EP0163004B1 - Elektrische Widerstandszusammensetzung und Verfahren zur Herstellung der Widerstandselemente - Google Patents

Elektrische Widerstandszusammensetzung und Verfahren zur Herstellung der Widerstandselemente Download PDF

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Publication number
EP0163004B1
EP0163004B1 EP85101524A EP85101524A EP0163004B1 EP 0163004 B1 EP0163004 B1 EP 0163004B1 EP 85101524 A EP85101524 A EP 85101524A EP 85101524 A EP85101524 A EP 85101524A EP 0163004 B1 EP0163004 B1 EP 0163004B1
Authority
EP
European Patent Office
Prior art keywords
weight
elements
paste
srru
binder component
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
EP85101524A
Other languages
German (de)
English (en)
French (fr)
Other versions
EP0163004A1 (de
Inventor
Dana L. Dr. Hankey
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.)
WC Heraus GmbH and Co KG
Original Assignee
WC Heraus GmbH and Co KG
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
Application filed by WC Heraus GmbH and Co KG filed Critical WC Heraus GmbH and Co KG
Publication of EP0163004A1 publication Critical patent/EP0163004A1/de
Application granted granted Critical
Publication of EP0163004B1 publication Critical patent/EP0163004B1/de
Expired legal-status Critical Current

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Classifications

    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01C—RESISTORS
    • H01C17/00—Apparatus or processes specially adapted for manufacturing resistors
    • H01C17/06—Apparatus or processes specially adapted for manufacturing resistors adapted for coating resistive material on a base
    • H01C17/065—Apparatus or processes specially adapted for manufacturing resistors adapted for coating resistive material on a base by thick film techniques, e.g. serigraphy
    • H01C17/06506—Precursor compositions therefor, e.g. pastes, inks, glass frits
    • H01C17/06573—Precursor compositions therefor, e.g. pastes, inks, glass frits characterised by the permanent binder
    • H01C17/0658—Precursor compositions therefor, e.g. pastes, inks, glass frits characterised by the permanent binder composed of inorganic material
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01C—RESISTORS
    • H01C17/00—Apparatus or processes specially adapted for manufacturing resistors
    • H01C17/06—Apparatus or processes specially adapted for manufacturing resistors adapted for coating resistive material on a base
    • H01C17/065—Apparatus or processes specially adapted for manufacturing resistors adapted for coating resistive material on a base by thick film techniques, e.g. serigraphy
    • H01C17/06506—Precursor compositions therefor, e.g. pastes, inks, glass frits
    • H01C17/06513—Precursor compositions therefor, e.g. pastes, inks, glass frits characterised by the resistive component
    • H01C17/06533—Precursor compositions therefor, e.g. pastes, inks, glass frits characterised by the resistive component composed of oxides
    • H01C17/0654—Oxides of the platinum group
    • 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
    • Y10T29/49099—Coating resistive material on a base

