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US4233277A Expired / Lapsed US ⏱️ 0.0 years remaining

Preparing refractory metal boride powder

Assignee: PPG Industries Inc
•
Filing: 1975-02-03
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Granted: 1980-11-11
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Expires: 1995-02-03
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Abstract

Abstract The preparation of refractory metal borides of Group 4b of the Periodic Table of the Elements by reaction in the vapor phase of the corresponding metal halide, e.g., metal chloride, with a boron source reactant in the presence of hydrogen in a reactor is described. Reactants are introduced into a reactant mixing zone containing hydrogen through reactant inlet assembly means. Refractory metal boride product deposits on the exposed surfaces of the reactant inlet assembly means are reduced significantly by introducing metal halide reactant and substantially anhydrous hydrogen halide into the hydrogen stream upstream of the boron source reactant while introducing boron source reactant mixed with inert carrier gas, e.g., argon, into said hydrogen stream downstream of the metal halide and hydrogen halide streams.

Inventors

  • 👤 Robert S. Sheppard

Bibliographic Details

Application Number —
Jurisdiction US
Data Source google_patents
Last Synchronized 2026-10-27 23:28
CPC Classifications
C; C01; C01B; C01B35/00; C01B35/02; C01B35/04

Claims Analysis

Total Claims: 19
Claim 1
Independent Claim 207 words
In the process for preparing refractory metal boride powder selected from the borides of the metals titanium, zirconium and hafnium by gas phase reaction of the corresponding metal halide reactant and boron source reactant selected from the group consisting of boron halide and boron hydride in the presence of hydrogen in a reactor wherein said reactants are introduced into a reactant mixing zone through reactant inlet assembly means and reacted within the reactor to form solid refractory metal boride powder and wherein the metal boride powder tends to deposit and accumulate on the surfaces of the assembly means exposed to said reactants, the improvement which comprises establishing a hydrogen-containing gas stream in close proximity to but spaced from the exposed surfaces of the reactant inlet assembly means, introducing boron source reactant mixed with inert carrier gas into said hydrogen-containing gas stream, introducing metal halide reactant and substantially anhydrous hydrogen halide into said hydrogen-containing gas stream upstream of the boron source reactant, the amount of hydrogen halide introduced being sufficient to retard growth of said metal boride powder on said exposed surfaces of the assembly means, the heat content of the hydrogen-containing gas stream and reactants being sufficient to establish refractory metal boride forming temperatures in said reactor.
Claim 2
Dependent Claim 207 words
In the process for preparing refractory metal boride powder selected from the borides of the metals titanium, zirconium and hafnium by gas phase reaction of the corresponding metal halide reactant and boron source reactant selected from the group consisting of boron halide and boron hydride in the presence of hydrogen in a reactor wherein said reactants are introduced into a reactant mixing zone through reactant inlet assembly means and reacted within the reactor to form solid refractory metal boride powder and wherein the metal boride powder tends to deposit and accumulate on the surfaces of the assembly means exposed to said reactants, the improvement which comprises establishing a hydrogen-containing gas stream in close proximity to but spaced from the exposed surfaces of the reactant inlet assembly means, introducing boron source reactant mixed with inert carrier gas into said hydrogen-containing gas stream, introducing metal halide reactant and substantially anhydrous hydrogen halide into said hydrogen-containing gas stream upstream of the boron source reactant, the amount of hydrogen halide introduced being sufficient to retard growth of said metal boride powder on said exposed surfaces of the assembly means, the heat content of the hydrogen-containing gas stream and reactants being sufficient to establish refractory metal boride forming temperatures in said reactor.
Claim 3
Dependent Claim 18 words
The process of claim 1 wherein the anhydrous hydrogen halide is introduced mixed with the metal halide reactant.
Claim 4
Dependent Claim 20 words
The process of claim 1 wherein the inert carrier gas mixed with the boron source reactant is a noble gas.
Claim 5
Dependent Claim 30 words
The process of claim 1 wherein the amount of anhydrous hydrogen halide used is between about 50 and about 350 mole percent hydrogen halide based on the metal halide reactant.
