US2972524A - Crystallizing centrifuge - Google Patents

Crystallizing centrifuge Download PDF

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US2972524A
US2972524A US695267A US69526757A US2972524A US 2972524 A US2972524 A US 2972524A US 695267 A US695267 A US 695267A US 69526757 A US69526757 A US 69526757A US 2972524 A US2972524 A US 2972524A
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ring
crucible
carbon
axis
rotation
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Ross John
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B04CENTRIFUGAL APPARATUS OR MACHINES FOR CARRYING-OUT PHYSICAL OR CHEMICAL PROCESSES
    • B04BCENTRIFUGES
    • B04B5/00Other centrifuges
    • B04B5/12Centrifuges in which rotors other than bowls generate centrifugal effects in stationary containers
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00Carbon; Compounds thereof
    • C01B32/25Diamond
    • C01B32/26Preparation
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10TTECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T117/00Single-crystal, oriented-crystal, and epitaxy growth processes; non-coating apparatus therefor
    • Y10T117/10Apparatus
    • Y10T117/1024Apparatus for crystallization from liquid or supercritical state
    • Y10T117/1096Apparatus for crystallization from liquid or supercritical state including pressurized crystallization means [e.g., hydrothermal]

Definitions

  • This invention relates to a method and apparatus for producing crystals having a hardness, on the Mohsscale, equal to diamond, i.e., to 10.6 on said scale.
  • the present method approaches the problem of syn- 1 thesis of diamond-hard carbon crystals by causing molten carbon to separate by precipitation out of solution with either silver or iron, the two metals that are solvents of carbon. Accordingly, it is an object of this invention to provide a method for producing carbon by precipitation, as above indicated.
  • Another object of the invention is to employ centrifugal force to effect such precipitation, the force being effective in all directions rather than being uni-planar.
  • a corollary object is to provide novel apparatus to produce such centrifugal force so that the precipitation of the carbon can be effected by centrifugal force in an infinite number of directions.
  • Another object of the invention is to precipitate carbon as above indicated, in the presence of high heat and while enclosed in a restricted crucible cavity, the invention contemplating provision of such heat during universal centrifuging as above.
  • Fig. l is a front elevational view of a centrifuge for carrying out the contemplated precipitation and crystallizing of carbon.
  • Fig. 2 is a top plan view thereof in a different position.
  • Fig. 3 is an enlarged fragmentary longitudinal view of a crucible used in the centrifuge.
  • Fig. 4 is a cross-sectional view as taken on line 4-4 of Fig. 3.
  • a mechanical mix comprising 90% carbon and 10% silver by volume, both in powdered form, is placed in a relatively small chamber and subjected to both heat and centrifugal force.
  • the carbon content may vary and may be as high as 95% and as low as the hardness of the resultant crystal would vary accordingly, being harder when the proportion of carbon is higher.
  • the chamber is preferably substantially filled with Patented Feb. 21, 1961 these two ingredients and the same is subjected to heat which is preferred to be at 3500 F. and may vary between 2300 F. minimum and 5000 F. maximum.
  • the speed of the apparatus will, of course, depend on its size and the force achieved on the mass being centrifuged, 3000 rpm. is deemed to provide the force desired in apparatus of the type illustrated.
  • present method separates or precipitates carbon from solution in silver or iron by the simultaneous application of heat and centrifugal force and, thereby crystallizing the carbon in the process.
  • the apparatus there illustrated comprises, generally a support 5, an outer gimbal ring 6' mounted to rotate in said support on one axis, means 7 to drive the ring 6, an inner gimbal ring 8 mounted to rotate on a transverse axis in said ring 6, means 9 to drive ring 8, a crucible 10 carried by the inner gimbal ring, means 11 to heat said crucible, and means 12 to bring electric current to the means 9 and 11.
  • the support 5 is shown as a pair of bearings 15 that are arranged in alignment as shown and, while shown as separated, may be made as part of a base frame. In any case, said bearings are spaced to accommodate the outer gimbal ring 6.
