U.S. patent number 3,750,741 [Application Number 05/105,719] was granted by the patent office on 1973-08-07 for method for improved extrusion of essentially inviscid jets.
Invention is credited to Lawrence F. Rakestraw.
United States Patent |
3,750,741 |
Rakestraw |
August 7, 1973 |
METHOD FOR IMPROVED EXTRUSION OF ESSENTIALLY INVISCID JETS
Abstract
High density, high purity polycrystalline and single crystal
beryllium oxide orifice plates have been successfully employed in
wire manufacturing processes which comprise spinning molten metals
through fine diameter orifices as molten metallic jets.
Inventors: |
Rakestraw; Lawrence F.
(Raleigh, NC) |
Family
ID: |
26802879 |
Appl.
No.: |
05/105,719 |
Filed: |
January 11, 1971 |
Related U.S. Patent Documents
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Application
Number |
Filing Date |
Patent Number |
Issue Date |
|
|
845336 |
Jul 28, 1969 |
3584678 |
|
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Current U.S.
Class: |
164/462;
164/138 |
Current CPC
Class: |
B22D
11/005 (20130101); C03B 37/083 (20130101); D01D
4/022 (20130101); C04B 35/08 (20130101) |
Current International
Class: |
C04B
35/01 (20060101); D01D 4/00 (20060101); D01D
4/02 (20060101); B22D 11/00 (20060101); C04B
35/08 (20060101); C03B 37/00 (20060101); C03B
37/083 (20060101); B22d 011/00 (); B22c
001/00 () |
Field of
Search: |
;164/66,82,138,273R
;264/176F |
References Cited
[Referenced By]
U.S. Patent Documents
Primary Examiner: Annear; R. Spencer
Parent Case Text
This is a division of application Ser. No. 845,336, filed July 28,
1969.
Claims
I claim:
1. In a process for the manufacture of fine diameter steel or
copper wire directly from a molten metallic charge which comprises
spinning a molten metallic charge under pressure through a fine
diameter orifice, the improvement which comprises passing said
molten metallic charge through an orifice defined by single crystal
beryllium oxide or polycrystalline beryllium oxide having a purity
of at least 99.5 percent and a density greater than 95 percent of
the theoretical density for beryllium oxide.
2. The improvement of claim 1 wherein the molten metallic charge is
maintained at a temperature greater than 1,000.degree. C.
3. The improvement of claim 2 wherein the molten metallic charge
comprises copper.
4. The improvement of claim 2 wherein the molten metallic charge
comprises steel.
Description
This invention relates to improvements in the spinning of molten
metals and alloys thereof.
More particularly, this invention relates to improvements in
spinning processes and assemblies employed for melt spinning of
metals and alloys thereof in the manufacture of fine diameter
wire.
Processes for the formation of fine diameter wire by spinning
molten metals through an orifice as a free molten filamentary
stream have been disclosed in U.S. Pat. No. 3,658,979 and in U.S.
Pat. No. 3,216,076. According to these processes a molten
filamentary metallic jet is spun into a film-forming atmosphere
whereupon a thin stabilizing film is rapidly formed on the surface
of the molten filamentary stream. The film negates the effects of
surface tension and prevents breakup of the molten stream for a
sufficient period of time to allow the molten stream to freeze or
solidify in filamentary form. The apparatus employed to facilitate
spinning of molten filamentary jets in forming fine diameter wire
generally comprises a crucible having an orifice in its base,
either as a part of the crucible base, or preferably, as an orifice
insert. Typically, the crucible is provided with means for melting
the metallic charge and maintaining a desired degree of superheat
for the molten metal charge contained in the crucible and,
additionally, means for applying a positive pressure to the head of
the molten charge to force the molten metal through the orifice at
desirable jet velocities.
The FIGURE is a cross-sectional view of a representative unit
useful for spinning fine diameter wire where a molten metal is
contained in crucible 2 having base plate 3, the crucible and base
plate being supported on pedestal 4 and enclosed within an
insulating cylinder 5 and a susceptor 6 employed in conjunction
with induction heating coils 7. The unit is pressurized within by a
pressure source 8 through top 9. Sealing rings 10 serve to maintain
the pressure within the enclosure and prohibit leakage past the
base plate. The molten metal 1 is forced through orifice 11 in
orifice plate 12 by the force of pressure supplied by pressure
source 8 at sufficient velocities to provide a filamentary shaped
molten jet 13. The nascent jet passes through a film-forming
atmosphere contained within the cavity 14 generally provided by the
pedestal 4.
