WO2018216510A1 - 導体形成用組成物とその製造方法、導体とその製造方法、チップ抵抗器 - Google Patents

導体形成用組成物とその製造方法、導体とその製造方法、チップ抵抗器 Download PDF

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WO2018216510A1
WO2018216510A1 PCT/JP2018/018368 JP2018018368W WO2018216510A1 WO 2018216510 A1 WO2018216510 A1 WO 2018216510A1 JP 2018018368 W JP2018018368 W JP 2018018368W WO 2018216510 A1 WO2018216510 A1 WO 2018216510A1
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Prior art keywords
conductor
particles
mass
forming composition
composition
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PCT/JP2018/018368
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English (en)
French (fr)
Japanese (ja)
Inventor
太田　陽介
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住友金属鉱山株式会社
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Priority to CN201880034587.4A priority Critical patent/CN110692110B/zh
Priority to KR1020197035130A priority patent/KR102569071B1/ko
Publication of WO2018216510A1 publication Critical patent/WO2018216510A1/ja

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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
    • H01B1/14—Conductive material dispersed in non-conductive inorganic material
    • H01B1/16—Conductive material dispersed in non-conductive inorganic material the conductive material comprising metals or alloys
    • 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
    • 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
    • H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B13/00—Apparatus or processes specially adapted for manufacturing conductors or cables
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B5/00—Non-insulated conductors or conductive bodies characterised by their form
    • H01B5/14—Non-insulated conductors or conductive bodies characterised by their form comprising conductive layers or films on insulating-supports
    • 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
    • H01—ELECTRIC ELEMENTS
    • H01C—RESISTORS
    • H01C13/00—Resistors not provided for elsewhere
    • 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
    • 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

Definitions

  • the present invention relates to a conductor-forming composition and a manufacturing method thereof, a conductor and a manufacturing method thereof, and a chip resistor.
  • a chip resistor is composed of a pair of conductors (surface electrode and back electrode) provided on the front and back surfaces of a substrate, a resistor provided between the pair of surface electrodes, and an insulating material covering the resistor.
  • a protective layer and a pair of end surface electrodes provided on the end surface of the substrate and conducting the front surface electrode and the back surface electrode are provided.
  • a plating layer is formed so as to cover these electrodes. The back electrode electrically joins the chip resistor and the circuit board when the chip resistor is mounted on the circuit board.
  • the chip resistor is manufactured by the following method, for example. First, prepare a substrate (slit substrate) with slits in a desired dimension according to the chip size in advance, and print and dry the conductor-forming composition so as to straddle the slit on this substrate, By firing, a plurality of pairs of conductors (surface electrode and back electrode) are formed on the front surface and the back surface of the substrate, respectively. Next, after forming a resistor on the surface of the substrate so that each pair of surface electrodes is arranged at both ends, a glass layer called a precoat is formed on the resistor, and the resistance value is adjusted by trimming Further, for example, a resin layer is formed thereon as a protective layer. Next, the substrate is divided into strips along the slits to form end face electrodes, and the strip-shaped substrate is further divided and plated to obtain a chip-shaped resistor.
  • Conductors are formed into a required shape by, for example, screen-printing or the like on a substrate with a conductive composition in which an electrically conductive powder having high electrical conductivity and glass frit are dispersed in an organic vehicle. It is formed by coating and drying at about 120 ° C. to 250 ° C. and then baking at about 600 ° C. to 900 ° C. Also, in the case where conductors (surface electrode and back electrode) are formed on both sides of a substrate, conventionally, a conductor forming composition is printed on one surface of the substrate, and then dried and baked to conduct the conductor (eg, back electrode). After that, a method of forming a conductor (for example, a surface electrode) by printing, drying and firing in the same manner on the other surface of the substrate is widely used.
  • a conductor for example, a surface electrode
  • the process from drying to baking has been simplified for the purpose of cost reduction and energy saving.
  • the conductor-forming composition is printed on one side of the substrate and dried to form a dry film (eg, back side dry film), and then the other side of the substrate.
  • a method of omitting the firing step once by printing the conductor-forming composition on the surface and drying it to obtain a dry film (for example, a surface dry film) and then simultaneously firing the dry film on both sides of the substrate has been studied. Yes.
  • the dried film is baked in a belt furnace, when the dried film formed on the surface facing the belt touches the belt portion of the belt furnace during firing, the belt and the conductor are joined.
