
Dependent Claim
21 words
The method according to claim 1 wherein the cathode is formed from an alloy selected from indium/tin, indium/germanium, indium/phosphorus, and indium/tellurium.
Claim 10
Dependent Claim
24 words
The method of claim 1 wherein the potential difference between the cathode and the substrate is in the range of from -1kV to -5kV.
Claim 11
Dependent Claim
24 words
The method of claim 1 wherein the potential difference between the cathode and the substrate is in the range of from -2kV to -3.5kV.
Claim 12
Dependent Claim
22 words
The method of claim 1 wherein said selected temperature of said substrate is in the range of from 200° to 350° C.
Claim 13
Dependent Claim
22 words
The method of claim 1 wherein said selected temperature of said substrate is in the range of from 270° to 320° C.
Claim 14
Dependent Claim
34 words
The method of claim 1 wherein said selected value of oxygen concentration is in the range of from 1 to 9% by volume present within the space between the cathode and the substrate surface.
Claim 15
Dependent Claim
34 words
The method of claim 1 wherein said selected value of oxygen concentration is in the range of from 1 to 6% by volume present within the space between the cathode and the substrate surface.
Claim 16
Dependent Claim
40 words
The method of claim 1 wherein said selected value of oxygen concentration is in the range of from 1.6 to 1.9% by volume and said selected temperature of said substrate is in the range of from 280° and 300° C.
Claim 17
Dependent Claim
24 words
The method of claim 1 wherein said selected vacuum chamber pressure is in the range of from 10 microns Hg to 100 microns Hg.
Claim 18
Dependent Claim
20 words
The method of claim 1 wherein said selected vacuum chamber pressure is from 40 microns Hg to 90 microns Hg.
Claim 19
Dependent Claim
15 words
The method according to claim 1 wherein the substrate is a refractory os siliceous material.
Claim 20
Dependent Claim
16 words
The method according to claim 1 wherein the substrate is selected from porcelain, silica and mica.
Claim 21
Dependent Claim
32 words
An article with a transparent and haze-free, electrically conductive metal oxide coating having a specific electrical resistivity below 10 × 10 -4 ohm.cm. applied thereon by a process according to claim 1.
Claim 22
Dependent Claim
27 words
An article according to claim 20 wherein the coating has a specific electrical resistivity between 2.5 × 10 -4 ohm. cm. and 10 × 10 -4 ohm.cm.
Claim 23
Dependent Claim
33 words
An article with a transparent and haze-free, electrically conductive metal oxide coating having a specific electrical resistivity below 20 × 10 -4 ohm. cm. applied thereon by a process according to claim 1.
Claim 24
Dependent Claim
34 words
A glass article with a stable, transparent and haze-free, electrically conductive coating having a resistance in the range of from 2 ohm/sq. to 100 ohm/sq. applied thereon by a process according to claim 1.
Claim 25
Independent Claim
264 words
A method of depositing a transparent electrically conductive metal oxide coating onto the surface of a glass substrate by reactive sputtering, the process comprising the following steps: supporting the substrate in a chamber in spaced relationship with a cathode of an alloy which is to be sputtered, evacuating the chamber, heating the surface of the substrate to a selected temperature in the range of from 200° to 350° C before commencing sputtering, providing an atmosphere in the chamber comprising an inert gas and a controlled oxygen concentration and maintaining the pressure of the atmosphere in the chamber at a selected value of from 10 to 100 microns Hg, maintaining the oxygen in the space between the cathode and the substrate at a selected oxygen concentration within the range of 1 to 9% by volume, causing deposition of a metal oxide film on the substrate by reactive sputtering by applying a negative potential to the cathode selected such that the potential difference between cathode and substrate is in the range of from -1kV to -5kV, and controlling the heating of the surface of the substrate during sputtering to maintain the substrate temperature substantially constant at said selected temperature, the selected values of the oxygen concentration, substrate temperature, vacuum chamber pressure, and cathode potential being so chosen that the deposited coating is haze-free, and its specific electrical resistivity lies at or close to the minimum of the curve which is obtained by plotting specific electrical resistivity against oxygen concentration while maintaining the substrate temperature, vacuum chamber pressure and cathode potential all constant at said selected values.
