CN116375465A - Bi for X7R type MLCC 2 O 3 Doped BaTiO 3 Base ceramic material and preparation method thereof - Google Patents

Bi for X7R type MLCC 2 O 3 Doped BaTiO 3 Base ceramic material and preparation method thereof Download PDF

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CN116375465A
CN116375465A CN202310366023.3A CN202310366023A CN116375465A CN 116375465 A CN116375465 A CN 116375465A CN 202310366023 A CN202310366023 A CN 202310366023A CN 116375465 A CN116375465 A CN 116375465A
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batio
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李欣
赵志雄
刘森伟
张齐
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Shaanxi University of Science and Technology
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Abstract

The invention relates to the field of ceramic materials, and in particular discloses Bi for an X7R type MLCC 2 O 3 Doped BaTiO 3 The preparation method of the base ceramic material comprises the following steps: according to the chemical formula (BaTiO) 3 ‑0.01Nb 2 O 5 ‑0.01MgO)‑xBi 2 O 3 (0 < x < 0.02) by mole percent, taking Nb 2 O 5 、MgO、BaCO 3 、TiO 2 And Bi (Bi) 2 O 3 Mixing to obtain a mixture, performing ball milling on the mixture for the first time, drying, grinding and sieving to obtain a pre-powder body, and pre-sintering the pre-powder body to obtain a blocky solid; crushing the massive solids to obtain solid powder, performing secondary ball milling on the solid powder, drying and sieving to obtain material powder; pouring the material powder into a mould, pressing the material powder into a tablet under the pressure of 550-600N, and demoulding to obtain the finished productPlacing the sample into a cold isostatic press for molding, maintaining the pressure for 180s under the pressure of 250-350 Mpa to obtain a ceramic green sheet, and sintering the ceramic green sheet to obtain Bi 2 O 3 Doped BaTiO 3 A base ceramic material. The ceramic material has the advantages of higher dielectric constant, low dielectric loss and good temperature stability.

Description

Bi for X7R type MLCC 2 O 3 Doped BaTiO 3 Base ceramic materialPreparation method
Technical Field
The invention relates to the technical field of ceramic materials, in particular to Bi for an X7R type MLCC 2 O 3 Doped BaTiO 3 A base ceramic material and a preparation method thereof.
Background
The capacitor is an indispensable electronic element in the circuit, plays roles of energy storage, filtering, decoupling, bypass of alternating current signals, alternating current coupling of alternating current-direct current circuits and the like, and along with continuous development of the electronic industry in recent years, the requirements on the ceramic capacitor in the market are also higher and higher, and miniaturization and high reliability are required. An X7R type multilayer ceramic capacitor (MLCC) is an electronic device with better dielectric constant and temperature stability, and the specific requirements are as follows: the rate of change of capacitance of the ceramic with respect to room temperature (25 ℃) is between-15% and +15% over a temperature range of-55 ℃ and +125 ℃; in view of the superior temperature stability of the X7R type MLCCs, the X7R type MLCCs have been widely used in various electronic terminal devices.
The X7R type MLCC raw material is mainly made of lead-based ceramic material or BaTiO 3 Based on X7R ceramic materials, but existing BaTiO 3 The temperature stability of the base X7R ceramic material is required to be improved, which is not beneficial to the production of subsequent ceramic products; and lead-based ceramic materials are more contaminated.
Therefore, there is a need for a BaTiO for X7R type MLCC having a high dielectric constant, low dielectric loss, and good temperature stability 3 The base ceramic material is used for replacing the lead base ceramic material with larger pollution to become an important candidate material for the multilayer ceramic capacitor in terms of both technology and economy.
Disclosure of Invention
Aiming at the defects existing in the prior art, the invention aims to provide Bi for an X7R type MLCC with higher dielectric constant, low dielectric loss and good temperature stability 2 O 3 Doped BaTiO 3 A base ceramic material and a preparation method thereof.
