WO2006132086A1 - 誘電体セラミック、及び積層セラミックコンデンサ - Google Patents
誘電体セラミック、及び積層セラミックコンデンサ Download PDFInfo
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- WO2006132086A1 WO2006132086A1 PCT/JP2006/310321 JP2006310321W WO2006132086A1 WO 2006132086 A1 WO2006132086 A1 WO 2006132086A1 JP 2006310321 W JP2006310321 W JP 2006310321W WO 2006132086 A1 WO2006132086 A1 WO 2006132086A1
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- ceramic
- dielectric
- capacitance
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- 239000000919 ceramic Substances 0.000 title claims abstract description 90
- 239000003985 ceramic capacitor Substances 0.000 title claims abstract description 43
- 239000002245 particle Substances 0.000 claims abstract description 54
- 229910052749 magnesium Inorganic materials 0.000 claims abstract description 5
- 229910052692 Dysprosium Inorganic materials 0.000 claims description 4
- 229910052691 Erbium Inorganic materials 0.000 claims description 4
- 229910052688 Gadolinium Inorganic materials 0.000 claims description 4
- 229910052775 Thulium Inorganic materials 0.000 claims description 4
- 229910052769 Ytterbium Inorganic materials 0.000 claims description 4
- 229910052804 chromium Inorganic materials 0.000 claims description 4
- 229910052748 manganese Inorganic materials 0.000 claims description 4
- 229910052750 molybdenum Inorganic materials 0.000 claims description 4
- 238000005245 sintering Methods 0.000 claims description 4
- 229910052720 vanadium Inorganic materials 0.000 claims description 4
- 229910052727 yttrium Inorganic materials 0.000 claims description 4
- 229910052684 Cerium Inorganic materials 0.000 claims description 3
- 229910052693 Europium Inorganic materials 0.000 claims description 3
- 229910052689 Holmium Inorganic materials 0.000 claims description 3
- 229910052765 Lutetium Inorganic materials 0.000 claims description 3
- 229910052779 Neodymium Inorganic materials 0.000 claims description 3
- 229910052777 Praseodymium Inorganic materials 0.000 claims description 3
- 229910052772 Samarium Inorganic materials 0.000 claims description 3
- 229910052771 Terbium Inorganic materials 0.000 claims description 3
- 229910052782 aluminium Inorganic materials 0.000 claims description 3
- 229910052721 tungsten Inorganic materials 0.000 claims description 3
- 229910052761 rare earth metal Inorganic materials 0.000 abstract description 25
- 150000001875 compounds Chemical class 0.000 abstract description 18
- 229910052751 metal Inorganic materials 0.000 abstract description 13
- 239000002184 metal Substances 0.000 abstract description 11
- 239000000523 sample Substances 0.000 description 60
- 239000010949 copper Substances 0.000 description 47
- 239000012071 phase Substances 0.000 description 33
- 239000000843 powder Substances 0.000 description 29
- 239000010410 layer Substances 0.000 description 24
- 238000000034 method Methods 0.000 description 22
- 239000002994 raw material Substances 0.000 description 22
- 239000000203 mixture Substances 0.000 description 19
- 230000015556 catabolic process Effects 0.000 description 15
- 239000013078 crystal Substances 0.000 description 13
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 13
- 238000012360 testing method Methods 0.000 description 12
- 230000002829 reductive effect Effects 0.000 description 11
- 230000002950 deficient Effects 0.000 description 9
- 239000006104 solid solution Substances 0.000 description 9
- 238000010304 firing Methods 0.000 description 8
- 238000004458 analytical method Methods 0.000 description 7
- JRPBQTZRNDNNOP-UHFFFAOYSA-N barium titanate Chemical compound [Ba+2].[Ba+2].[O-][Ti]([O-])([O-])[O-] JRPBQTZRNDNNOP-UHFFFAOYSA-N 0.000 description 7
- 229910002113 barium titanate Inorganic materials 0.000 description 7
- 229910052802 copper Inorganic materials 0.000 description 7
- 230000007423 decrease Effects 0.000 description 7
- 229910052759 nickel Inorganic materials 0.000 description 7
- 230000007547 defect Effects 0.000 description 6
- 230000001771 impaired effect Effects 0.000 description 6
- 239000011812 mixed powder Substances 0.000 description 6
- 229910002077 partially stabilized zirconia Inorganic materials 0.000 description 6
- 239000011230 binding agent Substances 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- 238000009413 insulation Methods 0.000 description 5
- 230000003068 static effect Effects 0.000 description 5
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 4
- 230000001133 acceleration Effects 0.000 description 4
- 239000004020 conductor Substances 0.000 description 4
- 239000012535 impurity Substances 0.000 description 4
- 238000005259 measurement Methods 0.000 description 4
- 229910052760 oxygen Inorganic materials 0.000 description 4
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 3
- 230000005684 electric field Effects 0.000 description 3
- 239000011521 glass Substances 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 229910052742 iron Inorganic materials 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 3
