US4085248A
Expired / Lapsed
US
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Method to apply a protective layer to the surface of optical reflectors, and so-made reflectors, particularly automotive vehicle head lamps
Assignee: Robert Bosch GmbH
•
Filing: 1976-08-20
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Granted: 1978-04-18
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Expires: 1996-08-20
Abstract
Abstract The reflectors, for example for automotive vehicle head lamps are reflectorized by evaporating aluminum thereon in a vacuum vessel at a vacuum of about 10 -7 bar; thereafter, and without removing the reflectors, a gaseous monomer is introduced raising the pressure to about 5 × 10 -6 bar to deposit a protective layer by polymerization from the gaseous phase. The monomer gases, preferably, are low molecular weight siloxanes having methyl-, vinyl- or phenyl groups, preferably hexamethyldisiloxane (HMDS), or methyl-, vinyl- or alkoxy silanes, preferably vinyltrimethylsilane (VTMS), polymerization being accelerated and ensured by an electrical discharge generated within the vessel by a heated electron emitter placed at a negative voltage with respect to the reflector blanks. After polymerization, the layer is rendered hydrophilic by treatment with oxygen at a pressure of about 10 -2 to 10 -3 m bar to form an organosilicon polymeric protective layer which is inherently hydrophobic and has a hydrophilic surface.
Inventors
- 👤 Ernst Zehender
- 👤 Bernhard Blaich
- 👤 Helmut Stein
- 👤 Karl Kerner
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-10-25 17:21
CPC Classifications
C; C23; C23C; C23C14/00; C23C14/22; C23C14/50; B; B05; B05D; B05D1/00; B05D1/62; B05D7/00; B05D7/24; B29; B29D; B29D11/00; B29D11/00865; C23C14/06; C23C14/12; C23C14/14; C23C14/58; C23C14/5846; C23C14/5853; F; F21; F21S; F21S41/00; F21S41/30; F21S41/37; F21V; F21V7/00; F21V7/22; F21V7/28; G; G02; G02B; G02B1/00; G02B1/10; G02B1/18; Y; Y10; Y10T; Y10T428/00; Y10T428/26; Y10T428/263; Y10T428/264; Y10T428/265; Y10T428/31504; Y10T428/31678; Y10T428/31692; Y10T428/31696
Claims Analysis
Total Claims: 56
Claim 1
Independent Claim
163 words
Method to apply a protective layer to the surface of optical reflectors in an evacuated vacuum vessel (10) comprising the steps of locating an electron emissive wire (16) in said vessel, locating a mass of reflecting metal in said vessel, locating reflector substrates (15) in said vessel, heating said mass of reflecting metal to the evaporation temperature of said reflecting metal to vaporize said metal and deposit a thin reflective layer of said metal on said reflector substrates, then exposing the metal coated reflector substrates to an organic monomeric gas, generating electrons by heating said electron emissive wire (16) to a temperature sufficiently high to emit electrons and biassing said wire (16) to a negative voltage with respect to said reflector substrates (15) thereby polymerizing the gas at the surface of the substrate to form a protective hydrophobic polymer layer from said monomer by polymerization from the gas phase by exposure to electrons generated by thermal emission from said heated electron emissive wire.
Claim 2
Dependent Claim
163 words
Method to apply a protective layer to the surface of optical reflectors in an evacuated vacuum vessel (10) comprising the steps of locating an electron emissive wire (16) in said vessel, locating a mass of reflecting metal in said vessel, locating reflector substrates (15) in said vessel, heating said mass of reflecting metal to the evaporation temperature of said reflecting metal to vaporize said metal and deposit a thin reflective layer of said metal on said reflector substrates, then exposing the metal coated reflector substrates to an organic monomeric gas, generating electrons by heating said electron emissive wire (16) to a temperature sufficiently high to emit electrons and biassing said wire (16) to a negative voltage with respect to said reflector substrates (15) thereby polymerizing the gas at the surface of the substrate to form a protective hydrophobic polymer layer from said monomer by polymerization from the gas phase by exposure to electrons generated by thermal emission from said heated electron emissive wire.
