CN111825446B - Dielectric ceramic material for BT-BRT composite ultra-low loss multilayer ceramic dielectric capacitor and preparation method and application thereof - Google Patents
Dielectric ceramic material for BT-BRT composite ultra-low loss multilayer ceramic dielectric capacitor and preparation method and application thereof Download PDFInfo
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Abstract
The invention belongs to the technical field of electronic ceramic materials, and provides a dielectric ceramic material for a BT-BRT composite ultralow-loss multilayer ceramic dielectric capacitor, and a preparation method and application thereof. The dielectric ceramic material is prepared by mixing a BT-BRT compound and a modified additive. The dielectric constant of the dielectric ceramic material is 40 at 1MHz, and the dielectric loss value tg delta is less than 1.5 multiplied by 10 ‑4 The dielectric loss value is small; in the temperature range of-55 to 125 ℃, the temperature coefficient of the capacity is closer to zero, and the COG characteristic of the American EIA standard is met. The preparation method of the dielectric ceramic material comprises the following steps: (1) ba 2 Ti 9 O 20 The synthesis of (2): (2) ba 6‑ 3x Re 8+2x Ti 18 O 54 Synthesizing; (3) and (3) preparing a dielectric ceramic material. The preparation method can effectively improve the dielectric loss of the dielectric ceramic and improve the reliability of the dielectric ceramic material.
Description
Technical Field
The invention belongs to the technical field of electronic ceramic materials, and particularly relates to a dielectric ceramic material for a BT-BRT composite ultralow-loss multilayer ceramic dielectric capacitor, and a preparation method and application thereof.
Background
The ultralow-loss dielectric ceramic material is a key material for manufacturing a high-frequency chip multilayer ceramic capacitor (MLCC), the MLCC is an important component which plays roles of coupling, tuning, filtering, direct current isolation and the like when being applied to a circuit under the frequency condition of 1MHz, has excellent performances of high reliability, ultralow loss value, low temperature coefficient and the like, and is widely applied to circuits in the fields of military affairs, aviation and aerospace.
According to the American Electrical Association (EIA) standard, MLCCs of different dielectric ceramic materials fall into three categories in terms of temperature stability: dielectric materials of the hyperstable grade (class i) such as COG or NPO; a stabilizing grade (class II) dielectric material such as X7R; a class (iii) dielectric material such as Y5V can be used.
The main difference of the above three dielectric ceramic materials is that the main crystal phase systems are different, different polarization mechanisms exist in the dielectrics, and the difference of the dielectric polarization modes under the same electric field strength is expressed as the difference of the capacitor capacity, which brings different dielectric losses, capacity stability and the like of the capacitor. The dielectric properties of the dielectric ceramic material are decisive for the final properties of the MLCC. Among them, the COG or NPO capacitor is one of the most stable capacitors in capacitance and dielectric loss. The change in capacitance is 0 + -30 ppm/deg.C at a temperature from-55 deg.C to +125 deg.C, and the drift or lag of COG capacitance is less than + -0.05%.
With the recent higher requirement on the performance of the MLCC, on the basis of meeting the requirements of dielectric ceramic materials on the dielectric properties such as the dielectric constant, the temperature coefficient and the like of the MLCC, the higher requirement is put forward on the dielectric loss index for preventing the MLCC product from heating failure and ensuring the high reliability of the MLCC product. Dielectric loss is the energy loss caused by the dielectric material under the action of an electric field due to the hysteresis effect of dielectric conductance and dielectric polarization. Measuring the value of the dielectric loss factor (tg δ) is an important index for judging the internal energy consumption of the medium.
In recent years, the ultra-low loss dielectric ceramic material system having a dielectric constant of 40 and satisfying COG characteristics is used as follows: ba 2 Ti 9 O 3 、CaTiO 3 、Ba 6-3x Ln 8+2x Ti 18 O 54 And the like; however, when the above system is applied alone, tg δ is high, and COG characteristics are difficult to realize, so that the application requirements of the ultra-low loss MLCC product cannot be met.
Disclosure of Invention
Aiming at the defects in the prior art, the first purpose of the invention is to provide a dielectric ceramic material for a BT-BRT composite ultra-low loss multilayer ceramic dielectric container; the dielectric constant of the dielectric ceramic material is 40 at 1MHz, and the dielectric loss value tg delta is less than 1.5 multiplied by 10 -4 The dielectric loss value is small; in the temperature range of-55-125 ℃, the capacity is closer to zero along with the temperature coefficient, and the capacity accords with the C of the American EIA standardAnd OG characteristics.
