WO2004052804A1 - 高強度低温焼成セラミック組成物及びその製造方法、並びにこれを用いた積層電子部品 - Google Patents
高強度低温焼成セラミック組成物及びその製造方法、並びにこれを用いた積層電子部品 Download PDFInfo
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- WO2004052804A1 WO2004052804A1 PCT/JP2003/015664 JP0315664W WO2004052804A1 WO 2004052804 A1 WO2004052804 A1 WO 2004052804A1 JP 0315664 W JP0315664 W JP 0315664W WO 2004052804 A1 WO2004052804 A1 WO 2004052804A1
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- WIPO (PCT)
- Prior art keywords
- sral
- temperature
- ceramic composition
- low
- hexagonal
- Prior art date
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- 239000000203 mixture Substances 0.000 title claims abstract description 111
- 239000000919 ceramic Substances 0.000 title claims abstract description 104
- 238000000034 method Methods 0.000 title description 5
- 239000013078 crystal Substances 0.000 claims abstract description 86
- 229910003668 SrAl Inorganic materials 0.000 claims description 105
- 238000010304 firing Methods 0.000 claims description 47
- IATRAKWUXMZMIY-UHFFFAOYSA-N strontium oxide Inorganic materials [O-2].[Sr+2] IATRAKWUXMZMIY-UHFFFAOYSA-N 0.000 claims description 25
- 239000010949 copper Substances 0.000 claims description 17
- 238000002441 X-ray diffraction Methods 0.000 claims description 16
- 229910052751 metal Inorganic materials 0.000 claims description 15
- 239000002184 metal Substances 0.000 claims description 15
- 229910052709 silver Inorganic materials 0.000 claims description 14
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims description 12
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 11
- 239000004332 silver Substances 0.000 claims description 11
- 229910052802 copper Inorganic materials 0.000 claims description 10
- 238000006243 chemical reaction Methods 0.000 claims description 9
- 229910052712 strontium Inorganic materials 0.000 claims description 9
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 7
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 7
- 239000004020 conductor Substances 0.000 claims description 7
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 7
- 229910052737 gold Inorganic materials 0.000 claims description 7
- 239000010931 gold Substances 0.000 claims description 7
- 239000012535 impurity Substances 0.000 claims description 7
- 238000002844 melting Methods 0.000 claims description 7
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 7
- 229910052814 silicon oxide Inorganic materials 0.000 claims description 7
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 6
- 229910052797 bismuth Inorganic materials 0.000 claims description 5
- 238000001354 calcination Methods 0.000 claims description 5
- 238000004519 manufacturing process Methods 0.000 claims description 5
- 230000008018 melting Effects 0.000 claims description 5
- 239000000956 alloy Substances 0.000 claims description 4
- 229910045601 alloy Inorganic materials 0.000 claims description 4
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 3
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims description 2
- 229910007266 Si2O Inorganic materials 0.000 claims 1
- 239000004744 fabric Substances 0.000 claims 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 abstract description 11
- 229910052593 corundum Inorganic materials 0.000 abstract 1
- 229910001845 yogo sapphire Inorganic materials 0.000 abstract 1
- 239000000843 powder Substances 0.000 description 46
- 238000005452 bending Methods 0.000 description 16
- 230000000694 effects Effects 0.000 description 11
- 239000002002 slurry Substances 0.000 description 11
- 239000002245 particle Substances 0.000 description 10
- 239000010936 titanium Substances 0.000 description 7
- 229910052710 silicon Inorganic materials 0.000 description 6
- 238000012360 testing method Methods 0.000 description 6
- 239000004372 Polyvinyl alcohol Substances 0.000 description 5
- 229910052782 aluminium Inorganic materials 0.000 description 5
- 239000007772 electrode material Substances 0.000 description 5
- 239000011521 glass Substances 0.000 description 5
- 229920002451 polyvinyl alcohol Polymers 0.000 description 5
- 238000005245 sintering Methods 0.000 description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- 229910052726 zirconium Inorganic materials 0.000 description 5
- 239000010433 feldspar Substances 0.000 description 4
- 229910052748 manganese Inorganic materials 0.000 description 4
- 150000002739 metals Chemical class 0.000 description 4
- 239000007921 spray Substances 0.000 description 4
- 239000000758 substrate Substances 0.000 description 4
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 3
- 229910010413 TiO 2 Inorganic materials 0.000 description 3
- 230000005540 biological transmission Effects 0.000 description 3
- 239000003990 capacitor Substances 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 238000009766 low-temperature sintering Methods 0.000 description 3
- 238000001556 precipitation Methods 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- -1 W and Mo Chemical class 0.000 description 2
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000002425 crystallisation Methods 0.000 description 2
- 230000008025 crystallization Effects 0.000 description 2
- 239000008187 granular material Substances 0.000 description 2
- 230000001771 impaired effect Effects 0.000 description 2
- 238000010030 laminating Methods 0.000 description 2
- 229910052750 molybdenum Inorganic materials 0.000 description 2
- 238000000465 moulding Methods 0.000 description 2
- 238000013001 point bending Methods 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 230000008054 signal transmission Effects 0.000 description 2
- 229910052721 tungsten Inorganic materials 0.000 description 2
- KYARBIJYVGJZLB-UHFFFAOYSA-N 7-amino-4-hydroxy-2-naphthalenesulfonic acid Chemical class OC1=CC(S(O)(=O)=O)=CC2=CC(N)=CC=C21 KYARBIJYVGJZLB-UHFFFAOYSA-N 0.000 description 1
- 229910015902 Bi 2 O 3 Inorganic materials 0.000 description 1
- GOJCZVPJCKEBQV-UHFFFAOYSA-N Butyl phthalyl butylglycolate Chemical compound CCCCOC(=O)COC(=O)C1=CC=CC=C1C(=O)OCCCC GOJCZVPJCKEBQV-UHFFFAOYSA-N 0.000 description 1
- 229910002483 Cu Ka Inorganic materials 0.000 description 1
- 239000004698 Polyethylene Substances 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
