CN114188156A - Ceramic dielectric material and COG type multilayer ceramic capacitor - Google Patents
Ceramic dielectric material and COG type multilayer ceramic capacitor Download PDFInfo
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- 239000003985 ceramic capacitor Substances 0.000 title claims abstract description 18
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- 238000005516 engineering process Methods 0.000 description 1
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- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 description 1
- 229910052808 lithium carbonate Inorganic materials 0.000 description 1
- 238000009766 low-temperature sintering Methods 0.000 description 1
- 239000001095 magnesium carbonate Substances 0.000 description 1
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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
-
- 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
- H01G4/30—Stacked capacitors
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- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Ceramic Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Inorganic Chemistry (AREA)
- Compositions Of Oxide Ceramics (AREA)
- Inorganic Insulating Materials (AREA)
Abstract
The invention provides a ceramic dielectric material and a COG type multilayer ceramic capacitor, wherein the ceramic dielectric material comprises a main crystal phase component, a modified additive and a sintering aid, and the main crystal phase component is xCaZrO3+ySrZrO3Wherein x/y is more than or equal to 1 and less than or equal to 20; the modifying additive comprises Re2O3And MnCO3、Al2O3、SrCO3、MgTiO3、CaTiO3Re is at least one rare earth element selected from Y, Ho, Yb, Gd, Dy, Sm, Nd and Er. The invention ensures that the material has excellent dielectric property and reliability by selecting the components of the material, can be matched with a nickel electrode, and can be sintered at low temperature in a reducing atmosphere, effectively inhibit the growth of crystal grains, ensure that the crystal grains are fine, uniform and compact, be beneficial to improving the reliability and thinning of products, and finally obtain the ceramic dielectric material for the COG type multilayer ceramic capacitor.
Description
Technical Field
The invention relates to the technical field of multilayer ceramic capacitors, in particular to a ceramic dielectric material and a COG type multilayer ceramic capacitor.
Background
A capacitor is one of electronic components used in a large number of electronic devices, and is used in a wide range and in a large amount, and is irreplaceable. With the rapid development of electronic technology, such as the emergence and development of new electronic products represented by mobile phones, flat panel displays, automotive electronics, etc., good opportunities are brought to the development of capacitors. A Multi-layer Ceramic Capacitor (MLCC) as an important component of a Capacitor has many advantages such as small size, high insulation resistance, and low inductance, and is particularly suitable for increasing the circuit packaging density and reducing the overall size, so that the MLCC becomes an element with the largest usage amount and faster development. With the rapid development of miniaturization and high performance of electric and electronic devices, multilayer ceramic capacitors used in these devices are also subject to small size and high reliability requirements. That is, it is certainly a more challenging task to require the dielectric layer thickness of the multilayer ceramic capacitor to be thinner and thinner without losing other properties.
In order to realize large capacity, the dielectric material is required to have high dielectric constant on one hand, and the fired crystal grains are required to be small on the other hand, so that the thickness of the MLCC dielectric layer is reduced and the number of dielectric layers is increased. CN105174947A discloses a COG dielectric ceramic material for a low-temperature sintering thin-dielectric multilayer ceramic capacitor, which contains main components and additives, wherein the main components are as follows: (Ca)1-xSrx)zZryO3Wherein x is more than or equal to 0.2 and less than or equal to 0.4, y is more than or equal to 0.90 and less than or equal to 1.0, and z is more than or equal to 0.985 and less than or equal to 1.003; the additive comprises the following components: al (Al)2O3、MnCO3、MgO、TiO2、SiO2、BaCO3At least two or more compounds of ZnO; as can be seen from the SEM picture of the surface of the porcelain body, the grains of the porcelain body after being fired are about 700nm on average, and the maximum grains are less than 2 mu m. The fired crystal grains were large, and it was impossible to prepare an MLCC having a grain size of 3 μm or less, and the dielectric layer could not be thinned, and a large capacity could not be realized. CN102964122A discloses a dielectric ceramic composition and a method for manufacturing an electronic component thereof, wherein the dielectric ceramic composition comprises a main crystal phase, a modified additive and a sintering aid, and the structural formula of the main crystal phase is (Mg)γSrαCa(1-α-γ))m(TiβZr1-β)O3Wherein alpha is more than or equal to 0 and less than or equal to 1, gamma is more than or equal to 0 and less than or equal to 1, beta is more than or equal to 0 and less than or equal to 0.1, m is more than or equal to 0.9 and less than or equal to 1.1, and the modified additive is MnCO3，MgCO3，Re2O3Wherein Re is2O3Is a rare earth oxide, and the sintering aid comprises BaCO3，CaCO3，SiO2，Li2CO3，B2O3，Al2O3One or more of them, but the dielectric constant is only 20-30, and is low, so that the large capacity can not be realized.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a ceramic dielectric material and a COG type multilayer ceramic capacitor.