Aiming at the defects in the prior art, the second purpose of the invention is to provide a preparation method of the dielectric ceramic material for the BT-BRT composite ultra-low loss multilayer ceramic dielectric capacitor; the preparation method is simple to operate, adopts a composite main crystal phase system, is easier to obtain a compact ceramic structure compared with a single main crystal phase system, can effectively improve the dielectric loss of the dielectric ceramic, and improves the reliability of the dielectric ceramic material.
The third purpose of the invention is to provide an application of the dielectric ceramic material on a multilayer ceramic dielectric capacitor.
In order to achieve the above purpose, the solution adopted by the invention is as follows:
a dielectric ceramic material for a BT-BRT composite ultra-low loss multilayer ceramic dielectric capacitor is prepared from BT-BRT composite and a modified additive; the chemical composition formula of the BT-BRT compound is as follows: yBa 2 Ti 9 O 20 - zBa 6-3x Re 8+2x Ti 18 O 54 Wherein, x is not less than 0.4 and not more than 0.6, y is 0.6, z is 0.4(y + z is 1.0), and Re is selected from at least one of Nd, La and Sm.
A preparation method of the dielectric ceramic material for the BT-BRT composite ultra-low loss multilayer ceramic dielectric capacitor comprises the following steps: (1) ba 2 Ti 9 O 20 The synthesis of (2): weighing BaCO according to the molar ratio of 1:4.5 3 And TiO 2 Mixing to obtain a first mixture; then ball-milling the first mixture, drying, sieving and calcining to synthesize the Ba 2 Ti 9 O 20 Sintering the blocks; (2) ba 6-3x Re 8+2x Ti 18 O 54 The synthesis of (2): taking x as 0.4-0.6, and mixing the components in a molar ratio of 6-3 x: 8+2 x: 18 weigh BaCO 3 、Re 2 O 3 And TiO 2 And mixing in a ball mill to obtain a second mixture; calcining the second mixture to synthesize Ba 6-3x Re 8+2x Ti 18 O 54 Sintering the blocks; (3) preparing a dielectric ceramic material: weighing Ba in y 0.6 and z 0.4(y + z 1.0) 2 Ti 9 O 20 And Ba 6-3x Re 8+2x Ti 18 O 54 Grinding and mixing the modified additive to obtain a dielectric ceramic material; (4) mixing a medium ceramic material with paraffin according to the ratio of material powder to paraffin being 100: 7.5, performing wax operation, pressing the ceramic plate under the pressure of 200MPa to form a blank of a phi 14 multiplied by 1.5 wafer, flatly placing the blank on a zirconia plate, placing the blank in a program control furnace, heating the blank to 1260 to 1280 ℃ at the heating rate of 2.1 ℃/min, preserving the heat for 3 hours, cooling the blank along with the furnace, taking out the cooled blank to form a wafer ceramic body, coating silver electrodes on two surfaces of the wafer ceramic body, and testing the electrical property of the wafer ceramic body.
A preparation method of a dielectric ceramic material for a BT-BRT composite ultra-low loss multilayer ceramic dielectric capacitor comprises the following steps: (1) ba 2 Ti 9 O 20 The synthesis of (2): weighing BaCO according to the molar ratio of 1:4.5 3 And TiO 2 2 Mixing to obtain a first mixture; then the first mixture is dried after ball milling, and then calcined after sieving to synthesize Ba 2 Ti 9 O 20 Sintering the blocks; (2) ba 6-3x Re 8+2x Ti 18 O 54 The synthesis of (2): taking x as 0.4-0.6, and mixing the components according to a molar ratio of 6-3 x: 8+2 x: 18 weigh BaCO 3 、Re 2 O 3 And TiO 2 Mixing to obtain a second mixture; calcining the second mixture to synthesize Ba 6-3x Re 8+2x Ti 18 O 54 Sintering the blocks; (3) preparing a dielectric ceramic material: weighing Ba in y 0.6 and z 0.4(y + z 1.0) 2 Ti 9 O 20 、Ba 6-3x Re 8+2x Ti 18 O 54 Grinding and mixing the modified additive to obtain a dielectric ceramic material; (4) mixing a medium ceramic material with paraffin according to the ratio of material powder to paraffin being 100: 7.5, performing wax operation, pressing the ceramic plate under the pressure of 200MPa to form a blank of a phi 14 multiplied by 1.5 wafer, flatly placing the blank on a zirconia plate, placing the blank in a program control furnace, heating the blank to 1260 to 1280 ℃ at the heating rate of 2.1 ℃/min, preserving the heat for 3 hours, cooling the blank along with the furnace, taking out the cooled blank to form a wafer ceramic body, coating silver electrodes on two surfaces of the wafer ceramic body, and testing the electrical property of the wafer ceramic body.
