CN114605144A - Medium-high voltage ceramic capacitor dielectric material and application thereof - Google Patents
Medium-high voltage ceramic capacitor dielectric material and application thereof Download PDFInfo
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- 239000003985 ceramic capacitor Substances 0.000 title claims abstract description 66
- 239000003989 dielectric material Substances 0.000 title claims abstract description 57
- 239000000463 material Substances 0.000 claims abstract description 75
- 230000015556 catabolic process Effects 0.000 claims abstract description 21
- 229910002113 barium titanate Inorganic materials 0.000 claims abstract description 16
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 14
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 10
- 229910052681 coesite Inorganic materials 0.000 claims abstract description 10
- 229910052593 corundum Inorganic materials 0.000 claims abstract description 10
- 229910052906 cristobalite Inorganic materials 0.000 claims abstract description 10
- JYTUFVYWTIKZGR-UHFFFAOYSA-N holmium oxide Inorganic materials [O][Ho]O[Ho][O] JYTUFVYWTIKZGR-UHFFFAOYSA-N 0.000 claims abstract description 10
- FKTOIHSPIPYAPE-UHFFFAOYSA-N samarium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[Sm+3].[Sm+3] FKTOIHSPIPYAPE-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 10
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 10
- 229910052682 stishovite Inorganic materials 0.000 claims abstract description 10
- 229910052905 tridymite Inorganic materials 0.000 claims abstract description 10
- 229910001845 yogo sapphire Inorganic materials 0.000 claims abstract description 10
- MCMNRKCIXSYSNV-UHFFFAOYSA-N ZrO2 Inorganic materials O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims abstract description 9
- NLQFUUYNQFMIJW-UHFFFAOYSA-N dysprosium(III) oxide Inorganic materials O=[Dy]O[Dy]=O NLQFUUYNQFMIJW-UHFFFAOYSA-N 0.000 claims abstract description 9
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 7
- 239000000919 ceramic Substances 0.000 claims description 15
- 238000005245 sintering Methods 0.000 claims description 15
- 239000002245 particle Substances 0.000 claims description 11
- 239000002002 slurry Substances 0.000 claims description 8
- 238000002360 preparation method Methods 0.000 claims description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- 239000002904 solvent Substances 0.000 claims description 4
- 238000005266 casting Methods 0.000 claims description 3
- 238000005520 cutting process Methods 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- 238000010030 laminating Methods 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims description 3
- 238000000034 method Methods 0.000 claims description 3
- 239000000654 additive Substances 0.000 claims description 2
- 230000000996 additive effect Effects 0.000 claims description 2
- 238000007731 hot pressing Methods 0.000 claims description 2
- 229920000642 polymer Polymers 0.000 claims description 2
- 238000007650 screen-printing Methods 0.000 claims description 2
- 239000010953 base metal Substances 0.000 abstract description 2
- 230000000052 comparative effect Effects 0.000 description 10
- 239000003990 capacitor Substances 0.000 description 6
- JRPBQTZRNDNNOP-UHFFFAOYSA-N barium titanate Chemical class [Ba+2].[Ba+2].[O-][Ti]([O-])([O-])[O-] JRPBQTZRNDNNOP-UHFFFAOYSA-N 0.000 description 5
- 238000009826 distribution Methods 0.000 description 5
- 239000000203 mixture Substances 0.000 description 5
- 238000011056 performance test Methods 0.000 description 5
- 238000012360 testing method Methods 0.000 description 5
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 4
- 229910052802 copper Inorganic materials 0.000 description 4
- 239000010949 copper Substances 0.000 description 4
- 238000010586 diagram Methods 0.000 description 4
- 238000009472 formulation Methods 0.000 description 4
- 239000000843 powder Substances 0.000 description 4
- 238000000498 ball milling Methods 0.000 description 3
- 238000010405 reoxidation reaction Methods 0.000 description 3
- 239000011230 binding agent Substances 0.000 description 2
- 229910010293 ceramic material Inorganic materials 0.000 description 2
- 238000004891 communication Methods 0.000 description 2
- 238000007598 dipping method Methods 0.000 description 2
- 239000002270 dispersing agent Substances 0.000 description 2
- 238000009713 electroplating Methods 0.000 description 2
- 239000004973 liquid crystal related substance Substances 0.000 description 2
- 239000004014 plasticizer Substances 0.000 description 2
