CN1447780A - 介电陶瓷组合物和电子器件 - Google Patents
介电陶瓷组合物和电子器件 Download PDFInfo
- Publication number
- CN1447780A CN1447780A CN01814363A CN01814363A CN1447780A CN 1447780 A CN1447780 A CN 1447780A CN 01814363 A CN01814363 A CN 01814363A CN 01814363 A CN01814363 A CN 01814363A CN 1447780 A CN1447780 A CN 1447780A
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- Prior art keywords
- minor component
- dielectric
- ceramic composition
- oxide compound
- dielectric ceramic
- Prior art date
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- 239000003989 dielectric material Substances 0.000 title abstract description 9
- 229910052573 porcelain Inorganic materials 0.000 title abstract 2
- 150000001875 compounds Chemical class 0.000 claims abstract description 71
- 239000000203 mixture Substances 0.000 claims abstract description 68
- 229910052712 strontium Inorganic materials 0.000 claims abstract description 14
- 229910052751 metal Inorganic materials 0.000 claims abstract description 13
- 229910052788 barium Inorganic materials 0.000 claims abstract description 11
- 229910052804 chromium Inorganic materials 0.000 claims abstract description 8
- 229910052749 magnesium Inorganic materials 0.000 claims abstract description 8
- 229910052750 molybdenum Inorganic materials 0.000 claims abstract description 6
- 229910052758 niobium Inorganic materials 0.000 claims abstract description 6
- 229910052715 tantalum Inorganic materials 0.000 claims abstract description 6
- 229910052721 tungsten Inorganic materials 0.000 claims abstract description 6
- 229910052720 vanadium Inorganic materials 0.000 claims abstract description 6
- 239000000919 ceramic Substances 0.000 claims description 51
- 239000000470 constituent Substances 0.000 claims description 43
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 23
- 239000003990 capacitor Substances 0.000 claims description 23
- 238000006243 chemical reaction Methods 0.000 claims description 13
- 229910052759 nickel Inorganic materials 0.000 claims description 13
- 239000004020 conductor Substances 0.000 claims description 10
- 229910000990 Ni alloy Inorganic materials 0.000 claims description 8
- 239000004615 ingredient Substances 0.000 claims description 7
- 229910052791 calcium Inorganic materials 0.000 claims description 6
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- 229910004762 CaSiO Inorganic materials 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 229910000881 Cu alloy Inorganic materials 0.000 description 1
- IOVCWXUNBOPUCH-UHFFFAOYSA-M Nitrite anion Chemical compound [O-]N=O IOVCWXUNBOPUCH-UHFFFAOYSA-M 0.000 description 1
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- 241000779819 Syncarpia glomulifera Species 0.000 description 1
- KXKVLQRXCPHEJC-UHFFFAOYSA-N acetic acid trimethyl ester Natural products COC(C)=O KXKVLQRXCPHEJC-UHFFFAOYSA-N 0.000 description 1
