U.S. patent application number 12/386073 was filed with the patent office on 2009-08-13 for preparation of alloys by the armstrong method.
Invention is credited to Richard Paul Anderson, Donn Reynolds Armstrong, Lance E. Jacobsen.
Application Number | 20090202385 12/386073 |
Document ID | / |
Family ID | 31978706 |
Filed Date | 2009-08-13 |
United States Patent
Application |
20090202385 |
Kind Code |
A1 |
Armstrong; Donn Reynolds ;
et al. |
August 13, 2009 |
Preparation of alloys by the armstrong method
Abstract
A method and apparatus for making alloys or ceramics by the
subsurface injection of an equilibrium vapor of a boiling liquid of
the ceramic or alloys constituents is disclosed. Various powders
and products are disclosed.
Inventors: |
Armstrong; Donn Reynolds;
(Lisle, IL) ; Anderson; Richard Paul; (Clarendon
Hills, IL) ; Jacobsen; Lance E.; (Minooka,
IL) |
Correspondence
Address: |
DUNLAP CODDING, P.C. - CRISTAL
P.O. BOX 16370
OKLAHOMA CITY
OK
73113
US
|
Family ID: |
31978706 |
Appl. No.: |
12/386073 |
Filed: |
April 14, 2009 |
Related U.S. Patent Documents
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Application
Number |
Filing Date |
Patent Number |
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11372660 |
Mar 10, 2006 |
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12386073 |
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10654493 |
Sep 3, 2003 |
7041150 |
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11372660 |
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60408934 |
Sep 7, 2002 |
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Current U.S.
Class: |
420/417 ;
266/166 |
Current CPC
Class: |
C01B 21/06 20130101;
B22F 9/28 20130101; C22B 34/1272 20130101 |
Class at
Publication: |
420/417 ;
266/166 |
International
Class: |
C22C 14/00 20060101
C22C014/00; C22B 9/00 20060101 C22B009/00 |
Claims
1. A powder made by the exothermic subsurface reduction of a mixed
halide vapor comprising principally a titanium halide and an amount
of a halide of at least one other element in a preselected atomic
ratio with a liquid reductant metal comprising liquid alkali or
alkaline earth metal or mixtures thereof, wherein the mixed halide
vapor is generated by boiling a liquid mixture of halides until an
equilibrium vapor is attained, and thereafter introducing the
equilibrium vapor into the liquid reductant metal to form the
powder comprising principally titanium and an amount of the at
least one other element in the preselected atomic ratio.
2. The powder of claim 1, wherein the at least one other element is
B.
3. The powder of claim 2, wherein the powder is a titanium alloy
powder and the at least one other element further includes one or
more elements selected from the group consisting of Al, Sb, Be, Ta,
Zr, V, Nb, Mo, Ga, U, Re and Si.
4. The powder of claim 3, wherein the titanium alloy powder
includes Al and V.
5. The powder of claim 4, wherein the alloy powder is substantially
6% Al and 4% V with the remainder substantially Ti.
6. The powder of claim 1, wherein the liquid reductant metal is Na
or Mg.
7. The powder of claim 1, wherein the halide is a chloride.
8. The powder of claim 1, wherein the liquid reductant metal is
present in excess of the stoichiometric amount.
9. The powder of claim 8, wherein the liquid reductant metal is
present as a flowing stream.
10. The powder of claim 1; wherein the equilibrium vapor is
introduced into the liquid reductant metal by subsurface injection
at greater than sonic velocity.
11. A solid produced from the powder of claim 1.
12. An apparatus for producing a powder by the exothermic
subsurface reduction of a mixed halide vapor comprising principally
a titanium halide and an amount of a halide of at least one other
element in a preselected atomic ratio with a liquid reductant metal
comprising liquid alkali metal or alkaline earth metal or mixtures
thereof, the apparatus comprising: a storage container for storing
the liquid reductant metal, halide containers for storing each of
the titanium halide and the halide of the at least one other
element in liquid form, a boiler in communication with each of the
halide containers, wherein the titanium halide and the halide of
the at least one other element are transferred in a preselected
atomic ratio to the boiler to form a liquid mixture of halides,
heating mechanism in heat exchange relationship with the boiler to
generate an equilibrium vapor from the liquid mixture of halides, a
reactor in communication with the boiler and the storage container
for the liquid reductant metal, wherein the liquid reductant metal
is transferred from the storage container to the reactor, and
injection mechanism for subsurface injecting the equilibrium vapor
from the boiler into the liquid reductant metal in the reactor to
produce the powder in the preselected atomic ratios.
13. The apparatus of claim 12, wherein the at least one other
element is B.
14. The apparatus of claim 13, wherein the powder is a titanium
alloy powder and the at least one other element further includes
one or more elements selected from the group consisting of Al, Sb,
Be, Ta, Zr, V, Nb, Mo, Ga, U, Re and Si.
15. The apparatus of claim 14, wherein the titanium alloy powder
includes Al and V.
16. The apparatus of claim 15, wherein the alloy powder is
substantially 6% Al and 4% V with the remainder substantially
Ti.
