WO2012120712A1 - 積層セラミックコンデンサ - Google Patents
積層セラミックコンデンサ Download PDFInfo
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- WO2012120712A1 WO2012120712A1 PCT/JP2011/071789 JP2011071789W WO2012120712A1 WO 2012120712 A1 WO2012120712 A1 WO 2012120712A1 JP 2011071789 W JP2011071789 W JP 2011071789W WO 2012120712 A1 WO2012120712 A1 WO 2012120712A1
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- dielectric ceramic
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- ceramic capacitor
- multilayer ceramic
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Definitions
- the present invention is a multilayer ceramic capacitor composed of a dielectric layer mainly composed of barium titanate, particularly satisfying the temperature characteristics of X7R even when fired at a low temperature, and further excellent in the case of further thinning.
- the present invention relates to a multilayer ceramic capacitor having a structure improved to have a long life.
- the melting point of copper is 1085 ° C., which is lower than that of nickel. Therefore, it is necessary to fire at 1030 ° C., preferably 1000 ° C. or less, at a lower temperature than conventional. There is a problem that a dielectric material for a multilayer ceramic capacitor that exhibits sufficient characteristics even when fired is necessary.
- the present inventors can perform sintering at 1030 ° C., preferably 1000 ° C. or less in a reducing atmosphere, and lead (Pb) or bismuth is used as a material for the dielectric ceramic layer.
- a multilayer ceramic capacitor which does not contain (Bi) has a dielectric constant of 2000 or more, has a temperature characteristic of dielectric constant of X7R, and has a high temperature accelerated lifetime characteristic equivalent to that of a conventional Ni internal multilayer ceramic capacitor is obtained.
- the dielectric ceramic composition mainly composed of a BaTiO 3 -based compound
- the conditions for the Ba / Ti ratio, the composition ratio of rare earths as subcomponents, and the composition ratio of MnO were found.
- the dielectric ceramic layer is ABO 3 + aRe 2 O 3 + bMnO (where ABO 3 is a perovskite mainly composed of BaTiO 3).
- Re 2 O 3 is one or more metal oxides selected from La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu, and Y, a , B represents the number of moles relative to 100 mol of ABO 3 ), the range is 1.000 ⁇ A / B ⁇ 1.035, and 0.05 ⁇ a ⁇ 0.
- Patent Document 1 including 0.25 ⁇ b ⁇ 2.0, a main component and one or more of B, Li, or Si, each of B 2 O 3 , Li 2 O, and SiO 2 And a sub-component whose total when converted is 0.16 to 1.6 parts by mass, and a laminated body characterized in that the internal electrode is made of Cu or a Cu alloy A ceramic capacitor was proposed (Patent Document 1).
- the inventors of the present invention have a multilayer ceramic capacitor in which the internal electrode is made of Cu or Cu alloy, and the dielectric ceramic is composed of grains and grain boundaries whose average diameter when viewed in cross section is 400 nm or less. It has also been proposed that by using a sintered body of a probskite-type dielectric material mainly composed of BaTiO 3 , a temperature characteristic having an X7R characteristic or an X8R characteristic can be obtained (Patent Document 2). In the example, as a starting material of the sintered body, a mixture of MnO, rare earth oxide as an additive, and B 2 O 3 , Li 2 O, and SiO 2 as a sintering aid is used. .
- the inventors of the present invention have described a dielectric ceramic composition comprising a main component composed of BaTiO 3 and subcomponents composed of Re, Mn, V, Mo, Cu, B, Li, Ca, and Sr.
- a dielectric ceramic composition comprising a main component composed of BaTiO 3 and subcomponents composed of Re, Mn, V, Mo, Cu, B, Li, Ca, and Sr.
- the total content of V and Mo has been found to affect the life characteristics of a multilayer ceramic capacitor using an internal electrode mainly composed of Cu.
- Patent Document 5 as a structure capable of thinning and obtaining high life characteristics, a method for limiting the number of particles per layer to be small and facilitating diffusion of Mn and V to the entire grain boundary.
- a Li-based compound is contained as a sintering aid, the average grain diameter Rg [ ⁇ m] of the dielectric ceramic is 0.06 ⁇ Rg ⁇ 0.17, and its standard deviation ⁇ g [ ⁇ m].
- ⁇ g ⁇ 0.75 a thin layer of less than 1 ⁇ m and good lifetime characteristics are realized at the same time.
- Patent Document 7 generation of a secondary phase that causes a decrease in reliability is limited.