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- RBNWAMSGVWEHFP-UHFFFAOYSA-N trans-p-Menthane-1,8-diol Chemical compound CC(C)(O)C1CCC(C)(O)CC1 RBNWAMSGVWEHFP-UHFFFAOYSA-N 0.000 description 1
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- 229910052726 zirconium Inorganic materials 0.000 description 1
Classifications
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- H01G4/08—Inorganic dielectrics
- H01G4/12—Ceramic dielectrics
- H01G4/1209—Ceramic dielectrics characterised by the ceramic dielectric material
- H01G4/1236—Ceramic dielectrics characterised by the ceramic dielectric material based on zirconium oxides or zirconates
- H01G4/1245—Ceramic dielectrics characterised by the ceramic dielectric material based on zirconium oxides or zirconates containing also titanates
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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
- C04B35/48—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 zirconium or hafnium oxides, zirconates, zircon or hafnates
- C04B35/49—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 zirconium or hafnium oxides, zirconates, zircon or hafnates containing also titanium oxides or titanates
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- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/63—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B using additives specially adapted for forming the products, e.g.. binder binders
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- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B3/00—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties
- H01B3/02—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of inorganic substances
- H01B3/12—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of inorganic substances ceramics
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
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- H01G4/002—Details
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- H01G4/1209—Ceramic dielectrics characterised by the ceramic dielectric material
- H01G4/1218—Ceramic dielectrics characterised by the ceramic dielectric material based on titanium oxides or titanates
- H01G4/1227—Ceramic dielectrics characterised by the ceramic dielectric material based on titanium oxides or titanates based on alkaline earth titanates
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- C04B2235/3206—Magnesium oxides or oxide-forming salts thereof
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- C04B2235/3213—Strontium oxides or oxide-forming salts thereof
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- C04B2235/3224—Rare earth oxide or oxide forming salts thereof, e.g. scandium oxide
- C04B2235/3225—Yttrium oxide or oxide-forming salts thereof
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- C04B2235/3227—Lanthanum oxide or oxide-forming salts thereof
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Abstract
