CN110885249A - Barium-based perovskite ceramic material, and preparation method and application thereof - Google Patents
Barium-based perovskite ceramic material, and preparation method and application thereof Download PDFInfo
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- 229910010293 ceramic material Inorganic materials 0.000 title claims abstract description 31
- 229910052788 barium Inorganic materials 0.000 title claims abstract description 25
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 title claims abstract description 25
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 239000002994 raw material Substances 0.000 claims abstract description 32
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims abstract description 24
- 238000005245 sintering Methods 0.000 claims abstract description 17
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000001035 drying Methods 0.000 claims abstract description 14
- AYJRCSIUFZENHW-UHFFFAOYSA-L barium carbonate Chemical compound [Ba+2].[O-]C([O-])=O AYJRCSIUFZENHW-UHFFFAOYSA-L 0.000 claims abstract description 12
- 239000000463 material Substances 0.000 claims abstract description 12
- 238000002156 mixing Methods 0.000 claims abstract description 12
- 238000007873 sieving Methods 0.000 claims abstract description 12
- 239000004372 Polyvinyl alcohol Substances 0.000 claims abstract description 10
- 229920002451 polyvinyl alcohol Polymers 0.000 claims abstract description 10
- YBMRDBCBODYGJE-UHFFFAOYSA-N germanium oxide Inorganic materials O=[Ge]=O YBMRDBCBODYGJE-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000000227 grinding Methods 0.000 claims abstract description 6
- 239000000843 powder Substances 0.000 claims description 9
- 238000000498 ball milling Methods 0.000 claims description 8
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 229920000728 polyester Polymers 0.000 claims description 4
- 238000003825 pressing Methods 0.000 claims description 4
- 239000003985 ceramic capacitor Substances 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims 8
- 238000005265 energy consumption Methods 0.000 abstract description 4
- 239000003989 dielectric material Substances 0.000 abstract description 2
- 238000000034 method Methods 0.000 description 4
- 239000003990 capacitor Substances 0.000 description 2
- 239000011363 dried mixture Substances 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000010532 solid phase synthesis reaction Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 1
- 229910021523 barium zirconate Inorganic materials 0.000 description 1
- DQBAOWPVHRWLJC-UHFFFAOYSA-N barium(2+);dioxido(oxo)zirconium Chemical compound [Ba+2].[O-][Zr]([O-])=O DQBAOWPVHRWLJC-UHFFFAOYSA-N 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 239000011812 mixed powder Substances 0.000 description 1
- 238000010295 mobile communication Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 230000010287 polarization Effects 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
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- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/48—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on zirconium or hafnium oxides, zirconates, zircon or hafnates
- C04B35/49—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on zirconium or hafnium oxides, zirconates, zircon or hafnates containing also titanium oxides or titanates
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3205—Alkaline earth oxides or oxide forming salts thereof, e.g. beryllium oxide
- C04B2235/3215—Barium oxides or oxide-forming salts thereof
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3287—Germanium oxides, germanates or oxide forming salts thereof, e.g. copper germanate
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Abstract
A barium-based perovskite ceramic material, a preparation method and applications thereof, wherein the preparation method comprises the step of using a raw material BaCO3、TiO2、ZrO2、GeO2According to Ba (Zr)0.2Ti0.8‑xGex)O3The stoichiometric formula of (1) is prepared, pretreated and then presintered, wherein x is 0.001 to 0.00175; mixing the pre-sintered raw materials with polyvinyl alcohol, grinding, drying and sieving; preparing the sieved material into a green body; and sintering the blank to obtain the barium-based perovskite ceramic material. The invention keeps Ba (Zr)0.2Ti0.8)O3On the basis of high dielectric constant of the dielectric material, the dielectric loss of the material is further reduced, and the requirement that the MLCC gradually develops towards miniaturization and low energy consumption is met.
Description
Technical Field
The invention belongs to the field of ceramic materials, and particularly relates to a barium-based perovskite ceramic material, and a preparation method and application thereof.
Background
With the development of electronic equipment towards miniaturization, informatization and high intelligence, the requirements of miniaturization, integration and low energy consumption are also put forward for electronic components. A Multi-layer ceramic chip capacitor (MLCC) is a chip capacitor suitable for Surface mounting of Surface Mount Technology (SMT), and has a wide application in electronic products such as the internet, mobile communication devices, computers, digital cameras, smart phones, new-generation digital home appliances, and the like, and therefore, it is very important to reduce the size of the MLCC and reduce the power consumption of the MLCC to achieve the miniaturization and low energy consumption of electronic devices and electronic equipment.