- Patent Document 8 discloses an M 4 R 6 O (SiO 4 ) 6-type crystal phase (where M is at least one selected from alkaline earth metals) and an intergranular boundary between main phase particles made of BaTiO 3. The temperature characteristics of the capacitance, the dielectric breakdown voltage, and the high temperature load life are improved when it is deposited in layers and triple points and thinned.
- Patent Document 9 surplus alkaline earth metal such as Ba or Si is deposited as a non-crystalline substance at the triple point, which reduces the reliability. Therefore, the cross-sectional area of 80% or more of the triple point is suppressed to 8 nm or less, and instead, a crystalline oxide particle containing Ba, Ti and Si is deposited in the dielectric ceramic layer, thereby forming a thin layer. High reliability is realized even in the case of the system.
- surplus alkaline earth metal such as Ba or Si is deposited as a non-crystalline substance at the triple point, which reduces the reliability. Therefore, the cross-sectional area of 80% or more of the triple point is suppressed to 8 nm or less, and instead, a crystalline oxide particle containing Ba, Ti and Si is deposited in the dielectric ceramic layer, thereby forming a thin layer. High reliability is realized even in the case of the system.
- Patent Documents 1 to 3 already proposed have been studied in a thick place of several ⁇ m or more. It has been found that there is still room for study in terms of ensuring reliability when the ceramic layer is thinned to 2 ⁇ m or less, preferably 1 ⁇ m or less. On the other hand, in the conventional reliability design described in Patent Documents 4 to 9 and the like when thinned, firing at a low temperature as described above is not intended, but it has been found that it is not sufficient. did. *
- Patent Documents 4 and 5 Ni is used for the internal electrode, the firing temperature is as high as 1150 ° C., and the firing temperature is high in order to use Cu as the internal electrode. Further, in Patent Document 6, it is possible to fire at a low temperature of 1025 ° C., but only Si and Li are contained as components for sintering at a low temperature. In such a system, Li tends to volatilize during the firing process, and it is difficult to obtain stable characteristics. Moreover, the thing of patent document 7 also has a high firing temperature of 1200 degreeC or more, and cannot use Cu as an internal electrode. In the composition described in Patent Document 8, the firing temperature is as high as 1200 ° C. or higher, and Cu cannot be used as the internal electrode. Further, in Patent Document 9, firing at a low temperature is not intended, and in fact, firing at 1030 ° C. or lower is impossible only with the described composition. *
- the present invention has been made in view of the current situation, and can be fired at a low temperature of 1030 ° C. or lower, and even when thinned, has a high dielectric constant, good life characteristics,
- An object of the present invention is to provide a multilayer ceramic capacitor having both temperature characteristics satisfying X7R.
- main phase particles mainly composed of BaTiO 3 and at least Re (Re is Eu, Gd, Dy, Ho, Er, Yb, and Y
- a secondary phase particle containing Ba and Ti and a dielectric ceramic composed of a grain boundary phase containing at least one of or both of B (boron) and Li (lithium).
- a substantially rectangular parallelepiped ceramic laminate formed by laminating a plurality of dielectric ceramic layers having a layer thickness of 2 ⁇ m or less, and formed so as to face each other through the dielectric ceramic and alternately be drawn to different end faces.
- An internal electrode made of Cu or Cu alloy, and an external electrode formed on both end faces of the ceramic laminate and electrically connected to each of the internal electrodes drawn to the end face By specifying the particle size distribution of the main phase particles in the multilayer ceramic capacitor having the above, it is possible to achieve both a high dielectric constant and a long life even when sintered at a low temperature using B or Li. I found out.
- the presence of relatively large secondary phase particles containing rare earth promotes the sintering of the main phase particles, and the rare earth gradually diffuses from the secondary phase into the grain boundary phase, thereby sinterability. And found that both reliability and reliability can be achieved.
- Main phase particles containing BaTiO 3 as a main component, and at least Re contains at least one of Eu, Gd, Dy, Ho, Er, Yb, and Y
- secondary containing Ba and Ti Phase particles and a ceramic laminate having a substantially rectangular parallelepiped shape, in which a plurality of dielectric ceramic layers are laminated, the dielectric ceramic comprising a grain boundary phase containing at least one of B (boron) and Li (lithium).
