CN115073165B - Giant dielectric constant BaTiO 3 Ceramic and preparation method thereof - Google Patents

Giant dielectric constant BaTiO 3 Ceramic and preparation method thereof Download PDF

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CN115073165B
CN115073165B CN202210690327.0A CN202210690327A CN115073165B CN 115073165 B CN115073165 B CN 115073165B CN 202210690327 A CN202210690327 A CN 202210690327A CN 115073165 B CN115073165 B CN 115073165B
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朱归胜
徐堃
徐华蕊
赵昀云
张秀云
蒋坤朋
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Guilin University of Electronic Technology
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Abstract

The invention discloses a giant dielectric constant BaTiO 3 Ceramic and preparation method thereof, the BaTiO 3 The ceramic has a V in structure o ·· ‑2Ti′ Ti Defect configuration, the preparation method comprises: (1) BaTiO of 20-200nm size 3 Pressing the powder into a ceramic green body; (2) Sintering under the condition of mixed gas in a 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 giant dielectric constant BaTiO 3 New solutions for ceramic materials.

Description

Giant dielectric constant BaTiO 3 Ceramic and preparation method thereof
Technical Field
The invention relates to the technical field of electronic ceramic materials, in particular to a giant dielectric constant BaTiO 3 Ceramic and its preparation method are provided.
Background
BaTiO 3 Ceramic materials as dielectric materials for monolithic capacitors (MLCC) are currently being developed to enhance BaTiO 3 The ceramic dielectric properties are obtained by adding various compounds and BaTiO 3 Uniformly mixing to prepare slurry, and finally sintering to prepare BaTiO meeting the performance requirement 3 A ceramic dielectric material. The choice of doping element will vary depending on the dielectric material properties requirements, such as La, li, na, K, bi, nd, lu, fe, cr, mn, mg, Y, sm, dy. BaTiO after general doping control 3 Room temperature relative dielectric constant epsilon r < 8000. The giant dielectric constant effect refers to the relative dielectric constant epsilon at room temperature r For schemes doped with special elements, the dielectric constant can reach hundreds of thousands, and the giant dielectric constant has great significance for the development of high capacity of the MLCC.
Disclosure of Invention
The invention providesIn the structure has V o ·· -2Ti′ Ti BaTiO with defect configuration and giant dielectric constant 3 Ceramic dielectric material having a room temperature relative permittivity epsilon at a frequency of 1kHz r > 260000, up to 340000, 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) BaTiO of 20-200nm size 3 The powder is pressed into ceramic green bodies and the glue is discharged in a common way.
(2) Sintering under the condition of mixed gas in a 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 shows the giant dielectric constant BaTiO of the present invention 3 XRD pattern of the ceramic;
FIG. 2 shows the giant dielectric constant BaTiO of the present invention 3 SEM image of ceramic;
FIG. 3 shows the giant dielectric constant BaTiO of the present invention 3 XPS diagram of ceramic;
FIG. 4 shows the giant dielectric constant BaTiO of the present invention 3 Dielectric properties of the ceramic.
Detailed Description
Specific examples are given below to facilitate better understanding of the technical scheme and the technical effects obtained by the present invention.
Example 1:
(1) Taking 1g of nano BaTiO 3 Powder (size 20-200 nm), adding 0.1g of 5% polyvinyl alcohol (PVA), mixing thoroughly, grinding and granulating, and then maintaining under 5Mpa pressure on a tablet press for 90s to obtain ceramic green body.
(2) Heating to 600 ℃ at a heating rate of 2 ℃/min under the air atmosphere, preserving heat for 2 hours, cooling to room temperature along with the furnace, and placing the ceramic green body after glue discharge into a tubular furnace.
(3) In a tube furnace at 1%H 2 Under the atmosphere condition of 99 percent Ar, the temperature is raised to 1150 ℃ at the heating rate of 2 ℃/min, and the BaTiO is obtained after the heat preservation for 2 hours and cooling to the room temperature along with the furnace 3 And (3) ceramics.
The obtained sample tests the room temperature relative dielectric constant epsilon at 1kHz r 340000, dielectric loss tan δ=0.09.
Example 2:
(1) Taking 1g of nano BaTiO 3 The powder (size 20-200 nm) is added with 0.1g of 5% concentration polyvinyl alcohol, fully mixed, ground and granulated, and then the mixture is kept for 90 seconds on a tablet press under the pressure of 5Mpa to prepare the ceramic green body.
(2) Heating to 600 ℃ at a heating rate of 2 ℃/min under the air atmosphere, preserving heat for 2 hours, cooling to room temperature along with the furnace, and placing the ceramic green body after glue discharge into a tubular furnace.
(3) Heating to 1250 ℃ at a heating rate of 2 ℃/min under the atmosphere conditions of 2% CO and 98% Ar in a tube furnace, preserving heat for 1h, and then cooling to room temperature along with the furnace to obtain BaTiO 3 And (3) ceramics.
The obtained sample tests the room temperature relative dielectric constant epsilon at 1kHz r =280000, dielectric loss tan δ=0.11.
Example 3:
(1) Taking 1g of nano BaTiO 3 The powder (size 20-200 nm) is added with 0.1g of 5% concentration polyvinyl alcohol, fully mixed, ground and granulated, and then the mixture is kept for 90 seconds on a tablet press under the pressure of 5Mpa to prepare the ceramic green body.
(2) Heating to 600 ℃ at a heating rate of 2 ℃/min under the air atmosphere, preserving heat for 2 hours, cooling to room temperature along with the furnace, and placing the ceramic green body after glue discharge into a tubular furnace.