Barium zirconate titanate (Ba (Zr)0.2Ti0.8)O3) The ceramic material has high dielectric constant and moderate dielectric loss, has wide application prospect in MLCC, and needs to further reduce the dielectric loss on the basis of keeping the high dielectric constant in order to adapt to the development trend of miniaturization and low loss of the MLCC.
Disclosure of Invention
In view of the above, one of the main objects of the present invention is to provide a barium-based perovskite ceramic material, a preparation method and applications thereof, which are intended to at least partially solve at least one of the above technical problems.
In order to achieve the above object, as one aspect of the present invention, there is provided a method for preparing a barium-based perovskite ceramic material, comprising the steps of:
(1) mixing the raw material BaCO3、TiO2、ZrO2、GeO2According to Ba (Zr)0.2Ti0.8-xGex)O3The stoichiometric formula of (1) is prepared, pretreated and then presintered, wherein x is 0.001 to 0.00175;
(2) mixing the pre-sintered raw materials with polyvinyl alcohol, grinding, drying and sieving;
(3) preparing the material sieved in the step (2) into a green body;
(4) and sintering the blank to obtain the barium-based perovskite ceramic material.
As another aspect of the invention, a barium-based perovskite ceramic material is also provided, which is obtained by the preparation method.
As a further aspect of the present invention, there is also provided a use of the barium-based perovskite ceramic material as described above in the field of multilayer chip ceramic capacitors.
Based on the technical scheme, compared with the prior art, the barium-based perovskite ceramic material, the preparation method and the application thereof have at least one of the following advantages:
1. the invention keeps Ba (Zr)0.2Ti0.8)O3On the basis of high dielectric constant of the dielectric material, the dielectric loss of the material is further reduced, and the requirement that the MLCC gradually develops towards miniaturization and low energy consumption is met;
2. the invention prepares high dielectric constant low dielectric loss ceramic material Ba (Zr) for MLCC by a solid phase method0.2Ti0.8-xGex)O3(x is 0.001 to 0.00175). Measured at a frequency of 1kHz, and has a dielectric constant ε at room temperaturer9357 to 11220, and a dielectric loss of 0.001 to 0.003.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments.
The invention discloses a preparation method of a barium-based perovskite ceramic material, which comprises the following steps:
(1) mixing the raw material BaCO3、TiO2、ZrO2、GeO2According to Ba (Zr)0.2Ti0.8-xGex)O3The stoichiometric formula of (1) is prepared, pretreated and then presintered, wherein x is 0.001 to 0.00175;
(2) mixing the pre-sintered raw materials with polyvinyl alcohol, grinding, drying and sieving;
(3) preparing the material sieved in the step (2) into a green body;
(4) and sintering the blank to obtain the barium-based perovskite ceramic material.
The pre-sintering step in the step (1) comprises the steps of putting the raw materials into a medium-temperature furnace, and pre-sintering for 2 to 6 hours at the temperature of 1000 to 1100 ℃.
Wherein the pretreatment step in step (1) comprises:
putting the raw materials into a polyester tank, adding deionized water and zirconia balls, carrying out ball milling for 4-8 hours, drying the ball-milled raw materials at 100-120 ℃, and sieving the dried raw materials with a 40-60-mesh sieve to obtain the pretreated raw materials.
Wherein the total mass ratio of the polyvinyl alcohol to the raw material in the step (2) is 0.5 wt% to 1 wt%.
Wherein the grinding time in the step (2) is 12 to 14 hours;
the drying temperature in the step (2) is 100 to 120 ℃.
Wherein, the mesh number of the sieve in the sieving step in the step (2) is 80 to 100 meshes.
Wherein the blank in the step (3) has a diameter of 10 to 15mm and a thickness of 0.8 to 1 mm;
and (3) the preparation method of the green body comprises the step of pressing the material sieved in the step (2) into the green body by using a powder tablet press under the pressure of 2-6 MPa.
Wherein the sintering temperature in the step (4) is 1300-1350 ℃, and the sintering time is 4 hours.
The invention also discloses a barium-based perovskite ceramic material which is obtained by adopting the preparation method;
the barium-based perovskite ceramic material is tested at the frequency of 1kHz, the room-temperature dielectric constant is 9357-11220, and the dielectric loss is 0.001-0.003.
The invention also discloses application of the barium-based perovskite ceramic material in the field of multilayer chip ceramic capacitors.