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- 229910052791 calcium Inorganic materials 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
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- 229910052804 chromium Inorganic materials 0.000 description 1
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- 238000001035 drying Methods 0.000 description 1
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- 238000001704 evaporation Methods 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 229910052733 gallium Inorganic materials 0.000 description 1
- 239000002241 glass-ceramic Substances 0.000 description 1
- 238000005469 granulation Methods 0.000 description 1
- 230000003179 granulation Effects 0.000 description 1
- 125000001475 halogen functional group Chemical group 0.000 description 1
- 230000017525 heat dissipation Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000003780 insertion Methods 0.000 description 1
- 230000037431 insertion Effects 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000011812 mixed powder Substances 0.000 description 1
- 239000012046 mixed solvent Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000010295 mobile communication Methods 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
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- 239000004014 plasticizer Substances 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 239000003870 refractory metal Substances 0.000 description 1
- 229910052654 sanidine Inorganic materials 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000005476 soldering Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 230000000007 visual effect Effects 0.000 description 1
- 229910052727 yttrium Inorganic materials 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C3/00—Glass compositions
- C03C3/04—Glass compositions containing silica
- C03C3/062—Glass compositions containing silica with less than 40% silica by weight
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/16—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on silicates other than clay
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- C04B35/195—Alkaline earth aluminosilicates, e.g. cordierite or anorthite
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- C04B35/6262—Milling of calcined, sintered clinker or ceramics
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- C04B2235/3481—Alkaline earth metal alumino-silicates other than clay, e.g. cordierite, beryl, micas such as margarite, plagioclase feldspars such as anorthite, zeolites such as chabazite
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- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
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- Y10T428/24802—Discontinuous or differential coating, impregnation or bond [e.g., artwork, printing, retouched photograph, etc.]
- Y10T428/24926—Discontinuous or differential coating, impregnation or bond [e.g., artwork, printing, retouched photograph, etc.] including ceramic, glass, porcelain or quartz layer
Definitions
- the present invention relates to a high-strength low-temperature sintering ceramic composition for a laminated circuit board, and particularly to a high-strength low-temperature sintering which has high mechanical strength and can be simultaneously sintered with an electrode made of a low melting point metal such as silver, gold, or copper.
- the present invention relates to a ceramic composition, a method for producing the same, and a laminated electronic component using the ceramic composition, which is mainly used for a mobile phone or the like. Background art
- the laminated circuit board had significantly poorer mechanical strength than the alumina substrate.
- the flexural strength of an alumina substrate is about 400 MPa
- the flexural strength of the above-mentioned laminated circuit board is about 150 MPa.
- the bending strength of the laminated circuit board was 150 MPa or more, but as electronic components used in mobile phones, etc. became thinner, the laminated circuit boards used in them also increased. 1 mm, the mechanical strength of conventional ceramic laminated circuit boards was insufficient.
- a laminated circuit board used for a mobile phone or the like is required to have high strength so that cracks and breakage do not occur, for example, due to deformation such as twisting or bending of the mounting board or impact when dropped.
- an object of the present invention is to provide a high-strength, low-temperature fired ceramic composition that can be simultaneously fired with a low-melting-point metal and can form a circuit board that is less likely to crack or break.
- Another object of the present invention is to provide a method for producing such a low temperature fired ceramic composition.
- Still another object of the present invention is to provide a laminated electronic component having a dielectric layer made of such a low-temperature fired ceramic composition. Disclosure of the invention
- the tissue of SrAl 2 Si 2 0 8 composition (a) has a slightly monoclinic SrAl 2 Si 2 O 8 in a temperature region of 950 ° C ⁇ 1050 ° C, mostly hexagonal SrAl a 2 Si 2 0 8 and unreacted A1 2 0 3 crystal ⁇ Pi SrSi0 3 crystal, (b) in the 1050 ° C ultra to 1100 ° C or less temperature region, the hexagonal SrAl 2 Si 2 O 8 is monoclinic crystal (b-axis) changes to SrAl 2 Si 2 0 8, ( c) not hexagonal SrAl 2 Si 2 O 8 in 1100 ° C greater, monoclinic SrAl 2 Si 2 0 8, A1 2 0 3 crystal ⁇ It
- SrAl 2 Si 2 0 becomes a 8 of bending strength of the stoichiometric composition 300 MPa or more, Si'Al 2 Si 2 0 in the tissue If the eight crystals are monoclinic, it will drop to about 150 MPa. Hexagonal SrAl 2 Si 2 0 8 and monoclinic SrAl 2 Si 2 O 8 It is not clear why there is a significant difference in mechanical strength, but it is the main crystal phase
- the high-strength low-temperature fired ceramic composition according to an embodiment of the present invention is characterized by having a hexagonal SrAl 2 Si 2 O 8 ⁇ Pi [alpha] 1 2 Omicron 3 crystals in the tissue.
- Second high-strength low-temperature fired ceramic composition includes the Al 2 0 3 -SiO 2 hexagonal base made mainly of -SrO SrAl 2 Si 2 0 8, to the base A1 2 0 It is characterized in that three crystal grains are precipitated.