一种介电陶瓷组合物,其包含含有由组成分子式{(Ca1-xMex)O}·(Zr1-yTiy)O2表示的介电氧化物的主成分和包含选自V、Nb、W、Ta、Mo和Cr的氧化物以及在烧成后变成这些金属氧化物的化合物中的至少一种的第一辅助成分,其中,在所述主成分中包含的分子式中的符号Me是Sr、Mg和Ba的至少之一,符号m、x和y表示在所述主成分中包含的分子式中的组成摩尔比,其为0.8≤m≤1.3、0≤x≤1.00和0.1≤y≤0.8,并且第一辅助成分与100摩尔主成分的比例用氧化物中的金属元素表示满足0.01原子%≤第一辅助成分<5原子%。
Description
发明背景
技术领域
本发明涉及例如用作多层陶瓷电容器的介电层的介电陶瓷组合物,和使用所述介电陶瓷组合物作为介电层的电子器件。
技术背景
通过在由预定的介电陶瓷组合物制备的陶瓷生坯片印刷导电浆料,堆叠其上印刷了导电浆料的多个生坯片,并整体烧成这些生坯片和内电极,形成作为电子器件的一个实例的多层陶瓷电容器。
传统的介电陶瓷组合物在具有低氧气分压的中性或还原气氛中烧成时,具有被还原并变成半导体的性质。所以,在生产多层陶瓷电容器时,不可避免地在具有高氧气分压的氧化气氛中烧成。由于这一原因,作为与介电陶瓷组合物一起烧成的内电极材料,一直要求使用贵金属(例如钯和铂),它们在烧结介电陶瓷组合物的温度下不熔化并且在氧化气氛中烧成时不会被氧化。这已经成为实现生产低价格多层陶瓷电容器的一个大障碍。
为了使用便宜的贱金属(例如镍和铜)作为内电极材料,必须开发即使在中性或还原气氛中烧成也不会变成半导体的介电陶瓷组合物,即具有优良抗还原性并具有足够的比介电常数和在烧成后具有优异介电特性(例如具有小电容-温度变化率)的介电陶瓷组合物。
传统上,已经对能使用贱金属作为内电极材料的介电陶瓷组合物提出了各种方案。
例如,日本未审专利公开No.11-224827公开了一种介电陶瓷组合物,其由组成表示为(Ca1-xMex)m·(Zr1-yTiy)O3(注意:0.90<m<1.10,0.1≤x≤0.9,0≤y≤0.5)的介电氧化物制成的主成分和SiO2、B2O3、Mn2O3和Ln2O3组成(注意:Ln是至少一种或两种选自Sc、Y、La、Ce、Pr、Nd、Pm、Sm、Eu、Gd、Tb、Dy、Ho、Er、Tm、Yb和Lu的元素),其中,在该介电陶瓷组合物中SiO2+B2O3的含量比为0.1-5重量%,Mn2O3的含量比为0.1-3.0原子%,Ln2O3的含量比为0.03-1.0原子%。
日本未审专利公开No.60-131708也公开了一种介电陶瓷组合物,其由组成表示为(Ca1-xSrx)m·(Zr1-yTiy)O3(注意:0.85<m<1.30,0≤x<0.6,0≤y<0.6)的介电氧化物制成的主成分和zMnO2组成(注意:相对于1.00的主成分,重量比为0.005<z<0.08)。
此外,日本未审专利公开No.57-37081公开了一种介电陶瓷组合物,其由组成表示为(Ca1-xBax)m·ZrO3(注意:0.85<m<1.30,0<x<0.2)的介电氧化物制成的主成分和zMnO2组成(注意:相对于1.00的主成分,重量比为0.005<z<0.08)。
而且,日本未审专利公开No.63-126117公开了一种介电陶瓷组合物,其含有组成表示为(Ca1-xSrx)m·(Zr1-yTiy)O3(注意:0.85<m<1.30,0≤x<0.6,0≤y<0.6)的介电氧化物和相对于100重量份主成分为0.5-8重量份的MnO2和0.5-8重量份的玻璃组分(注意:该玻璃组分使用预定摩尔比的Li2O、RO(注意:R是选自Ba、Sr、Ca、Mg的至少一种)、(Ti,Si)O2和Al2O3)。
但是,在上述公开中描述的任何介电陶瓷组合物都有缺点,即烧成后低频使介电性能(容量变化、介电损耗)恶化,或者绝缘电阻的加速寿命短,以及在使用该介电陶瓷组合物生产具有贱金属如镍内电极的多层陶瓷电容器时,所得的多层陶瓷电容器的可靠性变差。
发明内容
本发明的目的是提供一种在烧成时具有优异抗还原性且在烧成后具有优异低频介电特性的介电陶瓷组合物,而且其能够改善绝缘电阻的加速寿命。本发明的另一个目的是提供一种具有优异容量-温度特性和高可靠性的片式电容器和其它电子器件。
为了实现上述目的,提出了一种介电陶瓷组合物,其包含:
主成分,其包括由组成分子式{(Ca1-xMex)O}·(Zr1-yTiy)O2表示的介电氧化物,和
第一副成分,其包括选自V、Nb、W、Ta、Mo和Cr的氧化物以及在烧成后变成这些金属氧化物的化合物中的至少一种,
其中,在主成分中包含的分子式中的符号Me是Sr、Mg和Ba的至少之一,
符号m、x和y表示在主成分中包含的分子式中的组成摩尔比,为0.8≤m≤1.3、0≤x≤1.00和0.1≤y≤0.8,并且
第一副成分转换成氧化物中的金属元素与100摩尔主成分的比例为0.01原子%≤第一副成分<5原子%。
优选地,根据本发明的介电陶瓷组合物还包含第三副成分,其包含Si、M(注意:M是Ba、Ca、Sr和Mg中的至少一种元素)、Li和B的氧化物和在烧成后变成这些元素的氧化物的化合物的至少一种;并且其中,第三副成分折算为氧化物与100摩尔主成分的比例为0摩尔<第三副成分<15摩尔。
第三副成分的特别优选的状态如下所述。更优选地,根据本发明的介电陶瓷组合物还包含第三副成分,其包括Si和Sr的氧化物和在烧成后变成这些元素的氧化物的化合物的至少一种;并且其中第三副成分折算为氧化物与100摩尔主成分的比例为0摩尔<第三副成分<15摩尔。第三副成分主要用作烧结助剂。
优选地,在根据本发明的介电陶瓷组合物中,在至少25-125℃的温度范围内,静电容量随温度的变化率(ΔC)为-3000-0ppm/℃,优选为-2000-0ppm/℃,更优选为-1000-0ppm/℃。注意:静电容量C的参比温度为25℃。
为了实现以上目的,本发明的电子器件包含由任何以上介电陶瓷组合物构成的介电层。
优选地,本发明的电子器件包含电容器元件主体,其中交替堆叠介电层和内电极层。
优选地,在本发明的电子器件中,在内电极层中包含的导电材料是镍或镍合金。
通过向含有具有特定组成的介电氧化物的主成分中加入预定量的特定第一副成分,本发明的介电陶瓷组合物在烧成时具有优异的抗还原性,在烧成后具有优异的容量-温度特性,其中,与没有加入第一种副成分的情况相比,抑制了低频介电色散(例如在160℃和100Hz下的介电损耗)并改善了绝缘电阻的加速寿命(高温负载寿命)。
在本发明的电子器件如片式电容器中,由于提供了由本发明的介电陶瓷组合物构成的介电层,获得了优异的容量-温度特性,抑制了低频介电色散并改善了绝缘电阻的加速寿命(高温负载寿命),结果,改善了电子器件的可靠性。
附图简述
图1是本发明的一个实施方案的多层陶瓷电容器的截面图。
图2是在作为第三副成分的(Srp,Ca1-p)SiO3中Sr的含量比与电容器样品中初始绝缘电阻(IR)的合格率的关系图。
实施本发明的最佳方式
以下将基于在附图中表明的优选实施方案来解释本发明。
在本实施方案中,表示在图1中的多层陶瓷电容器将描述为电子器件的一个实例,并且将解释其结构和生产方法。
多层陶瓷电容器
