US3326648A - Method of providing a black layer on a metal object - Google Patents

Method of providing a black layer on a metal object Download PDF

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US3326648A
US3326648A US275495A US27549563A US3326648A US 3326648 A US3326648 A US 3326648A US 275495 A US275495 A US 275495A US 27549563 A US27549563 A US 27549563A US 3326648 A US3326648 A US 3326648A
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layer
metal
antimony oxide
black layer
black
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US275495A
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Provisor Henri
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US Philips Corp
North American Philips Co Inc
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    • 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
    • H01J9/02—Manufacture of electrodes or electrode systems
    • H01J9/04—Manufacture of electrodes or electrode systems of thermionic cathodes
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J19/00—Details of vacuum tubes of the types covered by group H01J21/00
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J2893/00—Discharge tubes and lamps
    • H01J2893/0001—Electrodes and electrode systems suitable for discharge tubes or lamps
    • H01J2893/0012—Constructional arrangements
    • H01J2893/0019—Chemical composition and manufacture
    • H01J2893/0022—Manufacture
    • H01J2893/0023—Manufacture carbonising and other surface treatments
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10S428/00—Stock material or miscellaneous articles
    • Y10S428/922—Static electricity metal bleed-off metallic stock
    • Y10S428/9265—Special properties
    • Y10S428/927—Decorative informative
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10S428/00—Stock material or miscellaneous articles
    • Y10S428/922—Static electricity metal bleed-off metallic stock
    • Y10S428/9265—Special properties
    • Y10S428/929—Electrical contact feature
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10S428/00—Stock material or miscellaneous articles
    • Y10S428/922—Static electricity metal bleed-off metallic stock
    • Y10S428/9335—Product by special process
    • Y10S428/936—Chemical deposition, e.g. electroless plating
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/12—All metal or with adjacent metals
    • Y10T428/12493—Composite; i.e., plural, adjacent, spatially distinct metal components [e.g., layers, joint, etc.]
    • Y10T428/12681—Ga-, In-, Tl- or Group VA metal-base component
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/12—All metal or with adjacent metals
    • Y10T428/12493—Composite; i.e., plural, adjacent, spatially distinct metal components [e.g., layers, joint, etc.]
    • Y10T428/12736—Al-base component
    • Y10T428/1275—Next to Group VIII or IB metal-base component
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/12—All metal or with adjacent metals
    • Y10T428/12493—Composite; i.e., plural, adjacent, spatially distinct metal components [e.g., layers, joint, etc.]
    • Y10T428/12771—Transition metal-base component
    • Y10T428/12778—Alternative base metals from diverse categories
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/12—All metal or with adjacent metals
    • Y10T428/12493—Composite; i.e., plural, adjacent, spatially distinct metal components [e.g., layers, joint, etc.]
    • Y10T428/12771—Transition metal-base component
    • Y10T428/12861—Group VIII or IB metal-base component
    • Y10T428/12944—Ni-base component

