US3861029A - Method of making heater cable - Google Patents

Method of making heater cable Download PDF

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Publication number
US3861029A
US3861029A US287444A US28744472A US3861029A US 3861029 A US3861029 A US 3861029A US 287444 A US287444 A US 287444A US 28744472 A US28744472 A US 28744472A US 3861029 A US3861029 A US 3861029A
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US
United States
Prior art keywords
temperature
resistivity
black
annealing
polymeric material
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 - Lifetime
Application number
US287444A
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English (en)
Inventor
Robert Smith-Johannsen
Jack Mclean Walker
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Raychem Corp
Original Assignee
Raychem Corp
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 to US287444A priority Critical patent/US3861029A/en
Application filed by Raychem Corp filed Critical Raychem Corp
Priority to NL7312393A priority patent/NL7312393A/xx
Priority to FR7332300A priority patent/FR2199175B1/fr
Priority to DE2345303A priority patent/DE2345303C2/de
Priority to SE7312196A priority patent/SE411086B/xx
Priority to CA180,537A priority patent/CA996171A/en
Priority to GB4214073A priority patent/GB1449262A/en
Priority to NO3500/73A priority patent/NO141489C/no
Priority to JP48101001A priority patent/JPS5818722B2/ja
Priority to BE135466A priority patent/BE804628A/xx
Priority to AU60168/73A priority patent/AU489046B2/en
Application granted granted Critical
Publication of US3861029A publication Critical patent/US3861029A/en
Priority to HK14/82A priority patent/HK1482A/xx
Priority to US07/195,558 priority patent/US4954695A/en
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

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Classifications

    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01C—RESISTORS
    • H01C7/00—Non-adjustable resistors formed as one or more layers or coatings; Non-adjustable resistors made from powdered conducting material or powdered semi-conducting material with or without insulating material
    • H01C7/02—Non-adjustable resistors formed as one or more layers or coatings; Non-adjustable resistors made from powdered conducting material or powdered semi-conducting material with or without insulating material having positive temperature coefficient
    • H01C7/027—Non-adjustable resistors formed as one or more layers or coatings; Non-adjustable resistors made from powdered conducting material or powdered semi-conducting material with or without insulating material having positive temperature coefficient consisting of conducting or semi-conducting material dispersed in a non-conductive organic material
    • 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
    • Y10T29/49082—Resistor making
    • 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
    • Y10T29/49082—Resistor making
    • Y10T29/49083—Heater type