Although materials science has developed at a rapid pace in recent
years there nevertheless appears to be limited data reported on the
strength, solubilities and chemical reactivities of materials at
temperatures above 1,000.degree. C. Thus, in the manufacture of
copper and steel wire, for example, directly from their respective
melts considerable time and effort have been spent defining the
nature and performance of materials used to handle molten metals at
high temperature as well as the effect of molten metals on such
materials.
Perhaps the most critical element of the spinning assemblies used
to make wire according to the process outlined above is the member
defining the orifice through which molten metal is spun under
pressure. While the glass fiber art has developed its "bushings"
and the synthetic fiber art its "spinnerets," little useful
information has been reported in the literature relating to orifice
defining members employed for spinning molten metals. Because of
the nature of the charge and conditions employed in the manufacture
of fine diameter wire (below about 35 mils) by melt spinning
processes process, development has been seriously handicapped by
repeated failure of the materials used to define the spinning
orifice. Materials such as high density alumina, sapphire, zirconia
(calcium oxide stabilized), Al.sub.2 O.sub.3 .sup.. Cr.sub.2
O.sub.3 ceramic and others frequently employed to contain molten
metals, such as steel, in metallurgical processes fail to perform
satisfactorily as orifice defining members through which molten
metals can be spun as fine diameter filamentary jets. The cause of
such failures can be variously attributed to insufficient strength,
low thermal fracture resistance and poor chemical stability under
the conditions of temperature and pressure required to spin molten
metals from orifices having diameters below about 35 mils. Such
failures have been noted to be particularly aggravated at
temperatures above about 1,000.degree. C. and with decreases in
orifice diameter, particularly where the orifice diameter is below
about 15 mils.
As already indicated the requirements for materials used to define
fine diameter orifices in melt spinning processes are critical to
the successful operation of prolonged spinning. Initially, the
material must be resistant to thermal fracture generally caused by
elevating the temperature and by temperature gradients across the
face of the disc during the spinning operation. Insofar as it is
desirable to employ orifices having aspect ratios of between about
1 and 20 the orifice defining plate or disc from which fine
diameter wire is spun is usually quite thin in the vicinity of the
orifice and yet its strength at the spinning temperature, of steel
for example, must be of such magnitude that it can withstand the
high pressure necessary to force the molten metal through the samll
orifice at reasonably high velocities. Cracked orifice defining
discs caused by thermal fracture or by mechanical failure under
pressure result in abortive operations in wire manufacturing
process. Chemical reactivity or solubility with the molten metallic
charge can result in erosion of the orifice or deposition of
occlusions in the fine diameter orifice, neither of which can be
tolerated in an industrial spinning process. Moreover, chemical
reactivity of the ceramic material with graphite assembly parts
presents serious problems. For example, both alumina and zirconia
readily react with graphite at elevated temperatures.
Thus, a suitable orifice defining member of a spinning assembly
must adhere to a combination of physical and chemical
requirements.
While the property requirements of orifice plate are severe in high
temperature spinning, the crucible assembly as a whole should
adhere to the chemical reactivity and solubility requirements.
It has now been discovered that polycrystalline beryllium oxide
having a density of greater than 95 percent of the theoretical
density and purity of at least 99.5 percent and single crystal
beryllium oxide serve well as orifice defining materials in the
spinning of molten metals without significant problems of thermal
or mechanical failure, chemical reactivity, or orifice erosion or
occlusion due to the solubility characteristics of beryllia.
Plates or discs of single crystal or polycrystalline beryllia can
be readily machined to suitable size, shapes by means known to
those skilled in the art. Fine diameter orifices are generally
provided by machining a countersink in the feed face of the orifice
plate and thereafter drilling and polishing an orifice of desired
diameter concentric with the countersink. Additionally, orifice
plates composed of polycrystalline beryllia can be conveniently
prepared by a bisque process wherein the plate is shaped and the
orifice drilled before the final firing. The greenware plate is
thereafter fired to appropriate densities, after which the orifice
is polished to reduce minor crystal imperfection.
As above indicated the orifice defining member may additionally
serve as the base plate of the crucible assembly. However, it has
been found desirable to employ orifice plate inserts in the base
plate of the crucible as indicated in the FIGURE. The insert type
or orifice plate is conveniently circular and may, if desired, be
secured in the base plate using a clamp or hold down ring. Multiple
orifice insert discs may, of course, be employed in the base plate
of the crucible. The orifice should have an aspect ratio of between
1 and 20, preferably less than 10, exclusive of the countersink
and, although slightly tapered orifices have been used, straight
bore orifices are preferred because of greater ease in
fabrication.
