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US20100230402A1 - Apparatus for porous material densification - Google Patents

Apparatus for porous material densification Download PDF

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Publication number
US20100230402A1
US20100230402A1 US12/376,391 US37639107A US2010230402A1 US 20100230402 A1 US20100230402 A1 US 20100230402A1 US 37639107 A US37639107 A US 37639107A US 2010230402 A1 US2010230402 A1 US 2010230402A1
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Prior art keywords
spiral
induction heating
coil
induction
coils
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Inventor
Kenny Chang
Bruce Zimmerman
Arnaud Fillion
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Safran Landing Systems SAS
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Messier Bugatti SA
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Priority to US12/376,391 priority Critical patent/US20100230402A1/en
Assigned to MESSIER-BUGATTI reassignment MESSIER-BUGATTI ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: CHANG, KENNY H., FILLION, ARNAUD, ZIMMERMAN, BRUCE
Publication of US20100230402A1 publication Critical patent/US20100230402A1/en
Assigned to MESSIER-BUGATTI-DOWTY reassignment MESSIER-BUGATTI-DOWTY CHANGE OF NAME (SEE DOCUMENT FOR DETAILS). Assignors: MESSIER-BUGATTI
Abandoned legal-status Critical Current

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    • H—ELECTRICITY
    • H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
    • H05B6/00—Heating by electric, magnetic or electromagnetic fields
    • H05B6/02—Induction heating
    • H05B6/10—Induction heating apparatus, other than furnaces, for specific applications
    • H05B6/105—Induction heating apparatus, other than furnaces, for specific applications using a susceptor
    • H05B6/108—Induction heating apparatus, other than furnaces, for specific applications using a susceptor for heating a fluid
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
    • C04B35/56—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides
    • C04B35/565—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on silicon carbide
    • C04B35/571—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on silicon carbide obtained from Si-containing polymer precursors or organosilicon monomers
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
    • C04B35/58—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides
    • C04B35/584—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides based on silicon nitride
    • C04B35/591—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides based on silicon nitride obtained by reaction sintering
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/71—Ceramic products containing macroscopic reinforcing agents
    • C04B35/78—Ceramic products containing macroscopic reinforcing agents containing non-metallic materials
    • C04B35/80—Fibres, filaments, whiskers, platelets, or the like
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/71—Ceramic products containing macroscopic reinforcing agents
    • C04B35/78—Ceramic products containing macroscopic reinforcing agents containing non-metallic materials
    • C04B35/80—Fibres, filaments, whiskers, platelets, or the like
    • C04B35/83—Carbon fibres in a carbon matrix
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/04—Coating on selected surface areas, e.g. using masks
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F16—ENGINEERING ELEMENTS AND UNITS; GENERAL MEASURES FOR PRODUCING AND MAINTAINING EFFECTIVE FUNCTIONING OF MACHINES OR INSTALLATIONS; THERMAL INSULATION IN GENERAL
    • F16D—COUPLINGS FOR TRANSMITTING ROTATION; CLUTCHES; BRAKES
    • F16D69/00—Friction linings; Attachment thereof; Selection of coacting friction substances or surfaces
    • F16D69/02—Composition of linings ; Methods of manufacturing
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F16—ENGINEERING ELEMENTS AND UNITS; GENERAL MEASURES FOR PRODUCING AND MAINTAINING EFFECTIVE FUNCTIONING OF MACHINES OR INSTALLATIONS; THERMAL INSULATION IN GENERAL
    • F16D—COUPLINGS FOR TRANSMITTING ROTATION; CLUTCHES; BRAKES
    • F16D69/00—Friction linings; Attachment thereof; Selection of coacting friction substances or surfaces
    • F16D69/02—Composition of linings ; Methods of manufacturing
    • F16D69/023—Composite materials containing carbon and carbon fibres or fibres made of carbonizable material
    • H—ELECTRICITY
    • H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
    • H05B6/00—Heating by electric, magnetic or electromagnetic fields
    • H05B6/02—Induction heating
    • H05B6/36—Coil arrangements
    • H05B6/362—Coil arrangements with flat coil conductors
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/48—Organic compounds becoming part of a ceramic after heat treatment, e.g. carbonising phenol resins
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/48—Organic compounds becoming part of a ceramic after heat treatment, e.g. carbonising phenol resins
    • C04B2235/483—Si-containing organic compounds, e.g. silicone resins, (poly)silanes, (poly)siloxanes or (poly)silazanes
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
    • C04B2235/72—Products characterised by the absence or the low content of specific components, e.g. alkali metal free alumina ceramics
    • Y—GENERAL 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
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T29/00—Metal working
    • Y10T29/49—Method of mechanical manufacture
    • Y10T29/49002—Electrical device making
    • Y10T29/4902—Electromagnet, transformer or inductor

Definitions

  • the present invention relates to densifying porous articles with a desirably high rate of production, particularly, but not necessarily only, with respect to the field of friction braking articles, such as aircraft brakes.
