CN109970446B - Strontium bismuth titanium-based energy storage medium material for medium-temperature sintering and preparation method thereof - Google Patents
Strontium bismuth titanium-based energy storage medium material for medium-temperature sintering and preparation method thereof Download PDFInfo
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- 239000000463 material Substances 0.000 title claims abstract description 56
- 238000005245 sintering Methods 0.000 title claims abstract description 46
- 238000004146 energy storage Methods 0.000 title claims abstract description 34
- NOJHQZPGGBLCPR-UHFFFAOYSA-N [Bi].[Sr].[Ti] Chemical compound [Bi].[Sr].[Ti] NOJHQZPGGBLCPR-UHFFFAOYSA-N 0.000 title claims abstract description 23
- 238000002360 preparation method Methods 0.000 title abstract description 8
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 26
- 239000003607 modifier Substances 0.000 claims abstract description 22
- UPWOEMHINGJHOB-UHFFFAOYSA-N cobalt(III) oxide Inorganic materials O=[Co]O[Co]=O UPWOEMHINGJHOB-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000003989 dielectric material Substances 0.000 claims abstract description 11
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 claims abstract description 10
- 239000000347 magnesium hydroxide Substances 0.000 claims abstract description 10
- 229910001862 magnesium hydroxide Inorganic materials 0.000 claims abstract description 10
- 239000011656 manganese carbonate Substances 0.000 claims abstract description 10
- 229910000016 manganese(II) carbonate Inorganic materials 0.000 claims abstract description 10
- 229910014031 strontium zirconium oxide Inorganic materials 0.000 claims abstract description 9
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 claims abstract description 7
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims abstract description 4
- VTYYLEPIZMXCLO-UHFFFAOYSA-L calcium carbonate Substances [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims abstract description 4
- 229910000019 calcium carbonate Inorganic materials 0.000 claims abstract description 4
- 229910052681 coesite Inorganic materials 0.000 claims abstract description 4
- 229910052906 cristobalite Inorganic materials 0.000 claims abstract description 4
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 4
- 229910052682 stishovite Inorganic materials 0.000 claims abstract description 4
- 229910052905 tridymite Inorganic materials 0.000 claims abstract description 4
- 238000000498 ball milling Methods 0.000 claims description 20
- 238000001035 drying Methods 0.000 claims description 18
- 239000000203 mixture Substances 0.000 claims description 17
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 16
- 239000000919 ceramic Substances 0.000 claims description 12
- 239000008367 deionised water Substances 0.000 claims description 10
- 229910021641 deionized water Inorganic materials 0.000 claims description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- 239000000843 powder Substances 0.000 claims description 9
- 239000002994 raw material Substances 0.000 claims description 9
- 238000005303 weighing Methods 0.000 claims description 8
- WMWLMWRWZQELOS-UHFFFAOYSA-N bismuth(III) oxide Inorganic materials O=[Bi]O[Bi]=O WMWLMWRWZQELOS-UHFFFAOYSA-N 0.000 claims description 7
- 238000000227 grinding Methods 0.000 claims description 7
- 238000000034 method Methods 0.000 claims description 6
- 238000007873 sieving Methods 0.000 claims description 6
- 239000012856 weighed raw material Substances 0.000 claims description 5
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 4
- 239000007864 aqueous solution Substances 0.000 claims description 4
- 238000005469 granulation Methods 0.000 claims description 4
- 230000003179 granulation Effects 0.000 claims description 4
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 4
- 238000001354 calcination Methods 0.000 claims description 3
- 238000000465 moulding Methods 0.000 claims 1
- 230000015556 catabolic process Effects 0.000 abstract description 13
- 238000009413 insulation Methods 0.000 abstract description 9
- 238000010532 solid phase synthesis reaction Methods 0.000 abstract description 3
- 239000003990 capacitor Substances 0.000 description 15
- 238000009472 formulation Methods 0.000 description 12
- 229910010293 ceramic material Inorganic materials 0.000 description 4
- 238000011161 development Methods 0.000 description 4
- 238000012986 modification Methods 0.000 description 4
- 230000004048 modification Effects 0.000 description 4
- 229910000018 strontium carbonate Inorganic materials 0.000 description 4
- LEDMRZGFZIAGGB-UHFFFAOYSA-L strontium carbonate Chemical compound [Sr+2].[O-]C([O-])=O LEDMRZGFZIAGGB-UHFFFAOYSA-L 0.000 description 4
- VEALVRVVWBQVSL-UHFFFAOYSA-N strontium titanate Chemical class [Sr+2].[O-][Ti]([O-])=O VEALVRVVWBQVSL-UHFFFAOYSA-N 0.000 description 4
