US3461943A - Process for making filamentary materials - Google Patents

Process for making filamentary materials Download PDF

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US3461943A
US3461943A US587009A US3461943DA US3461943A US 3461943 A US3461943 A US 3461943A US 587009 A US587009 A US 587009A US 3461943D A US3461943D A US 3461943DA US 3461943 A US3461943 A US 3461943A
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filament
jet
molten
cooling
gas
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US587009A
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Richard D Schile
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Raytheon Technologies Corp
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United Aircraft Corp
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    • C04B35/62227—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products obtaining fibres
    • C04B35/62272—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products obtaining fibres based on non-oxide ceramics
    • C04B35/62277—Fibres based on carbides
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
    • B22D11/00—Continuous casting of metals, i.e. casting in indefinite lengths
    • B22D11/005—Continuous casting of metals, i.e. casting in indefinite lengths of wire
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    • C03B37/01—Manufacture of glass fibres or filaments
    • C03B37/02—Manufacture of glass fibres or filaments by drawing or extruding, e.g. direct drawing of molten glass from nozzles; Cooling fins therefor
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    • Y10S264/19—Inorganic fiber

Definitions

  • This application relates to a method of manufacturing fibers and filaments directly from a molten starting material. More particularly, it relates to the rapid cooling of molten filaments to yield satisfactory, coherent fibers and filaments.
  • fibers and filaments of some materials can be produced by melting the desired material in a crucible and forcing the molten material through an orifice in the crucible.
  • fibers can be formed by permitting the extruded jet of molten material to cool by free fall through an essentially stagnant gas atmosphere.
  • the cooling rate required to form fibers of a given material is a unique function of the physical properties of the material and of the diameter of the molten jet.
  • the use of the rapid cooling methods of this invention permits the carrying out of chemical reactions with the molten filament to produce coatings on or alloying or reactions with the molten filament prior to cooling.
  • the use of the rapid cooling techniques in conjunction with the reaction techniques facilitates the control of the reaction.
  • the cooling methods of this invention require that the molten filament be cooled at a rate between about 0.001 to 0.04 calories per second per square centimeter per degree Centigrade.
  • the required cooling rate can be determined more precisely but still only approximately by use of the following formula, it being understood that the precise rate is best determined through trial and error using the approximation as a convenient starting point:
  • the filaments used in this invention are produced by melting a metal, such as titanium, in a crucible provided with an orifice whose size and shape conform to the configuration desired of the filament and then pressuring the crucible with a suitable inert gas or fluid or other pressuring means, such as a mechanical piston, to thereby force molten metal through the orifice in a substantially downwardly and vertical direction.
  • a metal such as titanium
  • a preferred method of rapid cooling in accordance with this invention involves the use of a plurality of gas jets located such that gas impinges laterally in one direction on the molten filament, coupled with a means for electrostatically attracting the filament toward the gas source.
  • Lateral gas flow has been found to be the only type of flow which does not appreciably disturb the molten metal jet and cause it to disintegrate int-o droplets.
  • a flow of cooling gas longitudinally along the axis of the molten jet causes rapid droplet formation.
  • a convenient means for eelctrostatic attraction is to cause the jet to bear an electrical charge of one polarity and to cause a fixed object located apart therefrom, such as the gas blowing means, to bear a charge of the opposite polarity.
  • the gas jets would push the molten filament in one direction (i.e., away from the gas source), while the electrostatic charge would cause the filament to be pushed in the 0pposite direction (i.e., toward the gas source).
  • the electrostatic force of attraction is required in order to maintain the molten jet in a fixed position with respect to the gas discharge, otherwise the jet would be displaced to a region of lower gas velocity and lower cooling rate.
  • any inert gas which is non-reactive with the filament under the conditions of operation can be employed as the cooling medium for use in the gas jets.
  • the coolant gas be provided in a plurality of air streams transverse to the filament, one above the other in the same vertical direction along the axis of the molten jet.
