EP0342197A1 - Verfahren zur herstellung eines kompositmaterials - Google Patents

Verfahren zur herstellung eines kompositmaterials

Info

Publication number
EP0342197A1
EP0342197A1 EP88901042A EP88901042A EP0342197A1 EP 0342197 A1 EP0342197 A1 EP 0342197A1 EP 88901042 A EP88901042 A EP 88901042A EP 88901042 A EP88901042 A EP 88901042A EP 0342197 A1 EP0342197 A1 EP 0342197A1
Authority
EP
European Patent Office
Prior art keywords
fibers
matrix
electric current
electrostatic field
induced
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
EP88901042A
Other languages
English (en)
French (fr)
Inventor
Michel Berger
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Pradom Ltd
Original Assignee
Pradom Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Priority claimed from FR878700797A external-priority patent/FR2609934B2/fr
Priority claimed from US07/027,793 external-priority patent/US4857244A/en
Application filed by Pradom Ltd filed Critical Pradom Ltd
Publication of EP0342197A1 publication Critical patent/EP0342197A1/de
Pending legal-status Critical Current

Links

Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C70/00—Shaping composites, i.e. plastics material comprising reinforcements, fillers or preformed parts, e.g. inserts
    • B29C70/04—Shaping composites, i.e. plastics material comprising reinforcements, fillers or preformed parts, e.g. inserts comprising reinforcements only, e.g. self-reinforcing plastics
    • B29C70/06—Fibrous reinforcements only
    • B29C70/10—Fibrous reinforcements only characterised by the structure of fibrous reinforcements, e.g. hollow fibres
    • B29C70/12—Fibrous reinforcements only characterised by the structure of fibrous reinforcements, e.g. hollow fibres using fibres of short length, e.g. in the form of a mat
    • B29C70/14—Fibrous reinforcements only characterised by the structure of fibrous reinforcements, e.g. hollow fibres using fibres of short length, e.g. in the form of a mat oriented
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
    • B29B15/00—Pretreatment of the material to be shaped, not covered by groups B29B7/00 - B29B13/00
    • B29B15/08—Pretreatment of the material to be shaped, not covered by groups B29B7/00 - B29B13/00 of reinforcements or fillers
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C70/00—Shaping composites, i.e. plastics material comprising reinforcements, fillers or preformed parts, e.g. inserts
    • B29C70/04—Shaping composites, i.e. plastics material comprising reinforcements, fillers or preformed parts, e.g. inserts comprising reinforcements only, e.g. self-reinforcing plastics
    • B29C70/06—Fibrous reinforcements only
    • B29C70/10—Fibrous reinforcements only characterised by the structure of fibrous reinforcements, e.g. hollow fibres
    • B29C70/16—Fibrous reinforcements only characterised by the structure of fibrous reinforcements, e.g. hollow fibres using fibres of substantial or continuous length
    • B29C70/20—Fibrous reinforcements only characterised by the structure of fibrous reinforcements, e.g. hollow fibres using fibres of substantial or continuous length oriented in a single direction, e.g. roofing or other parallel fibres
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29D—PRODUCING PARTICULAR ARTICLES FROM PLASTICS OR FROM SUBSTANCES IN A PLASTIC STATE
    • B29D30/00—Producing pneumatic or solid tyres or parts thereof
    • B29D30/06—Pneumatic tyres or parts thereof (e.g. produced by casting, moulding, compression moulding, injection moulding, centrifugal casting)
    • B29D30/38—Textile inserts, e.g. cord or canvas layers, for tyres; Treatment of inserts prior to building the tyre
    • C—CHEMISTRY; METALLURGY
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    • C04B20/00—Use of materials as fillers for mortars, concrete or artificial stone according to more than one of groups C04B14/00 - C04B18/00 and characterised by shape or grain distribution; Treatment of materials according to more than one of the groups C04B14/00 - C04B18/00 specially adapted to enhance their filling properties in mortars, concrete or artificial stone; Expanding or defibrillating materials
    • C04B20/0048—Fibrous materials
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    • C04B20/00—Use of materials as fillers for mortars, concrete or artificial stone according to more than one of groups C04B14/00 - C04B18/00 and characterised by shape or grain distribution; Treatment of materials according to more than one of the groups C04B14/00 - C04B18/00 specially adapted to enhance their filling properties in mortars, concrete or artificial stone; Expanding or defibrillating materials
    • C04B20/02—Treatment
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    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
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    • C04B35/486—Fine ceramics
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    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
    • C04B35/62605—Treating the starting powders individually or as mixtures
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    • C04B35/62605—Treating the starting powders individually or as mixtures
    • C04B35/62645—Thermal treatment of powders or mixtures thereof other than sintering
    • C04B35/62655—Drying, e.g. freeze-drying, spray-drying, microwave or supercritical drying
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    • C04B35/78—Ceramic products containing macroscopic reinforcing agents containing non-metallic materials
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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
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    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
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    • C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
    • C04B2235/52—Constituents or additives characterised by their shapes
    • C04B2235/5208—Fibers
    • C04B2235/5216—Inorganic
    • C04B2235/524—Non-oxidic, e.g. borides, carbides, silicides or nitrides
    • C04B2235/5244—Silicon carbide
    • 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
    • C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
    • C04B2235/52—Constituents or additives characterised by their shapes
    • C04B2235/5208—Fibers
    • C04B2235/5216—Inorganic
    • C04B2235/524—Non-oxidic, e.g. borides, carbides, silicides or nitrides
    • C04B2235/5248—Carbon, e.g. graphite
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/60—Aspects relating to the preparation, properties or mechanical treatment of green bodies or pre-forms
    • C04B2235/616—Liquid infiltration of green bodies or pre-forms
    • 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
    • C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
    • C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
    • C04B2235/6562—Heating rate
    • 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
    • C04B2235/74—Physical characteristics
    • C04B2235/77—Density
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
    • C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
    • 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
    • C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
    • C04B2235/9646—Optical properties
    • C04B2235/9653—Translucent or transparent ceramics other than alumina
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2375/00—Characterised by the use of polyureas or polyurethanes; Derivatives of such polymers
    • C08J2375/04—Polyurethanes
    • 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
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10—Energy storage using batteries
    • 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
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/30—Hydrogen technology
    • Y02E60/50—Fuel cells

