U.S. patent number 3,850,368 [Application Number 05/331,792] was granted by the patent office on 1974-11-26 for apparatus for centrifugal compaction.
This patent grant is currently assigned to Kennametal Inc.. Invention is credited to Benjamin Clark Boeckeler.
United States Patent |
3,850,368 |
Boeckeler |
November 26, 1974 |
APPARATUS FOR CENTRIFUGAL COMPACTION
Abstract
A method and apparatus for the centrifugal compaction of
particulate material in which the particulate material is admixed
with a liquid to form a slurry and is then placed in a chamber and
centrifuged about a main axis to cause the material to compact into
a discrete body. A particular feature of the invention is to be
found in the fact that the chamber in which the slurry is contained
during compacting is caused to rotate about an axis inclined to the
main axis so that the particulate material is agitated and thereby
nests intimately together during the centrifuging operation thereby
resulting in workpieces significantly more dense than can be
arrived at by simple centrifuging or even by pressing.
Inventors: |
Boeckeler; Benjamin Clark
(Greensburg, PA) |
Assignee: |
Kennametal Inc. (Latrobe,
PA)
|
Family
ID: |
23295400 |
Appl.
No.: |
05/331,792 |
Filed: |
February 12, 1973 |
Current U.S.
Class: |
425/430; 366/214;
494/19 |
Current CPC
Class: |
B04B
9/08 (20130101); B04B 5/02 (20130101); B04B
5/04 (20130101) |
Current International
Class: |
B04B
5/04 (20060101); B04B 5/00 (20060101); B04B
9/08 (20060101); B04B 9/00 (20060101); B04B
5/02 (20060101); B04b 009/08 () |
Field of
Search: |
;425/434,435,430
;233/23R,24,25,26 ;259/57 ;210/380 |
References Cited
[Referenced By]
U.S. Patent Documents
Foreign Patent Documents
Primary Examiner: Krizmanich; George H.
Attorney, Agent or Firm: Crosby; Melvin A.
Claims
What is claimed is:
1. In an apparatus for the centrifugal compaction for granular
materials, a support, means engaging said support and defining a
first axis of rotation thereof, flasks pivotally mounted on said
support in circumferentially distributed relation and radially
spaced from said first axis, each flask being swingable outwardly
at the bottom in response to rotation of said support, chamber
means carried by each flask and having a cavity adapted to receive
a slurry consisting of the said granular material to be compacted
and a liquid, a drive shaft on said first axis for rotating said
chamber means about respective second axes extending angularly to
said first axis as said support rotates about said first axis, said
second axes being inclined at a predetermined angle to a plane
perpendicular to said first axis, drive means responsive to outward
swinging movement of the lower ends of said flasks on said support
for drivingly connecting said chamber means to said drive shaft,
and means on said support for engaging and halting said flasks at
said predetermined angle of inclination to said plane.
2. An apparatus according to claim 1 in which said chamber means
comprises a hollow cylindrical metallic shell adapted to receive
therein mold elements defining the size and shape of the article to
be made.
3. An apparatus according to claim 1 in which said drive means
includes output shaft means coupled at one end to said drive shaft
and extending radially along said support to the region of said
chamber means.
4. An apparatus according to claim 1 which includes a speed reducer
having an input shaft on said first axis and forming said drive
shaft and an output shaft for each chamber extending on said
support to near the respective chamber, and cooperating elements of
a brake connected to said input shaft and to a stationary point and
operable when actuated to hold said input shaft stationary during
rotation of said support thereby to cause said output shafts to
rotate and drive the said chamber means on said second axis.
5. An apparatus according to claim 4 which includes means
selectively operable for actuating said brake means.
6. An apparatus according to claim 1 which includes a ring for
supporting each said flask, trunnions on each ring pivotally
connecting the ring to said support on a horizontal axis which is
perpendicular to a radius extending therefrom to said first axis,
each said flask being generally cylindrical and being insertable
into the respective ring from above and including flange means near
the top to engage the top of said ring, each said chamber means
being insertable into the respective said flask from above, and
bearing means interposed between each said chamber means and the
pertaining said flask to permit free relative rotation of the
chamber means in said flask.
