CN1182941A - Conducting composition used as end electrode of sheet resistance - Google Patents

Conducting composition used as end electrode of sheet resistance Download PDF

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Publication number
CN1182941A
CN1182941A CN97115541A CN97115541A CN1182941A CN 1182941 A CN1182941 A CN 1182941A CN 97115541 A CN97115541 A CN 97115541A CN 97115541 A CN97115541 A CN 97115541A CN 1182941 A CN1182941 A CN 1182941A
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CN
China
Prior art keywords
composition
paste
conductor
scolder
oxide
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Granted
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CN97115541A
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Chinese (zh)
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CN1090368C (en
Inventor
稻叶明
柴田浩
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EIDP Inc
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EI Du Pont de Nemours and Co
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Publication of CN1182941A publication Critical patent/CN1182941A/en
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    • 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
    • H01B1/22—Conductive material dispersed in non-conductive organic material the conductive material comprising metals or alloys
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
    • H01G4/00—Fixed capacitors; Processes of their manufacture
    • H01G4/002—Details
    • H01G4/228—Terminals
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
    • C09D5/24—Electrically-conducting paints
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01C—RESISTORS
    • H01C1/00—Details
    • H01C1/14—Terminals or tapping points or electrodes specially adapted for resistors; Arrangements of terminals or tapping points or electrodes on resistors
    • H01C1/142—Terminals or tapping points or electrodes specially adapted for resistors; Arrangements of terminals or tapping points or electrodes on resistors the terminals or tapping points being coated on the resistive element
    • H—ELECTRICITY
    • H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
    • H05K1/00—Printed circuits
    • H05K1/02—Details
    • H05K1/09—Use of materials for the conductive, e.g. metallic pattern
    • H05K1/092—Dispersed materials, e.g. conductive pastes or inks

Abstract

The invention relates to conductive paste which consists of a plurality of conductive components which are dispersed in organic adhesive and inorganic adhesive. The paste can be used for end electrode material of a chip element. The invention in particular relates to the conductive paste. Even when precious metals are used as conductor composition, the paste is still provided with good solder leaching resistance during the process of assembling the chip element into a circuit substrate. And the invention is highly applicable to electrodes of plate-type resistors.