Definitions

  • L percent by weight black and R is resistivity of the extrudate expressed in ohm-cm.
  • R resistivity of the extrudate expressed in ohm-cm.
  • the articles exhibit room temperature resistivity in the range from about 5 to 100,000 ohm-cm and may be employed, e.g., in heat tracing and thermostating applications.
  • thermoplastic compositions have previously been achieved by the addition of conductive carbon black to a polymeric base.
  • advantage has been taken of a non-linear positive temperature resistivity coefficient displayed by the particular material to obtain selfregulating or currentdimiting semicondu ctive articles.
  • U.S. Pat. No. 3,243,753 to Kohler one such composition is described as containing from 25 to 75 percent carbon black about which the polymeric matrix has been formed by in situ polymerization.
  • Self-regulating conductive compositions may, of course, be used in employments other than resistive heating, for example, in heat sensing and circuitbreaking applications.
  • the high carbon black content characteristic of most prior art compositions is disadvantageous.
  • High black loadings are associated with inferior elongation and stress crack resistance, as well as low temperature brittleness.
  • high black loading appears to adversely affect the current-regulating properties of the conductive compositions.
  • a semi-conductive thermoplastic composition is externally heated and its resistivity plotted against temperature (on the abscissa) the resulting curve will show resistivity rising with temperature from the low room temperature value (Ri) to a point of peak resistance (Rp), following which additional increase in temperature occasions a precipitous resistivity drop associated with the melt phase of the polymer matrix.
  • Ri room temperature value
  • Rp point of peak resistance
  • the practice of cross-linking the polymer matrix has grown up, in which event resistivity levels off at the peak temperature and remains constant upon further increase in ambient temperature.
  • Cross-linked semiconductive articles with high black loadings exhibit undesirably low resistivity when brought to peak temperature by exposure to very high or low ambient tempera tures. In such instances poor heat transfer characteristics can prevent dissipation of I Rp generation, causing burnout.
  • the resulting articles are suitable for freeze protection and other selflimiting applications, exhibit high Rp/Ri, and are otherwise advantaged by low black content.
  • their resistivity-temperature properties are stable in storage and unaffected by temperature cycling.
  • FIG. 1 is a cross-sectioned end-on view of one jacketed extrudate formed according to the practice of this invention.
  • FIG. 2 is a flow chart which depicts the steps of the preferred manner of obtaining jacketed extrudates like those depicted in FIG. 1.
  • the polymeric matrix in which conductive black is dispersed in whatever proportion must exhibit overall an appropriately non-linear coefficient of thermal expansion, for which reason a degree of crystallinity is believed essential.
  • polymers exhibiting at least about percent crystallinity as determined by x-ray diffraction are suited to the practice of the invention.
  • polystyrene resin such as low, medium and high density polyethylenes and polypropylene, polybutene-l, poly(dodecamethylene pyromellitimide), ethylene-propylene copolymers and terpolymers with non-conjugated dienes, polyvinylidine fluoride, polyvinylidine fluoride-tetrafluoroethylene copolymers, etc.
  • polyolefins such as low, medium and high density polyethylenes and polypropylene, polybutene-l, poly(dodecamethylene pyromellitimide), ethylene-propylene copolymers and terpolymers with non-conjugated dienes, polyvinylidine fluoride, polyvinylidine fluoride-tetrafluoroethylene copolymers, etc.
  • limiting temperatures tailored to the application intended eg., freeze protection, thermostatting,
  • polymeric matrix material may be obtained by appropriate selection of polymeric matrix material.
  • elements which self-limit at temperatures on the order of 100F, 130F, 150F, 180F and 250F may be produced with, respectively, wax-poly(ethylene-vinyl acetate) blends, low density polyethylene, high density polyethylene, polypropylene and polyvinylidene fluoride.
  • Other criteria of polymer selection will, in particular instances, include desired elongation, environmental resistance, ease of extrusibility, etc., as is well known.
  • Particularly preferred matrix materials are multicomponent blends in which black is mixed with a first blend component to form a master batch which is in turn mixed with the principal polymeric component.
  • the first and second polymer blend components are chosen such that they exhibit a positive free energy of mixing, one with the other. Their attendant incompatibility apparently has the effect of segregating contained black into generally delimited regions of the polymer matrix, and such blends have proven extremely stable in the face of temperature cycling in use. In the case of single component matrices, cycling has occasionally had the effect of requiring that successively higher temperatures be attained to provide identical wattage values. Of course, even in the case of single component matrices, the low black loadings achieved according to this invention can result in satisfactory stability to cycling.
  • the minor polymeric blend component is chosen for superior compatibility with carbon black relative to the blend component present in major proportion, while the latter component is selected for the particular physical properties desired in the overall extrudate.
  • the principal blend component is preferably present in at least'about 3:1 weight ratio relative to the minor component with which the black is first mixed.
  • the blends most preferred have a polyethylene as the principal component, the other being an ethylene-vinyl ester copolymer, such as ethylene-vinyl acetate or ethylene-ethylacrylate copolymers.
  • An especially preferred extrudate contains about 70:20 polyethylene: ethylene-ethyl acrylate copolymer by weight.
  • the carbon blacks employed are those conventionally used in conductive plastics, eg., high structure varieties such as furnace and channels blacks.
  • Other conventional addends such as antioxidants. etc., may be employed provided only that their quantities and characteristics do not subvert the objects of the invention.