  • friction members In the field of friction materials, it is generally known to use porous material substrates to manufacture friction members, such as friction brake disks.
  • the manufacture of such friction members generally begins with the construction of a porous preform.
  • annular preforms are used.
  • the annular preforms can be constructed using several different known methods. For example, carbon fiber fabric plies can be needled together and annular preforms can be cut from the stacked material.
  • Oxidized polyacrylonitride (“PAN”) fibers or pitch-based fibers are common examples of starting fibers used in this type of application. Subsequently, these fibers may be carbonized in a high temperature treatment step prior densification.
  • porous preforms are densified.
  • a generally known method of densification uses a liquid precursor of a material that deposited within the porous preform to densify the preform. This kind of densification is sometimes referred to in the art as “film boiling.”
  • film boiling densification involves immersing a porous preform in a liquid hydrocarbon so that the liquid substantially completely infiltrates the pores and interstices of the preform. Thereafter, the immersed preform is inductively heated to a temperature above the decomposition temperature of liquid hydrocarbon (typically 1000° C. or more, typically up to about 1400° C.). More particularly, the liquid hydrocarbon adjacent to the inductively heated preform structure dissociates into various gas phase species within the preform porosity. Further thermal decomposition of the gas phase species results in the formation of pyrolitic carbon on interior surfaces in the open regions of the porous material.
  • a temperature above the decomposition temperature of liquid hydrocarbon typically 1000° C. or more, typically up to about 1400° C.
  • the liquid hydrocarbon adjacent to the inductively heated preform structure dissociates into various gas phase species within the preform porosity. Further thermal decomposition of the gas phase species results in the formation of pyrolitic carbon on interior surfaces in the open regions of the porous material.
  • FIG. 1 is a cutaway schematic side view of a liquid densification apparatus
  • FIG. 2 is a cutaway schematic top view of a liquid densification apparatus generally corresponding to that seen in FIG. 1 ;
  • FIG. 3 is a schematic cross sectional view of a porous article mounted relative to conventional induction coils for inductively heating the article;
  • FIG. 4 is a schematic cross sectional view of a porous article mounted relative to induction coils according to the present invention, for inductively heating the article;
  • FIG. 5 is a close-up cross sectional view of a part of an induction coil as illustrated in FIG. 4 ;
  • FIG. 6 is an enlarged partial view of the arrangement illustrated in FIG. 4 ;
  • FIG. 7 is a schematic side view illustrating an arrangement for mounting a porous article in the apparatus of the present invention.
  • FIG. 8 is a schematic perspective view of an exemplary apparatus for liquid densification of multiple porous articles
  • FIG. 9 is a schematic cross sectional view of an exemplary apparatus for liquid densification of multiple porous articles.
  • FIGS. 10-12 are X-ray images of a densified porous preform for illustrating an effect that the structure of the inductive heating coils has on densification.
  • a typical densification facility includes one or more reactor chambers generally sized and constructed to hold one or more preform members therein, with corresponding induction heating coils, while substantially immersed in the liquid precursor of choice.
  • the reactor chambers could be suitably manufactured from aluminum.
  • suitable materials are non-magnetic and include, without limitation, glass, stainless steel, ceramic or combinations thereof.
  • Dedicated inner buses and coils are provided depending on the size of the preforms being densified. Typical examples of preform diameters range from about 10′′ to about 25′′ and the thickness ranges from 15 mm to 50 mm. Particularly common examples include 15′′ and 20′′ diameter preforms.
