US3813293A - Method of applying a satisfactorily adhering,poorly reflecting,conductive layer to an insulating surface and electric discharge tube having a layer applied by said method - Google Patents

Method of applying a satisfactorily adhering,poorly reflecting,conductive layer to an insulating surface and electric discharge tube having a layer applied by said method Download PDF

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Publication number
US3813293A
US3813293A US00195525A US19552571A US3813293A US 3813293 A US3813293 A US 3813293A US 00195525 A US00195525 A US 00195525A US 19552571 A US19552571 A US 19552571A US 3813293 A US3813293 A US 3813293A
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US
United States
Prior art keywords
layer
applying
insulating surface
electric discharge
discharge tube
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 - Lifetime
Application number
US00195525A
Inventor
Esdonk J Van
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
US Philips Corp
Original Assignee
US Philips Corp
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
Priority claimed from NL6813017A external-priority patent/NL6813017A/xx
Application filed by US Philips Corp filed Critical US Philips Corp
Priority to US00195525A priority Critical patent/US3813293A/en
Application granted granted Critical
Publication of US3813293A publication Critical patent/US3813293A/en
Anticipated expiration legal-status Critical
Expired - Lifetime 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
    • 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
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/14—Metallic material, boron or silicon
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
    • C09K11/02—Use of particular materials as binders, particle coatings or suspension media therefor
    • C09K11/025—Use of particular materials as binders, particle coatings or suspension media therefor non-luminescent particle coatings or suspension media
    • 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
    • C23C14/58—After-treatment
    • 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
    • C23C14/58—After-treatment
    • C23C14/5806—Thermal treatment
    • 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
    • C23C14/58—After-treatment
    • C23C14/5846—Reactive treatment
    • C23C14/5853—Oxidation
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J29/00—Details of cathode-ray tubes or of electron-beam tubes of the types covered by group H01J31/00
    • H01J29/02—Electrodes; Screens; Mounting, supporting, spacing or insulating thereof
    • H01J29/10—Screens on or from which an image or pattern is formed, picked up, converted or stored
    • H01J29/18—Luminescent screens
    • H01J29/28—Luminescent screens with protective, conductive or reflective layers
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J9/00—Apparatus or processes specially adapted for the manufacture, installation, removal, maintenance of electric discharge tubes, discharge lamps, or parts thereof; Recovery of material from discharge tubes or lamps
    • H01J9/20—Manufacture of screens on or from which an image or pattern is formed, picked up, converted or stored; Applying coatings to the vessel
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J9/00—Apparatus or processes specially adapted for the manufacture, installation, removal, maintenance of electric discharge tubes, discharge lamps, or parts thereof; Recovery of material from discharge tubes or lamps
    • H01J9/24—Manufacture or joining of vessels, leading-in conductors or bases
    • H01J9/28—Manufacture of leading-in conductors

Definitions

  • the invention relates to a method of applying a satisfactorily adhering, poorly reflecting, conductive layer to an insulating surface, particularly to the inner wall of an electric discharge tube.
  • the invention furthermore relates to an electric discharge tube, particularly an image intensifier or a cathoderay tube provided with a conducting, poorly reflecting layer applied by said method to part of the inner surface of the tube bulb.
  • nickel oxide layer adheres poorly. This is particularly disadvantageous when such a layer is applied in an electric discharge tube, which is heated at a comparatively high temperature during degassing. The nickel oxide layer may then scale olf or particles may be released therefrom.
  • a satisfactorily adhering, smooth conductive layer with poor reflection can be applied to an insulating surface when in accordance with the invention the surface is first coated by vapor deposition in vacuo with a chromium-nickel layer, to which a nickel layer is applied from the vapor phase, which is converted at least partly into nickel-oxide by heating in an oxidizing atmosphere. It appears that the layer is conductive, adheres very satisfactorily to the insulating surface and has a reflection of less than 10% of that of a brilliant aluminium layer for light of a wavelength of 5000 to 7000 A.
  • Such layers are quite suitable for partially covering the inner surface of the glass bulb of an electric discharge tube, particularly of an image intensifier or of a cathoderay tube.
  • the oxidation of the nickel layer may be performed by heating in air at 250 C. to 500 C.
  • the thickness of the nickel layer may be about In.
  • a method of applying a satisfactorily adhering, smooth, conducting layer of poor reflection to an insulating surface comprising the steps of vapor depositing in vacuum a chromium-nickel layer on said surface, thereafter depositing a nickel layer about I thick on said chromium-nickel layer, and heating the nickel layer in an oxidizing atmosphere to partially convert said nickel layer into nickel oxide until the reflection for light of a wave-length between 5000 and 7000 A. is less than 10%.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Manufacturing & Machinery (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Formation Of Various Coating Films On Cathode Ray Tubes And Lamps (AREA)

Abstract

A SMOOTH CONDUCTIVE LAYER OF POOT REFLECTIVITY ON AN INSULATING SURFACE IN OBTAINED BY FIRST APPLYING A CHROMINUM NICKEL LAYER WHICH IS OXIDIZED BY HEATING IN IS APPLIED A NICKEL LAYER WHICH IS OXIDIZED BY HEATING IN AIR AT 250* CTO500*C.