Definitions

  • the present invention relates to a process for preparing composite materials ; it also relates to the intermediate or finished products which can be obtained with said process, notably vulcanized products, in particular tires, ceramics and electrodes.
  • Composite materials are materials constituted of reinforcing elements (mostly fibers - or filaments - such as glass fibers, carbon fibers, boron or poly amide fibers, etc%) and of a matrix (constituted either by a resin or a resistant material such as metal or ceramics).
  • the properties of composite materials are particularly dependent, as we know : of :
  • the invention provides a main process for the preparation of a composite material that includes fibers used to reinforce the composite material comprising the steps of : subjecting the fibers to an electrostatic field induced by a high voltage alternating electric current for a time interval sufficient to cause a modification of the surface of said fibers ; and impregnating said fibers after the elapse of said time interval with a liquid matrix material or precursor of matrix, while still under the influence of said field, thereby consolidating bonding between the fibers and the matrix.
  • this process for the preparation of a composite material that includes fibers used to reinforce the composite material comprises the steps of : subjecting the fibers to an electrostatic field induced by a high voltage direct electric current for a first time interval sufficient to cause charging said fibers ; subjecting the fibers to an electrostatic field induced by a high voltage alternating electric current for a second time interval sufficient to cause a modification of the surface of the fibers ; after the elapse of said two time intervals, impregnating said fibers with a liquid matrix or precursor of matrix, while still under the influence of said field, thereby consolidating bonding between the fibers and the matrix.
  • this process for the preparation of a composite material that includes fibers used to reinforce the composite material comprises the successive steps of : subjecting the fibers to an electrostatic field induced by a high voltage alternating electric current for a first time interval sufficient to cause a modification of the surface of the fibers ; subj ecting the fibers to an electrostatic field induced by a high voltage direct electric current for a second time interval sufficient to cause charging said fibers ; after the elapse of said two time intervals, impregnating said fibers with a liquid matrix or precursor of matrix, while still under the influence of said field, thereby consolidating bonding between the fibers and the matrix.
  • high voltage current-induced electrostatic field is meant a field at least equal to the field obtained by applying between two electrodes 20 mm apart, a voltage equal to at least 20,000 volts in alternating current and to a least 40,000 volts in direct current.
  • the reinforcing elements, and in particular the fibers, fibrils or roves used, are then positioned between the electrodes subjected to the very high voltage current.
  • any type of fibers can be used as reinforcing elements, but they must be in a dielectric material, namely a material which, when under the effect of the field, becomes electrically charged and remains charged for a certain time.
  • the charged fibers having a tendency to push one another back, a bed of fibers is obtained at the output of the field, of which the thickness is between two and four times the thickness of the bed of fibers initially introduced between the electrodes, and it is when the fibers are in that "swollen" state that they should be impregnated.
  • any one of the currently known and used matrix material is suitable for the process according to the invention, for example resins (epoxy or polyamide) resins or hardened carbon mixtures, or silica based mixtures capable of forming ceramics, and metals.
  • the resulting product can either be sold as is (normally after a first solidification) or it can be transformed by molding and solidification of the matrix. And as known, the matrix itself can be charged. It has been found that with the above process according to the invention, called main or basic process, the reinforcing elements (fibers) become thoroughly impregnated by the matrix.
  • the electrostatic field is produced with a direct current, it is noted that, besides the swelling action of the bundle of initial fibers, there occurs a complementary orientation of said fibers. This orientation will permit the preparation of a composite material having specific properties.
  • a preferred embodiment comprises using first a D.C. electrostatic field and secondly a A.C. electrostatic field.
  • the present invention according to a second object relates to a use of the above main process for preparing composite materials with oriented reinforcing elements, to the vulcanization and production of tires, and also the vulcanized products, in particular tires , obtained according to said process .
