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US4956202A Expired / Lapsed US ⏱️ 0.0 years remaining

Firing and milling method for producing a manganese activated zinc silicate phosphor

Assignee: Osram Sylvania Inc
•
Filing: 1989-10-27
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Granted: 1990-09-11
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Expires: 2009-10-27
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Abstract

Abstract A method for producing manganese activated zinc silicate phosphor wherein the individual phosphor particles are surrounded with a non-particulate, conformal aluminum oxide coating is disclosed. The method comprises dry blending a mixture of components consisting essentially of zinc oxide, silicic acid, a source of manganese, ammonium chloride, ammonium fluoride, tungstic oxide, and silica, wherein the Zn+Mn/Si mole ratio is from about 1.95 to about 2.02, wherein the silica is colloidal and has a surface area of from about 50 to about 410 m 2 per gram, and wherein the colloidal silica makes up from about 0.01% to about 1.0% by weight of the mixture; firing the resulting dry blend of components in a nitrogen atmosphere at a temperature of from about 1200° C. to about 1300° C. for a sufficient time to produce the phosphor; milling the resulting phosphor for a period of time of from about 60 minutes to about 120 minutes; firing the resulting milled phosphor in air at a temperature of from about 1175° C. to about 1275° C. for a sufficient time to diffuse the tungsten and manganese to the surfaces of the phosphor particles; applying a non-particulate, conformal aluminum oxide coating to the outer surface of individual particles of the phosphor while the phosphor particles are suspended in a fluid bed having a midpoint temperature between 400° and 480° C., the aluminum oxide coating being formed by a chemical vapor deposition reaction involving oxidation of trimethyl aluminum; and annealing the aluminum oxide coated phosphor for a period of time from 4-16 hours at a temperature between 750° and 800° C.

Inventors

  • 👤 Anthony F. Kasenga
  • 👤 A. Gary Sigai
  • 👤 Thomas E. Peters
  • 👤 Roger B. Hunt

Bibliographic Details

Application Number —
Jurisdiction US
Data Source google_patents
Last Synchronized 2026-10-23 15:07
CPC Classifications
C; C09; C09K; C09K11/00; C09K11/08; C09K11/59; C09K11/592; C09K11/595

