US3207706A - Resistor compositions - Google Patents

Resistor compositions Download PDF

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Publication number
US3207706A
US3207706A US225121A US22512162A US3207706A US 3207706 A US3207706 A US 3207706A US 225121 A US225121 A US 225121A US 22512162 A US22512162 A US 22512162A US 3207706 A US3207706 A US 3207706A
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United States
Prior art keywords
resistor
palladium
less
silver
compositions
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Expired - Lifetime
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US225121A
Inventor
Hoffman Lewis Charles
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EI du Pont de Nemours and Co
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EI du Pont de Nemours and Co
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Application filed by EI du Pont de Nemours and Co filed Critical EI du Pont de Nemours and Co
Priority to US225121A priority Critical patent/US3207706A/en
Priority claimed from FR948068A external-priority patent/FR1370296A/en
Application granted granted Critical
Publication of US3207706A publication Critical patent/US3207706A/en
Anticipated expiration legal-status Critical
Application status is Expired - Lifetime legal-status Critical

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Classifications

    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C32/00Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides whether added as such or formed in situ
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL COMPOSITION OF GLASSES, GLAZES, OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C3/00Glass compositions
    • C03C3/04Glass compositions containing silica
    • C03C3/062Glass compositions containing silica with less than 40% silica by weight
    • C03C3/064Glass compositions containing silica with less than 40% silica by weight containing boron
    • C03C3/066Glass compositions containing silica with less than 40% silica by weight containing boron containing zinc
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL COMPOSITION OF GLASSES, GLAZES, OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C3/00Glass compositions
    • C03C3/04Glass compositions containing silica
    • C03C3/062Glass compositions containing silica with less than 40% silica by weight
    • C03C3/07Glass compositions containing silica with less than 40% silica by weight containing lead
    • C03C3/072Glass compositions containing silica with less than 40% silica by weight containing lead containing boron
    • C03C3/074Glass compositions containing silica with less than 40% silica by weight containing lead containing boron containing zinc
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL COMPOSITION OF GLASSES, GLAZES, OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C8/00Enamels; Glazes; Fusion seal compositions being frit compositions having non-frit additions
    • C03C8/14Glass frit mixtures having non-frit additions, e.g. opacifiers, colorants, mill-additions
    • C03C8/18Glass frit mixtures having non-frit additions, e.g. opacifiers, colorants, mill-additions containing free metals
    • HELECTRICITY
    • H01BASIC ELECTRIC ELEMENTS
    • H01CRESISTORS
    • H01C17/00Apparatus or processes specially adapted for manufacturing resistors
    • H01C17/06Apparatus or processes specially adapted for manufacturing resistors adapted for coating resistive material on a base
    • H01C17/065Apparatus or processes specially adapted for manufacturing resistors adapted for coating resistive material on a base by thick film techniques, e.g. serigraphy
    • H01C17/06506Precursor compositions therefor, e.g. pastes, inks, glass frits
    • H01C17/06513Precursor compositions therefor, e.g. pastes, inks, glass frits characterised by the resistive component
    • HELECTRICITY
    • H01BASIC ELECTRIC ELEMENTS
    • H01CRESISTORS
    • H01C17/00Apparatus or processes specially adapted for manufacturing resistors
    • H01C17/06Apparatus or processes specially adapted for manufacturing resistors adapted for coating resistive material on a base
    • H01C17/065Apparatus or processes specially adapted for manufacturing resistors adapted for coating resistive material on a base by thick film techniques, e.g. serigraphy
    • H01C17/06506Precursor compositions therefor, e.g. pastes, inks, glass frits
    • H01C17/06513Precursor compositions therefor, e.g. pastes, inks, glass frits characterised by the resistive component
    • H01C17/06533Precursor compositions therefor, e.g. pastes, inks, glass frits characterised by the resistive component composed of oxides
    • H01C17/06546Oxides of zinc or cadmium
    • HELECTRICITY
    • H01BASIC ELECTRIC ELEMENTS
    • H01CRESISTORS
    • H01C17/00Apparatus or processes specially adapted for manufacturing resistors
    • H01C17/06Apparatus or processes specially adapted for manufacturing resistors adapted for coating resistive material on a base
    • H01C17/065Apparatus or processes specially adapted for manufacturing resistors adapted for coating resistive material on a base by thick film techniques, e.g. serigraphy
    • H01C17/06506Precursor compositions therefor, e.g. pastes, inks, glass frits
    • H01C17/06573Precursor compositions therefor, e.g. pastes, inks, glass frits characterised by the permanent binder
    • H01C17/0658Precursor compositions therefor, e.g. pastes, inks, glass frits characterised by the permanent binder composed of inorganic material
    • HELECTRICITY
    • H01BASIC ELECTRIC ELEMENTS
    • H01CRESISTORS
    • H01C7/00Non-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