  • MLCC multilayer ceramic capacitor
  • adjacent external electrodes are joined together, or a shelf board made of ceramic or the like on which the multilayer ceramic capacitor is placed,
  • the external electrode may be joined.
  • a conductive paste is applied to a ceramic element, and then an inorganic powder such as alumina powder or zirconia powder is applied.
  • an inorganic powder such as alumina powder or zirconia powder is applied.
  • work which removes these after baking is required and there also existed a problem that a process became complicated.
  • several proposals have been made in order to prevent bonding between the external electrode of the multilayer ceramic capacitor and another member.
  • Patent Document 1 describes that metal powder having various types of particles, for example, two kinds of large and small spherical powders and scale-like metal powders, etc. are used for the conductive paste.
  • Patent Document 2 describes a conductive paste containing metal powder and glass frit, and containing 1 to 10 wt% of a metal additive having a melting point higher than that of the metal powder.
  • the purpose of including the metal powder in these conductive pastes is to suppress the sintering of the metal powder during firing, and to form a gap between the metal components without causing the metal component to be densely contracted. The formation of this gap prevents the glass component that causes bonding from oozing out onto the surface of the conductor layer.
  • Patent Document 3 it is described that an inorganic powder having an average particle size of 0.1 mm or less is used. A method is described in which the inorganic powder is exposed on the surface of the conductor layer to prevent seizure between MLCC chips or a ceramic mortar in which the MLCC chip is installed in the MLCC firing step. Moreover, in patent document 4, in order to control the fluidity
  • JP-A-8-306580 Japanese Patent Laid-Open No. 10-12481 JP-A-9-129480 JP 2001-297628 A
  • an object of the present invention is to provide a conductor-forming composition that does not join in a firing step even if the dry film contacts other members such as a belt of a belt furnace, and a method for producing the same. To do.
  • Patent Documents 1 to 4 have the following problems when forming the conductors of the resistor (front electrode and back electrode). That is, in the conductive paste described in Patent Document 1 and Patent Document 2, a gap is formed between the metal components when the conductor is formed, so that the conductive powder is not sufficiently sintered, and the electrical resistivity of the conductor is low. It cannot be said that it is sufficiently adapted to the electrodes of electronic components such as resistors, which tend to be high and require a low resistance conductor. In addition, these conductive pastes have a problem that the conductor tends to become brittle and the bonding strength between components via the conductor tends to be insufficient.
  • inorganic particles having an average particle diameter of 0.05 mm to 0.2 mm are used in the examples.
  • a conductive paste containing such large particles is used as a chip resistor.
  • an alkali metal oxide is contained in the glass powder.
  • the alkali component is It may easily enter other members and may affect the characteristics of the members.
  • the composition of the glass powder used in the conductive paste it is difficult to obtain adhesion strength to the base material when the conductor layer is formed on the ceramic as described in that it is difficult to wet the ceramic body.
  • a conductor-forming composition comprising a conductive powder, particles other than the conductive powder, a glass frit, and an organic vehicle, wherein 50 in a cumulative distribution on a volume basis of the particles.
  • % Particle size D50 is 1.5 times or more and 4 times or less with respect to the film thickness of the obtained conductor, and the particle content a is 30 parts by mass or less with respect to 100 parts by mass of conductive powder.
  • Formula (1) 80 ⁇ D50 ( ⁇ m) ⁇ a (part by mass)
  • the particle diameter D50 of the particles is 4.5 ⁇ m or more and 24 ⁇ m or less.
  • the particles preferably contain at least one of a metal oxide or a metal nitride.
  • the particles preferably contain at least one of Al and Cu.
  • the particles preferably contain aluminum oxide particles.
  • the conductive powder preferably contains at least one of Au, Ag, Pd and Pt.
  • the organic vehicle contains a binder resin and a solvent, and is preferably contained in an amount of 5 to 120 parts by mass with respect to 100 parts by mass of the conductor-forming composition.
  • the conductor-forming composition preferably further contains a thixotropic agent.
  • the conductive composition is preferably used for at least one of the front electrode and the back electrode of the chip resistor.
  • particles other than the conductive powder are added to the mixture obtained by dispersing the raw material containing the conductive powder, the glass frit, and the organic vehicle using a three-roll mill.
  • the particles have a particle diameter D50 of 1.5 times or more and 4 times or less with respect to the film thickness of the conductor, and the content a of the particles is 100% of the conductive powder.