  • the present invention therefore relates to a use of the invention main process such as above-described to vulcanization, and in particular to the production of tires, such a as radial-ply tires.
  • the invention concerns a process for the manufacture of a vulcanized composite material having improved mechanical and wear properties, the composite material having reinforced fibers that reinforce a vulcanizable matrix, comprising the steps of : subjecting the fibers to an electrostatic field that is induced by a high-voltage electric current to prepare the fibers to be impregnated ; impregnating said fibers with a vulcanizable liquid matrix or precursor of vulcanizable matrix while still under the influence of said electrosatic field thereby consolidating bonding between the fibers and the matrix ; and vulcanizing the imprenated fibers/matrix composite, thereby obtaining said vulcanized composite material.
  • said electrostatic field includes time sequential first and second fields that are induced by high voltage electric currents.
  • one of said fields is induced by an A.C. electric current and the other of said fields is induced by a O.C. electric current.
  • the first of said fields is induced by D.C. electric current and the second one of said fields is induced by A.C. electric current.
  • it is further including the step of shaping the impregnated fibers/matrix composite into a vehicle tire to obtain a vehicle tire as the vulcanized composite material.
  • the fibers used as reinforcing elements are selected from the group consisting of polyamide fibers, plant fibers and glass fibers.
  • the matrix is selected from the group consisting of polyurethane elastomer, natural rubber, synthetic rubber, rhodorsil, silicon, thermoplastic elastomer, and mixtures thereof.
  • woven Kevlar fibers as reinforcing fibers are used with polyurethane elastomer as matrix, the relative proportion being about 40 % by weight of woven Kevlar fibers with about 60 % by weight of polyurethane elastomer.
  • the D.C. electric current is about a 40,000 V D.C. electric current and the A.C. electric current is about a 20 ,000 V electric current.
  • the D.C. electric current is about a 100, 000 V D.C. electric current and the A.C. electric current is about a 25,000 V electric current.
  • said fibers are of a dielectric material, which can be advantageously selected from the group consisting of polyamide fibers, glass fibers, metallic oxide fibers, carbon fibers and mixtures thereof.
  • the invention also concerns a process for the manufacture of a composite material usable as a vehicle tire having improved mechanical and wear properties, the composite material having tire reinforcing fibers that reinforce a tire matrix, comprising the steps of : subjecting the fibers to an electrostatic field that is induced by a high-voltage electric current to prepare the fibers to be impregnated ; impregnating said fibers with a liquid matrix or precursor of matrix while still under the influence of said electrostatic field thereby consolidating bonding between the fibers and the matrix ; and vulcanizing the impregnated fibers/matrix composite so that the resulting vulcanized material is usable as a vehicle tire.
  • this process includes the step of shaping the impregnated fibers/matrix composite into a vehicle tire.
  • an A.C. type high-voltage electrostatic field causes a roughness of the fibers surface, thus radically and totally unexpectedly improving the surface bonding strength of the elastomer vulcanized on the surface of the fibers, thereby radically improving the mechanical properties of the vulcanized products and in particular of tires, such as radial-ply tires.
  • the present invention also relates to the vulcanized products obtained according to said process, such as tires, and preferably radial-ply tires.
  • the present invention according to a third object relates to a use of the above main process for the preparation of composite materials with oriented reinforcing elements, in the manufacture of ceramic composites and the ceramic composites obtained with said process.
  • the invention concerns a process for the manufacture of a ceramic composite material having improved mechanical and wear properties, the composite material having reinforcing fibers that reinforce a ceramic or ceramic precursor matrix, comprising the steps of : subjecting the fibers to an electrostatic field that is induced by a high-voltage electric current to prepare the fibers to be impregnated ; impregnating said fibers with a ceramic matrix or precursor of ceramic matrix while still under the influence of said electrostatic field thereby consolidating bonding between the fibers and the matrix ; and baking the impregnated fibers/matrix composite, thereby obtaining said ceramic composite material.
  • the present invention therefore relates to a use of the above-said main process using electrostatic fields in the production of ceramic composites notably of the ceramic-ceramic type or of the mixed ceramic and different fibers type.