- 229910052573 porcelain Inorganic materials 0.000 description 2
- VEALVRVVWBQVSL-UHFFFAOYSA-N strontium titanate Chemical class [Sr+2].[O-][Ti]([O-])=O VEALVRVVWBQVSL-UHFFFAOYSA-N 0.000 description 2
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 239000011258 core-shell material Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- NKZSPGSOXYXWQA-UHFFFAOYSA-N dioxido(oxo)titanium;lead(2+) Chemical compound [Pb+2].[O-][Ti]([O-])=O NKZSPGSOXYXWQA-UHFFFAOYSA-N 0.000 description 1
- 235000019441 ethanol Nutrition 0.000 description 1
- 238000004880 explosion Methods 0.000 description 1
- 238000009499 grossing Methods 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 229910052451 lead zirconate titanate Inorganic materials 0.000 description 1
- HFGPZNIAWCZYJU-UHFFFAOYSA-N lead zirconate titanate Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Ti+4].[Zr+4].[Pb+2] HFGPZNIAWCZYJU-UHFFFAOYSA-N 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 238000007639 printing Methods 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 229910001404 rare earth metal oxide Inorganic materials 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000012795 verification Methods 0.000 description 1
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Abstract
The invention discloses a medium-high voltage ceramic capacitor dielectric material and application thereof. The dielectric material comprises a main body material, a first doping auxiliary material and a second doping auxiliary material; the main material is BaTiO3The content is 94-99.2 mol%; the first doping auxiliary material is Dy2O3、Y2O3、Ho2O3And Sm2O30.1-2 mol% of any one or more of the above; the second doping auxiliary material is selected from V2O5、CaO、Al2O3、ZrO2And SiO2Any one or more of them, content0.7-4 mol%; the total content of the first doping auxiliary material and the second doping auxiliary material is 0.8-6 mol%. The invention also discloses a multilayer ceramic capacitor prepared by the medium-high voltage ceramic capacitor dielectric material, and the dielectric material of the ceramic capacitor is well matched with nickel electrode nickel and other base metal inner electrodes, has higher breakdown voltage resistance and high temperature stability, and meets the requirement of X7S of EIA.
Description
Technical Field
The invention relates to the technical field of ceramic capacitor elements, in particular to a medium-high voltage ceramic capacitor dielectric material and application thereof.
Background
With the explosion of the consumer electronics industry, there is an increasing demand for passive devices. The MLCC device is widely used in various devices as a capacitor with a large amount, and is mainly used in a communication basic device circuit of communication equipment, automotive electronics, industrial machines, medical machines, and the like. MLCCs are now being developed toward miniaturization, high temperature stability, high capacity, high voltage and high reliability. The middle-high voltage MLCC is used as a power supply bypass capacitor in a liquid crystal module, a liquid crystal driving voltage circuit, LSI of a high voltage power supply, IC and an OP amplifier; DC-DC converters, switching power supplies, and inverters are used as smoothing capacitors. According to EIA standard of American electronic industries Association, capacitor ceramic material type X7S is based on a capacitance value of 25 ℃, and a capacitance change rate (TCC) must be between + 22% and-22% in a temperature range of-55 ℃ to +125 ℃.
At present, three dielectric materials commonly used as medium-high voltage ceramic capacitors are provided, namely barium titanate series, strontium titanate series and antiferroelectric dielectric ceramics, wherein the last two non-ferroelectric phase material systems contain lead, for example, the strontium titanate series are mostly doped with lead titanate to ensure high dielectric constant, and the antiferroelectric ceramic is mainly modified by a lead zirconate titanate system. Generally, maintaining a high dielectric constant requires a material with strong ferroelectric properties (e.g., barium titanate, which is a typical ferroelectric ceramic), while maintaining a high voltage requires a high proportion of non-ferroelectric phase to be present. Generally, the sintering temperature of a barium titanate system is higher than 1300 ℃, the sintering temperature can be reduced by adding a sintering aid, but the introduction of the sintering aid can reduce the dielectric constant of the system.