- the cumulative number distribution (hereinafter referred to as the particle size distribution) obtained by measuring the particle diameter of the main phase particles in the medium is 20% cumulative, When the particle diameters at 50% and 95% are D20, D50, and D95, respectively, D20 ⁇ D50 ⁇ 70%, D50 ⁇ t / 4, D95 ⁇ t / 2, CV value (standard between D20 and D95) Deviation / D50) ⁇ 40%, multilayer ceramic capacitor.
- the dielectric ceramic comprises a dielectric ceramic composition comprising a main component composed of BaTiO 3 and subcomponents composed of Re, Mn, V, Mo, Cu, B, Li, Ca, and Sr.
- the dielectric ceramic composition is BaTiO 3 + aRe 2 O 3 + bMnO + cV 2 O 5 + dMoO 3 + eCuO + fB 2 O 3 + gLi 2 O + xSrO + yCaO (where Re is selected from Eu, Gd, Dy, Ho, Er, Yb, and Y)
- a to g, x, and y represent the number of moles relative to 100 mol of the main component of BaTiO 3 ), and the molar ratio of (Ba + Sr + Ca) / Ti contained in the dielectric ceramic composition is m.
- the temperature satisfies a high dielectric constant of 1800 or higher and X7R characteristics.
- good life characteristics satisfying high life characteristics exceeding 100 hours even at a high temperature load corresponding to an electric field strength of 20 kV / mm at a temperature of 150 ° C. can be obtained.
- FIG. 1 Schematic diagram showing an embodiment of a multilayer ceramic capacitor according to the present invention
- Diagram showing cumulative number distribution of main phase particle size in dielectric ceramic layer A rare earth element map of a dielectric ceramic layer measured by STEM is shown.
- the multilayer ceramic capacitor 1 includes a ceramic multilayer body 2 including a plurality of dielectric ceramic layers 3 and internal electrodes 4 formed between the dielectric ceramic layers. External electrodes 5 are formed on both end faces of the ceramic laminate 2 so as to be electrically connected to the internal electrodes, and a first plating layer 6 and a second plating layer 7 are formed thereon as necessary. It is formed. The thickness of the dielectric ceramic layer 3 sandwiched between the adjacent internal electrodes 4 is less than 2 ⁇ m. *
- the dielectric ceramic constituting the dielectric ceramic layer 3 is a dielectric ceramic composition comprising a main component composed of BaTiO 3 and subcomponents composed of Re, Mn, V, Mo, Cu, B, Li, Ca, and Sr.
- the dielectric ceramic composition is BaTiO 3 + aRe 2 O 3 + bMnO + cV 2 O 5 + dMoO 3 + eCuO + fB 2 O 3 + gLi 2 O + xSrO + yCaO (where Re is Eu, Gd, Dy, Ho, Er, Yb, One or more selected, a to g, x and y represent the number of moles relative to 100 mol of the main component consisting of BaTiO 3 , and m represents the (Ba + Sr + Ca) / Ti mole ratio contained in the dielectric magnetic composition) 0.10 ⁇ a ⁇ 0.50 0.20 ⁇ b ⁇ 0.80 0 ⁇ c ⁇ 0.12 0 ⁇
- the amount of Re 2 O 3 that is, a is small, particularly when it is less than 0.10, the life is remarkably reduced.
- the sinterability is deteriorated, particularly less than 0.50.
- the range of 0.10 ⁇ a ⁇ 0.50 is desirable. More desirably, 0.20 ⁇ a ⁇ 0.35, which enables high life characteristics and densification at 1000 ° C. or lower.
- the life is shortened.
- the sinterability is lowered, and when it is more than 0.80, sintering at 1030 ° C. or less becomes difficult. Therefore, the range of 0.20 ⁇ b ⁇ 0.80 is desirable. More desirably, 0.20 ⁇ b ⁇ 0.60, which enables high life characteristics and densification at 1000 ° C. or lower.
- V and Mo are not contained as a subcomponent, the life characteristics are deteriorated. Therefore, c + d ⁇ 0.04 is desired.
- the range of 0.04 ⁇ c + d ⁇ 0.12 is desirable.
