WO2024181020A1 - 導電性ペースト - Google Patents

導電性ペースト Download PDF

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WO2024181020A1
WO2024181020A1 PCT/JP2024/003419 JP2024003419W WO2024181020A1 WO 2024181020 A1 WO2024181020 A1 WO 2024181020A1 JP 2024003419 W JP2024003419 W JP 2024003419W WO 2024181020 A1 WO2024181020 A1 WO 2024181020A1
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ionic radius
coordination
powder
ceramic
ratio
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English (en)
French (fr)
Japanese (ja)
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隆志 大原
英靖 大西
宏明 大地
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Murata Manufacturing Co Ltd
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Murata Manufacturing Co Ltd
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Priority to CN202480014638.2A priority Critical patent/CN120677544A/zh
Priority to JP2025503682A priority patent/JPWO2024181020A1/ja
Priority to KR1020257023176A priority patent/KR20250121094A/ko
Publication of WO2024181020A1 publication Critical patent/WO2024181020A1/ja
Priority to US19/293,595 priority patent/US20250364152A1/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, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
    • H01G4/00—Fixed capacitors; Processes of their manufacture
    • H01G4/30—Stacked capacitors
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
    • H01G4/00—Fixed capacitors; Processes of their manufacture
    • H01G4/002—Details
    • H01G4/005—Electrodes
    • H01G4/008—Selection of materials
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
    • H01G4/00—Fixed capacitors; Processes of their manufacture
    • H01G4/002—Details
    • H01G4/005—Electrodes
    • H01G4/008—Selection of materials
    • H01G4/0085—Fried electrodes
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
    • H01G4/00—Fixed capacitors; Processes of their manufacture
    • H01G4/002—Details
    • H01G4/005—Electrodes
    • H01G4/012—Form of non-self-supporting electrodes
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
    • H01G4/00—Fixed capacitors; Processes of their manufacture
    • H01G4/002—Details
    • H01G4/018—Dielectrics
    • H01G4/06—Solid dielectrics
    • H01G4/08—Inorganic dielectrics
    • H01G4/12—Ceramic dielectrics
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
    • H01G4/00—Fixed capacitors; Processes of their manufacture
    • H01G4/002—Details
    • H01G4/018—Dielectrics
    • H01G4/06—Solid dielectrics
    • H01G4/08—Inorganic dielectrics
    • H01G4/12—Ceramic dielectrics
    • H01G4/1209—Ceramic dielectrics characterised by the ceramic dielectric material
    • H01G4/1218—Ceramic dielectrics characterised by the ceramic dielectric material based on titanium oxides or titanates
    • H01G4/1227—Ceramic dielectrics characterised by the ceramic dielectric material based on titanium oxides or titanates based on alkaline earth titanates
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
    • H01G4/00—Fixed capacitors; Processes of their manufacture
    • H01G4/002—Details
    • H01G4/228—Terminals
    • H01G4/232—Terminals electrically connecting two or more layers of a stacked or rolled capacitor
    • H01G4/2325—Terminals electrically connecting two or more layers of a stacked or rolled capacitor characterised by the material of the terminals

Definitions

  • This invention relates to a conductive paste, and in particular to a conductive paste for forming internal electrodes in multilayer ceramic capacitors.
  • a multilayer ceramic capacitor typically comprises a laminate having a plurality of laminated dielectric layers made of ceramic and a plurality of internal electrodes respectively arranged along a plurality of interfaces between the dielectric layers, and a plurality of external electrodes provided on the outer surface of the laminate and electrically connected to the internal electrodes.
  • the internal electrodes comprise a plurality of first internal electrodes and a plurality of second internal electrodes arranged alternately in the stacking direction of the laminate, and the external electrodes comprise a first external electrode electrically connected to the first internal electrodes and a second external electrode electrically connected to the second internal electrodes.
  • the present invention was made in consideration of these problems, and aims to provide a conductive paste for forming internal electrodes that can maintain a relatively high level of coverage even when the internal electrodes are made thin.
  • This invention is directed to a conductive paste for forming internal electrodes of a multilayer ceramic capacitor, which contains a conductive metal powder, a ceramic powder, an organic solvent and an organic binder.
  • the ceramic powder contained in the conductive paste is intended to suppress a decrease in coverage, but the present inventors discovered a relationship between the metal constituting the conductive metal powder contained in the conductive paste and the A-site element in the ABO 3 type oxide constituting the ceramic powder, leading to the invention. More specifically, the present inventors focused on the ionic radius of the metal constituting the conductive metal powder and the ionic radius of the A-site element in the ABO 3 type oxide constituting the ceramic powder, and discovered that if the ratio of these ionic radii is within a predetermined range, it contributes to improving the coverage of the internal electrodes.
  • the appropriate ion radius ratio that can contribute to improved coverage of the internal electrode is not universal, but differs depending on the metal species that make up the conductive metal powder.
  • the inventors of the present invention have noticed that although the appropriate ion radius ratio differs depending on the metal species that make up the conductive metal powder, there are commonalities in the appropriate ion radius ratio even if the metal species are different.
  • At least a part of the ceramic powder is a powder made of an ABO3 type oxide in which the A-site element has a specific ionic radius, and the ratio of the ionic radius of the A-site element in ABO3 in 6-coordination to the ionic radius of the metal contained in the conductive metal powder in 6 -coordination is 0.97 or more and 1.02 or less.
  • the internal electrodes of a multilayer ceramic capacitor By forming the internal electrodes of a multilayer ceramic capacitor using the conductive paste of this invention, it is possible to increase the coverage of the internal electrodes regardless of the type of metal that makes up the conductive metal powder. Therefore, even if the internal electrodes are made thinner, the coverage of the internal electrodes can be maintained high, and the increase in capacity of the multilayer ceramic capacitor can be prevented from being hindered.
  • FIG. 1 is a cross-sectional view that illustrates a multilayer ceramic capacitor 1 to which a conductive paste according to the present invention is applied.
  • the multilayer ceramic capacitor 1 comprises a laminate 2.
