CN114388267A - Dielectric material for multilayer ceramic capacitor and preparation method thereof - Google Patents
Dielectric material for multilayer ceramic capacitor and preparation method thereof Download PDFInfo
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- CN114388267A CN114388267A CN202210032510.1A CN202210032510A CN114388267A CN 114388267 A CN114388267 A CN 114388267A CN 202210032510 A CN202210032510 A CN 202210032510A CN 114388267 A CN114388267 A CN 114388267A
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- 239000003989 dielectric material Substances 0.000 title claims abstract description 62
- 239000003985 ceramic capacitor Substances 0.000 title claims abstract description 32
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 238000005245 sintering Methods 0.000 claims abstract description 39
- 229910002113 barium titanate Inorganic materials 0.000 claims abstract description 34
- 229910002976 CaZrO3 Inorganic materials 0.000 claims abstract description 33
- 239000002994 raw material Substances 0.000 claims abstract description 22
- 238000002156 mixing Methods 0.000 claims description 76
- 239000000919 ceramic Substances 0.000 claims description 35
- 239000000654 additive Substances 0.000 claims description 34
- 230000000996 additive effect Effects 0.000 claims description 34
- 239000000203 mixture Substances 0.000 claims description 30
- 239000001095 magnesium carbonate Substances 0.000 claims description 27
- 229910000021 magnesium carbonate Inorganic materials 0.000 claims description 27
- 239000011656 manganese carbonate Substances 0.000 claims description 27
- 229910000016 manganese(II) carbonate Inorganic materials 0.000 claims description 27
- 238000001035 drying Methods 0.000 claims description 25
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 24
- ZLNQQNXFFQJAID-UHFFFAOYSA-L magnesium carbonate Chemical compound [Mg+2].[O-]C([O-])=O ZLNQQNXFFQJAID-UHFFFAOYSA-L 0.000 claims description 24
- FIXNOXLJNSSSLJ-UHFFFAOYSA-N ytterbium(III) oxide Inorganic materials O=[Yb]O[Yb]=O FIXNOXLJNSSSLJ-UHFFFAOYSA-N 0.000 claims description 23
- 238000001354 calcination Methods 0.000 claims description 15
- 229910000881 Cu alloy Inorganic materials 0.000 claims description 12
- 229910000990 Ni alloy Inorganic materials 0.000 claims description 12
- 239000000853 adhesive Substances 0.000 claims description 12
- 230000001070 adhesive effect Effects 0.000 claims description 12
- 238000000034 method Methods 0.000 claims description 12
- 229910052759 nickel Inorganic materials 0.000 claims description 12
- 230000001681 protective effect Effects 0.000 claims description 12
- 238000007789 sealing Methods 0.000 claims description 12
- 239000002904 solvent Substances 0.000 claims description 12
- VQCBHWLJZDBHOS-UHFFFAOYSA-N erbium(III) oxide Inorganic materials O=[Er]O[Er]=O VQCBHWLJZDBHOS-UHFFFAOYSA-N 0.000 claims description 7
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 6
- JKQOBWVOAYFWKG-UHFFFAOYSA-N molybdenum trioxide Chemical compound O=[Mo](=O)=O JKQOBWVOAYFWKG-UHFFFAOYSA-N 0.000 claims description 6
- 230000008569 process Effects 0.000 claims description 4
- NLQFUUYNQFMIJW-UHFFFAOYSA-N dysprosium(III) oxide Inorganic materials O=[Dy]O[Dy]=O NLQFUUYNQFMIJW-UHFFFAOYSA-N 0.000 claims description 3
- CMIHHWBVHJVIGI-UHFFFAOYSA-N gadolinium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[Gd+3].[Gd+3] CMIHHWBVHJVIGI-UHFFFAOYSA-N 0.000 claims description 3
- JYTUFVYWTIKZGR-UHFFFAOYSA-N holmium oxide Inorganic materials [O][Ho]O[Ho][O] JYTUFVYWTIKZGR-UHFFFAOYSA-N 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims description 2
- 239000007858 starting material Substances 0.000 claims 1
- 230000008859 change Effects 0.000 abstract description 5
- 238000007639 printing Methods 0.000 description 30
- 238000010030 laminating Methods 0.000 description 21
- 239000002002 slurry Substances 0.000 description 20
- 239000010410 layer Substances 0.000 description 16
- 230000000052 comparative effect Effects 0.000 description 14
- 239000003990 capacitor Substances 0.000 description 12
- 239000003054 catalyst Substances 0.000 description 11
- 238000005266 casting Methods 0.000 description 10
- 238000007650 screen-printing Methods 0.000 description 10
- 238000009413 insulation Methods 0.000 description 9
- 238000012360 testing method Methods 0.000 description 7
- 239000013078 crystal Substances 0.000 description 6
- JRPBQTZRNDNNOP-UHFFFAOYSA-N barium titanate Chemical compound [Ba+2].[Ba+2].[O-][Ti]([O-])([O-])[O-] JRPBQTZRNDNNOP-UHFFFAOYSA-N 0.000 description 5
- 230000005684 electric field Effects 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 239000012071 phase Substances 0.000 description 4
- 230000009286 beneficial effect Effects 0.000 description 3
- 230000007547 defect Effects 0.000 description 3
- 230000009467 reduction Effects 0.000 description 3
- 229910010293 ceramic material Inorganic materials 0.000 description 2
- 239000012792 core layer Substances 0.000 description 2
- 239000011258 core-shell material Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000007772 electrode material Substances 0.000 description 2