- the life characteristics were also deteriorated. Therefore, 0 ⁇ c ⁇ 0.12 and 0 ⁇ d ⁇ 0.07 A range of is desirable. In particular, when the range is 0 ⁇ c ⁇ 0.10, even better life characteristics are exhibited. *
- Cu When Cu is used for the internal electrode, it is known that Cu diffuses from the internal electrode to the dielectric layer. Therefore, it is considered that Cu is contained in the dielectric layer without adding Cu, and the life characteristics are improved by including Cu. At this time, when CuO is not added, it is considered that the diffusion of Cu from the internal electrode to the dielectric layer reaches an equilibrium state and is stabilized. However, when Cu was added from the outside and excessive Cu was present, there was a tendency that the life decreased. Therefore, 0 ⁇ e ⁇ 1.00 is desirable. Further, Cu can be contained in the dielectric layer by adding Cu as a raw material in the raw material process or by diffusing Cu from the Cu internal electrode into the dielectric layer in the firing process. *
- the range of 0.50 ⁇ f ⁇ 2.00 is desirable. Further, in order to perform firing at a lower temperature, the range of 0.65 ⁇ f ⁇ 1.5 is desired, which enables high life characteristics and densification at 1000 ° C. or lower.
- the amount of Li 2 O that is, g, when (100 (m ⁇ 1) +2 g) / 2f is less than 0.6, the life is reduced, and conversely, when it is greater than 1.3, the sinterability is increased. It becomes low and densification at 1030 ° C. or less becomes difficult. Therefore, the range of 0.6 ⁇ (100 (m ⁇ 1) +2 g) /2f ⁇ 1.3 is desirable. Further, when m ⁇ 1, it is desirable that m> 1 since the life characteristics are deteriorated. However, the value of m is not uniquely determined by the synthesis of the BaTiO 3 -based compound.
- an oxide or carbide of Ba, Sr, or Ca is added in the raw material process.
- the same effect can be obtained.
- 100 (m-1) / 2g is less than 0.50, the life characteristics are deteriorated.
- it is larger than 5.1 the sinterability is lowered and sintering at 1030 ° C. or less becomes difficult. Therefore, the range of 0.50 ⁇ 100 (m ⁇ 1) /2h ⁇ 5.1 is desirable.
- Sr and Ca can be used as an adjustment element for m as in the case of Ba. In the present invention, it has been confirmed that m is effective in the range of 0 ⁇ x ⁇ 1.5 and 0 ⁇ y ⁇ 1.5.
- Si is desirably not included for low-temperature sintering, but is highly likely to be contained in a manufacturing process such as a dispersion process. Therefore, when SiO 2 was intentionally added and the stability of the system with respect to the Si content was confirmed, it was confirmed that if it was 1.0 mol% or less in terms of SiO 2 , the characteristics were not significantly affected. On the other hand, in order to decrease the sintering properties and contains more than 1.0 mol% is significant, the impurity content of SiO 2 is, SiO 2 in terms of the principal component composed of BaTiO 3 is taken as 100mol 1.0 mol or less.
- the dielectric porcelain composition used for the dielectric layer 2 even if the composition does not contain lead, bismuth or the like harmful to the environment or the human body, it is 1030 ° C. or lower, preferably 1000 It can be sintered at a low temperature of °C or less, and can be co-sintered with a metal having excellent conductivity mainly composed of Cu, and exhibits a high dielectric constant and dielectric characteristics satisfying X7R characteristics and X5R characteristics, It is possible to propose a dielectric ceramic composition and a multilayer ceramic capacitor that have high insulation resistance and excellent life characteristics such as high temperature load even when fired in a neutral or reducing atmosphere. *
- a main component material made of a BaTiO 3 compound is added to at least Re as a subcomponent material (where Re is Eu, Gd, Dy, Ho, Er, Yb, and Y And one or more selected from V, Mo, or Cu, Ba, Sr, Ca, oxide, glass, other compounds, etc.
- Re is Eu, Gd, Dy, Ho, Er, Yb, and Y And one or more selected from V, Mo, or Cu, Ba, Sr, Ca, oxide, glass, other compounds, etc.
- the average particle diameter of the BaTiO 3 powder which is the main component of the dielectric ceramic layer 3 of the present invention, is 0.10 ⁇ m or more and 0.30 ⁇ m or less.
- the internal electrode 4 is made of Cu or Cu alloy.
- Cu alloys include Cu- Ni alloy, Cu-Ag alloy and the like can be mentioned.
- the internal electrode 4 is formed by printing a conductive paste on a ceramic green sheet by a method such as screen printing.
- the conductive paste includes substantially the same ceramic material as the ceramic material constituting the dielectric ceramic layer 3. include.
- a green ceramic laminate is obtained by laminating ceramic green sheets on which the conductive paste is printed.
- the molded body is reduced in a nitrogen atmosphere or mixed with hydrogen gas having a concentration of less than 3.0%.