  • One particular embodiment of the invention consists in producing a ceramic in which the ceramic matrix is of the zirconium type and the fibers are silicium carbide fibers, which are advantageously long fibers, woven or non-woven, the length of which is identical or near to the length of the piece to be produced.
  • Another particular embodiment of the invention consists in using alumina as ceramic matrix, the fibers being also in alumina and being advantageously long but non-woven fibers.
  • the present invention also covers the ceramic composites obtained according to said process.
  • the present invention according to a fourth object relates to a use of the above main process for the preparation of composite materials with oriented reinforcing elements, in the production of electrodes, as well as the electrodes obtained according to said process and electrochemical generators equipped with such electrodes. It has now been found, quite unexpectedly, that the use of the invention process has given totally unexpected results in the production of electrodes and that it was therefore especially advantageous for producing electrodes which can be used in electrochemical generators, such as accumulator batteries, primary cells, fuel cells, etc.
  • the electrodes produced according to these methods have a relatively poor lamination resistance because of the poor quality interface bonding between active material and conducting fibers. Moreover, the active surface/apparent surface ratio is relatively low and has to be improved in order to improve efficiency.
  • the solution proposed is also meant to be particularly simple.
  • the present invention further relates to a use of the invention process as above-described in the manufacture of electrodes as well as those electrodes.
  • the invention thus concerns a process for the manufacture of a composite electrode having improved mechanical and wear properties, the composite material having reinforcing fibers that reinforce a conducting adhesive forming matrix, comprising the steps of : subjecting the fibers to an electrostatic field that is induced by a high-voltage electric current to prepare the fibers to be impregnated ; impregnating said fibers with an electroactive conducting matrix while still under the influence of said electrostatic field thereby consolidating bonding between the fibers and the matrix ; optionally compressing said impregnated fibers (matrix composite) thereby obtaining said composite electrodes.
  • fibers capable of receiving, by electrolytic deposition, negative active materials for producing the anodes, or positive active materials for producing cathodes, therefore said fibers will have to be either conducting or made to be conducting by metal deposition, such as for example of "electroless" type.
  • carbon or boron fibers are preferably used as conducting fibers, the preferred ones being graphite fibers, and advantageously in the form of weaves of fibers, out to the size of the electrodes to be produced.
  • negative electrodes are produced by deposition of a metal selected from the group consisting advantageously of zinc, lithium, magnesium, cadmium. According to yet another embodiment of the invention for producing negative electrodes, it is preferably proceeded to a deposition of manganese dioxide, nickel oxide, silver dioxide, titanium dioxide.
  • the invention also covers the eletrodes obtained according to said process as well as the electrochemical generators equipped with such electrodes, namely accumulator batteries, primary cells, fuel cells, etc.
  • FIG. 1 shows a casing in insulating material 1 resting on insulating support members 2, and containing, in position between wedge members 3 and resting on an insulating base 4 : a first plate-shaped lower electrode 5, a first dielectric 6, a gap 7, a second dielectric 8 and a second, equally plate-shaped electrode 9.
  • the fibrous bundle 10 is placed between the two dielectrics.
  • the two electrodes 5 and 9 are connected to a generator of direct current of voltage about 100,000 volts.
  • the assembly is charged for about 10 mins. for fibrils of between 5 and 6 mm thickness.
  • Figure 2 shows the bundle before being charged
  • figure 3 shows the bundle after a 10-minute charging treatment.
  • Figure 4 shows a microscopic view of a fibril before the treatment
  • Figure 5 shows the same fibril as ground after the treatment. From a practical standpoint, it has been found that the fact of subj ecting the whole bundle of fibrils to a first A.C. field in order to obtain a more effecient etching with alternating current, and then subjecting it to a D.C. field in order to create an expansion , greatly contributes to obtaining a ground , expanded and tidy bundle. Indeed, a third effect noted is that a rather disorderly bundle, such as illustrated in Figure 6, becomes perfectly orderly after a treatment in a high-voltage D.C. electrostatic field, as illustrated in Figure 7.
  • Woven Kevlar fibers are placed between the plates of an electrostatic field generating device, which plates can be fed with a high-voltage alternating or direct current.
