CN115073165A - Giant dielectric constant BaTiO 3 Ceramic and preparation method thereof - Google Patents
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Abstract
The invention discloses a giant dielectric constant BaTiO 3 Ceramic and preparation method thereof, BaTiO 3 The ceramic having V in the structure o ·· ‑2Ti′ Ti A defect configuration, the method of making comprising: (1) mixing BaTiO with 20-200nm size 3 Pressing the powder into a ceramic green body; (2) sintering under the condition of mixed gas of reducing atmosphere, wherein the mixed gas consists of 0.5-5% of reducing gas and 95-99.5% of inert gas; (3) sintering at 1150-1400 deg.C for 0.5-4 hr. The invention provides a method for obtaining a giant dielectric constant BaTiO 3 A new scheme of ceramic material.
Description
Technical Field
The invention relates to the technical field of electronic ceramic materials, in particular to a giant dielectric constant BaTiO 3 Ceramics and a preparation method thereof.
Background
BaTiO 3 Ceramic materials as dielectric materials for monolithic capacitors (MLCC) are now being developed to enhance BaTiO 3 The performance of the ceramic medium is improved by adding various compounds and BaTiO 3 Evenly mixing the mixture to prepare slurry, and finally sintering the slurry to prepare BaTiO meeting the performance requirement 3 A ceramic dielectric material. The selection of doped elements varies according to the performance requirements of the dielectric material, such as La, Li, Na, K, Bi, Nd, Lu, Fe, Cr, Mn, Mg, Y, Sm, Dy, and the like. General doping-regulated BaTiO 3 Relative dielectric constant ε at room temperature r Is less than 8000. The giant dielectric constant effect refers to the relative dielectric constant ε at room temperature r And the dielectric constant can reach hundreds of thousands for some schemes of doping special elements, and the giant dielectric constant has great significance for the high-capacity development of the MLCC.
Disclosure of Invention
The invention provides a structure having V o ·· -2Ti′ Ti BaTiO with defect configuration and giant dielectric constant 3 A ceramic dielectric material having a relative dielectric constant ε at room temperature at a frequency of 1kHz r 260000 and up to 340000, with a dielectric loss tan delta < 0.19.
The invention also provides the giant dielectric constant BaTiO 3 The preparation method of the ceramic dielectric material comprises the following steps:
(1) mixing BaTiO with 20-200nm size 3 The powder is pressed into a ceramic green body and the binder is removed in the usual way.
(2) Sintering under the condition of mixed gas of reducing atmosphere, wherein the mixed gas consists of 0.5-5% of reducing gas and 95-99.5% of inert gas.
(3) Sintering at 1150-1400 deg.C for 0.5-4 hr.
The reducing gas may be hydrogen (H) 2 ) Carbon monoxide (CO) or methane (CH) 4 )。
The inert gas may be helium (He), neon (Ne), argon (Ar), or nitrogen (N) 2 )。
Drawings
FIG. 1 isThe invention has the advantages of giant dielectric constant BaTiO 3 XRD pattern of the ceramic;
FIG. 2 is a diagram of the giant dielectric constant BaTiO of the present invention 3 SEM images of the ceramics;
FIG. 3 shows the giant dielectric constant BaTiO of the present invention 3 XPS plot of ceramics;
FIG. 4 shows the giant dielectric constant BaTiO of the present invention 3 Dielectric property diagram of ceramics.
Detailed Description
Specific examples are given below to facilitate a better understanding of the technical solutions of the present invention and the technical effects obtained.
Example 1:
(1) 1g of nano-sized BaTiO is taken 3 Adding 0.1g of 5% polyvinyl alcohol (PVA) into the powder (with the size of 20-200nm), mixing, grinding and granulating, and maintaining the pressure at 5Mpa for 90s on a tabletting machine to obtain a ceramic green body.
(2) Heating to 600 ℃ at the heating rate of 2 ℃/min in the air atmosphere, keeping the temperature for 2h, cooling to room temperature along with the furnace, and putting the ceramic green body subjected to rubber removal into a tubular furnace.
(3) 1% H in a tube furnace 2 Heating to 1150 ℃ at the heating rate of 2 ℃/min under the atmosphere condition of 99% Ar, preserving heat for 2h, and cooling to room temperature along with the furnace to obtain BaTiO 3 A ceramic.
The obtained sample was tested for the relative dielectric constant ε at room temperature at a frequency of 1kHz r 340000, the dielectric loss tan δ is 0.09.