Although many documents are published on medium-high voltage ceramic dielectric capacitor materials, the ceramic materials have excellent comprehensive properties of being lead-free, high in dielectric constant, X7S temperature characteristic and high in breakdown voltage, and are rarely reported at present.
Disclosure of Invention
In order to solve the technical problems, the invention provides a medium-high voltage ceramic capacitor dielectric material with high temperature stability and a multilayer ceramic capacitor (MLCC) prepared from the medium-high voltage ceramic capacitor dielectric material.
In order to achieve the purpose, the invention adopts the technical scheme that:
the invention provides a medium-high voltage ceramic capacitor dielectric material in a first aspect, which comprises a main material, a first doping auxiliary material and a second doping auxiliary material; the main material is BaTiO3The first doping auxiliary material is selected from Dy2O3、Y2O3、Ho2O3And Sm2O3Any one or more of the second doping auxiliary materials are selected from V2O5、CaO、Al2O3、ZrO2And SiO2Any one or more of them; the content of the main material is 94-99.2 mol% based on the medium-high voltage ceramic capacitor dielectric material; the total content of the first doping auxiliary material and the second doping auxiliary material is 0.8-6 mol% based on the medium-high voltage ceramic capacitor dielectric material, wherein the content of the first doping auxiliary material is 0.1-2 mol% based on the medium-high voltage ceramic capacitor dielectric material; the content of the second doping auxiliary material is 0.7-4 mol% based on the medium-high voltage ceramic capacitor dielectric material.
In certain specific embodiments, based on the medium-high voltage ceramic capacitor dielectric material:
the content of the main body material is 94 mol%, 95 mol%, 96 mol%, 97 mol%, 98 mol%, 99 mol%, 99.1 mol%, 99.2 mol% or any value between the two;
the total content of the first doping auxiliary material and the second doping auxiliary material is 0.8 mol%, 1 mol%, 2 mol%, 3 mol%, 4 mol%, 5 mol%, 6 mol% or any value between the two;
the content of the first doping auxiliary material is 0.1 mol%, 0.2 mol%, 0.5 mol%, 0.7 mol%, 1.0 mol%, 1.2 mol%, 1.5 mol%, 1.7 mol%, 2 mol% or any value between the two;
the content of the second doping auxiliary material is 0.7 mol%, 1 mol%, 1.5 mol%, 2 mol%, 2.5 mol%, 3 mol%, 3.5 mol%, 4 mol% or any value therebetween.
As a preferred embodiment, the content of each component in the first doping auxiliary material based on the medium-high voltage ceramic capacitor dielectric material is as follows:
Dy2O30.1 to 1 mol% of (B) and Y2O3Is 0 to 0.8 mol%, Ho2O30 to 0.5 mol% of Sm2O3The content of (B) is 0 to 0.5 mol%.
In some specific embodiments, the content of each component in the first doping auxiliary material based on the medium-high voltage ceramic capacitor dielectric material is as follows:
Dy2O3the content of (b) is 0.1 mol%, 0.2 mol%, 0.3 mol%, 0.4 mol%, 0.5 mol%, 0.6 mol%, 0.7 mol%, 0.8 mol%, 0.9 mol%, 1 mol% or any value therebetween;
Y2O3the content of (b) is 0 mol%, 0.1 mol%, 0.2 mol%, 0.3 mol%, 0.4 mol%, 0.5 mol%, 0.6 mol%, 0.7 mol%, 0.8 mol% or any value therebetween;
Ho2O3the content of (b) is 0 mol%, 0.1 mol%, 0.2 mol%, 0.3 mol%, 0.4 mol%, 0.5 mol% or any value therebetween;
Sm2O3the content of (b) is 0 mol%, 0.1 mol%, 0.2 mol%, 0.3 mol%, 0.4 mol%, 0.5 mol% or any value therebetween.
