CN106747420B - Thin dielectric material for X5R type multilayer ceramic capacitor and preparation method thereof - Google Patents
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Abstract
The invention provides a thin dielectric material for an X5R type multilayer ceramic capacitor, which consists of a main component and an auxiliary additive, wherein the main component is BaTi(1‑x)CrxO3，0.005<x is less than or equal to 0.05, the addition amount of the auxiliary additive is 0.32-5.6 mol based on 100 mol of the main component, and the auxiliary additive is acetate, transition metal oxide and glass powder. The dielectric material provided by the invention has good temperature stability and high reliability. The chromium barium titanate is used as a main component, and the additive is introduced into the formula and mostly adopts water-soluble acetate, so that the additive and the main component can be mixed at an atomic level. The problem of poor product reliability caused by nonuniform mixing of the main component and the oxide serving as the main additive in the conventional dielectric material is solved. The glass powder is added into the formula, so that the sintering temperature of the product can be effectively reduced, and the sintering compactness of the product is improved; the introduced rare earth elements can improve the reduction resistance of the dielectric material.
Description
Technical Field
The invention belongs to the field of energy materials, and particularly relates to a dielectric material of a capacitor and a preparation method thereof.
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) which is an important component of a Capacitor is preferred because it has many advantages such as a small volume, a high insulation resistance, and a low inductance. The method is particularly suitable for improving the circuit assembly density and reducing the volume of the whole machine, so that the MLCC becomes an element with the largest use amount and the 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. In order to realize smaller size and larger capacity, it is required that the dielectric layers of the multilayer ceramic capacitor are thinner and thinner. The trend toward thinner layers requires MLCC dielectric layers to maintain high reliability while meeting existing performance requirements. As a more common dielectric material, the X5R type multilayer ceramic capacitor also has challenges.
Although the MLCC dielectric material related to a plurality of patent documents meets the requirement of X5R characteristic, the MLCC dielectric material has short service life under the load of high temperature and high pressure and cannot meet the specific product performance. In order to improve the high-temperature load life of a thin-layer X5R product, tin oxide is added into a hydrothermal synthesis barium titanate product as a main component, acetate is used as a main additive, and the atomic-level mixing of the additive and the main component can be increased, so that the microstructure of the dielectric porcelain is more uniform, and the reliability of the product is improved. In addition, on the premise of ensuring that the performance of the original product is not damaged, the nano glass is added to effectively reduce the sintering temperature. Finally, the X5R type dielectric material with thin layer and high reliability is obtained, and is suitable for sintering in a reducing atmosphere, wherein the sintering temperature is 1200-1280 ℃. The dielectric constant of the multilayer ceramic capacitor prepared by the dielectric material is more than or equal to 3500, and the temperature characteristic meets the X5R characteristic of the American EIA standard; and the high-temperature load reliability has an average life of 48h or more when a DC voltage of 50V/um is applied at 150 ℃.
Disclosure of Invention
The invention aims to provide a thin dielectric material for a multilayer ceramic capacitor, which uses a nickel electrode and has high reliability according to the X5R characteristic, aiming at the defects of the prior art.
Another object of the invention is to propose a process for the preparation of said medium.
A third object of the invention is to propose a capacitor comprising said dielectric material.
The specific technical scheme for realizing the purpose of the invention is as follows:
the thin dielectric material for X5R type multilayer ceramic capacitor consists of main component BaTi and auxiliary additive(1-x)CrxO3，0.005<x is less than or equal to 0.05, the addition amount of an auxiliary additive is 0.32-5.6 mol based on 100 mol of the main component, and the auxiliary additive is acetate, transition metal oxide and glass powder; the acetate is Mn (Ac)2、Mg(Ac)2Rare earth elementsOne or more of acetate salts of (a).
Wherein the particle size of the main component is 150-300 nm.
Preferably, the acetate salt is 0.01 to 0.6 mole of Mn (Ac)20.1 to 2.0 mol of Mg (Ac)2And 0.1 to 2.0 moles of a compound selected from the group consisting of Y (Ac)3、Ho(Ac)3、Er(Ac)3、Yb(Ac)3、Gd(Ac)3、Dy(Ac)3Acetate salt of one or more of them.