- the base of the high strength low-temperature-sintered ceramic composition in (a) an amorphous phase consists force ⁇ (b) substantially SrAl 2 Si 2 0 8 crystal hexagonal SrAl2Si 2 0 8 therein is precipitated, at least a portion of is preferably hexagonal SrAl2Si 2 0 8.
- the base may comprise a monoclinic Si'Al 2 Si 2 O 8.
- the tissue SrAl 2 Si 2 0 8 has a crystal ⁇ Pi A1 2 0 3 crystal
- the SrAl 2 Si 2 0 8 crystal hexagonal SrAl consists 2 Si 2 O 8 alone or hexagonal SrAl 2 Si 2 0 8 ⁇ Pi monoclinic SrAl 2 Si 2 0 8, in X-ray diffraction measurement using CirKa line
- the hexagonal SrAl 2 Si 2 O 8 (101 ) surface 1 101 peak intensity of, when a monoclinic SrAl 2 Si 2 O 8 in (002) 1 peak intensity of plane 002, ⁇ / ( ⁇ + Ioo2 ) peak intensity ratio represented by x 100 5 % Or more.
- the peak intensity ratio is preferably at least 10%, more preferably at least 50%.
- High strength low-temperature fired ceramic compositions of the present invention includes a base consisting essentially of SrAl 2 Si 2 0 8 crystal, the structure having a A1 2 0 3 grains to the base, the SrAl2Si 2 O 8 crystal hexagonal SrAl 2 Si 2 0 8 alone or hexagonal Si'Al 2 Si 2 O 8 ⁇ Pi monoclinic SrAl 2 Si 2 O 8 or Rannahli, the SrAl 2 Si 2 0 8 wherein the crystalline hexagonal SrAl 2 the ratio of Si 2 0 8 is more than 60%, and preferably has a flexural strength of at least 400 MPa.
- CoO terms Co and K and 0.1 to 5% by weight of (0 conversion) (CoO terms)
- Cu of 0.01 to 5 wt% (CuO basis) 0.01 to 5 mass% (Mn0 2 And (c) unavoidable impurities and at least one element selected from the group consisting of Mn, 0.01-5 mass 0 / o Ag and 0.01-2 mass% (ZrO 2 conversion) Zr.
- Preferred second composition of the high strength low-temperature-sintered ceramic composition of the present invention Si of (a) Al of 10 to 60 weight 0/0 ( ⁇ 1 2 ⁇ 3 equivalent), 25 to 60 wt% (SiO 2 conversion) , 7.5-50 mass. /.
- the A1 2 0 3 average crystal grain size of the crystal grains is preferably not more than 1 ⁇ .
- the method for producing the high-strength low-temperature fired ceramic composition comprises: a ceramic molding using aluminum oxide, silicon oxide and strontium oxide, or aluminum oxide, silicon oxide, strontium oxide and titanium oxide as main raw materials.
- SrAl 2 Si 2 O 8 crystal formed in the ceramic tissue to set the temperature ⁇ Pi time such that the ratio of the hexagonal SrAl 2 Si 2 0 8 becomes 5% or more Features.
- Baking temperature ⁇ Pi time is preferably the ratio of the hexagonal SrAl2Si 2 0 8 is by Uni setting of 10% or more, more preferably be set such that 50% or more, so that more than 60% Especially preferred to set! / ,.
- the laminated electronic component according to the present invention is obtained by laminating a plurality of dielectric layers made of the high-strength low-temperature fired ceramic composition, wherein each of the dielectric layers has a conductor made of a low melting point metal. It is characterized in that a pattern is formed.
- the low melting point metal is preferably silver, copper, gold or an alloy thereof.
- the conductor pattern preferably forms an inductance element and / or a capacitance element. It is preferable that at least one selected from the group consisting of an inductance element, a capacitance element, a switching element, and a filter element is mounted on the multilayer electronic component.
- FIG. 1 is a graph showing an X-ray diffraction pattern of a low-temperature fired ceramic composition (sample 8) according to one embodiment of the present invention.
- FIG. 2 is a graph showing an X-ray diffraction pattern of a low-temperature fired ceramic composition (sample 12) according to another example of the present invention.
- FIG. 3 is a graph showing an X-ray diffraction pattern of a low-temperature fired ceramic composition (sample 13) according to another example of the present invention.
- FIG. 4 is a graph showing the X-ray diffraction pattern of the low-temperature fired ceramic composition (Sample 14) which is outside the scope of the present invention.
- FIG. 5 is a transmission electron microscope (TEM) photograph of the low-temperature fired ceramic composition of one example of the present invention
- FIG. 6 is a schematic diagram showing a structure corresponding to the TEM photograph of FIG. 5,
- FIG. 7 is a graph showing the relationship between firing temperature and bending strength for various low-temperature fired ceramic compositions in Example 2.
- FIG. 8 is a graph showing the relationship between the holding time at the firing temperature and the transverse rupture strength for various low-temperature fired ceramic compositions in Example 2.
- FIG. 9 is an exploded perspective view showing the multilayer circuit board of Example 4,
- FIG. 10 is a perspective view showing a laminated electronic component of Example 4.
- FIG. 11 is a diagram showing an equivalent circuit of the multilayer electronic component of the fourth embodiment. BEST MODE FOR CARRYING OUT THE INVENTION
- the main component of the high-strength low-temperature fired ceramic composition of the present invention is Al, Si and Sr, or Al, Si, and Sr, and, 1050 ° C or less, preferably calcined at a temperature below 1000 ° C, at least hexagonal SrAl 2 Si 2 08 ⁇ Pi A1 2 0 3 grains in the structure.