  • the length of the gas stream i.e., the number of individual jets located one above the other depends to a large extent upon the rapidity of cooling desired and the temperatures involved as well as the practical problem of being able to conveniently maintain an adequate electrical charge over the entire distance of cooling.
  • a cooling distance of from about six inches to four feet can be employed satisfactorily.
  • the velocity of the cooling gas impinging on the molten filament can vary with the degree of cooling required and the various heat transfer coefiicients, but will generally be in the range from about ten to fifty feet per second.
  • a suitable means of applying the cooling gas is to cause the gas to flow, under suitable pressure through a metal tube having a porous wall opposite the filament.
  • the radial gas velocity through a porous tube decreases with the distance from the tube surface in such a way that the aerodynamic drag, in conjunction with the electrostatic force acting in the molten jet allows a stable balancing of the two forces. In this way, slight accidental variations in the position of the molten jet automatically give rise to corrective forces which return the jet to the desired position.
  • the combination of a porous cylindrical gas nozzle and electrostatic field is unique in this respect.
  • the electrostatic force is produced by applying a direct current voltage between the molten filament and the surface of the metal tube through which the cooling gas flows. Electrical connection to the filament is preferably made through the melt in the crucible.
  • the precise voltage for use with any air velocity and volume can easily be determined by conventional calculations or by trial and error through varying impressed voltage until a stable position of the filament is achieved.
  • This method of cooling is most advantageous in forming filaments of very high temperature materials. Filament formation is best accomplished if the cooling takes place as close to the crucible orifice as possible. Since the cooling gas may be circulated by the electric field generated by a very fine wire electrode, the problems associated with the use of gas nozzles and other cooling equipment at very high temperatures is avoided. In addition, if the material which is to be converted into fiber is heated by means of an induction coil, all parts in the vicinity of the coil must be nonconductors of electricity in order to avoid undesirable heating of these parts and loss of power from the coil. The corona generating electrode, however, may be placed even within the induction coil with no heating whatsoever.
  • flux particles rather than inert gas can 4 be placed in the vicinity of the filament. These particles can be ionized and caused to be attracted to the filament, in which case upon contact with the filament, the cooler flux particles absorb heat from the filament.
  • the flux particles must be electrically charged by passing them through a region containing unipolar ions. This may be accomplished by placing a fine wire adjacent the jet and connecting a high voltage D.C. power supply between the melt and this elect-rode such that the electrode (charging electrode) is negative. The voltage is then adjusted so that a corona discharge occurs at the negative electrode but not at the molten jet. A stream of negative gas ions then flows across the space between the charging electrode and the jet. Flux particles are introduced into this ionization region, are negatively charged by collision with the gas ions and are attracted to and deposited on the jet. Alternatively, the flux particles can be charged by passing them through an ionization region between two fixed electrodes and then collected on the molten jet which is maintained at a lower positive potential in order to prevent back-ionization at the jet.
  • Representative fiux particles include the following:
  • the flux particles can be introduced to the ionization zone in the form of a fine powder sprayed periodically or continuously into the ionization region in the form of a suspension in an inert gas.
  • the flux particles should be inert to the filament material and also should not ionize at the filament temperature.
  • the flux should have a melting point somewhat lower than that of the filament forming material in order that the flux particles melt on contact with the molten jet and thus absorb from the jet the heat equal to the latent heat of the flux. Good deposition is obtained if the flux particles have an average diameter of 20 microns or smaller.
  • the inert flux particles can be permitted to remain on the filament surface. For other purposes, they can be removed by a suitable chemical aftertreatment.
  • the flux particles reactive with the filament, as indicated below so that the flux particles act as both reactant and coolant.
  • the filament Prior to cooling with subsequent solidification of the molten filament, the filament can be contacted with a reactant at a concentration and of a type adequate to form a refractory fiber or other reaction product.