The invention provides a ceramic dielectric material which comprises a main crystal phase component, a modified additive and a sintering aid, wherein the main crystal phase component is xCaZrO3+ySrZrO3Wherein x/y is more than or equal to 1 and less than or equal to 20; the modifying additive comprises Re2O3And MnCO3、Al2O3、SrCO3、MgTiO3、CaTiO3Wherein Re is at least one rare earth element selected from Y, Ho, Yb, Gd, Dy, Sm, Nd and Er.
The ceramic dielectric material of the invention adopts xCaZrO3+ySrZrO3Specific modified additives and sintering aids are added as main crystal phase components, and the dielectric constant of the ceramic dielectric material is ensured to be maintained between 32 and 40 and the dielectric loss is lower than 4 x 10 through the selection of the main crystal phase components and the selection of the additive material composition-4Insulation resistance at 25 DEG C>10*1011Omega, insulation resistance at 125 DEG C>1*1010The temperature characteristic in the temperature range of-55-125 ℃ of omega meets the COG characteristic of EIA standard. The main crystal phase, the modified additive and the sintering aid are mixed and then subjected to wet mixing dispersion and drying, and then a calcining treatment mode is adopted, so that the improvement of the uniform mixing degree of the main crystal phase and the additive is facilitated, the dielectric property and the reliability of the product are facilitated, and the ceramic dielectric material is suitable for the ceramic dielectric material of the COG type multilayer ceramic capacitor.
Furthermore, x/y in the main crystal phase components is more than or equal to 10 and less than or equal to 15.
Further, the modifying additive is formed from MnCO3、Al2O3、SrCO3、MgTiO3、CaTiO3And Re2O3The components have the molar ratio of (1.5-3.5) to (0.3-0.7) to (0.2-1.0) to (0.1-0.3) to (0.5-2.5) to (0.2-0.66).
Further preferably, the Re2O3Is Y2O3。
Further, the sintering aid is SiO2、H3BO3And ZnO. By adding the sintering aid, the ceramic dielectric material can be matched with a nickel electrode, and can be sintered at a low temperature in a reducing atmosphere, so that the growth of crystal grains is effectively inhibited, the crystal grains are fine, uniform and compact, the dielectric strength is high, and the reliability and the thinning of the product are improved.
Further, SiO in the sintering aid2、H3BO3The mol ratio of ZnO is (0.5-3.0): (0.2-0.7): 0.5-3.5).
Furthermore, the molar ratio of the main crystal phase component, the modified additive and the sintering aid is 100 (2.5-6.5) to (1.0-3.5). Namely, calculated according to the amount of substances, the main crystal phase is 100mol, the modified additive is 2.5-6.5mol, and the addition amount of the sintering aid is 1.0-3.5 mol. Within the dosage range, the effective dosage of the main crystal phase can be ensured, and the overall performance of the material is further ensured.
Further, the main crystal phase component is prepared by a solid phase method.
In a preferred embodiment of the present invention, the solid phase method specifically comprises the steps of:
CaCO with purity of more than 99.5 percent is selected3、ZrO2According to CaZrO3The composition ratio is weighed, the calcination temperature is 1000-1080 ℃, and 100-200nmCaZrO is obtained3(ii) a SrCO with the purity of more than 99.5 percent is selected3、ZrO2According to SrZrO3The composition ratio is weighed, the calcination temperature is 1000-1100 ℃, and 100-200nm SrZrO is obtained3(ii) a Then the two main crystal phases are mixed according to xCaZrO3+ySrZrO3Weighing the powder x/y, and adding corresponding additives for subsequent operation.