  • an alternative current at a voltage of preferably at least 20,000 volts is applied for a few minutes, in order to obtain a roughness of the fibers surface due to an etching effect created on the surface by localized discharges when the electrostatic field is modified by reversing the polarity of the electric field.
  • Kevlar fibers While the Kevlar fibers are still under the influence of the electrostatic field, said fibers are embedded in a polyurethane elastomer which may contain one or more of the conventional vulcanizing agents, such as sulphur, in a relative proportion of 40 % by weight of Kevlar fibers and 60 % by weight of polyurethane elastomer.
  • a polyurethane elastomer which may contain one or more of the conventional vulcanizing agents, such as sulphur, in a relative proportion of 40 % by weight of Kevlar fibers and 60 % by weight of polyurethane elastomer.
  • the conventional vulcanizing treatment which may comprise a shaping in order to obtain a tire.
  • the process may be carried out so as to obtain a radial-ply tire in a quite conventional way.
  • the resulting vulcanized product is found to have mechanical properties which are radically improved over the conventionally vulcanized products which have not been submitted to the process described in the French patent namely through a treatment by a high-voltage A.C. or D.C. electric field.
  • the procedure is the same as in Example 1, except that the fibers used are KEVLAR type polyamide fibers woven at 60 % lengthwise and at 40 % widthwise. These fibers are subjected for 10 minutes to a direct current of 100,000 V, then for 15 minutes to an alternating current of 25,000 V.
  • Each one of these two electrostatic treatments consisting in causing first a stream of hot air at 90°C followed by a stream of hotter air, at more than 100°C, for example around 130°C, to flow between the plates, then the treated fibers are impregnated, while still under the influence of an electrostatic discharge, with a soft matrix composed of a polyurethane elastomer containing an adhesive bond constituted by a phenolic resin of the "Rhone-Poulenc" A.R.P. 27 type.
  • the resulting material is then put under a pressure of 2 t/dm 2 and baked by polymerisation at 140°C for four hours, then heating is stopped and the resulting product is allowed to cool for 24 hours.
  • the resulting vulcanized elastomer can be used as vehicle tire and is found to have the following characteristics : Characteristics :
  • the matrix used here may be replaced for example by natural rubber. It is also possible for various applications to obtain the same supple products with pre-treated vegetable fibers (such as for example, fibers pre-treated in phenol-based solutions).
  • Said fibers are then subjected to a treatment by the electrostatic process described in the French patent 84 14800, preferably conducted as follows :
  • a high D.C. voltage of at least 40,000 volts is applied to the plates, preferably 100,000 volts, for a few minutes, preferably 10 minutes, so as to space out the fibers and cause them to swell, the thickness of the fibers assembly then reaching between two and four times the thickness of the bed of fibers initially introduced between the plates forming electrodes, as described in the French patent.
  • an A.C. voltage at least equal to 20,000 volts, and preferably around 25,000 volts, is then applied for a few minutes, preferably about 10 minutes, in order to obtain a roughness of the fibers surface by a stripping effect on the surface, or by etching, resulting from localized discharges when the electrostatic field is modified by reversing the polarity of the electric field.
  • This treatment of the fibers is advantageously carried out under a stream of hot air heated to a temperature exceeding 100°C, and preferably equal to about 130°C.
  • the silicium carbide fibers are coated with a ceramic matrix which in this case is preferably composed of ZrO 2 (70 % by weight) and of SiO 2 (30 % by weight), which matrix can contain an adhesive binder and, advantageously, an activating binder, in the relative proportion given hereunder, in % by weight : % by weight
  • a second baking operation is then conducted in the same conventional oven using ambient air, by raising the temperature progressively of 150°C every hour, until a temperature of 1050°C is reached ;
  • said third baking operation is conducted in an oven with a neutral or reducing atmosphere, such as for example Xenon or H 2 . Thereagain, the temperature is raised progressively of 150°C every hour , for two hours ;
  • the heating is then turned off and the product is cooled slowly for 24 hours.
  • the ceramic composites prepared in this way which are known as of the "zirconia-silicium carbide” type, exhibits the following characteristics :
  • the matrix contains an adhesive binder such as of "CONTRONICS" RTC 70 type, the relative proportions being the same as in Example 1.
