Patent US5372629A successfully refreshed from Google Patents.
US5372629A
Expired / Lapsed
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Method of making environmentally stable reactive alloy powders
Assignee: Iowa State University Research Foundation Inc
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Filing: 1992-08-05
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Granted: 1994-12-13
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Expires: 2012-08-05
Abstract
Abstract Apparatus and method for making powder from a metallic melt by atomizing the melt to form droplets and reacting the droplets downstream of the atomizing location with a reactive gas. The droplets are reacted with the gas at a temperature where a solidified exterior surface is formed thereon and where a protective refractory barrier layer (reaction layer) is formed whose penetration into the droplets is limited by the presence of the solidified surface so as to avoid selective reduction of key reactive alloyants needed to achieve desired powder end use properties. The barrier layer protects the reactive powder particles from environmental constituents such as air and water in the liquid or vapor form during subsequent fabrication of the powder to end-use shapes and during use in the intended service environment.
Inventors
- 👤 Iver E. Anderson
- 👤 Barbara K. Lograsso
- 👤 Robert L. Terpstra
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-11-06 15:17
CPC Classifications
B; B22; B22F; B22F9/00; B22F9/02; B22F9/06; B22F9/08; B22F9/082; B22F1/00; B22F1/14; B22F1/145; B22F1/16; H; H01; H01F; H01F1/00; H01F1/01; H01F1/03; H01F1/032; H01F1/04; H01F1/047; H01F1/053; H01F1/055; H01F1/0551; H01F1/0552; H01F1/057; H01F1/0571; H01F1/0572; H01F1/0574; B22F2998/00; Y; Y10; Y10T; Y10T428/00; Y10T428/29; Y10T428/2982; Y10T428/2991
Claims Analysis
Total Claims: 57
Claim 1
Independent Claim
154 words
A method of making powder from a metallic melt having a composition including a reactive alloying element, comprising the steps of: a) atomizing the melt in a chamber using an atomizing gas that is inert to said melt so as to avoid reaction therewith during atomization and form molten droplets, and b) contacting a reactive gas and the droplets at a downstream location in the chamber relative to the location of melt atomization where at said downstream location the droplets have cooled to a temperature where they have at least a solidified exterior surface and where the reactive gas reacts with said reactive alloying element to form a reaction product layer whose penetration into the droplets is limited by the presence of said solidified surface to not exceed about 500 Angstroms reaction product layer thickness so as to avoid selective removal of the reactive alloying element from the melt composition at the droplet core.
Claim 2
Independent Claim
154 words
A method of making powder from a metallic melt having a composition including a reactive alloying element, comprising the steps of: a) atomizing the melt in a chamber using an atomizing gas that is inert to said melt so as to avoid reaction therewith during atomization and form molten droplets, and b) contacting a reactive gas and the droplets at a downstream location in the chamber relative to the location of melt atomization where at said downstream location the droplets have cooled to a temperature where they have at least a solidified exterior surface and where the reactive gas reacts with said reactive alloying element to form a reaction product layer whose penetration into the droplets is limited by the presence of said solidified surface to not exceed about 500 Angstroms reaction product layer thickness so as to avoid selective removal of the reactive alloying element from the melt composition at the droplet core.
Claim 3
Dependent Claim
40 words
The method of claim 1 wherein in step b, the reactive gas reacts with the reactive alloying element to form an environmentally protective barrier layer on the droplet, said barrier layer comprising a refractory compound of the reactive alloying element.
Claim 4
Dependent Claim
49 words
The method of claim 1 wherein in step b, the droplets are passed through a zone of the reactive gas disposed in the chamber downstream of the location where the melt is atomized, said droplets cooling to said temperature as they pass from the atomization location to said zone.
Claim 5
Dependent Claim
22 words
The method of claim 1 including the additional step of forming in the chamber a carbon-bearing layer on the reaction product layer.
Claim 6
Dependent Claim
16 words
The method of claim 4 wherein a graphite layer is formed on the reaction product layer.
Claim 7
Dependent Claim
27 words
The method of claim 4 wherein the droplets are contacted at an elevated temperature with a gaseous carbonaceous material in the chamber to form said carbon-bearing layer.
