US3922179A - Method of coating a chromium-nickel component with a chromium oxide-containing layer, and component having such a layer - Google Patents

Method of coating a chromium-nickel component with a chromium oxide-containing layer, and component having such a layer Download PDF

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Publication number
US3922179A
US3922179A US418585A US41858573A US3922179A US 3922179 A US3922179 A US 3922179A US 418585 A US418585 A US 418585A US 41858573 A US41858573 A US 41858573A US 3922179 A US3922179 A US 3922179A
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United States
Prior art keywords
component
heating
layer
cathode
chromium
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Expired - Lifetime
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US418585A
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English (en)
Inventor
Theodorus Hendrikus Weekers
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US Philips Corp
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US Philips Corp
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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
    • C23C8/00—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
    • C23C8/02—Pretreatment of the material to be coated
    • 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
    • C23C8/00—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
    • C23C8/06—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases
    • C23C8/08—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases only one element being applied
    • C23C8/10—Oxidising
    • C23C8/12—Oxidising using elemental oxygen or ozone
    • 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
    • C23C8/00—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
    • C23C8/80—After-treatment

Definitions

  • ABSTRACT 30 1 Foreign Application priority Data A chrornium nickel component destined for prolonged ea in in a vacuum, or exam e a or o a ca 0 e, 1972 Netherlands 7216664 gr id or an anode is heated irF air z i fte r c leanin is '1 Q c L Us Cl 148/6 117/50 17/130 hydrogen atmosphere. at 600-900C for 15 to 45 1 48/70 minutes and is then reduced in moist hydrogen. [51] Int. Cl.
  • the invention relates to a-method of covering a component of an electron discharge tube consisting of a chromium-nickel alloy with a chromium oxide-containing layer which is resistant to paling in a vacuum, in which the component isfirst heated in a dry hydrogen atmosphere, is then oxidised in air, is then heated in a moist hydrogen atmosphere and is-subsequently incorporated in the electron tube.
  • the invention relates in particular to a method of covering such a component, for example, a part of cathode, a grid or an anode, with a dark-coloured chromium oxide-containing layer which is resistant in a vacuum at an operating temperature of approximately 900C or the colour of which during the life of the tube becomes darker.
  • a chromium oxide layer obtained in such manner is not resistant to paling in a vacuum at an operating temperature of approximately 900C.
  • the dark colour of the Cr O layer goes gradually pale as a result of which the temperature of the electrode becomes higher and higher as a result of the decreasing thermal radiation.
  • a chromium oxide-containing layer which is completely paling resistant in a vacuum at approximately 900C can be obtained by using the said known method, if, according to the invention, the oxidation in air is carried out by heating for to 45 minutes, preferably 25 to 35 minutes at a temperature of approximately 600-900C.
  • the oxidation in air is carried out by heating for to 45 minutes, preferably 25 to 35 minutes at a temperature of approximately 600-900C.
  • a nickel-containing chromium oxide layer is obtained after heating at 800-l 100C in a moist hydrogen atmosphere the colour of which does not vary throughout the life of the electron tube.
  • a nickel-containing chromium oxide layer is obtained after the heating in a moist hydrogen atmosphere the colour of which is initially less dark but which, instead becomes darker and darker during the life of the electron tube.
  • FIG. 1 is a cross-sectional view through a cathode for an cathode ray tube, comprising a dark-coloured chromium oxide-containing layer according to the invention
  • FIG. 2 is a cross-sectional view through a cylindrical cathode of the electron tube which also comprises such a layer.
  • Reference numerall in FIG. 1 denotes a nickel cap which serves as a support for the emissive layer 2.
  • the cap 1 is welded to a cylindrical component 3 which consists of a chromium-nickel alloy having, for example, 80% by weight of Ni andwhich serves as an envelope of the heating member 8.
  • the cathode comprises suspension strips 4.
  • this assembly is cleaned by heating in,a dry hydrogen atmosphere at 8 OO-l 100C, Upon heating above 900C the components must be separatefrom each other since otherwise they start sticking together as a result of diffusion.
  • the cylindrical part 3 is to be covered with a dark readily heat-radiating layer so that comparatively much heating energy has to be supplied to the cathode to maintain it at the operating temperature of 900C. Since the radiation of the cylinder 3 increases by the 4" power of the temperature, the radiated thermal energy upon heating the cathode is small so' that the comparatively large heating energy ensures a rapid heating of the cathode.
  • the dark layer 5 on the chromium-nickel cylinder 3 is obtained according to the invention in that the assembly of cap 1 and cylinder 3 and the strips 4 is heated in air for 15 to 45 minutes after cleaning in hydrogen. Chromium oxide and nickel oxide are formed at the surface.
  • the nickel oxide which has formed on the cap 1 and the cylinder 3 is reduced to Ni, whereas the Cr O is not reduced. Since the moist hydrogen atmosphere has an oxidising effect for chromium, even more chromium oxide is formed by said prolonged heating at high temperature.
  • the cathode is incorporated in an electron tube. It has been found that the chromium oxide-containing layer maintains a constant thermal radiation at the operating temperature of 900C of the cathode in a vacuum throughout the life of the cathode. The heating in air proves to be critical.
  • a heating at 800-l 100C for 30 minutes after the reduction in a wet hydrogen atmosphere provides a chromium oxide-containing layer which initially has a lower coefficient of thermal radiation than the above-mentioned layer but the coefficient of thermal radiation of which increases gradually during the life of the cathode. So the cathode temperature decreases gradually during the life, which is favourable in connection with the barium evaporation of the cathode. A given barium evaporation is favourable initially so as to bind residual gases which are detrimental to the emission.
  • the support 6 for the emissive layer 2 was previously welded to a chromium nickel tube 7.
  • the tube 7 projects on both sides from the cylindrical support 6 and serves for the connection of the cathode in mica members.
  • the thermal radiation is stimulated in that the tube 7 is covered with a resistant chromium oxide layer obtained by means of the method according to the invention.
  • a heating member 9 is present in the tube 7.
  • a method of covering a component of an electron discharge tube consisting essentially of a chromiumnickel alloy with a chromium oxide-containing layer which is resistant to paling in a vacuum comprising the steps of heating said component in a dry hydrogen atmosphere to clean the surface thereof; heating said component in air at a temperature of approximately 600 to 900C for about to 45 minutes; heating said component in a moist hydrogen atmosphere to reduce 4 the nickel oxide and subsequently incorporating the thus treated said component in the discharge tube.
  • a component for an electron discharge tube in particular a grid, an anode or a part of a cathode, that is covered with a darkcoloured chromium oxide-containing layer which is paling resistant in a vacuum at 900C and produced according to the method recited in claim 1.
  • a component as in claim 5, comprising a cylindrical member on which a nickel support for the emissive layer of a cathode is previously secured.