- JRPBQTZRNDNNOP-UHFFFAOYSA-N barium titanate Chemical class [Ba+2].[Ba+2].[O-][Ti]([O-])([O-])[O-] JRPBQTZRNDNNOP-UHFFFAOYSA-N 0.000 description 3
- 239000011248 coating agent Substances 0.000 description 3
- 238000000576 coating method Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 229910052573 porcelain Inorganic materials 0.000 description 3
- 238000004381 surface treatment Methods 0.000 description 3
- XLJMJLOJFWPNRF-UHFFFAOYSA-N [O-2].[Ti+4].[Bi+3].[Sr+2] Chemical compound [O-2].[Ti+4].[Bi+3].[Sr+2] XLJMJLOJFWPNRF-UHFFFAOYSA-N 0.000 description 2
- 229910002113 barium titanate Inorganic materials 0.000 description 2
- 229910052797 bismuth Inorganic materials 0.000 description 2
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 description 2
- CETPSERCERDGAM-UHFFFAOYSA-N ceric oxide Chemical compound O=[Ce]=O CETPSERCERDGAM-UHFFFAOYSA-N 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 239000010410 layer Substances 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 238000004806 packaging method and process Methods 0.000 description 2
- 238000003825 pressing Methods 0.000 description 2
- 238000007789 sealing Methods 0.000 description 2
- 239000002356 single layer Substances 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- PWYYWQHXAPXYMF-UHFFFAOYSA-N strontium(2+) Chemical compound [Sr+2] PWYYWQHXAPXYMF-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000033228 biological regulation Effects 0.000 description 1
- QAKMMQFWZJTWCW-UHFFFAOYSA-N bismuth titanium Chemical compound [Ti].[Bi] QAKMMQFWZJTWCW-UHFFFAOYSA-N 0.000 description 1
- 239000003985 ceramic capacitor Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- -1 ions forms ion Chemical class 0.000 description 1
- 229910052451 lead zirconate titanate Inorganic materials 0.000 description 1
- HFGPZNIAWCZYJU-UHFFFAOYSA-N lead zirconate titanate Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Ti+4].[Zr+4].[Pb+2] HFGPZNIAWCZYJU-UHFFFAOYSA-N 0.000 description 1
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical class [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 230000010287 polarization Effects 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 239000006104 solid solution Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000011232 storage material Substances 0.000 description 1
- 229910052712 strontium Inorganic materials 0.000 description 1
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
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- C04B35/46—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 titanium oxides or titanates
- C04B35/462—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 titanium oxides or titanates based on titanates
- C04B35/465—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 titanium oxides or titanates based on titanates based on alkaline earth metal titanates
- C04B35/47—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 titanium oxides or titanates based on titanates based on alkaline earth metal titanates based on strontium titanates
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- C04B35/63—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B using additives specially adapted for forming the products, e.g.. binder binders
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- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G4/00—Fixed capacitors; Processes of their manufacture
- H01G4/002—Details
- H01G4/018—Dielectrics
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- H01G4/12—Ceramic dielectrics
- H01G4/1209—Ceramic dielectrics characterised by the ceramic dielectric material
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- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G4/00—Fixed capacitors; Processes of their manufacture
- H01G4/002—Details
- H01G4/018—Dielectrics
- H01G4/06—Solid dielectrics
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Abstract
The invention discloses a strontium bismuth titanium-based energy storage medium material for medium-temperature sintering and a preparation method thereof, wherein the strontium bismuth titanium-based energy storage medium material comprises a base material, a modifier and a sintering aid; the base material is SrO-xBi2O3‑(1+3x)TiO2X is more than or equal to 0.04 and less than or equal to 0.11; the modifier comprises MnCO3、Mg(OH)2、Co2O3And SrZrO3、CeO2And Y2O3One or more than one of the above; the sintering aid comprises H3BO3、ZnO、CaCO3And SiO2Two or more of them. The invention adopts a solid phase method to prepare SrO-xBi2O3‑(1+3x)TiO2The base material is added with the modifier and the sintering aid to obtain the energy storage dielectric material which has higher dielectric constant, breakdown strength and insulation resistivity, lower loss and sintering temperature and stable and adjustable temperature coefficient.