- 238000010304 firing Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- DJOYTAUERRJRAT-UHFFFAOYSA-N 2-(n-methyl-4-nitroanilino)acetonitrile Chemical compound N#CCN(C)C1=CC=C([N+]([O-])=O)C=C1 DJOYTAUERRJRAT-UHFFFAOYSA-N 0.000 description 1
- 229910052581 Si3N4 Inorganic materials 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- FQNGWRSKYZLJDK-UHFFFAOYSA-N [Ca].[Ba] Chemical compound [Ca].[Ba] FQNGWRSKYZLJDK-UHFFFAOYSA-N 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 229910021523 barium zirconate Inorganic materials 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 238000013016 damping Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 230000030279 gene silencing Effects 0.000 description 1
- 238000003837 high-temperature calcination Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000003607 modifier Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 229910001404 rare earth metal oxide Inorganic materials 0.000 description 1
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 238000010532 solid phase synthesis reaction Methods 0.000 description 1
- 230000001629 suppression Effects 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
Classifications
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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
- H01G4/00—Fixed capacitors; Processes of their manufacture
- H01G4/002—Details
- H01G4/018—Dielectrics
- H01G4/06—Solid dielectrics
- 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
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- C04B35/46—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 titanium oxides or titanates
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- H01G4/00—Fixed capacitors; Processes of their manufacture
- H01G4/002—Details
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- H01G4/1209—Ceramic dielectrics characterised by the ceramic dielectric material
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Abstract
The invention relates to a dielectric material, in particular to a dielectric material for a multilayer ceramic capacitor and a preparation method thereof. The raw material of the dielectric material comprises 100mol of BaTiO3(ii) a The raw material also comprises CaZrO3(ii) a The BaTiO3And said CaZrO3In a molar ratio of 100: (1.0-2.0). The dielectric material provided by the invention has high bias stability, meets the X7R standard, and is an X7R type dielectric material with high bias stability; the multilayer ceramic capacitor prepared by the dielectric material is suitable for sintering in a reducing atmosphere, and the sintering temperature is 1180-1280 ℃ and the multilayer ceramic capacitor has a dielectric constant of 2000 or more, a temperature characteristic of X7R characteristic according to the EIA standard in the united states, and a capacitance change rate of a high voltage load of less than 30%, and shows very excellent dc bias resistance.
Description
Technical Field
The invention relates to a dielectric material, in particular to a dielectric material for a multilayer ceramic capacitor and a preparation method thereof.
Background
MLCCs are widely used in various electronic devices, among them for applications in high voltage environments, relating to switching power supplies and voltage doubling circuits for military, aerospace, aviation, and communication facilities, damping and silencing devices for high frequency power transformers, ac adapters, connectors, high voltage coupling/DC modules, protection modules for power facilities, in particular, various low noise and low leakage current design circuits and surge suppression circuits; in the special fields of satellites, airplanes, missiles and the like, high-voltage ceramic capacitors are required to meet special requirements of miniaturization, high stability, high reliability and the like. The high-voltage ceramic MLC is widely applied to the technical field of electronics, and is required to have high dielectric coefficient and temperature stability (meeting the IEA 'X7R' standard in the aspect of high performance, and the change rate (delta C/C) of capacitance value relative to 25 ℃ in the test temperature range from-55 ℃ to 125 DEG C25℃)≤±15%)。
With the technological progress, MLCCs are gradually developed toward light, thin, short and small ones, and MLCCs are formed by alternately laminating electrode materials and ceramic materials in parallel in multiple layers, firing the laminated electrode materials into a whole at high temperature, and then firing end external electrodes. In order to meet the requirements of miniaturization and large capacity, the dielectric layer needs to be thinner and thinner, and the distance between layers is reduced, which correspondingly brings about relative increase of the bias electric field, and the stability of the MLCC to the dc bias is also examined. If the performance of the capacitor is unstable under high voltage, the capacitance is reduced along with the increase of the electric field strength, and further the electronic component is failed, which may cause a safety problem in severe cases. Therefore, in pursuit of miniaturization and high capacity, attention is paid to a capacitor element having high bias performance stability.