Claim 3
Dependent Claim
22 words
Method according to claim 1, wherein said monomeric gas comprises an organasilicon compound and the protective layer is formed by polymerization thereof.
Claim 4
Dependent Claim
19 words
Method according to claim 1, wherein said monomeric gas comprises low molecular weight siloxanes having methyl-, vinyl- or phenyl-groups.
Claim 5
Dependent Claim
11 words
Method according to claim 1, wherein said substance comprises hexamethyldisiloxane (HMDS).
Claim 6
Dependent Claim
15 words
Method according to claim 1, wherein said monomeric gas comprises methyl-, vinyl- or alkoxy silane.
Claim 7
Dependent Claim
12 words
Method according to claim 1, wherein said monomeric gas comprises vinyltrimethylsilane (VTMS).
Claim 8
Dependent Claim
11 words
Method according to claim 1, wherein the reflecting metal is aluminum.
Claim 9
Dependent Claim
27 words
Method according to claim 1, wherein said biassing comprises applying a negative bias voltage in the order of about 100 to 500 V, to said wire (16).
Claim 10
Dependent Claim
31 words
Method according to claim 1, wherein the heating of the wire (16) to an, electron-emitting temperature comprises heating the wire to a temperature of between about 1600° C to 2000° C.
Claim 11
Dependent Claim
61 words
Method according to claim 1, further comprising the step of evacuating the vessel (10) to a vacuum of at least 10 -7 bar, and then carrying out the steps of exposing the reflector to the monomeric gas by introducing the monomeric gas into the vessel to obtain a vacuum within the vessel of between about 10 -6 to 10 -5 bar.
Claim 12
Dependent Claim
33 words
Method according to claim 2, wherein oxygen is introduced into said vessel and the generation of said electrons by electric heating of said wire (16) is continued during the introduction of said oxygen.
Claim 13
Dependent Claim
60 words
Method according to claim 11, wherein the step of rendering hydrophilic the surface of the hydrophobic protective layer comprises admitting oxygen to the vessel at a pressure of about one-third of the gas pressure of the monomeric gas and for a period of time of about 30% of that during which the protective layer is formed by deposition and polymerization.
Claim 14
Dependent Claim
17 words
Method according to claim 11, wherein said oxygen is a component of air admitted to said vessel.
Claim 15
Dependent Claim
111 words
Method for applying a transparent protective layer to protect the surface of optical reflectors comprising a reflector substrate having at least one metal reflecting surface, and a polymerized organosilicon protective layer on said metal layer comprising supporting a reflector substrate having at least one metal reflecting surface in an evacuated vacuum vessel, providing gaseous organosilicon in said vessel, generating electrons in said vessel by heating an electron emissive substance to a temperature sufficiently high to emit electrons thereby causing said organosilicon to form a hydrophobic polymerized organosilicon layer on said metal reflecting surface, and then, while continuing the generating of electrons, oxygen is incorporated into the surface of said polymer layer.
Claim 16
Dependent Claim
111 words
Method for applying a transparent protective layer to protect the surface of optical reflectors comprising a reflector substrate having at least one metal reflecting surface, and a polymerized organosilicon protective layer on said metal layer comprising supporting a reflector substrate having at least one metal reflecting surface in an evacuated vacuum vessel, providing gaseous organosilicon in said vessel, generating electrons in said vessel by heating an electron emissive substance to a temperature sufficiently high to emit electrons thereby causing said organosilicon to form a hydrophobic polymerized organosilicon layer on said metal reflecting surface, and then, while continuing the generating of electrons, oxygen is incorporated into the surface of said polymer layer.
Claim 17
Dependent Claim
43 words
Th method of claim 14 comprising locating a reflector substrate in said evacuated vacuum vessel, then vapor depositing a layer of a reflecting metal on at least one reflective surface of said substrate, and then introducing said gaseous organosilicon monomer into said vessel.
Claim 18
Dependent Claim
45 words
The method of claim 15 wherein said evacuated vacuum vessel has a vacuum of at least 10 -7 bar, and then introducing said gaseous organosilicon monomer into the vessel to obtain a vacuum within the vessel of between about 10 -6 to 10 -5 bar.