In order to achieve the above purpose, the invention is realized by adopting the following technical scheme:
bi for X7R type MLCC 2 O 3 Doped BaTiO 3 The preparation method of the base ceramic material comprises the following steps:
1) Preparing a massive solid: according to the chemical formula (BaTiO) 3 -0.01Nb 2 O 5 -0.01MgO)-xBi 2 O 3 (0 < x < 0.02) by mole percent, taking Nb 2 O 5 、MgO、BaCO 3 、TiO 2 And Bi (Bi) 2 O 3 Mixing to obtain a mixture, performing ball milling on the mixture for the first time, drying, grinding and sieving to obtain a pre-powder body, and pre-sintering the pre-powder body to obtain a blocky solid;
the presintering temperature is 1080-1120 ℃, and the presintering system is as follows: heating to presintering temperature at 5 ℃/min, preserving heat for 2 hours, cooling to 500 ℃ at 5 ℃/min, and cooling to room temperature along with a furnace;
2) Preparing material powder: crushing the massive solids to obtain solid powder, performing secondary ball milling on the solid powder, drying and sieving to obtain material powder;
3) Preparation of Bi 2 O 3 Doped BaTiO 3 Ceramic material: pouring the material powder into a mould, pressing into a wafer under the pressure of 550-650N, demoulding to obtain a sample with perfect shape, placing the sample into a cold isostatic press for molding, maintaining the pressure for 180s under the pressure of 250-350 Mpa to obtain a ceramic green sheet, and sintering the ceramic green sheet to obtain Bi 2 O 3 Doped BaTiO 3 A base ceramic material;
the sintering temperature is 1250-1300 ℃, and the sintering system is as follows: heating to sintering temperature at 5 deg.c/min, maintaining for 2 hr, cooling to 500 deg.c at 5 deg.c/min, and cooling to room temperature with furnace.
Further, in the first ball milling step in the step 1), the auxiliary materials are zirconia balls and deionized water, and the mass ratio of the mixture, the zirconia balls and the deionized water is 1:5:1.
further, the mixture in the step 1) is subjected to ball milling for the first time, and is dried at 80 ℃ and then is screened by a 120-mesh screen to obtain a pre-powder body.
Further, the drying temperature in the step 1) is 36h.
Further, in the second ball milling step in the step 2), the auxiliary materials are zirconia balls and deionized water, and the mass ratio of the solid powder, the zirconia balls and the deionized water is 1:5:1.
further, in the step 2), after the solid powder is ball-milled for the second time, the solid powder is dried at 80 ℃ and then is screened by a 120-mesh screen to obtain the material powder.
Further, the drying time in the step 2) is 36h.
Bi for X7R type MLCC prepared by the preparation method 2 O 3 Doped BaTiO 3 A base ceramic material.
Compared with the prior art, the invention has the following technical effects:
bi is adopted in the invention 2 O 3 Doped into BaTiO 3 -0.01Nb 2 O 5 In the MgO base material of 0.01, the trivalent Bi ion is synthesized by a solid phase method through the formula design, so that the trivalent Bi ion replaces the divalent Ba ion at the A position. Bi (Bi) 2 O 3 The addition of the (C) can effectively reduce the ferroelectric property of the sample, improve the temperature stability of the sample and widen the temperature range, because of Bi 2 O 3 The doping of the (B) can weaken the ferroelectricity of BT-Nb-Mg ceramics, and simultaneously plays roles of peak shifting and peak pressing, thereby obtaining good temperature stability. In addition, bi 2 O 3 Is doped such that BaTiO 3 -0.01Nb 2 O 5 -0.01 increase of carriers in MgO ceramic material, increase of dielectric constant, and increase of BaTiO 3 -0.01Nb 2 O 5 The temperature stability of the 0.01MgO ceramic is improved.
The preformed powder obtained in the invention enables the solid phase chemical reaction of the raw materials to be fully and uniformly carried out through presintering, forms solid solution with fixed composition, forms a main crystalline phase, simultaneously eliminates carbon dioxide, moisture and the like in the raw materials, reduces shrinkage and deformation of the blank body during sintering, and can also reduce the temperature during sintering. The powder after presintering can realize fine grinding under the action of secondary ball milling, and the ceramic prepared by sintering at a certain temperature is more compact, so that higher dielectric constant, lower dielectric loss and wider temperature stability can be obtained.