Claim 26
Independent Claim
264 words
A method of depositing a transparent electrically conductive metal oxide coating onto the surface of a glass substrate by reactive sputtering, the process comprising the following steps: supporting the substrate in a chamber in spaced relationship with a cathode of an alloy which is to be sputtered, evacuating the chamber, heating the surface of the substrate to a selected temperature in the range of from 200° to 350° C before commencing sputtering, providing an atmosphere in the chamber comprising an inert gas and a controlled oxygen concentration and maintaining the pressure of the atmosphere in the chamber at a selected value of from 10 to 100 microns Hg, maintaining the oxygen in the space between the cathode and the substrate at a selected oxygen concentration within the range of 1 to 9% by volume, causing deposition of a metal oxide film on the substrate by reactive sputtering by applying a negative potential to the cathode selected such that the potential difference between cathode and substrate is in the range of from -1kV to -5kV, and controlling the heating of the surface of the substrate during sputtering to maintain the substrate temperature substantially constant at said selected temperature, the selected values of the oxygen concentration, substrate temperature, vacuum chamber pressure, and cathode potential being so chosen that the deposited coating is haze-free, and its specific electrical resistivity lies at or close to the minimum of the curve which is obtained by plotting specific electrical resistivity against oxygen concentration while maintaining the substrate temperature, vacuum chamber pressure and cathode potential all constant at said selected values.
Claim 27
Dependent Claim
15 words
The method according to claim 24 wherein the substrate is a sheet of soda-lime-silica glass.
Claim 28
Dependent Claim
17 words
The method according to claim 25 wherein the glass is toughened before having said coating sputtered therein.
Claim 29
Dependent Claim
28 words
The method of claim 24 wherein the cathode is an alloy of a base metal having an atomic number of from 48 to 52 and another compatible metal.
Claim 30
Dependent Claim
42 words
The method of claim 24 wherein the cathode is an alloy of a base metal having an atomic number of from 48 to 52 and another compatible metal having a valency difference of 1 or 2 with respect to the base metal.
Claim 31
Dependent Claim
24 words
The method of claim 24 wherein the cathode is an indium/tin alloy comprising between 50 and 98% indium and between 2 and 50% tin.
Claim 32
Dependent Claim
24 words
The method of claim 24 wherein the cathode is an indium/tin alloy comprising between 80 and 90% indium and between 10 and 20% tin.
Claim 33
Dependent Claim
21 words
The method according to claim 24 wherein the cathode is formed from an alloy selected from indium/tin, indium/germanium, indium/phosphorus, and indium/tellurium.
Claim 34
Dependent Claim
24 words
The method of claim 24 wherein the potential difference between the cathode and the substrate is in the range of from -2kV to -3.5kV.
Claim 35
Dependent Claim
22 words
The method of claim 24 wherein said selected temperature of said substrate is in the range of from 270° to 320° C.
Claim 36
Dependent Claim
34 words
The method of claim 24 wherein said selected value of oxygen concentration is in the range of from 1 to 6% by volume present within the space between the cathode and the substrate surface.
Claim 37
Dependent Claim
40 words
The method of claim 24 wherein said selected value of oxygen concentration is in the range of from 1.6 to 1.9% by volume and said selected temperature of said substrate is in the range of from 280° and 300° C.
Claim 38
Dependent Claim
20 words
The method of claim 24 wherein said selected vacuum chamber pressure is from 40 microns Hg to 90 microns Hg.
Claim 39
Dependent Claim
15 words
The method according to claim 24 wherein the substrate is a refractory or siliceous material.
Claim 40
Dependent Claim
16 words
The method according to claim 24 wherein the substrate is selected from porcelain, silica and mica.
Claim 41
Dependent Claim
34 words
A glass article with a transparent and haze-free, electrically conductive metal oxide coating having a specific electrical resistivity below 10 × 10 -4 ohm. cm. applied thereon by a process according to claim 24.
Claim 42
Dependent Claim
28 words
A glass article according to claim 39 wherein the coating has a specific electrical resistivity between 2.5 × 10 -4 ohm. cm. and 10 × 10 -4 ohm.cm.
Claim 43
Dependent Claim
34 words
A glass article with a transparent and haze-free, electrically conductive metal oxide coating having a specific electrical resistivity below 20 × 10 -4 ohm. cm. applied thereon by a process according to claim 24.
Claim 44
Dependent Claim
34 words
A glass article with a stable, transparent and haze-free, electrically conductive coating having a resistance in the range of from 2 ohm/sq. to 100 ohm/sq. applied thereon by a process according to claim 24.
References Cited (Backward Citations)
USPTO Annuity & Maintenance Windows
| Annuity Stage | Window Opens | Payment Deadline | Surcharge Period Until | Estimated Fee | Status |
|---|---|---|---|---|---|
| 3.5 Years (Year 4) | 1980-12-26 | 1981-06-27 | 1981-12-27 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1984-12-26 | 1985-06-27 | 1985-12-27 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1988-12-26 | 1989-06-27 | 1989-12-27 | $7700.00 | Window Closed / Lapsed |