EP0311142A2 - Vernetzung von PTC-leitfähigen Polymeren durch Strahlung - Google Patents

Vernetzung von PTC-leitfähigen Polymeren durch Strahlung Download PDF

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Publication number
EP0311142A2
EP0311142A2 EP88117360A EP88117360A EP0311142A2 EP 0311142 A2 EP0311142 A2 EP 0311142A2 EP 88117360 A EP88117360 A EP 88117360A EP 88117360 A EP88117360 A EP 88117360A EP 0311142 A2 EP0311142 A2 EP 0311142A2
Authority
EP
European Patent Office
Prior art keywords
electrodes
mrads
ptc element
ptc
cross
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.)
Granted
Application number
EP88117360A
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English (en)
French (fr)
Other versions
EP0311142A3 (en
EP0311142B1 (de
Inventor
Stephen M. Jacobs
Mary Sandra Mctavish
James Michael Taylor
Frank Anthony Doljack
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
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Raychem Corp
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Filing date
Publication date
Priority claimed from US06/254,352 external-priority patent/US4426633A/en
Application filed by Raychem Corp filed Critical Raychem Corp
Priority to AT88117360T priority Critical patent/ATE98807T1/de
Publication of EP0311142A2 publication Critical patent/EP0311142A2/de
Publication of EP0311142A3 publication Critical patent/EP0311142A3/en
Application granted granted Critical
Publication of EP0311142B1 publication Critical patent/EP0311142B1/de
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

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    • 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
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
    • H01B1/20—Conductive material dispersed in non-conductive organic material
    • H01B1/24—Conductive material dispersed in non-conductive organic material the conductive material comprising carbon-silicon compounds, carbon or silicon
    • 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
    • H05B3/00—Ohmic-resistance heating
    • H05B3/10—Heating elements characterised by the composition or nature of the materials or by the arrangement of the conductor
    • H05B3/12—Heating elements characterised by the composition or nature of the materials or by the arrangement of the conductor characterised by the composition or nature of the conductive material