In the preparation process of the ceramic material, a more advanced cold isostatic pressing technology is adopted, so that the waste of samples and the addition of binders are avoided, the manufacturing cost is saved, the production period is shortened, the possibility of the binders polluting the samples is avoided, the subsequent steps of binder elimination and resource waste and the waste of manufacturing time are reduced, in addition, as the cold isostatic pressing technology utilizes liquid to transmit pressure, compared with the traditional single-pressurized pressing, the cold isostatic pressing technology can enable the samples to be stressed in all directions, the pressure is larger, the prepared green body is more compact, and a foundation is laid for the next excellent experimental result.
In addition, along with the enhancement of environmental awareness of people, the production of the material avoids the influence on the environment, and the raw materials adopted by the invention are environment-friendly because of no heavy metal elements such as lead and the like, so the preparation process cannot damage the environment. The sintering process adopted by the invention is efficient and energy-saving, reduces the time cost and the power consumption, and accords with the carbon neutralization gist. The material prepared by the invention has good compactness, no obvious air holes exist, and the grain size is uniform, so the invention can ensure Bi 2 O 3 Doped BaTiO 3 -0.01Nb 2 O 5 0.01MgO has better temperature stability.
Drawings
FIG. 1 shows a ceramic material (BaTiO) in example 1 of the present invention 3 -0.01Nb 2 O 5 -0.01MgO)-xBi 2 O 3 An XRD pattern of (x=0.0025, 0.005, 0.010, 0.015);
FIG. 2 shows a ceramic material (BaTiO) in example 1 of the present invention 3 -0.01Nb 2 O 5 -0.01MgO)-xBi 2 O 3 A plot of dielectric constant and dielectric loss versus temperature;
FIG. 3 shows a ceramic material (BaTiO) in example 2 of the present invention 3 -0.01Nb 2 O 5 -0.01MgO)-xBi 2 O 3 A plot of dielectric constant and dielectric loss versus temperature;
FIG. 4 shows a ceramic material (BaTiO) in example 3 of the present invention 3 -0.01Nb 2 O 5 -0.01MgO)-xBi 2 O 3 A plot of dielectric constant and dielectric loss versus temperature;
FIG. 5 shows a ceramic material (BaTiO) in example 4 of the present invention 3 -0.01Nb 2 O 5 -0.01MgO)-xBi 2 O 3 A plot of dielectric constant and dielectric loss versus temperature;
FIG. 6 shows a ceramic material (BaTiO) in example 1 of the present invention 3 -0.01Nb 2 O 5 -0.01MgO)-xBi 2 O 3 (x=0.0025, 0.005, 0.010, 0.015);
FIG. 7 shows a ceramic material (BaTiO) in example 1 of the present invention 3 -0.01Nb 2 O 5 -0.01MgO)-xBi 2 O 3 SEM images of (a);
FIG. 8 shows a ceramic material (BaTiO) in example 2 of the present invention 3 -0.01Nb 2 O 5 -0.01MgO)-xBi 2 O 3 SEM images of (a);
FIG. 9 shows a ceramic material (BaTiO) in example 3 of the present invention 3 -0.01Nb 2 O 5 -0.01MgO)-xBi 2 O 3 SEM images of (a);
FIG. 10 shows a ceramic material (BaTiO) in example 4 of the present invention 3 -0.01Nb 2 O 5 -0.01MgO)-xBi 2 O 3 SEM images of (a).
Detailed Description
The following examples illustrate the invention in further detail.