  • the laminate 2 comprises a plurality of laminated dielectric layers 3 made of ceramic, and a plurality of internal electrodes 4 and 5 arranged along the interfaces between the plurality of dielectric layers 3.
  • the internal electrodes 4 and 5 are classified into a plurality of first internal electrodes 4 and a plurality of second internal electrodes 5 arranged alternately in the lamination direction of the laminate 2.
  • a first external electrode 6 and a second external electrode 7 are provided on the outer surface of the laminate 2, more specifically, on each of the opposing end faces.
  • the first external electrode 6 is electrically connected to the first internal electrode 4, and the second external electrode 7 is electrically connected to the second internal electrode 5.
  • the dielectric layer 3 is made of a ceramic mainly composed of ABO3 (A is at least one of Ba, Ca and Sr, and B is at least one of Ti and Zr).
  • the ceramic mainly composed of ABO3 may further contain at least one of Mn, Mg, Si, Y, Dy and Gd as a secondary component.
  • the internal electrodes 4 and 5 preferably contain, as a conductive component, one selected from nickel, copper, silver, and a silver/palladium alloy. Furthermore, as a characteristic composition, the internal electrodes 4 and 5 contain, as a ceramic component, an ABO 3 type oxide having a specific ionic radius, in which the ratio of the ionic radius of the A site element in ABO 3 in 6-coordination to the ionic radius of the metal element serving as the conductive component in 6-coordination is 0.97 or more and 1.02 or less. This ABO 3 type oxide preferably has an ilmenite crystal structure.
  • the dielectric layer 3 is made of a ceramic mainly composed of at least one selected from BaTiO 3 , SrTiO 3 and CaZrO 3.
  • the internal electrodes 4 and 5 may further contain, as a ceramic component, at least one selected from BaTiO 3 , SrTiO 3 and CaZrO 3 contained in the dielectric layer 3, if necessary, in addition to the ABO 3 type oxide having the specific ionic radius described above.
  • the content of the ceramic components in the internal electrodes 4 and 5 is preferably selected to be 5% by mass or more and 15% by mass or less.
  • the content is ⁇ (mass of ceramic components)/(mass of ceramic components + mass of conductive metal or alloy containing conductive metal) ⁇ x 100 (hereinafter the same).
  • the external electrodes 6 and 7 are formed, for example, by applying a conductive paste containing Ag or Cu as the main conductive component to the end faces of the laminate 2 and baking this. If necessary, for example, Ni plating and Sn plating may be applied on the thick film formed by baking.
  • the multilayer ceramic capacitor 1 is manufactured, for example, through the following steps. First, a ceramic slurry is prepared containing ceramic raw material powder having the above-mentioned composition. Next, a suitable sheet forming method is applied to the ceramic slurry to form ceramic green sheets. Next, a conductive paste that is to become each of the internal electrodes 4 and 5 is applied by printing or the like onto predetermined ceramic green sheets out of the multiple ceramic green sheets. Next, the multiple ceramic green sheets are stacked and then pressed together to obtain a green laminate. Next, the green laminate is fired. In this firing process, the ceramic green sheets become the dielectric layers 3. After that, external electrodes 6 and 7 are formed on the end faces of the laminate 2.
  • the conductive paste to be used to form the internal electrodes 4 and 5 in the manufacture of the multilayer ceramic capacitor 1 described above is preferably prepared as follows.
  • the conductive paste is produced in the following steps: a first step of preparing a ceramic powder slurry containing ceramic powder, an organic solvent, and a dispersant; a second step of preparing a metal powder slurry containing conductive metal powder, an organic solvent, and a dispersant; a third step of preparing an organic vehicle containing an organic resin component and an organic solvent; and a fourth step of mixing the ceramic powder slurry, metal powder slurry, and organic vehicle.
  • a ceramic powder slurry is prepared by mixing a ceramic powder and a dispersant in an organic solvent.
  • the ceramic powder is made of the ABO 3 type oxide having the specific ion radius described above.
  • at least one selected from BaTiO 3 , SrTiO 3 and CaZrO 3 may be used as a co-material.
  • a powder made of at least one selected from BaTiO 3 , SrTiO 3 and CaZrO 3 it is preferable that 10% by volume or more of the ceramic powder is a powder made of the ABO 3 type oxide having the specific ion radius, and the remainder of the ceramic powder is a powder mainly composed of at least one selected from BaTiO 3 , SrTiO 3 and CaZrO 3 .
  • the ABO 3 type oxide with a specific ionic radius is determined by the metal species constituting the conductive metal powder contained in the metal powder slurry produced in the second step described below. That is, the ABO 3 type oxide with a specific ionic radius is an ABO 3 type oxide in which the ionic radius of the metal contained in the conductive metal powder in 6 -coordination is obtained, and the A-site element is an element whose ionic radius in 6-coordination is 0.97 or more and 1.02 or less to this ionic radius. The range of 0.97 or more and 1.02 or less, which is the ratio of the ionic radius, is derived from the results of an experiment described below.
  • the ceramic powder made of the ABO 3 type oxide with a specific ionic radius can suppress the reaction that may occur between the conductive metal powder contained in the metal powder slurry produced in the second step during firing.
  • the ceramic powder contained in the conductive paste may contain the ABO 3 oxide as the main component and at least one of Mn, Mg, Si, Y, Dy and Gd as a subcomponent. When such a subcomponent is contained, the grain growth of the ceramic particles is suppressed, and the sintering of the metal particles may be more effectively suppressed.
  • the dispersant mixed with the ceramic powder in the first step may be, for example, an anionic polymer dispersant, and the organic solvent may be, for example, dihydroterpineol.
  • a metal powder slurry is prepared by mixing a conductive metal powder and a dispersant with an organic solvent.
  • the conductive metal powder may be, for example, a powder of one type selected from nickel, copper, silver, and a silver/palladium alloy.
  • the dispersant and organic solvent used in the second step may be the same as those used in the first step.
  • an organic vehicle is produced by mixing an organic resin component with an organic solvent.