7. An apparatus according to claim 6 in which said bearing means
include thrust bearing means interposed between the bottom of each
said chamber means and the bottom of the pertaining said flask and
radial bearing means disposed between an upper region of each said
chamber means and an upper region of the pertaining said flask.
Description
The present invention relates to a method and apparatus for the
centrifugal compaction of granular or particulate materials.
Granular or particulate or powdered materials are employed for the
making of ceramic articles and also for the making of articles from
metals and the like. The use of granular material is of benefit, in
some cases, for reasons of economy, because the workpiece formed by
the compacting operation can be formed nearly to size and shape
thereby eliminating expensive machining operations.
In other cases, as in the case of some ceramics and cermets and
certain metals, the product is so difficult to machine that it is
highly uneconomical to attempt to form the article by any other
method than by the compaction of powders. Ceramic articles fall
into this class, as do articles formed of hard metallic
carbides.
A characteristic of the harder materials is that the particles or
powders, which are employed for the manufacture thereof, are quite
often jagged in nature, having points and sharp edges thereon, so
that no simple compacting method will bring the powders into such
intimate relation that all bridging of the particles on each other,
which produces voids and flaws, is greatly reduced and, in most
cases, completely eliminated.
Lubricants are usually employed in respect of such powders to
assist in the free movement of the particles relative to each other
during compaction, but even in the presence of a lubricant, the
jagged particles from which carbide materials and ceramic materials
are made will tend to form bridges between particles, with voids
and flaws resulting.
With the foregoing in mind, it is a particular object of the
present invention to provide an improved method and apparatus for
effecting the compaction of powdered materials which will result in
the formation of workpieces which are more uniformly compacted and
more dense than have been attainable heretofore by known
practices.
A particular object of the present invention is the provision of a
method and apparatus for compacting particulate materials in which
the compacting force on the materials is developed in a
centrifuge.
Still another object is the provision of a method and apparatus for
centrifuging particulate material into a condition of compaction
which develops simultaneous controlled agitation of the materials
together with motion between particles relative to each other at
the time of compaction and which results in a superior uniformity
and density of the final product.
These and other objects and advantages of the present invention
will become more apparent upon reference to the detailed
specification taken in connection with the accompanying drawings in
which:
FIG. 1 is a somewhat schematic perspective view showing one form of
centrifuging apparatus according to the present invention utilizing
two flasks with one shown in outwardly swung position and the other
in vertical position.
FIG. 2 is a plan view of the centrifuge shown in FIG. 1 with one of
the flasks thereof hanging vertically and the other shown in swung
out position.
FIG. 3 is a partial vertical section through the centrifuging
apparatus showing one side thereof and is indicated by line
III--III on FIG. 2.
FIG. 4 is a vertical section through one of the flasks of the
apparatus showing the construction thereof and the member inside
the flask forming the material receiving chamber.
FIG. 5 is a fragmentary perspective view showing one form which the
clutch can take for connecting a drive to the chambers in the
flasks.
FIG. 6 is a fragmentary sectional view showing one form which the
brake can take which is associated with the drive for the chambers
in the flasks.
FIG. 7 is a sectional view like FIG. 4 but shows a modified
arrangement of the flask and chamber.
FIG. 8 is a schematic view illustrating the manner in which the
arrangement of FIG. 4 functions.
FIG. 9 is a schematic view like FIG. 8 but shows the manner in
which the modification of FIG. 7 functions.
FIG. 10 shows a modification in which the cross sectional area of
the cavities is relatively small and the cavities are inclined to
the axis of the flask to obtain substantial action in the liquid
contents in the cavities;
FIG. 11 is a sectional view schematically illustrating a flask
having a mold member therein for producing a complex shape.
BRIEF SUMMARY OF THE INVENTION
The present invention discloses a centrifuge in which flasks are
mounted on a structure rotatable on a main axis by means of
trunnions so that the flasks will be swingable radially with
respect to the main axis. When the main axis is vertical, as is
usually the case, the flasks will swing outwardly at the bottom
when the rotating structure is driven in rotation. This arrangement
permits the flasks to be loaded from the top and for the
centrifugal action to impel the material being compacted toward the
bottoms of the flasks which, when the rotary structure is rotating,
will be radially outermost.