Claim 19
Dependent Claim
23 words
The method of claim 15 wherein said electron emissive substance is heated to a temperature of between about 1600° C and 2000° C.
Claim 20
Dependent Claim
29 words
The method of claim 15 wherein said organosilicon monomer comprises low molecular weight siloxanes containing substituents selected from the group consisting of methyl groups, vinyl groups, and phenyl groups.
Claim 21
Dependent Claim
11 words
Method according to claim 15, wherein said organosilicon monomer is hexamethyldisiloxane.
Claim 22
Dependent Claim
27 words
Method according to claim 15 wherein said organosilicon monomer is a silane having substituents selected from the group consisting of methyl groups, vinyl groups, and alkoxy groups.
Claim 23
Dependent Claim
11 words
Method according to claim 15 wherein said organosilicon monomer is vinyltrimethylsilane.
Claim 24
Dependent Claim
19 words
Method according to claim 15 wherein said oxygen is introduced into said vessel by introducing air into said vessel.
Claim 25
Dependent Claim
66 words
The method of claim 15 wherein said oxygen is admitted into said vessel at a pressure of about 1/3 of the gas pressure of said gaseous organosilicon monomer and wherein the period of time during which said oxygen is introduced into said vessel is about 30% of the time during which the protective layer is formed by deposition and polymerization on said metal surfaced reflector substrate.
Claim 26
Dependent Claim
24 words
Method of claim 14 wherein said vessel containing said gaseous organosilicon is at a vacuum of between about 10 -6 to 10 -5 bar.
Claim 27
Dependent Claim
41 words
The method of claim 24 wherein said electron emissive substance is biassed to a negative voltage with respect to said reflector substrates and wherein said electron emissive substance is heated to a temperature of between about 1600° C and 2000° C.
Claim 28
Dependent Claim
21 words
The method of claim 25 wherein said organosilicon has a vapour pressure of more than 10 -5 bar at 20° C.
Claim 29
Dependent Claim
15 words
The method of claim 26 wherein said metal reflecting surface is an aluminum reflecting surface.
Claim 30
Dependent Claim
19 words
The method of claim 27 wherein said gaseous organosilicon is selected from the group consisting of hexamethyldisiloxane and vinyltrimethylsilane.
Claim 31
Dependent Claim
27 words
The method of claim 28 wherein said oxygen is admitted into said vessel at a pressure of about 1/3 of the gas pressure of said gaseous organosilicon.
Claim 32
Dependent Claim
33 words
The method of claim 29 wherein said oxygen is admitted into said vessel for a period of time which is about 30% of the time during which said polymerized organosilicon layer is formed.
Claim 33
Dependent Claim
28 words
The method of claim 26 wherein said organosilicon is a low molecular weight siloxane containing substituent groups selected from the group consisting of methyl, vinyl and phenyl groups.
Claim 34
Dependent Claim
22 words
The method of claim 26 wherein said organosilicon is a silane selected from the group consisting of methyl-, vinyl-, and alkoxy silanes.
Claim 35
Dependent Claim
64 words
A coated optical reflector having at least one reflective surface comprising a reflector substrate coated on its reflective surface with a thin reflective layer of a reflecting metal, said layer of reflecting metal being coated with a clear protective layer, and said protective layer consisting essentially of a hydrophobic polymerized organosilicon in contact with said reflecting metal and having its surface enriched with oxygen.
Claim 36
Dependent Claim
64 words
A coated optical reflector having at least one reflective surface comprising a reflector substrate coated on its reflective surface with a thin reflective layer of a reflecting metal, said layer of reflecting metal being coated with a clear protective layer, and said protective layer consisting essentially of a hydrophobic polymerized organosilicon in contact with said reflecting metal and having its surface enriched with oxygen.
Claim 37
Dependent Claim
19 words
The coated optical reflector of claim 33 wherein said protective layer is between about 10 and 60 nm thick.
Claim 38
Dependent Claim
13 words
The coated optical reflector of claim 33 wherein said reflecting metal is aluminum.
