US3867207A - Method of blackening a steel component for a color cathode ray tube - Google Patents

Method of blackening a steel component for a color cathode ray tube Download PDF

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Publication number
US3867207A
US3867207A US364975A US36497573A US3867207A US 3867207 A US3867207 A US 3867207A US 364975 A US364975 A US 364975A US 36497573 A US36497573 A US 36497573A US 3867207 A US3867207 A US 3867207A
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United States
Prior art keywords
component
cathode ray
immersing
aperture mask
ray tube
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US364975A
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John J Decker
Susan V Zito
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GTE Sylvania Inc
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GTE Sylvania Inc
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Priority to US364975A priority Critical patent/US3867207A/en
Priority to BE143855A priority patent/BE814473A/en
Priority to DE19742423732 priority patent/DE2423732C3/en
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Publication of US3867207A publication Critical patent/US3867207A/en
Assigned to NORTH AMERICAN PHILIPS CONSUMER ELECTRONICS CORP. reassignment NORTH AMERICAN PHILIPS CONSUMER ELECTRONICS CORP. ASSIGNS ITS ENTIRE RIGHT TITLE AND INTEREST, UNDER SAID PATENTS AND APPLICATIONS, SUBJECT TO CONDITIONS AND LICENSES EXISTING AS OF JANUARY 21, 1981. (SEE DOCUMENT FOR DETAILS). Assignors: GTE PRODUCTS CORPORATION A DE CORP.
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Classifications

    • 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
    • H01J9/14—Manufacture of electrodes or electrode systems of non-emitting electrodes
    • H01J9/142—Manufacture of electrodes or electrode systems of non-emitting electrodes of shadow-masks for colour television tubes
    • H01J9/146—Surface treatment, e.g. blackening, coating

Definitions

  • the black nickel or cobalt compound formed on the surface is a nickel or cobalt phosphide having the formula Ni P or Co P.
  • a particularly workable nickel plating bath is composed of 30 grams per liter of nickel chloride, 50 grams per liter of sodium glycollate, and 10 grams per liter of sodium hypophosphite.
  • the pH of the plating bath should be between 4 and 6 and the temperature of the bath should be about l9()F. If necessary the pH can be adjusted by the addition of sodium hydroxide.
  • a suitable cobalt plating bath is composed of 30 grams per liter of cobalt chloride, 35 grams per liter of sodium citrate, 50 grams per liter of ammonium chloride and 20 grams per liter of sodium hypophosphite. As this is an alkaline bath the pH should be about 9-10 and the temperature about lF to 205F. If necessary, the pH can be adjusted by addition of ammonium hydroxide.
  • the component After immersion in the electroless nickel or cobalt plating bath which as has been mentioned above, should be for about 15 minutes.
  • the component is removed from the bath and rinsed in deionized water.
  • the component is immersed in a strong oxidizing acid for 30 to 45 seconds.
  • a suitable oxidizing acid contains 3 parts phosphoric, 1 part sulfuric, and 1 part nitric, all in concentrated form.
  • the component is removed and quickly rinsed in warm tap water. Further rinses are then performed in deionized water, and anhydrol.
  • the component is then dried and fired for about 1 hour in air at about 450C.
  • the black surface coating that is now formed on the component is a complex nickel or cobalt compound which is believed to be Ni P or Co P, that is, a nickel or cobalt phosphide.
  • Ni P or Co P that is, a nickel or cobalt phosphide.
  • These compounds have been found to be extremely stable during the various processing procedures used to fabricate a cathode ray tube, and these procedures involve numerous bak ings in air at above 400C.
  • either coating is very stable during operation of the cathode ray tube in which the component is incorporated even though it is being bombarded with electrons in a vacuum and is subject to repeated heating and cooling.
  • a method of blackening a steel component which comprises the steps of: degreasing said component; immersing said component in a 50% hydrochloric acid bath for about 1 minute; rinsing said component in deionized water; immersing said component in an electro less plating bath selected from the group consisting of nickel or cobalt for about 15 minutes, said plating bath 2.
  • said component is a steel frame of an aperture mask.
  • oxidizing acid is comprised of 3 parts phosphoric, 1 part sulfuric, and 1 part nitric acid.

Abstract

The steel components of a cathode ray tube, mainly the aperture mask and the aperture mask frame are blackened by immersing the same in an electroless plating bath selected from the group consisting of nickel and cobalt and after subsequent rinses immersing again in a strong oxidizing acid and firing the component in air at about 450*C to form a black, complex nickel or cobalt compound on the surface of the component.