Claim 8
Dependent Claim
31 words
The method of claim 1 wherein in step b, the reactive gas and the droplets are contacted when the droplets are solidified from the exterior surface substantially to the droplet core.
Claim 9
Independent Claim
163 words
A method of making powder from a rare earth-transition metal alloy melt having a composition selected to provide desired powder magnetic properties, comprising the steps of: a) atomizing the rare earth-transition metal alloy melt in a chamber using an atomizing gas that is inert to said melt so as to avoid reaction therewith during atomization and form molten droplets, and b) contacting a reactive gas and the droplets at a downstream location in the chamber relative to the location of melt atomization where at said downstream location the droplets have cooled to a temperature where they have at least a solidified exterior surface and where the reactive gas reacts with said rare earth element to form a reaction product layer whose penetration into the droplets is limited by the presence of said solidified surface to not exceed about 500 Angstroms reaction product layer thickness so as to avoid selective removal of the rare earth element from said melt composition at the droplet core.
Claim 10
Independent Claim
163 words
A method of making powder from a rare earth-transition metal alloy melt having a composition selected to provide desired powder magnetic properties, comprising the steps of: a) atomizing the rare earth-transition metal alloy melt in a chamber using an atomizing gas that is inert to said melt so as to avoid reaction therewith during atomization and form molten droplets, and b) contacting a reactive gas and the droplets at a downstream location in the chamber relative to the location of melt atomization where at said downstream location the droplets have cooled to a temperature where they have at least a solidified exterior surface and where the reactive gas reacts with said rare earth element to form a reaction product layer whose penetration into the droplets is limited by the presence of said solidified surface to not exceed about 500 Angstroms reaction product layer thickness so as to avoid selective removal of the rare earth element from said melt composition at the droplet core.
Claim 11
Dependent Claim
39 words
The method of claim 8 wherein in step b, the reactive gas reacts with the rare earth to form an environmentally protective barrier layer on the droplet, said barrier layer comprising a refractory compound of the reactive alloying element.
Claim 12
Dependent Claim
49 words
The method of claim 8 wherein in step b, the droplets are passed through a zone of the reactive gas disposed in the chamber downstream of the location where the melt is atomized, said droplets cooling to said temperature as they pass from the atomization location to said zone.
Claim 13
Dependent Claim
21 words
The method of claim 8 including the additional step of forming in the chamber carbon-bearing layer on the reaction product layer.
Claim 14
Dependent Claim
16 words
The method of claim 11 wherein a graphite layer is formed on the reaction product layer.
Claim 15
Dependent Claim
26 words
The method of claim 11 wherein the droplets are contacted at elevated temperature with a gaseous carbonaceous material in the chamber to form said carbon-bearing layer.
Claim 16
Dependent Claim
30 words
The method of claim 8 wherein in step b, the reactive gas and the droplets are contacted when the droplets are solidified from the exterior surface to the droplet core.
Claim 17
Independent Claim
171 words
A method of making powder from a rare earth-iron-boron alloy melt having a composition selected to provide desired powder magnetic properties, comprising the steps of: a) atomizing the rare earth-iron-boron alloy melt in a chamber using an atomizing gas that is inert to said melt so as to avoid reaction therewith during atomization and form molten droplets, and b) contacting a reactive gas and the droplets at a downstream location in the chamber relative to the location of melt atomization where at said downstream location the droplets have cooled to a temperature where they have at least a solidified exterior surface and where the reactive gas reacts with at least one of said rare earth and said boron to form a reaction product layer whose penetration into the droplets is limited in surface depth by the presence of said solidified surface to not exceed about 500 Angstroms reaction product layer thickness so as to avoid selective removal of the rare earth and boron from said melt composition at the droplet core.
Claim 18
Independent Claim
171 words
A method of making powder from a rare earth-iron-boron alloy melt having a composition selected to provide desired powder magnetic properties, comprising the steps of: a) atomizing the rare earth-iron-boron alloy melt in a chamber using an atomizing gas that is inert to said melt so as to avoid reaction therewith during atomization and form molten droplets, and b) contacting a reactive gas and the droplets at a downstream location in the chamber relative to the location of melt atomization where at said downstream location the droplets have cooled to a temperature where they have at least a solidified exterior surface and where the reactive gas reacts with at least one of said rare earth and said boron to form a reaction product layer whose penetration into the droplets is limited in surface depth by the presence of said solidified surface to not exceed about 500 Angstroms reaction product layer thickness so as to avoid selective removal of the rare earth and boron from said melt composition at the droplet core.
