EP0222507B1 - Formteile aus vernetzten Polymeren - Google Patents

Formteile aus vernetzten Polymeren Download PDF

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Publication number
EP0222507B1
EP0222507B1 EP86307817A EP86307817A EP0222507B1 EP 0222507 B1 EP0222507 B1 EP 0222507B1 EP 86307817 A EP86307817 A EP 86307817A EP 86307817 A EP86307817 A EP 86307817A EP 0222507 B1 EP0222507 B1 EP 0222507B1
Authority
EP
European Patent Office
Prior art keywords
cross
layer
polymer
linking agent
psi
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.)
Expired
Application number
EP86307817A
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English (en)
French (fr)
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EP0222507A1 (de
Inventor
Hans E. Lunk
Ashok Mehan
Neal Enault
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.)
Raychem Corp
Original Assignee
Raychem Corp
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Filing date
Publication date
Application filed by Raychem Corp filed Critical Raychem Corp
Priority to AT86307817T priority Critical patent/ATE48720T1/de
Publication of EP0222507A1 publication Critical patent/EP0222507A1/de
Application granted granted Critical
Publication of EP0222507B1 publication Critical patent/EP0222507B1/de
Expired legal-status Critical Current

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Classifications

    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B7/00—Insulated conductors or cables characterised by their form
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B3/00—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties
    • H01B3/18—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances
    • H01B3/30—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances plastics; resins; waxes
    • H01B3/44—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances plastics; resins; waxes vinyl resins; acrylic resins
    • H01B3/443—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances plastics; resins; waxes vinyl resins; acrylic resins from vinylhalogenides or other halogenoethylenic compounds