An application of the dielectric ceramic material on a multilayer ceramic dielectric capacitor.
The dielectric ceramic material for the BT-BRT composite ultra-low loss multilayer ceramic dielectric capacitor, the preparation method and the application thereof have the beneficial effects that:
(1) the BT-BRT composite ultralow-loss multilayer ceramic dielectric ceramic material for the dielectric container provided by the invention; the dielectric loss can be greatly reduced by adopting a composite main crystal phase system; at 1MHz, the dielectric constant is 40, and the dielectric loss value tg delta is less than 1.5 multiplied by 10 -4 (ii) a And the capacity is within +/-30 ppm/DEG C along with the temperature coefficient within the temperature range of-55-125 ℃, thereby meeting the COG characteristic of the American EIA standard; and the material does not contain harmful substances such as lead and the like, and accords with the ROHS instruction.
(2) The invention provides a preparation method of a dielectric ceramic material for a BT-BRT composite ultra-low loss multilayer ceramic dielectric capacitor, which synthesizes two single main crystal phases Ba twice at high temperature 2 Ti 9 O 20 And Ba 6-3x Re 8+2x Ti 18 O 54 Then, two main crystal phase systems are simultaneously used in the preparation of the dielectric ceramic material; in the process of sintering the dielectric ceramic material, the two main crystal phases are mutually bonded through solid particles, ion diffusion and crystal boundary migration to form a composite main crystal phase, thereby fundamentally changing the microstructure of the system and effectively reducing the dielectric loss value tg delta under 1 MHz.
Drawings
FIG. 1 is an SEM surface topography of a dielectric ceramic material provided in Experimental example 5 of the present invention;
FIG. 2 is a phase structure diagram of XRD of the dielectric ceramic material provided in Experimental example 5 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 will be clearly and completely described below. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
The dielectric ceramic material for the BT-BRT composite ultra-low loss multilayer ceramic dielectric capacitor, and the preparation method and the application thereof provided by the embodiment of the invention are specifically explained below.
The inventionThe embodiment provides a dielectric ceramic material for a BT-BRT composite ultra-low loss multilayer ceramic dielectric container, wherein the main crystal phase of the dielectric ceramic material is a BT-BRT composite; the chemical composition formula of the BT-BRT compound is as follows: yBa 2 Ti 9 O 20 -zBa 6-3x Re 8+ 2x Ti 18 O 54 Wherein x is not less than 0.4 and not more than 0.6, y is 0.6, z is 0.4(y + z is 1.0), Re is at least one selected from Nd, La and Sm, and the doping modifier is added into the BT-BRT compound, and then the mixture is ground and uniformly mixed to prepare the dielectric ceramic material.
In this example, a metal oxide was used as the modifying additive. Further, the mass percentage of the metal oxide to the mass of the BT-BRT composite is less than or equal to 18%. So that the modifying additive can modify the BT-BRT compound in an optimal range.
Specifically, in the present embodiment, the metal oxide includes: al (Al) 2 O 3 、ZnO、SiO 2 、Nb 2 O 5 、 MnO 2 And MgO. The additives can complement each other and cooperate with each other to realize synergism.
In this example, Al 2 O 3 The mass percentage of the BT-BRT compound is less than or equal to 3 percent; the percentage of ZnO in the BT-BRT compound is less than or equal to 3 percent; SiO 2 2 The mass percentage of the BT-BRT compound is less than or equal to 3 percent; nb 2 O 5 The mass percentage of the BT-BRT compound is less than or equal to 3 percent; MnO 2 The mass percentage of the BT-BRT compound is less than or equal to 3 percent; the weight percentage of MgO in the BT-BRT compound is less than or equal to 3 percent.
yBa 2 Ti 9 O 20 -zBa 6-3x Re 8+2x Ti 18 O 54 The composite compound is used as a main crystal phase to carry out trace modifier doping, so that the tg delta value of the dielectric ceramic material can be further reduced, and the reliability of the dielectric ceramic material is improved.