Preferably, the addition amount of the transition metal oxide is 0.01-0.4 mol, and is selected from WO3、V2O5、MoO3One or more of them.
Preferably, the glass powder is CaO and SiO2、ZnO、BaO、B2O3Obtained by mixing, represented by the following formula:
gCaO+hSiO2+iZnO+jBaO+kB2O3，
wherein the molar coefficients g, h, i, j and k satisfy the following relations: in mol percent, g + h + i + j + k is 100, g is more than or equal to 0 and less than or equal to 25, h is more than or equal to 50 and less than or equal to 80, i is more than or equal to 10 and less than or equal to 25, j is more than or equal to 5 and less than or equal to 15, and k is more than or equal to 5 and less than or equal to 20. The glass powder has a particle size of 30-100nm and an addition amount of 0.1-0.6 mol.
The invention also provides a preparation method of the thin dielectric material for the X5R type multilayer ceramic capacitor, which comprises the following steps:
(1) preparing a main component: preparation of BaTiO by hydrothermal method3Mixing BaTiO3Putting the chromium oxide and the chromium oxide into a ball milling tank using zirconium oxide as a grinding medium, and carrying out ball milling, drying, sieving and calcining;
(2) preparing glass powder: CaO, SiO2、ZnO、BaO、B2O3Adding the mixture into a ball milling tank taking zirconium oxide as a grinding medium for ball milling, then drying, sieving, vitrifying and sintering, and performing sand milling and dispersion on the sintered material until the particle size is 30-100 nm;
(3) adding the main component and the auxiliary additive into a ball milling tank using zirconia as a grinding medium for ball milling;
(4) adjusting the pH value of the ball-milled slurry to 6.5-8.5, then carrying out spray drying on the slurry, and calcining the dried powder;
(5) and adding the sieved mixture into a ball milling tank of a zirconia milling medium, and drying and sieving the mixture after ball milling.
Further, in the step (1), control is made to 0.996<Hydrothermal method for preparing BaTiO with Ba/Ti ratio less than or equal to 1.0023(ii) a Adding deionized water into the ball milling tank, and controlling the materials: 1:1.0-1.5 of water; after drying, sieving the mixture by a sieve of 60 meshes to 80 meshes, wherein the calcining temperature is 800-1050 ℃.
In the step (2), deionized water is added into the ball milling tank, and the material control: 1: 1-1.5 of water, ball-milling for 3-5 hours, drying, and sieving with a 60-80 mesh sieve, wherein the vitrification sintering temperature is 1100-1250 ℃, and the heat preservation time is 2 hours.
In the step (3), deionized water is added into the ball milling tank, and the material control: and (3) ball milling for 2-4 hours under the condition that water accounts for 1: 1.3-1.8.
In the step (4), one of ammonia water, sodium bicarbonate and potassium carbonate is used for adjusting the pH value to 6.5-8.5. In the step (4), the calcining temperature is 650-850 ℃, and the calcined product is sieved by a sieve of 60 meshes to 80 meshes;
in the step (5), deionized water is added into the ball milling tank, and the material control: water 1: dispersing 1.3-1.8, ball milling for 2-4 hours, drying, and sieving with a 60-80 mesh sieve.
The capacitor contains the thin dielectric material for the X5R type multilayer ceramic capacitor.
The invention has the beneficial effects that:
the dielectric material provided by the invention has good temperature stability and high reliability. The chromium barium titanate is used as a main component, and water-soluble acetate is mostly adopted as an additive introduced into the formula, so that the additive and the main component are more favorably mixed at an atomic level. Therefore, the problem of poor product reliability caused by nonuniform mixing of the oxide serving as a main additive and the main component in the conventional dielectric material is solved. The glass powder is added into the formula, so that the sintering temperature of the product can be effectively reduced, and the sintering compactness of the product is improved. The various additives cause the media material to satisfy the X5R characteristic; the introduced rare earth elements can improve the reduction resistance of the dielectric material.