Claim 6
Dependent Claim 23 words
The process of claim 1 wherein the halide portion of said hydrogen halide corresponds to the halide portion of the metal halide reactant.
Claim 7
Dependent Claim 30 words
The process of claim 1 wherein the metal halide reactant is titanium tetrachloride, the boron source reactant is boron trichloride and the carrier gas for the boron trichloride is argon.
Claim 8
Dependent Claim 17 words
The process of claim 6 wherein a hydrogen carrier gas is used with the titanium tetrahalide reactant.
Claim 9
Dependent Claim 18 words
The process of claim 1 wherein the hydrogen-containing stream is produced by heating hydrogen in plasma heating means.
Claim 10
Dependent Claim 181 words
In the process for preparing submicron finely-divided titanium diboride by gas phase reaction of titanium halide and boron source reactants in the presence of hydrogen in a reactor wherein the reactants are introduced through reactant inlet assembly means into a reactant mixing zone housing a hot hydrogen gas stream and reacted within the reactor to form solid titanium diboride product and wherein the titanium diboride product tends to deposit and accumulate on the surfaces of the assembly means exposed to said reactants, the improvement which comprises the steps of introducing a hot hydrogen gas stream into the reactant mixing zone, introducing titanium tetrahalide reactant and substantially anhydrous hydrogen halide into said hydrogen stream upstream of the boron source reactant, the amount of hydrogen halide being between 50 and 350 mole percent hydrogen halide based on the metal halide reactant, introducing boron source reactant mixed with inert carrier gas into said hydrogen stream, the heat content of the hydrogen stream and the reactants being sufficient to establish titanium diboride forming temperatures in said reactor, and removing solid titanium diboride from the reactor.
Claim 11
Dependent Claim 181 words
In the process for preparing submicron finely-divided titanium diboride by gas phase reaction of titanium halide and boron source reactants in the presence of hydrogen in a reactor wherein the reactants are introduced through reactant inlet assembly means into a reactant mixing zone housing a hot hydrogen gas stream and reacted within the reactor to form solid titanium diboride product and wherein the titanium diboride product tends to deposit and accumulate on the surfaces of the assembly means exposed to said reactants, the improvement which comprises the steps of introducing a hot hydrogen gas stream into the reactant mixing zone, introducing titanium tetrahalide reactant and substantially anhydrous hydrogen halide into said hydrogen stream upstream of the boron source reactant, the amount of hydrogen halide being between 50 and 350 mole percent hydrogen halide based on the metal halide reactant, introducing boron source reactant mixed with inert carrier gas into said hydrogen stream, the heat content of the hydrogen stream and the reactants being sufficient to establish titanium diboride forming temperatures in said reactor, and removing solid titanium diboride from the reactor.
Claim 12
Dependent Claim 20 words
The process of claim 9 wherein the titanium tetrahalide is titanium tetrachloride, and the boron source reactant is boron trichloride.
Claim 13
Dependent Claim 12 words
The process of claim 10 wherein the inert carrier gas is argon.
Claim 14
Dependent Claim 18 words
The process of claim 10 wherein the hydrogen-containing stream is produced by heating hydrogen in plasma heating means.
Claim 15
Dependent Claim 15 words
The process of claim 12 wherein the plasma heating means is an arc plasma heater.
Claim 16
Dependent Claim 12 words
The process of claim 10 wherein the hydrogen halide is hydrogen chloride.
Claim 17
Dependent Claim 17 words
The process of claim 10 wherein a hydrogen carrier gas is used with the titanium tetrachloride reactant.
Claim 18
Dependent Claim 19 words
The process of claim 12 wherein the inert carrier gas is argon and the hydrogen halide is hydrogen chloride.
Claim 19
Dependent Claim 17 words
The process of claim 16 wherein a hydrogen carrier gas is used with the titanium tetrachloride reactant.

References Cited (Backward Citations)

US2768061A Cited
US3253886A Cited
US3340020A Cited
US3455745A Cited
FR1533423A Cited
GB1194415A Cited
US3812239A Cited
US3661523A Cited
US3979500A Cited

USPTO Annuity & Maintenance Windows

Annuity Stage Window Opens Payment Deadline Surcharge Period Until Estimated Fee Status
3.5 Years (Year 4) 1983-11-11 1984-05-12 1984-11-11 $2000.00 Window Closed / Lapsed
7.5 Years (Year 8) 1987-11-11 1988-05-12 1988-11-11 $3760.00 Window Closed / Lapsed
11.5 Years (Year 12) 1991-11-11 1992-05-12 1992-11-11 $7700.00 Window Closed / Lapsed

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