(3) In a tube furnace with 0.5% CH 4 Under the atmosphere condition of 99.5 percent Ar, the temperature is raised to 1300 ℃ at the heating rate of 2 ℃/min, and the BaTiO is obtained after the heat preservation for 2 hours and cooling to the room temperature along with the furnace 3 And (3) ceramics.
The obtained sample tests the room temperature relative dielectric constant epsilon at 1kHz r 310000, dielectric loss tan δ=0.10.
Example 4:
(1) Taking 1g of nano BaTiO 3 The powder (size 20-200 nm) is added with 0.1g of 5% concentration polyvinyl alcohol, fully mixed, ground and granulated, and then the mixture is kept for 90 seconds on a tablet press under the pressure of 5Mpa to prepare the ceramic green body.
(2) Heating to 600 ℃ at a heating rate of 2 ℃/min under the air atmosphere, preserving heat for 2 hours, cooling to room temperature along with the furnace, and placing the ceramic green body after glue discharge into a tubular furnace.
(3) In a tube furnace at 4%H 2 Under the atmosphere condition of 96 percent of He, the temperature is raised to 1200 ℃ at the heating rate of 2 ℃/min, and the mixture is cooled to room temperature along with the furnace after the heat preservation for 4 hours, thus obtaining the BaTiO 3 And (3) ceramics.
The obtained sample tests the room temperature relative dielectric constant epsilon at 1kHz r =260000, dielectric loss tan δ=0.19.
Example 5:
(1) Taking 1g of nano BaTiO 3 The powder (size 20-200 nm) is added with 0.1g of 5% concentration polyvinyl alcohol, fully mixed, ground and granulated, and then the mixture is kept for 90 seconds on a tablet press under the pressure of 5Mpa to prepare the ceramic green body.
(2) Heating to 600 ℃ at a heating rate of 2 ℃/min under the air atmosphere, preserving heat for 2 hours, cooling to room temperature along with the furnace, and placing the ceramic green body after glue discharge into a tubular furnace.
(5) In a tube furnace with 3% CO and 97% N 2 Under the atmosphere condition of (2) and at the heating rate of 2 ℃/min, heating to 1400 ℃, preserving heat for 0.5h, and then cooling to room temperature along with the furnace to obtain BaTiO 3 And (3) ceramics. The obtained sample tests the room temperature relative dielectric constant epsilon at 1kHz r =280000, dielectric loss tan δ=0.13.
Example 6:
(1) Taking 1g of nano BaTiO 3 Adding 0.1g of 5% polyvinyl alcohol, mixing, grinding, granulating, and tabletting under 5MpaHolding for 90s to prepare a ceramic green body.
(2) Heating to 600 ℃ at a heating rate of 2 ℃/min under the air atmosphere, preserving heat for 2 hours, cooling to room temperature along with the furnace, and placing the ceramic green body after glue discharge into a tubular furnace.
(3) In a tube furnace at 1%H 2 Under the atmosphere condition of 99% Ne, the temperature is raised to 1300 ℃ at the heating rate of 2 ℃/min, and the furnace is cooled to the room temperature after the heat preservation is carried out for 2 hours. Obtaining BaTiO 3 And (3) ceramics. The obtained sample tests the room temperature relative dielectric constant epsilon at 1kHz r 310000, dielectric loss tan δ=0.11.
The invention has the technical characteristics and beneficial effects that:
unlike conventional method for doping element to obtain giant dielectric effect, the present invention adopts one ion-free doping process to obtain giant dielectric constant BaTiO 3 Ceramic, baTiO can be prepared by constructing a low oxygen partial pressure environment and a certain reducing atmosphere 3 Lattice oxygen is taken out to form V o ·· -2Ti′ Ti Defects, the presence of which causes BaTiO 3 The dielectric constant of the ceramic is greatly improved.
The invention obtains the defect configuration (V) by adopting the specific raw material size, the specific atmosphere condition, the sintering temperature and the heat preservation time o ·· -2Ti′ Ti ) BaTiO causing giant dielectric constant effect 3 Ceramics whose X-ray photoelectron spectroscopy (XPS) shows: the O1s orbit has peak positions of 529-532 eV; the Ti2p orbitals 456-459eV have peak positions.
The specific size of the raw material is generally 20-200nm, and depends on the common influence of sintering atmosphere conditions, sintering temperature and heat preservation time. When the size of the nano powder is larger, the corresponding sintering activity is lower, so that the ratio of the reducing gas in the mixed gas needs to be increased, the sintering temperature is increased, the heat preservation time is prolonged, and the giant dielectric constant BaTiO caused by specific defect configuration can be prepared 3 A ceramic; similarly, when the nano-size is smaller, the ratio of the reducing gas in the mixed gas can be reduced, the sintering temperature can be reduced, and the heat preservation time can be reduced. Therefore, whether or not such giant dielectric constant BaTiO can be produced 3 The key point of the ceramic is that the powder size, the atmosphere condition, the sintering temperature and the heat preservation time act together.

Claims (2)

1. Giant dielectric constant BaTiO 3 Ceramic, characterized in that the BaTiO 3 Ceramic is BaTiO with specific size of 20-200nm 3 The powder is prepared with V in the structure o ·· -2Ti′ Ti Defect configuration.
2. The BaTiO as recited in claim 1 3 A method for preparing a ceramic, the method comprising the steps of:
(1) BaTiO of 20-200nm size 3 Pressing the powder into a ceramic green body;
(2) Sintering under the condition of mixed gas in a 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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JP2003146697A (en) * 2001-11-13 2003-05-21 Sanwa Denzai:Kk Dielectric composition
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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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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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