Definitions

  • This invention relates to insulated electrical conductors.
  • insulated wires include wires coated with a layer of a radiation cross-linked fluorocarbon polymer, particularly an ethylene/tetrafluoroethylene copolymer (often referred to as an ETFE polymer), which are extensively used for the wiring in aircraft.
  • ETFE polymer ethylene/tetrafluoroethylene copolymer
  • Military Specification No. MiL-W-22759 sets various standards for such standards for such insulated wires. Reference may be made for example to U.S. Patents Nos. 3 763 222,3 840 619,3 894118,3 911 192, 3 970 770, 985 716,3 995 091,4 031 167,4 155 823 and 4 353 961.
  • Such wires have the significant disadvantage that if the outer surface of the insulation is damaged, subsequent flexing of the wire causes the damage to propagate through the insulation, at a rate which is highly undesirable. This disadvantage is especially serious when the insulated wire is to be used in an aircraft or in other high performance situations where the consequences of insulation failure can be so serious. A quantitative measure of this disadvantage can be obtained from a notch propagation test such as that described below.
  • insulation which comprises an inner layer of a polymer which has little cross-linking and an outer layer of polymer which has a relatively high level of cross-linking. Furthermore, this improvement is obtained with little or no substantial deterioration of other important properties of the insulation, for example, resistance to scrape abrasion, resistance to crossed wire abrasion and resistance to cut-through.
  • the present invention provides an insulated electrical conductor, especially a wire, which comprises:
  • the M 100 values given herein are modulus values measured at a temperature above the melting point of the polymer by the procedure described in detail below, and therefore reflect the level of cross-linking in the layer.
  • a preferred method of making such an insulated conductor comprises:
  • the polymeric component in the polymeric compositions used in the present invention preferably comprises, and more preferably consists essentially of, a melt-shapeable crystalline polymer having a melting point of at least 200 ° C, preferably at least 250 ° C, or a mixture of such polymers.
  • melting point is used herein to denote the temperature above which no crystallinity exists in the polymer (or, when a mixture of crystalline polymers is used, in the major crystalline component of the mixture).
  • fluorocarbon polymer is used herein to denote a polymer or mixture of polymers which contains more than 10%, preferably more than 25%, by weight of fluorine.
  • the fluorocarbon polymer may be a single fluorine-containing polymer, a mixture of two or more fluorine-containing polymers, or a mixture of one or more fluorine-containing polymers with one or more polymers which do not contain fluorine.
  • the fluorocarbon polymer comprises at least 50%, particularly at least 75%, especially at least 85%, by weight of one or more thermoplastic crystalline polymers each containing at least 25% by weight of fluorine, a single such crystalline polymer being preferred.
  • Such a fluorocarbon polymer may contain, for example, a fluorine-containing elastomer and/or a polyolefin, preferably a crystalline polyolefin, in addition to the crystalline fluorine-containing polymer or polymers.
  • the fluorine-containing polymers are generally homo- or co-polymers of one or more fluorine-containing olefinically unsaturated monomers, or copolymers of one or more such monomers with one or more olefins.
  • the fluorocarbon polymer has a melting point of at least 200 ° C, and will often have a melting point of at least 250°C, e.g. up to 300°C.
  • the polymeric composition has a viscosity of less than 105 poise at a temperature not more than 60 ° C above its melting point.
  • a preferred fluorocarbon polymer is a copolymer of ethylene and tetrafluoroethylene and optionally one or more other comonomers, especially a copolymer comprising 35 to 60 mole percent of ethylene, 35 to 60 mole percent of tetrafluoroethylene and up to 10 mole percent of one or more other comonomers.
  • polymers which can be used include copolymers of ethylene and chlorotrifluoroethylene; copolymers of vinylidene fluoride with one or both of hexafluoropropylene and tetrafluoroethylene, or with hexafluoroisobutylene; and copolymers of tetrafluoroethylene and hexafluoropropylene.
  • the polymeric composition can optionally contain suitable additives such as pigments, antioxidants, thermal stabilisers, acid acceptors and processing aids.
  • the first and second compositions preferably contain the same polymeric components, and more preferably are substantially the same in all respects except for the level of cross-linking.
  • the conductor is preferably a metal (e.g. copper) wire, which may be stranded or solid.
  • the wire may be for example from 10 to 26 AWG in size.
  • the first layer preferably contacts the conductor.
  • the second member is preferably also in the form of a layer which has the same general shape as the first layer or which serves to join together a number of wires each of which is surrounded by a first layer, thus forming a ribbon cable.
  • the layers are preferably in direct contact, but may be joined together by a layer of adhesive.
  • the first and second members are preferably formed by melt-extrusion, particularly by sequential extrusion, which may be tubular or pressure extrusion, so that the layers are hot when first contacted, in order to promote migration of the cross-linking agent.
  • the polymeric compositions should preferably be selected so that at least the outer layer has a tensile strength of at least 3,000 psi (210 kg/cm 2 ); and since a higher tensile strength is usually desired in the cross-linked product and there is frequently a loss of tensile strength during the irradiation step, a higher initial tensile strength is preferred, e.g. greater than 6,000 psi (420 kg/cm 2 ), preferably at least 7,000 psi (490 kg/cm2), particularly at least 8,000 psi (560 kg/cm2).