  • Manufacture of the composition for conductor formation which is 30 mass parts or less with respect to a mass part, and the relationship between the particle diameter D50 of particle
  • a method is provided.
  • a layered conductor comprising a metal, particles other than the metal, and glass formed on the substrate, the particles are formed using the conductor-forming composition. Is provided with a conductor having a particle size of 1.5 times or more and 4 times or less with respect to the thickness of the conductor, and a part of the particles are exposed on the surface of the conductor.
  • the particles preferably have the same composition as that of the substrate.
  • a method for producing a conductor comprising: applying the above-described conductor-forming composition onto a substrate, drying the composition, and then firing the composition at 600 ° C. to 900 ° C. in an acidic atmosphere.
  • the particle has a particle size of 1.5 to 4 times the thickness of the conductor, and a method for producing a conductor is provided in which a part of the particle is exposed from the surface of the conductor.
  • a chip resistor that includes at least a substrate, a conductor, and a resistor, and the conductor is formed using the conductor.
  • the conductor-forming composition of the present invention is difficult to prevent by the conventional technique in the conductor manufacturing process, and the conductor (dry film) is, for example, other members such as a belt of a belt furnace.
  • the phenomenon of joining can be suppressed.
  • the manufacturing method of the composition for conductor formation of this invention can produce the said composition for conductor formation simply.
  • the conductor obtained using the said conductor formation composition is obtained by making it contact with the belt of a belt furnace and baking, the joining of the conductor component to a belt is suppressed.
  • FIG. 1A is a cross-sectional view schematically showing an example of a conductor formed on a substrate portion
  • FIG. 1B is an enlarged cross-sectional view of a part including the conductor.
  • FIG. 2A is a cross-sectional view schematically showing an example of a state in which the substrate portion on which the dry film is formed is placed on the belt of the belt furnace
  • FIG. 2B is a partial view including the dry film.
  • FIG. FIG. 3 is a flowchart showing an example of a method for producing a conductor-forming composition.
  • FIG. 4 is a flowchart showing an example of a conductor manufacturing method.
  • FIG. 5 is a schematic diagram illustrating an example of a chip resistor.
  • FIG. 6 is a graph showing the relationship between the average particle diameter (D50), the particle content a, and the presence or absence of seizure in the belt furnace.
  • the conductor forming composition of the present embodiment includes conductive powder, particles other than the conductive powder, glass frit, and an organic vehicle.
  • the particles can have an average particle size larger than the thickness of the conductor when the conductive powder is sintered to form a layered conductor.
  • FIG. 1, 2 the conductor formed using the composition for conductor formation of this embodiment is demonstrated.
  • FIG. 1A is a schematic diagram showing an example of a conductor of the present embodiment formed on a substrate part.
  • the conductor 10 is formed in layers on one or both surfaces of the substrate unit 20.
  • the conductor 10 is formed by applying a conductor-forming composition to a slit substrate (substrate portion 20), drying, and firing.
  • substrate part 20 means the part which forms one chip
  • the conductor 10 may be formed on one surface (front surface or back surface) of the board
  • FIG. 1 (B) is an enlarged view of a conductor portion surrounded by a broken line in FIG. 1 (A).
  • the conductor 10 includes particles 1 other than the conductive powder (hereinafter also referred to as “particle 1”), and a conductor portion 2 formed by sintering the conductive powder. including.
  • the conductor part 2 contains the metal derived from electroconductive powder, and the glass derived from a glass frit.
  • the component originating in the organic vehicle contained in the composition for conductor formation is removed by the process of drying and baking.
  • the particle 1 has a particle size larger than the thickness of the conductor part 2 (conductor), and a part of the particle 1 is exposed from the surface of the conductor part 2.
  • the particle diameter of the particle 1 is, for example, 1.5 times or more and 4 times or less, preferably 1.5 times or more and 2.5 times or less, and 1.5 times the film thickness of the conductor portion 2. More preferably, it is less than 2 times.
  • the thickness of the conductor part 2 can be measured using a contact-type surface roughness meter.
  • the thickness of the conductor portion 2 can be 1 ⁇ m or more and 10 ⁇ m or less, and is 3 ⁇ m or more and 6 ⁇ m or less. Is preferred.
  • the particle diameter D50 of the particles 1 is, for example, 1 ⁇ m or more and 40 ⁇ m or less, and when the thickness of the conductor portion 2 is 3 ⁇ m or more and 6 ⁇ m or less, it is preferably 4.5 ⁇ m or more and 24 ⁇ m or less.