In one exemplary embodiment, the high dielectric constant low dielectric loss barium-based perovskite of the present inventionA mineral ceramic material having the chemical formula: ba (Zr)0.2Ti0.8-xGex)O3Wherein x is 0.001-0.00175;
the preparation method of the ceramic material comprises the following specific steps:
(1) mixing BaCO3、TiO2、ZrO2、GeO2In stoichiometric formula Ba (Zr)0.2Ti0.8-xGex)O3(wherein x is 0.001-0.00175), burdening, putting the powder raw materials into a polyester tank, adding deionized water and zirconia balls, and ball-milling for 4-8 hours;
(2) putting the ball-milled raw materials in the step (1) into a drying oven, drying at 100-120 ℃, and then sieving with a 40-mesh sieve;
(3) putting the dried and sieved powder raw material in the step (2) into a medium-temperature furnace, pre-sintering at 1000-1100 ℃, and preserving heat for 2-6 hours;
(4) mixing the pre-sintered powder raw material in the step (3) with PVA (polyvinyl alcohol), putting the mixture into a ball milling tank, adding zirconia balls and deionized water, carrying out ball milling for 10-14 hours, drying the mixture, sieving the dried mixture by using an 80-mesh sieve, and pressing the dried mixture by using a powder tablet press at the pressure of 2-6 MPa to form a blank; wherein the mass of the PVA is 0.5 percent of the total mass of the raw materials
(5) And (4) sintering the green body obtained in the step (4) at 1300-1325 ℃, and preserving heat for 2-6 hours to prepare the high-dielectric-constant low-dielectric-loss ceramic material for the MLCC.
Wherein, the diameter of the green body in the step (4) is 10mm, and the thickness is 1 mm.
Wherein the forming pressure of the blank body in the step (4) is 2-6 MPa, such as 4 MPa.
Wherein the sintering temperature of the step (5) is 1325 ℃.
Wherein said step (4) x is 0.0015.
The technical solution of the present invention is further illustrated by the following specific examples. It should be noted that the following specific examples are given by way of illustration only and the scope of the present invention is not limited thereto.
The chemicals and raw materials used in the following examples were either commercially available or self-prepared by a known preparation method.
BaCO is used in the following examples3(analytically pure), TiO2(analytical grade), ZrO2(analytically pure), GeO2(super pure) is used as an initial raw material, and the dielectric ceramic material for the MLCC is prepared by a solid phase method.
Example 1
The specific embodiment is as follows:
(1) mixing BaCO3、TiO2、ZrO2、GeO2In stoichiometric formula Ba (Zr)0.2Ti0.8-xGex)O3(x is 0.001-0.00175), mixing, putting the mixed powder raw material into a polyester tank, adding 200ml of deionized water, adding 150g of zirconium balls, and then ball-milling for 6 hours on a planetary ball mill at the rotating speed of 400 r/min;
(2) putting the ball-milled raw materials into a drying box respectively, drying at 100 ℃, and then sieving with a 40-mesh sieve respectively;
(3) putting the dried and sieved powder raw material into a medium-temperature furnace, pre-sintering at 1000-1100 ℃, and preserving heat for 4 hours;
(4) adding PVA with the mass ratio of 0.5 wt% of the total raw materials into the pre-sintered powder raw materials in the step (3), mixing, putting into a ball milling tank, adding zirconia balls and deionized water, carrying out ball milling for 12 hours, drying at 100 ℃, sieving with an 80-mesh sieve, and pressing and molding into a blank by using a powder tablet press under the pressure of 4 MPa; the diameter of the blank body is 10mm, and the thickness of the blank body is 1 mm.
(5) Sintering the green body at 1300-1350 ℃, and preserving heat for 4 hours to prepare Ba (Zr) with high dielectric constant and low dielectric loss0.2Ti0.8-xGex)O3A material.
The resulting article was tested for dielectric properties by TH 2828S.
Examples 2 to 12
Examples 2-12 the specific process steps are substantially the same as in example 1, with the relevant main process parameters and their dielectric properties detailed in table 1.
TABLE 1
As can be seen from Table 1, the barium-based perovskite ceramic material prepared by the present invention has a higher dielectric constant and a lower dielectric loss, which is due to the barium-based perovskite ceramic material prepared by the present invention, Ge4+Ions and Zr4+/Ti4+The electrovalence is the same, and the ionic radius is similar, so that redundant electrons and holes are not generated, and the dielectric loss is reduced. In addition, a small amount of Ge4+The ion substitution ensures that the polarization mechanism of the material is not influenced, so that the dielectric constant of the material is basically unchanged. In conclusion, the barium-based perovskite ceramic material prepared by the method can greatly reduce the dielectric loss (2 orders of magnitude) while maintaining the high dielectric constant of the original material system.