  • Said outer ring is shown with aligned oppositely directed trunnions 16 that are disposed in bearings 15 and are provided with thrust bearings 17, arranged in opposition, to center the ring between said bearings.
  • the outer ring is shown as of rectangular form and may have the desired mass to provide forces of inertia during rotation around the axis of trunnions 16.
  • the drive means 7 is shown as an electric motor 18 and a drive connection 19 between said motor and one trunnion 16 which may be extended for the purpose.
  • a belt and pulley drive connection is shown although, a chain drive, etc. may be used.
  • the inner gimbal ring 8 is shown with aligned trunnions 20 disposed in bearings 21 provided in ring 6, the axis of trunnions 20 being normal to the axis of trunnions 16 of the outer ring. Thrust bearings 22, arranged in opposition, center ring 8 between its bearings.
  • the drive 9 is shown as an electric motor 23 carried by ring 6 and a gearing connection 24 between said motor and one of the trunnions 20.
  • the crucible 10 preferably'comprises a solidly massive and elongated body comprising two separate parts 25 and 26, each provided with half of a spherical cavity 27. Said parts 25 and 26 are connected by threads 28. Since the crucible is subject to high heat, the same may be made of a material suitably resistant to melting or disintegration under the heat used. One alloy suggested for this purpose is ferrozirconium.
  • the crucible is removably mounted in ring 8, as shown, such mounting comprising end caps 29 of heat insulating material, threaded studs 30 on said caps, and threaded bearings 31 in diametrally opposite parts of ring 8 and receptive of said studs. Set screws 32 may be used to lock the studs after adjustment of caps 29 to crucible-holding position, as in Fig. 1.
  • the means 11 may preferably be of the electrical'induction type and the same is here represented as a coil 33 surrounding the portion of the crucible in which the chamber or cavity 27 is provided.
  • Means 12 shows a system of siip ring means 34 and 35 to bring currentfrom any outer part, such as one bearing 15, firstto the outer ring 6, and then, from the latter, to theinner ring 3 and the means 11. While the wires or conduotors, in the main, have' been omitted, the manner of their provision shouldbe clear.
  • vibration dampers may be incorporated in the device; a speed indicator, such as a tachometer, may measure the speed of one or both rings, etc.
  • Apparatus oi the character described comprising an outer gimbal ring having an axis of rotation, an inner gimbal ring .on an axis of rotation transverse to the axis of rotation of the outer ring and carried by the latter, a seaied crucible carried by the inner ring and subject to the compound movement of rotation of said inner ring, and electrical heating means to heat the crucible, and means to drive each ring independently of the other, said driving means including a driving member carried by the outer ring and having driving engagement with the inner ring.
  • a centrifuging device comprising outer and inner gimbal rings on two respectively transverse axes, means to rotate each ring around its axis, the inner ring being carried by theouter ring and subject to the centrifugal force imparted thereto by rotation of both rings and completely closed crucible removably carried by said inner ring, the means to rotate one ring being independent of the means to rotate the other ring.
  • a centrifuging device comprising outer and inner gimbal rings on two respectively transverse axes, electrically powered means to rotate each ring independently of the other, around its own axis, the inner ring being rotatably carried by the outer ring, a completely sealed, removabie crucible carried by the inner ring and subject to the centrifugal forces imparted thereto by rotation of both rings, themeans for rotating the inner ring comprising an electric motor carried by the outer ring, power transmission means operatively connecting said electric motor to a trunnion of the inner ring to rotate said inner ring relative to said outer ring, slip ring means to conduct electric current to the means for rotating the inner ring, said latter means being provided between the outer and inner rings and an electrical heater coil embracing said crucible.