- the sintered ceramic laminate 2 is obtained by firing in a neutral atmosphere. When firing in a reducing atmosphere, it is necessary to perform heat treatment at a temperature of about 700 ° C. in an atmosphere of nitrogen or the like in the temperature lowering step.
- the sintered dielectric ceramic layer 3 contains BaTiO 3 as main phase particles.
- the main phase particles exhibit a particle size distribution as shown in FIG. 2 when the thickness of the dielectric ceramic layer sandwiched between the internal electrodes 4 is t.
- FIG. 2 shows the particle size distribution of the main phase particles in the dielectric ceramic layer.
- the vertical axis indicates the total number and the horizontal axis indicates the particle size.
- D20 when the particle sizes at 20%, 50%, and 95% are D20, D50, and D95, respectively, D20 ⁇ D50 ⁇ 70%, D50 ⁇ t / 4, D95 ⁇ t / 2, CV value (standard deviation between D20 to D95 / D50) ⁇ 40%, more preferably 100 nm ⁇ D50 ⁇ t / 4. That is, D20 is distributed such that D50 has a value of 70% or less of D50, D50 has a value of t / 4 or less, D95 has a value of t / 2 or less, and CV values (D20 ⁇ The standard deviation between D95 / D50) is less than 40%. *
- the dielectric ceramic of the present invention ensures reliability by designing a high-resistance grain boundary phase, and when D50> t / 4, the lifetime due to the decrease in the number of grain boundaries between the internal electrodes. The decline of is inevitable. However, when D50 is less than 100 nm, the dielectric constant is drastically reduced. From the viewpoint of securing the dielectric constant, it is desirable that D50 is 100 nm or more. Further, when D95 is t / 2 or more, the number of coarse particles increases, so that a portion having few electrode interfaces is locally formed in the dielectric layer sandwiched between the two electrodes, and that is the starting point. The service life is deteriorated.
- microparticles sufficiently smaller than the average particle diameter are present together with other particles, thereby reducing the dielectric constant and increasing the number of grain boundaries to improve reliability.
- the apparent dielectric constant of the dielectric layer is lowered, which is not preferable.
- the decrease in the dielectric constant can be suppressed conversely by reducing D20 to an extremely small value of less than D50 ⁇ 70%. That is, it is important that minute particles exist in the range up to D20.
- the CV value in the range of D20 to D95 is as small as less than 40 and the particle diameter is uniform, both high dielectric constant and long life are achieved. When the CV value is 40% or more, the lifetime is reduced due to the variation in particle diameter.
- the sintered dielectric ceramic layer 3 includes at least Re (Re includes at least one of Eu, Gd, Dy, Ho, Er, Yb, and Y), Ba, and Secondary phase particles composed of Ti are included.
- the abundance of the secondary phase particles is characterized in that, in an arbitrary 5 ⁇ m ⁇ 5 ⁇ m region of the dielectric ceramic layer 3, particles having a particle diameter of 0.1 ⁇ m or more are on average 5 or more.
- the main phase particles having a particle size larger than D80 are characterized by an average of less than two particles.
- the presence of rare earth in the grain boundary phase together with B—Li—Ba enhances the insulation of the grain boundary phase and ensures reliability.
- the rare earth is dissolved in B-Li in the early stage of sintering, the sinterability of the main phase particles is hindered. Therefore, the presence of a relatively large rare earth as the secondary phase promotes the sintering of the main phase particles, and the rare earth gradually diffuses from the secondary phase into the grain boundary phase, thereby improving the sinterability. This is a balance between reliability.
- the sinterability deteriorates because the diffusion of the rare earth into the grain boundary is accelerated. Conversely, if there are a large number of secondary phases larger than D80 of the main phase particles, the diffusion rate will be slow, and sufficient rare earth will not be distributed at the grain boundaries, leading to a decrease in reliability.
- the grain boundary phase Ba / Ti ratio in the grain boundary phase and the Ba / Ti ratio in the particles obtained by EELS analysis is used.
- a value obtained by dividing the ratio by the Ba / Ti ratio in the particles is less than 1.2.
- a part of Ba is diffused from the main component BaTiO 3 into the grain boundary phase, so that it is necked at a low temperature to form a dense state.
- the crystallinity at the interface of the main phase particles is lowered, and it is considered that the reliability is lowered by creating defects. Therefore, it is necessary to design so that the value obtained by dividing the Ba / Ti ratio of the grain boundary phase by the Ba / Ti ratio in the grains does not exceed 1.2.