Further, the average particle diameter of the main crystal phase component is 100-200 nm.
The invention also provides a preparation method of the ceramic dielectric material, which comprises the following steps: and (3) carrying out wet mixing and dispersion on the main crystal phase component, the modified additive and the sintering aid, drying and calcining.
The invention mixes the main crystal phase, the modified additive and the sintering aid, then carries out wet mixing dispersion and drying, and then adopts a calcining treatment mode, thereby being beneficial to improving the uniform mixing degree of the main crystal phase and the additive and improving the dielectric property and reliability of the product, and being suitable for the ceramic dielectric material of the COG type multilayer ceramic capacitor.
Further, the temperature of the calcination is 800-1000 ℃.
The invention also provides a COG type multilayer ceramic capacitor which comprises the ceramic dielectric material. Preferably, the inner electrode of the COG type multilayer ceramic capacitor is a nickel electrode.
The dielectric material of the invention conforms to the COG characteristic of EIA standard, and has uniform material particles, narrow particle size distribution and excellent dielectric property. The dielectric material is applied to manufacturing MLCC, a nickel inner electrode is matched, and the surface grains of the sintered ceramic body are small and the average grains are about 250 nm. The ceramic body has uniform and compact section and is suitable for manufacturing thin-medium, large-capacity and high-reliability MLCC products.
The invention provides a ceramic dielectric material and a COG type multilayer ceramic capacitor, which ensure that the material has excellent dielectric property and the grain diameter of the surface grains of a ceramic body is superior to the prior art level (average grains are 250nm, and the prior grain level is 600-700nm) through the selection of main crystal phase components and the addition of a modified additive and a sintering aid. The material has high reliability through the preparation process and the calcination process of the powder. The material can be matched with a nickel electrode, is sintered in a reducing atmosphere and at low temperature, effectively inhibits the growth of crystal grains, ensures that the crystal grains are fine, uniform and compact, has high dielectric strength, is favorable for improving the reliability and thinning of products, and finally obtains the ceramic dielectric material for the COG type multilayer ceramic capacitor.
Drawings
FIG. 1 is an SEM image of a ceramic dielectric material obtained in example 10 of the present invention;
FIG. 2 is a surface SEM image of a MLCC made of a ceramic dielectric material according to example 10 of the present invention;
FIG. 3 is an SEM cross-section of an MLCC made of a ceramic dielectric material according to example 10 of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention are clearly and completely described below, and it is obvious that the described embodiments are a part of the embodiments of the present invention, but not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The raw materials and auxiliary materials used in the following examples are all commercially available unless otherwise specified.
Examples 1 to 32
This example provides a ceramic dielectric material consisting of a primary crystal phase (xCaZrO)3+ySrZrO3X/y is 10), modifying additive and sintering aid, and the specific formula is shown in table 1.
TABLE 1 composition table of main crystal phase, modification additive and sintering aid formulation
The preparation method of the ceramic dielectric material of each embodiment is as follows:
(1) preparation of main crystal phase components: CaCO with purity of more than 99.5 percent is selected3、SrCO3、ZrO2Starting material according to CaZrO3、SrZrO3The components are respectively weighed and respectively calcined to obtain CaZrO3、SrZrO3Then adding CaZrO3、SrZrO3Weighing according to the molar ratio of x to y for later use.
(2) Preparing a ceramic dielectric material: and (3) carrying out wet mixing dispersion and drying on the main crystal phase, the modified additive and the sintering aid obtained in the previous step, and calcining the dried mixture at 900 ℃ to obtain the ceramic dielectric material.