  • organic resin component ethyl cellulose resin
  • the organic solvent used in the third step can be the same as that used in the first step.
  • the ceramic powder slurry, the metal powder slurry, and the organic vehicle are mixed together to obtain a conductive paste that will become the internal electrodes 4 and 5.
  • This conductive paste contains a ceramic powder slurry, and as described above, the ceramic powder slurry contains a ceramic powder made of an ABO3 oxide having a specific ionic radius, so that the internal electrodes 4 and 5 provided in the multilayer ceramic capacitor 1 manufactured through the firing step contain an ABO3 oxide having a specific ionic radius.
  • the content of ceramic powder in the conductive paste is preferably selected to be 5% by mass or more and 15% by mass or less.
  • NiTiO 3 , MgTiO 3 and MnTiO 3 were prepared as ABO 3 oxides with specific ionic radii constituting the ceramic powder contained in the conductive paste for forming the internal electrodes, and CuTiO 3 , BaTiO 3 , CaZrO 3 and SrTiO 3 were prepared as other ABO 3 oxides.
  • Table 1 shows the "crystal structure", “coordination number”, "A site element” and "ionic radius” for these ABO 3 oxides.
  • Ba, Ca and Sr have 12 coordinations in the original perovskite structure, but Ba, Ca and Sr also have 6 coordinations when they are dissolved in the site of the 6-coordinated elements (Ni, Mg, Mn) of the ilmenite structure, so the "ionic radius" in Table 1 shows the value for 6 coordinations.
  • nickel powder as a conductive metal powder, dihydroterpineol as an organic solvent, and an anionic polymer dispersant as a dispersant were dispersed in a three-roll mill to produce a metal powder slurry (second process).
  • the metal powder slurry and the ceramic powder slurry were added to the organic vehicle and mixed and dispersed to produce a conductive paste for forming the internal electrodes (fourth step).
  • the ceramic powder content in the conductive paste for forming the internal electrodes was set to 10 mass%.
  • Table 2 shows the ratio of the ionic radius of the A-site element in 6-coordination to the ionic radius of nickel in 6-coordination to be included in the internal electrode, i.e., the "ionic radius ratio (A-site element/metallic nickel)."
  • the ratio of the ionic radius of Ba in 6-coordination (1.35 ⁇ ) shown in Table 1 to the ionic radius of Ni in 6-coordination (0.69 ⁇ ) is shown.
  • the internal electrode and dielectric layer located at the center in the height direction of the laminate in the sample multilayer ceramic capacitor were peeled off from each other by electrochemical peeling.
  • the ionic radius of nickel in 6-coordination is 0.69 ⁇ , as shown in the "NiTiO 3 " section of Table 1.
  • the ionic radius of the A-site element in each of NiTiO 3 , MgTiO 3 and MnTiO 3 as the ABO 3 oxides contained in the internal electrodes of Samples 1 to 3 and 5 to 7 in 6-coordination is 0.69 ⁇ , 0.72 ⁇ and 0.67 ⁇ , respectively, as shown in Table 1.
  • NiTiO 3 , MgTiO 3 and MnTiO 3 as the ABO 3 oxides in samples 1 to 3 and 5 to 7 have an ionic radius in 6-coordination of the A-site element in ABO 3 that is equal to or close to the ionic radius in 6-coordination of nickel as the conductive metal to be contained in the internal electrode, so that the energy difference with the nickel in the internal electrode is zero or small, and the oxides remain without being expelled from the internal electrode portion, thereby acting to improve the heat resistance of the internal electrode.
  • the coverage was high at 84% or more in samples 1 to 3 and 5 to 7.
  • the addition ratio of NiTiO 3 , MgTiO 3 and MnTiO 3 is not necessarily 100%, and if it is 10% or more, an effect of improving coverage was observed compared to the case where none of NiTiO 3 , MgTiO 3 and MnTiO 3 is included. It is also noteworthy that in Experimental Example 1-1, the coverage of samples 5 to 7, in which the addition ratio of NiTiO 3 , MgTiO 3 and MnTiO 3 is 10%, shows a value equal to the coverage of samples 1 to 3, in which the addition ratio is 100%.
  • the "ionic radius ratio" was outside the range of 0.97 or more and 1.04 or less, and it is presumed that CuTiO3 and BaTiO3 were expelled from the internal electrode portion, so that the heat resistance of the internal electrode was not improved and the coverage was reduced.
  • the ceramic powder content in the conductive paste for forming the internal electrodes was set to 10 mass%.
  • the ionic radius of nickel in 6-coordination is 0.69 ⁇ , as shown in the "NiTiO 3 " section of Table 1.
  • the ionic radius of the A-site element in each of NiTiO 3 , MgTiO 3 and MnTiO 3 as the ABO 3 oxides contained in the internal electrodes of Samples 11 to 13 and 15 to 17 in 6-coordination is 0.69 ⁇ , 0.72 ⁇ and 0.67 ⁇ , respectively, as shown in Table 1.
  • the ionic radius of the A site element in ABO 3 in 6-coordination is equal to or close to the ionic radius of nickel in 6-coordination as the conductive metal to be contained in the internal electrode, so that the energy difference with the nickel in the internal electrode is zero or small, and so the oxide remains without being expelled from the internal electrode portion, and acts to improve the heat resistance of the internal electrode, and as a result, it is presumed that the coverage was high at 81% or more in samples 11 to 13 and 15 to 17.
  • the addition ratio of NiTiO 3 , MgTiO 3 and MnTiO 3 is not necessarily 100%, but if it is 10% or more, an effect of improving coverage was observed compared to the case where none of NiTiO 3 , MgTiO 3 and MnTiO 3 was included.
  • the "ionic radius ratio" was outside the range of 0.97 or more and 1.04 or less, and it is presumed that CuTiO3 and CaZrO3 were expelled from the internal electrode portion, respectively, so that the heat resistance of the internal electrode was not improved and the coverage was reduced.