- An internal electrode made of a low-melting-point metal (silver, copper, gold, or an alloy thereof) having high conductivity is formed on a dielectric layer made of such a low-temperature fired ceramic composition.
- A1 is preferably 10 to 60 wt% in A1 2 0 3 in terms
- Si is preferably a 25 to 60% by weight Si0 2 in terms
- Sr is 7.5 to 50 mass at Si'O terms. / 0 is preferable. If the content of these metals is out of these ranges, the low-temperature fired ceramic composition becomes porous because low-temperature fired at a low temperature of 1000 ° C or less does not provide a sufficient fired density. No characteristics can be obtained.
- Ti has the effect of increasing f as a function of the temperature coefficient of the resonant frequency of the low temperature fired ceramic composition.
- Ti is preferably 0 to 20 mass% in the Ti0 2 terms.
- the temperature coefficient of the resonance frequency of the low-temperature fired ceramic composition increases. If the temperature coefficient of the resonance frequency of the low-temperature fired ceramic composition is on the minus side of f force -40 ppm / ° C, f content can be easily adjusted to 0 ppm / ° C by increasing the Ti content. be able to.
- the low-temperature fired ceramic composition further includes, as subcomponents, at least one selected from the group consisting of Bi, Na, K, and Co, and at least one selected from the group consisting of Cu, Mn, Ag, and Zr. It is preferable to include one kind. Unless otherwise specified, the amount of these metals added is the total of 100% of the main components. /. Is shown as an oxide conversion value. These metals are preferably added in the form of acid or carbonate.
- Bi is 0.1 in terms of Bi 2 O 3: preferably in the L0 mass 0/0. If Bi is higher by 10% by mass, the Q value becomes smaller. The more preferable addition amount of Bi is 5% by mass or less. If the amount of Bi is less than 0.1% by mass, the effect of lowering the firing temperature is insufficient. A more preferable addition amount of Bi is 0.2% by mass or more.
- Na is preferably 0.1 to 5% by mass in terms of Na 20 . 0.1 mass of Na. If it is less than / 0, the effect of lowering the firing temperature is insufficient. On the other hand, if Na exceeds 5% by mass, the resulting low-temperature fired ceramic composition will have too large a dielectric loss, and will not be practical.
- K is preferably 0.1 to 5% by mass in terms of K 20 .
- ⁇ is less than 0.1% by mass, the effect of lowering the firing temperature is insufficient.
- ⁇ exceeds 5% by mass, the resulting low-temperature fired ceramic composition will have too large a dielectric loss, and will not be practical.
- Na and K form feldspars such as NaAlSi 3 O 8 crystal and KAlSi 3 O 8 crystal together with A1 and Si, and improve the fQ of the low-temperature fired ceramic composition.
- Co is preferably 0.1 to 5% by mass in terms of CoO.
- Co is less than 0.1% by mass, the effect of lowering the firing temperature is insufficient, and it is difficult to obtain a dense low-temperature fired ceramic composition by firing at 900 ° C or lower.
- Co exceeds 5% by mass, the crystallization temperature of the low-temperature fired ceramic composition exceeds 1000 ° C, and if it is lower than 1000 ° C, the dielectric loss becomes too large, and the practicality is lost.
- Cu, Mn, Ag and Zr mainly have an effect of promoting crystallization of the dielectric ceramic composition in the firing step, and are added to achieve low-temperature firing.
- Cu is preferably 0.01 to 5% by mass in terms of CuO.
- Cu is 0.01 mass 0 /. If it is less than 0.5, the effect of the addition is small, and it is difficult to obtain a low-temperature fired ceramic composition having a high Q value by firing at 900 ° C or less. Further, if Cu is more than 5 mass 0/0, the low temperature sintering property is impaired.
- Mn is preferably 0.01 to 5 mass 0/0 MnO 2 basis. When Mn is less than 0.01% by mass, the effect of the addition is small, and it is difficult to obtain a low-temperature fired ceramic composition having a high Q value by firing at 900 ° C or less. On the other hand, if Mn exceeds 5% by mass, the low-temperature firing property is impaired.
- Ag is preferably set to 0.01 to 5% by mass. If Ag exceeds 5% by mass, the dielectric loss becomes too large, making it impractical.
- the more preferable addition amount of Ag is 2% by mass or less.
- Zr is preferably 0.01 to 2 % by mass in terms of ZrO 2 .
- Zr is less than 0.01% by mass, the effect of improving the mechanical strength of the low-temperature fired ceramic composition is insufficient, and when it exceeds 2% by mass, the content decreases.
- 0.3 mass is required in order to further expect the effect of improving the mechanical strength by adding ZrO 2 . /. More preferably, it is set to 1.5 mass%.
- Inevitable impurities include, for example, Y, Fe, Ca, Ga, Cr and the like. The content of unavoidable impurities must be within a range that does not deteriorate the properties of the low-temperature fired ceramic composition.
- the low-temperature fired ceramic composition comprises aluminum oxide, silicon oxide and strontium oxide (or aluminum oxide, or aluminum oxide) which are the main components consisting of Al, Si and Sr (or Al, Si, Sr and Ti).
- the low-temperature fired ceramic composition preferably has a flexural strength of 300 MPa or more, and more preferably 400 MPa or more, so that the firing temperature and time are adjusted to satisfy this condition. I prefer to do that.