Description

nited States Patent Decker et al.
[451 Feb. 18, 1975 METHOD OF BLACKENING A STEEL COMPONENT FOR A COLOR CATHODE RAY TUBE Inventors: John J. Decker; Susan V. Zito, both of Emporium, Pa.
GTE Sylvania Incorporated, Stamford, Conn.
Filed: May 29, 1973 Appl. No.1 364,975
Assignee:
U.S. Cl. l48/6.l4 R, 148/615 R, 117/130 E Int. Cl. C23f 5/02 Field of Search 117/130 E; 148/63, 6.14,
References Cited UNITED STATES PATENTS 5/1958 Bolin 117/130 E 3,088,846 5/1963 Lee [17/71 M Primary Examiner-Leon D. Rosdol Assistant ExaminerCharles R. Wolfe, Jr. Attorney, Agent, or Firm-Norman J. OMalley; William H. McNeill; Donald R. Castle [57] ABSTRACT 4 Claims, No Drawings METHOD OF BLACKENING A STEEL COMPONENT FOR A COLOR CATHODE RAY TUBE BACKGROUND OF THE INVENTION This invention relates generally to the aperture mask and aperture mask frames of color picture tubes and more particularly to a method of applying thereto a black surface coating. It has been common practice for many years to blacken the surface of the aperture mask and aperture mask frame of a color picture tube to provide better heat radiation characteristics. Generally, this has been accomplished by merely firing the frames or masks in a wet atmosphere. This process generally yields a black oxide of iron; however, many disadvantages are present in this process. For example, under many conditions a brown oxide of iron is formed either during the process itself or at some point in time during the storage of the component. Further, iron oxide has a tendency to decompose in a vacuum when it is heated and bombarded with electrons as is the case during operation of the color cathode ray tube in which it is employed.
Therefore, it would be advantageous if a process could be found which would blacken these steel components without having the disadvantages of the prior art techniques.
OBJECTS AND SUMMARY OF THE INVENTION It is, therefore, an object of this invention to obviate the disadvantages of the prior art.
It is another object of the invention to provide a simple and reliable method of blackening steel components of color cathode ray tubes.
It is yet another object of the invention to provide a stable blackened surface upon the steel components of a color cathode ray tube,
These objects are accomplished in one aspect of the invention by the provision of a method whereby the steel components of a color cathode ray tube, such as the aperture mask frame and the aperture mask itself, are provided with a nickel or cobalt compoundcoating from an electroless plating bath and subjecting this coating to a strong oxidizing acid and subsequently firing the same in air at about 450C to provide a complex black nickel or cobalt compound upon the surface. The
compound formed by this process is extremely stable and has shown the advantage of remaining black even after many passes at about 450C in an air atmosphere.
It is believed that the black nickel or cobalt compound formed on the surface is a nickel or cobalt phosphide having the formula Ni P or Co P.
DESCRIPTION OF THE PREFERRED EMBODIMENTS ponent is next placed in an electroless nickel or cobalt plating bath for about 15 minutes. A number of such electroless nickel plating baths are commercially available and excellent results have been had with a bath known as Shipley NL-62, which is available from the Shipley Company, Newton, Mass. A number of other nickel plating baths both acid and alkaline are disclosed in US. Pat. No. 2,532,283. Additionally, cobalt plating baths are disclosed in US. Pat. No. 2,532,284.
A particularly workable nickel plating bath is composed of 30 grams per liter of nickel chloride, 50 grams per liter of sodium glycollate, and 10 grams per liter of sodium hypophosphite. The pH of the plating bath should be between 4 and 6 and the temperature of the bath should be about l9()F. If necessary the pH can be adjusted by the addition of sodium hydroxide.
A suitable cobalt plating bath is composed of 30 grams per liter of cobalt chloride, 35 grams per liter of sodium citrate, 50 grams per liter of ammonium chloride and 20 grams per liter of sodium hypophosphite. As this is an alkaline bath the pH should be about 9-10 and the temperature about lF to 205F. If necessary, the pH can be adjusted by addition of ammonium hydroxide.
After immersion in the electroless nickel or cobalt plating bath which as has been mentioned above, should be for about 15 minutes. the component is removed from the bath and rinsed in deionized water. Next, the component is immersed in a strong oxidizing acid for 30 to 45 seconds. A suitable oxidizing acid contains 3 parts phosphoric, 1 part sulfuric, and 1 part nitric, all in concentrated form. After the oxidizing acid bath the component is removed and quickly rinsed in warm tap water. Further rinses are then performed in deionized water, and anhydrol. The component is then dried and fired for about 1 hour in air at about 450C.
As stated above, the black surface coating that is now formed on the component is a complex nickel or cobalt compound which is believed to be Ni P or Co P, that is, a nickel or cobalt phosphide. These compounds have been found to be extremely stable during the various processing procedures used to fabricate a cathode ray tube, and these procedures involve numerous bak ings in air at above 400C. Furthermore, either coating is very stable during operation of the cathode ray tube in which the component is incorporated even though it is being bombarded with electrons in a vacuum and is subject to repeated heating and cooling.
It will be seen from the above that use of this process obviates many of the disadvantages of the prior art and when applied to the aperture mask frame or the aperture mask itself of a color cathode ray tube has many unique properties.
While there has been shown what is at present considered to be the preferred embodiments of the invention, it will be apparent to those skilled in the art that various changes and modifications can be made herein without departing from the scope of the invention as defined by the appended claims.
What is claimed is:
l. A method of blackening a steel component which comprises the steps of: degreasing said component; immersing said component in a 50% hydrochloric acid bath for about 1 minute; rinsing said component in deionized water; immersing said component in an electro less plating bath selected from the group consisting of nickel or cobalt for about 15 minutes, said plating bath 2. The method of claim 1 wherein said component is a steel frame of an aperture mask.
3. The method of claim 1 wherein said component is a steel aperture mask.
4. The method of claim 1 wherein said oxidizing acid is comprised of 3 parts phosphoric, 1 part sulfuric, and 1 part nitric acid.