In this embodiment, a plurality of metal oxides are doped simultaneously, and the amount of doping is controlled to further improve the comprehensive dielectric properties of the dielectric ceramic material and further reduce the dielectric loss.
The preparation method of the dielectric ceramic material comprises the following steps: (1) ba 2 Ti 9 O 20 The synthesis of (2): weighing BaCO according to the molar ratio of 1:4.5 3 And TiO 2 Mixing to obtain a first mixture; and then mixing the first mixture, deionized water and a ball milling medium according to a mass ratio of 1: 1.5: 5 mixing in a ball mill and drying; adding water, sieving, calcining in a heating furnace to synthesize Ba 2 Ti 9 O 20 Sintering the blocks; in this step, BaCO 3 And TiO 2 The powder is adopted, so that the contact area of the powder and the powder is larger, and the contact is more sufficient.
(2)Ba 6-3x Re 8+2x Ti 18 O 54 The synthesis of (2): taking x as 0.4-0.6, and mixing the components in a molar ratio of 6-3 x: 8+2 x: 18 weigh BaCO 3 、Re 2 O 3 And TiO 2 And mixing in a ball mill to obtain a second mixture; the second mixture is sent into a heating furnace for calcination to synthesize Ba 6-3x Re 8+2x Ti 18 O 54 Sintering the blocks; in this step, BaCO 3 、 Re 2 O 3 And TiO 2 The powder is adopted, so that the contact area of the powder and the powder is larger, and the contact is more sufficient.
(3) Preparing a dielectric ceramic material: weighing Ba (0.6 and 0.4) in terms of y and z 2 Ti 9 O 20 、Ba 6-3x Re 8+2x Ti 18 O 54 Mixing with a modifying additive to obtain a third mixture; and then mixing the third mixture, deionized water and a ball milling medium according to a mass ratio of 1: 1.4: 5, performing vibration grinding in a vertical vibration mill for 20-28 h; then, sieving the mixture by a 320-mesh sieve to obtain ceramic slurry; and drying the ceramic slurry at the temperature of 100-140 ℃, and then sieving the dried ceramic slurry with a 100-mesh sieve to obtain the dielectric ceramic material.
(4) Mixing a medium ceramic material with paraffin according to the ratio of material powder to paraffin being 100: 7.5, performing wax operation, pressing the ceramic plate under the pressure of 200MPa to form a blank of a phi 14 multiplied by 1.5 wafer, flatly placing the blank on a zirconia plate, placing the blank in a program control furnace, heating the blank to 1260 to 1280 ℃ at the heating rate of 2.1 ℃/min, preserving the heat for 3 hours, cooling the blank along with the furnace, taking out the cooled blank to form a wafer ceramic body, coating silver electrodes on two surfaces of the wafer ceramic body, and testing the electrical property of the wafer ceramic body.
The features and properties of the present invention are described in further detail below with reference to examples.
Example 1
The embodiment provides a preparation method of a dielectric ceramic material for a BT-BRT composite ultra-low loss multilayer ceramic dielectric capacitor, which comprises the following steps: (1) ba 2 Ti 9 O 20 The synthesis of (2): weighing BaCO according to the molar ratio of 1:4.5 3 Powder and TiO 2 Mixing the powder to obtain a first mixture; and then mixing the first mixture, deionized water and a ball milling medium according to a mass ratio of 1: 1.5: 5 mixing in a ball mill and drying; adding deionized water, sieving, calcining in a heating furnace to synthesize Ba 2 Ti 9 O 20 Sintering the blocks; (2) ba 6-3x Re 8+2x Ti 18 O 54 The synthesis of (2): taking x as 0.4-0.6, and mixing the components in a molar ratio of 6-3 x: 8+2 x: 18 weigh BaCO 3 Powder, Re 2 O 3 Powder and TiO 2 Mixing the powder in a ball mill to obtain a second mixture; the second mixture is sent into a heating furnace for calcination to synthesize Ba 6-3x Re 8+2x Ti 18 O 54 Sintering the blocks; (3) preparing a dielectric ceramic material: weighing Ba in y 0.6 and z 0.4(y + z 1.0) 2 Ti 9 O 20 And Ba 6-3x Re 8+2x Ti 18 O 54 (ii) a Weighing Ba 2 Ti 9 O 20 And Ba 6-3x Re 8+2x Ti 18 O 54 1 percent of Al in percentage by mass 2 O 3 Powder, 3% ZnO powder, 2.3% SiO 2 Powder, 2.4% Nb 2 O 5 Powder and 0.04% MnO 2 Mixing the powder to obtain a third mixture; and then mixing the third mixture, deionized water and a ball milling medium according to a mass ratio of 1: 1.4: 5, performing vibration grinding in a vertical vibration mill for 20-28 h; then, sieving the mixture by a 320-mesh sieve to obtain ceramic slurry; and drying the ceramic slurry at the temperature of 100-140 ℃, and then sieving the dried ceramic slurry with a 100-mesh sieve to obtain the dielectric ceramic material.