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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)
  • Solid Thermionic Cathode (AREA)
US418585A 1972-12-08 1973-11-23 Method of coating a chromium-nickel component with a chromium oxide-containing layer, and component having such a layer Expired - Lifetime US3922179A (en)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
NL7216664.A NL156193B (nl) 1972-12-08 1972-12-08 Werkwijze voor het bedekken van een chroom-nikkel-onderdeel met een chroomoxydehoudende laag, en onderdeel voorzien van een dergelijke laag.

Publications (1)

Publication Number Publication Date
US3922179A true US3922179A (en) 1975-11-25

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US418585A Expired - Lifetime US3922179A (en) 1972-12-08 1973-11-23 Method of coating a chromium-nickel component with a chromium oxide-containing layer, and component having such a layer

Country Status (10)

Country Link
US (1) US3922179A (enrdf_load_stackoverflow)
JP (1) JPS5330581B2 (enrdf_load_stackoverflow)
AR (1) AR200416A1 (enrdf_load_stackoverflow)
BE (1) BE808327A (enrdf_load_stackoverflow)
BR (1) BR7309541D0 (enrdf_load_stackoverflow)
CA (1) CA1009911A (enrdf_load_stackoverflow)
FR (1) FR2209855B1 (enrdf_load_stackoverflow)
GB (1) GB1390880A (enrdf_load_stackoverflow)
IT (1) IT999898B (enrdf_load_stackoverflow)
NL (1) NL156193B (enrdf_load_stackoverflow)