Claims (4)

1. A METHOD OF BLACKENING A STEEL COMPONENT WHICH COMPRISES THE STEPS OF: DEGREASING SAID COMPONENT; IMMERSING SAID COMPONENT IN A 50% HYDROCHLORIC ACID BATH FOR ABOUT 1 MINUTE; RINSING SAID COMPONENT IS DEIONIZED WATER; IMMERSING SAID COMPONENT IN AN ELECTROLESS PLATING BATH SELECTED FROM THE GROUP CONSISTING OF NICKEL OF COBATH FOR ABOUT 15 MINUTES, SAID PLATING BATH INCLUDING AN EFFECTIVE AMOUNT OF A REDUCING AGENT INCLUDING A HYPOPHOSPHITE COMPOUND; RINSING SAID COMPONENT IN DEIONIZED WATER; IMMERSING SAID COMPONENT IN A STRONG OXIDING ACID BATH FOR 30 TO 45 SECONDS, RINSING SAID COMPONENT IN WARM TAP WATER; RERINSING SAID COMPONENT IN DEIONIZED WATER; RERINSING SAID COMPONENT IN ANHYDROL; DRYING SAID COMPONENT; AND FIRING SAID COMPONENT IN AIR FOR ABOUT 1 HOUR AT ABOUT 450*C.
2. The method of claim 1 wherein said component is a steel frame of an aperture mask.
3. The method of claim 1 wherein said component is a steel aperture mask.
4. The method of claim 1 wherein said oxidizing acid is comprised of 3 parts phosphoric, 1 part sulfuric, and 1 part nitric acid.
US364975A 1973-05-29 1973-05-29 Method of blackening a steel component for a color cathode ray tube Expired - Lifetime US3867207A (en)

Priority Applications (3)

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US364975A US3867207A (en) 1973-05-29 1973-05-29 Method of blackening a steel component for a color cathode ray tube
BE143855A BE814473A (en) 1973-05-29 1974-05-02 PROCESS FOR BLACKENING A STEEL COMPONENT ELEMENT FOR A CATHODIC RAY TUBE WITH COLOR IMAGES AND PRODUCT SO OBTAINED
DE19742423732 DE2423732C3 (en) 1973-05-29 1974-05-16 Blackening process for steel components of cathode ray tubes