By using the formula and the process, the X5R type dielectric material with thin layer and high reliability can be obtained. The multilayer ceramic capacitor prepared by the dielectric material is suitable for sintering in a reducing atmosphere, and the sintering temperature is 1200-1280 ℃. The dielectric constant of the multilayer ceramic capacitor prepared by the dielectric material is more than or equal to 3500, and the temperature characteristic meets the X5R characteristic of the American EIA standard; and the high-temperature load reliability has an average life of 48h or more when a DC voltage of 50V/um is applied at 150 ℃.
Detailed Description
The following examples are intended to illustrate the invention but are not intended to limit the scope of the invention.
A high-reliability dielectric material for X5R type multi-layer ceramic capacitor is prepared through hydrothermal preparing barium titanate, adding chromium oxide as main component, controlling the grain size of additive powder and its diffusion rate in crystal grain during calcining to make additive and main component mix uniformly to obtain uniform lattice structure, and making product MLCC have high reliability and meet X5R standard.
The main component of the dielectric porcelain material is 100 mol of BaTi(1-x)CrxO3(0.005<x is less than or equal to 0.05), and the auxiliary additive mainly adopts acetate: 0.01-0.6 mol Mn (Ac)20.1 to 2.0 mol of Mg (Ac)20.1 to 2.0 mol of a compound selected from the group consisting of Y (Ac)3、Ho(Ac)3、Er(Ac)3、Yb(Ac)3、Gd(Ac)3、Dy(Ac)30.01-0.4 mol of at least one or more compounds selected from WO3、V2O5、MoO3At least one or more compounds of (a). The glass powder has a particle size of about 30-100nm, and the composition comprises CaO and SiO2、ZnO、BaO、B2O3。
The following is a description of specific processes of examples. Unless otherwise specified, the means in the examples are all the means known to those skilled in the art.
Example 1:
the preparation method of the dielectric material comprises the following steps:
(1) preparing main component BaTiO by hydrothermal method3Wherein Ba/Ti is 1. Mixing BaTiO3Adding chromium oxide and the mixture into a ball milling tank using zirconium oxide as a grinding medium according to the x of 0.01, adding deionized water (material: water of 1:1.3) for mixing, carrying out ball milling for 5 hours, drying, sieving (60 meshes or 80 meshes), and calcining (800-.
(2) The preparation method of the glass powder comprises the following steps: weighing CaO and SiO2、ZnO、BaO、B2O3According to molar ratio 5: 65: 10: 10: 10, and mixing. Mixing, adding into a ball milling tank of a zirconia milling medium, adding deionized water (material: water is 1:1.2), mixing, ball milling for 4 hours, drying, sieving with a 80-mesh sieve, vitrifying (sintering temperature is 1200 ℃, and keeping the temperature for 2 hours), and grinding and dispersing the calcined material until the particle size is 30-100 nm.
(3) Mixing BaTi(1-x)CrxO3Auxiliary additive Mn (Ac)2、Mg(Ac)2，Y(Ac)3、Ho(Ac)3、V2O5Glass powder, in a molar ratio of 100: 0.2: 0.2: 1.2: 0.8: 0.1: 0.2 mixing (the material mixing ratio is shown in table 1). The mixture was then added to a zirconia milling jar and mixed with deionized water (charge: water ═ 1: 1.6) and ball milled for 3 hours.
(4) Adjusting the pH value of the ball-milled slurry to 7.5 by using ammonia water, and performing spray drying on the adjusted slurry. The dried powder was calcined (calcination temperature 850 ℃). And sieving the calcined product by a 80-mesh sieve.
(5) And adding the sieved mixture into a ball milling tank of a zirconia milling medium, adding deionized water (material: water is 1: 1.6) for dispersing, drying after ball milling for 3 hours, and sieving by a 80-mesh sieve to obtain the MLCC medium material.
Example 2
The raw materials are in the proportion shown in table 1.
In the step (1), material in a ball milling tank: water 1:1.5, sieving with a 60-mesh sieve, and calcining at 1000 ℃.
In the step (2), material in the ball milling tank: 1:1.4 of water, the sintering temperature is 1200 ℃, and the temperature is kept for 2 h.
In the step (3), material in the ball milling tank: water 1: 1.8, ball milling for 3 hours.