如图1所示,作为本发明的一个实施方案的电子器件的多层陶瓷电容器1包含电容器元件主体10,其中介电层2和内电极层3交替叠层。电容器元件主体10的两端部分形成一对外电极4,分别连接到交替排列在元件主体10内的内电极3上。电容器元件主体10的形状不特别限定,但是通常制成平行六面体形。此外,电容器的尺寸不特别限定并且可以是根据用途的合适尺寸,但是,通常大约为(0.6-5.6mm)×(0.3-5.0mm)×(0.3-1.9mm)。
叠层内电极层3,使得其各个端面交替暴露到电容器元件主体10的两个相对端部的表面上。外电极对4在电容器元件主体10的两个端部形成,并连接到交替排列的内电极层3的暴露端面上,从而构成电容电路。
介电层2
介电层2包含本发明的介电陶瓷组合物。
根据本发明的介电陶瓷组合物至少包含含有由组成分子式{(Ca1-xMex)O}·(Zr1-yTiy)O2表示的介电氧化物的主成分和特定的第一副成分。此时,氧(O)含量可以与上式的化学剂量组成略有不同。
在上述组成分子式中,x满足0≤x≤1.00。x表示Me原子数量(注意:Me是Sr、Mg和Ba的至少一种),并且通过改变x,即Me/Ca比,可以自由地使晶体的相变点移动。因此,可以自由控制容量-温度系数和比介电常数。注意:在本发明中,Ca与Me的比例可以是任意的并且可以只含有二者之一。
在上式中,0.1≤y≤0.8。y表示Ti原子数,并且通过带有ZrO2,抗还原性往往变得更强,与TiO2相比,ZrO2难以被还原。在上式中,0.8≤m≤1.3,优选的是0.970≤m≤1.030。通过使m为0.8或更大,防止了在还原气氛中烧成时变成半导体,并且通过使m为1.3或更小,即使当烧成温度不高时也能获得致密的烧结体。
本发明的介电陶瓷组合物与传统介电陶瓷组合物不同的是y的范围是0.1≤y≤0.8并加入预定量的预定的第一副成分。通过加入预定量的预定的第一副成分,当作为主成分的y在0.1≤y≤0.8范围内时,在低温下烧成而不降低介电特性成为可能,即使当介电层变薄,也可以改善绝缘电阻的加速寿命(高温负载寿命)并抑制低频介电色散,所以可以大幅度提高可靠性。结果,可以使该电容器小型化、大容量。
在本发明中,第一副成分含有元素周期表第5族元素(V、Nb、Ta)的氧化物、周期表第6族元素(Cr、Mo、W)的氧化物和在烧成后变成这些氧化物的化合物的至少一种。第一副成分作为降低烧结温度和改善绝缘电阻加速寿命(高温负载寿命)并抑制低频介电色散的物质。
在本发明中,第一副成分折算为氧化物中的金属元素与100摩尔主成分的比例为0.01原子%≤第一副成分<5原子%。通过折算为氧化物中的金属元素,把第一副成分的比例设定在0.01原子%≤第一副成分<5原子%范围内,当y在0.1≤y≤0.8时,可以改善绝缘电阻的加速寿命(高温负载寿命)并抑制低频介电色散。
根据本发明的介电陶瓷组合物还优选加入第三副成分,其含有Si、M(注意M是Ba、Ca、Sr和Mg中的至少一种元素)、Li和B的氧化物(例如SiO2、MO、Li2O和B2O3)和在烧成后变成这些氧化物的化合物的至少一种。第三副成分主要作为烧结助剂并且在层变薄时还影响改善初始绝缘电阻(IR)的次品率的作用。在次品率改善方面,优选的是含有Si和Sr的氧化物(例如SiO2、SrO、SrSiO3)和在烧成后变成这些氧化物的化合物中的至少一种,特别优选的是含有SrSiO3。折算为氧化物,第三副成分与100摩尔主成分的比例为0摩尔<第三副成分<15摩尔,优选为0.2摩尔≤第三副成分≤6摩尔。通过使第三副成分的加入量大于0摩尔,可以有效降低初始IR次品率,而通过使该加入量小于15摩尔,比介电常数可以压低并保证足够的电容量。
注意,本发明的介电陶瓷组合物还可以加入第二副成分,其含有Mn的氧化物(例如MnO)和通过烧成变成Mn的氧化物的化合物(例如MnCO3)的至少一种。第二副成分赋予加速烧结并改善高温负载寿命的作用,此外当使介电层2更薄时,例如约4微米左右,则具有降低初始绝缘电阻次品率的作用。当加入第二副成分时,折算为氧化物中的金属元素,第二副成分与100摩尔主成分的比例为0摩尔≤第二副成分<4摩尔,优选为0.05摩尔≤第二副成分≤1.4摩尔。当第二副成分的加入量为4摩尔或更多时,不易获得初始绝缘电阻,而当第二副成分的加入量在0摩尔≤第二副成分<4摩尔时,加入量越大,高温负载寿命改善越好,此外,可以降低初始IR次品率,而加入量越小,容量-温度变化率越小。
本发明的介电陶瓷组合物还可以加入第四副成分,其含有R(注意:R是Sc、Y、La、Ce、Pr、Nd、Pm、Sm、Eu、Gd、Tb、Dy、Ho、Er、Tm、Yb和Lu中的至少一种元素)的氧化物。第四副成分赋予改善高温负载寿命的作用,当层变薄时还具有改善初始IR次品率的作用。在次品率改善方面,优选含有Sc、Y、Ce、Dy、Ho、Er、Tm、Yb和Lu的氧化物的至少一种。当加入第四副成分时,第四副成分与100摩尔主成分的比例为0.02原子%≤第四副成分<2原子%,优选为0.02原子%≤第四副成分≤1原子%。
注意,图1中所示的介电层2的层数、厚度和其它条件可以根据目的和用途适当确定。还优选介电层2由晶粒和晶界相组成,并且介电层2的晶粒的平均颗粒直径为0.2-5微米左右。通常,晶界相含有包括介电材料或内电极材料的材料的氧化物、单独加入的材料的氧化物、还含有在生产步骤中作为杂质混入其中的材料的氧化物作为其组成,并且通常由玻璃或玻璃化材料组成。
内电极层3
在内电极层3中包含的导电材料不特别限定,并且可以使用贱金属,因为介电层2的成分具有抗还原性。作为贱金属,Ni或Ni合金是优选的。作为Ni合金,至少一种选自Mn、Cr、Co和Al的元素与Ni的合金是优选的,并且合金中的Ni含量优选为95重量%或更多。应当注意,在Ni或Ni合金中可以包含约0.1重量%或更少各种痕量组分,如P、Fe和Mg。内电极层的厚度可以根据用途等适当确定,并且通常为0.5-5微米,特别是1-2.5微米左右。
外电极4
在外电极4中包含的导电材料不特别限定,并且通常使用Cu、Cu合金、Ni或Ni合金等。注意,自然可以使用Ag、Ag-Pd合金。应当注意,在本实施方案中,使用便宜的Ni、Cu或它们的合金。外电极4的厚度可以根据用途等适当确定,但是10-50微米左右通常是优选的。
多层陶瓷电容器的生产方法
用与传统的多层陶瓷电容器相同的方法来生产使用本发明的介电陶瓷组合物的多层陶瓷电容器,即通过通常的印刷法或使用浆料的坯片制造方法制备生片式元件,烧结该生片式元件,印刷或转印外电极并烧成。下面将具体解释生产方法。
首先,分别制备介电层浆料、内电极浆料和外电极浆料。
介电层浆料
所述介电层浆料可以是有机基涂料,其通过混捏介电陶瓷材料和有机载体获得,也可以是水基涂料。
构成主成分的材料和构成第一至第四副成分的材料用于上述本发明的介电陶瓷组合物的组成的介电材料。
作为构成主成分的材料,使用Sr、Ca、Ba、Ti、Zr和Mg的氧化物和/或通过烧成变成氧化物的化合物。
作为构成第一副成分的材料,使用选自V、Nb、W、Ta、Cr、Mo和Cr的氧化物至少之一的至少一种单一氧化物或复合氧化物和在烧成后变成这些氧化物的化合物。