  • SrTiO 3 1-3-1 Main component of ceramic constituting dielectric layer: SrTiO 3 1-3-1.
  • SrTiO3 -based ceramic raw material constituting dielectric layer As starting raw materials, the main components of SrCO3 and TiO2 powders, and the subcomponents of MnO, SiO2 and MgO powders were weighed and mixed in a ball mill for 72 hours, and then heat-treated at a top temperature of 1000°C for 2 hours to obtain SrTiO3 -based ceramic raw material powder.
  • the ceramic powder content in the conductive paste for forming the internal electrodes was set to 10 mass%.
  • the ionic radius of nickel in 6-coordination is 0.69 ⁇ , as shown in the "NiTiO 3 " section of Table 1.
  • the ionic radius of the A-site element in each of NiTiO 3 , MgTiO 3 and MnTiO 3 as the ABO 3 oxides contained in the internal electrodes of Samples 21 to 23 and 25 to 27 in 6-coordination is 0.69 ⁇ , 0.72 ⁇ and 0.67 ⁇ , respectively, as shown in Table 1.
  • the ionic radius of the A site element in ABO 3 in 6-coordination is equal to or close to the ionic radius of nickel in 6-coordination as the conductive metal to be contained in the internal electrode, so that the energy difference with the nickel in the internal electrode is zero or small, and so the oxide remains without being expelled from the internal electrode portion, and acts to improve the heat resistance of the internal electrode, and as a result, it is presumed that the coverage exceeded 80% in samples 21 to 23 and 25 to 27.
  • the addition ratio of NiTiO 3 , MgTiO 3 and MnTiO 3 is not necessarily 100%, and if it is 10% or more, an effect of improving coverage was observed compared to the case where none of NiTiO 3 , MgTiO 3 and MnTiO 3 was included.
  • sample 28 which was also evaluated as "x"
  • SrTiO 3 as a common material is added to the internal electrode.
  • Sr which is an element of the A site in ABO 3 of the perovskite structure
  • the ionic radius of Sr at 6 coordinations is 1.18 ⁇ , as shown in Table 1. Therefore, the ratio of the ionic radius of Sr at 6 coordinations to the ionic radius of nickel at 6 coordinations, that is, the "ionic radius ratio" is 1.71. Therefore, the "ionic radius ratio" is out of the range of 0.97 or more and 1.04 or less, and the coverage is low at 70%.
  • the "ionic radius ratio" was outside the range of 0.97 or more and 1.04 or less, and it is presumed that CuTiO3 and SrTiO3 were expelled from the internal electrode portion, respectively, so that the heat resistance of the internal electrode was not improved and the coverage was reduced.
  • CuTiO 3 , CoTiO 3 and CrTiO 3 were prepared as ABO 3 oxides with specific ionic radii constituting the ceramic powder contained in the conductive paste for forming the internal electrodes, and BaTiO 3 , CaZrO 3 and SrTiO 3 were prepared as other ABO 3 oxides.
  • Table 5 shows the "crystal structure", “coordination number”, "A site element” and "ionic radius” for these ABO 3 oxides .
  • Ba, Ca and Sr have 12 coordinations in the original perovskite structure, but Ba, Ca and Sr also have 6 coordinations when they are dissolved in the site of the 6-coordinated elements (Cu, Co, Cr) of the ilmenite structure, so the "ionic radius" in Table 5 shows the value for 6 coordinations.
  • the ceramic powder content in the conductive paste for forming the internal electrodes was set to 10 mass%.
  • Table 6 shows the ratio of the ionic radius of the A-site element in 6-coordination to the ionic radius of copper in 6-coordination to be included in the internal electrode, i.e., the "ionic radius ratio (A-site element/metallic copper)."
  • the ratio of the ionic radius of Ba element in 6-coordination (1.35 ⁇ ) shown in Table 5 to the ionic radius of copper in 6-coordination (0.77 ⁇ ) is shown.
  • Samples 31 to 36 in Table 6 are rated as " ⁇ ".
  • the internal electrodes contain any of CuTiO 3 , CoTiO 3 and CrTiO 3 as the ABO 3 oxide.
  • the internal electrodes also contain copper as a conductive component.
  • the ionic radius of copper in 6-coordination is 0.77 ⁇ , as shown in the "CuTiO 3 " section of Table 5.
  • the ionic radius of the A-site element in each of CuTiO 3 , CoTiO 3 and CrTiO 3 as the ABO 3 oxides contained in the internal electrodes of Samples 31 to 36 in 6-coordination is 0.77 ⁇ , 0.74 ⁇ and 0.80 ⁇ , respectively, as shown in Table 5.
  • the ionic radius of the A-site element in ABO 3 in 6-coordination is equal to or close to the ionic radius of copper in 6-coordination as the conductive metal to be contained in the internal electrode, so that the energy difference with the copper in the internal electrode is zero or small, and the oxide remains without being expelled from the internal electrode portion, thereby improving the heat resistance of the internal electrode.
  • the coverage was high at 84% or more in samples 31 to 36.
  • the addition ratio of CuTiO 3 , CoTiO 3 and CrTiO 3 is not necessarily 100%, and if it is 10% or more, an effect of improving coverage was observed compared to the case where none of CuTiO 3 , CoTiO 3 and CrTiO 3 is included. It is also noteworthy that in Experimental Example 2-1, the coverage of samples 34 to 36, in which the addition ratio of CuTiO 3 , CoTiO 3 and CrTiO 3 is 10%, shows a value equal to the coverage of samples 31 to 33, in which the addition ratio is 100%.
  • the "ionic radius ratio" was outside the range of 0.96 or more and 1.04 or less, and it is presumed that BaTiO 3 was expelled from the internal electrode portion, the heat resistance of the internal electrode was not improved, and the coverage was reduced.
  • the ceramic powder content in the conductive paste for forming the internal electrodes was set to 10 mass%.
  • Samples 41 to 46 in Table 7 are rated as " ⁇ ".
  • the internal electrodes contain any of CuTiO 3 , CoTiO 3 and CrTiO 3 as the ABO 3 oxide.