- 239000012299 nitrogen atmosphere Substances 0.000 description 3
- 238000007747 plating Methods 0.000 description 3
- 239000002002 slurry Substances 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 2
- 239000012298 atmosphere Substances 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 238000009713 electroplating Methods 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 229910052746 lanthanum Inorganic materials 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 230000036961 partial effect Effects 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 229910052702 rhenium Inorganic materials 0.000 description 2
- 229910052709 silver Inorganic materials 0.000 description 2
- 239000004332 silver Substances 0.000 description 2
- 239000002356 single layer Substances 0.000 description 2
- 238000010532 solid phase synthesis reaction Methods 0.000 description 2
- 230000036962 time dependent Effects 0.000 description 2
- 229910052726 zirconium Inorganic materials 0.000 description 2
- FIPWRIJSWJWJAI-UHFFFAOYSA-N Butyl carbitol 6-propylpiperonyl ether Chemical compound C1=C(CCC)C(COCCOCCOCCCC)=CC2=C1OCO2 FIPWRIJSWJWJAI-UHFFFAOYSA-N 0.000 description 1
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 1
- 229910001252 Pd alloy Inorganic materials 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- 238000000441 X-ray spectroscopy Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910052788 barium Inorganic materials 0.000 description 1
- 229910052790 beryllium Inorganic materials 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 239000003990 capacitor Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000003989 dielectric material Substances 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000007606 doctor blade method Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000014509 gene expression Effects 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 230000000670 limiting effect Effects 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 239000002075 main ingredient Substances 0.000 description 1
- 150000002736 metal compounds Chemical class 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 235000006408 oxalic acid Nutrition 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- SWELZOZIOHGSPA-UHFFFAOYSA-N palladium silver Chemical compound [Pd].[Ag] SWELZOZIOHGSPA-UHFFFAOYSA-N 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000002250 progressing effect Effects 0.000 description 1
- -1 rare earth compound Chemical class 0.000 description 1
- 229910001404 rare earth metal oxide Inorganic materials 0.000 description 1
- 238000010405 reoxidation reaction Methods 0.000 description 1
- 239000004576 sand Substances 0.000 description 1
- 238000007650 screen-printing Methods 0.000 description 1
- 230000001568 sexual effect Effects 0.000 description 1
- 229910000679 solder Inorganic materials 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000004071 soot Substances 0.000 description 1
- 229910052712 strontium Inorganic materials 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
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Definitions
- the present invention relates to a dielectric ceramic and a multilayer ceramic capacitor, and more specifically, a dielectric ceramic suitable for a dielectric material for a small-large capacity multilayer ceramic capacitor, and manufactured using the dielectric ceramic.
- the present invention relates to a laminated ceramic capacitor.
- This type of multilayer ceramic capacitor is a dielectric ceramic mainly composed of BaTiO or the like.
- the dielectric layer and the internal electrode are alternately laminated to produce a ceramic laminated body, and then the ceramic laminated body is subjected to a firing treatment to form a laminated sintered body, and the outer surface of the laminated sintered body It is manufactured by forming external electrodes.
- the dielectric layer can be reduced in size and increased in capacity by reducing the thickness of the dielectric layer.
- a plurality of dielectric layers and a plurality of internal electrodes are integrally laminated, and the dielectric layer is made of a sintered body of ceramic particles, and is the ceramic particle a solid solution?
- the ceramic particles contain one or more rare earth elements selected from Ho, Sc, Y, Gd, Dy, Er, Yb, Tb, Tm and Lu, and the concentration of the rare earth elements is
- a multilayer ceramic capacitor has been proposed in which the height increases from the center of the grain toward the grain boundary (Patent Document 1).
- Patent Document 1 includes ceramic particles containing one or more acceptor-type elements selected from Mn, V, Cr, Co, Fe, Cu, Ni, and Mo force.
- a multilayer ceramic capacitor is also disclosed in which the concentration of the type element increases from the center of the ceramic particle toward the grain boundary.