Definitions

  • the invention relates to blackening of metal surfaces, for example the inner surface of a metal support for the emissive alkaline-earth oxide layer of indirectly heated oxide cathodes for use in electron tubes, which black surface is located opposite the outer surface of the insulating layer of the filament wire, from which it is separated by a narrow high-vacuum space.
  • This process requires a thermal treatment in vacuo, in a reducing atmosphere or a neutral atmosphere between 610 and 650 C. for 15 to 30 minutes.
  • this heating produces an inadmissible reduction in rigidity, so that difficulties can occur when building the heater body into the cathode, while at a high temperature the black layer vanishes.
  • the invention relates to a novel method of blackening metal surfaces, for example the inner surface of the support for the emissive layer of a cathode, in which method said disadvantages are obviated.
  • the heating time, required for the formation of a blackish layer of intermetallic compounds is reduced, while the black layer itself has a greater thermal resistivity.
  • the new method consists in that a layer of a suspension of antimony oxide in a suitable liquid is applied to the metal surface to be blackened, which surface is heated for about minutes at a temperature of about 650 C. in a reducing atmosphere.
  • the antimony oxide (Sb O or Sb O is suspended in water or in a suitable organic liquid and then applied in known manner to the metal surface; the body thus coated is then heated at about 600 C. or more in a reducing atmosphere.
  • the released antimony reacts with the metal of the body and forms a blackish surface layer.
  • the speed with which this black layer is obtained is ascribed to the easy reduction of the antimony oxide and to the great reactivity of the locally formed antimony.
  • Preferably aluminum powder is added to the suspension.
  • nickel, molybdenum and iron which permit a reaction for obtaining a black surface
  • kinds of steel, even stainless steel are found to be suitable to this end, as well as aluminum.
  • the method according to the present invention may be carried out as follows:
  • a nickel support of an indirectly heated cathode is coated with a suspension of 20 gms of antimony oxide Sb 0 in 100 mls. of nitrocellulose solution.
  • the assembly is heated at about 650 C. for 5 minutes.
  • the antimony oxide alone provided a violet-like blackening, while the surface layer obtained by the thermal reaction is thin.
  • An addition of aluminum powder to the antimony oxide suspension prevents the occurrence of the violet-like reflections and yields more or less deepblack shades in accordance with the quantities of aluminum.
  • black layers obtained by means of mixtures of antimony oxide and aluminum have a much greater resistance to heat than layers obtained by the reactoin of antimony oxide alone with the metal of the support. It has particularly been found that the surface of a nickel support, subsequent to blackening by means of a mixture of antimony oxide and aluminum remains black after a treatment at 800 C. for 500 hours in vacuo, whereas the surface of such a support, subsequent to blackening with only antimony oxide, becomes blank at said temperature in vacuo after a few hours.
  • a suitable suspension of aluminum powder and antimony oxide (Sb O may be composed in the following manner: 2.50 gms. of nitrocellulose is dissolved in gms. of glycol ethylene and 22.5 gms. of butanol; in mls. of this solution is suspended 20 gms. of fine aluminum powder and 10 gms. of antimony oxide (Sb O).
  • the presence of aluminum powder in the antimony oxide suspension practically does not affect the application of the method according to the invention. This may be accounted for by the fact that the antimony forms intermetallic compounds not only with the metal of the support but also with the aluminum powder.
  • This method as described for the manufacture of indirectly heated oxide cathodes, may be employed substantially without any modification, in numerous other cases and will be successful with all surfaces which are heated in some way or other, and of which the heat absorption or the heat dissipation by radiation must be improved. This is the case, for example, with external surfaces of spaces provided with cooling vanes, with motors or heat exchangers.
  • This method may also be used for obtaining certain decorative effects, particularly for trinkets or for protection from corrosion of iron or steel structures.
  • a method of blackening surfaces of metal bodies comprising the steps of applying a layer of a suspension of antimony oxide in a suitable liquid to the metal surface to the blackened and heating said liquid for about 5 minutes at a temperature of about 650 C. in a reducing atmosphere.
  • An object having a blackened surface portion comprising a metal base of a metal selected from the group consisting of nickel, molybdenum, iron and alloys thereof having a layer thereon of an intermetallic compound of antimony and said base metal.
  • a support for an electron emissive layer comprising a nickel base and a black layer of an intermetallic compound of antimony, aluminum and nickel on the side of said base remote from the electron emissive layer.