Description

United States Patent Office 3,813,293- Patented May 28, 1974 Int. Cl. C23b 5/50, 5/64 US. Cl. 117-217 2 Claims ABSTRACT OF THE DISCLOSURE A smooth, conductive layer of poor reflectivity on an insulating surface is obtained by first applying a chromium-nickel layer from the vapor phase, to which layer is applied a nickel layer which is oxidized by heating in air at 250 C. to 500 C.
This application is a continuation of application Ser. No. 856,160 filed Sept. 8, 1969, now abandoned.
The invention relates to a method of applying a satisfactorily adhering, poorly reflecting, conductive layer to an insulating surface, particularly to the inner wall of an electric discharge tube.
The invention furthermore relates to an electric discharge tube, particularly an image intensifier or a cathoderay tube provided with a conducting, poorly reflecting layer applied by said method to part of the inner surface of the tube bulb.
From French Patent Specification 806,867 it is known that the reflection of a brilliant metal layer can be reduced by covering it with a black layer, for example, of nickel oxide. The nickel oxide is applied as such, for example, by a suspension.
It is found that such a nickel oxide layer adheres poorly. This is particularly disadvantageous when such a layer is applied in an electric discharge tube, which is heated at a comparatively high temperature during degassing. The nickel oxide layer may then scale olf or particles may be released therefrom.
It has been found that a satisfactorily adhering, smooth conductive layer with poor reflection can be applied to an insulating surface when in accordance with the invention the surface is first coated by vapor deposition in vacuo with a chromium-nickel layer, to which a nickel layer is applied from the vapor phase, which is converted at least partly into nickel-oxide by heating in an oxidizing atmosphere. It appears that the layer is conductive, adheres very satisfactorily to the insulating surface and has a reflection of less than 10% of that of a brilliant aluminium layer for light of a wavelength of 5000 to 7000 A.
Such layers are quite suitable for partially covering the inner surface of the glass bulb of an electric discharge tube, particularly of an image intensifier or of a cathoderay tube. The oxidation of the nickel layer may be performed by heating in air at 250 C. to 500 C. The thickness of the nickel layer may be about In.
What is claimed is:
1. A method of applying a satisfactorily adhering, smooth, conducting layer of poor reflection to an insulating surface comprising the steps of vapor depositing in vacuum a chromium-nickel layer on said surface, thereafter depositing a nickel layer about I thick on said chromium-nickel layer, and heating the nickel layer in an oxidizing atmosphere to partially convert said nickel layer into nickel oxide until the reflection for light of a wave-length between 5000 and 7000 A. is less than 10%.
2. A method as claimed in claim 1 wherein the nickel layer is heated in air at 250 C. to 500 C.
References Cited UNITED STATES PATENTS 2,935,717 5/1960 Solow 117217 X 2,927,048 3/ 1960 Pritikin 117-217 X 3,472,691 10/1969 Kooy et a1 117217 3,462,723 8/ 1969 Philips 117217 X 3,112,222 11/1963 Alger 117-217 LEON D. ROSDOL, Primary Examiner M. F. EPOSITO, Assistant Examiner US. Cl. X.R.
US00195525A 1968-09-12 1971-11-03 Method of applying a satisfactorily adhering,poorly reflecting,conductive layer to an insulating surface and electric discharge tube having a layer applied by said method Expired - Lifetime US3813293A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
US00195525A US3813293A (en) 1968-09-12 1971-11-03 Method of applying a satisfactorily adhering,poorly reflecting,conductive layer to an insulating surface and electric discharge tube having a layer applied by said method

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
NL6813017A NL6813017A (en) 1968-09-12 1968-09-12
US85616069A 1969-09-08 1969-09-08
US00195525A US3813293A (en) 1968-09-12 1971-11-03 Method of applying a satisfactorily adhering,poorly reflecting,conductive layer to an insulating surface and electric discharge tube having a layer applied by said method

Publications (1)

Publication Number Publication Date
US3813293A true US3813293A (en) 1974-05-28

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