- the particle diameter can be reduced by making the concentration of the acceptor type element and the rare earth element have a high concentration gradient from the center of the ceramic particle toward the grain boundary side. This improves the reduction resistance and reoxidation of the dielectric layer, increases the electrical resistance of the ceramic particles forming the dielectric layer, and improves reliability, especially when the dielectric layer is thinned. Reliability can be improved.
- Patent Document 1 Japanese Patent Application Laid-Open No. 2001-230148 (Claim 1, Claim 4)
- the concentration of the acceptor element and the rare earth element has a high concentration gradient from the center of the ceramic particle toward the grain boundary side.
- High relative dielectric constant, good temperature characteristics, and high reliability are possible, but since the rate of change of capacitance with time is large, it is substantially difficult to guarantee sufficient capacitance.
- the present invention has been made in view of such circumstances, and has high relative permittivity, capacitance temperature characteristics, high reliability, and excellent capacitance change with time. It is an object of the present invention to provide a dielectric ceramic, and a multilayer ceramic capacitor manufactured using the dielectric ceramic.
- the present invention has been made based on such knowledge, and the dielectric ceramic according to the present invention has a general formula: (Ba Ca) (Ti Zr Cu) O (provided that 0.96 ⁇ m ⁇ 1.02, 0.001 ⁇
- Re La, Ce ⁇ Pr, Nd, Sm ⁇ Eu, Gd , Tb, Dv ⁇ Ho, Er, Tm, Yb, L at least one selected from u and Y
- ⁇ is at least one selected from Mn, Ni, Fe, Co, V, W, Cr, Mo, Al
- Mg and Si Mg and Si
- the Cu is The main phase particles constituting the main component are present in a uniformly dispersed state, and the content of each subcomponent is Re: 0.:! To 1.5 mol parts with respect to 100 mol parts of the main components, respectively.
- Mg 0.1 to: 1.5 mol parts
- Si 0.:! To 2.0 mol parts.
- homogeneous means that it is unevenly distributed in a part of the region of the main phase particles, or is directed from the center in the grain direction to the grain boundary direction or in the direction of the grain boundary direction toward the grain center. Unlike the case where a concentration gradient occurs, it means that the particles are uniformly or substantially uniformly dispersed in the main phase particles.
- the average value of the region in which the predetermined rare earth element Re is dissolved in the main phase particles is set to 40% or less in terms of the area ratio in the cross section.
- the dielectric ceramic of the present invention is characterized in that the average value of the region where Re is dissolved in the main phase particles is 40% or less in terms of the area ratio in the cross section.
- the multilayer ceramic capacitor according to the present invention includes a multilayer sintered body obtained by sintering a ceramic multilayer body in which a plurality of dielectric layers and internal electrodes are alternately stacked, and the multilayer sintered body.
- a multilayer ceramic capacitor having an external electrode formed on an outer surface is characterized in that the dielectric layer is formed of the above-described dielectric ceramic.
- the relative permittivity ⁇ r is 2500 or more, the dielectric loss tan 5 force is less than 7%, and the temperature change rate power of the electrostatic capacity B characteristic specified in SJIS (-25 to + 85 ° C) In the range of 20 ° C
- the temperature change rate of the capacitance with respect to the capacitance is within ⁇ 10%), and no defective product occurs after 2000 hours even at high temperature load, and the capacitance change rate with time is ⁇
- a multilayer ceramic capacitor of less than 5% can be obtained.
- the average value of the region where Re is dissolved in the main phase particles is 40% or less in terms of the area ratio in the cross section, so that the laminated ceramic in which the temperature characteristics of the capacitance are further improved.
- the multilayer ceramic capacitor of the present invention a multilayer sintered body obtained by sintering a ceramic multilayer body in which a plurality of dielectric layers and internal electrodes are alternately laminated, and the multilayer sintered body Since the dielectric layer is formed of the above-mentioned dielectric ceramic, the static capacitance having a high dielectric constant as described above is provided.
- a desired multilayer ceramic capacitor having good capacitance temperature characteristics, excellent reliability, and small capacitance change with time can be obtained.
- FIG. 1 is a cross-sectional view schematically showing one embodiment of a multilayer ceramic capacitor manufactured using a dielectric ceramic of the present invention.
- the dielectric ceramic as one embodiment of the present invention has a general formula: (Ba Ca) (Ti Zr
- the specific rare earth element Re at least one kind selected from La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu, and Y force may be used.
- the specific metal element M at least one selected from Mn, Ni, Fe, Co, V, W, Cr, Mo, and Al force can be used.
- the present dielectric ceramic has a rare earth element Re mole part a, a metal element M mole part b, a Mg monolayer part c, and a Si mole part d with respect to 100 mole parts of the main component. ) To (8).