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Cited By (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4149908A (en) * 1977-09-26 1979-04-17 Rca Corporation Method for blackening the surfaces of a body of ferrous metal
US4233107A (en) * 1979-04-20 1980-11-11 The United States Of America As Represented By The Secretary Of Commerce Ultra-black coating due to surface morphology
US4355056A (en) * 1981-03-31 1982-10-19 The Babcock & Wilcox Company Method of manufacturing a combustibles sensor
US4361630A (en) * 1979-04-20 1982-11-30 The United States Of America As Represented By The Secretary Of The Commerce Ultra-black coating due to surface morphology
US4511614A (en) * 1983-10-31 1985-04-16 Ball Corporation Substrate having high absorptance and emittance black electroless nickel coating and a process for producing the same
US4657786A (en) * 1982-10-22 1987-04-14 Bayer Aktiengesellschaft Black-metallized substrate surfaces
US4756702A (en) * 1986-12-31 1988-07-12 Zenith Electronics Corporation Pretreatment process for flat tension mask
US4904218A (en) * 1987-12-02 1990-02-27 Zenith Electronics Corporation Blackening of non-iron-based flat tensioned foil shadow masks
US4929864A (en) * 1987-12-02 1990-05-29 Zenith Electronics Corporation NI-based FTM shadow masks having a nickel phosphide black layer
US4971590A (en) * 1987-12-02 1990-11-20 Zenith Electronics Corporation Process for improving the emissivity of a non-based tension shadow mask
US5078812A (en) * 1990-10-09 1992-01-07 Rca Thomson Licensing Corp. Method for darkening a color-selection electrode
US20140287208A1 (en) * 2013-03-22 2014-09-25 Surface Technology, Inc. Blackened composite electroless nickel coatings

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2836510A (en) * 1953-05-21 1958-05-27 Gen Motors Corp Nickel plating by chemical reduction
US3088846A (en) * 1962-01-24 1963-05-07 Gen Am Transport Processes of treating nickel-phosphorus alloy coatings and the resulting modified coatings

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2836510A (en) * 1953-05-21 1958-05-27 Gen Motors Corp Nickel plating by chemical reduction
US3088846A (en) * 1962-01-24 1963-05-07 Gen Am Transport Processes of treating nickel-phosphorus alloy coatings and the resulting modified coatings

Cited By (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4149908A (en) * 1977-09-26 1979-04-17 Rca Corporation Method for blackening the surfaces of a body of ferrous metal
US4233107A (en) * 1979-04-20 1980-11-11 The United States Of America As Represented By The Secretary Of Commerce Ultra-black coating due to surface morphology
US4361630A (en) * 1979-04-20 1982-11-30 The United States Of America As Represented By The Secretary Of The Commerce Ultra-black coating due to surface morphology
US4355056A (en) * 1981-03-31 1982-10-19 The Babcock & Wilcox Company Method of manufacturing a combustibles sensor
US4657786A (en) * 1982-10-22 1987-04-14 Bayer Aktiengesellschaft Black-metallized substrate surfaces
US4511614A (en) * 1983-10-31 1985-04-16 Ball Corporation Substrate having high absorptance and emittance black electroless nickel coating and a process for producing the same
US4756702A (en) * 1986-12-31 1988-07-12 Zenith Electronics Corporation Pretreatment process for flat tension mask
US4904218A (en) * 1987-12-02 1990-02-27 Zenith Electronics Corporation Blackening of non-iron-based flat tensioned foil shadow masks
US4929864A (en) * 1987-12-02 1990-05-29 Zenith Electronics Corporation NI-based FTM shadow masks having a nickel phosphide black layer
US4971590A (en) * 1987-12-02 1990-11-20 Zenith Electronics Corporation Process for improving the emissivity of a non-based tension shadow mask
US5078812A (en) * 1990-10-09 1992-01-07 Rca Thomson Licensing Corp. Method for darkening a color-selection electrode
US20140287208A1 (en) * 2013-03-22 2014-09-25 Surface Technology, Inc. Blackened composite electroless nickel coatings

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DE2423732B2 (en) 1977-07-14
BE814473A (en) 1974-09-02
DE2423732A1 (en) 1975-01-09

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Owner name: NORTH AMERICAN PHILIPS CONSUMER ELECTRONICS CORP.

Free format text: ASSIGNS ITS ENTIRE RIGHT TITLE AND INTEREST, UNDER SAID PATENTS AND APPLICATIONS, SUBJECT TO CONDITIONS AND LICENSES EXISTING AS OF JANUARY 21, 1981.;ASSIGNOR:GTE PRODUCTS CORPORATION A DE CORP.;REEL/FRAME:003992/0284

Effective date: 19810708

Owner name: NORTH AMERICAN PHILIPS CONSUMER ELECTRONICS CORP.,

Free format text: ASSIGNS ITS ENTIRE RIGHT TITLE AND INTEREST, UNDER SAID PATENTS AND APPLICATIONS, SUBJECT TO CONDITIONS AND LICENSES EXISTING AS OF JANUARY 21, 1981.;ASSIGNOR:GTE PRODUCTS CORPORATION A DE CORP.;REEL/FRAME:003992/0284

Effective date: 19810708