Description
Technical Field
The invention relates to the technical field of electronic information materials and components, in particular to a strontium bismuth titanium-based energy storage medium material for medium-temperature sintering and a preparation method thereof.
Background
The energy storage capacitor has wide application in the fields of hybrid electric vehicles, pulse power supplies, radars, aerospace and the like. With the development of technology, energy storage capacitors are mainly developed toward miniaturization, light weight, high withstand voltage, high reliability and high energy storage. In order to meet the development trend of the energy storage capacitor, the following measures are mainly taken: (1) optimizing a capacitor structure, and adopting a multilayer ceramic capacitor structure; (2) the dielectric material properties are improved, such as increased dielectric constant, increased breakdown strength, and reduced loss. At present, due to the limitation of equipment and process level, the multilayer ceramic dielectric capacitor structure is difficult to further improve. The development of a dielectric material with high dielectric constant, high breakdown strength and low loss is an effective path which can meet the development of the energy storage capacitor.
Currently, the dielectric materials commonly used in the production of energy storage capacitors are: barium titanate series, antiferroelectric dielectric ceramics, titanium dioxide series, and strontium titanate series. The barium titanate ceramic has the advantages of high dielectric constant, large dielectric loss (1-2%), low breakdown voltage (<100kV/cm) and electrostriction, and the characteristics of the barium titanate ceramic reduce the energy storage density of the energy storage capacitor and the reliability of the charging and discharging processes; the antiferroelectric dielectric ceramic is mainly a lead zirconate titanate system, has the advantages of high dielectric constant, high dielectric constant rise after voltage application and the like, but is a lead-containing material, can cause environmental pollution in the production and use processes, and is difficult to be widely applied along with the implementation of the limit or the forbidding of related regulations on the lead-containing material; the titanium dioxide has the advantages of high breakdown voltage (about 350kV/cm), low dielectric loss (about 0.05 percent) and the like, but the low dielectric constant (about 110) is difficult to produce a capacitor with high energy storage density; the strontium titanate system has the advantages of relatively high dielectric constant (approximately equal to 250), low high-frequency loss, high breakdown strength and the like, and in addition, the strontium titanate is of a paraelectric structure at normal temperature, and the electric domain rotation cannot be caused by applying a certain external electric field, so that the reliability of the capacitor is improved, and the service life of the capacitor is prolonged.
However, for energy storage materials, a higher dielectric constant is required to increase the energy storage density of the material system, and usually doping modification is adopted to achieve the purpose. Usually by means of doping modification. The advantage of doping bismuth titanium compound (strontium bismuth titanium material for short) in strontium titanate is mainly to improve the dielectric constant and insulation resistance of the material system and keep very low dielectric loss, mainly because of Sr2+And Bi3+Ion half ofThe diameter is close, bismuth can enter the strontium site to form a solid solution by adding bismuth, and the perovskite structure is still kept; and is due to Sr2+And Bi3+The non-equivalent replacement of two ions forms ion vacancies for maintaining electric neutrality, the vacancies relax the lattice structure, and the relaxed polarization of the ions greatly improves the dielectric constant of the material.