- Cu is solid-solved at the same site as the Ti element in the main component (hereinafter referred to as “Ti site”), and exists uniformly in the main phase particles constituting the main component. ing.
- uniform means that the concentration is unevenly distributed in a part of the region in the main phase particle, or the concentration from the center in the grain toward the grain boundary, or from the grain boundary direction toward the grain center. Unlike the case where a gradient is generated, it means that the particles are uniformly or substantially uniformly dispersed in the main phase particles.
- m is a force expressed by (Ba Ca) and indicates the molar ratio of Ba site to Ti site.
- the temperature characteristics of the capacitance will deteriorate and the B characteristics specified in JIS will not be satisfied, and the life may be reduced under high temperature loads, which may impair reliability.
- the molar ratio m is greater than 1.02, the relative dielectric constant ⁇ r decreases to less than 2500, and it becomes impossible to obtain a multilayer ceramic capacitor having a desired high relative dielectric constant.
- the molar ratio m of Ba site to Ti site is adjusted to 0 ⁇ 96 to 1.02.
- a dielectric ceramic according to the application by replacing part of Ba with Ca as necessary.
- the relative dielectric constant ⁇ r decreases to less than 2500, making it impossible to obtain a multilayer ceramic capacitor having a high relative dielectric constant.
- the Zr content molar ratio u in the Ti site is adjusted to be 0 to 0.06.
- the ability to improve the characteristics of dielectric ceramics by including a specific rare earth element Re in the dielectric ceramic When the molar part a per 100 molar parts of the main component is less than 0.1, There is a risk that the service life will decrease and the reliability will be impaired. On the other hand, if the molar part a with respect to 100 molar parts of the main component exceeds 1.5, the temperature characteristics of the capacitance deteriorate, which is not preferable.
- the molar part a of the specific rare earth element Re is prepared so as to be 0.:! To 1.5 with respect to 100 molar parts of the main component.
- the presence form of the rare earth element Re is preferably 40% or less in terms of the area ratio in the average value force section of the region in which the main phase particles are solid-solved. That is, the rare earth element Re is contained in an amount of 0.:! To 0.6 mol part with respect to 100 mol parts of the rare earth element Re, and these rare earth elements Re are mixed in the grain boundaries or / in the crystal grains.
- the temperature characteristics of the electrostatic capacity can satisfy the characteristics specified in IS and can obtain good temperature characteristics, but the average value of the region dissolved in the main phase particles can be obtained.
- the rare earth element Re in the dielectric ceramic so that the area ratio in the cross section is 40% or less, the temperature change rate of the capacitance can be further reduced, and the B characteristics can be provided with a margin. The power S can be fully satisfied.
- (6) b Strength that can improve the characteristics of dielectric ceramics by including specific metal element M in the dielectric ceramic and making these metal elements M exist in the crystal grains and / or grain boundaries. If the molar part b is less than 0.1, the life under high temperature load may be shortened and reliability may be impaired. In addition, the dielectric breakdown voltage is lowered. On the other hand, if the mole part b with respect to 100 mole parts of the main component exceeds 0.6, the life under high temperature load may be reduced, and the reliability may be impaired, and the dielectric breakdown voltage is lowered. In this case, the change in capacitance with time is also not preferable.
- the molar part b of the specific metal element M is prepared so as to be 0 ⁇ :! to 0 ⁇ 6 with respect to 100 mol parts of the main component.
- Mg can be contained in the dielectric ceramic, and these Mg can be present in the crystal grains and / or in the grain boundaries to improve the characteristics of the dielectric ceramic.
- the mole part c with respect to 100 mole parts of the component is less than 0.1, the life reduction at high temperature load becomes remarkable, and the change with time of the capacitance becomes large.
- the mole part c with respect to 100 mole parts of the main component exceeds 1.5, the temperature characteristics of the capacitance deteriorate, which is not preferable.
- preparation is made so that the molar part c of Mg is 0.1 to 1.5 with respect to 100 molar parts of the main component.
- Si has an effect as a sintering aid
- the presence of S content in the grain boundary can improve the sinterability. If it is less than 0.1, the life under high temperature load may be shortened and reliability may be impaired.
- the molar part d with respect to 100 molar parts of the main component exceeds 2.0, the life reduction at high temperature load becomes remarkable, and the force also increases with time in the capacitance. ,.
- the Si mole part d is prepared so as to be 0.:! To 2.0 with respect to 100 mole parts of the main component.