Definitions

  • This invention relates to the radiaton cross-­linking of PTC conductve polymers.
  • the invention provides a process for the preparation of an electrical device com­prising (a) a cross-linked PTC conductive polymer element and (b) two electrodes which can be connected to a power source to cause current to flow through the PTC element, which process comprises cross-linking the PTC element by irradiating it to a dosage of at least 50 Mrads, subject to the proviso that if each of the electrodes has a substan­tially planar configuration, then either (a) the element is irradiated to a dosage of at least 120 Mrads, or (b) the electrodes are metal foil electrodes which are secured to the PTC element after it has been cross-linked.
  • the radiaton dose is, therefore, preferably at least 60 Mrads, particularly at least 80 Mrads, wth yet higher dosages, e.g. at least 120 Mrads or at least 160 Mrads, being preferred when satisfactory PTC characteristics are maintained and the desire for improved performance outweighs the cost of radiation.
  • This method involves the use of a scanning electron microscope (SEM) to measure the maximum rate at which the voltage changes in the PTC element when the device is in the tripped state. This maximum rate occurs in the so-called "hot zone" of the PTC element. The lower the maximum rate, the greater the number of trips that the device will withstand.
  • SEM scanning electron microscope
  • an electrical device which comprises (a) a radiaton cross-linked PTC conductive polymer element and (b) two electrodes which can be connected to a power source to cause current to flow through the PTC element, said device, when subjected to SEM scanning (as hereinafter defined), showing a maximum difference in voltage between two points separated by 10 microns which is less than 4.2 volts, e.g. less than 4.0 volts, preferably less than 3.0 volts, particularly less than 2.0 volts, especially less than 1.0 volt, subject to the proviso that if each of the electrodes has a substantially planar configura­tion, the maximum difference is less than 3 volts.
  • SEM scanning is used heren to denote the following procedure.
  • the device is insopected to see whether the PTC element has an exposed clean surface which is suitable for scanning in an SEM and which lies between the electrodes. If there is no such surface, then one is created, keeping the alteration of the device to a minimum.
  • the device (or a portion of it if the device is too large, e.g. if it is an elongate heater) is then mounted in a scanning electron microscope so that the electron beam can be traversed from one electrode to the other and directed obliquely at the clean exposed surface.
  • a slowly increasing current is passed through the device, using a DC power source of 200 volts, until the device has been "tripped" and the whole of the potential dropped across it.
  • the electron beam is then traversed across the surface and, using voltage contrast techniques known to those skilled n the art, there is obtained a photomicrograph in which the trace is a measure of the brightness (and hence the potential) of the surface between the electrodes; such a photomicrograph is often known as a line scan.
  • a diagrammatic representation of a typical photomicrograph is shown in Figure 1. It will be seen that the trace has numerous small peaks and valleys and it is believed that these are due mainly or exclusively to surface imperfections. A single “best line” is drawn through the trace (the broken line in Figure 1) in order to average out small variations, and from this "best line", the maximum difference n voltage between two points separated by 10 microns is determined.
  • an electrode having a substantially planar configuration
  • each of the electrodes has a columnar shape.
  • Such a device is shown in isometric vew in Figure 2, in which wire electrodes 2 are embedded in PTC conductive polymer element 1 having a hole through its centre portion.
  • circuit protection devices In a second class of devices, usually circuit protection devices,
  • each of the electrodes has a substantially planar configuration.
  • Meshed planar electrodes can be used, but metal foil electrodes are preferred. If metal foil electrodes are applied to the PTC element before it is irradiated, there is a danger that gases evolved during irradiation will be trapped. It is preferred, therefore, that metal foil electrodes be applied after the radiation cross-linking step.
  • a preferred process comprises the
  • PTC conductive polymers suitable for use in this invention are disclosed in the patents and applications referenced above. Their resistivity at 23°C is preferively less than 1250 ohm.cm, eg. less than 750 ohm.cm, particularly less than 500 ohm.cm, with values less than 50 ohm.cm being preferred for circuit protection devices.
  • the polymeric component should be one which is cross-linked and not significantly degraded by radiation.
  • the polymeric component is preferably free of thermosetting polymers and often consists essentially of one or more crystalline polymers. Suitable polymers include polyolefins, eg.
  • the conductive filler is preferably carbon black.
  • the composition may also contain a non-conductive filler, eg. alumina trihydrate.
  • the composition can, but preferably does not, contain a radiation cross-linking aid. The presence of a cross-linking aid can substan­tially reduce the radiaton dose required to produce a particular degree of cross-linking, but its residue generally has an adverse effect on electrical charac­teristics.
  • Shaping of the conductive polymer will generally be effected by a melt-shaping technique, eg. by melt-­extrusion or molding.
  • the ingredents for the masterbatch were dry blended and then mixed for 12 minutes in a Banbury mixer turning at high gear. The mixture was dumped, cooled, and granulated. The final mix was prepared by dry blending 948.3 g. of Hydral 705 wth 2439.2 g. of the masterbatch, and then mixing the dry blend for 7 minutes in a Banbury mixer turning at high gear. The mixture was dumped, cooled, granulated, and then dried at 70°C and 1 torr for 16 hours.
  • the granulated final mix was melt extruded as a strip 1 cm. wide and 0.25 cm. thick, around three wires. Two of the wires were pre­heated 20 AWG (0.095 cm. diameter) 19/32 stranded nickel-plated copper wires whose centers were 0.76 cm. apart, and the third wire, a 24 AWG (0.064 cm. diameter) solid nickel-plated copper wire, was centered between the other two. Portions 1 cm. long were cut from the extruded product and from each portion the polymeric composition was removed from about half the length, and the whole of the center 24 AWG wire was removed, leaving a hole running through the polymeric element.
  • the products were heat treated in nitrogen at 150°C for 30 minutes and then in air at 110°C for 60 minutes, and were then irradiated.
  • Samples were irradiated to dosages of 20 Mrads, 80 Mrads or 160 Mrads. These samples, when subjected to SEM scanning, were found to have a maximum difference in voltage between two points separated by 10 microns of about 5.2, about 4.0 and about 2.0 respectively.
  • Some of these samples were then sealed inside a metal can, with a polypropylene envelope between the conductive element and the can.
  • the resulting circuit protection devices were tested to determine how many test cycles they would withstand when tested in a circuit consisting essentially of a 240 volt AC power supply, a switch, a fixed resistor and the device.
  • the devices had a resstance of 20-30 ohms at 23°C and the fixed resistor had a resistance of 33 ohms, so that when the power supply was first switched on, the initial current in the circuit was 4-5 amps.
  • Each test cycle consisted of closing the switch, thus tripping the device, and after a period of about 10 seconds, opening the switch and allowing the device to cool for 1 minute before the next test cycle.
  • the resistance of the device at 23°C was measured initially and after every fifth cycle.
  • the Table below shows the number of cycles needed to increase the resistance to 1-1/2 times its original value.