Disclosure of Invention
Aiming at the defects existing in the problems, the invention provides the strontium bismuth titanium-based energy storage medium material for medium-temperature sintering and the preparation method thereof, and the strontium bismuth titanium-based energy storage medium material has the characteristics of high dielectric constant, high breakdown strength, low insulation resistivity, low loss and sintering temperature, and stable and adjustable temperature coefficient.
In order to achieve the purpose, the invention provides a strontium bismuth titanium-based energy storage medium material for medium-temperature sintering, which comprises a base material, a modifier and a sintering aid;
the base material is SrO-xBi2O3-(1+3x)TiO2，0.04≤x≤0.11；
The modifier comprises MnCO3、Mg(OH)2、Co2O3And SrZrO3、CeO2And Y2O3One or more than one of the above;
the sintering aid comprises H3BO3、ZnO、CaCO3And SiO2Two or more of them.
As a further improvement of the invention, the dielectric material is based on 100 parts by weight of SrO-xBi2O3-(1+3x)TiO2The base material comprises the following components in percentage by weight:
SrO-xBi2O3-(1+3x)TiO2100 parts of the raw materials;
MnCO30.16-0.30 portion;
Mg(OH)20.08-0.25 part;
Co2O30.06-0.17 part;
SrZrO30 to 2.50 portions;
CeO20 to 0.18 portion;
Y2O30 to 0.15 portion;
1.50-2.50 parts of sintering aid.
As a further improvement of the invention, the mass fraction of the base stock is 94.30wt% to 98.23 wt%.
The invention also provides a preparation method of the strontium bismuth titanium-based energy storage medium material, which comprises the following steps:
preparing a base material;
weighing the base material, the modifier and the sintering aid, putting the base material, the modifier and the sintering aid into a ball milling tank filled with zirconia balls, adding deionized water for ball milling, drying, grinding and sieving, and bagging for later use.
As a further improvement of the invention, the preparation of the base stock comprises:
analytically pure SrCO is weighed according to the molar ratio of 1: x (1+3x)3、Bi2O3And TiO2Raw materials, wherein x is more than or equal to 0.04 and less than or equal to 0.11;
putting the weighed raw materials into a ball milling tank filled with zirconia balls, and performing mixed ball milling for 7-9 hours by taking deionized water as a medium;
drying in a drying oven at the temperature of 110-120 ℃ for 6-8 hours;
calcining the mixture for 2 to 3 hours in a muffle furnace at the temperature of 1100 to 1200 ℃ to obtain SrO-xBi2O3-(1+3x)TiO2And (3) powder.
As a further improvement of the invention, the ball milling is carried out for 5 hours, the drying is carried out for 6 hours at 120 ℃, and the grinding and the sieving are carried out by a 40-mesh sieve.
Compared with the prior art, the invention has the beneficial effects that:
the invention adopts the traditional solid phase method to prepare the strontium bismuth titanium oxide base material SrO-xBi2O3-(1+3x)TiO2Finally, the ceramic material with high dielectric constant (epsilon: 530-800) and low loss (tan delta: 6-15 multiplied by 10) is obtained by adding a modifier and a sintering aid-4) High insulation resistivity (ρ: 2.9 to 9.9 x 1013Omega cm), high breakdown voltage (> 210kv/cm) and stable temperature coefficient (fluctuation range within + -500 ppm/DEG C). The strontium bismuth titanium-based energy storage dielectric material can be used forThe production of the single-layer or multi-layer ceramic dielectric capacitor has good practical value and wide market prospect.
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 in conjunction with the embodiments of the present invention, and it is obvious that the described embodiments are a part of the embodiments of the present invention, but not all of the embodiments. All other embodiments, which can be obtained by a person skilled in the art without any inventive step based on the embodiments of the present invention, are within the scope of the present invention.