The calcining temperature in the step (4) is 750 ℃. And sieving the calcined product by a 60-mesh sieve.
Step (5), ball milling tank charging: water 1: 1.7, drying and sieving by a 60-mesh sieve after ball milling for 3 hours.
The other operations were the same as in example 1.
Examples 3 to 13
The raw materials are in the proportion shown in table 1. The preparation method is the same as example 1.
TABLE 1 media Material ingredients Table
Test examples
The dielectric materials of examples 1-13 were dispersed to prepare a slurry, the slurry was made into a dielectric green sheet by a casting machine, and a nickel electrode paste was printed on the surface of the sheet by a screen printer. And (3) laminating the membrane sheets and the printed electrodes according to the designed layer number, and alternately printing the dielectric films of the internal electrodes to form a green laminated sheet. Sintering the ceramic body in a reducing atmosphere at 1200-1280 ℃.
And sealing Cu end electrodes at two ends of the sintered ceramic body, and burning the ends in a protective atmosphere to obtain the multilayer ceramic capacitor MLCC. The MLCC sample was prepared with a medium thickness of 1.5 μm, a number of layers of 300, and a specification of 0402.
And (3) testing the dielectric property of the sample: measuring capacitance and loss by using a bridge under the conditions of 1KHz and 1V, and calculating a dielectric constant according to the capacitance and a silk screen coefficient; testing the insulation resistance IR by using an insulation resistance instrument TH2683 under the conditions of 100V and 25 ℃, wherein the testing time is 60 s; measuring the capacitance of each temperature point by using a Temperature Coefficient of Characteristics (TCC) test box in the range of-55 ℃ to +85 ℃, and calculating the change rate of the capacitance at each temperature according to a formula (delta C/C25) by taking the capacitance at 25 ℃ as a reference. The results are shown in Table 2.
TABLE 2 MLCC dielectric Property Table
As can be seen from Table 2, the multilayer ceramic capacitor of the nickel electrode X5R type MLCC dielectric material meets the EIA X5R standard in the temperature characteristic of-55-85 ℃, has the dielectric constant of not less than 3500, has good insulation resistance, and has the average service life of more than 48h when a DC voltage of 50V/um is applied at 150 ℃.
While the present invention has been described in detail with reference to the preferred embodiments, it should be understood that the above description should not be taken as limiting the invention. It will be apparent to those skilled in the art that variations, or modifications, derived or suggested from the disclosure and general knowledge, that achieve the same function and result as described herein, may be substituted for those of ordinary skill in the art, and that all such variations, modifications, and equivalents may be substituted for elements thereof without departing from the scope of the present disclosure.
Claims (8)
1. The thin dielectric material for the X5R type multilayer ceramic capacitor is characterized by comprising a main component and an auxiliary additive, wherein the main component is BaTi(1-x)CrxO3，0.005<x is less than or equal to 0.05, the addition amount of an auxiliary additive is 0.32-5.6 mol based on 100 mol of the main component, and the auxiliary additive is acetate, transition metal oxide and glass powder; the acetate is Mn (Ac)2、Mg(Ac)2One or more of acetate of rare earth elements;
the acetate is 0.01 to 0.6 mol of Mn (Ac)20.1 to 2.0 mol of Mg (Ac)2And 0.1 to 2.0 moles of a compound selected from the group consisting of Y (Ac)3、Ho(Ac)3、Er(Ac)3、Yb(Ac)3、Gd(Ac)3、Dy(Ac)3Acetate of one or more of them;
the addition amount of the transition metal oxide is 0.01-0.4 mol, and is selected from WO3、V2O5、MoO3One or more of the above;
the glass powder is CaO and SiO2、ZnO、BaO、B2O3Obtained by mixing, represented by the following formula:
gCaO+hSiO2+iZnO+jBaO+kB2O3，
wherein the molar coefficients g, h, i, j and k satisfy the following relations: in mol percent, g + h + i + j + k is 100, g is more than or equal to 0 and less than or equal to 25, h is more than or equal to 50 and less than or equal to 80, i is more than or equal to 10 and less than or equal to 25, j is more than or equal to 5 and less than or equal to 15, and k is more than or equal to 5 and less than or equal to 20.