Claim 19
Dependent Claim
45 words
The method of claim 15 wherein in step b, the reactive gas reacts with at least one of said rare earth and boron to form an environmentally protective barrier layer on the droplet, said barrier layer comprising a refractory compound of the reactive alloying element.
Claim 20
Dependent Claim
49 words
The method of claim 15 wherein in step b, the droplets are passed through a zone of the reactive gas disposed in the chamber downstream of the location where the melt is atomized, said droplets cooling to said temperature as they pass from the atomization location to said zone.
Claim 21
Dependent Claim
22 words
The method of claim 15 including the additional step of forming in the chamber a carbon-bearing layer on the reaction product layer.
Claim 22
Dependent Claim
16 words
The method of claim 18 wherein a graphite layer is formed on the reaction product layer.
Claim 23
Dependent Claim
27 words
The method of claim 18 wherein the droplets are contacted at an elevated temperature with a gaseous carbonaceous material in the chamber to form said carbon-bearing layer.
Claim 24
Dependent Claim
30 words
The method of claim 15 wherein in step b, the reactive gas and the droplets are contacted when the droplets are solidified from the exterior surface to the droplet core.
Claim 25
Independent Claim
175 words
A method of making powder from a melt having a composition including a reactive alloying element, comprising the steps of: a) atomizing the melt into molten droplets in a drop tube using an atomizing gas that is inert to said melt so as to avoid reaction therewith during atomization allowing for free fall of said droplets downwardly through the tube and cooling of said droplets as they fall, and b) establishing a zone of reactive gas in the tube downstream of the atomizing location where the droplet temperature is so reduced from said cooling that said droplets have at least a solidified exterior shell thereon and that the reactive gas reacts with the reactive alloying element as the droplets pass through the zone to form a reaction product layer thereon whose penetration into the droplets is limited in surface depth by the presence of said shell to not exceed about 500 Angstroms reaction product layer thickness so as to avoid selective removal of the reactive alloying element from said melt composition at the droplet core.
Claim 26
Independent Claim
175 words
A method of making powder from a melt having a composition including a reactive alloying element, comprising the steps of: a) atomizing the melt into molten droplets in a drop tube using an atomizing gas that is inert to said melt so as to avoid reaction therewith during atomization allowing for free fall of said droplets downwardly through the tube and cooling of said droplets as they fall, and b) establishing a zone of reactive gas in the tube downstream of the atomizing location where the droplet temperature is so reduced from said cooling that said droplets have at least a solidified exterior shell thereon and that the reactive gas reacts with the reactive alloying element as the droplets pass through the zone to form a reaction product layer thereon whose penetration into the droplets is limited in surface depth by the presence of said shell to not exceed about 500 Angstroms reaction product layer thickness so as to avoid selective removal of the reactive alloying element from said melt composition at the droplet core.
Claim 27
Dependent Claim
40 words
The method of claim 22 wherein in step b, the reactive gas reacts with the reactive alloying element to form an environmentally protective barrier layer on the droplet, said barrier layer comprising a refractory compound of the reactive alloying element.
Claim 28
Dependent Claim
16 words
The method of claim 22 wherein the melt is inert gas pressure atomized in step a.
Claim 29
Dependent Claim
28 words
The method of claim 22 wherein in step b, the droplets are passed through the zone when said droplets are solidified from the exterior surface to the core.
Claim 30
Dependent Claim
38 words
The method of claim 22 further including contacting the droplets at elevated temperature with a gaseous carbonaceous material in the chamber after formation of the reaction product layer to form a carbon-bearing layer on the reaction product layer.
Claim 31
Dependent Claim
16 words
The method of claim 26 wherein a graphite layer is formed on the reaction product layer.