- Peak of the hexagonal SrAl 2 Si 2 0 8 There is a correlation between the peak intensity ratio and the bending strength. Generally, the higher the peak strength ratio, the higher the bending strength. Therefore, it is preferable to adjust the firing temperature and the baking time so as to have a peak intensity ratio of 50% or more and a bending strength of 300 MPa or more. It is more preferable to adjust the sintering temperature and time so as to have.
- the optimal firing temperature and time will generally depend on the composition of the low temperature fired ceramic composition. Therefore, in order to ensure that each low-temperature fired ceramic composition has a high peak strength ratio and high flexural strength, it is necessary to experimentally determine the optimum firing temperature and time according to the fiber composition. .
- the firing temperature is preferably 1000 ° C or lower, more preferably 950 ° C or lower, and particularly preferably 900 ° C or lower.
- the firing time is preferably about 2 to 4 hours.
- the low-temperature fired ceramic composition of the present invention obtained by such a method further has a relative dielectric constant ⁇ of about 6 to 9 and a practical fQ of 3000 GHz (3 THz) or more (where f is the resonance frequency). It is preferred to have
- the laminated electronic component of the present invention has a conductor pattern formed of a low-melting-point metal (silver, copper, gold or an alloy thereof) formed on each dielectric layer made of the low-temperature fired ceramic composition. It is obtained by laminating a plurality of dielectric layers.
- the conductor pattern itself may be a known one, and constitutes, for example, an inductance * element and a z or capacitance element. At least one of an inductance element, a capacitance element, a switching element, and a filter element may be mounted on the multilayer electronic component.
- the layer configuration itself of the laminated electronic component may be a known one.
- Example 1 The present invention will be described in more detail with reference to the following examples, but the present invention is not limited thereto.
- Example 1
- A1 2 0 3 powder, SiO 2 powder, Si'C0 3 powder, TiO 2 powder, Bi 2 0 3 powder, CuO powder, Mn0 2 powder, a Na 2 CO 3 powder and K 2 CO 3 powder with pure water The mixture was mixed with a ball mill to obtain a slurry. After adding PVA to the slurry at a ratio of 1% by mass relative to the dry weight of the raw material powder, the slurry is dried with a spray drier to obtain a granular dry powder having an average particle size of about 0.1 mm. Powder was obtained.
- the resulting slurry was dried by heating and then crushed with a raikai machine.
- the obtained mixed powder was placed in ⁇ Lumina crucible and was calcined for 2 hours at 850 ° C, and the Ke I acid salt-based glass powder containing [alpha] 1 2 Omicron 3 crystals.
- the calcined powder was wet-pulverized by the above-mentioned ball mill for 40 hours and then dried. A part of the obtained dried calcined powder was put into a ball mill together with pure water and pulverized to an average particle size of 1.0 ⁇ . Polyvinyl alcohol (PVA) was added to the slurry containing the obtained milled powder at a ratio of 1.5% by weight to 100% by weight of powdered ore powder, and then granulated and dried using a spray dryer to obtain an average particle size. Of about 0.1 mm was obtained.
- PVA Polyvinyl alcohol
- the granulated powder was pressed under a pressure of 200 MPa to obtain a columnar compact.
- the molded body is heated in the air from room temperature to a temperature of 950 to 1200 ° C. at a rate of 200 ° C./hr, kept at the above temperature for 2 hours and fired, and then heated to a room temperature at a rate of 200 ° C./hr. Cool.
- the relative permittivity ⁇ of the obtained fired body was determined at a resonance frequency of 8 to 15 GHz using a cylindrical resonator.
- the crystal state of the sample was confirmed by X-ray diffraction using Cu-Ka line.
- a 3-point bending test (JIS C2141) was performed on a 38 mm X 12 mm XI mm test piece prepared in the same manner as above, with the fulcrum distance set to 30 mm and the load speed set to 0.5 mm / min.
- the bending strength (flexural strength) was determined from the maximum load at the time of failure. Table 1 shows the results. Table 1 also shows the data of alumina.
- S SrSiO 3 crystal.
- the tissue of the low-temperature fired ceramic composition obtained by the baking temperature of 950 ° C ⁇ 1050 ° C, SrAl 2 Si20 8 crystals, [alpha] 1 2 Omicron 3 there are crystal and SrSi0 3 crystals I do.
- A1 2 0 3 crystal ⁇ Pi SrSiO 3 crystal is a crystal has failed to reach a SrAl 2 Si 2 O 8 crystal.
- the SrAl 2 Si 2 O 8 crystals were almost entirely hexagonal. Temperature fired ceramic substantially hexagonal SrAl2Si 2 0 8, compositions exhibit flexural strength of at least 300 MPa, also 6.8 relative dielectric constant ⁇ and 14 of 8.0; 15 and fQ of THz excellent dielectric properties Indicated.
- the tissue of the resulting low-temperature fired ceramic composition is Lord SrAl 2 Si 2 0 8 crystals do not precipitate A1 2 0 3 crystal and glass phases, flexural strength ⁇ Both dielectric properties were inferior.
- A1 2 0 3 powder, Si0 2 powder, SrCO 3 powder, Ti0 2 powder, Bi 2 0 3 powder, CuO powder, Mn0 2 powder powder, dispersing the Na 2 C0 3 powder and K 2 C0 3 powder with pure water And a slurry was obtained.
- PVA was added to this slurry at a rate of 1% by mass relative to the dry weight of the raw material powder, and then dried with a spray drier to obtain a granular dry powder having an average particle size of about 0.1 mm.