Description

United States Patent M 3,207,706 RESISTOR COMPOSITIONS Lewis Charles Hofiman, Wyclifie, Wilmington, Del., assignor to E. I. du Pont de Nemours and Company, Wilmington, Del., a corporation of Delaware No Drawing. Filed Sept. 20, 1962, Ser. No. 225,121 3 Claims. (Cl. 252-514) This invention relates to electrical resistors; and more particularly, it relates to new and improved resistor compositions.

Precious metal resistor compositions containing a vitreous enamel binder have recently become highly desirable for use in the production of fired electrical resistors. Such resistor compositions and resistors prepared therefrom are, for example, shown in DAndrea US. Patent No. 2,924,540 and Dumesnil US. Patent 3,052,573.

Electrical resistors made with these and other prior art compositions have had an undesirably high temperature coefiicient of resistance and an objectionable high percentage of drift.

Temperature coefiicient of resistance, (TCR), generally expressed in parts per million per degree centigrade, is an important characteristic of resistors since changes in temperature will create relatively large changes in resistance when the TCR is high. TCR is generally measured by measuring (1) Resistance at room temperature (2) Resistance at -75 C. (3) Resistance at 105 C.

great care being taken to achieve thermal equilibrium at each temperature. The change in resistance is expressed as a function of the room temperature resistance, divided by the temperature increment to give the coefiicient.

Drift is referred to as an irreversible change of resistance upon heating. This effect may be noticeable at temperatures as low as 100 C. This was a severe limitation on the aforementioned prior art resistor-s. One Way of testing for this effect is to measure the resistance of a soldered, completed resistor and place it in an oven, at atmospheric conditions, at 150 C. for 16 hours. After this high temperature exposure, the resistance is remeasured and the change expressed as a percentage of the original value. The prior art compositions averaged about 5% under these test conditions.

It is an object of this invention to produce resistor compositions composed of finely divided silver and palladium and finely divided glass frit which when incorporated in a fired resistor will have a reduced TCR and lower percentage of drift.

Other objects will appear hereinafter.

These objects may be accomplished by mixing together 35 to 85 weight percent of a finely divided frit of a specific composition with to 65 weight percent of finely divided palladium and finely divided silver in a weight ratio of Pd:Ag of 3:2 to 2:3.

The finely divided dry mixture may be made into a paste or liquid by the addition of a vehicle in a known manner. Fifteen percent to sixty percent by weight of an inert liquid, for example, Water, methyl, ethyl, propyl, butyl or higher alcohols, the corresponding esters such as acetates, propionates, the terpenes and liquid resins such as pine oil or alpha or beta terpineol and the like may be used to prepare a suitable consistency for application purposes. The vehicles may contain or be composed of volatile liquids to promote fast setting after application, or they may contain waxes, thermoplastic resins, or wax-like materials which are thermofiuid by nature whereby the composition may be applied to a 3,207,706 Patented Sept. 21, 1965 ceramic insulator while at elevated temperature to set upon contact with a cold ceramic base.