Claim 39
Dependent Claim
14 words
The coated optical reflector of claim 33 wherein said polymerized organosilicon is polymerized vinyltrimethylsilane.
Claim 40
Dependent Claim
14 words
The coated optical reflector of claim 33 wherein said polymerized organosilicon is polymerized hexylmethyldisiloxane.
Claim 41
Dependent Claim
19 words
The coated optical reflector of claim 33 wherein said protective layer is between about 20 and 30 nm thick.
Claim 42
Dependent Claim
23 words
The coated optical reflector of claim 33 wherein said organosilicon has a vapor pressure of more than 10 -5 bar at 20° C.
Claim 43
Dependent Claim
30 words
The coated optical reflector of claim 33 wherein said organosilicon is a low molecular weight siloxane containing substituent groups selected from the group consisting of methyl, vinyl and phenyl groups.
Claim 44
Dependent Claim
24 words
The coated optical reflector of claim 33 wherein said organosilicon is a silane selected from the group consisting of methyl-, vinyl-, and alkoxy silanes.
Claim 45
Dependent Claim
13 words
The coated optical reflector of claim 36 wherein said reflecting metal is aluminum.
Claim 46
Dependent Claim
13 words
The coated optical reflector of claim 37 wherein said reflecting metal is aluminum.
Claim 47
Dependent Claim
13 words
The coated optical reflector of claim 39 wherein said reflecting metal is aluminum.
Claim 48
Dependent Claim
13 words
The coated optical reflector of claim 40 wherein said reflecting metal is aluminum.
Claim 49
Dependent Claim
13 words
The coated optical reflector of claim 41 wherein said reflecting metal is aluminum.
Claim 50
Dependent Claim
13 words
The coated optical reflector of claim 34 wherein said reflecting metal is aluminum.
Claim 51
Dependent Claim
31 words
The coated optical reflector of claim 47 wherein said polymerized organosilicon is a polymerized low molecular weight siloxane having substituents selected from the group consisting of methyl, vinyl, and phenyl groups.
Claim 52
Dependent Claim
14 words
The coated optical reflector of claim 47 wherein said polymerized organosilicon is polymerized hexamethyldisiloxane.
Claim 53
Dependent Claim
23 words
The coated optical reflector of claim 47 wherein said polymerized organosilicon is selected from the group consisting of polymerized methylsilane, vinylsilane, and alkoxysilane.
Claim 54
Dependent Claim
14 words
The coated optical reflector of claim 42 wherein said polymerized organosilicon is polymerized vinyltrimethylsilane.
Claim 55
Dependent Claim
119 words
Apparatus to apply a protective layer to the surface of optical reflectors comprising a vacuum vessel (10), and means (14) within the vessel supporting reflector substrates (15) therein; said vessel further comprising an electron discharge generating electrode wire (16) located within the vessel to thermally generate an electron discharge therein; and means (21) to heat the wire to electron emission and wherein the means (21) to heat the wire and is a controllable source of electrical current to heat the electrode wire selectively to: (a) a temperature at which reflecting metal can be evaporated, and (b) a temperature at which electrons are emitted whereby a single wire will serve, simultaneously, as a metal vaporizer and as an electron generator.
Claim 56
Dependent Claim
119 words
Apparatus to apply a protective layer to the surface of optical reflectors comprising a vacuum vessel (10), and means (14) within the vessel supporting reflector substrates (15) therein; said vessel further comprising an electron discharge generating electrode wire (16) located within the vessel to thermally generate an electron discharge therein; and means (21) to heat the wire to electron emission and wherein the means (21) to heat the wire and is a controllable source of electrical current to heat the electrode wire selectively to: (a) a temperature at which reflecting metal can be evaporated, and (b) a temperature at which electrons are emitted whereby a single wire will serve, simultaneously, as a metal vaporizer and as an electron generator.
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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) | 1981-04-17 | 1981-10-17 | 1982-04-18 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1985-04-17 | 1985-10-17 | 1986-04-18 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1989-04-17 | 1989-10-17 | 1990-04-18 | $7700.00 | Window Closed / Lapsed |