- the granulate powder was calcined for 2 hours at a maximum temperature of 800 ° C in a continuous furnace to obtain a calcined powder consisting of A1 2 0 3 crystal and Ti0 2 binding Kei acid salt-based glass containing crystal.
- the composition of the calcined powder in terms of oxide, of 49% by weight A1 2 0 3, 34 wt% of Si0 2, 8.2 wt% of SrO, 3 wt% of TiO 2, 2.5.
- a cylindrical molded body was obtained in the same manner as in Example 1.
- the molded body is heated in the air from room temperature to a temperature of 825 to 900 ° C. at a rate of 200 ° C./hr, kept at the above temperature for 2 hours and fired, and then heated to a room temperature at a rate of 200 ° C./hr. Cool.
- the relative permittivity ⁇ of the obtained fired body was determined at a resonance frequency of 8 to L5 GHz using a cylindrical resonator.
- a three-point bending test was performed on each test piece in the same manner as in Example 1, and the bending strength (flexural strength) was determined from the maximum load when the test piece broke.
- Table 2 shows the results.
- Table 2 also shows the data for alumina.
- N (Na, K) SisA10 8 crystals.
- Figures 1 to 4 show the low-temperature fired ceramic compositions fired at 850 ° CX 2 hr, 860 ° CX 2 hr, 875 ° CX 2 hr and 900 ° CX 2 hr, respectively (corresponding to samples 8, 12 to 14).
- the X-ray diffraction intensity pattern by Cu- ⁇ -ray is shown.
- ⁇ indicates A1 2 0 3 crystals
- ⁇ denotes a six-cubic SrAl 2 Si 2 0 8
- ⁇ indicates a monoclinic SrAl 2 Si 2 0 8.
- the peak intensity ratio represented by ⁇ ⁇ ⁇ ⁇ + ⁇ 2) ⁇ 100 (indicating the ratio of hexagonal SrAl 2 Si 2 O 8 in the structure) is 7.7%. This indicates that a bending strength of 300 MPa or more can be obtained.
- the peak intensity ratio indicating a ratio of the hexagonal SrAl 2 Si 2 0 8 in the tissue is preferably 5% or more.
- Sample 6-14, the SrSi0 3 crystal was confirmed in Example 1 was One or a observed in the tissue, containing Na ⁇ Pi Z or K considered sample 11, 13 ⁇ Pi 14 in sanidine and Time Kei Salt crystals (feldspar) were identified. Samples 11, 13 and 14 show excellent fQ, which may be due to feldspar.
- hexagonal proportion of SrAl 2 Si 2 0 8 in tissues varies in accordance with the composition and sintering conditions of the low-temperature fired ceramic composition (baking temperature ⁇ Pi time), adjusting the composition and baked formation conditions This makes it possible to easily control the ratio of hexagonal SrAl 2 Si 2 O 8 in the structure.
- FIG. 5 is a transmission electron microscope (TEM) photograph of the polished surface of sample 13 (875 ° C. for 2 hours), and FIG. 6 is a schematic diagram of the TEM photograph of FIG.
- TEM transmission electron microscope
- composition analysis revealed that the base of this organization was mainly composed of Al 2 O 3 , SiO 2 and SrO. Diffraction spots are observed in the selected area diffraction at this base. Although the grain boundaries are not clear, it is considered that they have crystallized. That is, the sample
- LTCC composition 13 is found to have a A1 2 0 3, Si0 2 and oxide grains are precipitated structure crystallized base mainly composed of SrO. This result is consistent with X-ray diffraction pattern monoclinic SrAl 2 Si 2 0 8 ⁇ Pi hexagonal SrAl 2 Si 2 0 8 in FIG. 3 is present.
- the average crystal grain size of the precipitated A1 2 0 3 crystals in the structure is not more than 1 Myuiotaita, tendency to growth proceeds of [alpha] 1 2 0 3 grains even firing temperature is changed in such seen cut Was.
- FIG. 7 shows the relationship between the firing temperature and the bending strength when the firing time is 2 hours.
- the flexural strength is the average of 10 samples.
- the transverse rupture strength becomes 300 MPa or more when the firing temperature is about 830 ° C, and becomes 400 MPa or more at about 840 to 870 ° C, but the firing temperature rises. It can be seen that the temperature drops rapidly as the temperature rises, and becomes less than 300 MPa when the temperature exceeds approximately 880 ° C.
- Figure 8 shows the relationship between holding time and bending strength when the firing temperature is 850 ° C.
- the flexural strength is the average of 10 samples. It can be seen that in the low-temperature fired ceramic composition of Example 2, even if the firing temperature is appropriate at 850 ° C, the transverse rupture strength is rather lowered when the holding time is too long. From FIG. 8, it can be seen that in the case of Example 2, a firing time of about 2 to 4 hours at a firing temperature of 850 ° C. is preferable for obtaining a transverse rupture strength of 400 MPa or more.
- the hexagonal crystal structure is set to 900 ° C or lower. Since SrAl 2 Si 2 08 there is a temperature region where precipitation, it is possible to obtain a low-temperature fired ceramic composition having a high strength by Rukoto optimize the calcination temperature depending on the composition.
- Example 3
- Example 2 In the same manner as in Example 1, A1 2 0 3 48.7% on a weight basis 34.5% of the SiO 2, 9.5 percent of SrO, 4% of the Ti0 2, 1 percent of Bi 2 0 3, 1% of the Na 2 0 , 0.5% K 20 , 0.3% CuO, and 0.5% MnO 2 were prepared.