Description

Feb. 21, 1961 J. Ross ORYSTALLIZING CENTRIFUGE Filed Nov. 8, 1957 IINVENTOR JOHN R055.
2 Sheets-Sheet 1 ATTORNEK Feb. 21,1961 J, Ross 2,972,524
' CRYSTALLIZING CENTRIFUGE Filed Nov. 8, 1957 2 Sheets-Sheet z INVENTOR.
JOHN K055.
United States Patent 2,97 2,524 CRYSTALLIZING CENTRIFUGE John Ross, Mount Vernon, N. (3701 Henry Hudson Parkway, New York 63, NY.)
Filed Nov. 8, 1957, Ser. No. 695,267 3 Claims. (Cl. 23-273) This invention relates to a method and apparatus for producing crystals having a hardness, on the Mohsscale, equal to diamond, i.e., to 10.6 on said scale.
Synthesis of diamond crystals have been attempted and, although the avenues of approach are few since methods used in connection with the synthetic production of lesser hard crystals, corundum, for instance, some attempts have been made to produce crystals of carbon by using a mixture of hydrocarbons and metallic lithium in an enclosed iron chamber, by creating high pressures resulting from the sudden cooling and the resulting rapid contraction of a mass of dissolved carbon in molten iron, and in other analogous ways. ,All either failed completely to produce hard crystalline carbon or, at enormous expense, produced microscopic crystals having little or no intrinsic value.
The present method approaches the problem of syn- 1 thesis of diamond-hard carbon crystals by causing molten carbon to separate by precipitation out of solution with either silver or iron, the two metals that are solvents of carbon. Accordingly, it is an object of this invention to provide a method for producing carbon by precipitation, as above indicated.
Another object of the invention is to employ centrifugal force to effect such precipitation, the force being effective in all directions rather than being uni-planar. A corollary object is to provide novel apparatus to produce such centrifugal force so that the precipitation of the carbon can be effected by centrifugal force in an infinite number of directions.
Another object of the invention is to precipitate carbon as above indicated, in the presence of high heat and while enclosed in a restricted crucible cavity, the invention contemplating provision of such heat during universal centrifuging as above.
The foregoing and other objects, features and advantages of the invention will be more fully realized as the following description of preferred stepsof the method and of preferred apparatus for carrying out the method progresses, the same having basis on the accompanying drawings, in which:
Fig. l is a front elevational view of a centrifuge for carrying out the contemplated precipitation and crystallizing of carbon.
Fig. 2 is a top plan view thereof in a different position.
Fig. 3 is an enlarged fragmentary longitudinal view of a crucible used in the centrifuge.
Fig. 4 is a cross-sectional view as taken on line 4-4 of Fig. 3.
In practice, a mechanical mix comprising 90% carbon and 10% silver by volume, both in powdered form, is placed in a relatively small chamber and subjected to both heat and centrifugal force. The carbon content may vary and may be as high as 95% and as low as the hardness of the resultant crystal would vary accordingly, being harder when the proportion of carbon is higher.
The chamber is preferably substantially filled with Patented Feb. 21, 1961 these two ingredients and the same is subjected to heat which is preferred to be at 3500 F. and may vary between 2300 F. minimum and 5000 F. maximum.
After the heat has been applied for a time suflicient to liquefy both ingredients, the same are subjected to 'the pressure generated by centrifugal force as applied by the apparatus herein disclosed.
The speed of the apparatus will, of course, depend on its size and the force achieved on the mass being centrifuged, 3000 rpm. is deemed to provide the force desired in apparatus of the type illustrated.
While silver is preferred as the metal, in solution, from which the carbon is precipitated, iron may be used. The
present method separates or precipitates carbon from solution in silver or iron by the simultaneous application of heat and centrifugal force and, thereby crystallizing the carbon in the process.
The silver being the heavier, the same will separate from the carbon and line the chamber walls, the carbon, being confined to the center of said chamber, crystallizes under the force imposed thereon.
Referring now to the drawings, the apparatus there illustrated comprises, generally a support 5, an outer gimbal ring 6' mounted to rotate in said support on one axis, means 7 to drive the ring 6, an inner gimbal ring 8 mounted to rotate on a transverse axis in said ring 6, means 9 to drive ring 8, a crucible 10 carried by the inner gimbal ring, means 11 to heat said crucible, and means 12 to bring electric current to the means 9 and 11. The support 5 is shown as a pair of bearings 15 that are arranged in alignment as shown and, while shown as separated, may be made as part of a base frame. In any case, said bearings are spaced to accommodate the outer gimbal ring 6.