  • An especially interesting class of beneficial addends are materials such as waxes which, while compatible with the predominant blend component, melt at lower temperature. The result is to permit obtainment of a given wattage at lower temperature, owing to a first peaking effect of the wax on the resistivity-temperature curve.
  • Compounding is conventional and generally involves banburying, milling and pelletizing prior to pressure extrusion of the selflimiting element from the melt.
  • the black-containing matrix 1 is extruded onto a spaced-apart pair of elongate electrodes 2 to form an element rod-shaped or, most preferably, dumbellshaped in cross-section, the extruded thermoplastic both encapsulating and interconnecting the electrodes. Thereafter, polymeric jackets 3 and 4 may be extruded thereover, as in the fourth and sixth steps of the flow chart which is FIG. 2.
  • resistivity values must be in the range from about 6,000 to 100,000 ohm-cm in order to generate 4-watts per foot and, of course, lower at a particular voltage to obtain as much as 8 watts/foot.
  • room temperature resistivity is greater than about 10 ohm-cm, and most commonly on the order of the resistivity of the dielectric polymer matrix itself. At such resistivities available wattage under power is essentially zero.
  • Annealing is performed at a temperature greater than about 250F, preferably at at least about 300F, and in any case at or above the melting point or range of the polymeric matrix in which the carbon black is dispersed.
  • the period over which annealing is effected will, it will be appreciated, vary with the nature of the particular matrix and the amount of carbon black contained therein.
  • annealing occurs over a time sufficient to reduce resistivity of the annealed element to satisfaction of the equation 2 L 5 log R s 45, preferably 40, and the time necessary in a particular case may be readily determined empirically.
  • annealing is conducted over a period in excess of 15 hours, and commonly at least about a 24 hour anneal is had.
  • control cooling is substantially less important where the requisite overall annealing residence time is divided into at least about three roughly equal stages, and the element returned to room temperature between each annealing stage.
  • the self-limiting element Upon completion of annealing and optional addition of a further insulative jacket of, e.g., polyethylene, the self-limiting element is desirably subjected to ionizing radiation sufficient in strength to cross-link the blackcontaining core.
  • Radiation dosage is selected with an eye to achieving cross-linking sufficient to impart a degree of thermal stability requisite to the particularly intended application without unduly diminishing crystallinity of the polymer matrix, i.e., overall crystallinity of the cross-linked black-containing matrix less than about 20 percent is to be avoided.
  • radiation dosage may in particular cases range from about 2 to megarads or more, and preferably is about 12 megarads.
  • EXAMPLE 1 Seventy-six lbs. of polyethylene (density 0.929 gm/cc, 32 lbs. ofa mixture of 34 percent Vulcan XC-72 and ethylene ethyl acrylate copolymer (density 0.930 gm/cc, 18 percent ethyl acrylate) were loaded with 1 lb. of antioxidant into a Banbury mixer. The ram was closed and mixing commenced. When temperature reached about 24050F the batch was dumped, placed in a 2-roll mill, and cut off in strips which were fed to a pelletizing extruder.
  • the pelletized compound was next extruded onto two parallel tinned copper electrodes AWG 19/32) to form an extrudate generally dumbbell-shaped in cross-section.
  • the electrodes were 0.275 inch apart (center-to-center), the interconnecting web being about 15 mils in thickness, at least 8 mils thickness of the semiconductive composition surrounding the electrodes.
  • Extrusion was performed in a plasticating extruder with crosshead attachment (Davis- Standard 2 inches extruder, 24/1 L/D, with PE screw. Thereafter, the same extruder was arranged to extrude an 8 mil thick insulation jacket of polyurethane (Texin 59l-A, available from the Mobay Corporation).
  • a conventional tube extrusion method was employed in which a vacuum (eg., 5-20 in. H O) is drawn in the molten tube to collapse it about the semiconductive core within about 3 inches of the extrusion head.
  • the jacketed product was next spooled onto aluminum disks (26 inches dia) and exposed to 300F for 24 hours in a circulating air oven. Following this thermal structuring procedure and cooling to room temperature oven about 1 /2 hours the resistivity of the sample was determined at various tem- Additional extrudates were prepared with various polymers and black loadings following the procedure of Example 1 save where otherwise indicated below.
  • the polymeric matrices for the various examples were as follows: (2) a 3:1 blend of low density polyethylene: ethylene ethyl acrylate copolymer; (3) a 5:1 blend of low density polyethylene: ethylene vinyl acetate copolymer; (4) polyvinylidene fluoride; (5) a 3:1 blend of medium density polyethylene: ethylene-ethyl acrylate copolymer; (6) a 3:1 blend of high density polyethylene: ethylene-ethyl acrylate copolymer; (7) ethylene/- propylene copolymer (Eastman Chemical Companys Polyallomer”); (8) polybutene-l; and (9) polyvinylidene fluoride/tetrafluoroethylene copolymer (Pennwalt Chemical Companys Kynar 5200).
  • an electrically conductive self-regulating article which comprises the steps of l extruding onto a pair of elongate parallel electrodes held in spaced-apart relation an electrodeinterconnecting web of a composition consisting essentially of a thermoplastic crystalline polymeric material exhibiting overall at least about 20 percent crystallinity as determined by x-ray diffraction and (b) conductive carbon black, the percentage by weight (L) of carbon black based on the total weight of said composition being not greater than about 15, the resulting extrudate exhibiting room temperature resistivity (R, ohm-cm) greater than about 10, and (2) annealing the extrudate at or above the melting temperature of said crystalline polymeric material for a period of time sufficient to reduce R to satisfaction of the equation 2L-l-Slog R s 45,
  • the value L being not more thanabout ten, annealing being performed at a temperature of at least about 300F over a period of not less than about 15 hours.
  • polymeric material is a blend of polyethylene and, in minor proportion relative thereto, a copolymer of ethylene and a vinyl ester.