The above-mentioned embodiments are intended to illustrate the objects, technical solutions and advantages of the present invention in further detail, and it should be understood that the above-mentioned embodiments are only exemplary embodiments of the present invention and are not intended to limit the present invention, and any modifications, equivalents, improvements and the like made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A preparation method of a barium-based perovskite ceramic material comprises the following steps:
(1) mixing the raw material BaCO3、TiO2、ZrO2、GeO2According to Ba (Zr)0.2Ti0.8-xGex)O3The stoichiometric formula of (1) is prepared, pretreated and then presintered, wherein x is 0.001 to 0.00175;
(2) mixing the pre-sintered raw materials with polyvinyl alcohol, grinding, drying and sieving;
(3) preparing the material sieved in the step (2) into a green body;
(4) and sintering the blank to obtain the barium-based perovskite ceramic material.
2. The production method according to claim 1,
the pre-sintering step in the step (1) comprises the steps of putting the raw materials into a medium-temperature furnace, and pre-sintering for 2 to 6 hours at the temperature of 1000 to 1100 ℃.
3. The production method according to claim 1,
the pretreatment step in step (1) comprises:
putting the raw materials into a polyester tank, adding deionized water and zirconia balls, carrying out ball milling for 4-8 hours, drying the ball-milled raw materials at 100-120 ℃, and sieving the dried raw materials with a 40-60-mesh sieve to obtain the pretreated raw materials.
4. The production method according to claim 1,
the total mass ratio of the polyvinyl alcohol to the raw material in the step (2) is 0.5 wt% to 1 wt%.
5. The production method according to claim 1,
the grinding time in the step (2) is 12 to 14 hours;
the drying temperature in the step (2) is 100 to 120 ℃.
6. The production method according to claim 1,
the mesh number of the sieve in the sieving step in the step (2) is 80 to 100 meshes.
7. The production method according to claim 1,
the diameter of the blank in the step (3) is 10-15 mm, and the thickness of the blank is 0.8-1 mm;
and (3) the preparation method of the green body comprises the step of pressing the material sieved in the step (2) into the green body by using a powder tablet press under the pressure of 2-6 MPa.
8. The production method according to claim 1,
the sintering temperature in the step (4) is 1300-1350 ℃, and the sintering time is 4 hours.
9. A barium-based perovskite ceramic material obtained by the production method as claimed in any one of claims 1 to 8,
the barium-based perovskite ceramic material has a room temperature dielectric constant of 9357 to 11220 and a dielectric loss of 0.001 to 0.003 when tested at a frequency of 1 kHz.
10. Use of the barium-based perovskite ceramic material as claimed in claim 9 in the field of multilayer chip ceramic capacitors.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101691298A (en) * | 2008-02-05 | 2010-04-07 | Tdk株式会社 | Dielectric ceramic composition and an electronic component |
| CN103650323A (en) * | 2011-07-05 | 2014-03-19 | 佳能株式会社 | Piezoelectric element, multilayered piezoelectric element, liquid discharge head, liquid discharge apparatus, ultrasonic motor, optical apparatus, and electronic apparatus |
| CN105272233A (en) * | 2015-10-30 | 2016-01-27 | 天津大学 | Dielectric material for ceramic capacitor and preparation method of dielectric material |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101691298A (en) * | 2008-02-05 | 2010-04-07 | Tdk株式会社 | Dielectric ceramic composition and an electronic component |
| CN103650323A (en) * | 2011-07-05 | 2014-03-19 | 佳能株式会社 | Piezoelectric element, multilayered piezoelectric element, liquid discharge head, liquid discharge apparatus, ultrasonic motor, optical apparatus, and electronic apparatus |
| CN105272233A (en) * | 2015-10-30 | 2016-01-27 | 天津大学 | Dielectric material for ceramic capacitor and preparation method of dielectric material |
Non-Patent Citations (1)
| Title |
|---|
| HA, JONG-YOON，ET AL: "Improved Dielectric Properties of Low-Temperature-Sintered (Ba,Sr)TiO3-Based Ceramics by Ge Substitution", 《JAPANESE JOURNAL OF APPLIED PHYSICS》 * |
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