Example 33
This example provides a ceramic dielectric material with a main crystal phase of xCaZrO3+ySrZrO3X/y is 1, the formula is 100mol of main crystal phase, MnCO3 2mol，Al2O3 0.7mol，SrCO30.8mol，MgTiO3 0.2mol，CaTiO3 2.0mol，Y2O30.66mol, sintering additive ZnO0.8mol and H3BO3 0.6mol、SiO2 1.7mol。
Example 34
This example provides a ceramic dielectric material with a main crystal phase of xCaZrO3+ySrZrO3X/y is 5, the formula is 100mol of main crystal phase, MnCO3 2mol，Al2O3 0.7mol，SrCO30.8mol，MgTiO3 0.2mol，CaTiO3 2mol，Y2O30.66mol, sintering additive ZnO0.8mol and H3BO3 0.6mol、SiO2 1.7mol。。
Example 35
This example provides a ceramic dielectric material with a main crystal phase of xCaZrO3+ySrZrO3X/y 15, in the formula of 100mol of main crystal phase, MnCO3 2mol，Al2O3 0.7mol，SrCO30.8mol，MgTiO3 0.2mol，CaTiO3 2mol，Y2O30.66mol, sintering additive ZnO0.8mol and H3BO3 0.6mol、SiO2 1.7mol。。
Example 36
This example provides a ceramic dielectric material with a main crystal phase of xCaZrO3+ySrZrO3X/y 20, in the formula of 100mol of a main crystal phase, MnCO3 2mol，Al2O3 0.7mol，SrCO30.8mol，MgTiO3 0.2mol，CaTiO3 2mol，Y2O30.66mol, sintering additive ZnO0.8mol and H3BO3 0.6mol、SiO2 1.7mol。
Example 37
This example provides a ceramic dielectric material with a main crystal phase of xCaZrO3+ySrZrO3X/y 10, in the formula of 100mol of a main crystal phase, MnCO3 2mol，Al2O3 0.7mol，SrCO30.8mol，MgTiO3 0.2mol，CaTiO3 2mol，Ho2O30.66mol, sintering additive ZnO0.8mol and H3BO3 0.6mol、SiO2 1.7mol。
Example 38
This example provides a ceramic dielectric material with a main crystal phase of xCaZrO3+ySrZrO3X/y 10, in the formula of 100mol of a main crystal phase, MnCO3 2mol，Al2O3 0.7mol，SrCO30.8mol，MgTiO3 0.2mol，CaTiO3 2mol，Dy2O30.7mol, sintering additive ZnO0.8mol, H3BO3 0.6mol、SiO2 1.7mol。
Example 39
This embodiment provides a ceramic dielectric materialMaterial with main crystal phase of xCaZrO3+ySrZrO3X/y 10, in the formula of 100mol of a main crystal phase, MnCO3 2mol，Al2O3 0.7mol，SrCO30.8mol，MgTiO3 0.2mol，CaTiO3 2mol，Er2O30.7mol, sintering additive ZnO0.8mol, H3BO3 0.6mol、SiO2 1.7mol。
Examples of the experiments
According to the common MLCC preparation process flow: paste preparation → tape casting → silk screen → lamination → cutting → binder removal → sintering → chamfer → end sealing → end burning and the like to carry out MLCC preparation; the specification of the product is 0805C223J500N, the thickness of the dielectric layer is 3 mu m, the nickel inner paste is used for silk-screen printing during silk-screen printing, the product is sintered at 1160 ℃ of reducing atmosphere, copper outer electrodes are sealed at two ends of the product after chamfering, the copper electrodes are subjected to heat treatment at 800 ℃ of nitrogen protective atmosphere, and then the detection of the related electrical properties can be carried out.
Under the conditions of room temperature of 25 ℃ and 45-65% RH, the capacity C and the dielectric loss DF of the MLCC are tested under 1MHz and 1Vrm by using an Agilent 4284A electric bridge, and the dielectric constant is calculated according to the thickness of a dielectric layer, the effective electrode area, the silk screen coefficient, the number of dielectric layers and the capacity; testing the insulation resistance IR of the MLCC by using a TH2683 insulation resistance tester under the conditions of 50VDC and 60S; testing the withstand voltage BDV of the MLCC by using a CJ2671S withstand voltage tester under the conditions that the charging current is less than 20mA and the voltage applying speed is 200V/60S; testing the temperature coefficient TCC of the MLCC at-55-125 ℃ by using a high-low temperature test box; and (3) testing the aging performance HALT of the MLCC under 500H by using an aging test box under the conditions of 125 ℃ and 4 times of working voltage, testing 40 samples in each group, setting the samples with the IR value of below 106 omega as failure, and setting the number of the failure particles of 40 samples in each group as the evaluation result of the aging performance.