Description

Be used as the conducting composition of end electrode of sheet resistance
The present invention relates to conducting paste, be made up of the multiple conductive compositions and the inorganic bond that are scattered in the organic bond, this thickener can be used for the termination electrode material of chip component.The invention particularly relates to conductive paste, even when noble metal is used as the conductor composition, this thickener still has good anti-scolder leaching in the process that chip component is assembled to circuitry substrate, and highly is applicable to the chip resistor electrode.
Along with electronic circuit trends towards more highdensity assembling, the assembling of chip component is widely used in the several years in the past, the method of taking this can be with many miniature circuit elements (claiming " chip component " here), and promptly chip resistor and chip capacitor are assembled on the circuitry substrate simultaneously.
The output terminal electrode that is used to be assemblied on the circuitry substrate must be installed in these chip components.
The Main Ingredients and Appearance that always extensively is used as the thick film conductor paste composition of termination electrode material so far comprises conductive component, adhesive and organic carrier.Precious metal palladium (Pd), fine-powder or its mixture or its alloy or palladium oxide and silver oxide or its mixture of platinum (Pt) and silver (Ag) are widely used in the conductor composition.Glass glue is used as adhesive, and inert organic liquid is used as organic carrier.Have the paste component of d spiss and rheological characteristic can be by with the conductor component, glass glue and and the inertia organic carrier mix, utilize the method for mechanical mixture to make its dispersion then and make.
Such as this type of chip component is connected on the circuitry substrate picture on surface is to utilize the method for welding to finish, and promptly the chip component terminal is welded in fusion welding in the circuitous pattern of copper-clad laminated printed circuit boards on the relevant position securely.
Therefore, this conduction paste composition not only should have bonding strength and conductivity after forming termination electrode, and should have solderability.The solderability of this termination electrode refers to be assembled to chip component on the circuitry substrate or in the maintenance process, good solder wettable that the termination electrode soldering is required and anti-scolder leaching.
The inventor has studied above-mentioned prior art, draws the conclusion that it has following problem.
Money base conductor composition has good practicality as the conduction composition, conduction composition in the conduction paste composition is as the termination electrode material of chip component, and money base conductor composition has lower connection resistance and good solder wettable, and can oxidized sintering.But when termination electrode is that the problem of appearance is the anti-scolder leaching that produces difference under the situation about forming with the conducting composition that contains money base conductor composition.In addition, when with RuO 2Or pyrochlore is the plate resistor termination electrode on basis when forming, and can produce such as other problemses such as resistance shakinesses after electrode generates.
Above-mentioned first problem is a kind of like this phenomenon, be when directly on electrode, carrying out promptly when conducting composition in the prior art is used to chip component termination electrode and welding, silver as the main conductor composition in the termination electrode spreads (being called as the scolder leaching) in scolder, and then spreads in conductor as the tin of a kind of composition of scolder.When the scolder of electrode is leached in when taking place in the element assembling process, this causes because the caused reliability of bad connection weakens.When the scolder of electrode is leached in when taking place in the maintenance, in fact scolder does not soak electrode, and this makes element not assemble.The diffusion of tin in electrode destroyed electrode and the chip adhesion at the contact-making surface place.The method of avoiding this problem is to utilize silver-palldium alloy to do electrode conductor to diffuse in the scolder to prevent silver.Yet even in this case, when solder temperature was higher, the scolder leaching was still and can not be avoided, and this also depends on the scolder kind.So service condition is very limited.
Second problem is, in chip resistor and analog production process thereof, when end electrode of sheet resistance generated by utilizing the conducting composition sintering, phase counterdiffusion and thermal stress produced between resistor and termination electrode, and this causes fluctuating widely of resistor resistance.
One of the object of the invention is to provide the conduction paste composition, even if this component is under the situation of using money base conductor composition, still have suitable conductance and bond strength, the good equilibrium that keeps whole performance simultaneously, therefore this can form the termination electrode of chip resistor comprising solder wettable and anti-scolder leaching.
Another object of the present invention is to provide the conducting composition of end electrode of sheet resistance, this composition comprises the inorganic conductive filler, metal oxide and/or the pyrochlore and/or the boride of diffusion did not take place in scolder in the welding stage, reach the unorganic glass adhesive that electroplate liquid is had good drag, and constitute by a kind of conductor composition of money base.