- the external electrode 5 is made of Cu, Ni, Ag, Cu—Ni alloy, Cu—Ag alloy, and is applied with a conductive paste on the fired ceramic laminate 2 and baked or unfired ceramic laminate 2.
- the conductive paste is applied to the dielectric ceramic layer 3 and fired simultaneously with the firing of the dielectric ceramic layer 3.
- plating layers 6 and 7 are formed by electrolytic plating or the like.
- the first plating layer 6 serves to protect the external electrode 5 and is made of Ni, Cu or the like.
- the second plating layer 7 has a role of improving solder wettability and is made of Sn or Sn alloy.
- BaTiO 3 powder having an average particle diameter and a specific surface area shown in Table 1 was prepared as a main starting material.
- BaCO 3 , Re 2 O 3 , MnO, MoO 3 , V 2 O 5 , B 2 O 3 , and Li 2 O powders were prepared.
- BaCO 3 was weighed so that the Ba / Ti ratio in the dielectric ceramic composition was expressed as m, and the values described in Table 1 were obtained.
- composition formula is 100BaTiO 3 + aRe 2 O 3 + bMnO + cV 2 O 5 + dMoO 3 + eCuO + fB 2 O 3 + gLi 2 O (where Re is one selected from Eu, Gd, Dy, Ho, Er, Yb, and Y)
- Re is one selected from Eu, Gd, Dy, Ho, Er, Yb, and Y
- a to g are expressed in terms of mol number relative to 100 mol of the main component of BaTiO 3 ).
- the raw laminate was heated to a temperature of 300 ° C. in an N 2 atmosphere to perform a binder removal process.
- Each sample after the binder removal treatment was fired at a temperature shown in Table 2 for 2 hours in a reducing atmosphere composed of N 2 , H 2 O, and hydrogen concentrations shown in Table 2.
- an annealing process at 700 ° C. in an N 2 atmosphere was performed to obtain a capacitor body formed by sintering the raw laminate.
- an external electrode paste containing Cu and glass powder was applied to both ends of the obtained capacitor body, and baked at 900 ° C. to form external electrodes.
- the outer dimensions of the multilayer ceramic capacitor thus obtained were 0.5 mm in width, 1.0 mm in length, and 0.5 mm in height. Further, the number of laminated dielectrics sandwiched between the internal electrodes was 80, and the average layer thickness t per layer was a value as shown in Table 3. *
- the mapping of rare earth elements in the 5 ⁇ m ⁇ 5 ⁇ m region as shown in FIG. 3 is performed on the dielectric ceramic layer sandwiched between the internal electrode layers using STEM. I went against it.
- the multilayer ceramic capacitor was polished in parallel with the internal electrodes to expose the dielectric layer between the internal electrodes, and sampled on the exposed surface.
- the part where the rare earth element is uniformly distributed in the grain is set as the secondary phase, and the particle is obtained by the same means as that for obtaining the particle diameter of the main phase particle from the TEM image corresponding to the part. The diameter was measured.
- the number of secondary phase particles having a diameter of 0.1 ⁇ m or more existing in the region was counted. Furthermore, the number of secondary phase particles having a diameter of D80 or more of the main phase particles was counted. In addition, about each sample, the average value was calculated
- the dielectric constant, temperature characteristics, and accelerated life of the multilayer ceramic capacitor according to each sample obtained were determined.
- the dielectric constant was calculated from the capacitance measured under the conditions of a temperature of 25 ° C., 1 kHz, and 1 Vrms, and a product having a dielectric constant of 1800 or more was regarded as a good product.
- the temperature characteristics were measured under the conditions of 1 kHz and 1 Vrms, and the maximum value of the rate of change in temperature capacity in the range of ⁇ 55 to 125 ° C. was calculated based on the capacitance at 25 ° C.
- a product having a change rate within this range within ⁇ 15% that is, a product satisfying the X7R characteristic of the EIA standard was regarded as a non-defective product.
- the accelerated life was conducted at a temperature of 150 ° C. under a high-temperature load test in which a voltage equivalent to 20 kV / mm was applied as the electric field strength.
- the time when the insulation resistance was less than 10 ⁇ 5 ⁇ was regarded as a failure, and the failure time was 100 hours.