  • the particle size D50 is in the above range, when the powder is pulverized and dispersed in the production process of the conductor-forming composition, sufficient shear stress of the powder is ensured, and the quality of the stable conductor-forming composition is improved. In the firing, bonding (seizure) of the dry film to other members such as a belt in a belt furnace can be efficiently suppressed.
  • the particle 1 in the conductor-forming composition is preferably 2 ⁇ m or more and 20 ⁇ m or less, preferably 2 ⁇ m or more and 10 ⁇ m or less, from the viewpoint that the particle size D50 further suppresses the dropping of the particles 1 from the conductor 10 after firing. It is more preferable that Further, when the particle diameter D50 of the particles 1 in the conductor-forming composition is within the above range, the particles 1 can be sufficiently prevented from falling off in the step of dividing the chip resistor, as will be described later.
  • the particle diameter D50 of the particle 1 means a particle diameter at the time of 50% accumulation in a volume-based cumulative distribution calculated by a dynamic light scattering method.
  • the particle size of the particle 1 can maintain substantially the same particle size as the particle 1 contained in the composition for conductor formation,
  • the particles 1 having a particle diameter D50 larger than the desired thickness of the conductor portion 2 can be used as a material for the conductor-forming composition.
  • the particle size of the particle 1 in the conductor-forming composition and the conductor 10 maintains substantially the same shape as the particle size of the particle 1 used as the material of the conductor-forming composition as described above, the conductor As the particle diameter D50 of the particles 1 in the forming composition and the conductor 10, the particle diameter D50 of the particles 1 used as the material can be used.
  • the actual particle size of the conductor-forming composition and the particles 1 in the conductor 10 can be confirmed by, for example, observation of a cross-section with a scanning electron microscope (SEM).
  • the particle diameter D50 ( ⁇ m) of the particles 1 and the content a (parts by mass) of the particles 1 with respect to 100 parts by mass of the conductive powder satisfy the relationship of the following formula (1).
  • the bonding (seizure) of the dry film to other members such as a belt in a belt furnace can be efficiently suppressed during firing.
  • the content a (parts by mass) of the particles 1 satisfies the above formula (1) and is preferably 30 parts by mass or less, and 20 parts by mass or less with respect to 100 parts by mass of the conductive powder. More preferably, the amount is 15 parts by mass or less. If the content of the particles 1 satisfies the above formula (1), the bonding (seizure) of the dry film to other members can be suppressed, but if the upper limit of the content is within the above range, the conductor Since the content of the particles 1 in the forming composition can be reduced and the content of the conductive powder can be increased, good conductivity can be maintained.
  • the particles 1 may be particles that are not sintered when the conductor-forming composition is fired at a temperature at which the conductive powder can be sintered. That is, as the particles 1, particles that have a higher sintering start temperature than the conductive powder and do not melt in the range of 120 ° C. or more and 900 ° C. or less can be used.
  • the melting point of the particles 1 is preferably 1400 ° C. or higher and 4300 ° C. or lower, for example.
  • the particle 1 for example, a particle including at least one of a metal oxide, a metal carbide, and a metal nitride can be used, and a particle including at least one of Al, Si, Zr, and Cu can be used.
  • the particles 1 may be ceramic particles such as aluminum nitride powder, alumina powder, silicon carbide powder, silicon nitride powder, zirconia powder, and preferably alumina powder (aluminum oxide particles) is used. it can.
  • Use of alumina powder as the particles 1 is industrially preferable because it is inexpensive and exhibits the same effect as other particles.
  • the particles 1 insulating particles can be used, and powder made of the same material as the substrate can be used.
  • the metal oxide particles 1 are preferably alumina particles.
  • the conductor 10 using alumina powder as the particles 1 is particularly suitable for a back electrode formed on an alumina substrate when manufacturing a square chip resistor.
  • FIG. 2 (A) is a schematic view showing a state in which the substrate portion on which the dry film is formed is placed on the belt of the belt furnace.
  • FIG. 2B is an enlarged view of the portion of the dry film surrounded by the broken line in FIG. 2A, and is an enlarged view of the portion of the dry film 11 that contacts the belt after firing. .
  • the dried film 11 formed using the conductor-forming composition of the present embodiment is baked in a belt furnace, the particles 1 exposed on the surface of the conductor portion 2 are in contact with the belt.