In the technical scheme of the invention, Dy2O3、Y2O3、Ho2O3And Sm2O3The content of (b) is not simultaneously maximized.
As a preferred embodiment, the content of each component in the second doping auxiliary material based on the medium-high voltage ceramic capacitor dielectric material is as follows:
V2O50.1 to 0.5 mol% of (A), 0 to 1 mol% of CaO, and Al2O3Is 0.1 to 0.5 mol% of ZrO2Is 0 to 0.1 mol% of SiO2The content of (B) is 0.1 to 2 mol%.
In some specific embodiments, the content of each component in the second doping auxiliary material based on the medium-high voltage ceramic capacitor dielectric material is as follows:
V2O5the content of (b) is 0.1 mol%, 0.2 mol%, 0.3 mol%, 0.4 mol%, 0.5 mol% or any value therebetween;
the content of CaO is 0 mol%, 0.1 mol%, 0.2 mol%, 0.3 mol%, 0.4 mol%, 0.5 mol%, 0.6 mol%, 0.7 mol%, 0.8 mol%, 0.9 mol%, 1 mol%, or any value therebetween;
Al2O3the content of (b) is 0.1 mol%, 0.2 mol%, 0.3 mol%, 0.4 mol%, 0.5 mol% or any value therebetween;
ZrO2the content of (b) is 0 mol%, 0.01 mol%, 0.02 mol%, 0.03 mol%, 0.04 mol%, 0.05 mol%, 0.06 mol%, 0.07 mol%, 0.08 mol%, 0.09 mol%, 0.1 mol% or any value therebetween;
SiO2the content of (b) is 0.1 mol%, 0.4 mol%, 0.6 mol%, 0.8 mol%, 1.0 mol%, 1.2 mol%, 1.4 mol%, 1.6 mol%, 1.8 mol%, 2 mol% or any value therebetween.
In the technical scheme of the invention, V2O5、CaO、Al2O3、ZrO2And SiO2The contents of (c) are not simultaneously at the maximum or minimum.
As a preferred embodiment, the host material BaTiO3The particle size of the (B) is 200 to 350 nm.
In a preferred embodiment, the particle size of the individual components of the first doping auxiliary material and of the second doping auxiliary material does not exceed 100 nm.
The invention also provides application of the medium-high voltage ceramic capacitance dielectric material in preparing electronic components, and particularly relates to multilayer ceramic capacitors.
The third aspect of the present invention provides a method for preparing a multilayer ceramic capacitor (MLCC) from the above medium-high voltage ceramic capacitor dielectric material, comprising the following steps: preparing a main material, a first doping auxiliary material and a second doping auxiliary material into slurry by matching with an ethanol solvent and a polymer additive (a dispersing agent, a binder and a plasticizer); secondly, casting the slurry obtained in the first step into a film, and drying to obtain a ceramic green sheet; screen printing nickel paste as inner electrode; cutting, laminating and hot pressing to obtain a laminated body; fifthly, sintering the laminated body obtained in the step IV in a reducing atmosphere at 1100-1200 ℃; and closing the end to prepare the MLCC device.
The fourth aspect of the present invention provides the multilayer ceramic capacitor obtained by the above production method, wherein the average grain size of the ceramic dielectric of the multilayer ceramic capacitor is 260 to 380 nm.
Furthermore, the multilayer ceramic capacitor has a capacitance change rate of-22% to + 22% within a temperature range of-55 to 125 ℃.
Furthermore, the breakdown field strength of the multilayer ceramic capacitor is 119-148 kV/mm.