  • the one or more reaction chambers are each provided with induction heating coils corresponding to each preform that is to be processed.
  • the induction coils and the preforms being processed are preferably mounted in position relative to each other using chemically non-reactive and thermally stable supports made from, for example, an electrically non-conductive glass composite material that can withstand a liquid hydrocarbon environment (such as that known in the art as “G-10”).
  • the induction heating coils are preferably water-cooled pancake spiral coils, and are commonly made from copper metal. For this reason, it is desirable to provide a heat exchanger dedicated to the water-cooling system for the induction coils, as will be discussed in further detail below.
  • a preform (or worn brake) being densified is heated by direct coupling from the induction coil.
  • FIGS. 1 and 2 are side and top schematic view of a coil/reactor chamber 100 generally in accordance with the present invention. Loading and unloading of one or more preforms 160 require, for example, a locking mechanism is provided for the selectably openable top lid 150 .
  • Each reactor chamber 100 (as many as are provided) is connected with a common precursor supply line 180 and a common exhaust line 140 to the condenser and thermal oxidizer.
  • Each reactor chamber 100 can be filled, drained, and monitored from the computer control system. The exhaust vapor from the densification process is condensed and fed back to the reactors, whereas the residual effluent gas is preferably then taken to a conventional thermal oxidizer (not shown) and burned.
  • the center of the preform initially be heated above the pyrolysis temperature of the precursor liquid.
  • the frequency of the power supply is set (in view of the material characteristics of the preform) to provide a skin depth roughly near the center of the preform.
  • the frequency of the power supply increases in response to changes in the electrical characteristics of the preform caused by densification.
  • the induction coils in a respective reaction chamber are associated with a corresponding power supply.
  • a commercially-available power supply suitable for this application is a Model No. LSP 14-400/30 Lepel induction-type power supply.
  • the power from the power supply is transferred to the induction coils by custom-built (depending on the physical arrangements of a given densification facility) copper bus bars with external water cooling networks.
  • the Lepel power supply for example, has remote PID loop control capability and can be monitored and controlled from a computer control terminal. Power density, voltage control, current control, frequency control, and/or temperature control of the densification process by known methods is also within the scope of the contemplated arrangement.
  • the system includes a conventional fluid transfer system for managing the transport of new (and used) precursor liquid (not shown).
  • the fuel transfer system may include one or more remote storage tanks for storing a new liquid precursor supply as well as possibly temporarily storing used precursor liquid. A relatively smaller local storage tank for new precursor liquid can also be provided.
  • a precursor liquid used according to the present system is cyclohexane (C 6 H 12 ).
  • the corresponding deposited material could be any of, strictly by way of example and without limitation, carbon, silicon carbide, silicon nitride, carbon-silicon carbide, or carbon-silicon nitride.
  • a hydrocarbon such as cyclohexane, n-hexane, benzene, toluene, or combinations thereof can be used.
  • Methyltrichlorosilane, dimethyldichlorosilane, and methydichiorosilane, tris-n-methyl amino silane, or other organosilane mixtures can be used for depositing silicon carbide and silicon nitride.
  • the precursor liquid can be chosen to co-deposit materials.
  • a mixture of silicon carbide and silicon nitride can be deposited using tris-n-methyl amino or other silane compound.
  • co-deposited materials such as carbon-silicon carbide and carbon-silicon nitride can be produced with an appropriately selected mixture of precursors.
  • silicon carbide or silicon nitride interface coating can be produced during an early stage of the densification or co-deposited throughout the matrix densification.
  • sufficient liquid precursor is provided to substantially immerse the preform being densified, as well as the induction heating coils associated therewith.
  • the film boiling process creates gaseous species that eventually cause the formation of pyrolitic carbon on interior surfaces of the preform porosity.
  • Precursor vapor is preferably captured to the extent possible and condensed for possible recycling in the process.
  • Effluent gas that is still left over is preferably conveyed to a thermal oxidizer of a known configuration to burn off residual hydrocarbons in the effluent gas.