  • the contact area between the dry film 11 and the belt 30 can be reduced, and the bonding (seizure) between the conductor portion 2 in the dry film 11 and the belt or other member in the belt furnace can be suppressed.
  • the dry film 11 may be baked in a place other than the belt furnace. In that case, the contact portion between the member on which the slit substrate on which the dry film 11 is formed and the dry film 11 is bonded (seizure). Can be prevented.
  • the conductive powder is not particularly limited, and those generally used for a conductor-forming composition can be used.
  • the conductive powder can include, for example, at least one of Au, Ag, Pd, and Pt. Further, the conductive powder can be contained in an amount of 40% by mass to 90% by mass with respect to the conductor-forming composition.
  • the glass frit used for the conductive composition of the present embodiment is not particularly limited, and a glass frit generally used for a conductor-forming composition is used.
  • a glass frit lead-free and substantially alkali metal such as borosilicate glass (SiO 2 —B 2 O 3 system) having an average particle diameter of 0.5 ⁇ m to 5 ⁇ m and a softening point of 500 ° C. to 700 ° C. Glass frit that does not contain can be used.
  • the glass frit includes components such as CaO, BaO, ZnO, TiO 2 and V 2 O 5 for the purpose of improving the wettability between the glass and the substrate, the adhesion between the substrate and the conductor, and further improving the oxidation resistance of the conductor. May be included as a glass component. Further, the glass frit can be contained in the range of 0.1% by mass or more and 10% by mass or less with respect to the conductor-forming composition.
  • the organic vehicle is obtained by dissolving a binder resin in a solvent.
  • a binder resin ethyl cellulose, acrylate, methacrylate, butyral, modified cellulose, modified acrylate, modified methacrylate, modified butyral and the like can be used as in the conventional case.
  • the binder resin is preferably contained in the range of 1% by mass to 15% by mass with respect to the conductor-forming composition.
  • the content of the binder resin is less than 1% by mass, the handling property of the conductor-forming composition is poor, and the viscosity characteristic as a paste necessary for forming a conductor may not be obtained.
  • the content of the binder resin exceeds 15% by mass, the viscosity becomes too high, and the screen dropout at the time of screen printing becomes worse, which may cause clogging.
  • Solvents include terpineol, carbitol, modified terpineol, modified carbitol, alcohol, phthalic acid ester, adipic acid ester, trimellitic acid ester, citric acid ester, sebacic acid ester, azelaic acid ester, maleic acid ester, benzoic acid ester
  • An organic solvent such as can be used.
  • the blending amount of the solvent in the organic vehicle can be used in the same blending amount as before, and for example, it can be contained in the range of 20 to 60% by mass with respect to the conductor-forming composition.
  • the conductor-forming composition may contain a thixotropic agent.
  • a thixotropic agent an oxide polyolefin, a hydrogenated castor oil system, an amide wax system, a polymer oil system, a surfactant system, or fumed silica can be used.
  • the thixotropic agent it is possible to suppress the separation of the conductor-forming composition and enhance the effect of suppressing the occurrence of slit flow.
  • FIG. 3 shows an example of a production method that can be suitably used as a method for producing the conductor-forming composition of the present embodiment.
  • the manufacturing method of the composition for conductor formation of this embodiment is demonstrated.
  • raw materials including conductive powder, glass frit, and organic vehicle are dispersed to obtain a mixture (step S10).
  • the method for dispersing the raw material is not particularly limited, and for example, the material containing the conductive powder, the glass frit, and the organic vehicle can be dispersed by mixing using a known dispersion apparatus. .
  • a dispersion device As a dispersion device, a high-pressure emulsification device, a mixing stirrer, a suction dispersion stirrer, a bead mill, a ball mill, a three-roll mill, and the like can be used. Among these, from the viewpoint of more uniformly crushing and dispersing the material It is preferable to use a three-roll mill.
  • the particles 1 are added to the obtained mixture and mixed to obtain a conductor-forming composition (step S20).
  • a pressure low pressure
  • the particle 1 to be added to the mixture has a particle diameter D50 of 1.5 to 4 times the conductor film thickness, and the particle content a is 100 parts by mass of the conductive powder. On the other hand, it is preferably 30 parts by mass or less, and the relationship between the particle diameter D50 ( ⁇ m) of the particles and the content a (parts by mass) of the particles satisfies the following formula (1).