Example 2
The embodiment provides a preparation method of a dielectric ceramic material for a BT-BRT composite ultra-low loss multilayer ceramic dielectric capacitor, which comprises the following steps: (1) ba 2 Ti 9 O 20 The synthesis of (2): weighing BaCO according to the molar ratio of 1:4.5 3 Powder and TiO 2 Mixing the powder to obtain a first mixture; and then mixing the first mixture, deionized water and a ball milling medium according to a mass ratio of 1: 1.5: 5 mixing in a ball mill and drying; adding deionized water, sieving, calcining in a heating furnace to synthesize Ba 2 Ti 9 O 20 Sintering the blocks; (2) ba 6-3x Re 8+2x Ti 18 O 54 The synthesis of (2): taking x as 0.4-0.6, and mixing the components in a molar ratio of 6-3 x: 8+2 x: 18 weigh BaCO 3 Powder, Re 2 O 3 Powder and TiO 2 Mixing the powder in a ball mill to obtain a second mixture; the second mixture is sent into a heating furnace for calcination to synthesize Ba 6-3x Re 8+2x Ti 18 O 54 Sintering the blocks; (3) preparing a dielectric ceramic material: y 0.6, z 0.4(y + z 1.0), weighing Ba 2 Ti 9 O 20 And Ba 6-3x Re 8+2x Ti 18 O 54 (ii) a Weighing Ba 2 Ti 9 O 20 And Ba 6-3x Re 8+2x Ti 18 O 54 1 percent of Al in percentage by mass 2 O 3 Powder, 3% ZnO powder, 2.3% SiO 2 Powder, 2.4% Nb 2 O 5 Powder, 0.04% MnO 2 Mixing the powder with 0.1% of MgO powder to obtain a third mixture; and then mixing the third mixture, deionized water and a ball milling medium according to a mass ratio of 1: 1.4: 5, performing vibration grinding in a vertical vibration mill for 20-28 h; then, sieving the mixture by a 320-mesh sieve to obtain ceramic slurry; and drying the ceramic slurry at the temperature of 100-140 ℃, and then sieving the dried ceramic slurry with a 100-mesh sieve to obtain the dielectric ceramic material.
Example 3
The embodiment provides a preparation method of a dielectric ceramic material for a BT-BRT composite ultra-low loss multilayer ceramic dielectric capacitor, which comprises the following steps: (1) ba 2 Ti 9 O 20 The synthesis of (2): weighing BaCO according to the molar ratio of 1:4.5 3 Powder and TiO 2 Mixing the powder to obtain a first mixture; and then mixing the first mixture, deionized water and a ball milling medium according to a mass ratio of 1: 1.5: 5 mixing in a ball mill and drying; adding deionized water, sieving, calcining in a heating furnace to synthesize Ba 2 Ti 9 O 20 Sintering the blocks; (2) ba 6-3x Re 8+2x Ti 18 O 54 The synthesis of (2): taking x as 0.4-0.6, and mixing the components in a molar ratio of 6-3 x: 8+2 x: 18 weigh BaCO 3 Powder, Re 2 O 3 Powder and TiO 2 Mixing the powder in a ball mill to obtain a second mixture; the second mixture is sent into a heating furnace for calcination to synthesize Ba 6-3x Re 8+2x Ti 18 O 54 Sintering the blocks; (3) preparing a dielectric ceramic material: weighing Ba in y 0.6 and z 0.4(y + z 1.0) 2 Ti 9 O 20 And Ba 6-3x Re 8+2x Ti 18 O 54 (ii) a Weighing Ba 2 Ti 9 O 20 And Ba 6-3x Re 8+2x Ti 18 O 54 1 percent of Al in percentage by mass 2 O 3 Powder, 3% ZnO powder, 2.5% SiO 2 Powder, 2.4% Nb 2 O 5 Powder, 0.04% MnO 2 Mixing the powder with 0.1% of MgO powder to obtain a third mixture; and then mixing the third mixture, deionized water and a ball milling medium according to a mass ratio of 1: 1.4: 5, performing vibration grinding in a vertical vibration mill for 20-28 h; then, sieving the mixture by a 320-mesh sieve to obtain ceramic slurry; and drying the ceramic slurry at the temperature of 100-140 ℃, and then sieving the dried ceramic slurry with a 100-mesh sieve to obtain the dielectric ceramic material.