Description

June 20, 1967 H. PROVISOR 3,325,648
METHOD OF PROVIDING A BLACK LAYER ON A METAL OBJECT Filed April 25, 1963 sb-m-m' Alloy INVENTOR.
HENRI PROVISOR AGENT United States Patent 4 Claims. (Cl. 29-194 The invention relates to blackening of metal surfaces, for example the inner surface of a metal support for the emissive alkaline-earth oxide layer of indirectly heated oxide cathodes for use in electron tubes, which black surface is located opposite the outer surface of the insulating layer of the filament wire, from which it is separated by a narrow high-vacuum space.
It is known that due to the reaction of aluminium with metals such as nickel, molybdenum, iron or with an alloy of these metals, a grey-black intermetallic layer can be obtained.
This process requires a thermal treatment in vacuo, in a reducing atmosphere or a neutral atmosphere between 610 and 650 C. for 15 to 30 minutes. Experience has shown that for certain cases this heating produces an inadmissible reduction in rigidity, so that difficulties can occur when building the heater body into the cathode, while at a high temperature the black layer vanishes.
The invention relates to a novel method of blackening metal surfaces, for example the inner surface of the support for the emissive layer of a cathode, in which method said disadvantages are obviated. Particularly the heating time, required for the formation of a blackish layer of intermetallic compounds is reduced, while the black layer itself has a greater thermal resistivity. The new method consists in that a layer of a suspension of antimony oxide in a suitable liquid is applied to the metal surface to be blackened, which surface is heated for about minutes at a temperature of about 650 C. in a reducing atmosphere.
To this end the antimony oxide (Sb O or Sb O is suspended in water or in a suitable organic liquid and then applied in known manner to the metal surface; the body thus coated is then heated at about 600 C. or more in a reducing atmosphere. The released antimony reacts with the metal of the body and forms a blackish surface layer. The speed with which this black layer is obtained is ascribed to the easy reduction of the antimony oxide and to the great reactivity of the locally formed antimony. Preferably aluminum powder is added to the suspension.
Apart from the said metals nickel, molybdenum and iron, which permit a reaction for obtaining a black surface, kinds of steel, even stainless steel, are found to be suitable to this end, as well as aluminum.
The figure shown in the drawing illustrates the article produced by the invention.
The method according to the present invention may be carried out as follows:
A nickel support of an indirectly heated cathode is coated with a suspension of 20 gms of antimony oxide Sb 0 in 100 mls. of nitrocellulose solution. The assembly is heated at about 650 C. for 5 minutes.
The antimony oxide alone provided a violet-like blackening, while the surface layer obtained by the thermal reaction is thin. An addition of aluminum powder to the antimony oxide suspension prevents the occurrence of the violet-like reflections and yields more or less deepblack shades in accordance with the quantities of aluminum. Moreover, experience has shown that black layers obtained by means of mixtures of antimony oxide and aluminum have a much greater resistance to heat than layers obtained by the reactoin of antimony oxide alone with the metal of the support. It has particularly been found that the surface of a nickel support, subsequent to blackening by means of a mixture of antimony oxide and aluminum remains black after a treatment at 800 C. for 500 hours in vacuo, whereas the surface of such a support, subsequent to blackening with only antimony oxide, becomes blank at said temperature in vacuo after a few hours.
A suitable suspension of aluminum powder and antimony oxide (Sb O may be composed in the following manner: 2.50 gms. of nitrocellulose is dissolved in gms. of glycol ethylene and 22.5 gms. of butanol; in mls. of this solution is suspended 20 gms. of fine aluminum powder and 10 gms. of antimony oxide (Sb O The presence of aluminum powder in the antimony oxide suspension practically does not affect the application of the method according to the invention. This may be accounted for by the fact that the antimony forms intermetallic compounds not only with the metal of the support but also with the aluminum powder.
This method, as described for the manufacture of indirectly heated oxide cathodes, may be employed substantially without any modification, in numerous other cases and will be successful with all surfaces which are heated in some way or other, and of which the heat absorption or the heat dissipation by radiation must be improved. This is the case, for example, with external surfaces of spaces provided with cooling vanes, with motors or heat exchangers. This method may also be used for obtaining certain decorative effects, particularly for trinkets or for protection from corrosion of iron or steel structures.
What is claimed is:
1. A method of blackening surfaces of metal bodies comprising the steps of applying a layer of a suspension of antimony oxide in a suitable liquid to the metal surface to the blackened and heating said liquid for about 5 minutes at a temperature of about 650 C. in a reducing atmosphere.
2. A method as claimed in claim 1, wherein aluminum powder is added to the antimony oxide suspension.
3. An object having a blackened surface portion comprising a metal base of a metal selected from the group consisting of nickel, molybdenum, iron and alloys thereof having a layer thereon of an intermetallic compound of antimony and said base metal.
4. A support for an electron emissive layer comprising a nickel base and a black layer of an intermetallic compound of antimony, aluminum and nickel on the side of said base remote from the electron emissive layer.
References Cited UNITED STATES PATENTS 2,710,253 6/1955 Willardson et al. 75149 2,816,023 12/1957 Genser et a1 75-149 FOREiGN PATENTS 478,754 4/1930 Germany. 932,858 9/ 1955 Germany.
ALFRED L. LEAVITT, Primary Examiner.
WILLIAM L. JARVIS, RALPH S. KENDALL,
Examiners.

Claims (1)

  1. 4. A SUPPORT FOR AN ELECTRON EMISSIVE LAYER COMPRISING A NICKEL BASE AND A BLACK LAYER OF AN INTERMETALLIC COMPOUND OF ANTIMONY, ALUMINUM AND NICKEL ON THE SIDE OF SAID BASE REMOTE FROM THE ELECTRON EMISSIVE LAYER.
US275495A 1962-04-28 1963-04-25 Method of providing a black layer on a metal object Expired - Lifetime US3326648A (en)

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FR896046A FR81588E (en) 1962-04-28 1962-04-28 Further development of indirectly heated oxide cathodes for electron tubes

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AT (1) AT238836B (en)
BE (1) BE631635A (en)
CH (1) CH438876A (en)
DE (1) DE1521891A1 (en)
FR (1) FR81588E (en)
GB (1) GB1009822A (en)
LU (1) LU43284A1 (en)
NL (1) NL291752A (en)

Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3620808A (en) * 1968-01-05 1971-11-16 James E Monroe Jr Method of forming a thermal emissivity coating on a metallic substrate
US3958146A (en) * 1974-02-08 1976-05-18 Gte Sylvania Incorporated Fast warm up picture tube cathode cap having high heat emissivity surface on the interior thereof
US4009409A (en) * 1975-09-02 1977-02-22 Gte Sylvania Incorporated Fast warmup cathode and method of making same
US4574778A (en) * 1984-03-19 1986-03-11 Hydro-Quebec Preparing selective surfaces for solar collectors by dry oxidation and selective surfaces so obtained
US5558644A (en) * 1991-07-16 1996-09-24 Heartport, Inc. Retrograde delivery catheter and method for inducing cardioplegic arrest
US5755687A (en) * 1997-04-01 1998-05-26 Heartport, Inc. Methods and devices for occluding a patient's ascending aorta
US5765568A (en) * 1994-05-27 1998-06-16 Heartport, Inc. Catheter system and method for venting the left ventricle
US5769812A (en) * 1991-07-16 1998-06-23 Heartport, Inc. System for cardiac procedures
US5792094A (en) * 1991-07-16 1998-08-11 Heartport, Inc. Method of delivering cardioplegic fluid to a patient's heart
US6482171B1 (en) 1991-07-16 2002-11-19 Heartport, Inc. Multi-lumen catheter

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE478754C (en) * 1929-07-02 Robert Plagwitz Projector for incident light
US2710253A (en) * 1953-10-19 1955-06-07 Battelle Development Corp Semiconducting alloy
DE932858C (en) * 1953-01-13 1955-09-12 Telefunken Gmbh Process for the treatment of electrodes or electrode materials for electrical discharge tubes for the purpose of giving them a high heat radiation capability using an aluminum-coated starting material which forms intermetallic compounds with the aluminum coating when heated
US2816023A (en) * 1955-11-02 1957-12-10 Battelle Development Corp Semiconductor material and method of preparing same

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE478754C (en) * 1929-07-02 Robert Plagwitz Projector for incident light
DE932858C (en) * 1953-01-13 1955-09-12 Telefunken Gmbh Process for the treatment of electrodes or electrode materials for electrical discharge tubes for the purpose of giving them a high heat radiation capability using an aluminum-coated starting material which forms intermetallic compounds with the aluminum coating when heated
US2710253A (en) * 1953-10-19 1955-06-07 Battelle Development Corp Semiconducting alloy
US2816023A (en) * 1955-11-02 1957-12-10 Battelle Development Corp Semiconductor material and method of preparing same

Cited By (18)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3620808A (en) * 1968-01-05 1971-11-16 James E Monroe Jr Method of forming a thermal emissivity coating on a metallic substrate
US3958146A (en) * 1974-02-08 1976-05-18 Gte Sylvania Incorporated Fast warm up picture tube cathode cap having high heat emissivity surface on the interior thereof
US4009409A (en) * 1975-09-02 1977-02-22 Gte Sylvania Incorporated Fast warmup cathode and method of making same
US4574778A (en) * 1984-03-19 1986-03-11 Hydro-Quebec Preparing selective surfaces for solar collectors by dry oxidation and selective surfaces so obtained
US5769812A (en) * 1991-07-16 1998-06-23 Heartport, Inc. System for cardiac procedures
US5738652A (en) * 1991-07-16 1998-04-14 Heartport, Inc. Retrograde delivery catheter and method for inducing cardioplegic arrest
US6482171B1 (en) 1991-07-16 2002-11-19 Heartport, Inc. Multi-lumen catheter
US5885238A (en) * 1991-07-16 1999-03-23 Heartport, Inc. System for cardiac procedures
US5558644A (en) * 1991-07-16 1996-09-24 Heartport, Inc. Retrograde delivery catheter and method for inducing cardioplegic arrest
US5792094A (en) * 1991-07-16 1998-08-11 Heartport, Inc. Method of delivering cardioplegic fluid to a patient's heart
US5810757A (en) * 1994-05-27 1998-09-22 Heartport, Inc. Catheter system and method for total isolation of the heart
US5800375A (en) * 1994-05-27 1998-09-01 Heartport, Inc. Catheter system and method for providing cardiopulmonary bypass pump support during heart surgery
US5765568A (en) * 1994-05-27 1998-06-16 Heartport, Inc. Catheter system and method for venting the left ventricle
US6398752B1 (en) 1994-05-27 2002-06-04 William P. Sweezer, Jr. Method of occluding a patient's ascending aorta and delivery cardioplegic fluid
US20020161321A1 (en) * 1994-05-27 2002-10-31 Sweezer, William P. Method of occluding a patient's ascending aorta and delivering cardioplegic fluid
US6056723A (en) * 1997-04-01 2000-05-02 Heartport, Inc. Methods and devices for occluding a patient's ascending aorta
US6423031B1 (en) 1997-04-01 2002-07-23 Brian S. Donlon Methods and devices for occluding a patient's ascending aorta
US5755687A (en) * 1997-04-01 1998-05-26 Heartport, Inc. Methods and devices for occluding a patient's ascending aorta

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DE1521891A1 (en) 1969-10-30
BE631635A (en)
GB1009822A (en) 1965-11-10
CH438876A (en) 1967-06-30
FR81588E (en) 1963-10-11
NL291752A (en)
AT238836B (en) 1965-03-10
LU43284A1 (en) 1963-05-02

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