- the results are shown in Table 3. *
- Multilayer ceramic capacitor 2 Ceramic multilayer body 3: Dielectric ceramic layer 4: Internal electrode 5: External electrode 6: External electrode first plating layer 7: External electrode second plating layer 8: Secondary phase in which rare earth elements are segregated 9: Two adjacent main phase particles 10: Center point of main phase particles 11: Analysis region of EELS 12: Grain boundary phase 13: EELS analysis region located on the grain boundary phase
Abstract
Description
及び少なくともB(ホウ素)又はLi(リチウム)のどちらか一方又は両方を含んだ粒界相からなる誘電体セラミックにより構成される、誘電体セラミック層が複数積層されてなる略直方体形状のセラミック積層体と、前記誘電体セラミックス層を介して対向しかつ交互に異なる端面へ引き出されるように形成された、Cu又はCu合金によりなる内部電極と、前記セラミック積層体の両端面に形成され、該端面に引き出された前記内部電極のそれぞれに電気的に接続された外部電極と、を有する積層セラミックコンデンサにおいて、 前記内部電極に挟まれた前記誘電体セラミック層の層厚をtとし、 上記誘電体セラミック層中における前記主相粒子の粒子径を測定して得られた累積個数分布(以下、粒子径分布と呼ぶ)の累計20%、累計50%及び累計95%における粒子径を、それぞれD20、D50、D95としたとき、 D20 ≦ D50×70%、 D50 ≦ t/4、 D95 ≦ t/2、 CV値(D20~D95の間の標準偏差/D50)<40%、となることを特徴とする積層セラミックコンデンサ。[2]前記誘電体セラミック層の任意の5μm×5μmの領域中に、粒子径が0.1μm以上の前記2次相粒子が、平均5個以上存在することを特徴とする[1]に記載の積層セラミックコンデンサ。[3]前記5μm×5μmの領域において、主相粒子の累積個数分布の累計80%(D80)よりも大きい粒子径をもつ2次相粒子の数が、平均2個未満であることを特徴とする[2]に記載の積層セラミックコンデンサ。[4]前記粒界相のBa/Ti比を、前記主相粒子の粒子内のBa/Ti比で割った値が、1.2以下であることを特徴とする[1]~[3]のいずれかに記載の積層セラミックコンデンサ。[5]前記誘電体セラミックが、BaTiO3からなる主成分と、Re、Mn、V、Mo、Cu、B、Li、Ca、Srからなる副成分とからなる誘電体磁器組成物からなり、 前記誘電体磁器組成を、BaTiO3+aRe2O3+bMnO+cV2O5+dMoO3+eCuO+fB2O3+gLi2O+xSrO+yCaO((ただし、ReはEu、Gd、Dy、Ho、Er、Yb、及びYから選ばれる1種以上、a~g、xおよびyはBaTiO3からなる主成分100molに対するmol数を示す。)で表記し、該誘電体磁器組成物に含まれる(Ba+Sr+Ca)/Tiのmol比をmとしたとき、 0.10≦a≦0.50 0.20≦b≦0.80 0≦c≦0.12 0≦d≦0.07 0.04≦c+d≦0.12 0≦e≦1.00 0.50≦f≦2.00 0.6≦(100(m-1)+2g)/2f≦1.3 0.5≦100(m-1)/2g≦5.1 0≦x≦1.5 0≦y≦1.5であることを特徴とする、[1]~[4]のいずれかに記載の積層セラミックコンデンサ。[6]前記誘電体磁器組成物に不純物として含まれるSiは、BaTiO3からなる主成分を100molとしたときにSiO2換算で1.0mol以下であることを特徴とする[5]に記載の積層セラミックコンデンサ。[7]前記誘電体磁器組成物は、焼結温度が1030℃以下で緻密化させることが可能であることを特徴とする[5]又は[6]に記載の積層セラミックコンデンサ。[8]前記誘電体セラミック層の層厚が2μm以下であることを特徴とする[1]~[7]のいずれかに記載の積層セラミックコンデンサ。
Ni合金、Cu-Ag合金などが挙げられる。この内部電極4は、導電ペーストをスクリーン印刷等の方法でセラミックグリーンシートに印刷することによって形成される。導電ペーストには、Cu又はCu合金の金属材料の他、誘電体セラミック層3の焼成収縮との収縮差を軽減するために、誘電体セラミック層3を構成するセラミック材料と略同一のセラミック材料が含まれている。