The essential combination of the present invention is the specific composition of the glass frit together with a ratio of Pd:Ag of 3:2 to 2:3. The glass frit must have a linear thermal expansion between about 3% and 7% lower than the linear expansion of the substrate on which it is fired to produce the resistor. It is common to fabricate resistor substrates, or bases, from ceramic bodies having a thermal expansion of around 10 C. Such bodies are usually composed of about 94 to 99% A1 0 Temperature coefficients of resistance of less than about 200 ppm./ C. may be obtained on such ceramic bodies with a frit having a thermal expansion of about 73 to 77 lO-"". Other ceramic bodies, e.g., steatite, titanates, mullite, glass and zircon porcelains may, however, be used as substrates for resistors of this invention.

The glass frit for use in accordance With this invention should contain, in weight percent, 2434% ZnO, 18-25% SiO 22-30% B 0 3-7% A1 0 4-10% Na O, 4 6% ZrO 0-4% CaO, 0-4% P 0 less than 1% each, or less than 2% total amount, of PbO, Sb O' TiO NiO or Fe O and less than 0.1% of other alkali metal oxides. The above percentages of the constituents are essential to obtain the low TCR and drift in resistors produced from the resistor compositions of this invention.The easily reducible oxides, PbO, Sb O TiO NiO and Fe O must either be entirely absent or in very small amounts, as indicated, since these can react with the silver and palladium metal powders and give rise to unstable alloy phases or semi-conducting oxides with deleterious effect. The presence of A1 0 in the compositions is essential for low drift and the minimizing of time consuming elastic recovery processes in the glass enamel. Zr0 is essential in my compositions for low voltage coefiicient and the prevention of dissolution of sodium ions in resistor surface moisture films with resulting ionic surface conductivity.

The following table discloses eight examples of frit compositions suitable for use in producing the low TCR and drift resistors of this invention.

TABLE I Frit compositions, weight percent The frit is prepared in the conventional manner by melting the constituents of the examples at about 1200 C. in a fire clay crucible for just sufficient time to dissolve all the constituents. It is then quenched in water and ball milled to a particle size of 0.1 to 50 microns and then dewatered and dried.

The resistor compositions are prepared by mixing with about 35-85% of the frit 65% to 15% of a mixture of finely divided silver and palladium in which the silver and palladium have a weight ratio of 3:2 to 2:3. The silver and palladium may be obtained by chemical precipitation techniques or in any other known manner and may consist of relatively pure silver and palladium or to a large extent of silver oxide or palladium oxide. The

3 silver and palladium or their oxides should have a particle size of 0.1 to 50 microns.

These materials may be dry mixed or they may be mixed with a liquid or pasty vehicle to produce liquid or pasty resistor compositions for easy application to a ceramic base. The most usual manner of forming resistors is to apply a paste form of the resistor composition by a screen stencil operation on a ceramic base and then subject the same to a firing operation to form a glaze resistor film in which the metal particles are imbedded. During the firing operation any silver oxide present is usually reduced to relatively pure silver and palladium or palladium oxide ends in a composition containing palladium and a minor amount of palladium oxide.

The firing of the resistor composition is commonly carried out at a temperature of 750 C. to 780 C. for about minutes.

The fired resistor pattern on the ceramic substrate should be provided with a solderable terminal connection. This may be done by applying a relatively heavy coating of the silver-palladium-frit resistor composition at each end of the fired resistor and refiring at a sufiicient temperature to form a glaze film. Alternatively, a solderable silver composition or a solderable platinum-gold composition can be applied over each end of the fired resistor pattern, and the whole refined at 750 C. to 780 C. If the solderable terminal compositions are applied under the resistor pattern at the ends thereof, only one firing operation will be necessary.

The new resistor compositions of this invention as illustrated in the above examples when tested for drift and TCR gave the following average results as compared to average results of these characteristics of prior art compositions as illustrated in the aforementioned DAndrea and Dumesnil patents.