  • the structure of the induction coils 130 used in film boiling densification processes is very important for obtaining densified preforms having suitable mechanical characteristics, including friction characteristics.
  • FIG. 3 shows a particular difference between the convention inductive coil of FIG. 3 and that of FIG. 4 .
  • the prior induction heating coil 200 shown in FIG. 3 is made from square or round hollow copper tubing 230 bent into the desired coil form.
  • the copper tubing functions both to transmit the power for inductive heating (through the copper metal) and convey cooling water through the inlet port 250 and the outlet port 260 .
  • the coil 200 of FIG. 3 has, for example, a nominal 3 ⁇ 4′′ gap with an inner diameter (ID) coverage of 18′′ and an outer diameter (OD) coverage of 8.5′′.
  • FIG. 3 shows a carbonized preform 240 placed inside of an alumina holder 220 and supported with a G-10 holder 270 .
  • FIG. 4 shows an example of an induction heating coil 300 according to the present invention is fabricated from, for example, 1 ⁇ 4′′ solid copper plate that is milled or otherwise machined into the desired coil form 330 , instead of being turned or bent into shape as the coil in FIG. 3 is.
  • a high precision machining operation is used to form the coil from the copper plate, such as, for example, CNC milling and the like.
  • a hollow metal (copper, for example) water cooling tube 335 is brazed on an exterior (i.e., opposite the side facing the preform in use) side of the machined copper coil 330 .
  • the braze composition may be any commercially available composition suitable for brazing copper as long as it can withstand the expected temperature environment.
  • the currently contemplated induction coil uses a machined flat copper plate, it can be produced with greater precision (particularly with respect to gaps between turns of the coil) than bending copper tubing.
  • the machined copper plate does not undergo stress and strain deformation like bent copper tubing.
  • a gap between adjacent turns of the coil according to the invention is substantially consistent, and is between about 4 mm to about 8 mm.
  • the conventional copper tube becomes distended and at least susceptible to rupture (in a manner not unlike a vascular aneurysm) (if rupture does not in fact occur). It is tentatively believed that the conventional copper tube induction coil can become too hot for the cooling water to adequately dissipate the heat. It is speculated that this can cause vaporization of the cooling water within the conventional copper tubing with an unacceptable pressure increase therein. This pressure is believed to result in the bulging tubing deformation and an elevated risk of tube rupture.
  • a prior induction coil made from copper tubing suffers from a spiral densification characteristic and weak densification at the radially inner and outer peripheries, as can be seen below in FIGS. 10 and 11 .
  • “Spiral densification” is an art-recognized term which generally refers to non-homogenous densification, particularly characterized by generally circumferential “streaks”—regions in which the densification is non-trivially different from adjacent regions. This problem is significantly related to imperfections in coil design, especially with respect to the gap distance between adjacent turns of the coil. It will be appreciated that if the coil structure is not carefully monitored, gaps between coil turns may occur that lead to insufficient heating of the adjacent preform. This results in turn in poor densification. In addition, pancake coil distance is usually in a fixed position which does not allow for any adjustment for the depth penetration.
  • the preforms illustrated in FIGS. 10 and 11 were formed with a conventional copper tubing induction coil in a film boiling densification process. In both images, large, circumferentially extending regions of density variation are evident. In particular, a region of very low density (corresponding to the white region at approximately the “10 o'clock” position of both preforms is noticeable. In addition, as mentioned above, poor densification can be seen, for example, at the radially outward periphery of the preforms. See, for example, the white region along approximately the bottom halves of each X-ray scan.
  • FIG. 12 is a similar type of X-ray scan which illustrates the densification of a preform densified using an induction coil made from a machined copper plate and having a cooling water tube brazed thereto, as described above with reference to FIG. 4 .
  • the important feature to note between FIGS. 10 and 11 relative to FIG. 12 is the absence of distinct or prominent circumferentially extending blotches and the like in FIG. 12 (unlike in FIGS. 10 and 11 ), which indicate large variations in densification levels, and more particularly, regions of undesirably low densification.
  • FIG. 5 hereinbelow is a cross-sectional view of one segment of an induction coil according to the present invention.
  • a cooling water tube 400 brazed to an exterior (with respect to a preform being densified) side of the machined copper coil 402 used as the induction heating coil.