At present, most of MLCC multilayer capacitors are applied to MLCC multilayer capacitors and are achieved by controlling a core-shell microstructure, a shell layer and a core layer can obtain good dielectric temperature characteristic stability after series-parallel connection effect, and the dielectric characteristic is adjusted by accurately controlling the concentration gradient of a doping modifier in a crystal grain, but the process has the defects that: it is difficult to precisely control the ratio of the shell layer to the core layer, the process conditions are quite narrow, the loss of general ferroelectric phase materials under an alternating current electric field is large, and the bias characteristics of the materials cannot meet the requirements of application in a high electric field environment.
In view of this, the invention is particularly proposed.
Disclosure of Invention
The invention aims to provide a dielectric material which has high bias stability and meets the X7R characteristic; the invention also aims to provide a preparation method and application of the dielectric material.
Specifically, the invention provides the following technical scheme:
the invention provides a dielectric material, the raw material of which comprises 100mol of BaTiO3;
The raw material also comprises CaZrO3;
The BaTiO3And said CaZrO3In a molar ratio of 100: (1.0-2.0).
The invention discovers that a dielectric material with high bias voltage stability is hopeful to be obtained by using the paraelectric phase dielectric ceramic material to partially replace the traditional ferroelectric dielectric material;
specifically, barium titanate is used as a main component, calcium zirconate of a paraelectric phase is partially dissolved in the barium titanate to form calcium barium zirconate titanate, a shell layer of a core-shell structure is formed, the shell layer is thickened, the stability of direct-current bias voltage resistance is improved, and the obtained dielectric material has high bias voltage stability.
Preferably, the BaTiO is3Prepared by a hydrothermal method.
In the prior art, the production process of barium titanate comprises a solid phase method, a hydrothermal method, a sol-gel method and the like; the invention also discovers that the barium titanate prepared by the hydrothermal method has the characteristics of complete crystal grain development, light agglomeration and no holes in particles, and the powder does not need high-temperature calcination treatment, so that the problems of crystal grain growth, defect formation and impurity introduction caused in the sintering process are avoided; that is, the barium titanate prepared by the hydrothermal method has no holes and few defects in crystal grains, and can enable the dielectric material to have higher reliability.
In addition, the invention further discovers that the addition of specific additive components into the raw materials of the dielectric material can improve the reduction resistance of the dielectric material and is very beneficial to the temperature stability and the high-temperature characteristic; the additive comprises the following components:
preferably, the raw material also comprises 1.5-6.0mol of BaSiO30.5-2.0mol of MgCO30.1 to 1.0mol of MnCO30.5-6.0mol of additive I, 0.5-5.0mol of additive II and 0.01-0.5mol of additive III;
wherein the additive I is selected from Er2O3、Yb2O3、Gd2O3One or more of the above; the additive II is selected from Y2O3、Ho2O3、Dy2O3One or more of the above; the additive III is selected from WO3、MoO3、V2O5One or more of them.
In the invention, by adopting the additive components, the Curie peak can be straightened and the Curie point can move towards the high-temperature direction, so that the capacity-temperature change rate of the dielectric material can more easily meet the X7R standard, and the introduced rare earth oxide can also improve the reduction resistance of the dielectric material; the obtained dielectric material has better temperature stability and stability.
As a better technical scheme of the invention, the raw materials of the dielectric material comprise the following components in molar ratio:
BaTiO3 100mol,CaZrO3 1.0-3.0mol,BaSiO3 1.5-6.0mol、MgCO3 0.5-2.0mol,MnCO30.1-1.0mol of additive I, 0.5-6.0mol of additive II, 0.5-5.0mol of additive III and 0.01-0.5mol of additive III;
wherein the additive I is selected from Er2O3、Yb2O3、Gd2O3One or more of the above; the additive II is selected from Y2O3、Ho2O3、Dy2O3One or more of the above; the additive III is selected from WO3、MoO3、V2O5One or more of them.