Claims Analysis

Total Claims: 15
Claim 1
Independent Claim 282 words
A method for producing manganese activated zinc silicate phosphor particles wherein the individual phosphor particles are surrounded by a continuous, non-particulate, conformal aluminum oxide coating, said method comprising: dry blending a mixture of components consisting essentially of zinc oxide, silica acid, a source of manganese, ammonium chloride, ammonium fluoride, tungstic oxide in an amount sufficient to improve phosphor maintenance in a fluorescent lamp, and silica, and having a Zn+Mn/Si mole ratio from about 1.95 to about 2.02, wherein said silica is colloidal and has a surface area of from about 50 to about 410 m 2 per gram, and wherein said colloidal silica makes up from about 0.01% to about 1.0% by weight of said mixture; firing the resulting dry blend of components in a nitrogen atmosphere at a temperature of from about 1200° C. to about 1300° C. for a sufficient time to produce said phosphor particles; milling the resulting phosphor particles for a period of time of from about 60 minutes to about 120 minutes; firing the resulting milled phosphor particles in air at a temperature of from about 1175° C. to about 1275° C. for a sufficient time to diffuse the tungsten and manganese to the surfaces of the phosphor particles; applying a continuous, non-particulate, conformal aluminum oxide coating to the outer surface of individual particles of the phosphor while said phosphor particles are suspended in a fluid bed having a midpoint temperature between 400° and 480° C., said aluminum oxide coating being formed by oxidation of trimethyl aluminum in a chemical vapor deposition reaction; and annealing the aluminum oxide coated phosphor particles for a period of time from 4-16 hours at a temperature between 750° and 800° C.
Claim 2
Independent Claim 282 words
A method for producing manganese activated zinc silicate phosphor particles wherein the individual phosphor particles are surrounded by a continuous, non-particulate, conformal aluminum oxide coating, said method comprising: dry blending a mixture of components consisting essentially of zinc oxide, silica acid, a source of manganese, ammonium chloride, ammonium fluoride, tungstic oxide in an amount sufficient to improve phosphor maintenance in a fluorescent lamp, and silica, and having a Zn+Mn/Si mole ratio from about 1.95 to about 2.02, wherein said silica is colloidal and has a surface area of from about 50 to about 410 m 2 per gram, and wherein said colloidal silica makes up from about 0.01% to about 1.0% by weight of said mixture; firing the resulting dry blend of components in a nitrogen atmosphere at a temperature of from about 1200° C. to about 1300° C. for a sufficient time to produce said phosphor particles; milling the resulting phosphor particles for a period of time of from about 60 minutes to about 120 minutes; firing the resulting milled phosphor particles in air at a temperature of from about 1175° C. to about 1275° C. for a sufficient time to diffuse the tungsten and manganese to the surfaces of the phosphor particles; applying a continuous, non-particulate, conformal aluminum oxide coating to the outer surface of individual particles of the phosphor while said phosphor particles are suspended in a fluid bed having a midpoint temperature between 400° and 480° C., said aluminum oxide coating being formed by oxidation of trimethyl aluminum in a chemical vapor deposition reaction; and annealing the aluminum oxide coated phosphor particles for a period of time from 4-16 hours at a temperature between 750° and 800° C.
Claim 3
Dependent Claim 19 words
A method in accordance with claim 1 wherein said Zn+Mn/Si mole ratio is from about 1.95 to about 1.99.
Claim 4
Dependent Claim 24 words
A method in accordance with claim 1 wherein the colloidal silica makes up from about 0.03% to about 0.3% by weight of said mixture.
Claim 5
Dependent Claim 26 words
A method in accordance with claim 1 wherein the surface area of the colloidal silica is from about 100 to about 300 m 2 per gram.
Claim 6
Dependent Claim 22 words
A method in accordance with claim 4 wherein said surface area is from about 175 to about 225 m 2 per gram.
Claim 7
Dependent Claim 34 words
A method in accordance with claim 1 wherein the aluminum oxide coated phosphor particles are annealed at a temperature from about 760° C. to about 770° C. for a period of about 4 hours.
Claim 8
Dependent Claim 24 words
A method in accordance with claim 6 wherein the midpoint temperature of the fluid bed is from about 420° C. to about 440° C.
Claim 9
Dependent Claim 19 words
A method in accordance with claim 6 wherein the midpoint temperature of the fluid bed is about 430° C.
Claim 10
Dependent Claim 30 words
A method in accordance with claim 1 wherein the aluminum oxide coated phosphor particles are annealed at a temperature of about 768° C. for a period of about 4 hours.
Claim 11
Dependent Claim 24 words
A method in accordance with claim 9 wherein the midpoint temperature of the fluid bed is from about 420° C. to about 440° C.
Claim 12
Dependent Claim 19 words
A method in accordance with claim 9 wherein the midpoint temperature of the fluid bed is about 430° C.
Claim 13
Dependent Claim 23 words
A method in accordance with claim 11 wherein the weight percent of aluminum oxide coating is from about 2.6 to 2.8 weight percent.
Claim 14
Dependent Claim 24 words
A method in accordance with claim 1 wherein the midpoint temperature of the fluid bed is from about 420° C. to about 440° C.
Claim 15
Dependent Claim 19 words
A method in accordance with claim 1 wherein the midpoint temperature of the fluid bed is about 430° C.

References Cited (Backward Citations)

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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) 1993-09-10 1994-03-12 1994-09-11 $2000.00 Window Closed / Lapsed
7.5 Years (Year 8) 1997-09-10 1998-03-12 1998-09-11 $3760.00 Window Closed / Lapsed
11.5 Years (Year 12) 2001-09-10 2002-03-12 2002-09-11 $7700.00 Window Closed / Lapsed

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