Definitions

  • the present invention relates to compositions for producing electrical resistance elements and methods for producing the resistance elements.
  • Electrical resistance elements made from certain compositions are particularly useful for creating micro-miniature circuits for the electronics industry, where the electronic elements (or pastes) are screen printed onto substrates.
  • US Pat. No. 3,304,199 describes an electrical resistance element which is composed of a mixture of Ru0 2 or 1r0 2 and lead borosilicate glass.
  • the mixture is combined with a carrier, for example an organic screen printing agent, such as ethyl cellulose dissolved in acetone-toluene.
  • a carrier for example an organic screen printing agent, such as ethyl cellulose dissolved in acetone-toluene.
  • the resulting mixture which contains the carrier, is applied to an electrically non-conductive substrate and then baked in air.
  • US Pat. No. 3,324,049 describes a cermet resistance material which contains 40 to 99% by weight of a lead borosilicate glass, 0.5 to 20% by weight of a noble metal such as Ag, Au, Pd, Pt, Rh, Ir, Os or Ru and 0.5 to 40 wt .-% Mn0 2 or Cu0 contains. The resulting resistance material is then burned in air.
  • U.S. Patent 3,655,440 relates to a resistance composition containing Ru0 2 , lr0 2 or PdO, a glassy lead borosilicate binder and an electrically non-conductive crystal growth control agent, such as A10 3 , which contains submicron small inert particles.
  • a resistance composition containing Ru0 2 , lr0 2 or PdO, a glassy lead borosilicate binder and an electrically non-conductive crystal growth control agent, such as A10 3 , which contains submicron small inert particles.
  • Such a resistance composition is baked in air at 975 to 1025 ° C for 45 minutes to 1 hour.
  • the US Patent 3,682,840 relates to electrical resistance compositions containing lead ruthenate and mixtures thereof with Ru0 2 in conjunction with lead borosilicate binder.
  • U.S. Patent 4,065,743 relates to a glassy enamel resistor containing a glass frit and electrically conductive particles.
  • Such electrically conductive particles contain tin oxide and tantalum oxide.
  • U.S. Patent 4,101,708 is directed to a printable composition of finely divided powder in an inert liquid vehicle for making film resistors that adhere to a dielectric substrate; such compositions contain Ru0 2 , a glass containing Pb0, Nb 2 0 5 , CaF 2 and an inert carrier.
  • German patent 2115814 relates to a resistance paste for baking on ceramics in air.
  • This resistance paste contains BaRu0 3 , SrRu0 3 and CaRu0 3 in a lead borosilicate glass.
  • Resistance compositions were also made using Ag-Pd and / or PdO, Ru0 2 , 1r0 2 and the so-called "du Pont" pyrochlore compounds.
  • the pyrochlore structures are complex oxides of the general formula A 2 B 2 0 6 - 7 , the large cation A being in eightfold coordination and the small cation B being in octahedral coordination. Their success is mainly due to their stability in changeable atmospheres (reducing) and their ability to change their electrical properties through multiple substitution of elements.
  • Examples of pyrochlore compounds specifically used in these compositions and discussed in U.S. Patents 3,553,109, 3,560,410 and 3,583,931 (all of which patents include lead borosilicate binders) contain B! 2 R U2 0 7 and Pb 2 Ru 2 O 7-x, where 0 ⁇ x ⁇ 1.
  • the perovskite crystal structure was described by UM Goldsmith, Skrifter Norske Videnskaps - Akad., Oslo., I: Mat. Naturv. Cl. 2: 8 (1926).
  • the A cation is in twelve-fold coordination with oxygen and the smaller B-cation is in octahedral coordination.
  • the perovskite structure has high lattice energy and is generally a very stable structure.
  • Resistance compositions were applied using the screen printing process, which require baking in an oxidizing atmosphere (air), which necessitates the use of expensive precious metals such as Au, Ag, Pt and Pd.
  • the less expensive copper could not be used because copper oxidizes easily. Accordingly, there is a need for a stable copper compatible resistor composition that could be baked in a non-oxidizing atmosphere such as nitrogen.
  • Typical resistance compositions used previously use lead borosilicate glass binders. After burning in air, decomposes in the resistance compositions, e.g. Strontium ruthenate contained in a lead borosilicate binder, the strontium ruthenate to strontium oxide, which dissolves in the binder, and ruthenium oxide.
  • strontium ruthenate is stoved in a strontium borosilicate binder under nitrogen, there is no decomposition of the electrically conductive component, i.e. the strontium ruthenate remains unchanged.
  • Another object of the present invention is to provide a thick film resistor system which has property reproducibility and reduced processing sensitivity.
  • the present invention relates to a composition for producing an electrical resistance element, which is composed of an electrically conductive component and a binder.
  • the present invention also relates to a method for producing an electrical resistance element by producing the above-described composition, pasting this composition with an organic carrier, applying the paste to a substrate by screen printing and baking.
  • the binder component can also contain 0.1 to 2.5% by weight of Al 2 O 3 .
  • the binder component can also still contain 0.1 to 1.5% by weight of TiO 2 or NaF. If appropriate, the binder component can also contain 5 to 15% by weight of CaO.
  • composition for manufacturing electrical resistance elements contains an electrically conductive metal oxide perovskite component and a glass binder component.
  • B ' 1-y B " y include Ruo, sTio, z and Ru 0.9 Ti 0.1 .
  • Preferred electrically conductive components include SrRu o , 8 , Ti 0.2 O 3, SrRu0 3 and SrRu 0.9 Ti 0.1 O 3 . Combinations of these components can also be used, such as SrRu0 3 + SrRu o , s / Tio, z0 3 or SrRu0 3 + SrRu 0.9 Ti 0.1 O 3 .
  • the conductive components include SrRu 0.95 Cd 0.05 O 3, Sr 0.90 Na 0.10 RuO 3, Sr 0.90 Y 0.10 RuO 3, Sr 0.80 Na 0 , 10 / La 0.10 RuO 3 and SrRu o , 8 Ti o , 2 0 3 SrRu0 3 , SrRuo, s / Zro, 2 0 3 , SrRu 0.9 Zr 0.1 O 3, SrRu 0.75 V 0 , 25 O 3 and SrRu 0.8 CO 0.2 O 3 .
  • substitutions based on ionic radii and valency of A and B are as follows:
  • the main components of the binder component of the present invention are C ', ie Sr0 or Ba0 or Sr0 + BaO, and B 2 0 3 , Si0 2 and Zn0 in the following amounts:
  • binder component can also comprise one or more of the following constituents:
  • Nonlimiting examples of preferred compositions of the binder component include the following:
  • compositions of the binder component include the following:
  • the weight% ratio of binder component / electrically conductive component can vary from 25 to 75% by weight of binder component / 75 to 25% by weight of electrically conductive component, i.e. the binder component can e.g. 30, 35, 40, 50, 60, 65 or 70 wt .-%.
  • the binder component and the electrically conductive component are mixed with a suitable “organic carrier”.
  • An organic vehicle is a medium that volatilizes at a relatively low temperature (approximately 400 to 500 ° C) without causing a reduction in other paste components.
  • An organic carrier serves as a transfer medium for screen printing.
  • An organic vehicle for use in the present invention is preferably a resin, e.g. an acrylic acid ester resin, preferably an isobutyl methacrylate, and a solvent, e.g. an alcohol, preferably tridecyl alcohol ("TDA").
  • TDA tridecyl alcohol
  • the resin can be any polymer that depolymerizes in nitrogen at or below 400 ° C.
  • solvents that can be used are Terpineol or "TE-XANOL" from Eastman Kodak.
  • the solvent for use in the present invention may be any solvent which dissolves the resin in question and which has an appropriate vapor pressure consistent with the subsequent milling and screen printing.
  • the organic carrier consists of 10 to 30% by weight of isobutyl methacrylate and 90 to 70% by weight of TDA.
  • the binder component, the electrically conductive component and the organic carrier are mixed and applied in a screen printing process to the copper connection on a suitable substrate, for example made of 96% Al 2 0 3 , in a screen printing process and then in a nitrogen atmosphere at a temperature of 900 ° C, for example suitable time, e.g. 7 minutes, baked.
  • a suitable substrate for example made of 96% Al 2 0 3
  • suitable time e.g. 7 minutes
  • the binder component (glass matrix) of the present invention prevents decomposition of the electrically conductive component during baking, i.e. the crystal structure (physical) and the chemical composition of the electrically conductive component remain stable and unchanged during baking.
  • the binder is synthesized using analytical grade materials, each in the oxide form except for the strontium, barium and copper compounds which are present as carbonates.
  • the individual components are weighed out and homogenized for 1 hour in a V-mixer (which is a dry mixing process). After mixing is complete, the homogenized powders are placed in a cyanite crucible, in which they are then melted.
  • the binders are preheated at 600 ° C for 1 hour and then transferred to another furnace where they are then melted in a temperature range of 1100 to 1300 ° C for a period of 1 to 1.5 hours. The molten material is removed from the furnace at the melting temperature and poured into a stainless steel tub filled with deionized water.
  • the electrically conductive components are prepared by attaching the appropriate connection (eg SrRu0 3 ), calculating the equimolar amount of eg SrC0 3 and Ru0 2 that have to be weighed to ensure the stoichiometry and ultimately weighing the individual components. Correction factors for the Ru metal content, water content and other volatile components that are lost when annealing at 600 ° C are also included in the calculation. A similar correction factor for the loss on ignition was also included in the calculation for the weights of the other components, if necessary.
  • the Ru0 2 has a surface area of more than 70 m 2 / g, while the other components have a surface area of less than 5 m 2 / g.
  • the weighed starting materials are ground in a ceramic ball mill with aluminum oxide grinding devices for 2 hours together with deionized water, that is to say subjected to a wet grinding process. After 2 hours, the homogenized slurry is poured into stainless steel troughs and dried at 80 ° C for 24 hours. The dried mixture is sieved through an 80 mesh screen before calcination.
  • the sieved powders are calcined in crucibles made of high-purity aluminum oxide (purity 99.8%), this step being carried out precisely with microprocessor control.
  • the heating and cooling rates are not critical per se, they concern general 500 ° C / h
  • the holding times at the relevant temperatures vary between 1 and 2 hours.
  • the powders are ground in a Sweeco vibratory mill for 2 hours. This is a high energy milling process using alumina milling media and isopropyl alcohol.
  • the Peroswkite are sieved wet (200 mesh) at the end of the grinding stage, dried at room temperature in a convection oven (explosion-proof) and prepared for characterization and incorporation in the resistance paste.
  • the electrically conductive components which were produced according to the above-described method, contain the following:
  • Example 3 Combination of binder components of electrically conductive components
  • the binder components made in accordance with Example 1 are combined with electrically conductive components made in Example 2 together with an organic carrier.
  • “ACRYLOID” B67 a resin (an isobutyl methacrylate) from Rohm & Haas, Philadelphia, Pennsylvania, and tridecyl alcohol (“TDA”) in a weight ratio of 30:70 is used as the organic carrier.
  • the relevant binder components, the electrically conductive components and the organic carrier are weighed to produce the desired paste mixture.
  • the solids content (binder + electrically conductive phase) is kept at 70% by weight, based on the total paste weight.
  • the paste is ground in a three-roller mill to a fineness of 10 ⁇ m. Resistance test samples are screen printed with the following printing thicknesses: wet 29 to 32 ⁇ m; fired 10 to 13 ⁇ m.
  • the pastes are then pressed either through a 325 mesh screen with a 0.6 mil emulsion or through a 280 mesh screen with a 0.5 mil emulsion.
  • the moist prints are dried for 5 to 10 minutes at 150 ° C before baking.
  • the stoving profile was dependent on the composition of the binder component, e.g. pastes containing Composition I were baked at 850 ° C, while pastes containing Composition II or III were baked at 900 ° C.
  • the 850 ° C profile length was 58 minutes from 100 ° C to 100 ° C, i.e. from the furnace entrance to the furnace exit.
  • the heating rate was 45 ° C per minute, the cooling rate 60 ° C per minute, and the residence time at the maximum temperature was 10 minutes.
  • the 900 ° C profile had a duration of 55 minutes and 100 ° C to 100 ° C, a heating rate of 50 ° C per minute and a cooling rate of 60 ° C per minute, the residence time at the maximum temperature varied between 5 and 14 minutes .