  • the invention also covers the ceramic composites obtained according to said process. Therefore, the two examples given hereinabove form an integral part of the invention.
  • long fibers fibers of which the length is not preset.
  • the length of these fibers is adapted to the length of the piece to be produced.
  • the length of the fibers is normally chosen to be either identical or near to the length of the piece. There is therefore no restriction of size for the fibers, contrary to what was the case in prior art processes. This then constitutes a particularly unexpected advantage of the present invention.
  • the fibers used as reinforcing elements may be of different types without departing from the scope of the invention.
  • they may be in silicium carbide, boron, alumina, carbon and polyamides, in any forms.
  • the matrix may also be different type provided that it leads to the formation of a ceramic type material. It will advantageously be a matrix of ZrO 2 ; ZrO 2 SiO ; SiO 2 ; Al 2 O 3 ; SiO 2 Al 2 O 3 ; LiO ; TiO 2 ; ZnO ; MnO ; CaO ; CeO 2 ; MgO 5 ; Al 2 TiO 5 ; NiSiO 2 and mixtures thereof in all proportions.
  • ZrO 2 ZrO 2 SiO ; SiO 2 ; Al 2 O 3 ; SiO 2 Al 2 O 3 ; LiO ; TiO 2 ; ZnO ; MnO ; CaO ; CeO 2 ; MgO 5 ; Al 2 TiO 5 ; NiSiO 2 and mixtures thereof in all proportions.
  • a first step consists in cutting elements from a weave of graphite fibers, to the size of the electrodes.
  • cut fibers in woven form, are then placed between the plates of an electrical field generating device, which plates can be fed with a high A.C. or D.C. voltage.
  • the plates receive for a few minutes, preferably about 15 minutes, a high-voltage direct current of at least 40,000 V, preferably around 100,000 V, for spacing and swelling up the fibers, the thickness of the fibers assembly then reaching between two and four times the thickness of the bed of fibers initially introduced between the plates forming electrodes. Then, preferably, an alternating current at least equal to 20,000 V, and preferably to 25,000 V, is applied for a few minutes, preferably 15 minutes, in order to obtain a roughness of the fiber surface by surface stripping effect, or etching, resulting from localized discharges when the electrostatic field is modified by reversing the polarity of the electric field.
  • a high-voltage direct current of at least 40,000 V, preferably around 100,000 V
  • these two treatments by an electrostatic field are preferably conducted after heating the fibers in an oven, at about 350°C, said treatments being conducted by causing a steam of hot air to pass between the plates at a temperature of about 150°C.
  • another step consists in placing on each side of a metal grid in stainless steel, such as of the GANTOIS R. 0.25 type, a bulky and treated weave, then still under the effect of the electrostatic field, and coating these weaves with a view to bonding them, with a conducting adhesive forming matrix, such as for example an M. Ag type conducting adhesive, sold by the company 3M.
  • Said adhesive having been left to test as prescribed in the notice of use thereof, it is then proceeded, in an electrolytic bath, to the deposition of a metal, in this case zinc, on the swollen and etched fibers, according to the following method.
  • a metal in this case zinc
  • the electrolytic bath is prepared as follows, for 2 1 of solution :
  • the pH of the obtained solution is brought to between 2 and 5.5 with KOH.
  • the electrolytic bath solution can be used serveral times on condition that 20 g of gluconate are added in after each filtration, said gluconate being preferably sodium gluconate.
  • Electrolytic deposition of zinc is performed conventionally, a slight strirring being kept up throughout the deposition.
  • the intensity is preferably under 7 A. In the case where the intensity is below 7 A, it suffices to clean the zinc plates every two hours, whereas if the intensity is higher than 7 A, the zinc plastes must be cleaned every hour.
  • the same process can be used in particular to produce anodes in zinc, in cadmium, in lithium, in magnesium, as well as to produce cathodes in nickel, in silver, in cobalt, in titanium and in manganese.
  • the invention corresponds to an important technical progress which was totally unexpected for any one skilled in the art.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Structural Engineering (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Composite Materials (AREA)
  • General Chemical & Material Sciences (AREA)
  • Electrochemistry (AREA)
  • Mechanical Engineering (AREA)
  • Textile Engineering (AREA)
  • Inorganic Chemistry (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Thermal Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Physics & Mathematics (AREA)
  • Reinforced Plastic Materials (AREA)
  • Chemical Or Physical Treatment Of Fibers (AREA)
  • Moulding By Coating Moulds (AREA)
  • Heating, Cooling, Or Curing Plastics Or The Like In General (AREA)
  • Compositions Of Macromolecular Compounds (AREA)
EP88901042A 1987-01-23 1988-01-21 Verfahren zur herstellung eines kompositmaterials Pending EP0342197A1 (de)