Throughout the specification and claims, any reference to parts, proportions and percentages refers to parts, proportions and percentages by weight unless otherwise specified.

Since it is obvious that many changes and modifications can be made in the above-described details without departing from the nature and spirit of the invention, it is to be understood that the invention is not to be limited to said details except as set forth in the appended claims.

I claim:

1. A resistor composition consisting essentially of 35 to 85 percent of a frit having 2434% ZnO, 18-25% SiO 22-30% B 0 3-7% A1 0 4-10% Na O, 46% ZrO 04% CaO, 04% P 0 less than 1% each and less than 2% total amount of PbO, Sb O TiO NiO and Fe O and less than 0.1% of other alkali metal oxides, and to 15% of silver and a substance of the group consisting of palladium and palladium oxide, in which the ratio of Ag:the Pd content of said substance is between 3:2 and 2:3.

2. A resistor composition consisting essentially of 35 to percent of a frit having 24-34% ZnO, 18-25% SiO 22-30% B 0 3-7% A1 0 4-10% Na O, 46% ZrO 0-4% CaO, O-4% P 0 less than 1% each and less than 2% total amount of PbO, Sb O TiO NiO and F3203 and less than 0.1% of other alkali metal oxides, and 65% to 15 of silver and a substance of the group consisting of palladium and palladium oxide, in which the ratio of Agzthe Pd content of said sustance is between 3:2 and 2:3, in admixture with 15 to 60 percent by weight of the aforesaid composition of an inert vehicle.

3. A glass enamel frit suitable for use in a resistor composition consisting essentially of 24-34% ZnO, 18- 25% SiO 22-30% B 0 3-7% A1 0 4l0% Na O, 46% ZrO 0-4% CaO, 04% P 0 less than 1% each andless than 2% total amount of PbO, Sb O TiO NiO and Fe O and less than 0.1% of other alkali metal oxides.

References Cited by the Examiner UNITED STATES PATENTS 2,688,560 9/54 Armistead 106--54 XR 2.726,965 12/55 Cressman et al. 106-48 2,924,540 2/60 DAndrea 252514 XR 3,052,573 9/62 Dumesnil 252520 XR JULIUS GREENWALD, Primary Examiner.

Claims (1)

1. A RESISTOR COMPOSITION CONSISTING OF 35 TO 85 PERCENT OF A FRIT HAVING 24-34% ZNO, 18-25% SIO2, 22-30% B2O3, 3-7% AL2O3, 4-10% NA2O, 4-6% ZRO2, 0-4% CAO, 0-4% P2O5, LESS THAN 1% EACH AND LESS THAN 2 TOTAL.AMOUNT OF PBO, SB2O3, TIO2, NIO AND FE2O3 AND LESS THAN 0.1% OF OTHER ALKALI METAL OXIDES, AND 65% TO 15% OF SILVER AND A SUBSTANCE OF THE GROUP CONSISTING OF PALLADIUM AND PALLADIUM OXIDE, IN WHICH THE RATIO OF AG:THE PD CONTENT OF SAID SUBSTANCE IS BETWEEN 3:2 AND 2:3.
US225121A 1962-09-20 1962-09-20 Resistor compositions Expired - Lifetime US3207706A (en)

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Application Number Priority Date Filing Date Title
US225121A US3207706A (en) 1962-09-20 1962-09-20 Resistor compositions

Applications Claiming Priority (5)

Application Number Priority Date Filing Date Title
NL298179D NL298179A (en) 1962-09-20
US225121A US3207706A (en) 1962-09-20 1962-09-20 Resistor compositions
DE19631490160 DE1490160B2 (en) 1962-09-20 1963-09-17 Silver and palladium-containing glaze composition for the production of electric resistances
GB3694263A GB982788A (en) 1962-09-20 1963-09-19 Improvements in and relating to glass enamel frits
FR948068A FR1370296A (en) 1962-09-20 1963-09-19 Electrical resistance