The invention is described in further detail below:
the invention provides a strontium bismuth titanium-based energy storage medium material for medium-temperature sintering, which comprises a base material, a modifier and a sintering aid; wherein:
the base material is SrO-xBi2O3-(1+3x)TiO2，0.04≤x≤0.11；
The modifier comprises MnCO3、Mg(OH)2、Co2O3And SrZrO3、CeO2And Y2O3One or more than one of the above; namely, MnCO3、Mg(OH)2、Co2O3Is an essential component, and SrZrO is added on the basis of the essential component3、CeO2And Y2O3One or more than one of the above;
the sintering aid comprises H3BO3、ZnO、CaCO3And SiO2Two or more of them.
The invention uses 100 weight portions of SrO-xBi2O3-(1+3x)TiO2The base material comprises the following components in percentage by weight:
SrO-xBi2O3-(1+3x)TiO2100 parts of the raw materials;
MnCO30.16-0.30 portion;
Mg(OH)20.08-0.25 part;
Co2O30.06-0.17 part;
SrZrO30 to 2.50 portions;
CeO20 to 0.18 portion;
Y2O30 to 0.15 portion;
1.50-2.50 parts of sintering aid.
Further, a base material (SrO-xBi)2O3-(1+3x)TiO2) The mass fraction of (A) is 94.30wt% -98.23 wt%.
The invention relates to a preparation method of a strontium bismuth titanium-based energy storage medium material for medium-temperature sintering, which comprises the following steps:
step 1, preparing a base material:
analytically pure SrCO is weighed according to the molar ratio of 1: x (1+3x)3、Bi2O3And TiO2Raw materials, wherein x is more than or equal to 0.04 and less than or equal to 0.11; putting the weighed raw materials into a ball milling tank filled with zirconia balls, and performing mixed ball milling for 7-9 hours by taking deionized water as a medium; drying in a drying oven at the temperature of 110-120 ℃ for 6-8 hours; calcining the mixture for 2 to 3 hours in a muffle furnace at the temperature of 1100 to 1200 ℃ to obtain SrO-xBi2O3-(1+3x)TiO2And (3) powder.
And 2, weighing the base material, the modifier and the sintering aid according to the ratio of the base material, the modifier and the sintering aid, putting the base material, the modifier and the sintering aid into a ball milling tank filled with zirconia balls, adding deionized water, ball milling for 5 hours, drying for 6 hours at 120 ℃, grinding, sieving with a 40-mesh sieve, and bagging for later use.
When the performance of the strontium bismuth titanium-based energy storage medium material is required to be tested:
adding the strontium bismuth titanium-based energy storage medium material into a polyvinyl alcohol aqueous solution for granulation and tablet forming, preserving heat at 600 ℃ for 3 hours, raising the temperature to 1140 +/-20 ℃ at 4-5 ℃/min, sintering to form porcelain, performing surface treatment on a wafer sample, coating and firing an electrode, and further testing the performance of the wafer sample.
Example 1:
the invention provides a strontium bismuth titanium-based energy storage medium material for medium-temperature sintering, which comprises a base material, a modifier and a sintering aid; wherein:
SrO-xBi2O3-(1+3x)TiO2to analytically pure SrCO3、Bi2O3And TiO2Raw materials are mixed according to a molar ratio of 1: 0.04: 1.12 weighing SrCO3、Bi2O3And TiO2Putting the weighed raw materials into a ball milling tank filled with zirconia balls, and carrying out mixed ball milling for 9 hours by taking deionized water as a medium; then drying in a drying oven at the drying temperature of 110 ℃ for 8 hours; then calcined in a muffle furnace for 2 hours at 1200 ℃ to obtain SrO-0.04Bi2O3-1.12TiO2And (3) powder.
Weighing the base material, the modifier and the sintering aid according to the weight ratio of the raw materials in the table 1 (unit: g), ball-milling and mixing for 5 hours by taking deionized water as a medium, drying for 6 hours at 120 ℃, taking out ceramic powder, grinding, sieving by a 40-mesh sieve, and then packaging and storing by a self-sealing bag.