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  • Engineering & Computer Science (AREA)
  • Physics & Mathematics (AREA)
  • Chemical & Material Sciences (AREA)
  • Dispersion Chemistry (AREA)
  • Microelectronics & Electronic Packaging (AREA)
  • Spectroscopy & Molecular Physics (AREA)
  • Ceramic Engineering (AREA)
  • Electromagnetism (AREA)
  • Thermistors And Varistors (AREA)
  • Compositions Of Macromolecular Compounds (AREA)
  • Processes Of Treating Macromolecular Substances (AREA)
  • Conductive Materials (AREA)
EP88117360A 1981-04-02 1982-04-02 Vernetzung von PTC-leitfähigen Polymeren durch Strahlung Expired - Lifetime EP0311142B1 (de)

Priority Applications (1)

Application Number Priority Date Filing Date Title
AT88117360T ATE98807T1 (de) 1981-04-02 1982-04-02 Vernetzung von ptc-leitfaehigen polymeren durch strahlung.

Applications Claiming Priority (4)

Application Number Priority Date Filing Date Title
US25049181A 1981-04-02 1981-04-02
US250491 1981-04-02
US06/254,352 US4426633A (en) 1981-04-15 1981-04-15 Devices containing PTC conductive polymer compositions
US254352 1981-04-15

Related Parent Applications (1)

Application Number Title Priority Date Filing Date
EP82301765.2 Division 1982-04-02

Publications (3)

Publication Number Publication Date
EP0311142A2 true EP0311142A2 (de) 1989-04-12
EP0311142A3 EP0311142A3 (en) 1989-04-26
EP0311142B1 EP0311142B1 (de) 1993-12-15

Family

ID=26940917

Family Applications (2)

Application Number Title Priority Date Filing Date
EP88117360A Expired - Lifetime EP0311142B1 (de) 1981-04-02 1982-04-02 Vernetzung von PTC-leitfähigen Polymeren durch Strahlung
EP82301765A Expired EP0063440B1 (de) 1981-04-02 1982-04-02 Strahlungsvernetzung der PTC-leitfähigen Polymere

Family Applications After (1)

Application Number Title Priority Date Filing Date
EP82301765A Expired EP0063440B1 (de) 1981-04-02 1982-04-02 Strahlungsvernetzung der PTC-leitfähigen Polymere

Country Status (6)

Country Link
EP (2) EP0311142B1 (de)
JP (1) JPH053101A (de)
DE (2) DE3280447T2 (de)
GB (1) GB2096393B (de)
HK (1) HK83689A (de)
SG (1) SG89388G (de)

