CN110511026B - X8R type ceramic capacitor dielectric material and preparation method thereof - Google Patents
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Abstract
The invention discloses an X8R type ceramic capacitor dielectric material and a preparation method thereof. Ball-milling barium carbonate, strontium carbonate, samarium oxide, ferric oxide and niobium pentoxide, refining raw materials, and obtaining BaSr according to a nominal chemical formula3SmFe0.5Nb9.5O30Proportioning according to stoichiometric ratio, pre-sintering, secondary ball milling and other procedures, and finally preparing the X8R type ceramic capacitor dielectric material BaSr by utilizing a solid phase reaction process3SmFe0.5Nb9.5O30. The method can obtain the dielectric ceramic material with excellent temperature stability, and meets the EIA X8R standard; the method is simple, energy-saving and emission-reducing, has moderate cost and is suitable for batch production.
Description
Technical Field
The invention relates to an X8R type ceramic capacitor dielectric material and a preparation method thereof, belonging to the technical field of electronic materials and devices.
Background
With the rapid development of the electronic information industry, the variety and use of electronic products are gradually increasing, and ceramic capacitors are important basic devices in the electronic information industry. Therefore, higher requirements are put on ceramic capacitor materials, such as wider temperature use range, more stable dielectric properties and the like. According to the EIA (electronic Industries Association) standard, the X8R type MLCC means that the change rate of capacitance (delta C/C25) is less than or equal to +/-15% in the temperature range from-55 ℃ to +150 ℃ on the basis of the capacitance value of 25 ℃. In the fields of military industry, aerospace, exploration and the like, electronic components capable of bearing high temperature are greatly required, however, most of the existing ceramic capacitors adopt an X7R ceramic formula, but the capacity-temperature characteristic of the material has certain limitation, the capacitance change rate (delta C/C25) is less than or equal to +/-15% in the range of-55 ℃ to +125 ℃, and the dielectric property of the temperature cannot be provided when the temperature exceeds +125 ℃. Therefore, the X8R type MLCC ceramic dielectric material with high temperature stability is developed and has important practical application value. In addition, most ceramic capacitors are based on perovskite structures, and the tungsten bronze structure is adopted in the invention, which is beneficial to expanding the structural types of ceramic capacitor materials.
Disclosure of Invention
The invention aims to provide an X8R type ceramic capacitor dielectric material and a preparation method thereof.
The nominal chemical formula of the X8R type ceramic capacitor dielectric material is BaSr3SmFe0.5Nb9.5O30。
The method for preparing the X8R type ceramic capacitor dielectric material comprises the following specific steps:
(1) BaCO with purity of more than 99.9 percent3、SrCO3、Sm2O3、Fe2O3And Nb2O5As starting material, according to BaCO3:SrCO3:Sm2O3:Fe2O3:Nb2O5The materials are mixed according to the molar ratio of 1:3:0.5:0.25:4.75, and then are subjected to ball milling for 24 hours by using absolute ethyl alcohol as a ball milling medium, and are dried for 4 hours at 100 ℃ to prepare a dried sample.
(2) And (2) pre-sintering the dried sample prepared in the step (1) at 1000-1150 ℃ for 4 hours to prepare pre-sintered powder.
(3) Grinding the pre-sintered powder prepared in the step (2), then ball-milling for 24 hours by taking absolute ethyl alcohol as a ball-milling medium, uniformly mixing, drying for 4 hours at 100 ℃, then grinding into powder, taking 5-10 wt% of polyvinyl alcohol aqueous solution as a binder for granulation, then sieving with a 60-mesh sieve, pressing and molding, keeping the temperature at 400-600 ℃ for 4-6 hours, discharging colloid, sintering at 1100-1300 ℃ for 4-10 hours in a high-temperature furnace air atmosphere, and then naturally cooling to room temperature along with the furnace to obtain the X8R type ceramic capacitor dielectric material.
The preferred concentration of the aqueous polyvinyl alcohol solution is 8 wt%.
The dielectric material is prepared by adopting a traditional solid phase method, the X8R type ceramic material with excellent performance can be obtained by sintering at a medium temperature, the process is simple, the cost is low, and the environment is not harmful, and the prepared X8R type ceramic capacitor dielectric material has good temperature stability, can meet the requirement that (delta C/C25) is less than or equal to +/-15% within the range of-55-150 ℃, and meets the X8R standard of EIA; the ceramic capacitor dielectric material and the preparation method thereof provided by the invention have good industrialization prospect.