Table 1 example 1 correlation formulation
| Material composition | Formulation 1 | Formulation 2 | Formulation 3 | Formulation 4 |
| SrO-0.04Bi2O3-1.12TiO2 | 100 | 100 | 100 | 100 |
| MnCO3 | 0.18 | 0.16 | 0.23 | 0.24 |
| Co2O3 | 0.15 | 0.12 | 0.06 | 0.06 |
| Mg(OH)2 | 0.24 | 0.08 | 0.16 | 0.12 |
| SrZrO3 | 0 | 0 | 0 | 1.2 |
| Y2O3 | 0 | 0.15 | 0.04 | 0 |
| CeO2 | 0.18 | 0 | 0.14 | 0.04 |
| Sintering aid | 2 | 2 | 2.5 | 2.2 |
The performance of the prepared ceramic material is checked: weighing 2g of ceramic powder, adding 0.5ml of 6.5 wt% polyvinyl alcohol aqueous solution for granulation, pressing into a wafer with phi of 10mm under 200MPa, putting the wafer into a resistance furnace, raising the temperature from room temperature to 600 ℃ at 2 ℃/min, preserving the heat for 2 hours, raising the temperature to 1140 ℃ at 5 ℃/min, sintering into porcelain, cooling along with the furnace, carrying out sample surface treatment, coating and sintering electrodes. After the wafer capacitor is manufactured, the capacitance value, the loss, the insulation resistance, the breakdown voltage and the temperature characteristic are tested, the relative dielectric constant, the insulation resistivity, the breakdown field strength and the temperature coefficient are calculated, and the performance parameters are shown in table 2.
Table 2 relevant properties of the formulation of example 1
Example 2:
the invention provides a strontium bismuth titanium-based energy storage medium material for medium-temperature sintering, which comprises a base material, a modifier and a sintering aid; wherein:
SrO-xBi2O3-(1+3x)TiO2to analytically pure SrCO3、Bi2O3And TiO2Raw materials are mixed according to a molar ratio of 1: 0.11: 1.33 weighing SrCO3、Bi2O3And TiO2Putting the weighed raw materials into a ball milling tank filled with zirconia balls, and carrying out mixed ball milling by taking deionized water as a mediumTime is 7 hours; then drying in a drying oven at the temperature of 120 ℃ for 6 hours; then calcined in a muffle furnace for 3 hours at 1100 ℃ to obtain SrO-0.11Bi2O3-1.33TiO2And (3) powder.
The base material, the modifier and the sintering aid are weighed according to the weight ratio in the table 3 (unit: g), deionized water is used as a medium, ball milling and mixing are carried out for 5 hours, drying is carried out for 6 hours at the temperature of 120 ℃, ceramic powder is taken out, grinding and sieving by a 40-mesh sieve are carried out, and then packaging and storage are carried out by a self-sealing bag.
Table 3 example 2 related formulations
| Material composition | Formulation 5 | Formulation 6 | Formulation 7 | Formulation 8 |
| SrO-0.11Bi2O3-1.33TiO2 | 100 | 100 | 100 | 100 |
| MnCO3 | 0.16 | 0.18 | 0.22 | 0.3 |
| Co2O3 | 0.17 | 0.14 | 0.08 | 0.08 |
| Mg(OH)2 | 0.2 | 0.25 | 0.16 | 0.16 |
| SrZrO3 | 0.8 | 0 | 1.8 | 2.5 |
| Y2O3 | 0.15 | 0 | 0.08 | 0 |
| CeO2 | 0 | 0.18 | 0.06 | 0 |
| Sintering aid | 1.5 | 1.6 | 1.5 | 1.8 |
And (3) performing performance test on the prepared ceramic material: weighing 2g of ceramic powder, adding 0.5ml of 6.5 wt% polyvinyl alcohol aqueous solution for granulation, pressing into a wafer with phi of 10mm under 200MPa, putting the wafer into a resistance furnace, raising the temperature from room temperature to 600 ℃ at 2 ℃/min, preserving the heat for 2 hours, raising the temperature to 1140 ℃ at 5 ℃/min, sintering into porcelain, cooling along with the furnace, carrying out sample surface treatment, coating and sintering electrodes. After the wafer capacitor is manufactured, the capacitance value, the loss, the insulation resistance, the breakdown voltage and the temperature characteristic are tested, the relative dielectric constant, the insulation resistivity, the breakdown field strength and the temperature coefficient are calculated, and the performance parameters are shown in table 4.