  • the internal electrodes also contain copper as a conductive component.
  • the ionic radius of copper in 6-coordination is 0.77 ⁇ , as shown in the "CuTiO 3 " section of Table 5.
  • the ionic radius of the A-site element in each of CuTiO 3 , CoTiO 3 and CrTiO 3 as the ABO 3 oxides contained in the internal electrodes of Samples 41 to 46 in 6-coordination is 0.77 ⁇ , 0.74 ⁇ and 0.80 ⁇ , respectively, as shown in Table 5.
  • the ionic radius of the A-site element in ABO3 in 6-coordination is equal to or close to the ionic radius of copper in 6-coordination as the conductive metal to be contained in the internal electrodes, and therefore the energy difference with the copper in the internal electrodes is zero or small, and therefore the oxides remain without being expelled from the internal electrode portion, and act to improve the heat resistance of the internal electrodes, and as a result, it is presumed that the coverage was high at 81% or more in samples 41 to 46.
  • the addition ratio of CuTiO 3 , CoTiO 3 and CrTiO 3 is not necessarily 100%, but if it is 10% or more, an effect of improving coverage was observed compared to the case where none of CuTiO 3 , CoTiO 3 and CrTiO 3 was included.
  • the "ionic radius ratio" was outside the range of 0.96 or more and 1.04 or less, and it is presumed that CaZrO3 was expelled from the internal electrode portion, the heat resistance of the internal electrode was not improved, and the coverage was reduced.
  • the ceramic powder content in the conductive paste for forming the internal electrodes was set to 10 mass%.
  • Samples 51 to 56 in Table 8 are rated as " ⁇ ".
  • the internal electrodes contain any of CuTiO 3 , CoTiO 3 and CrTiO 3 as the ABO 3 oxide.
  • the internal electrodes also contain copper as a conductive component.
  • the ionic radius of copper in 6-coordination is 0.77 ⁇ , as shown in the "CuTiO 3 " section of Table 5.
  • the ionic radius of the A-site element in each of CuTiO 3 , CoTiO 3 and CrTiO 3 as the ABO 3 oxides contained in the internal electrodes of Samples 51 to 56 in 6-coordination is 0.77 ⁇ , 0.74 ⁇ and 0.80 ⁇ , respectively, as shown in Table 5.
  • the ionic radius of the A-site element in ABO3 in 6-coordination is equal to or close to the ionic radius of copper in 6-coordination as the conductive metal to be contained in the internal electrodes, and therefore the energy difference with the copper in the internal electrodes is zero or small, and therefore the oxides remain without being expelled from the internal electrode portion, and act to improve the heat resistance of the internal electrodes, and as a result, it is presumed that the coverage exceeded 80% in samples 51 to 56.
  • the addition ratio of CuTiO 3 , CoTiO 3 and CrTiO 3 is not necessarily 100%, but if it is 10% or more, an effect of improving coverage was observed compared to the case where none of CuTiO 3 , CoTiO 3 and CrTiO 3 was included.
  • sample 57 which was evaluated as "x" only SrTiO 3 as a common material is added to the internal electrode.
  • Sr which is an element of the A site in ABO 3 of the perovskite structure, has 12 coordination numbers, but when it is dissolved in the A site of the ilmenite structure, it is necessary to compare the ionic radius at 6 coordination numbers, which is the coordination number of the A site of the ilmenite structure, and the ionic radius of Sr at 6 coordination numbers is 1.18 ⁇ , as shown in Table 5. Therefore, the ratio of the ionic radius of Sr at 6 coordination numbers to the ionic radius of copper at 6 coordination numbers, that is, the "ionic radius ratio" is 1.53. Therefore, the "ionic radius ratio" is out of the range of 0.96 or more and 1.04 or less, and the coverage is low at 70%.
  • the "ionic radius ratio" was outside the range of 0.96 or more and 1.04 or less, and it is presumed that SrTiO 3 was expelled from the internal electrode portion, the heat resistance of the internal electrode was not improved, and the coverage was reduced.
  • AgTiO 3 , EuTiO 3 and NaTiO 3 were prepared as ABO 3 oxides with specific ionic radii constituting the ceramic powder contained in the conductive paste for forming the internal electrodes, and CuTiO 3 , SrTiO 3 , BaTiO 3 and CaZrO 3 were prepared as other ABO 3 oxides.
  • Table 9 shows the "crystal structure", “coordination number”, "A site element” and "ionic radius” for these ABO 3 oxides.
  • Sr, Ba and Ca have 12 coordinations in the original perovskite structure, but Sr, Ba and Ca also have 6 coordinations when they are dissolved in the site of the 6-coordinated elements (Ag, Eu, Na) of the ilmenite structure, so the "ionic radius" in Table 9 shows the value for 6 coordinations.
  • Example 3-1 Main component of ceramic constituting dielectric layer: BaTiO 3 3-1-1.
  • Preparation of BaTiO3 -based ceramic raw material constituting dielectric layer BaTiO3 -based ceramic raw material powder was obtained through the same steps as in Experimental Example 1-1.
  • the ceramic powder content in the conductive paste for forming the internal electrodes was set to 10 mass%.
  • Table 10 shows the ratio of the ionic radius of the A-site element in 6-coordination to the ionic radius of silver in 6-coordination to be included in the internal electrode, i.e., the "ionic radius ratio (A-site element/metallic silver)."
  • the ratio of the ionic radius of Ba in 6-coordination (1.35 ⁇ ) shown in Table 9 to the ionic radius of silver in 6-coordination (1.15 ⁇ ) is shown.
  • Samples 61 to 63 and 65 to 67 in Table 10 are rated as " ⁇ ".
  • the internal electrodes contain AgTiO 3 , EuTiO 3 , or NaTiO 3 as the ABO 3 oxide.
  • the internal electrodes also contain silver as a conductive component.
  • the ionic radius of silver in 6-coordination is 1.15 ⁇ , as shown in the "AgTiO 3 " section of Table 9.