In the present invention, BaTiO is added in an amount of 100mol3,CaZrO3The addition amount of the dielectric material is 1.0-3.0mol, so that the temperature coefficient of the capacitor is flat, a non-ferroelectric phase in the dielectric material is increased, the stability of direct current bias voltage is improved, the stability of direct current bias voltage resistance cannot be realized due to low addition amount, and the dielectric constant is low due to high addition amount; BaSiO3The addition amount of the (1.5-6.0 mol) is a sintering aid, so that the sintering temperature of the material can be reduced and widened, the insulation resistance is deteriorated due to low addition amount, and the dielectric constant is low and the insulation resistance service life is deteriorated due to high addition amount; MgCO3The addition amount of the silicon nitride is 0.5-2.0mol, so that the temperature coefficient of the capacitor is flat and straight, the growth of crystal grains can be inhibited, the sintering characteristic is degraded when the addition amount is too large, and the growth of the crystal grains and the high temperature coefficient of the straight capacitor can not be obviously inhibited when the addition amount is too small; MnCO3The addition amount of (3) is 0.1-1.0mol, the sintering is accelerated, the insulation resistance and the IR durability are improved, the sufficient effect cannot be obtained when the addition amount is too large, and the temperature coefficient of the capacitor is not favorable when the addition amount is too small; the addition of the additive I is 0.5-6.0mol, so that the reduction resistance of the material sintered in a reducing atmosphere is improved, the Curie temperature is improved, the temperature coefficient of the capacitor is straightened, the insulation resistance is improved, and the average service life is prolonged; the addition amount of the additive II is 0.5-5.0mol, which mainly influences the insulation and the insulation life; the addition amount of the additive III is 0.01-0.5mol, the Curie temperature is increased, the temperature coefficient of the capacitor is straightened, the temperature coefficient of the capacitor cannot be straightened sufficiently when the addition amount is too small, and the insulation resistance is reduced when the addition amount is too large; the dielectric material prepared by the raw material formula meets the EIAX7R standard.
The invention also provides a preparation method of the dielectric material, and the raw materials are as above.
Preferably, the preparation method comprises the following steps:
step (1), BaTiO is added3And CaZrO3Mixing to obtain a mixture;
mixing BaSiO3、MgCO3、MnCO3Mixing the additive I, the additive II and the additive III and then calcining to obtain a calcined product;
and (2) mixing the mixture with the calcined product.
The invention also finds that the obtained dielectric material has a more uniform lattice structure by adopting the mode, and is beneficial to improving the reliability of the dielectric material.
Preferably, the calcination is carried out at 500-900 ℃.
Preferably, in step (1), BaTiO is added3And CaZrO3And mixing and drying to obtain the mixture.
Preferably, in the step (2), the mixture and the calcined product are mixed and then dried to obtain the dielectric material.
As a better technical scheme of the invention, the preparation method comprises the following steps:
(1) mixing BaTiO3And CaZrO3Mixing and drying to obtain a mixture;
mixing BaSiO3、MgCO3、MnCO3Mixing the additive I, the additive II and the additive III, and calcining at the temperature of 500-900 ℃ to obtain a calcined product;
(2) and mixing the mixture with the calcined product and then drying to obtain the catalyst.
The invention also provides a multilayer ceramic capacitor which contains the dielectric material.
Preferably, the multilayer ceramic capacitor is manufactured by the following method:
(1) preparing the dielectric material, the adhesive, the solvent and the nickel or nickel alloy electrode into a green body;
(2) sintering the green body in a reducing atmosphere into a ceramic body;
(3) and sealing Cu or Cu alloy electrodes at two ends of the ceramic body, and sintering in a protective atmosphere.
Preferably, in step (2), the sintering is carried out at 1180-1280 ℃;
further, in the step (2), the sintering is performed at 1280 ℃.
Preferably, in the step (3), the sintering is carried out at 900-1000 ℃;
further, in the step (3), the sintering is performed at 1000 ℃.
Based on the scheme, the invention has the following beneficial effects:
the dielectric material provided by the invention has high bias stability, meets the X7R standard, and is an X7R type dielectric material with high bias stability; the multilayer ceramic capacitor prepared by the dielectric material is suitable for sintering in a reducing atmosphere, the sintering temperature is 1180-1280 ℃, the multilayer ceramic capacitor has a dielectric constant of more than 2000, the temperature characteristic meets the X7R characteristic of the American EIA standard, and meanwhile, the capacitance change rate of high-voltage load is less than 30%, so that the multilayer ceramic capacitor has very excellent direct-current bias resistance.
Detailed Description
The following examples are intended to illustrate the invention but are not intended to limit the scope of the invention.
BaTiO referred to in the following examples3Prepared by a hydrothermal method.
The examples do not show the specific techniques or conditions, according to the technical or conditions described in the literature in the field, or according to the product specifications. The reagents or instruments used are conventional products available from regular distributors, not indicated by the manufacturer.