Example 4
The embodiment provides a preparation method of a dielectric ceramic material for a BT-BRT composite ultra-low loss multilayer ceramic dielectric capacitor, which comprises the following steps: (1) ba 2 Ti 9 O 20 The synthesis of (2): weighing BaCO according to the molar ratio of 1:4.5 3 Powder and TiO 2 Mixing the powder to obtain a first mixture; and then mixing the first mixture, deionized water and a ball milling medium according to a mass ratio of 1: 1.5: 5 mixing in a ball mill and drying; adding deionized water, sieving, and heating in a heating furnaceCalcining and synthesizing Ba 2 Ti 9 O 20 Sintering the blocks; (2) ba 6-3x Re 8+2x Ti 18 O 54 The synthesis of (2): taking x as 0.4-0.6, and mixing the components in a molar ratio of 6-3 x: 8+2 x: 18 weigh BaCO 3 Powder, Re 2 O 3 Powder and TiO 2 Mixing the powder in a ball mill to obtain a second mixture; the second mixture is sent into a heating furnace for calcination to synthesize Ba 6-3x Re 8+2x Ti 18 O 54 Sintering the blocks; (3) preparing a dielectric ceramic material: weighing Ba (0.6 and 0.4) in terms of y and z 2 Ti 9 O 20 And Ba 6-3x Re 8+2x Ti 18 O 54 (ii) a Weighing Ba 2 Ti 9 O 20 And Ba 6-3x Re 8+2x Ti 18 O 54 1 percent of Al in percentage by mass 2 O 3 Powder, 3% ZnO powder, 2.3% SiO 2 Powder, 2.4% Nb 2 O 5 Powder, 0.04% MnO 2 Mixing the powder and 0.2% of MgO powder to obtain a third mixture; and then mixing the third mixture, deionized water and a ball milling medium according to a mass ratio of 1: 1.4: 5, performing vibration grinding in a vertical vibration mill for 20-28 h; then, sieving the mixture by a 320-mesh sieve to obtain ceramic slurry; and drying the ceramic slurry at the temperature of 100-140 ℃, and then sieving the dried ceramic slurry with a 100-mesh sieve to obtain the dielectric ceramic material.
Example 5
The embodiment provides a preparation method of a dielectric ceramic material for a BT-BRT composite ultra-low loss multilayer ceramic dielectric capacitor, which comprises the following steps: (1) ba 2 Ti 9 O 20 The synthesis of (2): weighing BaCO according to the molar ratio of 1:4.5 3 Powder and TiO 2 Mixing the powder to obtain a first mixture; and then mixing the first mixture, deionized water and a ball milling medium according to a mass ratio of 1: 1.5: 5 mixing in a ball mill and drying; adding deionized water, sieving, calcining in a heating furnace to synthesize Ba 2 Ti 9 O 20 Sintering the blocks; (2) ba 6-3x Re 8+2x Ti 18 O 54 The synthesis of (2): taking x as 0.4-0.6, and mixing the components in a molar ratio of 6-3 x: 8+2 x: 18 weigh BaCO 3 Powder, Re 2 O 3 Powder and TiO 2 Mixing the powder in a ball mill to obtain a second mixture; the second mixture is sent into a heating furnace for calcination to synthesize Ba 6-3x Re 8+2x Ti 18 O 54 Sintering the blocks; (3) preparing a dielectric ceramic material: weighing Ba in y 0.6 and z 0.4(y + z 1.0) 2 Ti 9 O 20 And Ba 6-3x Re 8+2x Ti 18 O 54 (ii) a Weighing Ba 2 Ti 9 O 20 And Ba 6-3x Re 8+2x Ti 18 O 54 1 percent of Al in percentage by mass 2 O 3 Powder, 3% ZnO powder, 2.5% SiO 2 Powder, 2.4% Nb 2 O 5 Powder, 0.04% MnO 2 Mixing the powder with 0.2% of MgO powder to obtain a third mixture; and then mixing the third mixture, deionized water and a ball milling medium according to a mass ratio of 1: 1.4: 5, performing vibration grinding in a vertical vibration mill for 20-28 h; then, sieving the mixture by a 320-mesh sieve to obtain ceramic slurry; and drying the ceramic slurry at the temperature of 100-140 ℃, and then sieving the dried ceramic slurry with a 100-mesh sieve to obtain the dielectric ceramic material.