  • the ionic radius of the A-site element in each of AgTiO 3 , EuTiO 3 and NaTiO 3 as the ABO 3 oxides contained in the internal electrodes of Samples 61 to 63 and 65 to 67 in 6-coordination is 1.15 ⁇ , 1.17 ⁇ and 1.02 ⁇ , respectively, as shown in Table 9.
  • the ionic radius of the A-site element in ABO 3 in 6-coordination is equal to or close to the ionic radius of silver in 6-coordination as the conductive metal to be contained in the internal electrode, so that the energy difference with the silver in the internal electrode is zero or small, and the oxide remains without being expelled from the internal electrode portion, thereby improving the heat resistance of the internal electrode.
  • the coverage was high at 82% or more in samples 61 to 63 and 65 to 67.
  • the addition ratio of AgTiO 3 , EuTiO 3 and NaTiO 3 is not necessarily 100%, but as long as it is 10% or more, an effect of improving coverage was observed compared to the case where none of AgTiO 3 , EuTiO 3 and NaTiO 3 was included.
  • sample 64 which was evaluated as "x"
  • SrTiO3 was used as the ABO3 oxide
  • the ionic radius of Sr, an A-site element in ABO3 , in 6-coordination is 1.18 ⁇ , as shown in Table 9. Therefore, the ratio of the ionic radius of Sr in 6-coordination to the ionic radius of silver in 6-coordination, that is, the "ionic radius ratio”, is 1.03.
  • the "ionic radius ratio” was outside the range of 0.89 or more and 1.02 or less, and the coverage was low at 76%.
  • sample 68 which was also evaluated as "x"
  • Ba which is an element of the A site in ABO 3 of the perovskite structure
  • the ionic radius at 6 coordinations which is the coordination number of the A site of the ilmenite structure
  • the ionic radius of Ba at 6 coordinations is 1.35 ⁇ , as shown in Table 9. Therefore, the ratio of the ionic radius of Ba at 6 coordinations to the ionic radius of silver at 6 coordinations, that is, the "ionic radius ratio" is 1.17. Therefore, the "ionic radius ratio” is out of the range of 0.89 or more and 1.02 or less, and the coverage is low at 75%.
  • the "ionic radius ratio" was outside the range of 0.89 or more and 1.02 or less, and it is presumed that BaTiO 3 was expelled from the internal electrode portion, the heat resistance of the internal electrode was not improved, and the coverage was reduced.
  • the ceramic powder content in the conductive paste for forming the internal electrodes was set to 10 mass%.
  • Samples 71 to 73 and 75 to 77 in Table 11 are rated as " ⁇ ".
  • the internal electrodes contain AgTiO 3 , EuTiO 3 , or NaTiO 3 as the ABO 3 oxide.
  • the internal electrodes also contain silver as a conductive component.
  • the ionic radius of silver in 6-coordination is 1.15 ⁇ , as shown in the "AgTiO 3 " section of Table 9.
  • the ionic radius of the A-site element in each of AgTiO 3 , EuTiO 3 and NaTiO 3 as the ABO 3 oxides contained in the internal electrodes of Samples 71 to 73 and 75 to 77 in 6-coordination is 1.15 ⁇ , 1.17 ⁇ and 1.02 ⁇ , respectively, as shown in Table 9.
  • the ionic radius of the A-site element in ABO3 in 6-coordination is equal to or close to the ionic radius of silver in 6-coordination as the conductive metal to be contained in the internal electrodes, so that the energy difference with the silver in the internal electrodes is zero or small, and the oxides remain without being expelled from the internal electrode portion, thereby acting to improve the heat resistance of the internal electrodes, and as a result, it is presumed that the coverage was high at 81% or more in samples 71 to 73 and 75 to 77.
  • the addition ratio of AgTiO 3 , EuTiO 3 and NaTiO 3 is not necessarily 100%, and if it is 10% or more, an effect of improving coverage was observed compared to the case where none of AgTiO 3 , EuTiO 3 and NaTiO 3 was included.
  • sample 78 which was also evaluated as "x"
  • CaZrO3 as a common material is added to the internal electrode.
  • Ca which is an element of the A site in ABO3 of the perovskite structure, has 12 coordinations, but when it is dissolved in the A site of the ilmenite structure, it is necessary to compare the ionic radius at 6 coordinations, which is the coordination number of the A site of the ilmenite structure, and the ionic radius of Ca at 6 coordinations is 1.00 ⁇ , as shown in Table 9. Therefore, the ratio of the ionic radius of Ca at 6 coordinations to the ionic radius of silver at 6 coordinations, that is, the "ionic radius ratio" is 0.87. Therefore, the "ionic radius ratio" is out of the range of 0.89 or more and 1.02 or less, and the coverage is low at 72%.
  • the "ionic radius ratio" was outside the range of 0.89 or more and 1.02 or less, and it is presumed that CaZrO3 was expelled from the internal electrode portion, the heat resistance of the internal electrode was not improved, and the coverage was reduced.
  • the ceramic powder content in the conductive paste for forming the internal electrodes was set to 10 mass%.
  • Samples 81 to 83 and 85 to 87 in Table 12 are rated as " ⁇ ".
  • the internal electrodes contain AgTiO 3 , EuTiO 3 , or NaTiO 3 as the ABO 3 oxide.
  • the internal electrodes also contain silver as a conductive component.
  • the ionic radius of silver in 6-coordination is 1.15 ⁇ , as shown in the "AgTiO 3 " section of Table 9.
  • the ionic radius of the A-site element in each of AgTiO 3 , EuTiO 3 and NaTiO 3 as the ABO 3 oxides contained in the internal electrodes of samples 81 to 83 and 85 to 87 in 6-coordination is 1.15 ⁇ , 1.17 ⁇ and 1.02 ⁇ , respectively, as shown in Table 9.
  • the addition ratio of AgTiO 3 , EuTiO 3 and NaTiO 3 is not necessarily 100%, and if it is 10% or more, an effect of improving coverage was observed compared to the case where none of AgTiO 3 , EuTiO 3 and NaTiO 3 was included.