Example 1
The embodiment provides a dielectric material, which comprises the following raw material formula:
BaTiO3 100mol,CaZrO3 2.0mol,BaSiO3 3.0mol、MgCO3 1.5mol,MnCO3 0.5mol,Yb2O3 1.75mol,Y2O3 2mol,V2O5 0.1mol;
the preparation method comprises the following steps:
(1) mixing BaTiO3And CaZrO3Mixing and drying to obtain a mixture;
mixing BaSiO3、MgCO3、MnCO3、Yb2O3、Y2O3、V2O5After mixing, calcining at 650 ℃ to obtain a calcined product;
(2) and mixing the mixture with the calcined product and then drying to obtain the catalyst.
The present embodiment also provides a multilayer ceramic capacitor, which is prepared by the following steps:
(1) mixing the dielectric material with an adhesive and a solvent, dispersing to prepare slurry, preparing the slurry into a dielectric green-blank diaphragm through a casting machine, printing a nickel or nickel alloy electrode on the surface of the diaphragm through a screen printing machine, and then laminating the diaphragm and printing an inner electrode according to the designed layer number; alternately laminating and printing the dielectric films of the inner electrodes to form a green laminated sheet;
(2) sintering the green laminate into a ceramic body in a reducing atmosphere at 1280 ℃;
(3) and sealing Cu or Cu alloy electrodes at two ends of the ceramic body, and sintering at 1000 ℃ in a protective atmosphere to obtain the ceramic.
Example 2
The embodiment provides a dielectric material, which comprises the following raw material formula:
BaTiO3 100mol,CaZrO3 1.5mol,BaSiO3 3.0mol、MgCO3 1.5mol,MnCO3 0.5mol,Yb2O3 1.75mol,Y2O3 2mol,V2O5 0.1mol;
the preparation method comprises the following steps:
(1) mixing BaTiO3And CaZrO3Mixing and drying to obtain a mixture;
mixing BaSiO3、MgCO3、MnCO3、Yb2O3、Y2O3、V2O5After mixing, calcining at 650 ℃ to obtain a calcined product;
(2) and mixing the mixture with the calcined product and then drying to obtain the catalyst.
The present embodiment also provides a multilayer ceramic capacitor, which is prepared by the following steps:
(1) mixing the dielectric material with an adhesive and a solvent, dispersing to prepare slurry, preparing the slurry into a dielectric green-blank diaphragm through a casting machine, printing a nickel or nickel alloy electrode on the surface of the diaphragm through a screen printing machine, and then laminating the diaphragm and printing an inner electrode according to the designed layer number; alternately laminating and printing the dielectric films of the inner electrodes to form a green laminated sheet;
(2) sintering the green laminate into a ceramic body in a reducing atmosphere at 1280 ℃;
(3) and sealing Cu or Cu alloy electrodes at two ends of the ceramic body, and sintering at 1000 ℃ in a protective atmosphere to obtain the ceramic.
Example 3
The embodiment provides a dielectric material, which comprises the following raw material formula:
BaTiO3 100mol,CaZrO3 2.0mol,BaSiO3 3.0mol、MgCO3 1.5mol,MnCO3 0.5mol,Yb2O3 3.0mol,Y2O3 0.75mol,Er2O3 2mol,V2O5 0.1mol;
the preparation method comprises the following steps:
(1) mixing BaTiO3And CaZrO3Mixing and drying to obtain a mixture;
mixing BaSiO3、MgCO3、MnCO3、Yb2O3、Er2O3、V2O5After mixing, calcining at 650 ℃ to obtain a calcined product;
(2) and mixing the mixture with the calcined product and then drying to obtain the catalyst.
The present embodiment also provides a multilayer ceramic capacitor, which is prepared by the following steps:
(1) mixing the dielectric material with an adhesive and a solvent, dispersing to prepare slurry, preparing the slurry into a dielectric green-blank diaphragm through a casting machine, printing a nickel or nickel alloy electrode on the surface of the diaphragm through a screen printing machine, and then laminating the diaphragm and printing an inner electrode according to the designed layer number; alternately laminating and printing the dielectric films of the inner electrodes to form a green laminated sheet;
(2) sintering the green laminate into a ceramic body in a reducing atmosphere at 1280 ℃;
(3) and sealing Cu or Cu alloy electrodes at two ends of the ceramic body, and sintering at 1000 ℃ in a protective atmosphere to obtain the ceramic.
Example 4
The embodiment provides a dielectric material, which comprises the following raw material formula:
BaTiO3 100mol,CaZrO3 2.0mol,BaSiO3 3.0mol、MgCO3 1.5mol,MnCO3 0.5mol,Yb2O3 3.0mol,Y2O3 2.0mol,WO3 0.1mol;
the preparation method comprises the following steps:
(1) mixing BaTiO3And CaZrO3Mixing and drying to obtain a mixture;
mixing BaSiO3、MgCO3、MnCO3、Yb2O3、Y2O3、WO3After mixing, calcining at 650 ℃ to obtain a calcined product;
(2) and mixing the mixture with the calcined product and then drying to obtain the catalyst.