  • Formula (1) 80 ⁇ D50 ( ⁇ m) ⁇ a (part by mass)
  • the gap between the rolls of the three-roll mill is appropriately adjusted within the above range, each material is controlled while suppressing the pulverization of the particle 1 in the mixing step and controlling the particle size of the particle 1 in the resulting conductor-forming composition within a desired range. Can be uniformly dispersed.
  • FIG. 4 is a diagram illustrating an example of a conductor manufacturing method according to the present embodiment. Hereinafter, with reference to FIG. 4, the manufacturing method of the conductor of this embodiment is demonstrated.
  • the conductor forming composition is applied to at least one surface of the substrate (step S30).
  • coating can use screen printing etc., for example.
  • a slit substrate having a slit can be used as the substrate.
  • the slit substrate is divided along the slits to form respective chip components.
  • the substrate portion 20 shown in FIGS. 1 and 2 is a substrate portion corresponding to one chip in a chip component (for example, a chip resistor).
  • the substrate coated with the conductor-forming composition is dried to form a dry film on the substrate (step S40).
  • the drying conditions are not particularly limited as long as at least a part of the solvent contained in the conductor-forming composition can be removed. Drying can be performed using, for example, a belt drying furnace or a stationary drying furnace set so that the maximum temperature is 120 ° C. or higher and 250 ° C. or lower. The drying time can be appropriately adjusted according to the set temperature.
  • the conductor forming composition When applying the conductor forming composition to both surfaces (front and back surfaces) of the substrate, after applying and drying on one surface of the substrate by screen printing or the like, the conductor formation is similarly applied to the other surface of the substrate. Apply composition for drying. Through this step, for example, as shown in FIG. 2A, a pair of dry films 11 having a predetermined interval on both the back surface and the front surface of the substrate portion 20 can be obtained.
  • the substrate on which the dry film is formed is baked (step S50).
  • the conductive powder contained in the conductor-forming composition is sintered to form the conductor portion 2 as shown in FIG.
  • the firing conditions are not particularly limited, and the conditions under which the conductive powder is sintered can be used, but it is preferably performed in an air atmosphere. Firing can be performed, for example, in a belt furnace (belt drying furnace) set so that the maximum temperature is 600 ° C. or higher and 900 ° C. or lower. The firing time can be appropriately adjusted according to the set temperature.
  • Resistor FIG. 5 is a schematic diagram showing an example of a resistor (chip resistor) of the present embodiment.
  • the resistor 100 includes at least the substrate 20, the conductor 10, and the resistor 40.
  • the resistor 100 has a protective layer 50 such as a glass layer or a resin layer on the resistor 40.
  • the conductor 10 which comprises the resistor 100 contains the surface electrode 10a and the back surface electrode 10b, as shown in FIG.
  • the front electrode 10a and / or the back electrode 10b are formed from a conductor formed using the conductor-forming composition.
  • the resistor 100 can be manufactured by a conventionally known manufacturing method.
  • Example 1 Manufacture of a composition for forming a conductor 50% by mass of Ag powder as a conductive powder, 4% by mass of ethyl cellulose as a binder resin (as an organic vehicle dissolved in terpineol (solvent)), 4% by mass of glass frit, Further, 1% by mass of a thixotropic agent having a heating residue of 25% mainly composed of oxidized polyolefin was added, and the mixture was pulverized and dispersed with a three-roll mill (Bueller Co., Ltd., SDY-300) to prepare a mixture.
  • a three-roll mill Bueller Co., Ltd., SDY-300
  • Example 2 A conductor-forming composition was produced under the same conditions as in Example 1, except that 0.4% by mass of fumed silica was added as a thixotropic agent. Using the obtained conductor forming composition, the bonding with the belt portion and the residual state of the oxide powder were confirmed. The results are shown in Table 1.
  • Example 3 Conductor formation under the same conditions as in Example 1 except that 8 parts by mass (4% in 100% by mass of the conductor-forming composition) of alumina powder having an average particle diameter (D50) of 11 ⁇ m was added to the conductive powder. A composition was prepared. Using the obtained conductor forming composition, the bonding with the belt portion and the oxide powder remaining state were confirmed. The results are shown in Table 1.
  • Example 4 As a thixotropic agent, a mixture containing 0.4% by mass of fumed silica was prepared by a three-roll mill, and 8 parts by mass of an alumina powder having an average particle size (D50) of 11 ⁇ m with respect to the conductive powder (composition for forming a conductor) The composition for conductor formation was manufactured on the conditions similar to Example 1 except having added 4 mass% in 100 mass%. Using the obtained conductor forming composition, the bonding with the belt portion and the oxide powder remaining state were confirmed. The results are shown in Table 1.