Above-mentioned and other purpose of the present invention and notable feature thereof are conspicuous from the description of this specification and appended accompanying drawing.
Fig. 1 illustrates and is printing being used for conducting composition, behind drying and the burning conducting composition, because the measuring circuit that the conductivity that the scolder leaching is caused is assessed.Among Fig. 1: 1. are alumina substrates; 2. be the printing and the sintering figure of conduction paste composition; With 3. are resistance measurement device (4 terminal methods).
The object of the invention is to address the above problem.The present invention is a kind of conducting composition with end electrode of sheet resistance, comprises the metal dust as the conductor composition in the conducting composition of this end electrode of sheet resistance, inorganic bond and carrier; The mixture of powders that comprises silver powder, palladium powder, silver-palladium alloy powder or above-mentioned at least two kinds of metals as the metal dust of conductive compositions; Inorganic bond comprises glass glue, and the conduction inorganic filler comprises binary oxide and/or pyrochlore and/or is selected from metal boride in pincers, iridium, rhodium, ruthenium, the tin.
In conductor paste composition of the present invention, promptly convenient silver base conductive composition forms the back by the scolder leaching at termination electrode, has at least a kind of conduction inorganic filler to remain in the thick film conductor to form termination electrode in binary metal oxide, pyrochlore and the boride.Sufficient conductivity and bond strength have consequently been kept.This has been avoided being reduced and can't being assembled by the chip component that the solder wettable variation causes by the lost efficacy stability cause of the connection due to the scolder leaching in addition.
Among the present invention, will have less connection resistance, good solder wettable and material such as silver that can oxidation and sinter, pyrochlore and composition thereof and alloy thereof are feasible as conductive powder.The mixture of above-mentioned material and other noble metal powders also can be used.The form that these metal or alloy are used is a fine-powder.Although the particle optimum grain-diameter is in about 0.1-5 micrometer range, the metal powder granulates size is unimportant, as long as adapt with painting method.
About the glass glue that uses in the present invention, the composition of glass itself is not vital, does not anyly react mutually with above-mentioned conductor and all can use with any material of firing assistant metal particles sintering in the step, forming the conductor phase having enough viscosity and glass flow under the firing temperature.
Therefore, it is possible utilizing far-ranging oxidation glass, and wherein glass contains traditional forming of glass and glass-modified composition.The example of these oxidation glass comprises lead silicate salt such as lead borosilicate and lead silicate itself etc.Preferred frit is Pbo-SiO 2Base frit or Pbo-SiO 2-B 2O 3-Ji frit.The softening temperature of this frit is about 450～600 ℃, and the drag of pair electroplate liquid is arranged.Because to the bad drag of electroplate liquid, such glass does not contain with Bi 2O 3Constitute the glass ingredient of glass.
The granular size of glass glue there is no the value of particular importance.Yet glass particle should be in 0.1～10 micrometer range (preferred 0.5～5 micron), and average grain diameter should be at 2～3 microns.Tiny glass particle less than 0.1 micron has very high surface area, and this needs a large amount of organic solvents to obtain the adequate liquidity as the printing slurry.On the other hand, then be an impediment to printing during greater than 10 microns when particle diameter.
The content of silver accounts for 50～87% (weight) of thickener usually in the composition, and frit content accounts for 3%～10% (weight) of composition greatly in composition, and the conductor inorganic filler content is about base-material thickener 0.1～15% (weight).
In the present invention, above-mentioned conductive powder and glass glue and other inorganic fillers can be scattered in a kind of organic carrier and be prepared to the dispersion that is called as " thickener " that generally has the semifluid softness.
The ratio of inoganic solids depends on the application process of thickener and used organic solvent in organic carrier and the dispersion in thick film paste composition of the present invention, and can change to some extent.
In order to obtain the high-quality coating, dispersion contains 50%-90% (weight) inoganic solids and 10～50% (weight) carrier usually.
Any inert fluid all can be used as carrier.To its adding or do not add thickener and/or the water of stabilizer and/or other common additives or any multiple organic liquid all can be used as carrier.For example the organic liquid that can be used comprises aliphatic alcohol; The various esters of this class alcohol are as ethyl acetate and ethyl propionate; Terpenes such as loose ester and pine tar ester; And such as the resin solution in the monobutyl ether equal solvent of pine tar and ethylene glycol monoacetate, as the polymethacrylates of low mass molecule alcohol class, or ethyl cellosolve.Volatile liquid can be contained in the carrier, so that improve the speed that applies after-hardening on substrate, or carrier itself can constitute thus.