The material to be compacted is granular and is admixed with a
liquid to form a slurry. The liquid has a lower specific gravity
than the particles admixed therewith and, when the rotary structure
rotates, the centrifugal force acting on the particles will cause
them to migrate in the radially outwardly direction and thereby to
become compacted.
The liquid contains a lubricant and a binding agent so that the
particles will slide on one another during compaction and remain in
position at the end of the compacting operation thereby to form a
discrete body which can be removed from the flask and manually
handled.
A particular feature of the present invention is in the provision
of an inner chamber in the flask which is rotatable therein and
which, when the flask is swung outwardly to its outermost position,
is inclined to the horizontal and is driven in rotation. By
rotating the inner chamber as the rotary structure rotates, a sort
of tumbling action is produced on the particles within the chamber
which effectively breaks down bridges in the material and assists
in causing the particles to rest closely together so that a higher
degree of compaction of the material is obtained that can be
obtained by simply centrifuging the material.
After the material is compacted into a discrete body, it is removed
from the chamber and is then dried and sintered to form a solid
member. It has been found that articles made according to the
invention disclosed herein are markedly more free of pits and voids
than compacted granular workpieces made by other methods, including
straight centrifuging methods and dry pressing methods, and are
more dense thereby leading to a superior end product for most
purposes.
As mentioned, the main axis about which centrifuging takes place is
usually vertical, as a matter of convenience, but may be disposed
at any angle. When the main centrifuging axis is at an angle other
than vertical, the angle of the axis of rotation of the flasks is
inclined at an angle to a plane perpendicular to the main axis. In
any case, the angle of inclination of the axis of rotation of the
flasks can be quite small or quite large, say, as small as
1.degree. or as large as 89.degree.. In practice, an angle of about
15.degree. has been found to be satisfactory.
The speed of rotation of the chamber in the flask is preferably
only a fraction of the speed of the rotation of the rotary
structure and is sufficient to provide for the aforementioned
tumbling action of the particles until the particles commence to
compact in the radially outer end of the chamber. The speed of
rotation of the chamber is not sufficient to disturb the compacted
particles.
DETAILED DESCRIPTION OF THE INVENTION
Referring to the drawings somewhat more in detail and with
particular reference to FIGS. 1 to 3, the centrifuging apparatus
will be seen to comprise a drive mechanism generally indicated at
10 which is disposed inside a large circumferential shield member
10a. Mounted on the upper end of the output shaft of the drive
mechanism 10 is a plate 11 forming the central member of a rotary
structure which also comprises laterally extending spaced parallel
bars 12 secured to plate 11, as by cap screws 14, and notched at 16
so as to engage the edges of the plate 11. Bars 12 form the arms of
the centrifuge. The rotary structure rotates on a vertical main
axis but, as mentioned previously, the main axis could be at any
other angle.
Toward their outer ends, the arms are provided with laterally
aligned bores in which bushings 18 are mounted and which bushings
rotatably receive trunnions 20 of support rings 22. Each support
ring 22 is adapted for receiving a cylindrical flask member 24 from
above with each flask member having a flange 26 at its upper end to
engage the upper side of the respective ring 22.
It will be appreciated that the centers of gravity of flasks 24 are
disposed substantially lower than the horizontal pivot axes defined
by the respective trunnions 20 of the pertaining support rings so
that, when the rotary structure of the centrifuge rotates, the
flasks will swing outwardly at their lower ends.
As the centrifuge slows to a halt, however, the flasks return to a
vertical position thereby providing for free access to the upper
ends thereof for receiving the material to be centrifuged. In FIGS.
1 and 2, the right hand flask is shown in the dependent position it
will occupy when the rotary structure is at rest whereas the left
hand flask is swung outwardly to the position which it will occupy
when the rotary structure is rotating.