作为构成第二副成分的材料,使用Mn的氧化物和通过烧成变成Mn的氧化物的化合物的至少一种单一氧化物或复合氧化物。
作为构成第三副成分的材料,使用Si、M(注意M是Ba、Ca、Sr和Mg中的至少一种元素)、Li和B的氧化物和在烧成后变成这些氧化物的至少一种。
作为构成第四副成分的材料,使用R(注意:R是Sc、Y、La、Ce、Pr、Nd、Pm、Sm、Eu、Gd、Tb、Dy、Ho、Er、Tm、Yb和Lu中的至少一种元素)的氧化物。
注意,通过作为烧成变成氧化物的化合物,可以提及例如碳酸盐、亚硝酸盐、草酸盐、有机金属化合物等。不用说,氧化物与烧成后变成氧化物的化合物可以一起使用。可以确定介电材料中每种化合物的含量,以便在烧成后达到上述介电陶瓷组合物的组成。作为这些材料的粉末,通常使用平均颗粒直径为0.0005-5微米左右的那些。
有机载体通过在有机溶剂中溶解粘合剂获得。用于有机载体的粘合剂不特别限制,并且可以适当地选自通常的粘合剂,如乙基纤维素、聚乙烯基丁缩醛。此时所用的有机溶剂也不特别限定,并且可以根据所用方法如印刷方法、生片方法适当地选自萜品醇、丁基卡必醇、丙酮和甲苯。
通过在水中溶解水溶性粘合剂、分散剂等获得水溶性涂料。水溶性粘合剂不特别限定并且可以适当地选自聚乙烯醇、纤维素、水溶性丙烯酸树脂、乳液等。
内电极浆料、外电极浆料
通过把由上述各种导电金属和合金构成的导电材料、在烧成后变成以上导电材料的各种氧化物、有机金属化合物、树脂酸盐等与上述有机载体一起混捏合,来制备内电极层浆料。也可以用与上述内电极浆料中相同的方法制备外电极浆料。
在每种上述浆料中的有机载体含量不特别限定,并且可以是常用含量,即例如1-5重量%左右的粘合剂,10-50重量%左右的溶剂。所述浆料还可以根据需要加入选自分散剂、增塑剂、电介质、绝缘材料等的添加剂。
在使用印刷法时,电介质浆料和内电极浆料通过堆叠在聚对苯二甲酸乙二酯等制成的基材上来印刷,然后切成预定的形状,并从基材上取下,以获得生片式器件。另一方面,在使用生片方法时,使用电介质浆料形成生坯片,内电极浆料印刷在其上,然后把二者叠层以形成生片式器件。
然后,所述生片式元件经过脱脂(binder removing)处理和烧结。
脱脂处理
可以在通常条件下进行脱脂处理,但是特别是当使用贱金属如Ni和Ni合金作为内电极层的导电材料时,所述条件优选的是在空气气氛中,升温速度为5-300℃/小时,更优选为10-100℃/小时,保温温度为180-400℃,更优选为200-300℃,保温时间为0.5-24小时,更优选为5-20小时。
烧成
生片式器件的烧成气氛可以根据内电极浆料中的导电材料种类适当确定,但是在使用贱金属如Ni和Ni合金作为导电材料时,烧成气氛中的氧分压优选为10-10-10-3Pa,更优选为10-10-6×10-5Pa。当烧成时的氧分压太低时,内电极的导电材料产生异常烧结并且最终破坏;而当该氧分压太高时,则内电极容易被氧化。
烧成时的保温温度为1000-1400℃,更优选为1200-1380℃。这是因为当保温温度太低时,致密化不充分,而当保温温度太高时,则由于内电极材料的异常烧结产生电极断裂,或者由于内电极材料的分散导致容量-温度特性降低。
除了以上条件之外的烧成条件优选为:升温速度50-500℃/小时,更优选为200-300℃/小时,保温时间是0.5-8小时,更优选为1-3小时,冷却速度为50-500℃/小时,更优选为200-300℃/小时,并且烧成气氛优选为还原气氛,优选使用氮气和氢气的湿混合气体作为气氛气体。
当在还原气氛中烧结时,优选对电容器片式烧结体进行退火(热处理)。
退火(热处理)
退火是重新氧化介电层的过程,并且可能因此提高绝缘电阻。退火气氛的氧分压优选为10-4Pa或更大,更优选为10-1-10Pa。当氧分压太低时,介电层2的重新氧化变得困难,而当氧分压太高时,内电极3容易被氧化。
在退火时的保温温度优选为500-1100℃,但是不特别限制。当保温温度太低时,介电层的重新氧化往往不足,这导致绝缘电阻的降低并且其加速寿命也变短。而当保温温度太高时,不仅由于内电极层被氧化而使容量下降,而且发生与介电基体的反应,因此容量-温度特性、绝缘电阻和加速寿命容易恶化。应当注意,所述退火可以仅由升温步骤和降温步骤构成。在这种情况下,保温时间为0,并且保温温度与最高温度是同义的。
除了以上条件以外的退火条件优选为:保温时间0-20小时,更优选为6-10小时,冷却速度50-500℃/小时,更优选为100-300℃/小时,并且优选使用一种气氛气体进行退火,例如湿N2气。
注意到在上述脱脂处理和退火处理中,按用于上述烧成相同的方法,可以使用例如加湿器等为氮气或混合气体加湿。在这种情况下,水温优选为0-75℃。
脱脂处理、烧结和退火也可以连续进行或者单独进行。当连续进行这些处理时,优选的是在脱脂处理后,改变气氛而不冷却,然后提高温度到烧成保温温度进行烧成,然后当温度冷却达到退火保温温度时改变气氛以进行退火。另一方面,当分别进行时,优选的是在氮气或湿氮气气氛中使温度升高到脱脂保温温度后进行烧结,然后改变气氛继续升高温度,并在温度冷却到退火保温温度时,再改变气氛为氮气或湿氮气,以继续冷却。在退火过程中,在氮气气氛中使温度升高到保温温度后也可以改变气氛,或者整个退火处理都在湿氮气气氛中进行。
这样获得的电容器元件烧结体例如使用滚筒抛光或喷砂等进行端面抛光,然后印刷或转印外电极浆料并烧成,形成外电极4。外电极浆料的烧成条件优选的是例如在湿氮气和氢气的混合气体中在600-800℃烧成10分钟-1小时左右。根据需要,外电极对4的表面可以通过钎焊等形成覆盖层。
这样生产的本实施方案的多层陶瓷电容器1通过钎焊安装在印刷电路板上并用于各种电子设备中。
以上解释了本发明的实施方案,但是,本发明不限于这些实施方案并且可以在本发明范围内用各种方法来实施。
例如,在以上实施方案中,取多层陶瓷电容器作为本发明的电子器件的实例,但是,本发明的电子器件不限于多层陶瓷电容器,并且可以是含有由具有上述组成的介电陶瓷组合物构成的介电层的任何器件。
以下将以实施例进一步解释本发明,其中将更具体地实施本发明的实施方案。应该注意,本发明不限于这些实施例。
实施例1
首先,作为生产介电材料的原料,制备分别具有0.1-1微米平均颗粒直径的主成分(SrCO3、CaCO3、TiO2、ZrO2、MgO)和第一至第三副成分的材料。碳酸盐(第二副成分:MnCO3)用作MnO的材料,氧化物(第一副成分:V2O5,第三副成分:SiO2+CaO)用于其它材料。注意,对于第三副成分SiO2+CaO,通过使用对SiO2和CaO用球磨机进行16小时湿混、干燥后在空气中在1150℃进行烧成、再用球磨机进行100小时湿粉碎获得的CaSiO3,可以获得相同的特征。
称重上述材料,使得烧成后的组成具有以组成式{(Ca1-xSrx)O}m·(Zr1-yTiy)O2(主成分)+V2O5(第一副成分)+MnCO3(第二副成分)+(SiO2+CaO)(第三副成分)在表1和表2中所示的混合比例,然后把它们的每一种经过球磨机湿混约16小时并干燥,以获得介电陶瓷组合物(介电材料)。