Claim 32
Independent Claim
105 words
A method of making powder from a metallic melt having a composition including a reactive alloying element, comprising the steps of: a) atomizing the melt in a chamber using an atomizing gas that is inert to said melt so as to avoid reaction therewith during atomization and form molten droplets, and b) forming a reaction product layer not exceeding about 500 Angstroms in thickness on the droplets by reacting the reactive alloying element and a reactive gas at a downstream location in the chamber relative to the location of melt atomization where at the downstream location, the droplets have at least a solidified exterior shell.
Claim 33
Independent Claim
105 words
A method of making powder from a metallic melt having a composition including a reactive alloying element, comprising the steps of: a) atomizing the melt in a chamber using an atomizing gas that is inert to said melt so as to avoid reaction therewith during atomization and form molten droplets, and b) forming a reaction product layer not exceeding about 500 Angstroms in thickness on the droplets by reacting the reactive alloying element and a reactive gas at a downstream location in the chamber relative to the location of melt atomization where at the downstream location, the droplets have at least a solidified exterior shell.
Claim 34
Independent Claim
102 words
A method of making powder from a rare earth-transition metal alloy melt, comprising the steps of: a) atomizing the melt in a chamber using an atomizing gas that is inert to said melt so as to avoid reaction therewith during atomization and form molten droplets, and b) forming a reaction product layer not exceeding about 500 Angstroms in thickness on the droplets by reacting the rare earth of the alloy and a reactive gas at a downstream location in the chamber relative to the location of melt atomization where at the downstream location, the droplets have at least a solidified exterior shell.
Claim 35
Independent Claim
102 words
A method of making powder from a rare earth-transition metal alloy melt, comprising the steps of: a) atomizing the melt in a chamber using an atomizing gas that is inert to said melt so as to avoid reaction therewith during atomization and form molten droplets, and b) forming a reaction product layer not exceeding about 500 Angstroms in thickness on the droplets by reacting the rare earth of the alloy and a reactive gas at a downstream location in the chamber relative to the location of melt atomization where at the downstream location, the droplets have at least a solidified exterior shell.
Claim 36
Independent Claim
80 words
A method of making powder from a metallic melt having a composition including a reactive alloying element, comprising the steps of: a) atomizing the melt in a chamber using an atomizing gas so as to form droplets, b) forming a reaction product layer on the droplets by reacting a reactive gas in the chamber and the reactive alloying element, and c) forming a carbon-bearing layer on the reaction product layer by contacting a gaseous carbonaceous material in the chamber therewith.
Claim 37
Independent Claim
80 words
A method of making powder from a metallic melt having a composition including a reactive alloying element, comprising the steps of: a) atomizing the melt in a chamber using an atomizing gas so as to form droplets, b) forming a reaction product layer on the droplets by reacting a reactive gas in the chamber and the reactive alloying element, and c) forming a carbon-bearing layer on the reaction product layer by contacting a gaseous carbonaceous material in the chamber therewith.
Claim 38
Independent Claim
75 words
A method of making powder from a rare earth-transition metal alloy melt, comprising the steps of: a) atomizing the melt in a chamber using an atomizing gas that is inert to said melt, b) forming a reaction product layer on the droplets by reacting a reactive gas in the chamber and the rare earth, and c) forming a carbon-bearing layer on the reaction product layer by contacting a gaseous carbonaceous material in the chamber therewith.
Claim 39
Independent Claim
75 words
A method of making powder from a rare earth-transition metal alloy melt, comprising the steps of: a) atomizing the melt in a chamber using an atomizing gas that is inert to said melt, b) forming a reaction product layer on the droplets by reacting a reactive gas in the chamber and the rare earth, and c) forming a carbon-bearing layer on the reaction product layer by contacting a gaseous carbonaceous material in the chamber therewith.
Claim 40
Independent Claim
75 words
A method of making powder from a rare earth-iron-boron melt, comprising the steps of: a) atomizing the melt in a chamber using an atomizing gas that is inert to said melt, b) forming a reaction product layer on the droplets by reacting a reactive gas in the chamber and the rare earth and boron, and c) forming a carbon-bearing layer on the reaction product layer by contacting a gaseous carbonaceous material in the chamber therewith.