  • Reactants thus employed can be either a gas or a finely divided solid, e.g., boron carbide filaments can be made by forming a filament of molten boron and then introducing graphite in the form of a suspension of powdered graphite in an inert gas. Graphite reacts with the molten boron very rapidly under these conditions to form boron carbide. The same reaction can occur if a gaseous reactant such as methane is employed in place of the graphite.
  • titanium boride filaments can be made by using as the molten material either boron or titanium and then introducing correspondingly either titanium or boron to the reaction zone as a finely divided powder.
  • the speed of the reaction can be accelerated if a corona discharge as indicated previously is simultaneously caused to occur about the molten filament.
  • the use of the corona discharge will at this time in addition to accelerating the reaction, also serve to cool the filament thereby acting as a composite reaction and cooling step.
  • an inert flux can the deposited to cool the reaction product and/ or stop the reaction at the desired time.
  • Suitable metals that can be employed as the filamentary material in the practice of the invention include any fiber forming metal including preferably, nickel, chromium and chromium alloys, stainless steel, beryllium, boron, titanium, and non-metallic fibrous materials such as aluminum oxide alone or in mixture With magnesium oxide and/or silicon dioxide or with calcium oxide and silicon dioxide.
  • the reaction plus cooling concept is particularly applicable when the molten material is a eutectic alloy of two (or more) metals and the material which is electrostatically deposited on the molten jet is either one of these metals or a compound of both of them.
  • the electrostatically deposited material dissolves in and/or reacts with the molten metal in the jet to produce an alloy which has a higher liquidus temperature than the metal in the crucible.
  • the final product is an alloy which could not have been melted and contained in any existing crucible.
  • Vanadium+15 atomic Boron or vanadium boride Vanadium+15 atomic Boron or vanadium boride.
  • fibers formed from Mn-l-Bi when fiberized at high cooling rates have a fine enough grain structure so that subsequent heat treatment of the fiber will result in the conversion of the fibers to Cb Sn or MnBi, respectively.
  • Other compounds that can be formed through the rapid cooling techniques of this invention include BaTiO and KCbO as well as the eutectic between BaFe O and BaFe O
  • This invention is not limited .to those metals which cannot conveniently be formed into filaments at low cooling rates.
  • Certain metals which form coherent oxide films in air can be made into wire at low cooling rates.
  • the use of the higher cooling rates of this invention results in smoother wire and fewer kinks, bumps and bends.
  • the grain size decreases as the cooling rate is increased, resulting in a more homogeneous product.
  • FIGURE 1 represents a schematic view of a cooling operation performed on a molten filament using the balanced system of gas flow and electrical attraction.
  • FIGURE 2 represents a schematic View of a cooling operation performed on a molten filament using a corona discharge.
  • FIGURE 3 represents a schematic view of a cooling or combined cooling reacting operation performed on a molten filament using the introduction of flux particles and a corona discharge.
  • a high voltage supply is arranged so that the crucible and through it the molten filament is negatively charged while the porous metal tube is positively charged.
  • the voltage employed is correlated with the gas fiow to prevent lateral displacement of the filament, i.e., the lateral translation of the filament to the right due to the gas flow must equal its lateral translation to the left due to the electrical attraction, resulting in a net translation of zero.
  • electrodes are provided of a polarity opposite to that of the filament with a voltage high enough to cause a corona discharge.
  • FIGURE 3 a corona discharge occurs at the negative electrode with the introduction of fiux particles which are ionized at the ionizing wire as described above.
  • EXAMPLE 1 A cooling tube was prepared having an outside diameter 1 /2 inches, wall thickness of inch and a length of 24 inches. This tube was hot pressed from micron diameter stainless steel powder and seam welded into a porous tubular form. Air was supplied through this ⁇ tube by means of /2 horse power centrifugal blower operating at 12,000 r.p.m.
  • a crucible was prepared containing molten tin, maintained at a temperature above the melting point of tin, and provided with a small aperture through which molten tin was forced in the form of a downwardly flowing molten filament of diameter .005".
  • the velocity of the downwardly moving tin filament was approximately 600 feet per minute.
  • the top of the cooling tube was located 4 inches below the orifice of the crucible. Air was caused to impinge on the tin jet from the cooling tube at a rate of 53 cubic feet per minute. Simultaneously, electrical contact was made at the crucible and at the cooling tube with 1,100 volts of direct current.