Each of the bars 12 of the centrifuge arms on top thereof near the
outer end and radially outwardly from the position of trunnions 20
is provided with an elongated upwardly opening notch 28 that
receives the downwardly thickened region at the inner end of a
respective one of a pair of spaced parallel arms 30 which are
fixedly secured to bars 12 as by cap screws 32. On the lower sides
of arms 30, at the outer ends thereof, are formed the downwardly
opening inclined slots 34 in which pair of which is seated a member
36 extending transversely of the said arms and fixed thereto as by
cap screws 38.
The central portion of each member 36 is recessed, as at 40, and
mounted therein is an arcuate cushion member 42 made, for example,
of Teflon or the like. As will be seen at the left side of FIGS. 1
and 2, the cushion member 42 is arranged to engage the lower
finished circumference 44 of the respective flask when the flask
swings outwardly thereby to stop the respective flask with the
longitudinal axis thereof inclined to the horizontal and,
specifically, downwardly with respect to the horizontal. More
generally, the flasks are halted with the axes thereof inclined to
a plane perpendicular to the main centrifuging axis.
As will be seen in FIG. 4, each flask comprises a relatively thick
walled cylindrical member 50 closed at the bottom by a plate 54.
Resting on plate 54 is a bearing support plate 56 having a cavity
in which is mounted the outer race 58 of a thrust bearing which has
an inner race 60 and a tapered rollers 62 interposed between the
races. Inner race 60 is adapted for receiving a pintle or stub
shaft 64 formed on the bottom of a further support plate 66 which
has a cylindrical bore 68 in the upper side thereof.
Cylindrical bore 68 is adapted for receiving the pintle or stub
shaft portion 70 formed on the bottom of a cylindrical member 72
disposed in flask 24 and coaxial therewith and forming the chamber
which is to receive the material to be compacted. Cylindrical
member 72 extends to near the top of the flask and is adapted for
having the upper end thereof closed by a closure cap 74 held in
place by cap screws 76.
The upper end of flask 24 comprises a bearing support ring 78 held
in place in the upper end of member 50 as by radial set screws 80.
Ring 78 supports the radial bearing 82 which fits about the
enlarged portion 84 formed on the upper end of cylindrical member
72.
It will be noted that between the lower end of enlarged portion 84
and the upper end of an upstanding annular lip 86 of ring 78 there
is a substantial amount of axial clearance so that cylindrical
member 72 is always supported on the thrust bearing at the bottom
thereof and even conditions of high load at high centrifuging
speeds will not close the aforementioned gap.
The inside of cylindrical member 72 may itself receive the material
to be compacted but it is more advantageous to form the member 72
to a size larger than the piece to be made and to insert in member
72 a mold member 88, which can be formed of epoxy resin, for
example.
Mold members 88 is preferably provided with a film-like liner
member 90 of any suitable material, such as polyvinyl alcohol, and
it is into this member that the slurry 92 consisting of the
granular or particulate material to be compacted and the liquid
vehicle therefor is placed. The mold member 88 may have a single
cavity therein or it may have a plurality of cavities.
Further, two or more mold members may be placed in member 72 in end
to end relation. Thus, a single article can be made in each flask
or a plurality of members can be made in each flask.
The particulate material may consist of any sort of granular
material including that which is used to form ceramics as well as
any type of powdered metal and may also consist of such material as
hard metal carbides and a binder metal therefor.
In respect of the hard metal carbides, for example, the carbide may
be tungsten carbide or titanium carbide or tungsten titanium
carbide and the binder material may consist of any of several types
of metals, or alloys, or combinations thereof such as cobalt,
nickel, molybdenum, iron and other known binder materials. All such
materials are finely ground prior to compaction according to
practices well known in the art.
A particular characteristic of carbide particles is that they are
often somewhat dendritic in nature with sharp edges and points and
thus do not slide free upon one another. Accordingly, in the
compacting of such materials, whether by dry pressing, or by
centrifuging while suspended in a slurry, the particles tend to
engage each other in less than fully nested position and form
bridges which can show up as pronounced flaws in the finished
product.