The present embodiment also provides a multilayer ceramic capacitor, which is prepared by the following steps:
(1) mixing the dielectric material with an adhesive and a solvent, dispersing to prepare slurry, preparing the slurry into a dielectric green-blank diaphragm through a casting machine, printing a nickel or nickel alloy electrode on the surface of the diaphragm through a screen printing machine, and then laminating the diaphragm and printing an inner electrode according to the designed layer number; alternately laminating and printing the dielectric films of the inner electrodes to form a green laminated sheet;
(2) sintering the green laminate into a ceramic body in a reducing atmosphere at 1280 ℃;
(3) and sealing Cu or Cu alloy electrodes at two ends of the ceramic body, and sintering at 1000 ℃ in a protective atmosphere to obtain the ceramic.
Example 5
The embodiment provides a dielectric material, which comprises the following raw material formula:
BaTiO3 100mol,CaZrO3 2.0mol,BaSiO3 3.0mol、MgCO3 1.5mol,MnCO3 0.5mol,Yb2O3 3.0mol,Y2O3 0.75mol,Er2O3 2.0mol,WO3 0.1mol;
the preparation method comprises the following steps:
(1) mixing BaTiO3And CaZrO3Mixing and drying to obtain a mixture;
mixing BaSiO3、MgCO3、MnCO3、Yb2O3、Er2O3、WO3After mixing, calcining at 650 ℃ to obtain a calcined product;
(2) and mixing the mixture with the calcined product and then drying to obtain the catalyst.
The present embodiment also provides a multilayer ceramic capacitor, which is prepared by the following steps:
(1) mixing the dielectric material with an adhesive and a solvent, dispersing to prepare slurry, preparing the slurry into a dielectric green-blank diaphragm through a casting machine, printing a nickel or nickel alloy electrode on the surface of the diaphragm through a screen printing machine, and then laminating the diaphragm and printing an inner electrode according to the designed layer number; alternately laminating and printing the dielectric films of the inner electrodes to form a green laminated sheet;
(2) sintering the green laminate into a ceramic body in a reducing atmosphere at 1280 ℃;
(3) and sealing Cu or Cu alloy electrodes at two ends of the ceramic body, and sintering at 1000 ℃ in a protective atmosphere to obtain the ceramic.
Example 6
The embodiment provides a dielectric material, which comprises the following raw material formula:
BaTiO3 100mol,CaZrO3 2.0mol,BaSiO3 3.0mol、MgCO3 1.5mol,MnCO3 0.5mol,Yb2O3 3.0mol,Y2O3 2.0mol,WO3 0.1mol;
the preparation method comprises the following steps:
(1) mixing BaTiO3And CaZrO3Mixing and drying to obtain a mixture;
mixing BaSiO3、MgCO3、MnCO3、Yb2O3、Y2O3、WO3After mixing, calcining at 650 ℃ to obtain a calcined product;
(2) and mixing the mixture with the calcined product and then drying to obtain the catalyst.
The present embodiment also provides a multilayer ceramic capacitor, which is prepared by the following steps:
(1) mixing the dielectric material with an adhesive and a solvent, dispersing to prepare slurry, preparing the slurry into a dielectric green-blank diaphragm through a casting machine, printing a nickel or nickel alloy electrode on the surface of the diaphragm through a screen printing machine, and then laminating the diaphragm and printing an inner electrode according to the designed layer number; alternately laminating and printing the dielectric films of the inner electrodes to form a green laminated sheet;
(2) sintering the green laminate into a ceramic body in a reducing atmosphere at 1280 ℃;
(3) and sealing Cu or Cu alloy electrodes at two ends of the ceramic body, and sintering at 1000 ℃ in a protective atmosphere to obtain the ceramic.
Comparative example 1
The comparative example provides a dielectric material, which comprises the following raw material formula:
BaTiO3 100mol,CaZrO3 3.0mol,BaSiO3 3.0mol、MgCO3 1.5mol,MnCO3 0.5mol,Yb2O3 1.75mol,Y2O3 2.0mol,V2O5 0.1mol;
the preparation method comprises the following steps:
(1) mixing BaTiO3And CaZrO3Mixing and drying to obtain a mixture;
mixing BaSiO3、MgCO3、MnCO3、Yb2O3、Y2O3、V2O5After mixing, calcining at 650 ℃ to obtain a calcined product;
(2) and mixing the mixture with the calcined product and then drying to obtain the catalyst.