Applications Claiming Priority (8)

Application Number Priority Date Filing Date Title
FR878700797A FR2609934B2 (fr) 1984-09-26 1987-01-23 Application d'un procede de preparation de materiaux composites a elements de renforcement orientes a la fabrication de produits vulcanises tels que pneumatiques et produits vulcanises, notamment pneumatiques ainsi obtenus
FR8700797 1987-01-23
FR8702105 1987-02-18
FR878702106A FR2611086B2 (fr) 1984-09-26 1987-02-18 Application ou utilisation d'un procede de preparation de materiaux composites a elements de renforcement orientes, a la fabrication d'electrodes, ainsi que les electrodes obtenues et des generateurs electrochimiques comportant de telles electrodes
FR878702105A FR2610922B2 (fr) 1984-09-26 1987-02-18 Application ou utilisation d'un procede de preparation de materiaux composites a elements de renforcement orientes, a la fabrication de ceramiques composites, et les ceramiques composites ainsi obtenues
FR8702106 1987-02-18
US27793 1987-03-19
US07/027,793 US4857244A (en) 1984-09-26 1987-03-19 Process of making a composite product, especially a vehicle tire

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Publication Number Publication Date
EP0342197A1 true EP0342197A1 (de) 1989-11-23

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EP88901042A Pending EP0342197A1 (de) 1987-01-23 1988-01-21 Verfahren zur herstellung eines kompositmaterials
EP88200098A Expired - Lifetime EP0276041B1 (de) 1987-01-23 1988-01-21 Verfahren zur Vorbereitung von Verbundmaterial einschliesslich vulkanisierter Artikel, insbesondere Reifen, Keramik und Elektroden sowie nach diesem Verfahren hergestellte Produkte

Family Applications After (1)