The technical scheme has the following advantages or beneficial effects:
the invention uses BaTiO3As a host material, a rare earth oxide Dy2O3、Y2O3、Ho2O3、Sm2O3As a first doping material with V2O5、CaO、Al2O3、ZrO2、SiO2The medium-high voltage ceramic capacitor dielectric material with excellent high temperature stability, high voltage resistance and other performances is obtained by optimizing the dosage ratio of the doping material as a second doping material. The invention is prepared by the medium-high voltage ceramic capacitor dielectric materialA multilayer ceramic capacitor having a breakdown field strength of a ceramic dielectric material of up to 148 kV/mm; the capacitance change rate is between-22% and + 22% within the range of-55 to 125 ℃, and the requirement of EIA standard X7S is met. Wherein, the auxiliary material is Al2O3、SiO2The sintering aid is used for inhibiting the growth of crystal grains and improving the breakdown voltage resistance of the dielectric material so as to meet the medium-high voltage use environment; dy is selected2O3、Ho2O3、Y2O3、Sm2O3Doping rare earth elements to form a core-shell structure, thereby forming a ceramic medium with high temperature stability so as to meet the requirements of EIA standard X7S and manufacturing a corresponding multilayer ceramic capacitor with high temperature stability; in addition, V2O5The anti-reducibility of the dielectric material is improved, and Dy is combined2O3、Y2O3The reliability of the dielectric material is improved, and the CaO can improve the distance from the temperature point and enhance the reliability of the dielectric material. The ceramic capacitor dielectric material is simple in preparation process, can meet the sintering condition of a reducing atmosphere, is well matched with nickel and other base metal inner electrodes, has higher breakdown voltage resistance and high temperature stability, and meets the requirement of X7S of EIA.
Drawings
FIG. 1 is a curve of a TCC of an MLCC device prepared in example 1.
FIG. 2 is a curve of a TCC of an MLCC device prepared in example 2.
FIG. 3 is a curve of a TCC of an MLCC device prepared in example 3.
FIG. 4 is a curve of a TCC of an MLCC device prepared in example 4.
FIG. 5 is a comparative MLCC device TCC curve.
Fig. 6 is a weber distribution of the breakdown field strength of the MLCC device prepared in example 1.
Fig. 7 is a weber distribution of the breakdown field strength of the MLCC device prepared in example 2.
Fig. 8 is a weber distribution of the breakdown field strength of the MLCC device prepared in example 3.
Fig. 9 is a weber distribution of the breakdown field strength of the MLCC device prepared in example 4.
Fig. 10 is a weber distribution of the breakdown field strength of the MLCC device in the comparative example.
Detailed Description
The following examples are only a part of the present invention, and not all of them. Thus, the detailed description of the embodiments of the present invention provided below is not intended to limit the scope of the invention as claimed, but is merely representative of selected embodiments of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments of the invention without making creative efforts, belong to the protection scope of the invention.
The invention aims to relate to a barium titanate-based dielectric material which is suitable for MLCC capacitors with medium-high voltage and X7S requirements, and the barium titanate-based dielectric material comprises the following components: BaTiO 2394-99.2 mol% of Dy2O30.1 to 1 mol% of Y2O30 to 0.8 mol% of Ho2O30 to 0.5 mol% of Sm2O30 to 0.5 mol% of V2O50.1 to 0.5 mol% of CaO, 0 to 1 mol% of Al2O3ZrO in an amount of 0.1 to 0.5 mol% 20 to 0.1 mol% of SiO2The content is 0.1-2 mol%.