  • sample 88 which was also evaluated as "x"
  • SrTiO 3 which is an element of the A site in ABO 3 of the perovskite structure
  • Sr which is an element of the A site in ABO 3 of the perovskite structure
  • the ionic radius of Sr at 6 coordinations is 1.18 ⁇ , as shown in Table 9. Therefore, the ratio of the ionic radius of Sr at 6 coordinations to the ionic radius of silver at 6 coordinations, that is, the "ionic radius ratio" is 1.03. Therefore, the "ionic radius ratio” is out of the range of 0.89 or more and 1.02 or less, and the coverage is low at 70%.
  • the "ionic radius ratio" was outside the range of 0.89 or more and 1.02 or less, and it is presumed that SrTiO3 was expelled from the internal electrode portion, the heat resistance of the internal electrode was not improved, and the coverage was reduced.
  • Conductive metal powder silver/palladium alloy powder
  • silver/palladium alloy powder consisting of an alloy of 70 atm % silver and 30 atm % palladium was prepared as the conductive metal powder contained in the conductive paste for forming internal electrodes.
  • Ba, Ca, and Sr have 12 coordinations in the original perovskite structure, but Ba, Ca, and Sr also have 6 coordinations when they are dissolved in the site of the 6-coordinated element (Ag/Pd, Na, Eu) of the ilmenite structure, so the "ionic radius" in Table 13 shows the value for 6 coordinations.
  • the ceramic powder content in the conductive paste for forming the internal electrodes was set to 10 mass%.
  • Table 14 shows the ratio of the ionic radius of the A-site element in 6-coordination to the ionic radius of the silver/palladium alloy in 6-coordination to be included in the internal electrode, i.e., the "ionic radius ratio (A-site element/ Ag0.7Pd0.3 alloy)".
  • the ratio of the ionic radius of Ba element in 6-coordination (1.35 ⁇ ) shown in Table 13 to the ionic radius of silver/ palladium alloy in 6-coordination (1.06 ⁇ ) is shown.
  • Samples 91 to 96 in Table 14 are rated as " ⁇ ".
  • the internal electrodes contain any of ( Ag0.7 , Pd0.3 ) TiO3 , NaTiO3 , and EuTiO3 as the ABO3 oxide.
  • the internal electrodes also contain a silver/palladium alloy as a conductive component.
  • the ionic radius of a silver/palladium alloy in 6-coordination is 1.06 ⁇ , as shown in the "(Ag,Pd)TiO 3 " section of Table 13.
  • the ionic radii in 6-coordination of the A-site elements of (Ag 0.7 ,Pd 0.3 )TiO 3 , NaTiO 3 and EuTiO 3 as ABO 3 oxides contained in the internal electrodes of Samples 91 to 96 are 1.06 ⁇ , 1.02 ⁇ and 1.17 ⁇ , respectively, as shown in Table 13.
  • the ionic radius of the A-site element in ABO 3 , (Ag 0.7 , Pd 0.3 )TiO 3 , NaTiO 3 and EuTiO 3 as the ABO 3 oxide in samples 91 to 96, in 6-coordination is equal to or close to the ionic radius of the silver/palladium alloy as the conductive metal to be contained in the internal electrode in 6-coordination, so that the energy difference with the silver/palladium alloy in the internal electrode is 0 or small, and the oxide remains without being expelled from the internal electrode portion, thereby improving the heat resistance of the internal electrode.
  • the coverage was high at 82% or more in samples 91 to 96.
  • the addition ratio of ( Ag0.7 , Pd0.3 ) TiO3 , NaTiO3 and EuTiO3 is not necessarily 100%, and if it is 10% or more, an effect of improving coverage was observed compared to cases where none of ( Ag0.7 , Pd0.3 ) TiO3 , NaTiO3 and EuTiO3 was included.
  • the "ionic radius ratio" was outside the range of 0.96 or more and 1.10 or less, and it is presumed that BaTiO 3 was expelled from the internal electrode portion, the heat resistance of the internal electrode was not improved, and the coverage was reduced.
  • Example 4-2 Main component of ceramic constituting dielectric layer: CaZrO 3 4-2-1.
  • Preparation of CaZrO3 -based ceramic raw material constituting dielectric layer A CaZrO3 -based ceramic raw material powder was obtained through the same steps as in Experimental Example 1-2.
  • the ceramic powder content in the conductive paste for forming the internal electrodes was set to 10 mass%.
  • Samples 101 to 106 in Table 15 are rated as " ⁇ ".
  • the internal electrodes contain any of ( Ag0.7 , Pd0.3 ) TiO3 , NaTiO3 , and EuTiO3 as the ABO3 oxide.
  • the internal electrodes also contain a silver/palladium alloy as a conductive component.
  • the ionic radius of a silver/palladium alloy in 6-coordination is 1.06 ⁇ , as shown in the "(Ag,Pd)TiO 3 " section of Table 13.
  • the ionic radii in 6-coordination of the A-site elements of (Ag 0.7 ,Pd 0.3 )TiO 3 , NaTiO 3 and EuTiO 3 as ABO 3 oxides contained in the internal electrodes of Samples 101 to 106 are 1.06 ⁇ , 1.02 ⁇ and 1.17 ⁇ , respectively, as shown in Table 13.
  • the ionic radius of the A site element in ABO 3 in 6-coordination is equal to or close to the ionic radius of the silver/palladium alloy in 6-coordination as the conductive metal to be contained in the internal electrode, and therefore the energy difference with the silver/palladium alloy in the internal electrode is zero or small, and therefore the oxide remains without being expelled from the internal electrode portion, thereby acting to improve the heat resistance of the internal electrode, and as a result, it is presumed that the coverage was high at 81% or more in samples 101 to 106.
  • the addition ratio of ( Ag0.7 , Pd0.3 ) TiO3 , NaTiO3 and EuTiO3 is not necessarily 100%, and if it is 10% or more, an effect of improving coverage was observed compared to the case where none of ( Ag0.7 , Pd0.3 ) TiO3 , NaTiO3 and EuTiO3 was included.