Application Number Title Priority Date Filing Date
EP88200098A Expired - Lifetime EP0276041B1 (de) 1987-01-23 1988-01-21 Verfahren zur Vorbereitung von Verbundmaterial einschliesslich vulkanisierter Artikel, insbesondere Reifen, Keramik und Elektroden sowie nach diesem Verfahren hergestellte Produkte

Country Status (10)

Country Link
EP (2) EP0342197A1 (de)
JP (1) JPH02501996A (de)
AU (1) AU597789B2 (de)
BR (1) BR8807320A (de)
DE (1) DE3869432D1 (de)
DK (1) DK527288A (de)
ES (1) ES2031225T3 (de)
GR (1) GR3004197T3 (de)
PT (1) PT86601B (de)
WO (1) WO1988005375A2 (de)

Cited By (1)

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Publication number Priority date Publication date Assignee Title
RU2747940C2 (ru) * 2016-07-20 2021-05-17 Мануэль ТОРРЕС МАРТИНЕС Способ обработки волокон, установка для обработки волокон и полученная таким образом лента, образованная из обработанных волокон

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Publication number Priority date Publication date Assignee Title
GB9124816D0 (en) * 1991-11-22 1992-01-15 Rolls Royce Plc Method of manufacturing a composite material
GB9124822D0 (en) * 1991-11-22 1992-01-15 Rolls Royce Plc Method of manufacturing a composite material
US5468357A (en) * 1994-12-27 1995-11-21 Hughes Missile Systems Company Densification of porous articles by plasma enhanced chemical vapor infiltration
AT410073B (de) * 1997-12-17 2003-01-27 Klaus Dipl Ing Dr Hummel Verfahren zur verbesserung der haftung von kautschukvulkanisaten an kupferlegierungen
JP5233600B2 (ja) * 2008-11-06 2013-07-10 株式会社ニコン 粒子含有樹脂の製造方法
AU2017260086A1 (en) 2016-05-04 2018-11-22 Somnio Global Holdings, Llc Additive fabrication methods and devices for manufacture of objects having preform reinforcements
CN115852590B (zh) * 2022-09-28 2023-10-10 青岛德冠超导材料制造有限公司 天然抗菌防静电纳米纤维膜及其制备方法和用途

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US3634220A (en) * 1968-09-19 1972-01-11 Us Navy Method for improving graphite fibers for plastic reinforcement and products thereof
US3771202A (en) * 1971-03-31 1973-11-13 Us Agriculture Method for electrostatic yarn bulking and impregnating
US3919437A (en) * 1972-02-22 1975-11-11 Owens Corning Fiberglass Corp Method for electrostatically impregnating strand
US4302264A (en) * 1973-06-04 1981-11-24 The General Tire & Rubber Company Method for pretreating glass cords which minimizes cord blows
US3984366A (en) * 1973-11-21 1976-10-05 The General Tire & Rubber Company Bonding glass fibers to rubber
FR2570646B1 (fr) * 1984-09-26 1987-10-30 Pradom Ltd Procede de preparation de materiaux composites a elements de renforcement orientes et produits obtenus

Non-Patent Citations (1)

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Title
See references of WO8805375A2 *

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
RU2747940C2 (ru) * 2016-07-20 2021-05-17 Мануэль ТОРРЕС МАРТИНЕС Способ обработки волокон, установка для обработки волокон и полученная таким образом лента, образованная из обработанных волокон

Also Published As

Publication number Publication date
DK527288D0 (da) 1988-09-22
DK527288A (da) 1988-09-22
AU1158788A (en) 1988-08-10
JPH02501996A (ja) 1990-07-05
WO1988005375A3 (en) 1988-10-06
EP0276041B1 (de) 1992-03-25
EP0276041A2 (de) 1988-07-27
PT86601B (pt) 1991-12-31
EP0276041A3 (en) 1988-12-28
BR8807320A (pt) 1990-05-22
PT86601A (pt) 1988-02-01
ES2031225T3 (es) 1992-12-01
DE3869432D1 (de) 1992-04-30
GR3004197T3 (de) 1993-03-31
AU597789B2 (en) 1990-06-07
WO1988005375A2 (en) 1988-07-28

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