Preferred vector is that those are the carrier of base with ethyl cellosolve and β-terpinol.
Implement pattern of the present invention and described hereinafter, but the present invention is not limited to these embodiment.If there are not other explanations, shown in numeral be the percentage by weight of component.
The glass that is used as inorganic bond in following embodiments of the invention and Comparative Examples is Pbo-SiO 2-B 2O 3-Ji frit.
EXAMPLE Example 1-12
A kind of conductor paste feed composition is by through grinding silver powder (carefully be ground to particle diameter and be not more than 1 μ m), palladium powder, glass powder, ethyl cellulose and terpinol co-production pulp, stirred with blender, pass through milling processing then, each component ratio is listed in the table below.
Table 1
The embodiment of the invention
Component ??1 ??2 ??3 ??4 ??5 ??6 ??7 ??8 ??9 ??10 ??11 ??12
Silver powder ??68 ??68 ??68 ??68 ??68 ??68 ??68 ??68 ??56 ??56 ??65 ??63
The palladium powder ??0.5 ??0.5 ??0.5 ??0.5 ??0.5 ??0.5 ??0.5 ??0.5 ??0.5 ??0.5 ??0.5 ??0.5
Glass powder ??10 ??8 ??6 ??10 ??8 ??6.7 ??8.3 ??8 ??10 ??10 ??10 ??10
Inorganic filler ruthenium-oxide bismuth pyrochlore nickel borides (Ni 3B) lanthanum boride (LaB 6) tin oxide (SnO 2) ??3.5 ??3.5 ??3.5 ??1.5 ??1.5 ??2.18 ??2.82 ??0.75 ??1.75 ??10 ??10 ??2.0 ??2.0
The resin ethyl cellulose ??2 ??2 ??2 ??2 ??2 ??2 ??2 ??2 ??2 ??2 ??2 ??2
The organic solvent terpinol ??16 ??18 ??20 ??18 ??20 ??20.6 ??2 ??18.38 ??19 ??21.5 ??21.5 ??20.5 ??20.5
Comparative Examples
Conducting paste composition among the Comparative Examples 1-3 by following component use with embodiment 1 in same procedure form fully.
Table 2
Comparative Examples
????1 ????2 ???3
Silver powder ????68 ????71.5 ???68
The palladium powder ????2 ????0.5 ???2
Glass powder ????5 ????3 ???5
Resin (ethyl cellulose) ????2 ????2 ???2
Organic solvent (terpinol) ????23 ????23 ???23
In the conductor paste feed composition of these embodiment and Comparative Examples, to since the assessment (exist/do not exist and be electrically connected inefficacy) of the conductivity that the scolder leaching of when welding causes carry out as follows.
Then, conductor paste feed composition in Application Example and Comparative Examples uses 96% aluminium substrate printing by pattern shown in Figure 12, way is shown in Fig. 1 measuring circuit, printing in order to assessment conductor paste composition, dry and fire relation between back scolder leaching and the conductivity, after this under 150 ℃ of conditions dry 10 minutes, to form 20～24 microns thick film, temperature with 850 ℃ was fired under oxidation environment 10 minutes in the common electric band oven then, like this, total firing time is about 30 minutes.
When being dipped into temperature after so firing, the conductor paste feed composition in Application Example and the Comparative Examples remains on low its molten solder (Sn: Pb=63.37) reach 5 seconds of 280 ℃ of fusions, 10 seconds, when 15 seconds and 20 seconds, utilize four terminal measuring resistance methods commonly used to measure the resistance of the thick film conductor that on substrate, forms.Measurement is undertaken by mode shown in Figure 1, promptly uses a kind of resistance apparatus (as an Advantest R6871 digimer), and it is electrically connected with the thick film conductor figure 2 that forms on substrate.It the results are shown in the following table 3.Can find out obviously that from table 3 conductor paste feed composition of the present invention uses money base conductor component and is to contain conduct electricity the thickener of inorganic filler a kind of containing, this composition has suppressed because the electrical connection inefficacy that the scolder leaching causes.In addition, can further think, promptly require (as conductivity, adhesion etc.) to reach the degree that does not cause any practical problem at least the suchlike every other key property characteristic of conductor paste composition.
Table 3
The scolder soak time
5 seconds (Ω) 10 seconds (Ω) 15 seconds (Ω) 20 seconds (Ω)
Embodiment 1 ????1.2 ????1.2 ????1.2 ????1.2
Embodiment 2 ????1.1 ????1.1 ????1.1 ????1.0
Embodiment 3 ????1.0 ????1.0 ????1.0 ????1.0
Embodiment 4 ????1.0 ????1.0 ????1.0 ????1.0
Embodiment 5 ????1.0 ????1.0 ????1.0 ????1.0
Embodiment 6 ????1.0 ????1.0 ????1.0 ????1.0
Embodiment 7 ????1.0 ????1.1 ????1.0 ????1.0
Embodiment 8 ????1.0 ????1.0 ????1.0 ????1.0
Embodiment 9 ????6.8 ????7.0 ????7.1 ????7.6
Embodiment 10 ????1.5 ????1.5 ????1.6 ????1.7
Embodiment 11 ????1.5 ????1.8 ????1.8 ????1.9
Embodiment 12 ????1.8 ????2.0 ????2.1 ????2.3
Comparative Examples 1 ????0.5 Can't measure Can't measure Can't measure
Comparative Examples 2 ????0.5 Can't measure Can't measure Can't measure
Comparative Examples 3 ????0.5 Can't measure Can't measure Can't measure
The obtained main advantageous effects of the present invention gathers as follows.
Contain metal dust as the conductor composition as in addition binary oxide and/or pyrochlore and/or the metal boride that is selected from tin, iridium, rhodium, ruthenium and rhenium being included in as inorganic filler, the conducting paste composition that the end electrode of sheet resistance of inert binder and carrier is used is that convenient conductive compositions still can keep certain electrical connection during by the scolder leaching so. In addition, the electrical conductivity of the conductor paste feed composition that obtains and bond strength also are fully, and its all character comprise solder wettable and anti-scolder leaching, all are in good poised state.