Examples
Example 1
Bi for X7R type MLCC 2 O 3 Doped BaTiO 3 The preparation method of the base ceramic material comprises the following steps:
1) Preparing a massive solid: according to the chemical formula (BaTiO) 3 -0.01Nb 2 O 5 -0.01MgO)-xBi 2 O 3 (x=0.0025) mole percent of Nb 2 O 5 、MgO、BaCO 3 、TiO 2 And Bi (Bi) 2 O 3 Mixing to obtain a mixture, and taking the mixture and oxygen according to the mass ratio of 1:5:1Mixing zirconium balls and deionized water, ball milling for 10 hours, putting the ball-milled mixture into an electrothermal blowing drying oven, drying at 80 ℃ for 36 hours, grinding, and sieving with a 120-mesh screen to obtain uniform prefabricated powder;
placing the pre-sintered powder into a box furnace for pre-sintering to obtain blocky solid, wherein the pre-sintering temperature is 1080 ℃, and the pre-sintering system is as follows: heating to 1080 ℃ at 5 ℃/min, preserving heat for 2 hours, cooling to 500 ℃ at 5 ℃/min, and cooling to room temperature along with a furnace;
2) Preparing material powder: crushing the massive solids to obtain solid powder, mixing the solid powder, zirconia balls and water according to the mass ratio of 1:5:1, performing ball milling for 10 hours, drying in an electrothermal blowing drying oven at 80 ℃ for 36 hours, and sieving with a 120-mesh screen to obtain material powder with uniform size;
3) Preparation of Bi 2 O 3 Doped BaTiO 3 Ceramic material: weighing 0.35g of material powder, pouring the material powder into a die with the diameter of 10mm, pressing the die into a wafer under the pressure of 550N, demolding to obtain a sample with an intact shape, placing the sample into a cold isostatic press for molding, maintaining the pressure for 180s under the pressure of 250Mpa to obtain a ceramic green sheet, and sintering the ceramic green sheet to obtain Bi 2 O 3 Doped BaTiO 3 Based ceramic materials, i.e. (BaTiO) 3 -0.01Nb 2 O 5 -0.01MgO)-0.0025Bi 2 O 3 ；
The sintering temperature is 1250 ℃, and the sintering system is as follows: heating to 1250 ℃ at 5 ℃/min, preserving heat for 2 hours, cooling to 500 ℃ at 5 ℃/min, and cooling to room temperature along with the furnace.
Example 2
Bi for X7R type MLCC 2 O 3 Doped BaTiO 3 The preparation method of the base ceramic material comprises the following steps:
1) Preparing a massive solid: according to the chemical formula (BaTiO) 3 -0.01Nb 2 O 5 -0.01MgO)-xBi 2 O 3 (x=0.005) mole percent of Nb 2 O 5 、MgO、BaCO 3 、TiO 2 And Bi (Bi) 2 O 3 Mixing to obtain a mixture, mixing the mixture, zirconia balls and deionized water according to the mass ratio of 1:5:1, ball milling for 10 hours, and ball millingPlacing the mixture into an electrothermal blowing drying oven, drying at 80 ℃ for 36 hours, grinding, and sieving with a 120-mesh sieve to obtain uniform prefabricated powder;
placing the pre-sintered powder into a box furnace for pre-sintering to obtain blocky solid, wherein the pre-sintering temperature is 1100 ℃, and the pre-sintering system is as follows: heating to 1100 ℃ at 5 ℃/min, preserving heat for 2 hours, cooling to 500 ℃ at 5 ℃/min, and cooling to room temperature along with a furnace;
2) Preparing material powder: crushing the massive solids to obtain solid powder, mixing the solid powder, zirconia balls and water according to the mass ratio of 1:5:1, performing ball milling for 10 hours, drying in an electrothermal blowing drying oven at 80 ℃ for 36 hours, and sieving with a 120-mesh screen to obtain material powder with uniform size;
3) Preparation of Bi 2 O 3 Doped BaTiO 3 Ceramic material: weighing 0.35g of material powder, pouring the material powder into a die with the diameter of 10mm, pressing the die into a wafer under the pressure of 600N, demolding to obtain a sample with an intact shape, placing the sample into a cold isostatic press for molding, maintaining the pressure for 180s under the pressure of 300Mpa to obtain a ceramic green sheet, and sintering the ceramic green sheet to obtain Bi 2 O 3 Doped BaTiO 3 Based ceramic materials, i.e. (BaTiO) 3 -0.01Nb 2 O 5 -0.01MgO)-0.005Bi 2 O 3 ；
The sintering temperature is 1280 ℃, and the sintering schedule is as follows: heating to 1280 ℃ at 5 ℃/min, preserving heat for 2 hours, cooling to 500 ℃ at 5 ℃/min, and cooling to room temperature along with a furnace.