Said outer ring is shown with aligned oppositely directed trunnions 16 that are disposed in bearings 15 and are provided with thrust bearings 17, arranged in opposition, to center the ring between said bearings. The outer ring is shown as of rectangular form and may have the desired mass to provide forces of inertia during rotation around the axis of trunnions 16.
The drive means 7 is shown as an electric motor 18 and a drive connection 19 between said motor and one trunnion 16 which may be extended for the purpose. A belt and pulley drive connection is shown although, a chain drive, etc. may be used.
The inner gimbal ring 8 is shown with aligned trunnions 20 disposed in bearings 21 provided in ring 6, the axis of trunnions 20 being normal to the axis of trunnions 16 of the outer ring. Thrust bearings 22, arranged in opposition, center ring 8 between its bearings.
The drive 9 is shown as an electric motor 23 carried by ring 6 and a gearing connection 24 between said motor and one of the trunnions 20.
The crucible 10 preferably'comprises a solidly massive and elongated body comprising two separate parts 25 and 26, each provided with half of a spherical cavity 27. Said parts 25 and 26 are connected by threads 28. Since the crucible is subject to high heat, the same may be made of a material suitably resistant to melting or disintegration under the heat used. One alloy suggested for this purpose is ferrozirconium. In practice, the crucible is removably mounted in ring 8, as shown, such mounting comprising end caps 29 of heat insulating material, threaded studs 30 on said caps, and threaded bearings 31 in diametrally opposite parts of ring 8 and receptive of said studs. Set screws 32 may be used to lock the studs after adjustment of caps 29 to crucible-holding position, as in Fig. 1.
The means 11 may preferably be of the electrical'induction type and the same is here represented as a coil 33 surrounding the portion of the crucible in which the chamber or cavity 27 is provided.
It is evident that current can be brought to motor 9 and coil 33 in usual ways. Means 12, for example, shows a system of siip ring means 34 and 35 to bring currentfrom any outer part, such as one bearing 15, firstto the outer ring 6, and then, from the latter, to theinner ring 3 and the means 11. While the wires or conduotors, in the main, have' been omitted, the manner of their provision shouldbe clear.
Aiso, instrumentation, not forming part of this invention, may be used. Thus, vibration dampers may be incorporated in the device; a speed indicator, such as a tachometer, may measure the speed of one or both rings, etc.
Since variations of the invention may well be made,
1 desire to reserve to myself all modifications thereof that may fall within the spirit and scope of the appended claims. I
Havingthus described my invention, what I claim as new and desire to secure by Letters Patent is:
1. Apparatus oi the character described comprising an outer gimbal ring having an axis of rotation, an inner gimbal ring .on an axis of rotation transverse to the axis of rotation of the outer ring and carried by the latter, a seaied crucible carried by the inner ring and subject to the compound movement of rotation of said inner ring, and electrical heating means to heat the crucible, and means to drive each ring independently of the other, said driving means including a driving member carried by the outer ring and having driving engagement with the inner ring.
2.'A centrifuging device comprising outer and inner gimbal rings on two respectively transverse axes, means to rotate each ring around its axis, the inner ring being carried by theouter ring and subject to the centrifugal force imparted thereto by rotation of both rings and completely closed crucible removably carried by said inner ring, the means to rotate one ring being independent of the means to rotate the other ring.
3. A centrifuging device comprising outer and inner gimbal rings on two respectively transverse axes, electrically powered means to rotate each ring independently of the other, around its own axis, the inner ring being rotatably carried by the outer ring, a completely sealed, removabie crucible carried by the inner ring and subject to the centrifugal forces imparted thereto by rotation of both rings, themeans for rotating the inner ring comprising an electric motor carried by the outer ring, power transmission means operatively connecting said electric motor to a trunnion of the inner ring to rotate said inner ring relative to said outer ring, slip ring means to conduct electric current to the means for rotating the inner ring, said latter means being provided between the outer and inner rings and an electrical heater coil embracing said crucible.
References Cited in the file of this patent UNITED. STATES PATENTS 1,320,910 Perry Nov. 4, 1919 1,420,512 Baily June 20, 1922 1,637,291 Barnett July 26, 1927 1,658,084 Hudson Feb. 7, 1928 2,659,107 De Bell Nov. 17, 1953 2,740,176 Duval Apr. 3, 1956 2,811,747 Belz Nov. 5, 1957 FOREIGN PATENTS 1,308 Great Britain 1855