  • a mounting fixture, such as a bolt shaft 401 may be attached to an exterior of the cooling water tube 400 for mounting the coil to a support within the reaction chamber.
  • the reaction chamber according to the present invention includes at least one induction heating coil as described herein, for inductively heating a preform mounted adjacent thereto.
  • induction heating coil as described herein, for inductively heating a preform mounted adjacent thereto.
  • pairs of coils are provided and a preform being treating is mounted between them.
  • preforms are generally soft and pliable before being densified. Therefore, it is desirable to hold a preform relative to the inductive heating coil in such a manner so as to reduce bending and other forms of warping or deformation before the preform is densified.
  • support members may be used to hold the preform in place. See, for example, FIGS. 6 and 7 .
  • the preform is held in place by one or more supports 530 mounted, for example, on the same supports on which the induction coils are mounted.
  • the supports may be, for example, non-reactive quartz glass or alumina cylinders having an appropriately sized and aligned notch formed therein.
  • the radial (with respect to the preform) position of some or all of the supports can be adjusted to, for example, accommodate insertion of the preform relative to the heating coils, or to accommodate preforms of different diameters.
  • the distance between coils and the preform can be adjusted by screwing in or out of the bolt shaft 520 (corresponding to the bolt shaft 401 seen in FIG. 5 ) in order to provide effective heating during initial densification. Control of this spacing between the induction coils and the preform can help control current concentrations in the preform during inductive heating, so as to avoid “mirror effect” or “spiral” densification on the one hand, and to increase power yield by not spacing the coil too far away from the preform.
  • FIG. 8 hereinbelow is a perspective view of a reaction chamber 700 according to the present invention into which three preforms (and associated induction heating coils) are loaded. This illustration is strictly by way of example to illustrate the densification of multiple porous parts, and other loading arrangements with other numbers of preforms are possible.
  • the multiple-part densification shows another way of producing carbon disks in at least a three-part densification configuration.
  • the liquid precursor is supplied to the reaction chamber 700 through ports 710 .
  • the power from the power supply is transferred to the induction coils 730 by appropriately arranged (depending on the physical arrangements of a given densification facility) copper bus bars 760 with external water cooling networks.
  • the Lepel power supply for example, has remote PID loop control capability and can be monitored and controlled from a computer control terminal. Power density, voltage control, current control, and/or temperature control of the densification process by known methods is also within the scope of the contemplated arrangement.
  • the liquid precursor is supplied to the reaction chamber(s) 700 from the local precursor storage tank.
  • sufficient liquid precursor is provided to substantially immerse the preform(s) being densified, as well as the induction heating coils associated therewith.
  • the film boiling process creates gaseous species that in part causes the formation of pyrolitic carbon on interior surfaces of the preform porosity.
  • Precursor vapor is released thru an exhaust line 720 and vented to an external condenser (not shown) for possible recycling in the process. Effluent gas that is still left over is preferably conveyed to a thermal oxidizer (not shown).
  • each reactor chamber 700 (as many as are provided) is connected with a common precursor supply line and a common exhaust line 720 to the condenser and thermal oxidizer.
  • Each reactor chamber can be filled, drained, and monitored from the computer control system. The exhaust vapor from the densification process is condensed and fed back to the reactors, whereas the residual effluent gas is then taken to the thermal oxidizer and burned.
  • FIG. 9 illustrates another arrangement for the liquid densification of multiple porous parts.
  • This illustration shows the densification of multiple porous parts 870 inside of a sealed reaction chamber 800 .
  • a load stack consisting of multiple porous parts 870 and graphite plates 860 therebetween are pre-assembled.
  • the load stack is placed on a ceramic or electrically insulated stand 890 and the furnace lid 805 is removed during the loading and unloading operation.
  • the power from the power supply is transferred to the multi-zone coil 810 , 820 , and 830 through power port 880 .
  • Individual PID zone control is made possible through power density, voltage control, current control, frequency control, and/or temperature control for the densification process.
  • the heating of the porous parts 870 is accomplished by using, for example, a multi-zone induction coil 810 , 820 , 830 which is directly coupled to the graphite plates 860 .