The liquid in which the particles are suspended to form the slurry
includes a lubricant such as paraffin wax to facilitate the sliding
of the particles on one another but even in the presence of a
lubricant, as the particles begin to compact into a small space,
the aforementioned bridging effect will begin to take place. The
disrupting of such bridges during the compacting operation is,
therefore, a highly desirable objective to achieve.
The structure of the present invention is specifically designed to
prevent the formation of such bridges in the material during
compacting by creating controlled agitation in the material during
compaction which will promote the nesting of the particles together
but without, however, in any way interfering with the formation of
a discrete body which can be handled when it is removed from the
centrifuge.
As was pointed out above, the flask in its outwardly swung position
has the axis inclined to a plane perpendicular to the main axis and
for this reason the axis of inner member 72 is also so inclined and
by rotating this member in the flask while the rotary structure of
the centrifuge is rotating, sufficient agitation of the particles
within the chamber is created to cause the intimate nesting
together of the particles and to prevent the formation of the
bridges referred to.
Rotation of the inner member in the flask is accomplished by a
clutch arrangement provided on the inner member which couples with
a drive therefore when the flask is swung to its outermost
position. This clutch arrangement can take any of several forms but
for the purpose of the present disclosure will be seen to comprise
a pair of drive pins 100 extending axially outwardly from the upper
end of top closure member 74 of inner member 72. Pins 100 are
tapered on the end and are yieldably supported in the axial
direction.
Drive pins 100 are adapted for cooperation with a pair of drive
lugs 102 mounted on the end of a shaft 104 supported by bearings
106 in a bracket 108 carried by plate 11 and fixed thereto by
screws 109. The lugs 102 are tapered inwardly to permit pins 100 to
cam thereover, if necessary.
Lugs 102 are spaced apart so as to define a central slot 112 and,
when starting the centrifuge, shaft 104 is rotated till lugs 102
are horizontal and the respective inner member 72 is rotated so
that drive pins 100 will be in the vertical radial plane of the
slot so that, when the flask swings outwardly on its trunnions, one
of the drive pins will pass through slot 112 and, thereafter, when
shaft 104 is set into motion, the lugs 102 will engage drive pins
100 and drive inner member 72 in rotation in flask 24.
It will be apparent that other types of clutching arrangements
could be employed and that the important thing in respect of the
clutch is to establish a driving connection to the inner member 72
for each flask, at least, when the respective flask is swung to
outermost position.
Each shaft 104 is connected by a universal joint 110 (FIGS. 1, 2)
with a respective shaft 113, and each of which is connected by a
further universal joint 114 with a respective slow speed output
shaft 116 of a speed reducer 118 which has an input shaft 120
arranged on the axis of rotation of the rotary structure of the
centrifuge.
Shaft 120 carries one element 122 (FIG. 6) of a brake mechanism
which has another element 124 slidably keyed to a shaft 126
stationarily supported by a member 128. Element 124 of the brake is
connected to a lever 130 which is normally biased by spring 132 in
a direction to disengage the brake elements.
Also connected with lever 130 is the armature of a
solenoid-armature arrangement 134 which, upon energization, will
overcome the bias of spring 132 and move the brake elements 122 and
124 into an operative engagement with each other.
When the centrifuge is started, the solenoid is de-energized and
the brake elements are disengaged and input shaft 120 rotates with
the rotary structure of the centrifuge. However, after flasks have
swung to their outermost position thereby bringing drive pins 100
into operative relation relative to lugs 102, the solenoid is
energized and this will cause the elements of the brake to engage
and to hold input shaft 120 against rotation which will, in turn,
cause rotation of the output shafts 116 relative to the rotary
structure of the centrifuge whereby the inner members 72 of the
flasks will be driven in rotation.
In an arrangement wherein the distance from the center of rotation
of the rotary structure of the centrifuge to the trunnions for the
flasks is about 10 1/2 inches, and the bottoms of the flasks are
spaced about 10 inches from the trunnions, the rotary structure
might rotate at a speed of from, say, 600 to 800 revolutions per
minute while the drive to the chambers or inner members in the
flasks will cause rotation thereof at, say, from about 15 to 25
revolutions per minute.