Example 2:
(1) 1g of nano-sized BaTiO is taken 3 Adding 0.1g of 5% polyvinyl alcohol into the powder (with the size of 20-200nm), fully mixing, grinding and granulating, and keeping the pressure on a tablet machine at 5Mpa for 90s to prepare a ceramic green body.
(2) Heating to 600 ℃ at the heating rate of 2 ℃/min in the air atmosphere, keeping the temperature for 2h, cooling to room temperature along with the furnace, and putting the ceramic green body subjected to rubber removal into a tubular furnace.
(3) Heating to 1250 ℃ at the heating rate of 2 ℃/min in a tubular furnace under the atmosphere condition of 2% CO and 98% Ar, preserving heat for 1h, and cooling to the chamber along with the furnaceWarming to obtain BaTiO 3 A ceramic.
The obtained sample was tested for the relative dielectric constant ε at room temperature at a frequency of 1kHz r 280000, the dielectric loss tan δ is 0.11.
Example 3:
(1) 1g of nano-sized BaTiO is taken 3 Adding 0.1g of 5% polyvinyl alcohol into the powder (with the size of 20-200nm), fully mixing, grinding and granulating, and keeping the pressure on a tablet machine at 5Mpa for 90s to prepare a ceramic green body.
(2) Heating to 600 ℃ at the heating rate of 2 ℃/min in the air atmosphere, keeping the temperature for 2h, cooling to room temperature along with the furnace, and putting the ceramic green body subjected to rubber removal into a tubular furnace.
(3) In a tube furnace with 0.5% CH 4 Heating to 1300 ℃ at the heating rate of 2 ℃/min under the atmosphere condition of 99.5% Ar, preserving the heat for 2h, and then cooling to the room temperature along with the furnace to obtain BaTiO 3 A ceramic.
The obtained sample was tested for the relative dielectric constant ε at room temperature at a frequency of 1kHz r 310000, the dielectric loss tan δ is 0.10.
Example 4:
(1) 1g of nano-sized BaTiO is taken 3 Adding 0.1g of 5% polyvinyl alcohol into the powder (with the size of 20-200nm), fully mixing, grinding and granulating, and keeping the pressure on a tablet machine at 5Mpa for 90s to prepare a ceramic green body.
(2) Heating to 600 ℃ at the heating rate of 2 ℃/min in the air atmosphere, keeping the temperature for 2h, cooling to room temperature along with the furnace, and putting the ceramic green body subjected to rubber removal into a tubular furnace.
(3) 4% H in tube furnace 2 Heating to 1200 ℃ at a heating rate of 2 ℃/min under the atmosphere condition of 96% He, preserving heat for 4 hours, and then cooling to room temperature along with the furnace to obtain BaTiO 3 A ceramic.
The obtained sample was tested for the relative dielectric constant ε at room temperature at a frequency of 1kHz r 260000, and a dielectric loss tan δ of 0.19.
Example 5:
(1) 1g of nano-sized BaTiO is taken 3 Adding 0.1g of 5% polyvinyl alcohol into the powder (size 20-200nm)Mixing, grinding and granulating, and keeping on a tablet press at 5MPa for 90s to obtain ceramic green body.
(2) Heating to 600 ℃ at the heating rate of 2 ℃/min in the air atmosphere, keeping the temperature for 2h, cooling to room temperature along with the furnace, and putting the ceramic green body subjected to rubber removal into a tubular furnace.
(5) In a tube furnace at 3% CO, 97% N 2 Heating to 1400 ℃ at a heating rate of 2 ℃/min under the atmosphere condition of (1), preserving heat for 0.5h, and then cooling to room temperature along with the furnace to obtain BaTiO 3 A ceramic. The obtained sample was tested for the relative dielectric constant ε at room temperature at a frequency of 1kHz r 280000, and the dielectric loss tan δ is 0.13.
Example 6:
(1) 1g of nano-sized BaTiO is taken 3 Adding 0.1g of 5% polyvinyl alcohol into the powder (with the size of 20-200nm), fully mixing, grinding and granulating, and keeping the pressure on a tablet machine at 5Mpa for 90s to prepare a ceramic green body.
(2) Heating to 600 ℃ at the heating rate of 2 ℃/min in the air atmosphere, keeping the temperature for 2h, cooling to room temperature along with the furnace, and putting the ceramic green body subjected to rubber removal into a tubular furnace.
(3) 1% H in a tube furnace 2 And 99% Ne at a heating rate of 2 ℃/min to 1300 ℃, keeping the temperature for 2h, and then cooling to room temperature along with the furnace. To obtain BaTiO 3 A ceramic. The obtained sample was tested for the relative dielectric constant ε at room temperature at a frequency of 1kHz r 310000, the dielectric loss tan δ is 0.11.