  • the electrodes were set so that the cooling tube was positively charged and the jet making electrical contact through the crucible was negatively charged.
  • the jet was located approximately inch from the surface of the cooling tube as this was found to be its stable position. The jet was observed to flow vertically without any lateral movement due to the air blast.
  • EXAMPLE 2 A jet of molten boron of .003" diameter is caused to fiow from a crucible. The jet is charged positively through electrical connections at the crucible. A negative electrode is provided spaced 1% inch from the jet and 12 inches below the crucible. A mixture of propane and boron trichloride is injected just below the crucible, causing a layer of boron carbide to be chemically deposited on the surface of the boron jet. At 12 inches below the crucible an aerosol of finely powdered quartz suspended in a gaseous mixture of helium and boron trichloride is injected. At an electrode potential of 6000 volts, the silica powder is deposited on the jet, stopping the deposition of boron carbide and cooling the jet. The product is boron carbide fiber with a silica coating.
  • EXAMPLE 3 A jet of molten chromium of .002" diameter is caused to flow from a crucible.
  • the jet is positively charged and a negative electrode 12" long is positioned just below the crucible as described in Example 2.
  • a negative electrode 12" long is positioned just below the crucible as described in Example 2.
  • an aerosol of finely powdered silica suspended in helium is injected so as to flow parallel to the jet.
  • the silica powder is deposited on the jet, cooling it and at the same time forming a glass coating over the chromium.
  • a method of producing a continuous filament comprising forcing molten material through an orifice having substantially the diameter desired of the filament to form a jet of approximately the desired filament diameter and rapidly cooling the molten jet to produce a solid filament without causing appreciable oxidation by unidirectionally impinging a gas upon the molten pet in a direction substantially perpendicular thereto while simultaneously creating an electrostatic charge whose tendency is to push the jet in a direction opposite to the direction of gas flow, and correlating the rate of gas fiow with the magnitude of the electrostatic charge to substantially prevent lateral displacement of the jet.
  • a method of producing a continuous filament comprising forcing molten material through an orifice having substantially the diameter desired of the filament to form a jet of approximately the desired filament diameter and rapidly cooling the molten jet to produce a solid filament without causing appreciable oxidation by causing charged particles to impinge upon the surface of the molten jet, the rate of cooling being sufliciently rapid to prevent breakup of the filament and consequent droplet formation.
  • a method of producing a continuous filament comprising forcing molten material through a norifice having substantially the diameter desired of the filament to form a jet of approximately the desired filament diameter and rapidly cooling the molten jet to produce a solid filament without causing appreciable oxidation by causing charged particles to impinge on the surface of the molten jet by causing the jet to bear an electrical charge of one polarity and supplying flux particles to an ionization zone located between the said molten jet and a surface bearing an electrical charge of an opposite polarity, whereby said flux particles become electrically charged and are attracted to the jet.
  • a method of producing a continuous filament comprising forcing molten material through an orifice having substantially the diameter desired of the filament to form a jet of approximately the desired filament diameter and rapidly cooling the molten jet to produce a solid filament without causing appreciable oxidation by causing the formation of a corona discharge about the molten jet, in a substantially inert atmosphere, thereby causing a gas flow in the vicinity of the jet and the consequent removal of heat by convection from the jet.
  • corona discharge is created by imparting a negative electrical charge to the jet which is maintained in an atmosphere of an inert gas and spaced apart from an electrode to which is imparted a corresponding positive charge, the resulting negative charge causing negative ions of the inert gas to flow away from the jet toward the electrode, thereby setting up convection currents.
  • a method of producing a continuous filament of refractory fiber comprising forcing molten material through an orifice having substantially the diameter desired of the filament to form a jet of approximately the desired filament diameter, contacting the jet with a reactant of a type and at a concentration capable of reacting thcrewith to form a refractory material and thereafter rapidly cooling the molten jet to produce a solid filament without causing appreciable oxidation.