- the calcined powder was wet-pulverized with the same pole mill as in Example 1 for 40 hours and dried. Next, a part of the calcined powder was put into a pole mill together with pure water and pulverized to an average particle size of 1.0 ⁇ .
- N (Na, K) Si3A10 8 crystals.
- Bi by reducing the amount of ⁇ Pi Na, precipitation temperature comparison slightly SrAl 2 Si 2 0 8 crystals as in Example 2 was increased. And power, and, found that 875 ° C ⁇ 925 ° and precipitated hexagonal SrAl 2 Si 2 0 8 is at a temperature and C, and a range of precipitation temperature of the hexagonal SrAl 2 Si 2 0 8 extends Was.
- the set formed of the low-temperature fired ceramic composition can control the deposition temperature and the scope of the hexagonal SrAl 2 Si 2 0 8.
- silicate crystals containing Na and K were precipitated, and high bending strength, high resilience and dielectric properties were simultaneously obtained.
- a diode switch switching the connection of an antenna-side circuit, a reception-side circuit, and a transmission-side circuit used in a high-frequency circuit section of a mobile phone is described below. It was prepared as follows.
- Example 2 First, in the same manner as in Example 2, ⁇ 1 2 ⁇ 3 of 49% by weight, 34% of Si0 2, 8.2% of the SrO, 3 percent Ti0 2, 2.5% of the Bi 2 0 3, 2% of the Na A calcined powder consisting of 2 O, 0.5% of 0, 0.3% CuO, and 0.5% of MnO 2 was prepared.
- This calcined powder was dispersed in a mixed solvent of ethanol and butanol, and pulverized with a Paul mill to an average particle size of 1.0 ⁇ m .
- polybutyral as a binder and butyl phthalyl butyl glycolate as a plasticizer were dispersed at a ratio of 15% by mass and 7.5% by mass, respectively, with respect to 100% by mass of the calcined powder.
- a slurry for sheet molding was used. After defoaming and partially evaporating the solvent under reduced pressure to reduce the viscosity of this slurry to about 10,000 MPa's, it is sheet-formed with a doctor blade and has a dry thickness of about 80 ⁇ . Was obtained.
- This ceramic green sheet has a predetermined size for handling in the post-process. Cut into pieces.
- the wiring patterns Ll-1, Ll-2, L2-1, L2'2, the duland electrode pattern GND, and the switching element, which constitute a transmission line (inductance element) with silver paste on the surface of a plurality of ceramic green sheets, are made of silver paste.
- the electrode pattern for mounting was printed (see Fig. 9).
- Via holes filled with silver paste are formed in the ceramic green sheet as means for connecting wiring patterns between the layers.
- the ceramic green sheets on which the conductive patterns were printed were aligned, laminated with high precision, and then crimped.
- the crimping conditions were a pressure of 14 MPa, a temperature of 85 ° C, and a holding time of 10 minutes.
- the obtained laminate was cut into chip sizes, it was placed on a firing setter and debinding and firing were performed in a continuous furnace to obtain a 4.5 mm X 3.2 mm X 1.0 mm fired body.
- the calcination was performed by holding at 875 ° C. for 2 hours in an air atmosphere.
- the ceramic portion of the sintered body was crushed was measured X-ray diffraction, the hexagonal SrAl 2 Si 2 O 8 in tissue, monoclinic SrAl 2 Si 2 0 8, A1 2 0 3 crystal, TiO 2 crystals, It was confirmed that silicate crystals were obtained. Peak intensity ratio of SrAl 2 Si 2 0 8 hexagonal SrAl 2 Si 2 0 8 to the total crystal was 15.5%.
- terminal electrodes GND, TX, RX, and VC1 were electrically connected to the electrode pattern for mounting the switching element.
- Diodes Dl and D2 were mounted as switching elements on the mounting electrode pattern of the multilayer circuit board thus obtained, and a multilayer electronic component 1 shown in FIG. 10 was produced.
- the multilayer electronic component 1 constitutes a broken line portion of the equivalent circuit shown in FIG.
- the inductance element is configured by the electrode pattern, but a chip inductor, a coil, and the like may be mounted.
- a capacitor element for blocking a DC component may be formed on a circuit board with an electrode pattern, or may be mounted on the circuit board as a chip capacitor.
- a filter element such as a low-pass filter or a band-pass filter is connected to the diode switch.
- the element may be configured with a SAW filter and mounted on a circuit board.
- a filter element composed of an inductance element and a capacitance element may be formed in an electrode pattern on a circuit board, or may be mounted as a chip component on the circuit board.
- the conductor pattern of the low-melting-point metal is formed on the dielectric layer made of the low-temperature-fired ceramic composition of the present invention. It can be seen that the formation of a multilayer electronic component with excellent electrical characteristics and mechanical strength can be obtained.
- LTCC compositions of the present invention has a hexagonal SrAl 2 Si 2 0 8 in tissue, practical have dielectric properties, and firing possible at low temperatures below 1000 ° C with high strength It is. Therefore, simultaneous firing with low melting point electrode materials such as silver, gold, and copper is possible.
- the high-strength low-temperature fired ceramic composition of the present invention not only has excellent dielectric properties such as dielectric constant and fQ, but also has improved mechanical strength as compared with conventional ones. Simultaneous firing with metal is possible, and cracks and breakage hardly occur. Therefore, the laminated electronic component using the high-strength low-temperature fired ceramic composition of the present invention has excellent electrical properties and mechanical strength.