2. The thin dielectric material for multilayer ceramic capacitors of the X5R type according to claim 1,
the particle size of the glass powder is 30-100nm, and the addition amount is 0.1-0.6 mol.
3. A method for producing a thin dielectric material for multilayer ceramic capacitors of the X5R type according to claim 1 or 2, comprising the steps of:
(1) preparing a main component: preparation of BaTiO by hydrothermal method3Mixing BaTiO3Putting the chromium oxide and the chromium oxide into a ball milling tank using zirconium oxide as a grinding medium, and carrying out ball milling, drying, sieving and calcining;
(2) preparing glass powder: CaO, SiO2、ZnO、BaO、B2O3Adding the mixture into a ball milling tank taking zirconium oxide as a grinding medium for ball milling, then drying, sieving, vitrifying and sintering, and performing sand milling and dispersion on the sintered material until the particle size is 30-100 nm;
(3) mixing the main component and the auxiliary additive, and then adding the mixture into a ball milling tank taking zirconia as a grinding medium for ball milling;
(4) adjusting the pH value of the ball-milled slurry to 6.5-8.5, then carrying out spray drying on the slurry, and calcining the dried powder;
(5) and adding the sieved mixture into a ball milling tank of a zirconia milling medium, and drying and sieving the mixture after ball milling.
4. Preparation according to claim 3The method is characterized in that in the step (1), the control is 0.996<Hydrothermal method for preparing BaTiO with Ba/Ti ratio less than or equal to 1.0023(ii) a Adding deionized water into the ball milling tank, and controlling the materials: 1:1.0-1.5 of water; after drying, sieving the mixture by a sieve of 60 meshes to 80 meshes, wherein the calcining temperature is 800-1050 ℃.
5. The preparation method according to claim 3, wherein in the step (2), deionized water is added into the ball milling tank, and the ratio of the materials: 1: 1-1.5 of water, ball-milling for 3-5 hours, drying, and sieving with a 60-80 mesh sieve, wherein the vitrification sintering temperature is 1100-1250 ℃, and the heat preservation time is 2 hours.
6. The preparation method according to claim 3, wherein in the step (3), deionized water is added into the ball milling tank, and the ratio of the materials: and (3) ball milling for 2-4 hours under the condition that water accounts for 1: 1.3-1.8.
7. The preparation method as claimed in claim 3, wherein in the step (4), the calcination temperature is 650-850 ℃, and the calcined product is sieved by a sieve with 60 meshes to 80 meshes;
in the step (5), deionized water is added into the ball milling tank, and the material control: water 1: dispersing 1.3-1.8, ball milling for 2-4 hours, drying, and sieving with a 60-80 mesh sieve.
8. A capacitor comprising the thin dielectric material for the X5R type multilayer ceramic capacitor according to claim 1 or 2.
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| CN108975907A (en) * | 2018-09-05 | 2018-12-11 | 天津大学 | The method for improving barium titanate dielectric material resistance to reduction is adulterated by transition-metal ions |
| CN109305813A (en) * | 2018-09-05 | 2019-02-05 | 天津大学 | A method of improving barium titanate dielectric material resistance to reduction under reducing atmosphere |
| CN113800902B (en) * | 2021-09-18 | 2022-08-09 | 福建火炬电子科技股份有限公司 | BME ceramic dielectric capacitor with high dielectric constant and preparation method thereof |
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| CN1331478A (en) * | 2000-06-30 | 2002-01-16 | 太阳诱电株式会社 | Dielectric ceramic compsn. and ceramic capacitor |
| CN101333105A (en) * | 2008-07-01 | 2008-12-31 | 东营国瓷功能材料有限公司 | X7RMLCC medium porcelain of thin medium |
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Denomination of invention: The invention relates to a thin dielectric material for X5R multilayer ceramic capacitor and a preparation method thereof Effective date of registration: 20211227 Granted publication date: 20200107 Pledgee: SHANGHAI GUOCI NEW MATERIAL TECHNOLOGY Co.,Ltd. Pledgor: SHANDONG SINOCERA FUNCTIONAL MATERIAL Co.,Ltd. Registration number: Y2021980016312 |