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Cited By (17)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3581040A (en) * 1969-06-11 1971-05-25 Inland Steel Co Forming of thin metal filaments
US3602291A (en) * 1968-09-04 1971-08-31 Battelle Development Corp Apparatus for casting metal filaments through an aerosol atmosphere
US3720741A (en) * 1969-10-03 1973-03-13 Monsanto Co Melt spinning process
DE2364131A1 (de) 1972-12-26 1974-06-27 Allied Chem Amorphe metall-legierung und deren verwendung
US3824052A (en) * 1971-04-15 1974-07-16 Deering Milliken Res Corp Apparatus to produce nonwoven fabric
US3834847A (en) * 1970-01-16 1974-09-10 Du Pont Open cell foam device for gas distribution in filament quenching chimneys
US4178985A (en) * 1977-01-10 1979-12-18 Compagnie Generale Des Etablissements Michelin Installation for manufacturing a metal wire by continuous casting
EP0007581A1 (de) * 1978-07-28 1980-02-06 Kennecott Corporation Giessformanordnung und Verfahren zum Stranggiessen von metallischen Drahtlitzen bei aussergewöhnlich hohen Geschwindigkeiten
US4266918A (en) * 1978-03-13 1981-05-12 Pulp And Paper Research Institute Of Canada Apparatus for electrostatic fibre spinning from polymeric fluids
EP0066896A1 (de) * 1981-06-10 1982-12-15 Olin Corporation Einrichtung und Verfahren zum Kühlen und Erstarren von voll- oder halb-kontinuierlichem Stranggussmaterial
US4441542A (en) * 1981-06-10 1984-04-10 Olin Corporation Process for cooling and solidifying continuous or semi-continuously cast material
US4557742A (en) * 1984-07-02 1985-12-10 Polaroid Corporation Polarized optical fiber and method of forming same
US4614221A (en) * 1981-09-29 1986-09-30 Unitika Ltd. Method of manufacturing thin metal wire
US4736789A (en) * 1978-07-28 1988-04-12 Kennecott Corporation Apparatus and method for continuous casting of metallic strands at exceptionally high speeds using an oscillating mold assembly
USRE32925E (en) * 1972-12-26 1989-05-18 Allied-Signal Inc. Novel amorphous metals and amorphous metal articles
US20080047736A1 (en) * 2006-08-25 2008-02-28 David Levine Lightweight composite electrical wire
WO2015145420A1 (en) 2014-03-26 2015-10-01 Keshet Itamar Nut and method for fixing an object to a building structure