使用球磨机把100重量份的如此获得的干介电材料与4.8重量份的丙烯酸树脂、40重量份的二氯甲烷、20重量份的乙酸甲酯、6重量份的矿油精和4重量份的丙酮混合,来制备一种浆料,以获得一种介电层浆料。
然后,使用三辊混捏机混捏100重量份平均颗粒直径为0.2-0.8微米的Ni颗粒、40重量份有机载体(8重量份的乙基纤维素溶解在92重量份的丁基卡必醇中)和10重量份的丁基卡必醇,获得内电极浆料。
然后,通过混捏100重量份平均颗粒直径为0.5微米的Cu颗粒、35重量份有机载体(8重量份的乙基纤维素树脂溶解在92重量份的丁基卡必醇中)和7重量份的丁基卡必醇,获得外电极浆料。
然后,使用以上介电层浆料在PET薄膜上形成厚度为6微米的生片,在其上印刷内电极浆料,然后把生片从PET薄膜上剥离。
然后,把如此获得的生片和保护生片(其上未印刷内电极浆料)叠层,并加压,获得生片式器件。在具有内电极的片中叠层数量为4。
然后把生片切成预定的尺寸并进行脱脂处理、烧成和退火(热处理),以获得多层陶瓷烧结体。脱脂处理在空气气氛中,升温速度为15℃/小时,保温温度为280℃,保温时间为8小时的条件下进行。烧成在升温速度为200℃/小时,保温温度为1200-1380℃,保温时间为2小时,冷却速度为300℃/小时,在N2+H2的混合气体气氛下(氧气分压调节为2×10-7-5×10-4Pa)的条件下进行。退火在保温温度为900℃,保温时间为9小时,冷却速度为300℃/小时,在湿N2气氛下(氧气分压为3.54×10-2Pa)的条件下进行。
注意,使用水温为35℃的加湿器在烧成和退火时为气氛气体加湿。
然后,把烧成的多层陶瓷烧结体的端面通过喷砂抛光后,把外电极浆料转印到端面上,通过在湿N2+H2混合气体气氛中在800℃烧成10分钟形成外电极,以获得具有图1所示结构的多层陶瓷电容器样品。所获得的电容器样品的尺寸为3.2mm×1.6mm×0.6mm,其中,夹在两个内电极之间的介电层的层数为4,其厚度为4微米且内电极层的厚度为2微米。对各个样品进行以下性能评价。
比介电常数(ε)、介电损耗(tanδ)、绝缘电阻(IR)
在1MHz频率和1Vrms的输入信号水平(测量电压)的条件下,用数字LCR计(由YHP公司制造的4274A)在25℃的参比温度下,对电容器样品测定电容量和介电损耗(tanδ,单位为%)。然后,由所获得的静电容量、电极尺寸和电容器样品的电极间距计算比介电常数(ε,没单位)。在25℃对电容器样品施加DS 50V 60秒后,使用绝缘电阻测定仪(由Adanctest Co.制造的R8340A)测定比电阻ρ,并由电容器样品的测定值、电极面积和厚度计算,获得绝缘电阻(IR,单位为Ωcm)。结果表示在表1和表2中。由使用n=10的电容器样品数的测定值的平均值,获得了比介电常数ε、比电阻ρ和介电损耗tanδ的各个值。
静电容量的温度特性
使用LCR计对电容器样品测定1MHz和1V电压的静电容量,并研究当参比温度设定为25℃时在25-125℃温度范围内,静电容量关于温度的变化率是否满足-3000-0ppm/℃。结果表示在表1和表2中。由以下公式计算容量-温度常数τC(1MHz)(ppm/℃)。注意,在公式中,C125表示在125℃下的静电容量,C25表示在25℃(1MHz)下的静电容量。
注意,在公式2中用相同方式表示了在100Hz下的容量温度常数τC(100Hz)。
τC(1MHz)={(C125-C25)/C25}×(1/100)
....公式1
τC(100Hz)={(C125-C25)/C25}×(1/100)
....公式2
高温负载寿命(绝缘电阻的加速寿命)
通过使其保持在200℃施加15-60V/μm的直流电压的状态下,对电容器样品测定高温负载寿命。对10个电容器样品(介电层厚度为4微米)测定高温负载寿命并通过测定平均寿命进行评价。结果表示在表1和表2中。当使介电层更薄时,高温负载寿命是特别重要的,并且从施加开始时直到电阻降低一个数位(digit)的时间在评价中被定义为寿命。
注意,第一副成分的原子%和第二副成分的摩尔数是相对于100摩尔上述主成分的比例,是折算为金属元素表示的值。第三副成分的摩尔数是相对于100摩尔主成分的比例,是折算为氧化物表示的值。“mE+n”在表中的比电阻(ρ)值中表示“m×10+n”。
表1
表1
注:在主成分中m=1
样品编号 | 第一副成分 | 烧成温度(℃) | 比介电常数ε | 比电阻ρ(Ωcm) | 容量-温度特性τC(1MHz)(ppm/℃) | ΔτC(=τC100Hz-τC1MHz)(ppm/℃) | 介电损耗tanδ(%)(@100Hz.160℃) | 高温负载寿命(时间) | ||
种类 | 原子% | |||||||||
1 | 对比实施例 | V | 0 | 1300 | 126 | 8E+13 | -1540 | 140 | 2.3 | 0.9 |
2 | 实施例 | V | 0.1 | 1300 | 123 | 7E+13 | -1550 | 30 | 0.36 | 147 |
在主成分中x=0.4且y=0.6
在第二副成分(MnCO3)中折算为金属元素的摩尔数为0.37
第三副成分(SiO2+CaO)的摩尔数为(0.4+0.4)摩尔
测量高温负载寿命的条件:200℃,DC15V/μm
表2
表2
注:在主成分中m=1
样品编号 | 第一副成分 | 烧成温度(℃) | 比介电常数ε | 比电阻ρ(Ωcm) | 容量-温度特性τC(1MHz)(ppm/℃) | ΔτC(=τC100Hz-τC1MHz)(ppm/℃) | 介电损耗tanδ(%)(@100Hz,160℃) | 高温负载寿命(时间) | ||
种类 | 原子% | |||||||||
3 | 对比实施例 | V | 0 | 1300 | 80 | 2.3E+14 | -740 | 80 | 3.1 | 0.3 |
4 | 实施例 | V | 0.05 | 1300 | 82 | 5E+14 | -740 | 40 | 0.6 | 3 |
5 | 实施例 | V | 0.1 | 1300 | 79 | 5.8E+14 | -740 | 10 | 0.3 | 5 |
6 | 实施例 | V | 0.2 | 1280 | 84 | 6.5E+14 | -750 | 20 | 0.3 | 33 |
7 | 实施例 | V | 1 | 1280 | 81 | 9E+13 | -740 | 10 | 0.4 | 124 |
8 | 实施例 | V | 2 | 1280 | 83 | 3.3E+13 | -750 | 20 | 0.4 | >250 |
9 | 对比实施例 | V | 5 | 1280 | -* | -* | -* | -* | -* | -* |
在主成分中x=0.4且y=0.36
在第二副成分(MnCO3)中折算为金属元素的摩尔数为0.37
第三副成分(SiO2+CaO)的摩尔数为(0.4+0.4)摩尔