In the following examples, MLCC samples were prepared as follows:
(1) according to the proportion, BaTiO3The first doping auxiliary material and the second doping auxiliary material are matched with a dispersant with the mass fraction of 1.5%, a binder with the mass fraction of 2% and a plasticizer with the mass fraction of 3%, absolute ethyl alcohol is used as a solvent, and the materials are as follows: ball milling medium: the mass ratio of the solvent is 2: 1: 1.5, placing the ceramic capacitor dielectric material in a ball mill at the rotating speed of 400r/min, carrying out wet ball milling for 20h, and drying after ball milling is finished to obtain a medium-high voltage ceramic capacitor dielectric material;
(2) preparation of MLCC samples: preparing the medium-high voltage ceramic capacitor dielectric material obtained by the method into slurry, casting the slurry into a 6 mu m thick membrane, and then forming a green body with a certain shape and size by electrode printing, laminating, pressing and cutting; wherein, the nickel slurry is adopted as an inner electrode, and the number of the laminated layers is 150; reducing the green sheetAtmosphere (1% H)2+99％N2) Sintering for 2-4 h at the medium temperature of 1200-1300 ℃, then reducing the temperature to 950-1100 ℃ for reoxidation treatment, and reducing the temperature to 25 ℃ for sintering to form a monolithic ceramic body; and then, dipping copper slurry on two ends of the porcelain body in a copper dipping mode, sintering at 850 ℃ to form a copper electrode firmly combined with the porcelain body, electroplating a nickel layer on the surface of the copper electrode, and electroplating a tin layer for the second time to obtain the MLCC sample.
The MLCC sample was prepared with a medium layer thickness of 5 μm, a medium layer number of 150, and a specification of 0805B 105-50V.
And (3) performance testing: measuring capacitance and loss under 1kHz and 1V conditions by using a precision impedance analyzer (E4980A; Agilent; USA), and converting into dielectric constant according to the capacitance; under the condition of 100V, testing the insulation resistance IR by using a high resistance meter, and taking a stable value after 60S; a broadband dielectric tester (Alpha-A; Novocontrol GmbH; Germany) measures the dielectric temperature spectrum, and the capacitance-temperature change rate TCC (namely delta C/C) is calculated based on the capacitance at 25 DEG C25℃) A curve; and applying a direct current voltage with a boosting rate of 2V/s at two ends of the sample by using a program-controlled voltage-withstanding tester (CS9912 BX; Changsheng; Nanjing, China), and recording the converted breakdown field intensity of the breakdown voltage when the passing current value reaches 2mA, wherein the sample is regarded as being broken down.
The features and properties of the present invention are described in further detail below with reference to examples.
Example 1:
in this example, the host material BaTiO3The particle size of the powder is 200nm, and the particle size of the doping auxiliary material is less than 100 nm. In the preparation of MLCC samples, the green sheets were placed in a reducing atmosphere (1% H)2+99％N2) Sintering at 1200 deg.c for 4 hr, and re-oxidizing at 950 deg.c. In the embodiment, the components of the medium-high voltage ceramic capacitor dielectric material and the performance and other parameters of the MLCC sample prepared from the medium-high voltage ceramic capacitor dielectric material are shown in tables 1 and 2.
Table 1 formulation table of example 1
Table 2 table of performance test results of example 1
FIG. 1 is a TCC curve of the MLCC sample prepared in this example, and it can be seen from the diagram that the MLCC sample provided in this example has a capacitance change rate of-22% to + 22% in the range of-55 to 125 ℃, and meets the EIA standard X7S.
Example 2:
in this example, a host material BaTiO3The particle size of the powder is 250nm, and the particle size of the doping auxiliary material is less than 100 nm. In the preparation of MLCC samples, the green sheets were placed in a reducing atmosphere (1% H)2+99％N2) Sintering at 1250 deg.c for 3 hr, and re-oxidizing at 1000 deg.c. In the embodiment, the components of the medium-high voltage ceramic capacitor dielectric material and the performance and other parameters of the MLCC sample prepared from the medium-high voltage ceramic capacitor dielectric material are shown in tables 3 and 4.
Table 3 formulation table of example 2
Table 4 table of performance test results of example 2
FIG. 2 is a TCC curve of the MLCC sample prepared in this example, and it can be seen from the diagram that the MLCC sample provided in this example has a capacitance change rate of-22% to + 22% in the range of-55 to 125 ℃, and meets the EIA standard X7S.
Example 3:
in this example, the host material BaTiO3The particle size of the powder is 300nm, and the particle size of the doping auxiliary material is less than 100 nm. In the preparation of MLCC samples, the green sheets were placed in a reducing atmosphere (1% H)2+99％N2) Sintering for 2 hours at the temperature of medium 1300 ℃,then the temperature is reduced to 1050 ℃ for reoxidation treatment. In the embodiment, the components of the medium-high voltage ceramic capacitor dielectric material and the performance and other parameters of the MLCC sample prepared from the medium-high voltage ceramic capacitor dielectric material are shown in tables 5 and 6.