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Abstract
Description
Claims
Priority Applications (2)
Application Number | Priority Date | Filing Date | Title |
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EP03777345.4A EP1568668B1 (en) | 2002-12-06 | 2003-12-08 | Ceramic composition being fired at low temperature and having high strength and method for preparing the same, and laminated electronic parts using the same |
US10/537,461 US7285507B2 (en) | 2002-12-06 | 2003-12-08 | Ceramic composition being fired at low temperature and having high strength and method for preparing the same, and laminated electronic parts using the same |
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JP2002-354955 | 2002-12-06 | ||
JP2002354955 | 2002-12-06 |
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WO2004052804A1 true WO2004052804A1 (ja) | 2004-06-24 |
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PCT/JP2003/015664 WO2004052804A1 (ja) | 2002-12-06 | 2003-12-08 | 高強度低温焼成セラミック組成物及びその製造方法、並びにこれを用いた積層電子部品 |
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US (1) | US7285507B2 (ja) |
EP (1) | EP1568668B1 (ja) |
CN (1) | CN100475738C (ja) |
WO (1) | WO2004052804A1 (ja) |
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US8124047B2 (en) * | 2006-12-22 | 2012-02-28 | Ngk Insulators, Ltd. | Method for manufacturing (Li, Na, K)(Nb, Ta)O3 type piezoelectric material |
US7867932B2 (en) * | 2007-08-28 | 2011-01-11 | Corning Incorporated | Refractory glass ceramics |
US8247337B2 (en) * | 2007-11-28 | 2012-08-21 | Kyocera Corporation | Alumina sintered article |
CN102365249B (zh) | 2009-03-26 | 2014-06-04 | 日立金属株式会社 | 介电陶瓷组合物、多层介电基板、电子部件和介电陶瓷组合物的制备方法 |
CN101656335B (zh) * | 2009-09-22 | 2013-01-30 | 南京国博电子有限公司 | 非对称式的超大功率射频开关模块及其制备方法 |
US9050456B2 (en) * | 2011-07-21 | 2015-06-09 | Biotronik Se & Co. Kg | Unipolar multipurpose electrode line and stimulation and defibrillation assembly |
FR2983473A1 (fr) * | 2011-12-01 | 2013-06-07 | Centre Nat Rech Scient | Verres, vitroceramiques et ceramiques d'aluminates transparents |
KR101931108B1 (ko) * | 2014-07-09 | 2018-12-20 | 페로 코포레이션 | 미드-k ltcc 조성물 및 디바이스 |
US10696596B2 (en) | 2015-12-28 | 2020-06-30 | Hitachi Metals, Ltd. | Method for producing dielectric ceramic, and dielectric ceramic |
JP6728859B2 (ja) * | 2016-03-25 | 2020-07-22 | 日立金属株式会社 | セラミック基板およびその製造方法 |
CN116924774A (zh) * | 2022-04-02 | 2023-10-24 | 中国科学院上海硅酸盐研究所 | 一种高强度低介复合微波介质陶瓷材料及其制备方法 |
Citations (2)
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JPH06199541A (ja) * | 1993-01-05 | 1994-07-19 | Matsushita Electric Ind Co Ltd | ガラスセラミックス組成物 |
JP2000272960A (ja) * | 1999-01-20 | 2000-10-03 | Hitachi Metals Ltd | マイクロ波用誘電体磁器組成物およびその製造方法ならびにマイクロ波用誘電体磁器組成物を用いたマイクロ波用電子部品 |
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JP3297569B2 (ja) * | 1995-10-30 | 2002-07-02 | 京セラ株式会社 | 低温焼成磁器組成物 |
JP3761289B2 (ja) * | 1996-09-26 | 2006-03-29 | 日本特殊陶業株式会社 | 誘電体材料及びその製造方法並びにそれを用いた回路基板及び多層回路基板 |
US6201307B1 (en) * | 1998-06-23 | 2001-03-13 | Kyocera Corporation | Ceramics for wiring boards and method of producing the same |
JP4748435B2 (ja) * | 2001-08-21 | 2011-08-17 | 日本電気硝子株式会社 | 積層ガラスセラミック材料及び積層ガラスセラミック焼結体 |
-
2003
- 2003-12-08 CN CNB2003801050633A patent/CN100475738C/zh not_active Expired - Lifetime
- 2003-12-08 WO PCT/JP2003/015664 patent/WO2004052804A1/ja active Application Filing
- 2003-12-08 US US10/537,461 patent/US7285507B2/en not_active Expired - Lifetime
- 2003-12-08 EP EP03777345.4A patent/EP1568668B1/en not_active Expired - Lifetime
Patent Citations (2)
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JPH06199541A (ja) * | 1993-01-05 | 1994-07-19 | Matsushita Electric Ind Co Ltd | ガラスセラミックス組成物 |
JP2000272960A (ja) * | 1999-01-20 | 2000-10-03 | Hitachi Metals Ltd | マイクロ波用誘電体磁器組成物およびその製造方法ならびにマイクロ波用誘電体磁器組成物を用いたマイクロ波用電子部品 |
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See also references of EP1568668A4 * |
Also Published As
Publication number | Publication date |
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EP1568668A1 (en) | 2005-08-31 |
CN1720205A (zh) | 2006-01-11 |
CN100475738C (zh) | 2009-04-08 |
US20060100087A1 (en) | 2006-05-11 |
EP1568668A4 (en) | 2008-12-10 |
EP1568668B1 (en) | 2013-04-24 |
US7285507B2 (en) | 2007-10-23 |
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