Comparative example 1
The comparative example provides a preparation method of a dielectric ceramic material for an ultra-low loss multilayer ceramic dielectric capacitor, which comprises the following steps: (1) ba 6-3x Nd 8+2x Ti 18 O 54 The synthesis of (2): reference examples 1 to 5; (2) preparing a dielectric ceramic material: refer to example 5.
Comparative example 2
The comparative example provides a preparation method of a dielectric ceramic material for a BT-BRT composite ultra-low loss multilayer ceramic dielectric capacitor, which comprises the following steps: (1) ba 2 Ti 9 O 20 The synthesis of (2): reference examples 1 to 5; (2) ba 6-3x Re 8+2x Ti 18 O 54 The synthesis of (2): reference examples 1 to 5; (3) preparing a dielectric ceramic material: weighing Ba 2 Ti 9 O 20 And Ba 6-3x Re 8+2x Ti 18 O 54 9 percent of Al in percentage by mass 2 O 3 Powder, which is partially according to examples 1 to 5.
The formulation comparative examples of examples 1 to 5 and comparative examples 1 to 2 are shown in Table 1:
TABLE 1
The experimental method comprises the following steps: the dielectric ceramic materials prepared in examples 1-5 and comparative examples 1-2 were tested for dielectric constant (. epsilon.) using a precision LCR meter (4980AL, KEYSIGHT), model YD2682A insulation resistance tester, HM27003B capacitance parameter conversion device and high and low temperature test chamber, respectively r ) Dielectric loss factor (tg δ), insulation resistance and temperature coefficient of capacity (a) c ) The test results are shown in table 2:
TABLE 2 dielectric Properties of the dielectric ceramic Material
Serial number | ε r | tgδ(×10 -4 ) | Insulation resistance (x 10) 11 Ω) | a c (ppm/℃) |
Example 1 | 39.8 | 1.2 | >50 | -12.53 |
Example 2 | 39.6 | 1.2 | >50 | -20.9 |
Example 3 | 39.2 | 1.0 | >50 | -9.50 |
Example 4 | 38.9 | 0.9 | >50 | -25.9 |
Example 5 | 39.2 | 0.9 | >50 | -17.9 |
Comparative example 1 | 32.1 | 2.1 | >50 | -29.50 |
Comparative example 2 | 39.4 | 8.3 | >10 | -28.3 |
As can be seen from the data in Table 2: (1) as can be seen by comparing examples 1-5 with comparative example 1, practiceThe overall dielectric properties of examples 1-5 are better than those of comparative example 1, especially tg delta < 1.5X 10 -4 The minimum can be 0.9X 10 -4 Less than 1.0X 10 -4 . Comparative example 1 is a dielectric ceramic material prepared using a single phase doped modification additive. Therefore, the dielectric loss can be greatly reduced by adopting the composite main crystal phase system in the embodiment.
(2) As can be seen by comparing examples 1-5 with comparative example 2, the dielectric properties of examples 1-5 are superior to those of comparative example 2, and tg delta < 1.5X 10 for examples 1-5 -4 Tg δ of less than comparative example 2 is 1.5 × 10 -4 . Comparative example 2 is where the modifying additive used was a single additive. Therefore, the embodiment adopts a plurality of doped additives to improve the dielectric property of the material, and particularly can reduce the tg delta.
SEM characterization of the surface of the prepared dielectric ceramic material provided in example 5 is shown in FIG. 1. As can be seen from FIG. 1, the dielectric ceramic material has uniform and dense grain distribution and grain size less than 10 μm.