  • the annular graphite plates 860 have similar ID and OD dimensions as the annular porous parts and the thickness of the annular graphite plate ranges between 5 mm to 25 mm.
  • the densification fronts start from the heated preform surfaces which are in contact with the graphite plates 860 .
  • Liquid precursor is supplied to the reactor chamber 800 and the liquid can be filled and drained through port 895 .
  • a liquid level indicator 840 indicates the level of precursor fluid during the fill, drain, and densification.
  • Sufficient liquid precursor is provided to substantially immerse the load stack inside of the reactor chamber cavity 806 .
  • a continuous feed of liquid precursor is also possible during the densification process.
  • the densification process creates gaseous species and the vapor is released from port 850 and directed to the condenser for possible recycling purpose. Effluent gas that is not captured is conveyed to the thermal oxidizer to burn off the residual hydrocarbons.
  • a mounting assembly could be provided at the center of a given preform that could be appropriately connected to a driving device located outside of the respective reaction chamber.
  • the rate of rotation of the preform might be from about one to about five revolutions per minute, as currently contemplated.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Manufacturing & Machinery (AREA)
  • Structural Engineering (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Engineering & Computer Science (AREA)
  • Composite Materials (AREA)
  • Physics & Mathematics (AREA)
  • Electromagnetism (AREA)
  • Mechanical Engineering (AREA)
  • General Chemical & Material Sciences (AREA)
  • Metallurgy (AREA)
  • General Induction Heating (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
  • Glass Compositions (AREA)
  • Furnace Details (AREA)
  • Silicon Compounds (AREA)
  • Braking Arrangements (AREA)
  • Physical Or Chemical Processes And Apparatus (AREA)
US12/376,391 2006-08-07 2007-08-07 Apparatus for porous material densification Abandoned US20100230402A1 (en)

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US12/376,391 US20100230402A1 (en) 2006-08-07 2007-08-07 Apparatus for porous material densification
PCT/EP2007/058195 WO2008017677A2 (en) 2006-08-07 2007-08-07 Apparatus for porous material densification

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US12/376,396 Active 2029-07-29 US8568838B2 (en) 2006-08-07 2007-08-07 Power control for densification of one or more porous articles
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US12/376,399 Abandoned US20100297360A1 (en) 2006-08-07 2007-08-07 Method for densification of porous articles

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US (3) US20100230402A1 (zh)
EP (3) EP2051952B1 (zh)
JP (3) JP5357024B2 (zh)
KR (3) KR20090040458A (zh)
CN (5) CN101502168A (zh)
BR (3) BRPI0716037A2 (zh)
CA (3) CA2660200A1 (zh)
MX (3) MX2009001415A (zh)
RU (3) RU2410851C2 (zh)
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Publication number Priority date Publication date Assignee Title
WO2019023630A1 (en) * 2017-07-27 2019-01-31 CEM Corporation, Lucidity Division INDUCTION HEATED COLUMN GAS CHROMATOGRAPHING DEVICE AND METHOD OF USE THEREOF
US20190033268A1 (en) * 2017-07-27 2019-01-31 CEM Corporation, Lucidity Division Gas chromatograph device with inductively heated column and method of use thereof
US10935524B2 (en) 2017-07-27 2021-03-02 CEM Corporation, Lucidity Division Gas chromatograph device with inductively heated column and method of use thereof

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BRPI0716038A2 (pt) 2016-02-16
KR20090040458A (ko) 2009-04-24
MX2009001415A (es) 2009-04-08
TW200812934A (en) 2008-03-16
KR20090040371A (ko) 2009-04-23
EP2051952B1 (en) 2012-12-26
CN101528637B (zh) 2012-11-28
US20100297360A1 (en) 2010-11-25
US8568838B2 (en) 2013-10-29
MX2009001416A (es) 2009-05-11
RU2009107003A (ru) 2010-09-20
WO2008017678A3 (en) 2008-05-22
RU2410851C2 (ru) 2011-01-27
US20100156005A1 (en) 2010-06-24
RU2431629C2 (ru) 2011-10-20
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BRPI0716039A2 (pt) 2015-06-23
CN101502168A (zh) 2009-08-05

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