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107324816A (zh) * 2017-07-25 2017-11-07 云南省科学技术院 一种耐高温高纯氧化铝棉的制备方法及制备设备

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US705691A (en) * 1900-02-20 1902-07-29 William James Morton Method of dispersing fluids.
US2048651A (en) * 1933-06-23 1936-07-21 Massachusetts Inst Technology Method of and apparatus for producing fibrous or filamentary material
US2108361A (en) * 1936-03-23 1938-02-15 Asakaws Yukichi Apparatus for manufacturing luster-free rayon
US2336745A (en) * 1941-12-20 1943-12-14 Fred W Manning Method and apparatus for making unwoven and composite fabrics
US2338570A (en) * 1941-10-30 1944-01-04 Eastman Kodak Co Process of electrostatic spinning
US2879566A (en) * 1956-02-16 1959-03-31 Marvalaud Inc Method of forming round metal filaments
US2907082A (en) * 1956-02-06 1959-10-06 Marvaland Inc Production of continuous filaments of high vapor pressure metals
US3218681A (en) * 1961-04-10 1965-11-23 Du Pont Magnetic levitation support of running lengths

Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US705691A (en) * 1900-02-20 1902-07-29 William James Morton Method of dispersing fluids.
US2048651A (en) * 1933-06-23 1936-07-21 Massachusetts Inst Technology Method of and apparatus for producing fibrous or filamentary material
US2108361A (en) * 1936-03-23 1938-02-15 Asakaws Yukichi Apparatus for manufacturing luster-free rayon
US2338570A (en) * 1941-10-30 1944-01-04 Eastman Kodak Co Process of electrostatic spinning
US2336745A (en) * 1941-12-20 1943-12-14 Fred W Manning Method and apparatus for making unwoven and composite fabrics
US2907082A (en) * 1956-02-06 1959-10-06 Marvaland Inc Production of continuous filaments of high vapor pressure metals
US2879566A (en) * 1956-02-16 1959-03-31 Marvalaud Inc Method of forming round metal filaments
US3218681A (en) * 1961-04-10 1965-11-23 Du Pont Magnetic levitation support of running lengths

Cited By (22)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3602291A (en) * 1968-09-04 1971-08-31 Battelle Development Corp Apparatus for casting metal filaments through an aerosol atmosphere
US3581040A (en) * 1969-06-11 1971-05-25 Inland Steel Co Forming of thin metal filaments
US3720741A (en) * 1969-10-03 1973-03-13 Monsanto Co Melt spinning process
US3834847A (en) * 1970-01-16 1974-09-10 Du Pont Open cell foam device for gas distribution in filament quenching chimneys
US3824052A (en) * 1971-04-15 1974-07-16 Deering Milliken Res Corp Apparatus to produce nonwoven fabric
DE2366327C2 (de) * 1972-12-26 1986-01-02 Allied Corp., Morris Township, N.J. Verfahren zur Herstellung eines Drahtes aus einer überwiegend amorphen Legierung
DE2364131A1 (de) 1972-12-26 1974-06-27 Allied Chem Amorphe metall-legierung und deren verwendung
US3856513A (en) * 1972-12-26 1974-12-24 Allied Chem Novel amorphous metals and amorphous metal articles
USRE32925E (en) * 1972-12-26 1989-05-18 Allied-Signal Inc. Novel amorphous metals and amorphous metal articles
US4178985A (en) * 1977-01-10 1979-12-18 Compagnie Generale Des Etablissements Michelin Installation for manufacturing a metal wire by continuous casting
US4266918A (en) * 1978-03-13 1981-05-12 Pulp And Paper Research Institute Of Canada Apparatus for electrostatic fibre spinning from polymeric fluids
US4736789A (en) * 1978-07-28 1988-04-12 Kennecott Corporation Apparatus and method for continuous casting of metallic strands at exceptionally high speeds using an oscillating mold assembly
EP0007581A1 (de) * 1978-07-28 1980-02-06 Kennecott Corporation Giessformanordnung und Verfahren zum Stranggiessen von metallischen Drahtlitzen bei aussergewöhnlich hohen Geschwindigkeiten
US4441542A (en) * 1981-06-10 1984-04-10 Olin Corporation Process for cooling and solidifying continuous or semi-continuously cast material
EP0066896A1 (de) * 1981-06-10 1982-12-15 Olin Corporation Einrichtung und Verfahren zum Kühlen und Erstarren von voll- oder halb-kontinuierlichem Stranggussmaterial
US4614221A (en) * 1981-09-29 1986-09-30 Unitika Ltd. Method of manufacturing thin metal wire
US4557742A (en) * 1984-07-02 1985-12-10 Polaroid Corporation Polarized optical fiber and method of forming same
US20080047736A1 (en) * 2006-08-25 2008-02-28 David Levine Lightweight composite electrical wire
US7626122B2 (en) 2006-08-25 2009-12-01 David Levine Lightweight composite electrical wire
US20100071931A1 (en) * 2006-08-25 2010-03-25 David Levine Lightweight composite electrical wire with bulkheads
US8697998B2 (en) 2006-08-25 2014-04-15 David Levine Lightweight composite electrical wire with bulkheads
WO2015145420A1 (en) 2014-03-26 2015-10-01 Keshet Itamar Nut and method for fixing an object to a building structure

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DE1583715B2 (de) 1973-06-28
SE327787B (de) 1970-08-31
FR1551091A (de) 1968-12-27
DE1583715A1 (de) 1970-08-20
DE1583715C3 (de) 1974-10-10
GB1212355A (en) 1970-11-18

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