测量高温负载寿命的条件:200℃,DC30V/μm
*…变成半导性并且不能用作电容器
从表1和表2中所示的结果,对于第一副成分的加入量,可以清楚以下事实。当根本不加V时,例如在样品1和样品3中,高温负载寿命变得非常短。当V的加入量太大时,如在样品5中,其变成半导性的并且不能用作电容器。另一方面,在样品2和4-8中,其中包含预定量的第一副成分,证实获得了具有足够比介电常数和绝缘电阻、即使在还原气氛中烧成也不还原、不氧化作为内电极材料的镍并具有优异的抗还原性的介电陶瓷组合物。还证实容量-温度特性是优异的,而且可以抑制低频介电色散(在100Hz和160℃下的tanδ小,在1MHz和100Hz的容量-温度系数差ΔτC小),并且可以改善高温负载寿命(绝缘电阻的加速寿命)。注意,样品2和4-8是本发明的实施例,样品1和3是本发明的对比实施例。
实施例2
用与实施例1相同的方法制备电容器样品,但是使用W的氧化物代替V的氧化物并且烧成后的组成变成表3中所示的混合比。进行相同的评价。结果表示在表3中。
表3
表3
注:在主成分中m=1
样品编号 | 第一副成分 | 烧成温度(℃) | 比介电常数ε | 比电阻ρ(Ωcm) | 容量-温度特性τC(1MHz)(ppm/℃) | ΔτC(=τC100Hz-τC1MHz)(ppm/℃) | 介电损耗tanδ(%)(@100Hz,160℃) | 高温负载寿命(时间) | ||
种类 | 原子% | |||||||||
10 | 对比实施例 | W | 0 | 1300 | 55 | 8.1E+14 | -520 | 120 | 2.8 | 0.2 |
11 | 实施例 | W | 0.1 | 1300 | 53 | 1.2E+15 | -520 | 20 | 0.3 | 8 |
12 | 实施例 | W | 0.2 | 1280 | 58 | 9E+14 | -520 | 30 | 0.4 | 22 |
13 | 实施例 | W | 1 | 1280 | 56 | 3.4E+14 | -510 | 10 | 0.3 | 89 |
14 | 实施例 | W | 2 | 1280 | 52 | 9E+13 | -520 | 20 | 0.3 | 150 |
15 | 对比实施例 | W | 5 | 1280 | -* | -* | -* | -* | -* | -* |
在主成分中x=0.4且y=0.24
在第二副成分(MnCO3)中折算为金属元素的摩尔数为0.37
第三副成分(SiO2+CaO)的摩尔数为(0.4+0.4)摩尔
测量高温负载寿命的条件:200℃,DC60V/μm
*…变成半导性并且不能用作电容器
从表3所示的结果,对于第一副成分的加入量,可以清楚以下事实。当根本不加W时,例如在样品10中,高温负载寿命变得非常短。当W的加入量太大时,如在样品15中,其变成半导性的并且不能用作电容器。另一方面,在样品11-14中,其中包含预定量的第一副成分,证实获得了具有足够比介电常数和绝缘电阻,即使在还原气氛中烧成也不还原,不氧化作为内电极材料的镍并具有优异的抗还原性的介电陶瓷组合物。还证实容量-温度特性是优异的,而且可以抑制低频介电色散并且可以改善高温负载寿命。注意,样品11-14是本发明的实施例,样品10和15是本发明的对比实施例。
实施例3
用与实施例1相同的方法获得电容器样品,但是使用Mo的氧化物代替V的氧化物并且烧成后的组成变为表4中所示的混合比。进行相同的评价。结果表示在表4中。
表4
表4
注:在主成分中m=1
样品编号 | 第一副成分 | 烧成温度(℃) | 比介电常数ε | 比电阻ρ(Ωcm) | 容量-温度特性τC(1MHz)(ppm/℃) | ΔτC(=τC100Hz-τC1MHz)(ppm/℃) | 介电损耗tanδ(%)(@100Hz,160℃) | 高温负载寿命(时间) | ||
种类 | 原子% | |||||||||
16 | 对比实施例 | Mo | 0 | 1300 | 38 | 5.1E+15 | -220 | 70 | 1.8 | 3 |
17 | 实施例 | Mo | 0.1 | 1280 | 36 | 3.8E+15 | -230 | 10 | 0.1 | 62 |
18 | 实施例 | Mo | 0.2 | 1280 | 38 | 1.6E+15 | -220 | 20 | 0.1 | 183 |
19 | 实施例 | Mo | 1 | 1280 | 35 | 8E+14 | -210 | 10 | 0.2 | >250 |
20 | 实施例 | Mo | 2 | 1280 | 37 | 1E+14 | -220 | 10 | 0.1 | >250 |
21 | 对比实施例 | Mo | 5 | 1280 | -* | -* | -* | -* | -* | -* |
在主成分中x=0.4且y=0.12
在第二副成分(MnCO3)中折算为金属元素的摩尔数为0.37
第三副成分(SiO2+CaO)的摩尔数为(0.4+0.4)摩尔
测量高温负载寿命的条件:200℃,DC60V/μm
*…变成半导性并且不能用作电容器
从表4所示的结果,对于第一副成分的加入量,可以清楚以下事实。当根本不加Mo时,例如在样品16中,高温负载寿命变得非常短。当Mo的加入量太大时,如在样品21中,其变成半导性的并且不能用作电容器。另一方面,在样品17-20中,其中包含预定量的第一副成分,证实获得了具有足够比介电常数和绝缘电阻、即使在还原气氛中烧成也不还原、不氧化作为内电极材料的镍并具有优异的抗还原性的介电陶瓷组合物。还证实容量-温度特性是优异的,而且可以抑制低频介电色散并且可以改善高温负载寿命。注意,样品17-20是本发明的实施例,样品16和21是本发明的对比实施例。
Claims (9)
1.一种介电陶瓷组合物,其包含:
主成分,其包括由组成分子式{(Ca1-xMex)O}·(Zr1-yTiy)O2表示的介电氧化物,和
第一副成分,其包括选自V、Nb、W、Ta、Mo和Cr的氧化物以及在烧成后变成这些金属氧化物的化合物中的至少一种,
其中,在所述主成分中包含的分子式中的符号Me是Sr、Mg和Ba的至少之一,
符号m、x和y表示在所述主成分中包含的分子式中的组成摩尔比为0.8≤m≤1.3、0≤x≤1.00和0.1≤y≤0.8,并且
所述第一副成分转换成氧化物中的金属元素与100摩尔所述主成分的比例为0.01原子%≤第一副成分<5原子%。
2.权利要求1的介电陶瓷组合物,其还包含第三副成分,所述第三副成分包含Si、M(注意:M是Ba、Ca、Sr和Mg中的至少一种元素)、Li和B的氧化物和在烧成后变成这些元素的氧化物的化合物的至少一种;并且
其中,所述第三副成分折算为氧化物与100摩尔所述主成分的比例为0摩尔<第三副成分<15摩尔。
3.权利要求1的介电陶瓷组合物,其还包含第三副成分,所述第三副成分包括Si和Sr的氧化物和烧成后变成这些氧化物的化合物的至少一种;并且