Table 2 is a table of MLCC performance parameters from the dielectric materials of examples 1-39, respectively.
FIG. 1 is an SEM image of a ceramic dielectric material of example 10; FIG. 2 is a surface SEM image of an MLCC made using the dielectric material of example 10; FIG. 3 is a SEM cross-section of an MLCC made using the dielectric material of example 10.
TABLE 2 MLCC Performance parameter Table made of dielectric materials
From the above results, it can be seen that a dielectric material excellent in dielectric properties and aging properties can be obtained by controlling the addition amounts of the respective components. The MLCC is manufactured by applying the dielectric material of the invention, matched with a nickel inner electrode, and small, uniform and compact in crystal grain after sintering, thereby being suitable for manufacturing MLCC products with thin dielectric, large capacity and high reliability.
Finally, it should be noted that: the above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.
Claims (10)
1. The ceramic dielectric material is characterized by comprising a main crystal phase component, a modified additive and a sintering aid, wherein the main crystal phase component is xCaZrO3+ySrZrO3Wherein x/y is more than or equal to 1 and less than or equal to 20; the modifying additive comprises Re2O3And MnCO3、Al2O3、SrCO3、MgTiO3、CaTiO3Wherein Re is at least one rare earth element selected from Y, Ho, Yb, Gd, Dy, Sm, Nd and Er.
2. The ceramic dielectric material of claim 1, wherein the modifying additive is formed from MnCO3、Al2O3、SrCO3、MgTiO3、CaTiO3And Re2O3The components have the molar ratio of (1.5-3.5) to (0.3-0.7) to (0.2-1.0) to (0.1-0.3) to (0.5-2.5) to (0.2-0.66).
3. The ceramic dielectric material of claim 2, wherein Re is2O3Is Y2O3。
4. The ceramic dielectric material of any of claims 1-3, wherein the sintering aid is SiO2、H3BO3And ZnO.
5. The ceramic dielectric material of claim 4, wherein SiO is the sintering aid2、H3BO3The mol ratio of ZnO is (0.5-3.0): (0.2-0.7): 0.5-3.5).
6. A ceramic dielectric material as claimed in any one of claims 1 to 5 wherein the molar ratio of the main crystal phase component, modifying additive and sintering aid is 100 (2.5-6.5) to (1.0-3.5).
7. The ceramic dielectric material of claim 6, wherein the main crystalline phase component is prepared by a solid phase method; the average particle size of the main crystal phase component is 100-200 nm.
8. The method of making a ceramic dielectric material of any of claims 1-7, comprising: and (3) carrying out wet mixing and dispersion on the main crystal phase component, the modified additive and the sintering aid, drying and calcining.
9. The method as claimed in claim 8, wherein the temperature of the calcination is 800-1000 ℃.
10. A COG type multilayer ceramic capacitor comprising the ceramic dielectric material according to any one of claims 1 to 7.
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| EP1138652A1 (en) * | 2000-03-30 | 2001-10-04 | TDK Corporation | Method of producing ceramic composition and method of producing electronic device |
| CN1375835A (en) * | 2001-03-19 | 2002-10-23 | 株式会社村田制作所 | Dielectric ceramic and its producing and estimating method, and monolithic ceramic electronic element |
| CN102964122A (en) * | 2012-11-23 | 2013-03-13 | 潮州三环（集团）股份有限公司 | Dielectric ceramic composite and manufacturing method of electronic element thereof |
| CN105174947A (en) * | 2015-09-08 | 2015-12-23 | 山东国瓷功能材料股份有限公司 | COG dielectric ceramic material for low-temperature sintering thin-media multilayer ceramic capacitor |
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| EP1138652A1 (en) * | 2000-03-30 | 2001-10-04 | TDK Corporation | Method of producing ceramic composition and method of producing electronic device |
| CN1375835A (en) * | 2001-03-19 | 2002-10-23 | 株式会社村田制作所 | Dielectric ceramic and its producing and estimating method, and monolithic ceramic electronic element |
| CN102964122A (en) * | 2012-11-23 | 2013-03-13 | 潮州三环（集团）股份有限公司 | Dielectric ceramic composite and manufacturing method of electronic element thereof |
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