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Cited By (24)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3343985A (en) * 1963-02-12 1967-09-26 Beckman Instruments Inc Cermet electrical resistance material and method of using the same
US3380812A (en) * 1965-08-13 1968-04-30 Hitachi Ltd Sintered palladium materials for electric contact
US3479216A (en) * 1964-11-04 1969-11-18 Beckman Instruments Inc Cermet resistance element
US3497384A (en) * 1967-08-31 1970-02-24 Du Pont Process of metalizing ceramic substrates with noble metals
US3544330A (en) * 1967-04-24 1970-12-01 Du Pont Glasses and capacitor dielectric compositions made therefrom
US3547835A (en) * 1969-06-09 1970-12-15 Du Pont Processes of producing and applying silver compositions,and products therefrom
US3639274A (en) * 1967-09-06 1972-02-01 Allen Bradley Co Electrical resistance composition
US3643756A (en) * 1969-12-16 1972-02-22 Libbey Owens Ford Co Safety circuit control device
US3673092A (en) * 1970-06-05 1972-06-27 Owens Illinois Inc Multilayer dielectric compositions comprising lead-barium borosilicate glass and ceramic powder
US3717837A (en) * 1965-06-04 1973-02-20 Micro Electric Ag Potentiometer
US3808046A (en) * 1971-05-10 1974-04-30 Atomic Energy Authority Uk Metallising pastes
US3854957A (en) * 1973-08-28 1974-12-17 Du Pont Metallizations comprising nickel oxide
US3919441A (en) * 1972-12-20 1975-11-11 Seinosuke Horiki Panel-styled calorific devices and a process for manufacturing the same
US3922387A (en) * 1973-08-28 1975-11-25 Du Pont Metallizations comprising nickel oxide
US4110124A (en) * 1975-09-22 1978-08-29 Engelhard Minerals & Chemicals Corporation Thick film thermocouples
US4359536A (en) * 1981-06-24 1982-11-16 General Electric Company Frit glass composition
US4401767A (en) * 1981-08-03 1983-08-30 Johnson Matthey Inc. Silver-filled glass
US4409292A (en) * 1981-07-09 1983-10-11 Societe Anonyme Dite Compagnie General D'electricite Vitreous material and semiconductor component incorporating same
US4459166A (en) * 1982-03-08 1984-07-10 Johnson Matthey Inc. Method of bonding an electronic device to a ceramic substrate
US4476090A (en) * 1981-09-04 1984-10-09 Degussa Aktiengesellschaft Material for jewelry and commodities and process for its production
US4732802A (en) * 1986-09-26 1988-03-22 Bourns, Inc. Cermet resistive element for variable resistor
US20050104712A1 (en) * 2003-11-13 2005-05-19 Habboosh Samir W. Extended temperature range thermal variable-resistance device
US20060202792A1 (en) * 2003-11-13 2006-09-14 Habboosh Samir W Thermal variable resistance device with protective sheath
US9840663B2 (en) 2014-01-29 2017-12-12 Lg Innotek Co., Ltd Glass composition for photo-conversion member and ceramic photo-conversion member using the same

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
RU2446116C1 (en) * 2010-11-30 2012-03-27 Юлия Алексеевна Щепочкина Enamel coating

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2688560A (en) * 1953-04-27 1954-09-07 Corning Glass Works Eye-protective ophthalmic glass
US2726965A (en) * 1951-11-01 1955-12-13 Gen Electric Ultramarine blue enamel pigment
US2924540A (en) * 1958-05-23 1960-02-09 Du Pont Ceramic composition and article
US3052573A (en) * 1960-03-02 1962-09-04 Du Pont Resistor and resistor composition