- the Si component is contained in the dielectric ceramic in order to improve the sinterability. Therefore, if Si is the main component, elements that constitute other glass components such as Li, B, Sr, Ca, Ba, Be, Zr, Ga, Na, K, Mg, etc. It is also preferable to contain as needed.
- FIG. 1 is a cross-sectional view schematically showing one embodiment of a multilayer ceramic capacitor.
- the laminated ceramic capacitor 1 has a laminated sintered body 2 in which dielectric layers 3 and internal electrodes 4 and 5 are alternately laminated, and external electrodes are disposed on the outer surface of the laminated sintered body 2. 8 and 9 are formed, and on the surfaces of the external electrodes 8 and 9, first adhesion layers 10 and 11 made of nickel, copper, etc. are formed, and further, the first adhesion layers 10 and 11 are formed.
- the surface of the second is made of solder, tin, etc.
- Two contact layers 12 and 13 are formed.
- the internal electrode 4 is drawn out to one end face 6 and electrically connected to the external electrode 8.
- the internal electrode 5 is drawn to the other end face 7 and is electrically connected to the external electrode 9 so that the electrostatic capacity can be obtained through the dielectric layer 3.
- the conductive material for forming the internal electrodes 4 and 5 it is preferable to use nickel, copper, silver, and an alloy containing these at a low cost.
- the conductive material for forming the external electrodes 8, 9 the same material as that for the internal electrodes 4, 5 can be used, and further, silver, palladium, a silver-palladium alloy, or the like can be used.
- a ceramic raw material powder is synthesized by a solid phase method.
- a ceramic raw material As a ceramic raw material, a Ba compound, a Ca compound, a Ti compound, a Zr compound, and a Cu compound are prepared.
- the compound form of these ceramic raw materials is not particularly limited as long as a desired ceramic raw material powder can be obtained, but oxide powder, carbonate, etc. are preferably used.
- these ceramic raw materials are weighed so as to satisfy the above formulas (1) to (4), the ceramic raw materials are put into a ball mill, mixed and ground, dried, and then subjected to a predetermined calcining treatment. (Heat treatment) is performed, thereby producing a main component powder represented by the general formula: Ba (Ti Cu) 0 To make.
- a predetermined calcining treatment is performed, thereby producing a main component powder represented by the general formula: Ba (Ti Cu) 0 To make.
- the main component powder in which Cu is uniformly dissolved in the Ti site can be efficiently obtained by mixing the Cu compound simultaneously with other ceramic raw materials and performing the synthesis process.
- a rare earth compound containing a specific rare earth element Re, a metal compound containing a specific metal element M, an Mg compound, and an Si compound are prepared as subcomponent raw materials.
- the form of these subcomponent raw materials is not particularly limited, but an oxide raw material is preferably used.
- the subcomponent raw materials are weighed so as to satisfy the above formulas (5) to (8), put into a ball mill, and mixed with the main component powder. Dry the ceramic raw material powder.
- an organic solvent, an organic binder, and the like are mixed into the raw material powder and mixed to produce a ceramic slurry.
- the ceramic slurry is formed using a forming method such as a doctor blade method to produce a ceramic green sheet.
- a conductive paste containing a conductive material such as nickel or copper screen printing is performed on the ceramic green sheet to form a conductive pattern.
- the ceramic green sheets on which the conductive pattern is formed are appropriately laminated and pressed to form a ceramic laminate.
- the ceramic laminate is subjected to a binder removal treatment and then subjected to a firing treatment to obtain a laminated sintered body 2 Is made.
- a conductive paste in which glass frit is added to a conductive material such as nickel or copper is applied to both ends of the laminated sintered body 2 and subjected to a baking treatment to form the external electrodes 8 and 9.
- plating treatment such as electrolytic plating is performed to form first plating films 10 and 11 and second plating films 12 and 13 in sequence, thereby forming a multilayer ceramic capacitor.
- the dielectric layer 3 is formed of the above dielectric ceramic, it has a high relative dielectric constant, a temperature characteristic of capacitance, high reliability, and a capacitance. It is possible to obtain a multilayer ceramic capacitor that is excellent in change over time.
- the relative permittivity ⁇ r is 2500 or more
- the temperature characteristics of capacitance satisfy the B characteristics specified in IS, and in the high temperature load life test, defective products are observed even after 2000 hours. Does not occur, the dielectric breakdown voltage is large, and the rate of change with time of the capacitance is less than ⁇ 5%.
- a desired multilayer ceramic capacitor can be obtained.
- the present invention is not limited to the above-described embodiment.