17. The apparatus of claim 12, wherein the liquid reductant metal
is Na or Mg.
18. The apparatus of claim 12, wherein the halide is a
chloride.
19. The apparatus of claim 12, wherein the liquid reductant metal
in the reactor is present in excess of the stoichiometric
amount.
20. The apparatus of claim 19, wherein the liquid reductant metal
in the reactor is present as a flowing stream.
21. The apparatus of claim 12, wherein the equilibrium vapor is
injected into the liquid reductant metal at greater than sonic
velocity.
Description
CROSS REFERENCE TO RELATED APPLICATIONS
[0001] This application is a continuation of U.S. Ser. No.
11/372,660, filed Mar. 10, 2006; which is a divisional of U.S. Ser.
No. 10/654,493, filed Sep. 3, 2003, now U.S. Pat. No. 7,041,150;
which application pursuant to 37 C.F.R. 1.78(c), claims priority
based on provisional application U.S. Ser. No. 60/408,934, filed
Sep. 7, 2002; the entire disclosures of each of these applications
are hereby expressly incorporated herein by reference.
BACKGROUND OF THE INVENTION
[0002] This invention relates to the Armstrong process as described
in U.S. Pat. Nos. 5,779,761, 5,958,106 and 6,409,797, the
disclosures of each of which is incorporated herein by reference.
As disclosed in the above-three patents, alloys or ceramics can be
prepared by establishing a mixture of gases which are fed, as
disclosed in the above referenced patents, subsurface to a reducing
metal thereby to initiate the reduction of the gas mixture to the
corresponding alloy or ceramic. In general, the most obvious way to
provide the mixed vapor is to introduce the constituent vapors in
the required atomic ratio to a manifold and feed the mixed material
to the reducing metal.
[0003] The present invention relates to another means for mixing
the alloy or ceramic constituents prior to the introduction of the
mixed vapor to the reducing metal. In the present invention, the
various constituents of the alloy or ceramic are initially mixed as
a liquid which is thereafter boiled. After the liquid is boiled and
reaches equilibrium, the vapor coming off the liquid has the same
atomic ratio as the feed liquid to the boiler, which may or may not
be different than the liquid in the boiler. At steady state, the
vapor from the boiler can be fed to the Armstrong process in the
same manner as illustrated in the three referenced patents to
produce an alloy or ceramic having a constant atomic ratio.
[0004] This invention simplifies the handling of materials,
particularly those materials such as aluminum chloride which
sublimate rather than boil. For those materials, the solid is
heated in a vessel under pressure so that a liquid is formed and
that liquid is thereafter transmitted to a boiler, as will be
shown. By way of example, a boiler having feed streams of aluminum
chloride and vanadium chloride and titanium chloride in atomic
ratios of 6% Al and 4% V and the remainder Ti will produce at
equilibrium a vapor of 6% Al, 4% V and 90% Ti, even if the atomic
ratios of the constituents of the liquid in the boiler differ.
Using the equilibrium vapor as a feed in the process disclosed in
the referenced patents produces a 6% Al, 4% V, titanium alloy.
[0005] The invention applies to a wide variety of alloys or
ceramics and simplifies the materials handling of the constituent
parts of each alloy produced in the Armstrong Process.
SUMMARY OF THE INVENTION
[0006] Accordingly, an object of the present invention is to
provide a method and apparatus of producing an alloy or ceramic in
which the liquid constituents thereof are fed into a boiler. The
equilibrium vapor therefrom is thereafter used in the subsurface
reduction with a liquid alkali or alkaline earth metal to form the
alloy or ceramic.
[0007] Yet another object of the present invention is to provide a
method of producing an alloy or ceramic by the exothermic
subsurface reduction of a mixed halide vapor of the alloy or
ceramic constituents with liquid alkali or alkaline earth metal or
mixtures thereof, comprising providing a liquid mixture of halides
of the alloy or ceramic constituents in a preselected atomic ratio,
boiling the liquid until an equilibrium with the vapor is attained,
and thereafter introducing the equilibrium vapor into the liquid
reductant metal to form an alloy or ceramic powder of the
equilibrium vapor constituents in the preselected atomic ratio.
[0008] Still a further object of the present invention is to
provide a method of producing an alloy by the exothermic subsurface
reduction of a mixed halide vapor of the alloy constituents with
liquid alkali or alkaline earth metal or mixtures thereof,
comprising providing a liquid mixture of halides of the alloy
constituents in a preselected atomic ratio, boiling the liquid
until an equilibrium with the vapor is attained, and thereafter
injecting the equilibrium vapor into the liquid reductant metal at
greater than sonic velocity to form an alloy powder of the
equilibrium vapor constituents in the preselected atomic ratio.
[0009] Another object of the present invention is to provide an
apparatus for practicing the method hereinbefore discussed.
[0010] The invention consists of certain novel features and a
combination of parts hereinafter fully described, illustrated in
the accompanying drawings, and particularly pointed out in the
appended claims, it being understood that various changes in the
details may be made without departing from the spirit, or
sacrificing any of the advantages of the present invention.