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2726965A (en) * 1951-11-01 1955-12-13 Gen Electric Ultramarine blue enamel pigment
US2688560A (en) * 1953-04-27 1954-09-07 Corning Glass Works Eye-protective ophthalmic glass
US2924540A (en) * 1958-05-23 1960-02-09 Du Pont Ceramic composition and article
US3052573A (en) * 1960-03-02 1962-09-04 Du Pont Resistor and resistor composition

Cited By (26)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3343985A (en) * 1963-02-12 1967-09-26 Beckman Instruments Inc Cermet electrical resistance material and method of using the same
US3479216A (en) * 1964-11-04 1969-11-18 Beckman Instruments Inc Cermet resistance element
US3717837A (en) * 1965-06-04 1973-02-20 Micro Electric Ag Potentiometer
US3380812A (en) * 1965-08-13 1968-04-30 Hitachi Ltd Sintered palladium materials for electric contact
US3544330A (en) * 1967-04-24 1970-12-01 Du Pont Glasses and capacitor dielectric compositions made therefrom
US3497384A (en) * 1967-08-31 1970-02-24 Du Pont Process of metalizing ceramic substrates with noble metals
US3639274A (en) * 1967-09-06 1972-02-01 Allen Bradley Co Electrical resistance composition
US3547835A (en) * 1969-06-09 1970-12-15 Du Pont Processes of producing and applying silver compositions,and products therefrom
US3643756A (en) * 1969-12-16 1972-02-22 Libbey Owens Ford Co Safety circuit control device
US3673092A (en) * 1970-06-05 1972-06-27 Owens Illinois Inc Multilayer dielectric compositions comprising lead-barium borosilicate glass and ceramic powder
US3808046A (en) * 1971-05-10 1974-04-30 Atomic Energy Authority Uk Metallising pastes
US3919441A (en) * 1972-12-20 1975-11-11 Seinosuke Horiki Panel-styled calorific devices and a process for manufacturing the same
US3854957A (en) * 1973-08-28 1974-12-17 Du Pont Metallizations comprising nickel oxide
US3922387A (en) * 1973-08-28 1975-11-25 Du Pont Metallizations comprising nickel oxide
US4110124A (en) * 1975-09-22 1978-08-29 Engelhard Minerals & Chemicals Corporation Thick film thermocouples
US4359536A (en) * 1981-06-24 1982-11-16 General Electric Company Frit glass composition
US4409292A (en) * 1981-07-09 1983-10-11 Societe Anonyme Dite Compagnie General D'electricite Vitreous material and semiconductor component incorporating same
US4401767A (en) * 1981-08-03 1983-08-30 Johnson Matthey Inc. Silver-filled glass
US4476090A (en) * 1981-09-04 1984-10-09 Degussa Aktiengesellschaft Material for jewelry and commodities and process for its production
US4459166A (en) * 1982-03-08 1984-07-10 Johnson Matthey Inc. Method of bonding an electronic device to a ceramic substrate
US4732802A (en) * 1986-09-26 1988-03-22 Bourns, Inc. Cermet resistive element for variable resistor
US20050104712A1 (en) * 2003-11-13 2005-05-19 Habboosh Samir W. Extended temperature range thermal variable-resistance device
US7026908B2 (en) * 2003-11-13 2006-04-11 Harco Laboratories, Inc. Extended temperature range thermal variable-resistance device
US20060202792A1 (en) * 2003-11-13 2006-09-14 Habboosh Samir W Thermal variable resistance device with protective sheath
US7915994B2 (en) 2003-11-13 2011-03-29 Harco Laboratories, Inc. Thermal variable resistance device with protective sheath
US9840663B2 (en) 2014-01-29 2017-12-12 Lg Innotek Co., Ltd Glass composition for photo-conversion member and ceramic photo-conversion member using the same

Also Published As

Publication number Publication date
DE1490160B2 (en) 1971-12-02
DE1490160A1 (en) 1969-09-04
GB982788A (en) 1965-02-10
NL298179A (en)

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