The invention has the technical characteristics and beneficial effects that:
unlike conventional doping method to obtain giant dielectric effect, the present invention adopts one ion-free doping method to obtain giant dielectric constant BaTiO 3 Ceramic, BaTiO can be formed by creating a low oxygen partial pressure environment and a certain reducing atmosphere 3 Oxygen is taken out of the crystal lattice to form V o ·· -2Ti′ Ti A defect, the presence of which causes BaTiO 3 The dielectric constant of the ceramic is greatly improved.
The invention adopts specific raw material size, specific atmosphere condition and sintering temperatureAnd keeping the temperature for a certain time to obtain a specific defect configuration (V) o ·· -2Ti′ Ti ) BaTiO causing giant dielectric constant effect 3 Ceramics, whose X-ray photoelectron spectroscopy (XPS) shows: the O1s track 529-532eV has peak positions; the peak position exists at the Ti2p orbital 456-459 eV.
The specific size of the raw materials is generally 20-200nm, and depends on the combined influence of the sintering atmosphere condition, the sintering temperature and the holding time. When the size of the nano powder is larger, the corresponding sintering activity is lower, so the ratio of reducing gas in mixed gas needs to be increased, the sintering temperature needs to be increased, the heat preservation time needs to be prolonged, and the BaTiO with the giant dielectric constant caused by specific defect configuration can be prepared 3 A ceramic; similarly, when the nanometer size is smaller, the proportion of the reducing gas in the mixed gas can be reduced, the sintering temperature is reduced, and the heat preservation time is reduced. Therefore, whether or not such a giant dielectric constant BaTiO can be prepared 3 The key point of the ceramic lies in the combined action of powder size, atmosphere condition, sintering temperature and heat preservation time.
Claims (2)
1. Giant dielectric constant BaTiO 3 Ceramics, characterized in that the BaTiO 3 The structure of the ceramic has V o ·· -2Ti′ Ti Defect configuration.
2. The BaTiO of claim 1 3 A method for preparing a ceramic, the method comprising the steps of:
(1) mixing BaTiO with 20-200nm size 3 Pressing the powder into a ceramic green body;
(2) sintering under the condition of mixed gas of reducing atmosphere, wherein the mixed gas consists of 0.5-5% of reducing gas and 95-99.5% of inert gas;
(3) sintering at 1150-1400 deg.C for 0.5-4 hr.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN116332639A (en) * | 2022-12-08 | 2023-06-27 | 上海材料研究所有限公司 | Lead-free PTC thermal sensitive ceramic material with low room temperature resistivity and high lift-drag ratio and preparation method thereof |
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| JP2003146697A (en) * | 2001-11-13 | 2003-05-21 | Sanwa Denzai:Kk | Dielectric composition |
| CN103214237A (en) * | 2013-04-02 | 2013-07-24 | 武汉理工大学 | Preparation method of giant-dielectric-constant barium titanate ceramic |
| CN107759215A (en) * | 2017-11-01 | 2018-03-06 | 苏州大学 | The method for preparing huge dielectric constant low-loss ceramic capacitor |
| CN108546115A (en) * | 2018-04-29 | 2018-09-18 | 天津大学 | A kind of barium phthalate base low-loss huge dielectric constant dielectric substance and preparation method thereof |
| CN114230335A (en) * | 2021-12-22 | 2022-03-25 | 福建贝思科电子材料股份有限公司 | BaTiO with giant dielectric constant, low loss and high resistivity3Fine crystal ceramic and its prepn |
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Patent Citations (5)
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| JP2003146697A (en) * | 2001-11-13 | 2003-05-21 | Sanwa Denzai:Kk | Dielectric composition |
| CN103214237A (en) * | 2013-04-02 | 2013-07-24 | 武汉理工大学 | Preparation method of giant-dielectric-constant barium titanate ceramic |
| CN107759215A (en) * | 2017-11-01 | 2018-03-06 | 苏州大学 | The method for preparing huge dielectric constant low-loss ceramic capacitor |
| CN108546115A (en) * | 2018-04-29 | 2018-09-18 | 天津大学 | A kind of barium phthalate base low-loss huge dielectric constant dielectric substance and preparation method thereof |
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| 孙春莲等: "巨介电材料的研究进展", 《电镀与精饰》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116332639A (en) * | 2022-12-08 | 2023-06-27 | 上海材料研究所有限公司 | Lead-free PTC thermal sensitive ceramic material with low room temperature resistivity and high lift-drag ratio and preparation method thereof |
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