Table 5 formulation table of example 3
Table 6 table of results of performance test of example 3
FIG. 3 is a TCC curve of the MLCC sample prepared in this example, and it can be seen from the diagram that the MLCC sample provided in this example has a capacitance change rate of-22% to + 22% in the range of-55 to 125 ℃, and meets the EIA standard X7S.
Example 4:
in this example, the host material BaTiO3The particle size of the powder is 350nm, and the particle size of the doping auxiliary material is less than 100 nm. In the preparation of MLCC samples, the green sheets were placed in a reducing atmosphere (1% H)2+99％N2) Sintering at 1280 deg.C for 3 hr, and then cooling to 1100 deg.C for reoxidation. In the present example, the components of the medium-high voltage ceramic capacitor dielectric material and the performance parameters of the MLCC sample prepared therefrom are shown in tables 7 and 8.
Table 7 formulation table of example 4
Table 8 table of results of performance test of example 4
FIG. 4 is a TCC curve of the MLCC sample prepared in this example, and it can be seen from the diagram that the MLCC sample provided in this example has a capacitance change rate of-22% to + 22% in the range of-55 to 125 ℃, and meets the EIA standard X7S.
Comparative example
The MLCC test specimens in this comparative example were commercially available MLCC devices of the same specification (model: 0805B 105-50V). The base material is BaTiO3The grain size was 300 nm. The comparative examples were tested for performance as shown in Table 9.
TABLE 9 table of performance test results of comparative examples
FIG. 5 is a TCC curve for a MLCC sample in this comparative example.
As shown in tables 2, 4, 6, 8 and 9, the capacitance of 1 + -0.22 μ F is the standard product, the lower the dielectric loss, the better the product stability, and the higher the resistivity, the more stable the product. The medium-high voltage ceramic capacitor dielectric materials prepared in the embodiments 1, 2, 3 and 4 can form a tunable system ceramic dielectric material which has a dielectric constant of 2800-3900 at 25 ℃ and a maximum resistivity of 16.37G omega. m within a temperature range of 1200-1300 ℃ by adjusting the mixture ratio of the main body and the auxiliary material, and is superior to the MLCC device in the comparative example.
Meanwhile, for further verification, through breakdown voltage (BDV) tests (test graphs are shown in figures 6-10), the breakdown field strength of example 1 is 130kV/mm, the breakdown field strength of example 2 is 148kV/mm, the breakdown field strength of example 3 is 128kV/mm, the breakdown field strength of example 4 is 119kV/mm, the breakdown field strength of comparative example is 109kV/mm, and under the condition that the dielectric layer thickness is basically consistent, the breakdown field strength is strong, which represents better reliability, so that the reliable performance of example 1, example 2 and example 3 is better than that of the comparative example.
In conclusion, the ceramic dielectric material prepared by the invention has high dielectric constant and high reliability, and has wide application prospect.
The foregoing is a more detailed description of the invention in connection with specific preferred embodiments and it is not intended that the invention be limited to these specific details. For those skilled in the art to which the invention pertains, several alternatives or obvious modifications can be made without departing from the spirit of the invention, and all of the properties or uses are deemed to fall within the scope of the invention.
Claims (10)
1. The medium-high voltage ceramic capacitor dielectric material is characterized in that: the material comprises a main body material, a first doping auxiliary material and a second doping auxiliary material; the main material is BaTiO3The first doping auxiliary material is Dy2O3、Y2O3、Ho2O3And Sm2O3Any one or more of the second doping auxiliary materials are selected from V2O5、CaO、Al2O3、ZrO2And SiO2Any one or more of them; the content of the main material is 94-99.2 mol% based on the medium-high voltage ceramic capacitor dielectric material; the total content of the first doping auxiliary material and the second doping auxiliary material is 0.8-6 mol% based on the medium-high voltage ceramic capacitor dielectric material, wherein the content of the first doping auxiliary material is 0.1-2 mol% based on the medium-high voltage ceramic capacitor dielectric material; the content of the second doping auxiliary material is 0.7-4 mol% based on the medium-high voltage ceramic capacitor dielectric material.