BRIEF DESCRIPTION OF THE DRAWINGS
[0011] For the purpose of facilitating an understanding of the
invention, illustrated in the accompanying drawings is a preferred
embodiment thereof, from an inspection of which, when considered in
connection with the following description, the invention, its
construction and operation, and many of its advantages should be
readily understood and appreciated.
[0012] FIG. 1 is a schematic representation of the apparatus and
system for practicing the method of the present invention.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT
[0013] FIG. 1 illustrates a system 10 having a reactor 15 in
communication with a source 20 of liquid reductant metal connected
to the reactor by a pipe 21.
[0014] A boiler 25 has therein a liquid 26 which when boiled
produces at equilibrium a vapor 27 which is introduced via pipe 30
into the pipe 21 preferably but not necessarily carrying a flowing
stream the liquid metal from the source thereof 20, thereby
producing a slurry 40 of the same type, consisting of excess liquid
metal, ceramic or metal powder and a salt produced during the
reaction as discussed in the above referenced Armstrong et al.
patents.
[0015] The boiler 25 is provided with a heat source such as coils
28 and is connected or in communication with a plurality of sources
of the constituents of the ultimately produced alloy or ceramic,
three such sources 35, 36, and 37 being illustrated.
[0016] The advantage of the present invention is that during the
production of a ceramic or an alloy by the Armstrong method, liquid
handling is frequently easier and more efficacious than handling
vapors. To this end, representative constituent sources 35, 36 and
37 can each be a vessel (pressurized or not) in which the
individual constituent halide is maintained as a liquid and
thereafter transferred in a suitable, predetermined, atomic ratio
into the boiler 25. The atomic ratio of the constituents from each
of the sources 35, 36 and 37 determines the atomic ratio of the
constituents in the vapor 27 at equilibrium with the liquid 26.
Thereafter, the equilibrium vapor 27 in the preselected and
predetermined atomic ratios is injected subsurface into a stream of
liquid metal at greater than sonic velocity, as is taught in the
above-referenced Armstrong patents.
[0017] Although the reductant metal may be any suitable alkali or
alkaline earth metal or mixtures thereof, the preferred reductant
metal is sodium or magnesium, the most preferred reductant metal
being sodium. Although a variety of halides may be used, the
preferred halide is a chloride due to availability and cost.
Although frequently described with respect to titanium, the
invention is in fact applicable to a wide variety of alloys and
ceramics, particularly ceramics including a nitride, a carbide, or
a boride or mixtures thereof. In addition, many alloys may be
produced by the method and apparatus of the subject invention,
particularly those alloys or ceramics that include one or more of
Ti, Al, Sb, Be, B, Ta, Zr, V, Nb, Mo, Ga, U, Re, or Si. More
preferably, alloys or ceramics are produced which include one or
more of Ti, Al, Ta, Zr, V, Nb, Mo, Ga, Re, or Si.
[0018] Moreover, the powder ceramics or alloys produced by the
method and apparatus of the present invention are useful in a wide
variety of processes to make many different products. For instance,
various powder metallurgy techniques may be used to produce product
from the powder made by the method and apparatus of the present
invention. Moreover, a wide variety of alloy and ceramic powders
may be either melted or compressed to form a solid from the powder
of the present invention. A particularly important alloy at the
present time is the 6:4 alloy of titanium. This alloy is widely
used in aerospace and defense and is substantially 6% aluminum and
4% vanadium with the remainder being substantially titanium.
[0019] As taught in the cited Armstrong et al. patents, the
reductant metal is generally present in excess of the
stoichiometric amount needed to reduce the mixed halide vapor
injected subsurface of the reductant metal. More particularly, when
the reductant metal is present in the range of from about 20 to
about 50 times the stoichiometric amount, which enables the entire
steady state reaction to be maintained at or around 400.degree. C.,
an advantageous and mostly preferred temperature occurs. The exact
temperature at which the steady state reaction is maintained
depends, in part, upon the ratio of halide to reductant metal, as
well as the individual vapors being reduced and the reductant
metals used to reduce same. It is within the skill of the art to
calculate the exact ratios required to provide a predetermined
steady state operating temperature for the process producing any of
the wide variety of ceramics or alloys made by the method and
apparatus of the present invention.
[0020] As previously stated, although the examples herein are
discussed with respect to titanium or titanium alloys, a wide
variety of alloys and ceramics may be made by the present
invention. It is intended to cover in the claims appended hereto,
all such alloy and ceramics particularly, but not exclusively, the
nitride, boride or carbide ceramics. Representative alloys of the
present invention are those which include one or more of Ti, Al,
Sb, Be, B, Ta, Zr, V, Nb, Mo, Ga, U, Re, or Si and, most
preferably, one or more of Ti, Al, Ta, Zr, V, Nb, Mo, Ga, Re, or
Si.
[0021] While there has been disclosed what is considered to be the
preferred embodiment of the present invention, it is understood
that various changes in the details may be made without departing
from the spirit, or sacrificing any of the advantages of the
present invention.
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