  • the thickness of the inner layer is generally 0.0075 to 0.038 cm (0.003 to 0.015 inch), preferably 0.0075 to 0.0225 cm (0.003 to 0.009 inch).
  • the thickness of the outer layer is generally 0.01 to 0.063 cm (0.004 to 0.025 inch), preferably 0.01 to 0.023 cm (0.005 to 0.009 inch).
  • Preferred radiation cross-linking agents contain carbon-carbon unsaturated groups in a molar percentage greater than 15, especially greater than 20, particularly greater than 25.
  • the cross-linking agent contains at least two ethylenic double bonds, which may be present, for example, in allyl, methallyl, propargyl or vinyl groups.
  • cross- linking agents are triallyl cyanurate (TAC) and triallyl isocyanurate (TAIC); other specific cross-linking agents include triallyl trimellitate, triallyl trimesate, tetrallyl pyromellitate, the diallyl ester of 1,1,3-trimethyl-5-carboxy-3-(p-carboxyphenyl) indan.
  • TAC triallyl cyanurate
  • TAIC triallyl isocyanurate
  • Other cross-linking agents which are known for incorporation into fluorocarbon polymers prior to shaping, for example those disclosed in U.S. Patents referenced above, can also be used. Mixtures of cross-linking agents can be used.
  • the first composition as extruded contains little or no cross- linking agent (e.g. 0 to 2% by weight, preferably 0%), and the second composition as extruded contains more than is desired during the cross-linking step, e.g. at least 5%, preferably 5 to 25%, particularly 7 to 12%, by weight.
  • the time for which the layers should be maintained in contact prior to cross-linking depends upon the extent of migration which is needed and the temperature during such contact, which is preferably 5 to 150 ° C below the melting point of the polymer (or the lower melting polymer if there are two or more polymers in the layers).
  • the inner layer preferably contains 0 to 3% by weight of cross- linking agent and the outer layer preferably contains 3 to 10% by weight of crosslinking agent.
  • the dosage employed in the irradiation step is generally below 50 Mrads to ensure that the polymer is not degraded by excessive irradiation, and the dosages preferably employed will of course depend upon the extent of cross-linking desired, balanced against the tendency of the polymer to be degraded by high doses of irradiation. Suitable dosages are generally in the range 2 to 40 Mrads, for example 2 to 30 Mrads, preferably 3 to 20 Mrads, especially 5 to 25 or 5 to 20 Mrads, particularly 5 to 15 Mrads.
  • the ionising radiation can for example be in the form of accelerated electrons or gamma rays. Irradiation is generally carried out at about room temperature, but higher temperatures can also be used.
  • the inner layer preferably has an Mice value of at least 2.8 kg/cm2 (40 psi) and especially from 3.5 to 10.5 kg/cm 2 (50 to 150 psi).
  • the elongation of the inner layer is preferably at least 100%, particularly at least 125%, e.g. at least 150%, especially 200 to 300%.
  • the outer layer is preferably cross-linked so that it has an Mice value of at least 28 kg/cm 2 (400 psi), particularly at least 31.5 kg/cm 2 (450 psi), with yet higher values of at least 42 kg/cm 2 (600 psi) being valuable in many cases.
  • the elongation of the outer layer is preferably 40 to 150%, particularly 50 to 120%.
  • the Notch Propagation Values are measured on a piece of insulated wire about 30 cm (12 inch) long.
  • a notch is made in the insulation, about 5 cm (2 inch) from one end, by means of a razor blade at right angles to the axis of the wire.
  • the depth of the notch is controlled by mounting the razor blade between two metal blocks so that it protrudes by a distance which is 0.01 cm (0.004) inch or., if the insulation comprises two layers and the outer layer has a thickness t which is less than 0.018 cm (0.007 inch) thick, by a distance which is (t-0.0051) cm [(t-0.002) inch].
  • the end of the wire closer to the notch is secured to a horizontal mandrel whose diameter is three times the outer diameter of the insulation.
  • a 0.675 kg (1.5 Ib) weight is secured to the other end of the wire so that the wire hangs vertically.
  • the mandrel is then rotated clockwise, at about 60 revolutions a minute, until most of the wires has wrapped around the mandrel.
  • the mandrel is then rotated, counterclockwise, until the wire has unwrapped and most of the wire has again been wrapped around the mandrel.
  • the mandrel is then rotated clockwise until the wire has unwrapped and most of the wire has again been wrapped around the mandrel. This sequence is continued until visual observation of the notched area shows the conductor to be exposed.
  • the M 100 values are determined by a static modulus test as described in U.S. Patent No. 4,353,961 carried out at about 40°C above the melting point of the polymer, (e.g. at about 320 ° C for ETFE polymers).
  • the tensile strengths and elongations are determined in accordance with ASTM D 638-72 (i.e. at 23 ° C) at a testing speed of 50 mm (2 inch) per minute.
  • cross-wire abrasion values are measured by the tests described in U.S. Patent No. 4,353,961.
  • Example 1 is a comparative Example.
  • a 20 AWG (19/32) stranded tin-coated copper wire was insulated by melt-extruding over it, by sequential extrusion, an inner insulating layer 0.01 to 0.0125 cm (0.004 to 0.005 inch) thick and an outer insulating layer .018 to 0.020 cm (0.007 to 0.008 inch) thick.
  • the layers were composed of the following compositions:
  • the polymeric insulation was cross-linked by irradiating it to a dosage of 14 Mrads.
  • Example 1 The procedure of Example 1 was followed except that the composition of the inner layer was