Example 3
Bi for X7R type MLCC 2 O 3 Doped BaTiO 3 The preparation method of the base ceramic material comprises the following steps:
1) Preparing a massive solid: according to the chemical formula (BaTiO) 3 -0.01Nb 2 O 5 -0.01MgO)-xBi 2 O 3 (x=0.01) mole percent of Nb 2 O 5 、MgO、BaCO 3 、TiO 2 And Bi (Bi) 2 O 3 Mixing to obtain a mixture, mixing the mixture, zirconia balls and deionized water according to the mass ratio of 1:5:1, ball milling for 10 hours, putting the ball-milled mixture into an electrothermal blowing drying oven, and heating to 80 ℃Drying for 36h, grinding, and sieving with 120-mesh sieve to obtain uniform prefabricated powder;
placing the pre-sintered powder into a box furnace for pre-sintering to obtain massive solids, wherein the pre-sintering temperature is 1120 ℃, and the pre-sintering system is as follows: heating to 1120 ℃ at 5 ℃/min, preserving heat for 2 hours, cooling to 500 ℃ at 5 ℃/min, and cooling to room temperature along with a furnace;
2) Preparing material powder: crushing the massive solids to obtain solid powder, mixing the solid powder, zirconia balls and water according to the mass ratio of 1:5:1, performing ball milling for 10 hours, drying in an electrothermal blowing drying oven at 80 ℃ for 36 hours, and sieving with a 120-mesh screen to obtain material powder with uniform size;
3) Preparation of Bi 2 O 3 Doped BaTiO 3 Ceramic material: weighing 0.35g of material powder, pouring the material powder into a die with the diameter of 10mm, pressing the die into a wafer under the pressure of 650N, demolding to obtain a sample with an intact shape, placing the sample into a cold isostatic press for molding, maintaining the pressure for 180s under the pressure of 350Mpa to obtain a ceramic green sheet, and sintering the ceramic green sheet to obtain Bi 2 O 3 Doped BaTiO 3 Based ceramic materials, i.e. (BaTiO) 3 -0.01Nb 2 O 5 -0.01MgO)-0.01Bi 2 O 3 ；
The sintering temperature is 1300 ℃, and the sintering system is as follows: heating to 1300 ℃ at 5 ℃/min, preserving heat for 2 hours, cooling to 500 ℃ at 5 ℃/min, and cooling to room temperature along with the furnace.
Example 4
Bi for X7R type MLCC 2 O 3 Doped BaTiO 3 The preparation method of the base ceramic material comprises the following steps:
1) Preparing a massive solid: according to the chemical formula (BaTiO) 3 -0.01Nb 2 O 5 -0.01MgO)-xBi 2 O 3 (x=0.015) mole percent of Nb 2 O 5 、MgO、BaCO 3 、TiO 2 And Bi (Bi) 2 O 3 Mixing to obtain a mixture, mixing the mixture, zirconia balls and deionized water according to the mass ratio of 1:5:1, ball milling for 10 hours, putting the ball-milled mixture into an electrothermal blowing drying oven, drying at 80 ℃ for 36 hours, grinding, and sieving with a 120-mesh screen to obtain uniform pre-particlesPulverizing;
placing the pre-sintered powder into a box furnace for pre-sintering to obtain blocky solid, wherein the pre-sintering temperature is 1100 ℃, and the pre-sintering system is as follows: heating to 1100 ℃ at 5 ℃/min, preserving heat for 2 hours, cooling to 500 ℃ at 5 ℃/min, and cooling to room temperature along with a furnace;
2) Preparing material powder: crushing the massive solids to obtain solid powder, mixing the solid powder, zirconia balls and water according to the mass ratio of 1:5:1, performing ball milling for 10 hours, drying in an electrothermal blowing drying oven at 80 ℃ for 36 hours, and sieving with a 120-mesh screen to obtain material powder with uniform size;
3) Preparation of Bi 2 O 3 Doped BaTiO 3 Ceramic material: weighing 0.35g of material powder, pouring the material powder into a die with the diameter of 10mm, pressing the die into a wafer under the pressure of 600N, demolding to obtain a sample with an intact shape, placing the sample into a cold isostatic press for molding, maintaining the pressure for 180s under the pressure of 300Mpa to obtain a ceramic green sheet, and sintering the ceramic green sheet to obtain Bi 2 O 3 Doped BaTiO 3 Based ceramic materials, i.e. (BaTiO) 3 -0.01Nb 2 O 5 -0.01MgO)-0.015Bi 2 O 3 ；
The sintering temperature is 1280 ℃, and the sintering schedule is as follows: heating to 1280 ℃ at 5 ℃/min, preserving heat for 2 hours, cooling to 500 ℃ at 5 ℃/min, and cooling to room temperature along with a furnace.