  • Example 5 Conductor formation under the same conditions as in Example 1 except that 12 parts by mass (6% by mass in 100% by mass of the conductor-forming composition) of alumina powder having an average particle size (D50) of 8 ⁇ m was added to the conductive powder. A composition was prepared. Using the obtained conductor forming composition, the bonding with the belt portion and the oxide powder remaining state were confirmed. The results are shown in Table 1.
  • Example 6 The same conditions as in Example 1 except that 12 parts by mass of aluminum nitride having an average particle diameter (D50) of 8 ⁇ m as particles 1 was added to the conductive powder (6% by mass in 100% by mass of the conductor-forming composition). A conductor-forming composition was produced. Using the obtained conductor forming composition, the bonding with the belt portion and the oxide powder remaining state were confirmed. The results are shown in Table 1.
  • Example 7 Except that 12 parts by mass (6% by mass in 100% by mass of the conductor-forming composition) of silicon carbide having an average particle size (D50) of 8 ⁇ m as particles 1 was added to the conductive powder. A conductor-forming composition was produced under the conditions. Using the obtained conductor forming composition, the bonding with the belt portion and the oxide powder remaining state were confirmed. The results are shown in Table 1.
  • Example 8 The same conditions as in Example 1 except that 12 parts by mass (6% by mass in 100% by mass of the conductor-forming composition) of zirconia having an average particle size (D50) of 8 ⁇ m was added as particles 1 to the conductive powder. A conductor-forming composition was produced. Using the obtained conductor forming composition, the bonding with the belt portion and the oxide powder remaining state were confirmed. The results are shown in Table 1.
  • Example 1 A conductor forming composition was obtained under the same conditions as in Example 1 except that the alumina powder and the thixotropic agent were not added to the mixture. Using the obtained conductor forming composition, the bonding with the belt portion and the oxide powder remaining state were confirmed. The results are shown in Table 1.
  • Example 4 As a thixotropic agent, 1% by mass of a thixotropic agent having a heating residue of 25% mainly composed of oxidized polyolefin is added, and 12 parts by mass of alumina powder having an average particle size (D50) of 4.7 ⁇ m with respect to the conductive powder (for conductor formation) A conductor-forming composition was produced under the same conditions as in Example 1 except that 6% by mass was added to 100% by mass of the composition. Using the obtained conductor forming composition, the bonding with the belt portion and the oxide powder remaining state were confirmed. The results are shown in Table 1.
  • Example 9 A conductor-forming composition under the same conditions as in Example 1, except that 0.4% by mass of fumed silica was added as a thixotropic agent, and 8% by mass of oxide powder was replaced with silver powder having an average particle size of 10 ⁇ m. Manufactured. Using the obtained conductor forming composition, the bonding with the belt portion and the oxide powder remaining state were confirmed. The results are shown in Table 1.
  • Example 10 A conductor-forming composition under the same conditions as in Example 1 except that 8% by mass of Ag powder having an average particle diameter (D50) of 10 ⁇ m was added to 100% by mass of the conductor-forming composition instead of adding particles 1 Manufactured. Using the obtained conductor forming composition, the bonding with the belt portion and the oxide powder remaining state were confirmed. The results are shown in Table 1.
  • FIG. 6 shows the average particle diameter (D50), the content of the particles, and the seizure to the belt furnace when alumina particles are used as the particles 1 obtained from the evaluation results of the examples and comparative examples. Shows the relationship between presence and absence (no seizure ⁇ , seizure ⁇ ). As shown in Table 1 and FIG. 6, the average particle diameter (D50) of the particles 1 and the content a of the particles 1 include particles 1 that are 1.5 to 4 times the thickness of the conductor. As for the conductor formation composition of the Example which satisfy
  • fills the relationship of 80 ⁇ D50 (micrometer) xa (mass part), the seizure to a belt furnace was not observed. From the above, it has been shown that the conductor-forming composition according to the present embodiment can suppress the phenomenon of joining with other members such as a belt of a belt furnace in a firing process.

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JP7425958B2 (ja) 2019-06-28 2024-02-01 住友金属鉱山株式会社 厚膜抵抗体用組成物、厚膜抵抗体用ペーストならびに厚膜抵抗体

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