The present comparative example also provides a multilayer ceramic capacitor, which is prepared by the following method:
(1) mixing the dielectric material with an adhesive and a solvent, dispersing to prepare slurry, preparing the slurry into a dielectric green-blank diaphragm through a casting machine, printing a nickel or nickel alloy electrode on the surface of the diaphragm through a screen printing machine, and then laminating the diaphragm and printing an inner electrode according to the designed layer number; alternately laminating and printing the dielectric films of the inner electrodes to form a green laminated sheet;
(2) sintering the green laminate into a ceramic body in a reducing atmosphere at 1280 ℃;
(3) and sealing Cu or Cu alloy electrodes at two ends of the ceramic body, and sintering at 1000 ℃ in a protective atmosphere to obtain the ceramic.
Comparative example 2
The comparative example provides a dielectric material, which comprises the following raw material formula:
BaTiO3 100mol,CaZrO3 2.0mol,BaSiO3 5.0mol、MgCO3 1.5mol,MnCO3 0.5mol,Yb2O3 1.75mol,Y2O3 2.0mol,V2O5 0.1mol;
the preparation method comprises the following steps:
(1) mixing BaTiO3And CaZrO3Mixing and drying to obtain a mixture;
mixing BaSiO3、MgCO3、MnCO3、Yb2O3、Y2O3、V2O5After mixing, calcining at 650 ℃ to obtain a calcined product;
(2) and mixing the mixture with the calcined product and then drying to obtain the catalyst.
The present comparative example also provides a multilayer ceramic capacitor, which is prepared by the following method:
(1) mixing the dielectric material with an adhesive and a solvent, dispersing to prepare slurry, preparing the slurry into a dielectric green-blank diaphragm through a casting machine, printing a nickel or nickel alloy electrode on the surface of the diaphragm through a screen printing machine, and then laminating the diaphragm and printing an inner electrode according to the designed layer number; alternately laminating and printing the dielectric films of the inner electrodes to form a green laminated sheet;
(2) sintering the green laminate into a ceramic body in a reducing atmosphere at 1280 ℃;
(3) and sealing Cu or Cu alloy electrodes at two ends of the ceramic body, and sintering at 1000 ℃ in a protective atmosphere to obtain the ceramic.
Comparative example 3
The comparative example provides a dielectric material, which comprises the following raw material formula:
BaTiO3 100mol,CaZrO3 2.0mol,BaSiO3 3.0mol、MgCO3 1.5mol,MnCO3 0.5mol,Yb2O3 7.0mol,Y2O3 2.0mol,V2O5 0.1mol;
the preparation method comprises the following steps:
(1) mixing BaTiO3And CaZrO3Mixing and drying to obtain a mixture;
mixing BaSiO3、MgCO3、MnCO3、Yb2O3、Y2O3、V2O5After mixing, calcining at 650 ℃ to obtain a calcined product;
(2) and mixing the mixture with the calcined product and then drying to obtain the catalyst.
The present comparative example also provides a multilayer ceramic capacitor, which is prepared by the following method:
(1) mixing the dielectric material with an adhesive and a solvent, dispersing to prepare slurry, preparing the slurry into a dielectric green-blank diaphragm through a casting machine, printing a nickel or nickel alloy electrode on the surface of the diaphragm through a screen printing machine, and then laminating the diaphragm and printing an inner electrode according to the designed layer number; alternately laminating and printing the dielectric films of the inner electrodes to form a green laminated sheet;
(2) sintering the green laminate into a ceramic body in a reducing atmosphere at 1280 ℃;
(3) and sealing Cu or Cu alloy electrodes at two ends of the ceramic body, and sintering at 1000 ℃ in a protective atmosphere to obtain the ceramic.
Comparative example 4
The comparative example provides a dielectric material, which comprises the following raw material formula:
BaTiO3 100mol,CaZrO3 2.0mol,BaSiO3 3.0mol、MgCO3 1.5mol,MnCO3 0.5mol,Yb2O3 1.75mol,Y2O3 6.0mol,V2O5 0.1mol;
the preparation method comprises the following steps:
(1) mixing BaTiO3And CaZrO3Mixing and drying to obtain a mixture;
mixing BaSiO3、MgCO3、MnCO3、Yb2O3、Y2O3、V2O5After mixing, calcining at 650 ℃ to obtain a calcined product;
(2) and mixing the mixture with the calcined product and then drying to obtain the catalyst.