Performance detection
Bi prepared in examples 1 to 4 above was reacted 2 O 3 Doped BaTiO 3 Polishing and cleaning the base ceramic material, and then adding Bi into the ceramic material 2 O 3 Doped BaTiO 3 And uniformly coating silver electrode slurry on the front and back sides of the base ceramic material, and then carrying out heat treatment at 550 ℃ for 25min to obtain the ceramic material for testing. The test ceramic materials prepared from the ceramic materials of examples 1 to 4 were subjected to performance test, and the specific results are shown in FIGS. 1 to 10.
Referring to fig. 1, fig. 1 shows XRD curves of the ceramic materials for testing obtained in examples 1 to 4 described above, as can be seen from fig. 1: ceramic material (BaTiO) 3 -0.01Nb 2 O 5 -0.01MgO)-xBi 2 O 3 (x=0.0025, 0.005, 0.010, 0.015) at different timesThe ceramic material with perovskite crystal structure is synthesized under the doping amount.
Referring to fig. 2 to 5, fig. 2 to 5 are graphs showing the temperature change of the dielectric constant and the dielectric loss of the ceramic materials for test obtained in examples 1 to 4, respectively, and it can be seen that the dielectric constant of the ceramic materials increases and decreases with increasing bi3+ ion doping content, and the inflection point is at the doping amount of x=0.010.
Referring to fig. 6, fig. 6 is a graph showing the rate of change of the capacitance temperature of the ceramic materials for test obtained in examples 1 to 4, and it can be seen from fig. 6 that each of the curves shows good dielectric constant stability in a temperature range of-55 ℃ to +150 ℃ and meets the X7R standard.
Referring to FIGS. 7 to 10, FIGS. 7 to 10 are SEM pictures of the ceramic materials for test obtained in examples 1 to 4, respectively, and it can be seen that the ceramic materials (BaTiO 3 -0.01Nb 2 O 5 -0.01MgO)-xBi 2 O 3 (x=0.0025, 0.005, 0.010 and 0.015) all have good compactness, and with the addition of doping amount, the pores are obviously reduced, and the grain size is firstly reduced and then increased.