The inclination of the flasks from the horizontal is illustrated in
the drawings at 15.degree., but the exact amount of inclination of
the flask can be varied considerably, say, from 1.degree. to
89.degree., and the benefits derived from the practice of the
present invention may be realized. A suitable angle of inclination
of the flasks which can easily be arrived at might, for example, be
as little as 10.degree. or as much as 20.degree..
Further, the particular angle of inclination of the flask is, at
least in part, determined by the manner in which the inner member
forming the material chamber is arranged therein. In FIG. 4, the
inner member 72 is coaxial with the outer member 50 forming the
body of the flask and under these circumstances an angle of
inclination of 15.degree. has been found to be satisfactory.
In a modified form which the apparatus can take, as shown in FIG.
7, the trunnion mounted flask, indicated generally at 150, can be
permitted to swing outwardly to a substantially horizontal position
because the inner chamber member therein, indicated generally at
152, is inclined relative to the axis of the flask. This is
accomplished by mounting inner member 152 in a frame consisting of
an upper plate 154, a lower plate 156, tie bolts 158 connecting
plates 154 and 156 and with member 152 supported on the plates in
inclined relation, on suitable support bearings which permit
rotation of inner member 152.
The plates 154 and 156 are receivable in flask 150 and will support
inner member 152 in the illustrated inclined position therein. As
before, inner member 152 has an element 160 of a disengageable
clutch thereon so that when the flask is in its outwardly swung
position, the inner member is automatically coupled to a drive so
that the inner member can be driven in rotation thereby.
FIG. 8 schematically illustrates the manner in which a flask 200 is
stopped at an inclined position with the axis about 15.degree.
below the horizontal. Flask 200 has an inner container 202 therein
containing slurry 204. When the centrifuge is rotating at high
speed, the radially inner surface of the body of slurry in inner
container 202 is substantially vertical as shown by line 206. As
the inner container is rotated within the flask, the slurry will
continuously shift therein to maintain the surface plane at 206
thereby causing relative motion of the particles in the slurry and
the nesting together thereof described previously and leading to
the high degree of compaction referred to.
FIG. 9 illustrates the manner in which the modification of FIG. 7
can operate and wherein flask 208 is swung out substantially
horizontal position while inner container 210 is in an inclined
position due to its support within the flask. When inner container
210 is rotated on its axis, the same agitating action on the slurry
therein will be obtained as was described in connection with FIG.
8.
In FIG. 10, flask 212 has therein an inner container 214 within
which is mounted mold members having the relatively small diameter
cavities 216 therein. Flask 212 is stopped with its axis about
15.degree. below the horizontal and with the flask stopped at this
angle and the centrifuge in operation, rotation of the inner
container will bring about a substantial movement of the slurry
within the individual cavities 216.
FIG. 11 illustrates somewhat schematically one of the particular
advantages to be realized from the centrifugal compacting of
particulate material according to the present invention. In FIG.
11, a flask 230 is provided with an inner member 232 which may, for
example, consist of epoxy resin or the like.
Within the cavity in member 232 is a further member 234 having a
relatively complex cavity therein and in which the slurry to be
compacted is placed. After centrifuging the slurry to its desired
degree of compaction of the particulate material therein, member
234 is removed from member 232 and the free liquid on top of the
compacted body in member 234 is poured off.
By forming member 234 of a material such as polyvinyl alcohol which
can be dissolved completely away from the body therein by water and
the body can then be sintered according to standard practices.
Polyvinyl alcohol has been mentioned because it will dissolve in
the water and can be recovered for reuse, but it will be understood
that other materials having different solvents can be employed for
this purpose. The important thing is that the material forming the
mold cavity be strong enough to maintain the shape of the cavity
during centrifuging and thereafter be releasable from the compacted
body without imposing any strains on the body, as well as being
impervious to solvent or chemical action of the liquid used to form
the slurry.
