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US3676534A Expired / Lapsed US ⏱️ 0.0 years remaining

Process relating to ultra-pure metal halide particles

Assignee: APL Inc A CORP OF OHIO
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Filing: 1969-09-26
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Granted: 1972-07-11
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Expires: 1989-09-26
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Abstract

Abstract Compositions are described including free-flowing particles of controlled size of purified metal halides such as sodium iodide and mixtures of sodium iodide with scandium iodide. These ultrapure metal halide particles are particularly useful as a vaporizable fill disposed within an arc tube of a high pressure electric discharge device. The preparation and identification of the coordination entity Na ScI 4 (III) is also described. The process for producing purified metal halides of accurately controlled particle size includes evaporating volatiles from the solid impure metal halide, melting the impure halide, passing hydrogen, hydrogen halide, hydrogen and halogen, or mixtures thereof through the halide, and then passing the molten halide through a vibrating discharge conduit or nozzle into an inert quenching atmosphere to form the particles of purified halide.

Inventors

  • 👤 Scott Anderson

Bibliographic Details

Application Number —
Jurisdiction US
Data Source google_patents
Last Synchronized 2026-10-26 15:51
CPC Classifications
C; C01; C01G; C01G1/00; C01G1/06; C01D; C01D3/00; C01D3/14; C01D3/20; C01F; C01F17/00; C01F17/30; C01F17/36; C01G13/00; C01G13/04; C01P; C01P2004/00; C01P2004/60; C01P2004/61; C01P2006/00; C01P2006/40; C01P2006/80

Claims Analysis

Total Claims: 15
Claim 1
Independent Claim 33 words
The process of claim 1 wherein said member is passed through the halide while the halide is being raised to the temperature above its melting point and also while the halide is molten.
Claim 2
Dependent Claim 25 words
The process of claim 1 which further comprises passing an inert gas through the molten halide to scrub dissolved gases therefrom prior to step (c).
Claim 3
Dependent Claim 44 words
The process of claim 1 wherein the metal halide is selected from the group consisting of the iodides, bromides and chlorides of the metals of Groups 1a, 2a, 3a, 4a, 1b, 2b, 3b, and the Lanthanide series of the Periodic Table, and mixtures thereof.
Claim 4
Dependent Claim 35 words
The process of claim 4, wherein the metal halide is a solid metal iodide selected from the group consisting of the iodides of the alkali metals, the Lanthanides, mercury, thallium, indium, scandium and mixtures thereof.
Claim 5
Dependent Claim 21 words
The process of claim 1 wherein volatile impurities are evaporated from the metal halide prior to melting of the metal halide.
Claim 6
Dependent Claim 20 words
The process of claim 1 wherein the molten halide is filtered to remove insoluble impurities therefrom prior to step (c).
Claim 7
Dependent Claim 23 words
The process of claim 7 which further comprises evacuating the atmosphere surrounding the metal halide to subatmospheric pressure prior to the melting thereof.
Claim 8
Dependent Claim 48 words
The process of claim 8 wherein the dischaRge nozzle is vibrated at a resonant frequency, and the molten halide is continuously flowed through the conduit into the inert, quenching atmosphere to form particles having an average diameter of from 3 to 5 times the diameter of the conduit.
Claim 9
Dependent Claim 22 words
The process of claim 9 wherein the inert, quenching atmosphere comprises helium and is at a temperature between 0* and 50* C.
Claim 10
Dependent Claim 33 words
The process of claim 1 wherein hydrogen and a halogen are reacted in the presence of a platinum catalyst and the resultant gaseous product is passed through the metal halide in step (b).
Claim 11
Dependent Claim 203 words
A process for producing purified metal halide of controlled particle size from solid metal halide having oxygen-containing impurities therein, which process comprises the steps of: a. evaporating volatile impurities from the solid metal halide: b. passing through the halide at least one member selected from the group consisting of hydrogen halide, an admixture of hydrogen halide and hydrogen, and an admixture of hydrogen and halogen to convert at least a portion of the oxygen-containing impurities other than water present in the metal halide to water and volatile impurities and to remove at least a portion of the water and volatile impurities by scrubbing, the halogen, the halogen radical of the hydrogen halide and the halogen radical of the metal halide being of the same halogen species; c. during passage of the said member through the metal halide, melting the metal halide; d. evacuating dissolved gases from the molten metal halide; e. passing an inert gas through the molten halide to scrub dissolved gases therefrom. f. filtering the molten metal halide to remove insoluble impurities therefrom; and g. passing the filtered molten metal halide through a vibrating discharge nozzle into an inert, quenching atmosphere to form particles of purified metal halide of controlled size.
Claim 12
Dependent Claim 26 words
The process of claim 12 wherein steps (d) and (e) are repeated until substantially all of the dissolved gases in the molten metal halide are removed.
Claim 13
Dependent Claim 18 words
The process of claim 13 wherein said metal halide is a mixture of sodium iodide and scandium iodide.
Claim 14
Dependent Claim 141 words
A process for producing a purified mixture of sodium iodide and scandium iodide in a controlled particle size, which process comprises: a. providing a mixture of sodium iodide and scandium iodide having oxygen-containing impurities; b. melting the iodide mixture; c. passing through the molten iodide mixture at least one member selected from the group consisting of hydrogen iodide, and admixture of hydrogen iodide and hydrogen, and an admixture of hydrogen and iodine to convert at least a portion of the oxygen-containing impurities other than water present in the metal iodide to water and volatile impurities, and to remove at least a portion of water and volatile impurities by scrubbing; d. and passing the molten iodide mixture through a vibrating discharge conduit into an inert, quenching atmosphere to form particles of a purified mixture of sodium and scandium iodide of controlled size.
Claim 15
Dependent Claim 31 words
The process of claim 15 wherein the iodide is a mixture of from about 45 to about 99.99 mole percent sodium iodide and 55 to about 0.01 mole percent scandium iodide.

References Cited (Backward Citations)

US1798166A Cited
US1999873A Cited
US2538345A Cited
US2968833A Cited
US3048887A Cited
US3510546A Cited

USPTO Annuity & Maintenance Windows

Annuity Stage Window Opens Payment Deadline Surcharge Period Until Estimated Fee Status
3.5 Years (Year 4) 1975-07-11 1976-01-10 1976-07-11 $2000.00 Window Closed / Lapsed
7.5 Years (Year 8) 1979-07-11 1980-01-10 1980-07-11 $3760.00 Window Closed / Lapsed
11.5 Years (Year 12) 1983-07-11 1984-01-10 1984-07-11 $7700.00 Window Closed / Lapsed

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