Claims (8)

1. Bi for X7R type MLCC 2 O 3 Doped BaTiO 3 The preparation method of the base ceramic material is characterized by comprising the following steps: the method comprises the following steps:
1) Preparing a massive solid: according to the chemical formula (BaTiO) 3 -0.01Nb 2 O 5 -0.01MgO)-xBi 2 O 3 (0 < x < 0.02) by mole percent, taking Nb 2 O 5 、MgO、BaCO 3 、TiO 2 And Bi (Bi) 2 O 3 Mixing to obtain a mixture, performing ball milling on the mixture for the first time, drying, grinding and sieving to obtain a pre-powder body, and pre-sintering the pre-powder body to obtain a blocky solid;
the presintering temperature is 1080-1120 ℃, and the presintering system is as follows: heating to presintering temperature at 5 ℃/min, preserving heat for 2 hours, cooling to 500 ℃ at 5 ℃/min, and cooling to room temperature along with a furnace;
2) Preparing material powder: crushing the massive solids to obtain solid powder, performing secondary ball milling on the solid powder, drying and sieving to obtain material powder;
3) Preparation of Bi 2 O 3 Doped BaTiO 3 Ceramic material: pouring the material powder into a mould, pressing the material powder into a tablet under the pressure of 550-650N, demoulding to obtain a sample with an intact shape, placing the sample into a cold isostatic press for molding, maintaining the pressure for 180s under the pressure of 250-350 Mpa to obtain a ceramic green sheet, and sintering the ceramic green sheet to obtain Bi 2 O 3 Doped BaTiO 3 A base ceramic material;
the sintering temperature is 1250-1300 ℃, and the sintering system is as follows: heating to sintering temperature at 5 deg.c/min, maintaining for 2 hr, cooling to 500 deg.c at 5 deg.c/min, and cooling to room temperature with furnace.
2. The Bi for an X7R-type MLCC according to claim 1 2 O 3 Doped BaTiO 3 The preparation method of the base ceramic material is characterized in that in the first ball milling step in the step 1), the auxiliary materials are zirconia balls and deionized water, and the mass ratio of the mixture, the zirconia balls and the deionized water is 1:5:1.
3. the Bi for an X7R-type MLCC according to claim 1 or 2 2 O 3 Doped BaTiO 3 The preparation method of the base ceramic material is characterized in that the mixture in the step 1) is subjected to ball milling for the first time, and then is dried at 80 ℃ and is screened by a 120-mesh screen to obtain a pre-powder.
4. The Bi for an X7R-type MLCC according to claim 3 2 O 3 Doped BaTiO 3 The preparation method of the base ceramic material is characterized in that the drying temperature in the step 1) is 36h.
5. The Bi for an X7R-type MLCC according to claim 1 2 O 3 Doped BaTiO 3 The preparation method of the base ceramic material is characterized in that in the second ball milling step in the step 2), the auxiliary materials are zirconia balls and deionized water, and the mass ratio of the solid powder to the zirconia balls to the deionized water is 1:5:1.
6. a Bi for an X7R-type MLCC according to claim 1 or 5 2 O 3 Doped BaTiO 3 The preparation method of the base ceramic material is characterized in that the solid powder in the step 2) is subjected to ball milling for the second time, and is dried at 80 ℃ and then is screened by a 120-mesh screen to obtain the material powder.
7. The Bi for X7R-type MLCC according to claim 6 2 O 3 Doped BaTiO 3 The preparation method of the base ceramic material is characterized in that the drying time in the step 2) is 36h.
8. Bi for X7R type MLCC 2 O 3 Doped BaTiO 3 A ceramic-based material, characterized in that it is produced by the production method according to any one of claims 1 to 7.
CN202310366023.3A 2023-04-07 2023-04-07 Bi for X7R type MLCC 2 O 3 Doped BaTiO 3 Base ceramic material and preparation method thereof Pending CN116375465A (en)

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Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101811866A (en) * 2010-03-30 2010-08-25 武汉理工大学 Novel lead-free X8R type capacitor ceramic material and preparation method thereof

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101811866A (en) * 2010-03-30 2010-08-25 武汉理工大学 Novel lead-free X8R type capacitor ceramic material and preparation method thereof

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
LINGXIA LI: "Colossal permittivity (Nb, Mg) co-doped BaTiO3 ceramics with excellent temperature stability and high insulation resistivity", 《CERAMICS INTERNATIONAL》, vol. 47, no. 4, pages 10072 - 10078, XP086501603, DOI: 10.1016/j.ceramint.2020.12.154 *
WU SHUNHUA: "Effect of Bi2O3 Additive on the Microstructure and Dielectric Properties of BaTiO3-Based Ceramics Sintered at Lower Temperature", 《JOURNAL OF MATERIALS SCIENCE & TECHNOLOGY》, vol. 26, no. 5, pages 472 - 476 *

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