Landscapes

  • Physics & Mathematics (AREA)
  • Spectroscopy & Molecular Physics (AREA)
  • Organic Insulating Materials (AREA)
  • Processes Specially Adapted For Manufacturing Cables (AREA)
  • Compositions Of Macromolecular Compounds (AREA)
  • Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
  • Insulated Conductors (AREA)
  • Extrusion Moulding Of Plastics Or The Like (AREA)
  • Connection Or Junction Boxes (AREA)
  • Installation Of Indoor Wiring (AREA)
  • Patch Boards (AREA)
  • Laminated Bodies (AREA)
  • Processes Of Treating Macromolecular Substances (AREA)
  • Dental Preparations (AREA)
  • Materials For Medical Uses (AREA)

Claims (8)

1. Isolierter elektrischer Leiter, insbesondere Draht, der folgendes aufweist:
(1) einen elektrischen Leiter; und
(2) eine elektrische Isolierung, umfassend
(a) eine innere elektrisch isolierende Schicht, die
(i) aus einer ersten schmelzbearbeiteten, vernetzten polymeren Zusammensetzung besteht, wobei das Polymer ein Fluorcarbonpolymer mit einem Schmelzpunkt von mindestens 200°C aufweist, und die
(ii) einen ersten Mioo-Wert von 0 bis 17,5 kg/cm2 (0 bis 250 psi) hat; und
(b) eine äußere elektrisch isolierende Schicht, die
(i) durch eine innere Schicht vom Leiter getrennt ist,
(ii) aus einer zweiten schmelzbearbeiteten vernetzten polymeren Zusammensetzung besteht, wobei das Polymer ein Fluorcarbonpolymer mit einem Schmelzpunkt von mindestens 200°C aufweist, und
(iii) einen zweiten Mioo-Wert von mindestens 24,5 kg/cm2 (350 psi) hat.
2. Isolierter Leiter nach Anspruch 1, wobei das Polymer in mindestens einer der ersten und zweiten polymeren Zusammensetzungen im wesentlichen aus einem kristallinen Polymer besteht, das 35 bis 60 Molprozent von Ethylen abgeleitete Einheiten, 35 bis 60 Molprozent von Tetrafluorethylen abgeleitete Einheiten, sowie 0 bis 10 Prozent Einheiten enthält, die von mindestens einem zusätzlichen copolymerisierbaren Comonomer abgeleitet sind.
3. Isolierter Leiter nach Anspruch 1 oder 2, wobei die innere Schicht einen Mloo-Wert von 2,8 bis 17,5 kg/cm2 (40 bis 250 psi), vorzugsweise 3,5 bis 10,5 kg/cm2 (50 bis 150 psi), und die äußere Schicht einen Mloo-Wert von mindestens 28 kg/cm2 (400 psi), vorzugsweise mindestens 42 kg/cm2 (600 psi) aufweist.
4. Isolierter Leiter nach einem der vorangehenden Ansprüche, wobei die innere Schicht eine Dehnung von mindestens 100%, vorzugsweise 200 bis 300%, und die äußere Schicht eine Dehnung von 40 bis 150%, vorzugsweise 50 bis 120% aufweisen.
5. Isolierter Leiter nach einem der vorangehenden Ansprüche, wobei der Leiter ein Metalldraht ist und wobei die innere Schicht mit dem Draht in Kontakt steht, 0,0075 bis 0,038 cm (0,003 bis 0,015 Inch) dick ist und eine Dehnung von mindestens 125% aufweist; und wobei die äußere Schicht mit der inneren Schicht in Kontakt steht, 0,01 bis 0,063 cm (0,004 bis 0,025 Inch) dick ist und eine Dehnung von 50 bis 120% aufweist.
6. Isolierter Leiter nach einem der vorangehenden Ansprüche, wobei jede Schicht mit Hilfe von mindestens einer der Verbindungen Triallylcynanurat und Triallylisocyanurat durch Bestrahlung vernetzt worden ist.
7. Verfahren zur Herstellung eines isolierten Leiters nach einem der vorangehenden Ansprüche, das folgende Schritte umfaßt:
(1) Bildung einer ersten isolierenden Schicht durch Schmelzextrudieren einer ersten elektrisch isolierenden Zusammensetzung um einen Draht herum, wobei die erste elektrisch isolierende Zusammensetzung ein Fluorcarbonpolymer mit einem Schmelzpunkt von mindestens 200°C ist und 0 bis 2 Gew.-% eines durch Strahlung vernetzenden Agens enthält;
(2) Bildung einer zweiten isolierenden Schicht durch Schmelzextrudieren einer zweiten elektrisch isolierenden Zusammensetzung um die erste isolierende Schicht herum, wobei die zweite isolierende Zusammensetzung ein Fluorcarbonpolymer mit einem Schmelzpunkt von mindestens 200°C ist und mindestens 5 Gew.-% eines durch Strahlung vernetzenden Agens enthält;
(3) Aufrechterhalten des Kontaktes zwischen der ersten und der zweiten Schicht unter solchen Bedingungen, daß ein Teil des durch Strahlung vernetzenden Agens aus der zweiten Schicht in die erste Schicht hineinwandert; und
(4) Bestrahlung der ersten und der zweiten Schicht zur Durchführung der Vernetzung ohne weitere Zugabe von durch Strahlung vernetzendem Agens zu den Schichten, derart, daß die erste isolierende Schicht einen ersten Mioo-Wert von weniger als 17,5 kg/cm2 und die isolierende Schicht einen zweiten Mioo-Wert von mindestens 24,5 kg/cm2 erhält.
8. Verfahren nach Anspruch 7, wobei die erste polymere Zusammensetzung, wenn sie schmelzgeformt ist, im wesentlichen frei ist von durch Strahlung vernetzendem Agens, und die zweite polymere Zusammensetzung, unmittelbar nach dem sie schmelzgeformt wurde, mindestens 5 Gew.-% an durch Strahlung vernetzendem Agens enthält.
EP86307817A 1985-10-11 1986-10-09 Formteile aus vernetzten Polymeren Expired EP0222507B1 (de)