Drawings
FIG. 1 shows BaSr produced by the present invention3SmFe0.5Nb9.5O30X-ray diffraction pattern of the ceramic capacitor dielectric material.
FIG. 2 shows BaSr produced by the present invention3SmFe0.5Nb9.5O30And (3) a surface micro-topography photo of the ceramic capacitor dielectric material.
FIG. 3 shows BaSr produced by the present invention3SmFe0.5Nb9.5O30The dielectric constant of the ceramic capacitor dielectric material is in a regular graph along with the change of temperature.
FIG. 4 shows BaSr produced by the present invention3SmFe0.5Nb9.5O30The change rate of the capacitance of the ceramic capacitor dielectric material is shown by a rule graph along with the change of the temperature, and the change of the dielectric constant is within +/-15% within the temperature range of minus 55-150 ℃.
Detailed Description
Example 1:
BaCO with the purity of 99.99 percent3、SrCO3、Sm2O3、Fe2O3And Nb2O5The raw materials are BaSr according to the stoichiometric ratio3SmFe0.5Nb9.5O30Putting the ingredients into a ball milling tank; selecting a zirconia ball and a nylon tank; mass of added raw materialIs 8 percent of the mass of the grinding ball; the mixing and ball milling time is 24 hours, the rotating speed is 350 r/min, and the ball milling medium is absolute ethyl alcohol; the obtained product is placed in an oven at 100 ℃ to be dried for 4 hours, and is pre-sintered for 4 hours when the temperature is raised to 1000 ℃ at the heating rate of 5 ℃/min; taking out the presintered powder, grinding, ball-milling for 24 hours by taking absolute ethyl alcohol as a ball-milling medium, uniformly mixing, drying for 4 hours at 100 ℃, grinding into powder, granulating by taking a polyvinyl alcohol aqueous solution with the mass percentage concentration of 5% as a binder, sieving by a 60-mesh sieve, pressing into a wafer-shaped green body with the diameter of 10mm and the thickness of 1mm under the pressure of 100MPa, heating to 400 ℃ at the heating rate of 1.5 ℃/min, preserving heat for 4 hours, discharging colloid, heating to 1100 ℃ at the heating rate of 5 ℃/min, preserving heat for 4 hours in the air atmosphere of a high-temperature furnace, sintering, and naturally cooling to room temperature along with the furnace to obtain the BaSr 8R type ceramic capacitor medium material3SmFe0.5Nb9.5O30。
Example 2:
BaCO with the purity of 99.99 percent3、SrCO3、Sm2O3、Fe2O3And Nb2O5The raw materials are BaSr according to the stoichiometric ratio3SmFe0.5Nb9.5O30Putting the ingredients into a ball milling tank; selecting a zirconia ball and a nylon tank; the mass of the added raw materials is 8 percent of that of the grinding ball; the mixing and ball milling time is 24 hours, the rotating speed is 350 r/min, and the ball milling medium is absolute ethyl alcohol; the obtained product is placed in an oven at 100 ℃ to be dried for 4 hours, and is pre-sintered for 4 hours when the temperature is raised to 1100 ℃ at the heating rate of 5 ℃/min; taking out the presintered powder, grinding, ball-milling for 24 hours by taking absolute ethyl alcohol as a ball-milling medium, uniformly mixing, drying for 4 hours at 100 ℃, grinding into powder, granulating by taking a polyvinyl alcohol aqueous solution with the mass percentage concentration of 5% as a binder, sieving by a 60-mesh sieve, pressing into a wafer-shaped green body with the diameter of 10mm and the thickness of 1mm under the pressure of 100MPa, heating to 550 ℃ at the heating rate of 1.5 ℃/min, preserving heat for 5 hours, discharging colloid, heating to 1250 ℃ at the heating rate of 5 ℃/min, preserving heat for 6 hours in a high-temperature furnace air atmosphere, sintering, and naturally cooling to room temperature along with the furnace to obtain the X8R type ceramic capacitor medium material BaSr3SmFe0.5Nb9.5O30。
Example 3:
BaCO with the purity of 99.99 percent3、SrCO3、Sm2O3、Fe2O3And Nb2O5The raw materials are BaSr according to the stoichiometric ratio3SmFe0.5Nb9.5O30Putting the ingredients into a ball milling tank; selecting a zirconia ball and a nylon tank; the mass of the added raw materials is 8 percent of that of the grinding ball; the mixing and ball milling time is 24 hours, the rotating speed is 350 r/min, and the ball milling medium is absolute ethyl alcohol; the obtained product is placed in an oven at 100 ℃ to be dried for 4 hours, and is pre-sintered for 4 hours after being heated to 1150 ℃ at the heating rate of 5 ℃/min; taking out the presintered powder, grinding, ball-milling for 24 hours by taking absolute ethyl alcohol as a ball-milling medium, uniformly mixing, drying for 4 hours at 100 ℃, grinding into powder, granulating by taking a polyvinyl alcohol aqueous solution with the mass percentage concentration of 10% as a binder, sieving by a 60-mesh sieve, pressing into a wafer-shaped green body with the diameter of 10mm and the thickness of 1mm under the pressure of 100MPa, heating to 600 ℃ at the heating rate of 1.5 ℃/min, preserving heat for 6 hours, discharging colloid, heating to 1300 ℃ at the heating rate of 5 ℃/min, preserving heat for 10 hours in the air atmosphere of a high-temperature furnace, sintering, and naturally cooling to room temperature along with the furnace to obtain the X8R type ceramic capacitor medium material BaSr3SmFe0.5Nb9.5O30。
The dielectric material of X8R type ceramic capacitor prepared by the above example is fired with silver electrodes on both sides to form a wafer capacitor, and then the dielectric material is tested and calculated for the change of relative dielectric constant with temperature, as shown in FIG. 3, BaSr3SmFe0.5Nb9.5O30The ceramic material has stable temperature characteristics in a wide temperature range, as shown in figure 4, meets the X8R standard, namely the capacitance change rate is not more than +/-15% within the range of-55-150 ℃, and can be used as an X8R type ceramic capacitor dielectric material.
Claims (2)
1. An X8R type ceramic capacitor dielectric material, characterized in that the nominal chemical formula of the X8R type ceramic capacitor dielectric material is BaSr3SmFe0.5Nb9.5O30;
The preparation steps of the X8R type ceramic capacitor dielectric material are as follows:
(1) BaCO with purity of more than 99.9 percent3、SrCO3、Sm2O3、Fe2O3And Nb2O5As starting material, according to BaCO3:SrCO3:Sm2O3:Fe2O3:Nb2O5Mixing the materials according to a molar ratio of 1:3:0.5:0.25:4.75, then using absolute ethyl alcohol as a ball milling medium, mixing and ball milling the materials for 24 hours, and drying the materials for 4 hours at 100 ℃ to prepare a dried sample;
(2) pre-sintering the dried sample prepared in the step (1) at 1000-1150 ℃ for 4 hours to prepare pre-sintered powder;
(3) grinding the pre-sintered powder prepared in the step (2), then ball-milling for 24 hours by taking absolute ethyl alcohol as a ball-milling medium, uniformly mixing, drying for 4 hours at 100 ℃, then grinding into powder, taking 5-10 wt% of polyvinyl alcohol aqueous solution as a binder for granulation, then sieving with a 60-mesh sieve, pressing and molding, keeping the temperature at 400-600 ℃ for 4-6 hours, discharging colloid, sintering at 1100 ℃ in a high-temperature furnace air atmosphere for 4 hours, and then naturally cooling to room temperature along with the furnace to obtain the X8R type ceramic capacitor dielectric material.
2. The preparation method of the X8R type ceramic capacitor dielectric material as claimed in claim 1, characterized by comprising the following steps:
(1) BaCO with purity of more than 99.9 percent3、SrCO3、Sm2O3、Fe2O3And Nb2O5As starting material, according to BaCO3:SrCO3:Sm2O3:Fe2O3:Nb2O5Mixing the materials according to a molar ratio of 1:3:0.5:0.25:4.75, then using absolute ethyl alcohol as a ball milling medium, mixing and ball milling the materials for 24 hours, and drying the materials for 4 hours at 100 ℃ to prepare a dried sample;
(2) pre-sintering the dried sample prepared in the step (1) at 1000-1150 ℃ for 4 hours to prepare pre-sintered powder;
(3) grinding the pre-sintered powder prepared in the step (2), then ball-milling for 24 hours by taking absolute ethyl alcohol as a ball-milling medium, uniformly mixing, drying for 4 hours at 100 ℃, then grinding into powder, taking 5-10 wt% of polyvinyl alcohol aqueous solution as a binder for granulation, then sieving with a 60-mesh sieve, pressing and molding, keeping the temperature at 400-600 ℃ for 4-6 hours, discharging colloid, sintering at 1100 ℃ in a high-temperature furnace air atmosphere for 4 hours, and then naturally cooling to room temperature along with the furnace to obtain the X8R type ceramic capacitor dielectric material.
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