The present comparative example also provides a multilayer ceramic capacitor, which is prepared by the following method:
(1) mixing the dielectric material with an adhesive and a solvent, dispersing to prepare slurry, preparing the slurry into a dielectric green-blank diaphragm through a casting machine, printing a nickel or nickel alloy electrode on the surface of the diaphragm through a screen printing machine, and then laminating the diaphragm and printing an inner electrode according to the designed layer number; alternately laminating and printing the dielectric films of the inner electrodes to form a green laminated sheet;
(2) sintering the green laminate into a ceramic body in a reducing atmosphere at 1280 ℃;
(3) and sealing Cu or Cu alloy electrodes at two ends of the ceramic body, and sintering at 1000 ℃ in a protective atmosphere to obtain the ceramic.
Test examples
The dielectric properties of the multilayer ceramic capacitors of examples and comparative examples were measured as follows:
(1) the test method comprises the following steps: under the condition of 25 ℃, adopting an LCR bridge to test the capacity and the loss of each multilayer ceramic capacitor under the conditions of 1.0KHz and 1.0V; testing the insulation resistance of each multilayer ceramic capacitor at 100V for 10 seconds by using an insulation resistance instrument; adopting a high-low temperature box to test the temperature characteristic TCC of each multilayer ceramic capacitor at-55 to +125 ℃, 1.0KHz and 1.0V; the change in capacitance of each multilayer ceramic capacitor was measured at 1V/μm, 2.5V/μm, and 5V/μm, respectively, and the stability of the capacitor against voltage under DC bias was examined as compared with the capacitance at 0V/μm.
(2) The test results are shown in table 1;
TABLE 1 results of dielectric property test of the multilayer ceramic capacitors of examples and comparative examples
Although the invention has been described in detail hereinabove with respect to a general description and specific embodiments thereof, it will be apparent to those skilled in the art that modifications or improvements may be made thereto based on the invention. Accordingly, such modifications and improvements are intended to be within the scope of the invention as claimed.
Claims (10)
1. A dielectric material is characterized in that the raw material comprises 100mol of BaTiO3;
The raw material also comprises CaZrO3;
The BaTiO3And said CaZrO3In a molar ratio of 100: (1.0-2.0).
2. The dielectric material of claim 1, wherein the BaTiO3Prepared by a hydrothermal method.
3. A dielectric material as claimed in claim 1 or 2,the raw material also comprises 1.5-6.0mol of BaSiO30.5-2.0mol of MgCO30.1 to 1.0mol of MnCO30.5-6.0mol of additive I, 0.5-5.0mol of additive II and 0.01-0.5mol of additive III;
wherein the additive I is selected from Er2O3、Yb2O3、Gd2O3One or more of the above; the additive II is selected from Y2O3、Ho2O3、Dy2O3One or more of the above; the additive III is selected from WO3、MoO3、V2O5One or more of them.
4. A process for the preparation of a dielectric material, characterized in that its starting materials are as described in any one of claims 1 to 3.
5. The method of claim 4, comprising:
step (1), BaTiO is added3And CaZrO3Mixing to obtain a mixture;
mixing BaSiO3、MgCO3、MnCO3Mixing the additive I, the additive II and the additive III and then calcining to obtain a calcined product;
and (2) mixing the mixture with the calcined product.
6. The method as claimed in claim 5, wherein the calcination is carried out at 500-900 ℃.
7. The production method according to claim 5 or 6, wherein, in the step (1), BaTiO is added3And CaZrO3Mixing and drying to obtain the mixture;
and/or in the step (2), mixing the mixture with the calcined product and then drying to obtain the dielectric material.
8. A multilayer ceramic capacitor comprising the dielectric material according to any one of claims 1 to 3.
9. The multilayer ceramic capacitor according to claim 8, wherein the multilayer ceramic capacitor is produced by:
(1) preparing the dielectric material, the adhesive, the solvent and the nickel or nickel alloy electrode into a green body;
(2) sintering the green body in a reducing atmosphere into a ceramic body;
(3) and sealing Cu or Cu alloy electrodes at two ends of the ceramic body, and sintering in a protective atmosphere.
10. The multilayer ceramic capacitor as claimed in claim 9, wherein in the step (2), the sintering is carried out at 1180-1280 ℃;
and/or, in the step (3), the sintering is carried out at the temperature of 900-1000 ℃.
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CN107039177A (en) * | 2016-02-04 | 2017-08-11 | 禾伸堂企业股份有限公司 | The dielectric ceramic body of resistance to instant high-voltage |
CN106747419A (en) * | 2016-12-16 | 2017-05-31 | 山东国瓷功能材料股份有限公司 | A kind of dielectric material for mesohigh X7R characteristic multilayer ceramic capacitors |
Cited By (1)
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CN117153564A (en) * | 2023-09-06 | 2023-12-01 | 潮州三环(集团)股份有限公司 | Composite electronic element and preparation method and application thereof |
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