- a Cu compound in order to obtain a main component powder, a Cu compound is mixed and synthesized simultaneously with a Ba compound or Ti compound as a ceramic raw material, but Cu is contained in the main phase particles. It is not limited to the above production method as long as it is uniformly dispersed.
- the molar ratio m between the Ba site and the Ti site does not necessarily have to be satisfied when these ceramic raw materials are prepared.
- the molar ratio m may be weighed so as to be slightly reduced at the time of the preparation, and a deficient Ba compound or Ca compound may be added when adding a minor component such as rare earth element Re.
- the Ba compound or Ca compound added as a deficiency can be dissolved in the main phase particles mainly by firing to satisfy the desired molar ratio m.
- the ceramic raw material powder is synthesized by the solid phase method in the above embodiment, but using a wet synthesis method such as an oxalic acid method, a hydrothermal synthesis method, or a hydrolysis method. It's good.
- Example 1 changes in the characteristics of the multilayer ceramic capacitor were confirmed when the composition of the dielectric ceramic and the solid solution state of Cu were changed.
- the ceramic raw material powder is mixed and ground using ethanol as a solvent and a porobutyl petital binder, and then a ceramic slurry is prepared. Forming force was applied to obtain a ceramic green sheet.
- a conductive paste mainly composed of Ni was screen-printed on the surface of the ceramic green sheet to form a conductive pattern for constituting an internal electrode.
- the ceramic green sheets on which this conductive pattern was formed were laminated so that the side from which the conductive pattern was drawn was alternated to obtain a ceramic laminate.
- the ceramic laminate was heated at 350 ° C in a nitrogen atmosphere, after the binder removal processing, the oxygen partial pressure 10- 1Q MPa consisting of H- N-H_ ⁇ gas reduction sexual atmosphere
- the laminate was held at a temperature of 1100 ° C. for 2 hours to produce a laminated sintered body in which internal electrodes were embedded.
- a conductive paste mainly composed of Cu containing B—Li Si—Ba 0 glass frit was applied to both end faces of this laminated sintered body, and 800 ° in a nitrogen atmosphere.
- An external electrode was formed by baking with C.
- electrolytic plating was performed to sequentially form a Ni film and a Sn film on the external electrodes, thereby obtaining multilayer ceramic capacitors of sample numbers 1 to 31.
- Sample No. 32 as a comparative example was produced by the following method. That is, BaCO and
- the mixture was pulverized and dried to obtain a mixed powder. And this mixed powder was calcined at 1150 ° C for 2 hours, so that the barium titanate powder whose composition formula is represented by Ba TiO was obtained.
- Sample No. 33 was produced as a comparative example by the following method.
- a barium titanate powder whose composition formula is represented by Ba TiO is prepared by the same method and procedure as sample number 32.
- sample number 33 was prepared by the same method and procedure as sample numbers:! To 31.
- the outer dimensions of the multilayer ceramic capacitor thus obtained are 1.6 mm in length, 0.8 mm in width, and 1.0 mm in thickness.
- the thickness of the dielectric layer interposed between the internal electrodes is 0.7 ⁇ m. m, the number of effective dielectric layers for capacitance was 50, and the counter electrode area per dielectric layer was 0.8 mm 2 .
- Table 1 shows the component compositions of sample numbers:! -33.
- sample Nos. 32 and 33 have 0.01 mol part of CuO added to 100 mol parts of the main component.
- sample Nos.! To 33 were cut and FE-TEM-EDX ( Section of each sample using Field Emission Type ⁇ ransmission Electron Microscopy-Energy Dispersion X-ray spectroscopy The composition was analyzed. Specifically, 20 crystal particles were extracted from the cross section of each sample, and composition analysis was performed at 20 points in each crystal particle with a probe diameter of 1 nm and an acceleration voltage of 200 kV.
- Sample No. 32 contained almost no Cu in the main phase particles and Cu was mainly present at the grain boundaries.
- the relative permittivity ⁇ r and the dielectric loss tan 5 were measured for each of the samples 1 to 33 using an impedance analyzer under an AC electric field of temperature 25 ° C, lkHz, 0.5 Vrms. .
- the change rate of capacitance at 25 to 85 ° C was measured with reference to the capacitance at 20 ° C, the maximum change rate in the temperature range was obtained, and the temperature characteristics of the capacitance were determined. evaluated. If the maximum rate of change is within ⁇ 10%, the B characteristics specified in JIS will be satisfied.