In respect of powders pressed by conventional pressing techniques,
and even when hydrostatically compacted at pressures up to 50,000
psi, the shrinkage of the compacted body which takes placeupon
sintering will range from about 19.4 to 19.6 percent. The same
carbide powders when compacted as disclosed in the present
application had shrinkage factors as low as 14.5 percent without
hydrostatic compacting and as low as 13.6 percent when
hydrostatically compacted at about 35,000 pounds per square
inch.
Further, the pits and flaws in sintered compacts made as disclosed
in the present application were extremely low as compared to the
pit and flaw count in compacts made according to standard
practices, for example, by dry compacting.
Specific examples of the practice of the present invention are
given below.
EXAMPLE I
One typical mix of tungsten carbide powder was made as follows:
Tungsten Monocarbide -- 93.68 percent by weight
Cobalt -- 5.81 percent by weight
Paraffin Wax -- 0.51 percent by weight
The starting materials in powder form were ground together in a jar
mill in naptha containing paraffin wax in solution until reduced to
about 1.06 Fisher subsieve particle size. The resultant powder was
dried and then contained about 0.51 percent by weight of paraffin
wax.
A liquid vehicle solution was then prepared for making up the
powder slurry. It contained the following:
Perchloroethylene 100.00 milliliters (Sunoco 3420) A Paraffin Wax
having a melting point of about 137 degrees Fahrenheit (Sun Oil
Co.) 0.90 grams (Elvax 260) Vinyl Resin in the form of a Copolymer
of Ethylene and Vinyl Acetate. (E. I. DuPont de Nemours and Co.)
1.80 grams (Arquad 2C-75) A Dialkyl Quaternary Ammonium Chloride
derived from a fatty acid. (Armour Industrial Chemical Co.) 3.40
grams
This vehicle solution has a gel point of about 65.degree. F.
The above liquid vehicle solution was then mixed with the tungsten
carbide powder in the porportion of 90 milliliters of solution to 1
kilogram of powder. The resulting slurry was then charged to a
tungsten carbide lined jar mill and milled for 3 days at
115.degree. F. It was then ready to be centrifuged to form
compacts.
The centrifuging flask used is illustrated in FIG. 4 of this
application. The mold member shown (88 in the drawings) was made of
epoxy resin and the cavity therein was 2 1/8 inches diameter by 10
inches in depth. The film-like liner member (90 in the drawings)
with which the cavity was lined was made of polyvinyl alcohol.
Upon completion of milling, the slurry was poured into the
polyvinyl alcohol liner member contained inside the cavity and
centrifuged for 20.75 hours total time at 95.degree. F. During
centrifuging, the rotational speed about the main axis of rotation
was 530 revolutions per minute producing a force of 177 times G,
the acceleration of gravity. During this period the flask was
rotated about its axis at 53 revolutions per minute for a period of
20 hours and was not rotated during the final period of
centrifuging.
Upon completion of centrifuging, the powder compact together with
the polyvinyl alcohol liner member in which it was encased was
removed from the cavity of the mold member. The compact and
polyvinyl alcohol liner member were then moistened with water and
allowed to stand until the liner member softened and disintegrated
sufficiently to be stripped from the compact without causing any
surface damage or "pluck out." This was done at ambient temperature
and took about 1/2 hour.
The compact was then dried at 160.degree. F. for about 36 hours.
The compact was then cut into test pieces; in some cases it was
isostatically hydropressed before cutting into test pieces.
Test pieces were then sintered at about 200 microns absolute
pressure at 2,200.degree. F. for 1/2 hour.
For comparison, the same powder batch used in making the
centrifugal compacts described above was made into compacts by
conventional isostatic hydropressing at 50,000 pounds per square
inch. Test tips cut from these compacts were sintered under the
same conditions used for the centrifugal compacts.