Claims (1)

1, the conducting composition used of a kind of end electrode of sheet resistance, it comprises following fine particle: (a) 50-87% (weight) argent, its alloy or its mixture; (b) 3-10% (weight) inorganic bond is Pbo by composition, SiO 2Do not contain Bi 2O 3B 2O 3The frit that constitutes; And (c) base-material that is selected from tin oxide, yttrium oxide, rhodium oxide, ruthenium-oxide, rheium oxide iridium base and ruthenium base pyrochlore and the boride of 0.1-15% (weight) at least a is stuck with paste, all (a) and (b) and (c) being scattered in a kind of organic media (d).
CN97115541A 1996-06-25 1997-06-25 Conducting composition used as end electrode of sheet resistance Expired - Lifetime CN1090368C (en)

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JP182699/96 1996-06-25
JP18269996 1996-06-25

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CN1182941A true CN1182941A (en) 1998-05-27
CN1090368C CN1090368C (en) 2002-09-04

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Cited By (9)

* Cited by examiner, † Cited by third party
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CN1328348C (en) * 2003-05-12 2007-07-25 贵研铂业股份有限公司 Antiadhesion agent and method of preventing chip adhesion during sintering high temperature silve paste
CN101728002A (en) * 2010-01-15 2010-06-09 贵阳晶华电子材料有限公司 End-blocking slurry for flaky component
CN101826564A (en) * 2010-05-11 2010-09-08 中国乐凯胶片集团公司 Solar cell back surface field aluminum paste
CN101620893B (en) * 2009-05-22 2011-03-09 广东风华高新科技股份有限公司 All-silver electronic paste and preparation method thereof
CN101692410B (en) * 2009-08-21 2011-11-09 广东风华高新科技股份有限公司 Silver paste of MLCC terminal electrode
WO2011153695A1 (en) * 2010-06-09 2011-12-15 海洋王照明科技股份有限公司 Conductive glue mixture, fluorescent screen anode plate and manufacture method thereof
CN101719395B (en) * 2008-10-09 2013-04-24 北京印刷学院 Macromolecular solution dispersing medium with complete combustion and volatilization for dispensing organic powder
CN105139916A (en) * 2015-06-30 2015-12-09 苏州洋杰电子有限公司 Carbon powder doped molybdenum-based thick film resistance paste and preparation method thereof
CN107032623A (en) * 2017-02-20 2017-08-11 江苏瑞德新能源科技有限公司 A kind of lead-free glass powder used for solar batteries and positive silver paste

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KR100351230B1 (en) * 2000-06-09 2002-09-05 대주정밀화학 주식회사 Conductive paste composition for electrodes
JP3736802B2 (en) * 2002-11-25 2006-01-18 Ｔｄｋ株式会社 Conductive composition and ceramic electronic component

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JPS59185801U (en) * 1983-05-26 1984-12-10 アルプス電気株式会社 chip resistance
JPS6290905A (en) * 1985-05-29 1987-04-25 株式会社明電舎 Manufacture of voltage nonlinear resistance element
JP3015621B2 (en) * 1993-05-10 2000-03-06 松下電器産業株式会社 Conductive paste composition

Cited By (13)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1328348C (en) * 2003-05-12 2007-07-25 贵研铂业股份有限公司 Antiadhesion agent and method of preventing chip adhesion during sintering high temperature silve paste
CN101719395B (en) * 2008-10-09 2013-04-24 北京印刷学院 Macromolecular solution dispersing medium with complete combustion and volatilization for dispensing organic powder
CN101620893B (en) * 2009-05-22 2011-03-09 广东风华高新科技股份有限公司 All-silver electronic paste and preparation method thereof
CN101692410B (en) * 2009-08-21 2011-11-09 广东风华高新科技股份有限公司 Silver paste of MLCC terminal electrode
CN101728002A (en) * 2010-01-15 2010-06-09 贵阳晶华电子材料有限公司 End-blocking slurry for flaky component
CN101826564A (en) * 2010-05-11 2010-09-08 中国乐凯胶片集团公司 Solar cell back surface field aluminum paste
CN101826564B (en) * 2010-05-11 2011-10-05 中国乐凯胶片集团公司 Solar cell back surface field aluminum paste
WO2011153695A1 (en) * 2010-06-09 2011-12-15 海洋王照明科技股份有限公司 Conductive glue mixture, fluorescent screen anode plate and manufacture method thereof
CN102906823A (en) * 2010-06-09 2013-01-30 海洋王照明科技股份有限公司 Conductive glue mixture, fluorescent screen anode plate and manufacture method thereof
CN102906823B (en) * 2010-06-09 2014-04-02 海洋王照明科技股份有限公司 Conductive glue mixture, fluorescent screen anode plate and manufacture method thereof
CN105139916A (en) * 2015-06-30 2015-12-09 苏州洋杰电子有限公司 Carbon powder doped molybdenum-based thick film resistance paste and preparation method thereof
CN105139916B (en) * 2015-06-30 2017-01-04 苏州洋杰电子有限公司 Carbon dust doping molybdenio thick-film resistor paste and preparation method thereof
CN107032623A (en) * 2017-02-20 2017-08-11 江苏瑞德新能源科技有限公司 A kind of lead-free glass powder used for solar batteries and positive silver paste

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Publication number Publication date
TW533433B (en) 2003-05-21
CN1090368C (en) 2002-09-04
KR100268699B1 (en) 2000-11-01
KR980007893A (en) 1998-03-30
SG63719A1 (en) 1999-03-30

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