- a DC voltage was applied at a boosting rate of 100 VZ seconds, and a voltage at which a short circuit occurred, that is, a dielectric breakdown voltage was measured.
- the number of samples with the insulation resistance of 200 k ⁇ or less was counted as a defective product, and the defect occurrence rate was calculated.
- each sample was held at a temperature of 150 ° C. for 1 hour, and then allowed to stand at room temperature for 24 hours.
- the capacitance after the standing was measured to obtain an initial capacitance.
- the sample was allowed to stand at room temperature for 240 hours, and the capacitance was measured again to obtain the rate of change from the initial capacitance, and the time-dependent characteristics of the capacitance were evaluated.
- Example Nos. 32 and 33 have 0.01 mol parts of CuO added to 100 mol parts of the main component.
- Sample No. 2 contains no Cu in the dielectric ceramic, so the defect occurrence rate in the high temperature load life test is 2% after 1000 hours and 6% after 2000 hours. It was found that the rate of change in capacitance with time was as high as 15.8%, indicating poor reliability.
- Sample No. 21 has a molar ratio X of Cu in the main component of 0.035, which exceeds 0.03.
- the failure rate was 2% after 1000 hours and 12% after 2000 hours, and the dielectric breakdown voltage was as low as 90V, indicating poor reliability.
- Sample No. 22 had a molar ratio m of Ba site to Ti site of 0.958, less than 0.96, and the rate of change in capacitance with temperature was 12.6%. It was found that the force S exceeded 0% and the B characteristic specified in JIS could not be satisfied, and the temperature characteristic of the capacitance deteriorated. Moreover, the failure rate in the high-temperature load life test was 8% after 1000 hours and 32% after 2000 hours, indicating that the reliability was poor.
- Sample No. 23 had a relative dielectric constant ⁇ r as low as 2020 because the molar ratio m of Ba site to Ti site was 1.022 and exceeded 1.02.
- Sample No. 24 does not contain the rare earth element Re in the dielectric ceramic, so the defect occurrence rate in the high temperature load life test is 5% after 1000 hours and 39% after 2000 hours. It turned out to be inferior in reliability.
- Sample No. 25 is a total of 2.
- Sample No. 26 does not contain the metal element M in the dielectric ceramic. Therefore, in the high-temperature load life test, there was no defective product after 1000 hours, but the failure rate was over 2000 hours. It became 9%, and it turned out that it is inferior in reliability. It was also found that the breakdown voltage was as low as 70V.
- Sample No. 27 has a metal element M content of 0.7 mol in total with 100 mol parts of the main component, which is more than 0.6 mol parts. Although no defective products were generated at the time, the failure rate was 4% after 2000 hours, indicating poor reliability. It was also found that the rate of change with time of the capacitance, which has a low dielectric breakdown voltage of 80V, was as high as 15.2%.
- Sample No. 28 does not contain Mg in the dielectric ceramic, so the defect occurrence rate in the high-temperature load life test is 9% after 1000 hours and 34% after 2000 hours, resulting in poor reliability. I understood that. In addition, the rate of change with time of capacitance is as high as 6.7%. I understand.
- Sample No. 29 has a high Mg content of 2.0 parts per 100 mole parts of the main component, 1.
- Sample No. 30 is inferior in reliability because the dielectric ceramic does not contain Si, and the failure rate in the high-temperature load life test is 1% after 1000 hours and 18% after 2000 hours. I understood that.
- Sample No. 31 has a Si content of 2.5 moles per 100 moles of the main component, which is much higher than 2.0 moles. 14% after 1000 hours and 63% after 2000 hours, indicating a significant decrease in reliability. It was also found that the rate of change with time of the capacitance increased to 5.9%.
- Sample No. 33 had a capacitance change with time of 6.2% due to a concentration gradient in Cu in the main phase particles.
- Example 2 the influence of the solid solution ratio of the rare earth element Re in the main phase particles was confirmed.
- a ceramic laminate having the same composition as Sample No. 1 in [Example 1] was prepared, heated at 350 ° C in a nitrogen atmosphere and subjected to binder removal treatment.
- Gas acid
- each sample No. 4:! To 48 was cut, and as in [Example 1], the cross section of each sample was observed using FE-TEM-EDX.
- the solid solution area ratio of Dy was determined. In other words, 20 crystal particles were extracted from the cross section of each sample, and composition analysis was performed at 20 points in each crystal particle with a probe diameter of 1 nm and an acceleration voltage of 200 kV. The solid solution area ratio was determined.
- the solid solution area ratio in the main phase particles of the rare earth element Re, Dy increases as the firing temperature increases.