XRD characterization was performed on the dielectric ceramic material prepared as provided in example 5, and the results are shown in FIG. 2. The dielectric ceramic material is well-synthesized as can be seen from fig. 2.
In conclusion, the dielectric ceramic material for the BT-BRT composite ultra-low loss multilayer ceramic dielectric capacitor and the preparation method thereof are adopted. The dielectric ceramic material has a dielectric constant of 40 at 1MHz and a dielectric loss value tg delta less than 1.5 multiplied by 10 -4 The dielectric loss value is small; in the temperature range of-55-125 ℃, the capacity is closer to zero along with the temperature coefficient, and the COG characteristic of the American EIA standard is met. The preparation method is simple to operate, adopts a composite main crystal phase system, is easier to obtain a compact ceramic structure compared with a single main crystal phase system, can effectively improve the dielectric loss of the dielectric ceramic, and improves the reliability of the dielectric ceramic material.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (4)
1. The dielectric ceramic material for the BT-BRT composite ultra-low loss multilayer ceramic dielectric container is characterized in that: the raw material comprises BT-BRT compound; the chemical composition formula of the BT-BRT compound is as follows: yBa 2 Ti 9 O 20 -zBa 6-3x Re 8+2x Ti 18 O 54 Wherein x is more than or equal to 0.4 and less than or equal to 0.6, y =0.6, z =0.4, and Re is selected from at least one of Nd, La and Sm;
the raw materials also comprise a modifying additive; the modifying additive comprises a metal oxide;
the metal oxide includes: al (Al) 2 O 3 、ZnO、SiO 2 、Nb 2 O 5 、MnO 2 And MgO;
the Al is 2 O 3 Less than or equal to 3% of the mass of the BT-BRT compound; the ZnO accounts for less than or equal to 3 percent of the mass of the BT-BRT compound; the SiO 2 Less than or equal to 3% of the mass of the BT-BRT compound; the Nb 2 O 5 Less than or equal to 3% of the mass of the BT-BRT compound; the MnO 2 Less than or equal to 3% of the mass of the BT-BRT compound; the MgO accounts for less than or equal to 3% of the mass of the BT-BRT compound.
2. The preparation method of the BT-BRT composite ultra-low loss multilayer ceramic dielectric ceramic material for the capacitor as claimed in claim 1, which is characterized in that: the method comprises the following steps:
(1) said Ba 2 Ti 9 O 20 The synthesis of (2): weighing BaCO according to the molar ratio of 1:4.5 3 And TiO 2 Mixing to obtain a first mixture; then ball-milling the first mixture, drying, sieving and calcining to synthesize the Ba 2 Ti 9 O 20 Sintering the blocks;
(2) said Ba 6-3x Re 8+2x Ti 18 O 54 The synthesis of (2): get x=0.4-0.6, in a molar ratio of 6-3 ×: 8+2 x: 18 weigh BaCO 3 、Re 2 O 3 And TiO 2 Mixing to obtain a second mixture; calcining the second mixture to synthesize the Ba 6-3x Re 8+ 2x Ti 18 O 54 Sintering the blocks;
(3) the preparation of the dielectric ceramic material comprises the following steps: weighing Ba =0.6 and z =0.4 2 Ti 9 O 20 And said Ba 6-3x Re 8+ 2x Ti 18 O 54 Weighing the modified additive according to the proportion, grinding and mixing to obtain the dielectric ceramic material;
(4) mixing the medium ceramic material with paraffin according to the ratio of material powder to paraffin being 100: 7.5, performing wax operation, pressing the ceramic blank into a phi 14 multiplied by 1.5 wafer under the pressure of 200MPa, flatly placing the green blank on a zirconia plate, placing the zirconia plate in a program control furnace, heating the zirconia plate to 1260 to 1280 ℃ at the heating rate of 2.1 ℃/min, preserving the heat for 3 hours, cooling the zirconia plate along with the furnace, taking out the zirconia plate to form a wafer ceramic body, coating silver electrodes on two surfaces of the wafer ceramic body, and testing the electrical property of the wafer ceramic body.
3. The preparation method of the dielectric ceramic material for the BT-BRT composite ultra-low loss multilayer ceramic dielectric capacitor according to claim 2, which is characterized in that: in the step (1), the drying temperature is 100-140 ℃.
4. Use of a dielectric ceramic material according to claim 1 in a multilayer ceramic dielectric capacitor.
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