Differences in properties are shown in the tables which follow:
TABLE I ______________________________________ TRANSVERSE RUPTURE
STRENGTH IN LBS. PER SQ. IN./1000 Method Used Conventional
Centrifugal Compaction Compaction
______________________________________ Lowest Value 271 340 Highest
Value 384 445 Average Value 337 403
______________________________________
TABLE II ______________________________________ MACRO PIT AND FLAW
COUNT Method Used Conventional Centrifugal Compaction Compaction
______________________________________ Total Pits and Flaws per 100
square inches .002 inches and larger in diameter 41.8 0.9 .004
inches and larger in diameter 9.0 0.0 Total Area Examined -- square
inches 134.0 115.5 ______________________________________
It will be noted that the transverse rupture strength of the
samples made by centrifugal compaction according to the present
invention and the pit and flaw count are both substantially
improved over the values obtained when compacting by conventional
methods.
In the table which follows, Shrinkage Factors are expressed as the
ratio of a given dimension before and after sintering.
TABLE III ______________________________________ SHRINKAGE FACTORS
Method Used Conventional Centrifugal Compaction Compaction
______________________________________ Isostatic pressure used in
pounds per square inch No pressure used -- 1.134 to 1.146 35,000 --
1.132 to 1.137 50,000 1.194 to 1.196 1.138 to 1.140
______________________________________
The Shrinkage Factor data above illustrates the very substantial
improvement in density obtained by centrifugal compaction of the
present invention. With conventional compaction the lowest
shrinkage factor was 1.194 corresponding to 58.7 percent of
theoretical density. With Centrifugal Compaction densities ranged
from 66.4 to 68.9 percent of theoretical.
EXAMPLE II
A mix of tungsten carbide powder was made up of the following
powdered ingredients:
Tungsten Monocarbide 87.50% by weight Cobalt 12.15% by weight
Paraffin Wax 0.35% by weight
The powdered ingredients were ground together in a jar mill
containing naphtha with paraffin wax in solution until reduced to
about 1.18 Fisher subsieve particle size and then dried. It
contained about 0.35 percent by weight of paraffin wax after
drying.
The dried powder was then mixed with liquid vehicle solution of the
composition described under Example I, in the proportion of 85
milliliters of solution to 1 kilogram of powder. The resulting
slurry was milled in a tungsten carbide lined jar mill for 3 days
at 115.degree. F. after which it was ready for centrifuging to form
compacts.
The centrifuging equipment was the same as that used in Example I,
and a polyvinyl alcohol liner member was used as in Example I.
Rotational speed about the main axis of rotation was 530
revolutions per minute producing a force of 177 times G and the
flask was rotated about its own axis at 53 revolutions per minute.
Centrifuging time was about 20 hours and temperature was 95 to
105.degree. F.
Upon completion of centrifuging, the compacts were processed as in
Example I except that sintering temperature was 2,575.degree.
F.
Conventional hydropressed compacts were made from the same
composition for comparison as described under Example I.
Properties obtained by the centrifugal method of this invention as
compared to properties obtained by conventional hydropressing are
given in the tables which follow. The conventional compact was
hydropressed at 50,000 pounds per square inch; the Centrifugal
Compact was not hydropressed.
TABLE I ______________________________________ TRANSVERSE RUPTURE
STRENGTH IN LBS. PER SQ. IN./1000 Method Used Conventional
Centrifugal Compaction Compaction
______________________________________ Lowest Value 422 452 Highest
Value 481 504 Average Value 462 478 Hardness -- Rockwell A 88.0
88.1 ______________________________________
TABLE II ______________________________________ MACRO PIT AND FLAW
COUNT Method Used Conventional Centrifugal Compaction Compaction
______________________________________ Total Pits and Flaws per 100
square inches .002 inches and 10 larger in diameter 37.7 2.7 .004
inches and larger in diameter 6.8 1.8 Total Area Examined -- Square
Inches 103.4 110.0 ______________________________________
TABLE III ______________________________________ SHRINKAGE FACTORS
Method Used Conventional Centrifugal Compaction Compaction
______________________________________ Isostatic Pressure used in
pounds per square inch No Pressure Used -- 1.142 to 1.150 35,000 --
1.137 to 1.141 50,000 1.180 to 1.187 --
______________________________________
With conventional isostatic compaction the lowest shrinkage factor
was 1.180 corresponding to 60.9 percent of theoretical density.
With triaxial centrifugal compaction densities ranged from 65.8 to
68.0 percent of theoretical.
* * * * *