Cited By (14)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1996029711A1 (en) * 1995-03-22 1996-09-26 Raychem Corporation Electrical device
WO1997006660A2 (en) * 1995-08-15 1997-02-27 Bourns, Multifuse (Hong Kong), Ltd. Surface mount conductive polymer devices and method for manufacturing such devices
EP0780849A2 (de) 1995-12-23 1997-06-25 Abb Research Ltd. Verfahren zur Herstellung eines Materials für PTC-Widerstände
WO1997039461A1 (en) * 1996-04-12 1997-10-23 Littelfuse, Inc. Manufacturing methods for positive temperature coefficient materials
WO1998005503A1 (en) * 1996-08-01 1998-02-12 Raychem Corporation Method of making a laminate comprising a conductive polymer composition
DE102007007617A1 (de) 2007-02-13 2008-08-14 Tesa Ag Intrinsisch erwärmbare heißschmelzklebrige Flächengebilde
EP2148337A1 (de) 2008-07-24 2010-01-27 Tesa AG Flexibles beheiztes Flächenelement
DE102008063849A1 (de) 2008-12-19 2010-06-24 Tesa Se Beheiztes Flächenelement und Verfahren zu seiner Befestigung
EP2224784A1 (de) 2009-02-26 2010-09-01 tesa SE Beheiztes Flächenelement
US7820950B2 (en) 2003-03-10 2010-10-26 Tesa Se Intrinsically heatable pressure-sensitive adhesive planar structures
US10373745B2 (en) 2014-06-12 2019-08-06 LMS Consulting Group Electrically conductive PTC ink with double switching temperatures and applications thereof in flexible double-switching heaters
WO2020016853A1 (en) 2018-07-20 2020-01-23 LMS Consulting Group Thermal substrate with high-resistance magnification and positive temperature coefficient
US10822513B1 (en) 2019-04-26 2020-11-03 1-Material Inc Electrically conductive PTC screen printable ink composition with low inrush current and high NTC onset temperature
US11859094B2 (en) 2016-02-24 2024-01-02 Lms Consulting Group, Llc Thermal substrate with high-resistance magnification and positive temperature coefficient ink

Families Citing this family (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4724417A (en) * 1985-03-14 1988-02-09 Raychem Corporation Electrical devices comprising cross-linked conductive polymers
ATE70363T1 (de) 1986-02-20 1991-12-15 Raychem Corp Einen ionentauschenden stoff verwendende verfahren und gegenstand.
US4924074A (en) * 1987-09-30 1990-05-08 Raychem Corporation Electrical device comprising conductive polymers
US4907340A (en) * 1987-09-30 1990-03-13 Raychem Corporation Electrical device comprising conductive polymers
TW309619B (de) 1995-08-15 1997-07-01 Mourns Multifuse Hong Kong Ltd
US6020808A (en) 1997-09-03 2000-02-01 Bourns Multifuse (Hong Kong) Ltd. Multilayer conductive polymer positive temperature coefficent device
KR20010079908A (ko) 1998-09-25 2001-08-22 추후보정 정의 온도 계수 폴리머 재료 제조 방법
TW200520627A (en) * 2003-10-21 2005-06-16 Tyco Electronics Raychem Kk PTC element and starter circuit for fluorescent lamp
CN102412094B (zh) * 2010-09-20 2014-12-31 胜德国际研发股份有限公司 保护电路

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR2321751A1 (fr) * 1975-08-04 1977-03-18 Raychem Corp Perfectionnement aux compositions a coefficient de temperature positif
FR2368127A1 (fr) * 1976-10-15 1978-05-12 Raychem Corp Compositions a coefficient de temperature positif et dispositifs en comprenant
FR2423037A2 (fr) * 1978-04-14 1979-11-09 Raychem Corp Compositions a coefficient de temperature positif et dispositifs en comprenant
EP0008235A2 (de) * 1978-08-10 1980-02-20 Eaton Corporation Halbleitende Polymermassen, die für die Verwendung in elektrischen Heizvorrichtungen geeignet sind; biegsame Heizleitungen, die unter Verwendung genannter Polymermassen hergestellt sind und Verfahren zur Herstellung solcher Leitungen

Family Cites Families (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3351882A (en) * 1964-10-09 1967-11-07 Polyelectric Corp Plastic resistance elements and methods for making same
JPS5123543A (ja) * 1974-08-22 1976-02-25 Dainippon Printing Co Ltd Dodenseikobunshizairyo

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR2321751A1 (fr) * 1975-08-04 1977-03-18 Raychem Corp Perfectionnement aux compositions a coefficient de temperature positif
FR2368127A1 (fr) * 1976-10-15 1978-05-12 Raychem Corp Compositions a coefficient de temperature positif et dispositifs en comprenant
FR2423037A2 (fr) * 1978-04-14 1979-11-09 Raychem Corp Compositions a coefficient de temperature positif et dispositifs en comprenant
EP0008235A2 (de) * 1978-08-10 1980-02-20 Eaton Corporation Halbleitende Polymermassen, die für die Verwendung in elektrischen Heizvorrichtungen geeignet sind; biegsame Heizleitungen, die unter Verwendung genannter Polymermassen hergestellt sind und Verfahren zur Herstellung solcher Leitungen