其中,所述第三副成分折算成氧化物与100摩尔所述主成分的比例为0摩尔<第三副成分<15摩尔。
4.权利要求1的介电陶瓷组合物,其中,在至少25-125℃的温度范围内,静电容量随温度的变化率(ΔC)为-3000-0ppm/℃(注意:静电容量C的参比温度为25℃)。
5.权利要求2的介电陶瓷组合物,其中,在至少25-125℃的温度范围内,静电容量随温度的变化率(ΔC)为-3000-0ppm/℃(注意:静电容量C的参比温度为25℃)。
6.权利要求3的介电陶瓷组合物,其中,在至少25-125℃的温度范围内,静电容量随温度的变化率(ΔC)为-3000-0ppm/℃(注意:静电容量C的参比温度为25℃)。
7.一种电子器件,其包含由介电陶瓷组合物构成的介电层,其中:
所述介电陶瓷组合物包含:
主成分,其包括由组成分子式{(Ca1-xMex)O}·(Zr1-yTiy)O2表示的介电氧化物,和
第一副成分,其包括选自V、Nb、W、Ta、Mo和Cr的氧化物以及在烧成后变成这些金属氧化物的化合物中的至少一种,
其中,在所述主成分中包含的分子式中的符号Me是Sr、Mg和Ba的至少之一,
符号m、x和y表示在所述主成分中包含的分子式中的组成摩尔比,为0.8≤m≤1.3、0≤x≤1.00和0.1≤y≤0.8,并且
所述第一副成分转换成氧化物中的金属元素与100摩尔所述主成分的比例为0.01原子%≤第一副成分<5原子%。
8.权利要求7的电子器件,其包含电容器元件主体,其中,所述介电层和内电极层交替叠层。
9.权利要求8的电子器件,其中,在所述内电极中包含的导电材料是镍或镍合金。
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WO (1) | WO2002000568A1 (zh) |
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2001
- 2001-06-28 TW TW090115719A patent/TW492017B/zh not_active IP Right Cessation
- 2001-06-29 WO PCT/JP2001/005653 patent/WO2002000568A1/ja active IP Right Grant
- 2001-06-29 US US10/311,464 patent/US6962888B2/en not_active Expired - Lifetime
- 2001-06-29 CN CNB018143636A patent/CN100473626C/zh not_active Expired - Lifetime
- 2001-06-29 KR KR10-2002-7017850A patent/KR100497754B1/ko active IP Right Grant
- 2001-06-29 JP JP2002505319A patent/JP4461679B2/ja not_active Expired - Lifetime
- 2001-06-29 EP EP01945721.7A patent/EP1298105B1/en not_active Expired - Lifetime
Cited By (10)
Publication number | Priority date | Publication date | Assignee | Title |
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CN102964122A (zh) * | 2012-11-23 | 2013-03-13 | 潮州三环(集团)股份有限公司 | 介电陶瓷组合物及其电子元器件制作方法 |
CN105669192A (zh) * | 2014-12-08 | 2016-06-15 | 三星电机株式会社 | 陶瓷介电组合物以及包含其的多层陶瓷电容器 |
US9947470B2 (en) | 2014-12-08 | 2018-04-17 | Samsung Electro-Mechanics Co., Ltd. | Ceramic dielectric composition and multilayer ceramic capacitor containing the same |
CN111362694A (zh) * | 2014-12-08 | 2020-07-03 | 三星电机株式会社 | 陶瓷介电组合物以及包含其的多层陶瓷电容器 |
CN109721348A (zh) * | 2017-10-27 | 2019-05-07 | 信昌电子陶瓷股份有限公司 | 低介电常数介电瓷粉组合物制备方法及其制成的电容器 |
CN109721348B (zh) * | 2017-10-27 | 2021-07-02 | 信昌电子陶瓷股份有限公司 | 低介电常数介电瓷粉组合物制备方法及其制成的电容器 |
CN116635348A (zh) * | 2020-09-10 | 2023-08-22 | 基美电子公司 | 介电陶瓷组合物和使用该介电陶瓷组合物的陶瓷电容器 |
CN112759382A (zh) * | 2021-01-17 | 2021-05-07 | 苏州研资工业技术有限公司 | 一种微波介质陶瓷及其制备方法 |
CN113012939A (zh) * | 2021-02-22 | 2021-06-22 | 四川大学 | 高耐电压低损耗硅基薄膜电容器及其制备方法 |
CN113012939B (zh) * | 2021-02-22 | 2022-09-09 | 四川大学 | 高耐电压低损耗硅基薄膜电容器及其制备方法 |
Also Published As
Publication number | Publication date |
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JP4461679B2 (ja) | 2010-05-12 |
TW492017B (en) | 2002-06-21 |
EP1298105A1 (en) | 2003-04-02 |
KR100497754B1 (ko) | 2005-06-23 |
EP1298105A4 (en) | 2005-06-29 |
WO2002000568A1 (fr) | 2002-01-03 |
CN100473626C (zh) | 2009-04-01 |
KR20030026255A (ko) | 2003-03-31 |
EP1298105B1 (en) | 2013-09-25 |
US6962888B2 (en) | 2005-11-08 |
US20030186802A1 (en) | 2003-10-02 |
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