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4950543A (en) * 1986-09-06 1990-08-21 Kernforschungsanlage Julich Gmbh Process for making a structural element subjected to thermal stress with a protective coating
US6641450B2 (en) * 1999-11-05 2003-11-04 Samsung Sdi Co., Ltd. Method of making a cathode for an electron tube
US20040242113A1 (en) * 2002-04-04 2004-12-02 Daisuke Adachi Method for manufacturing plasma display panel
EP1312688A4 (en) * 2000-08-11 2004-12-15 Sumitomo Metal Ind ARTICLES OF NICKEL BASE ALLOY AND METHOD OF MANUFACTURING THEREOF
WO2005062334A1 (en) * 2003-12-23 2005-07-07 L.G. Philips Displays Netherlands B.V. Oxide cathode

Families Citing this family (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS50106555A (enrdf_load_stackoverflow) * 1974-01-29 1975-08-22
JPS5444551B2 (enrdf_load_stackoverflow) * 1974-10-29 1979-12-26
JPS51113451A (en) * 1975-03-28 1976-10-06 Toshiba Corp Cathode body for cathode-ray tube
JPS546761A (en) * 1977-06-17 1979-01-19 Matsushita Electronics Corp Manufacture of electronic cathode-ray tube
JPS5781027U (enrdf_load_stackoverflow) * 1980-11-06 1982-05-19
DE3104112C2 (de) * 1981-02-06 1984-12-13 M.A.N. Maschinenfabrik Augsburg-Nürnberg AG, 8000 München Verfahren zur Herstellung von Oxydschichten
DE3419638C2 (de) * 1984-05-25 1987-02-26 MAN Technologie GmbH, 8000 München Verfahren zur oxidativen Erzeugung von Schutzschichten auf einer Legierung

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US1760526A (en) * 1929-02-16 1930-05-27 Westinghouse Lamp Co Electrode
US3664884A (en) * 1968-03-11 1972-05-23 Concept Research Corp Method of coloring metals by the application of heat
US3703369A (en) * 1969-12-05 1972-11-21 Gen Electric Chromium-containing bodies of improved resistance to oxidation and nitrification

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US1760526A (en) * 1929-02-16 1930-05-27 Westinghouse Lamp Co Electrode
US3664884A (en) * 1968-03-11 1972-05-23 Concept Research Corp Method of coloring metals by the application of heat
US3703369A (en) * 1969-12-05 1972-11-21 Gen Electric Chromium-containing bodies of improved resistance to oxidation and nitrification

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4950543A (en) * 1986-09-06 1990-08-21 Kernforschungsanlage Julich Gmbh Process for making a structural element subjected to thermal stress with a protective coating
US6641450B2 (en) * 1999-11-05 2003-11-04 Samsung Sdi Co., Ltd. Method of making a cathode for an electron tube
EP1312688A4 (en) * 2000-08-11 2004-12-15 Sumitomo Metal Ind ARTICLES OF NICKEL BASE ALLOY AND METHOD OF MANUFACTURING THEREOF
US20040242113A1 (en) * 2002-04-04 2004-12-02 Daisuke Adachi Method for manufacturing plasma display panel
US7074101B2 (en) * 2002-04-04 2006-07-11 Matsushita Electric Industrial Co., Ltd. Method for manufacturing plasma display panel
WO2005062334A1 (en) * 2003-12-23 2005-07-07 L.G. Philips Displays Netherlands B.V. Oxide cathode

Also Published As

Publication number Publication date
FR2209855A1 (enrdf_load_stackoverflow) 1974-07-05
GB1390880A (en) 1975-04-16
BR7309541D0 (pt) 1974-08-29
AU6314073A (en) 1975-06-05
CA1009911A (en) 1977-05-10
DE2359454A1 (de) 1974-06-12
JPS5330581B2 (enrdf_load_stackoverflow) 1978-08-28
JPS4996935A (enrdf_load_stackoverflow) 1974-09-13
NL7216664A (enrdf_load_stackoverflow) 1974-06-11
BE808327A (fr) 1974-06-06
NL156193B (nl) 1978-03-15
FR2209855B1 (enrdf_load_stackoverflow) 1976-10-08
IT999898B (it) 1976-03-10
AR200416A1 (es) 1974-11-08
DE2359454B2 (de) 1977-04-14

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