Claims (1)

1. APPARATUS OF THE CHARACTER DESCRIBED COMPRISING AN OUTER GIMBAL RING HAVING AN AXIS OF ROTATION, AN INNER GIMBAL RING ON AN AXIS OF ROTATION TRANSVERSE TO THE AXIS OF ROTATION OF THE OUTER RING AND CARRIED BY THE LATTER, A SEALED CRUCIBLE CARRIED BY THE INNER RING AND SUBJECT TO THE COMPOUND MOVEMENT OF ROTATION OF SAID INNER RING, AND ELECTRICAL HEATING MEANS TO HEAT THE CRUCIBLE, AND MEANS TO DRIVE EACH RING INDEPENDENTLY OF THE OTHER, SAID DRIVING MEANS INCLUDIN A DRIVING MEMBER CARRIED BY THE OUTER RING AND HAVING DRIVING ENGAGEMENT WITH THE INNER RING.
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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3778215A (en) * 1972-09-01 1973-12-11 Container Corp Rotational moulding machine with inner and outer mold cages rotating about intersecting axes
US4010020A (en) * 1970-09-03 1977-03-01 Stephen Wyden Apparatus for forming curved surfaces by rotation
US4273608A (en) * 1979-01-04 1981-06-16 Kerlin Allen L Method of forming a sheet of single crystal semiconductor material

Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US1320910A (en) * 1919-01-29 1919-11-04 William John Perry Molding-machine.
US1420512A (en) * 1922-01-31 1922-06-20 Thaddeus F Baily Process of producing graphite
US1637291A (en) * 1923-10-06 1927-07-26 Leon H Barnett Method of producing gem materials
US1658084A (en) * 1925-06-25 1928-02-07 Hudson Alden Pattern elimination for molds
US2659107A (en) * 1947-11-14 1953-11-17 Bell George W De Method of making hollow plastic articles
US2740176A (en) * 1952-06-14 1956-04-03 Max Adolphe Bunford Means for centrifugal molding
US2811747A (en) * 1953-06-15 1957-11-05 Lloyd H Belz Centrifugal casting machines

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US1320910A (en) * 1919-01-29 1919-11-04 William John Perry Molding-machine.
US1420512A (en) * 1922-01-31 1922-06-20 Thaddeus F Baily Process of producing graphite
US1637291A (en) * 1923-10-06 1927-07-26 Leon H Barnett Method of producing gem materials
US1658084A (en) * 1925-06-25 1928-02-07 Hudson Alden Pattern elimination for molds
US2659107A (en) * 1947-11-14 1953-11-17 Bell George W De Method of making hollow plastic articles
US2740176A (en) * 1952-06-14 1956-04-03 Max Adolphe Bunford Means for centrifugal molding
US2811747A (en) * 1953-06-15 1957-11-05 Lloyd H Belz Centrifugal casting machines

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4010020A (en) * 1970-09-03 1977-03-01 Stephen Wyden Apparatus for forming curved surfaces by rotation
US3778215A (en) * 1972-09-01 1973-12-11 Container Corp Rotational moulding machine with inner and outer mold cages rotating about intersecting axes
US4273608A (en) * 1979-01-04 1981-06-16 Kerlin Allen L Method of forming a sheet of single crystal semiconductor material

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