Priority Applications (1)

Application Number Priority Date Filing Date Title
AT86307817T ATE48720T1 (de) 1985-10-11 1986-10-09 Formteile aus vernetzten polymeren.

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
US78680685A 1985-10-11 1985-10-11
US786806 1985-10-11

Publications (2)

Publication Number Publication Date
EP0222507A1 EP0222507A1 (de) 1987-05-20
EP0222507B1 true EP0222507B1 (de) 1989-12-13

Family

ID=25139639

Family Applications (1)

Application Number Title Priority Date Filing Date
EP86307817A Expired EP0222507B1 (de) 1985-10-11 1986-10-09 Formteile aus vernetzten Polymeren

Country Status (9)

Country Link
EP (1) EP0222507B1 (de)
JP (1) JPH0679451B2 (de)
KR (1) KR950007089B1 (de)
AT (1) ATE48720T1 (de)
BR (1) BR8604970A (de)
CA (1) CA1295574C (de)
DE (1) DE3667569D1 (de)
ES (1) ES2012452B3 (de)
IL (1) IL80269A (de)

Families Citing this family (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
AU606731B2 (en) * 1987-07-10 1991-02-14 Raychem Limited Electrical wire with polyamide/fluoropolymer insulation
CA2187219C (en) * 1994-04-07 2007-10-02 Steven C. Zingheim Insulated wire and cable
AU1105801A (en) * 1999-09-07 2001-04-10 Judd Wire, Inc. Dual layer system suitable for use as electrical insulation for wires and other conductors
US7915532B2 (en) 2007-06-08 2011-03-29 Westerngeco L.L.C. Enhanced electrical seismic land cable
JP5276891B2 (ja) * 2008-05-02 2013-08-28 株式会社クラベ 耐熱耐油絶縁電線及びその製造方法
CN106661297A (zh) * 2014-07-04 2017-05-10 旭硝子株式会社 氟树脂组合物及其制造方法、以及成形物、发泡成形物以及被覆电线

Family Cites Families (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3269862A (en) 1964-10-22 1966-08-30 Raychem Corp Crosslinked polyvinylidene fluoride over a crosslinked polyolefin
US4101699A (en) * 1973-11-23 1978-07-18 Samuel Moore & Company Synthetic resinous tube
US3852518A (en) 1973-11-29 1974-12-03 Gen Cable Corp Irradiation cross-linked composite low density/high density polyethylene insulated 600 volt power cables
JPS5391959A (en) * 1976-10-12 1978-08-12 Raychem Corp Molded article of cross bonded fluorinated carbon polymer and method of making same
US4155823A (en) * 1976-10-12 1979-05-22 Raychem Corporation Shaped article from crosslinked fluorocarbon polymer and process therefor
US4353961A (en) 1977-09-14 1982-10-12 Raychem Corporation Shaped article from crosslinked fluorocarbon polymer
US4310597A (en) * 1978-07-10 1982-01-12 Northern Telecom Limited Low voltage electrical wire
CA1151255A (en) * 1980-11-06 1983-08-02 Eric P. Marsden Electrical insulated wire with flexibility and abrasion-resistant layer

Also Published As

Publication number Publication date
DE3667569D1 (de) 1990-01-18
ATE48720T1 (de) 1989-12-15
BR8604970A (pt) 1987-07-14
IL80269A (en) 1991-03-10
JPH0679451B2 (ja) 1994-10-05
JPS6293806A (ja) 1987-04-30
EP0222507A1 (de) 1987-05-20
CA1295574C (en) 1992-02-11
IL80269A0 (en) 1987-01-30
KR950007089B1 (ko) 1995-06-30
KR870004466A (ko) 1987-05-09
ES2012452B3 (es) 1990-04-01

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