Cited By (24)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1996029711A1 (en) * 1995-03-22 1996-09-26 Raychem Corporation Electrical device
US6130597A (en) * 1995-03-22 2000-10-10 Toth; James Method of making an electrical device comprising a conductive polymer
WO1997006660A2 (en) * 1995-08-15 1997-02-27 Bourns, Multifuse (Hong Kong), Ltd. Surface mount conductive polymer devices and method for manufacturing such devices
WO1997006660A3 (en) * 1995-08-15 1997-08-21 Bourns Multifuse Hong Kong Ltd Surface mount conductive polymer devices and method for manufacturing such devices
EP0780849A2 (de) 1995-12-23 1997-06-25 Abb Research Ltd. Verfahren zur Herstellung eines Materials für PTC-Widerstände
DE19548741A1 (de) * 1995-12-23 1997-06-26 Abb Research Ltd Verfahren zur Herstellung eines Materials für PTC-Widerstände
WO1997039461A1 (en) * 1996-04-12 1997-10-23 Littelfuse, Inc. Manufacturing methods for positive temperature coefficient materials
US5814264A (en) * 1996-04-12 1998-09-29 Littelfuse, Inc. Continuous manufacturing methods for positive temperature coefficient materials
WO1998005503A1 (en) * 1996-08-01 1998-02-12 Raychem Corporation Method of making a laminate comprising a conductive polymer composition
CN1090087C (zh) * 1996-08-01 2002-09-04 雷伊化学公司 含导电聚合物组合物的层合板的制造法
US7820950B2 (en) 2003-03-10 2010-10-26 Tesa Se Intrinsically heatable pressure-sensitive adhesive planar structures
DE102007007617A1 (de) 2007-02-13 2008-08-14 Tesa Ag Intrinsisch erwärmbare heißschmelzklebrige Flächengebilde
DE102008034748A1 (de) 2008-07-24 2010-01-28 Tesa Se Flexibles beheiztes Flächenelement
EP2148337A1 (de) 2008-07-24 2010-01-27 Tesa AG Flexibles beheiztes Flächenelement
US9560697B2 (en) 2008-07-24 2017-01-31 Tesa Se Flexible heated planar element
DE102008063849A1 (de) 2008-12-19 2010-06-24 Tesa Se Beheiztes Flächenelement und Verfahren zu seiner Befestigung
US8383997B2 (en) 2008-12-19 2013-02-26 Tesa Se Heated planar element and method for its attachment
EP2224784A1 (de) 2009-02-26 2010-09-01 tesa SE Beheiztes Flächenelement
DE102009010437A1 (de) 2009-02-26 2010-09-02 Tesa Se Beheiztes Flächenelement
US8283612B2 (en) 2009-02-26 2012-10-09 Tesa Se Heated planar element
US10373745B2 (en) 2014-06-12 2019-08-06 LMS Consulting Group Electrically conductive PTC ink with double switching temperatures and applications thereof in flexible double-switching heaters
US11859094B2 (en) 2016-02-24 2024-01-02 Lms Consulting Group, Llc Thermal substrate with high-resistance magnification and positive temperature coefficient ink
WO2020016853A1 (en) 2018-07-20 2020-01-23 LMS Consulting Group Thermal substrate with high-resistance magnification and positive temperature coefficient
US10822513B1 (en) 2019-04-26 2020-11-03 1-Material Inc Electrically conductive PTC screen printable ink composition with low inrush current and high NTC onset temperature

Also Published As

Publication number Publication date
EP0063440B1 (de) 1989-10-04
HK83689A (en) 1989-10-27
DE3279970D1 (en) 1989-11-09
EP0311142A3 (en) 1989-04-26
DE3280447T2 (de) 1994-07-14
DE3280447D1 (de) 1994-01-27
EP0063440A3 (en) 1983-04-13
JPH053101A (ja) 1993-01-08
GB2096393B (en) 1986-01-02
SG89388G (en) 1989-07-14
GB2096393A (en) 1982-10-13
EP0063440A2 (de) 1982-10-27
EP0311142B1 (de) 1993-12-15

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