Claim 41
Independent Claim
75 words
A method of making powder from a rare earth-iron-boron melt, comprising the steps of: a) atomizing the melt in a chamber using an atomizing gas that is inert to said melt, b) forming a reaction product layer on the droplets by reacting a reactive gas in the chamber and the rare earth and boron, and c) forming a carbon-bearing layer on the reaction product layer by contacting a gaseous carbonaceous material in the chamber therewith.
Claim 42
Independent Claim
167 words
A method of making powder from a metallic melt having a composition including a reactive alloying element, comprising the steps of: a) atomizing the melt in a chamber using an atomizing gas that is inert to said melt so as to avoid reaction therewith during atomization and form molten droplets, b) contacting a reactive gas and the droplets at a downstream location in the chamber relative to the location of melt atomization where at said downstream location the droplets have cooled to a temperature where they have at least a solidified exterior surface and where the reactive gas reacts with said reactive alloying element to form a reaction product layer whose penetration into the droplets is limited by the presence of said solidified surface to not exceed about 500 Angstroms reaction product layer thickness so as to avoid selective removal of the reactive alloying element from the melt composition at the droplet core, and c) forming in the chamber a carbon-bearing layer on the reaction product layer.
Claim 43
Independent Claim
167 words
A method of making powder from a metallic melt having a composition including a reactive alloying element, comprising the steps of: a) atomizing the melt in a chamber using an atomizing gas that is inert to said melt so as to avoid reaction therewith during atomization and form molten droplets, b) contacting a reactive gas and the droplets at a downstream location in the chamber relative to the location of melt atomization where at said downstream location the droplets have cooled to a temperature where they have at least a solidified exterior surface and where the reactive gas reacts with said reactive alloying element to form a reaction product layer whose penetration into the droplets is limited by the presence of said solidified surface to not exceed about 500 Angstroms reaction product layer thickness so as to avoid selective removal of the reactive alloying element from the melt composition at the droplet core, and c) forming in the chamber a carbon-bearing layer on the reaction product layer.
Claim 44
Dependent Claim
16 words
The method of claim 33 wherein a graphite layer is formed on the reaction product layer.
Claim 45
Dependent Claim
27 words
The method of claim 33 wherein the droplets are contacted at an elevated temperature with a gaseous carbonaceous material in the chamber to form said carbon-bearing layer.
Claim 46
Independent Claim
176 words
A method of making powder from a rare earth-transition metal alloy melt having a composition selected to provide desired powder magnetic properties, comprising the steps of: a) atomizing the rare earth-transition metal alloy melt in a chamber using an atomizing gas that is inert to said melt so as to avoid reaction therewith during atomization and form molten droplets, b) contacting a reactive gas and the droplets at a downstream location in the chamber relative to the location of melt atomization where at said downstream location the droplets have cooled to a temperature where they have at least a solidified exterior surface and where the reactive gas reacts with said rare earth element to form a reaction product layer whose penetration into the droplets is limited by the presence of said solidified surface to not exceed about 500 Angstroms reaction product layer thickness so as to avoid selective removal of the rare earth element from said melt composition at the droplet core, and c) forming in the chamber a carbon-bearing layer on the reaction product layer.
Claim 47
Independent Claim
176 words
A method of making powder from a rare earth-transition metal alloy melt having a composition selected to provide desired powder magnetic properties, comprising the steps of: a) atomizing the rare earth-transition metal alloy melt in a chamber using an atomizing gas that is inert to said melt so as to avoid reaction therewith during atomization and form molten droplets, b) contacting a reactive gas and the droplets at a downstream location in the chamber relative to the location of melt atomization where at said downstream location the droplets have cooled to a temperature where they have at least a solidified exterior surface and where the reactive gas reacts with said rare earth element to form a reaction product layer whose penetration into the droplets is limited by the presence of said solidified surface to not exceed about 500 Angstroms reaction product layer thickness so as to avoid selective removal of the rare earth element from said melt composition at the droplet core, and c) forming in the chamber a carbon-bearing layer on the reaction product layer.
Claim 48
Dependent Claim
16 words
The method of claim 36 wherein a graphite layer is formed on the reaction product layer.
Claim 49
Dependent Claim
27 words
The method of claim 36 wherein the droplets are contacted at an elevated temperature with a gaseous carbonaceous material in the chamber to form said carbon-bearing layer.