除いた領域において、Ba/Ti比の平均値を算出し、これを主相粒子内のBa/Ti比とした。そして、前記粒界相のBa/Ti比を、前記主相粒子内のBa/Ti比で割った値を求めた。各サンプルに関して、任意の100箇所において計測を行い、平均値を求めた。 上記結果を表3に示す。
Claims (13)
- BaTiO3を主成分とする主相粒子と、少なくともRe(ReはEu、Gd、Dy、Ho、Er、Yb、及びYの少なくとも一つ以上を含む)、Ba、Tiを含む2次相粒子、及び少なくともB(ホウ素)又はLi(リチウム)のどちらか一方又は両方を含んだ粒界相からなる誘電体セラミックにより構成される、誘電体セラミック層が複数積層されてなる略直方体形状のセラミック積層体と、前記誘電体セラミックス層を介して対向しかつ交互に異なる端面へ引き出されるように形成された、Cu又はCu合金によりなる内部電極と、前記セラミック積層体の両端面に形成され、該端面に引き出された前記内部電極のそれぞれに電気的に接続された外部電極と、を有する積層セラミックコンデンサにおいて、 前記内部電極に挟まれた前記誘電体セラミック層の層厚をtとし、 上記誘電体セラミック層中における前記主相粒子の粒子径を測定して得られた累積個数分布の累計20%、累計50%及び累計95%における粒子径を、それぞれD20、D50、D95としたとき、 D20 ≦ D50×70%、 D50 ≦ t/4、 D95 ≦ t/2、 CV値(D20~D95の間の標準偏差/D50)<40%となることを特徴とする積層セラミックコンデンサ。
- 前記誘電体セラミック層の任意の5μm×5μmの領域中に、粒子径が0.1μm以上の前記2次相粒子が、平均5個以上存在することを特徴とする請求項1に記載の積層セラミックコンデンサ。
- 前記5μm×5μmの領域において、主相粒子の累積個数分布の累計80%(D80)よりも大きい粒子径をもつ2次相粒子の数が、平均2個未満であることを特徴とする請求項2に記載の積層セラミックコンデンサ。
- 前記粒界相のBa/Ti比を、前記主相粒子の粒子内のBa/Ti比で割った値が、1.2以下であることを特徴とする請求項1に記載の積層セラミックコンデンサ。
- 前記粒界相のBa/Ti比を、前記主相粒子の粒子内のBa/Ti比で割った値が、1.2以下であることを特徴とする請求項2に記載の積層セラミックコンデンサ。
- 前記粒界相のBa/Ti比を、前記主相粒子の粒子内のBa/Ti比で割った値が、1.2以下であることを特徴とする請求項3に記載の積層セラミックコンデンサ。
- 前記誘電体セラミック層の層厚が2μm以下であることを特徴とする請求項1~6のいずれか1項に記載の積層セラミックコンデンサ。
- 前記誘電体セラミックが、BaTiO3からなる主成分と、Re、Mn、V、Mo、Cu、B、Li、Ca、Srからなる副成分とからなる誘電体磁器組成物からなり、 前記誘電体磁器組成を、BaTiO3+aRe2O3+bMnO+cV2O5+dMoO3+eCuO+fB2O3+gLi2O+xSrO+yCaO((ただし、ReはEu、Gd、Dy、Ho、Er、Yb、及びYから選ばれる1種以上、a~g、xおよびyはBaTiO3からなる主成分100molに対するmol数を示す。)で表記し、該誘電体磁器組成物に含まれる(Ba+Sr+Ca)/Tiのmol比をmとしたとき、 0.10≦a≦0.50 0.20≦b≦0.80 0≦c≦0.12 0≦d≦0.07 0.04≦c+d≦0.12 0≦e≦1.00 0.50≦f≦2.00 0.6≦(100(m-1)+2g)/2f≦1.3 0.5≦100(m-1)/2g≦5.1 0≦x≦1.5 0≦y≦1.5であることを特徴とする、請求項1~6のいずれか1項に記載の積層セラミックコンデンサ。
- 前記誘電体磁器組成物に不純物として含まれるSiは、BaTiO3からなる主成分を100molとしたときにSiO2換算で1.0mol以下であることを特徴とする請求項8に記載の積層セラミックコンデンサ。
- 前記誘電体磁器組成物は、焼結温度が1030℃以下で緻密化させることが可能であることを特徴とする請求項8に記載の積層セラミックコンデンサ。
- 前記誘電体セラミック層の層厚が2μm以下であることを特徴とする請求項8記載の積層セラミックコンデンサ。
- 前記誘電体磁器組成物は、焼結温度が1030℃以下で緻密化させることが可能であることを特徴とする請求項9に記載の積層セラミックコンデンサ。
- 前記誘電体セラミック層の層厚が2μm以下であることを特徴とする請求項9又は10に記載の積層セラミックコンデンサ。
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