- the contrast force between sample numbers 41-46 and sample numbers 47 and 48 As is clear, when the solid solution area ratio of Dy is 40% or less, the capacitance temperature based on 20 ° C The rate of change was suppressed to within ⁇ 7.5% at -25 to 85 ° C, and therefore, it was found that the temperature characteristics of the capacitance can sufficiently satisfy the B characteristics with a margin, which is more preferable. .
- the firing temperature in the range of 980 to 1200 ° C. Even if the firing treatment is performed in this range, It was also found that it does not affect various characteristics and reliability.
- Example 3 the effects of the Ca molar ratio t at the Ba site and the Zr molar ratio u at the Ti site were confirmed.
- the main component is 100 monolayers, but 1.0 monoy Dy ⁇ , 0.3 monolayer Mn ⁇ , 1.0
- the mixture was dried in a ball mill and dried to obtain a ceramic raw material powder.
- each sample number 51 to 68 was cut, and similarly to [Example 1], the cross section of each sample was observed using FE-TEM-EDX, and the composition analysis was performed. That is, from the cross section of each sample Twenty crystal grains were extracted, and composition analysis was performed at 20 points in each crystal grain with a probe diameter of 1 nm and an acceleration voltage of 200 kV. As a result, it was confirmed that Cu did not cause a concentration gradient in the main phase particles and was uniformly dissolved in the main phase particles.
- Sample No. 66 the Ca molar ratio t of Ba site was 0 ⁇ 105, which exceeded 0.1, so the relative dielectric constant ⁇ r force S2430 was low.
- Sample No. 68 has a Zr molar ratio u of Ti site of 0.062 and exceeds 0.06. Therefore, the defect occurrence rate in the high-temperature load life test is 2% after 2000 hours and 2000 hours have elapsed. It became 12% at the time, and it turned out that it was inferior in reliability.
- Sample Nos. 51 to 55 and 56 had a Ba site Ca molar ratio t of 0.1 or less and a Ti site Zr molar ratio u of 0.06 or less. Therefore, the dielectric constant ⁇ r force S2500 or higher, the capacitance temperature characteristics satisfy the B characteristics, and the dielectric breakdown voltage is also high. Thus, it was found that a multilayer ceramic capacitor having excellent characteristics with excellent reliability and a capacitance change with time of ⁇ 5% or less can be obtained.
- Ba (Ti Cu) 0 is represented by the same method and procedure as in [Example 1].
- a main component of 1.010 0.090 0.010 3 was prepared.
- HfO, ZnO, AgO, PdO, SrO, NaO are prepared as impurity oxides.
- a multilayer ceramic capacitor was prepared.
- each sample No. 7:! To 77 was cut, and the cross-section of each sample was observed using FE-TEM-EDX as in [Example 1], and the composition analysis was performed. . That is, 20 crystal particles are extracted from the cross section of each sample, and probe diameter lnm is obtained at 20 points in each crystal particle.
- composition analysis was performed at an acceleration voltage of 200 kV. As a result, it was confirmed that Cu did not cause a concentration gradient in the main phase particles and was uniformly dissolved in the main phase particles.
- Table 5 shows the measurement results. As is clear from Table 5, the relative dielectric constant ⁇ r, dielectric loss tan ⁇ , and temperature characteristics of capacitance even if the total amount of impurities is less than 1 mole part per 100 mole parts of the main component It was confirmed that the dielectric breakdown voltage, reliability at high temperature load, and the rate of change of capacitance with time were hardly affected.
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DE112006001440T DE112006001440B4 (de) | 2005-06-10 | 2006-05-24 | Dielektrische Keramik und Vielschicht-Keramikkondensator |
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CN2006800201502A CN101193836B (zh) | 2005-06-10 | 2006-05-24 | 电介质陶瓷及层叠陶瓷电容器 |
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Also Published As
Publication number | Publication date |
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TWI298893B (ja) | 2008-07-11 |
KR20080017344A (ko) | 2008-02-26 |
JP4626892B2 (ja) | 2011-02-09 |
US20080112109A1 (en) | 2008-05-15 |
JPWO2006132086A1 (ja) | 2009-01-08 |
DE112006001440T5 (de) | 2008-04-17 |
DE112006001440B4 (de) | 2010-06-02 |
CN101193836A (zh) | 2008-06-04 |
KR100906079B1 (ko) | 2009-07-02 |
TW200705484A (en) | 2007-02-01 |
CN101193836B (zh) | 2010-09-29 |
US7397649B2 (en) | 2008-07-08 |
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