2. The medium-high voltage ceramic capacitor dielectric material as claimed in claim 1, wherein the content of each component in the first doping auxiliary material based on the medium-high voltage ceramic capacitor dielectric material is as follows:
Dy2O30.1 to 1 mol% of (B) and Y2O3Is 0 to 0.8 mol%, Ho2O30 to 0.5 mol% of Sm2O3The content of (B) is 0 to 0.5 mol%.
3. The medium-high voltage ceramic capacitor dielectric material as claimed in claim 1, wherein the second doping auxiliary material comprises the following components in percentage by weight based on the medium-high voltage ceramic capacitor dielectric material:
V2O50.1 to 0.5 mol% of CaO, 0 to 1 mol% of Al2O3Is 0.1 to 0.5 mol% of ZrO2Is 0 to 0.1 mol% of SiO2The content of (B) is 0.1 to 2 mol%.
4. The medium-high voltage ceramic capacitor dielectric material as claimed in claim 1, wherein the host material is BaTiO3The particle size of the (B) is 200 to 350 nm.
5. The medium-high voltage ceramic capacitor dielectric material as claimed in claim 1, wherein the grain size of each component of the first doping auxiliary material and the second doping auxiliary material is not more than 100 nm.
6. Use of the medium-high voltage ceramic capacitor dielectric material according to any one of claims 1 to 5 in the preparation of electronic components, wherein the electronic components are multilayer ceramic capacitors.
7. The method for preparing the multilayer ceramic capacitor from the medium-high voltage ceramic capacitor dielectric material as claimed in any one of claims 1 to 5, which is characterized by comprising the following steps: preparing a main material, a first doping auxiliary material and a second doping auxiliary material as well as an ethanol solvent and a polymer additive into slurry; secondly, casting the slurry obtained in the first step into a film, and drying to obtain a ceramic green sheet; thirdly, screen printing nickel paste as an inner electrode; cutting, laminating and hot pressing to obtain a laminated body; fifthly, sintering the laminated body obtained in the step IV in a reducing atmosphere at 1200-1300 ℃; and closing the end to prepare the MLCC device.
8. The multilayer ceramic capacitor obtained by the production method according to claim 7, wherein the average grain size of the ceramic dielectric of the multilayer ceramic capacitor is 260 to 380 nm.
9. The multilayer ceramic capacitor as claimed in claim 7, wherein the multilayer ceramic capacitor has a capacitance change rate of-22% to + 22% in a range of-55 to 125 ℃.
10. The multilayer ceramic capacitor according to claim 7, wherein the ceramic dielectric breakdown field strength of the multilayer ceramic capacitor is 119 to 148 kV/mm.
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| US20180033555A1 (en) * | 2016-07-28 | 2018-02-01 | Samsung Electro-Mechanics Co., Ltd. | Dielectric ceramic composition, multilayer ceramic capacitor containing the same, and manufacturing method of multilayer ceramic capacitor |
| CN114014649A (en) * | 2021-12-13 | 2022-02-08 | 深圳先进电子材料国际创新研究院 | Co-doped barium titanate ceramic dielectric material, preparation method and application thereof |
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| CN1330371A (en) * | 2000-06-20 | 2002-01-09 | Tdk株式会社 | Medium ceramics and electronic component |
| JP2002255639A (en) * | 2000-12-25 | 2002-09-11 | Tdk Corp | Dielectric ceramic composition and electronic component |
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| US20180033555A1 (en) * | 2016-07-28 | 2018-02-01 | Samsung Electro-Mechanics Co., Ltd. | Dielectric ceramic composition, multilayer ceramic capacitor containing the same, and manufacturing method of multilayer ceramic capacitor |
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