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  • Engineering & Computer Science (AREA)
  • Manufacturing & Machinery (AREA)
  • Microelectronics & Electronic Packaging (AREA)
  • Chemical & Material Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Non-Adjustable Resistors (AREA)
  • Conductive Materials (AREA)
  • Compositions Of Oxide Ceramics (AREA)
  • Apparatuses And Processes For Manufacturing Resistors (AREA)
EP85101524A 1984-05-30 1985-02-13 Elektrische Widerstandszusammensetzung und Verfahren zur Herstellung der Widerstandselemente Expired EP0163004B1 (de)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
US06/615,204 US4536328A (en) 1984-05-30 1984-05-30 Electrical resistance compositions and methods of making the same
US615204 1984-05-30

Publications (2)

Publication Number Publication Date
EP0163004A1 EP0163004A1 (de) 1985-12-04
EP0163004B1 true EP0163004B1 (de) 1988-01-07

Family

ID=24464435

Family Applications (1)

Application Number Title Priority Date Filing Date
EP85101524A Expired EP0163004B1 (de) 1984-05-30 1985-02-13 Elektrische Widerstandszusammensetzung und Verfahren zur Herstellung der Widerstandselemente

Country Status (5)

Country Link
US (1) US4536328A (ja)
EP (1) EP0163004B1 (ja)
JP (1) JPH0620001B2 (ja)
CA (1) CA1243196A (ja)
DE (1) DE3561369D1 (ja)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2003073442A1 (fr) * 2002-02-28 2003-09-04 Kojima Chemical Co., Ltd. Resisteur

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JP3579836B2 (ja) * 2002-02-28 2004-10-20 小島化学薬品株式会社 固定抵抗器
JP3630144B2 (ja) * 2002-02-28 2005-03-16 小島化学薬品株式会社 抵抗器
JP2004192853A (ja) * 2002-12-09 2004-07-08 National Institute Of Advanced Industrial & Technology 酸化物導電性ペースト
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Publication number Priority date Publication date Assignee Title
WO2003073442A1 (fr) * 2002-02-28 2003-09-04 Kojima Chemical Co., Ltd. Resisteur

Also Published As

Publication number Publication date
CA1243196A (en) 1988-10-18
US4536328A (en) 1985-08-20
JPS60262401A (ja) 1985-12-25
JPH0620001B2 (ja) 1994-03-16
DE3561369D1 (en) 1988-02-11
EP0163004A1 (de) 1985-12-04

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