Where spinning assemblies incorporating the beryllia orifice plates
of this invention are used it has been found convenient to use
beryllia crucible base plate members insofar as the chemical
reactivity and solubility characteristics are suitable for high
temperature spinning. Additionally, it has been discovered that
beryllia crucible assembly members are inert to graphite parts of
the spinning units.
The following examples illustrate the utilization of low viscosity
melt spinning orifices constructed of beryllium oxide (BeO) and
zirconium oxide (ZrO.sub.2) for spinning molten metals.
EXAMPLE I
An apparatus, similar in construction to that depicted in the
FIGURE, was employed to produce metal filaments from a composition
comprising 99 weight percent type 304 stainless steel and 1 weight
percent type 1345 aluminum.
The metal charge was placed in the crucible which had been
prefitted with a beryllium oxide (BeO) orifice insert 12 having a
tapered orifice construction wherein the taper, adjacent the melt,
had an included angle of 12.degree.. The orifice capillary diameter
was 6 mils and an aspect ratio (length/diameter) of approximately
2.5.
After placing the metal charge in the crucible it was elevated in
temperature to 1,670.degree. C under the influence of a vacuum.
Subsequent to melting an inert gas (argon) under 20 psig pressure
was applied to the melt whereby streaming of the melt through the
orifice was effected. Upon the initiation of streaming the melt
temperature was reduced to 1,620.degree. C (to reduce the amount of
superheat).
The molten metal streamed into the cavity 14 which was occupied by
an atmosphere of carbon monoxide (CO) whereby the molten stream was
stabilized against breakup until solidification thereof took place.
Very long filaments were produced having nodes spaced approximately
at 8 to 10 inch intervals.
Subsequent to the completion of the spinning run the apparatus was
cooled down and the beryllium oxide orifice insert was removed from
the crucible whereupon it was microscopically examined for
structural defects such as surface flaws and/or cracks and for
orifice erosion. The examination disclosed no imperfections nor any
measurable degree of orifice erosion.
EXAMPLE II
The orifice insert of Example I was reinstalled in the apparatus
thereof and an identical metal composition was melted and extruded
at a melt temperature of 1,690.degree. C into an atmosphere of
carbon monoxide. The melt extrusion pressure was increased to 30
psig and that in combination with the increase in the melt
temperature provided extremely long filaments having nodes spaced
at approximately 15 to 20 inch intervals.
After the spinning run was completed the beryllium oxide insert was
again microscopically examined as in Example I with no detectable
structural failure nor measurable degree of orifice erosion.
The results obtained in Example I and II were unexpected because
thermodynamic data indicated that beryllia would dissolve in molten
steel to such an extent that it would not be satisfactory orifice
material.
EXAMPLE III
The spinning run of Example I was repeated with the exception that
the orifice insert 12 was constructed of zirconium oxide
(ZrO.sub.2) and included a tapered orifice inlet having a
27.degree. included angle. The orifice capillary diameter was 7
mils and the orifice aspect ratio was 1.48.
Melt streaming was initiated through the orifice but ceased after
one minute duration.
Subsequent microscopic examination of the orifice disclosed that
plugging had occurred due to the formation of an oxide deposit
therein.
EXAMPLE IV
The apparatus of Example I with the exception that a one-piece
beryllium oxide crucible was employed for the production of copper
filaments.
The crucible was provided with an orifice having a diameter of 4
mils and a capillary length of 6 mils which was fabricated in the
base of the crucible.
The crucible along with a charge of electrolytic grade copper was
placed in the melt spinning heat whereupon it was melted and
extruded at a temperature of 1,200.degree. C by means of an inert
gas pressure of 40 psig. into a stabilizing atmosphere of
propane.
Subsequent to the complete melt extrusion of the copper charge the
spinning apparatus was cooled down and disassembled whereupon the
crucible and orifice were examined under a microscope. The
examination revealed that no apparent erosion of the orifice had
occurred.
EXAMPLE V
A ZrO.sub.2 orifice insert was fabricated having a 4 mil diameter
orifice with an aspect ratio of 5. The orifice insert was placed in
the melt spinning apparatus and the assembly was elevated in
temperature to 1,600.degree. C. in the absence of a metal charge.
The temperature was maintained for 5 hours and after cooling down
the equipment the orifice insert was removed therefrom and
microscopically examined.
The examination revealed that the orifice was completely plugged
with a clear crystalline material. The bottom of the insert in
contact with the graphite had undergone severe reaction resulting
in loss of gas pressure seals.
A similar study using an Al.sub.2 O.sub.3 single crystal orifice
insert substantially the same conditions as above resulted in
reaction with graphite to thereby destroy the gas seals and
severely damaged the orifice exit.
* * * * *