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  • Engineering & Computer Science (AREA)
  • Microelectronics & Electronic Packaging (AREA)
  • Chemical & Material Sciences (AREA)
  • Dispersion Chemistry (AREA)
  • Ceramic Engineering (AREA)
  • Physics & Mathematics (AREA)
  • Electromagnetism (AREA)
  • Compositions Of Macromolecular Compounds (AREA)
  • Conductive Materials (AREA)
  • Apparatuses And Processes For Manufacturing Resistors (AREA)
  • Semiconductor Integrated Circuits (AREA)
  • Thermistors And Varistors (AREA)
US287444A 1972-09-08 1972-09-08 Method of making heater cable Expired - Lifetime US3861029A (en)

Priority Applications (13)

Application Number Priority Date Filing Date Title
US287444A US3861029A (en) 1972-09-08 1972-09-08 Method of making heater cable
JP48101001A JPS5818722B2 (ja) 1972-09-08 1973-09-07 自己調節性電気物品およびその製造方法
DE2345303A DE2345303C2 (de) 1972-09-08 1973-09-07 Sich selbst regulierender elektrischer Widerstandskörper und Verfahren zu dessen Herstellung
SE7312196A SE411086B (sv) 1972-09-08 1973-09-07 Elektriskt resistivt foremal for sjelvreglerande och strombegrensande tillempningar samt forfarande for dess framstellning
CA180,537A CA996171A (en) 1972-09-08 1973-09-07 Self limiting conductive extrudates
GB4214073A GB1449262A (en) 1972-09-08 1973-09-07 Sel-limiting conductive extrudates and methods for their manufacture
NL7312393A NL7312393A (en, 2012) 1972-09-08 1973-09-07
FR7332300A FR2199175B1 (en, 2012) 1972-09-08 1973-09-07
BE135466A BE804628A (fr) 1972-09-08 1973-09-07 Produits manufactures extrudes conducteurs autolimitants
NO3500/73A NO141489C (no) 1972-09-08 1973-09-07 Fremgangsmaate ved fremstilling av et selvregulerende, baandformet, elektrisk motstandselement
AU60168/73A AU489046B2 (en) 1973-09-10 Self-limiting conductive extrudates
HK14/82A HK1482A (en) 1972-09-08 1982-01-14 Self-limiting conductive extrudates and methods for their manufacture
US07/195,558 US4954695A (en) 1972-09-08 1988-05-12 Self-limiting conductive extrudates and methods therefor

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
US287444A US3861029A (en) 1972-09-08 1972-09-08 Method of making heater cable

Related Child Applications (2)

Application Number Title Priority Date Filing Date
US54259275A Division 1975-01-20 1975-01-20
US54259275A Continuation 1975-01-20 1975-01-20

Publications (1)

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US3861029A true US3861029A (en) 1975-01-21

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US287444A Expired - Lifetime US3861029A (en) 1972-09-08 1972-09-08 Method of making heater cable

Country Status (11)

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US (1) US3861029A (en, 2012)
JP (1) JPS5818722B2 (en, 2012)
BE (1) BE804628A (en, 2012)
CA (1) CA996171A (en, 2012)
DE (1) DE2345303C2 (en, 2012)
FR (1) FR2199175B1 (en, 2012)
GB (1) GB1449262A (en, 2012)
HK (1) HK1482A (en, 2012)
NL (1) NL7312393A (en, 2012)
NO (1) NO141489C (en, 2012)
SE (1) SE411086B (en, 2012)

Cited By (116)

* Cited by examiner, † Cited by third party
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US4954695A (en) * 1972-09-08 1990-09-04 Raychem Corporation Self-limiting conductive extrudates and methods therefor
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US5052699A (en) * 1989-07-10 1991-10-01 Raychem Corporation Grommet
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DE2345303A1 (de) 1974-04-18
NO141489C (no) 1980-03-19
GB1449262A (en) 1976-09-15
NL7312393A (en, 2012) 1974-03-12
FR2199175B1 (en, 2012) 1977-09-23
FR2199175A1 (en, 2012) 1974-04-05
DE2345303C2 (de) 1984-09-20
CA996171A (en) 1976-08-31
JPS5818722B2 (ja) 1983-04-14
NO141489B (no) 1979-12-10
JPS4968296A (en, 2012) 1974-07-02
HK1482A (en) 1982-01-22
AU6016873A (en) 1975-03-13
BE804628A (fr) 1974-03-07
SE411086B (sv) 1979-11-26

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