  • sample 107 which was evaluated as "x" only CaZrO3 as a common material is added to the internal electrode.
  • Ca which is an element of the A site in ABO3 of the perovskite structure, has 12 coordinations, but when it is dissolved in the A site of the ilmenite structure, it is necessary to compare the ionic radius at 6 coordinations, which is the coordination number of the A site of the ilmenite structure, and the ionic radius at 6 coordinations of Ca is 1.00 ⁇ , as shown in Table 13. Therefore, the ratio of the ionic radius at 6 coordinations of Ca to the ionic radius at 6 coordinations of the silver/palladium alloy, that is, the "ionic radius ratio", is 0.94. Therefore, the "ionic radius ratio" is out of the range of 0.96 or more and 1.10 or less, and the coverage is low at 72%.
  • the "ionic radius ratio" was outside the range of 0.96 or more and 1.10 or less, and it is presumed that CaZrO3 was expelled from the internal electrode portion, the heat resistance of the internal electrode was not improved, and the coverage was reduced.
  • the ceramic powder content in the conductive paste for forming the internal electrodes was set to 10 mass%.
  • Table 16 shows the "ionic radius ratio (A-site element/ Ag0.7Pd0.3 alloy)" as in Table 14.
  • the ratio of the ionic radius of Sr element in 6-coordination ( 1.18 ⁇ ) shown in Table 13 to the ionic radius of silver/palladium alloy in 6-coordination (1.06 ⁇ ) is shown.
  • Samples 111 to 116 in Table 16 are rated as " ⁇ ".
  • the internal electrodes contain any of ( Ag0.7 , Pd0.3 ) TiO3 , NaTiO3 , and EuTiO3 as the ABO3 oxide.
  • the internal electrodes also contain a silver/palladium alloy as a conductive component.
  • the ionic radius of a silver/palladium alloy in 6-coordination is 1.06 ⁇ , as shown in the "(Ag,Pd)TiO 3 " section of Table 13.
  • the ionic radii in 6-coordination of the A-site elements of (Ag 0.7 ,Pd 0.3 )TiO 3 , NaTiO 3 and EuTiO 3 as ABO 3 oxides contained in the internal electrodes of Samples 111 to 116 are 1.06 ⁇ , 1.02 ⁇ and 1.17 ⁇ , respectively, as shown in Table 13.
  • the addition ratio of ( Ag0.7 , Pd0.3 ) TiO3 , NaTiO3 and EuTiO3 is not necessarily 100%, and if it is 10% or more, an effect of improving coverage was observed compared to the case where none of ( Ag0.7 , Pd0.3 ) TiO3 , NaTiO3 and EuTiO3 was included.
  • the "ionic radius ratio" was outside the range of 0.96 or more and 1.10 or less, and it is presumed that SrTiO 3 was expelled from the internal electrode portion, the heat resistance of the internal electrode was not improved, and the coverage was reduced.
  • Experimental Example 1 0.97 to 1.04
  • Experimental Example 2 0.96 to 1.04
  • Experimental Example 3 0.89 to 1.02
  • Experimental Example 4 0.96 to 1.10
  • the metal species constituting the conductive metal powder are different, for example, nickel in Experimental Example 1, copper in Experimental Example 2, silver in Experimental Example 3, and silver/palladium alloy in Experimental Example 4. However, even if the metal species are different, there is a common part in the range of the appropriate ionic radius ratio. This common part is defined as the scope of the present invention.
  • the present invention is characterized in that the powder is made of an ABO 3 type oxide, in which the ratio of the ionic radius of the A site element in ABO 3 in 6-coordination to the ionic radius of the metal contained in the conductive metal powder in 6-coordination is 0.97 or more and 1.02 or less.
  • the ABO 3 type oxide with a specific ionic radius may be any ABO 3 type oxide as long as the ratio of the ionic radius of the A site element in ABO 3 in 6-coordination to the ionic radius of the metal element contained in the conductive metal powder contained in the conductive paste in 6 -coordination is 0.97 or more and 1.02 or less.
  • a conductive paste for forming an internal electrode of a multilayer ceramic capacitor comprising a conductive metal powder, a ceramic powder, an organic solvent, and an organic binder, A conductive paste, wherein at least a portion of the ceramic powder is a powder made of an ABO3 type oxide having a specific ionic radius, in which the ratio of the ionic radius of an A site element in ABO3 in 6-coordination to the ionic radius of a metal contained in the conductive metal powder in 6 -coordination is 0.97 or more and 1.02 or less.
  • ⁇ 3> The conductive paste according to ⁇ 1> or ⁇ 2>, wherein the conductive metal powder contains one selected from nickel, copper, silver, and a silver/palladium alloy.
  • ⁇ 4> The conductive paste according to any one of ⁇ 1> to ⁇ 3>, wherein 10% by volume or more of the ceramic powder is a powder consisting of an ABO3 type oxide having the specific ionic radius, and the remainder of the ceramic powder is a powder mainly composed of at least one selected from BaTiO3 , SrTiO3 , and CaZrO3 .
  • a laminate including a plurality of laminated dielectric layers made of ceramic and a plurality of internal electrodes respectively disposed along a plurality of interfaces between the dielectric layers,
  • the internal electrodes include a conductive component and a ceramic component, and at least a portion of the ceramic component includes an ABO3 type oxide having a specific ionic radius, in which a ratio of an ionic radius of an A site element in ABO3 in 6 -coordination to an ionic radius of a metal included in the conductive component in 6-coordination is 0.97 or more and 1.02 or less.
  • Multilayer ceramic capacitor Multilayer ceramic capacitor.

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JPH0969467A (ja) * 1995-08-31 1997-03-11 Kyocera Corp 温度補償用積層セラミックコンデンサならびにその製造方法
JP2000232032A (ja) * 1999-02-10 2000-08-22 Tdk Corp 電極形成用ニッケル複合導体及び積層セラミックコンデンサ

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