Claim 50
Independent Claim
184 words
A method of making powder from a rare earth-iron-boron alloy melt having a composition selected to provide desired powder magnetic properties, comprising the steps of: a) atomizing the rare earth-iron-boron alloy melt in a chamber using an atomizing gas that is inert to said melt so as to avoid reaction therewith during atomization and form molten droplets, b) contacting a reactive gas and the droplets at a downstream location in the chamber relative to the location of melt atomization where at said downstream location the droplets have cooled to a temperature where they have at least a solidified exterior surface and where the reactive gas reacts with at least one of said rare earth and said boron to form a reaction product layer whose penetration into the droplets is limited in surface depth by the presence of said solidified surface to not exceed about 500 Angstroms reaction product layer thickness so as to avoid selective removal of the rare earth and boron from said melt composition at the droplet core, and c) forming in the chamber a carbon-bearing layer on the reaction product layer.
Claim 51
Independent Claim
184 words
A method of making powder from a rare earth-iron-boron alloy melt having a composition selected to provide desired powder magnetic properties, comprising the steps of: a) atomizing the rare earth-iron-boron alloy melt in a chamber using an atomizing gas that is inert to said melt so as to avoid reaction therewith during atomization and form molten droplets, b) contacting a reactive gas and the droplets at a downstream location in the chamber relative to the location of melt atomization where at said downstream location the droplets have cooled to a temperature where they have at least a solidified exterior surface and where the reactive gas reacts with at least one of said rare earth and said boron to form a reaction product layer whose penetration into the droplets is limited in surface depth by the presence of said solidified surface to not exceed about 500 Angstroms reaction product layer thickness so as to avoid selective removal of the rare earth and boron from said melt composition at the droplet core, and c) forming in the chamber a carbon-bearing layer on the reaction product layer.
Claim 52
Dependent Claim
16 words
The method of claim 39 wherein a graphite layer is formed on the reaction product layer.
Claim 53
Dependent Claim
27 words
The method of claim 39 wherein the droplets are contacted at an elevated temperature with a gaseous carbonaceous material in the chamber to form said carbon-bearing layer.
Claim 54
Independent Claim
182 words
A method of making powder from a melt having a composition including a reactive alloying element, comprising the steps of: a) atomizing the melt into molten droplets in a drop tube using an atomizing gas that is inert to said melt to avoid reaction therewith during atomization for free fall of said droplets downwardly through the tube and cooling as they fall, b) establishing a zone of reactive gas in the tube downstream of the atomizing location where the droplet temperature is so reduced from said cooling that said droplets have at least a solidified exterior shell thereon and that the reactive gas reacts with the reactive alloying element as the droplets pass through the zone to form a reaction product layer thereon whose penetration into the droplets is limited in surface depth by the presence of said shell to not exceed about 500 Angstroms reaction product layer thickness so as to avoid selective removal of the reactive alloying element from said melt composition at the droplet core, and c) forming in the chamber a carbon-bearing layer on the reaction product layer.
Claim 55
Independent Claim
182 words
A method of making powder from a melt having a composition including a reactive alloying element, comprising the steps of: a) atomizing the melt into molten droplets in a drop tube using an atomizing gas that is inert to said melt to avoid reaction therewith during atomization for free fall of said droplets downwardly through the tube and cooling as they fall, b) establishing a zone of reactive gas in the tube downstream of the atomizing location where the droplet temperature is so reduced from said cooling that said droplets have at least a solidified exterior shell thereon and that the reactive gas reacts with the reactive alloying element as the droplets pass through the zone to form a reaction product layer thereon whose penetration into the droplets is limited in surface depth by the presence of said shell to not exceed about 500 Angstroms reaction product layer thickness so as to avoid selective removal of the reactive alloying element from said melt composition at the droplet core, and c) forming in the chamber a carbon-bearing layer on the reaction product layer.
Claim 56
Dependent Claim
16 words
The method of claim 42 wherein a graphite layer is formed on the reaction product layer.
Claim 57
Dependent Claim
27 words
The method of claim 42 wherein the droplets are contacted at an elevated temperature with a gaseous carbonaceous material in the chamber to form said carbon-bearing layer.
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