Table 4 relevant properties of the example 2 formulation
From the above, it can be seen that:
the invention adopts the traditional solid phase method to prepare the strontium bismuth titanium oxide base material SrO-xBi2O3-(1+3x)TiO2Finally, the ceramic material with high dielectric constant (epsilon: 530-800) and low loss (tan delta: 6-15 multiplied by 10) is obtained by adding a modifier and a sintering aid-4) High insulation resistivity (ρ: 2.9 to 9.9 x 1013Omega cm), high breakdown voltage (> 210kv/cm) and stable temperature coefficient (fluctuation range within + -500 ppm/DEG C). The strontium bismuth titanium-based energy storage dielectric material can be used for producing single-layer or multi-layer ceramic dielectric capacitors, and has good practical value and wide market prospect.
The above is only a preferred embodiment of the present invention, and is not intended to limit the present invention, and various modifications and changes will occur to 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 (6)
1. A strontium bismuth titanium-based energy storage medium material for medium-temperature sintering is characterized by comprising a base material, a modifier and a sintering aid;
the base material is SrO-xBi2O3-(1+3x)TiO2，0.04≤x≤0.11；
The modifier comprises MnCO3、Mg(OH)2、Co2O3And SrZrO3、CeO2And Y2O3One or more than one of the above;
the sintering aid comprises H3BO3、ZnO、CaCO3And SiO2Two or more of them.
2. The strontium bismuth titanium-based energy storage dielectric material of claim 1, wherein the dielectric material is based on 100 parts by weight of SrO-xBi2O3-(1+3x)TiO2The base material comprises the following components in percentage by weight:
SrO-xBi2O3-(1+3x)TiO2100 parts of the raw materials;
MnCO30.16-0.30 portion;
Mg(OH)20.08-0.25 portion;
Co2O30.06-0.17 part;
SrZrO30 to 2.50 portions;
CeO20 to 0.18 portion;
Y2O30 to 0.15 portion;
1.50-2.50 parts of sintering aid.
3. The strontium bismuth titanium-based energy storage dielectric material as claimed in claim 1, wherein the mass fraction of the base material is 94.30wt% -98.23 wt%.
4. A method for preparing the strontium bismuth titanium-based energy storage dielectric material as claimed in any one of claims 1 to 3, which comprises the following steps:
preparing a base material;
weighing base materials, a modifier and a sintering aid, putting the base materials, the modifier and the sintering aid into a ball milling tank filled with zirconia balls, adding deionized water for ball milling, drying, grinding and sieving, and bagging for later use;
adding the strontium bismuth titanium-based energy storage medium material into a polyvinyl alcohol aqueous solution for granulation, tabletting and molding, keeping the temperature at 600 ℃ for 2-3 hours, raising the temperature to 1140 +/-20 ℃ at 4-5 ℃/min, and sintering to obtain the ceramic.
5. The method of claim 4, wherein preparing the base stock comprises:
analytically pure SrCO is weighed according to the molar ratio of 1: x (1+3x)3、Bi2O3And TiO2Raw materials, wherein x is more than or equal to 0.04 and less than or equal to 0.11;
putting the weighed raw materials into a ball milling tank filled with zirconia balls, and performing mixed ball milling for 7-9 hours by taking deionized water as a medium;
drying in a drying oven at the temperature of 110-120 ℃ for 6-8 hours;
calcining the mixture for 2 to 3 hours in a muffle furnace at the temperature of between 1100 and 1200 ℃ to obtain SrO-xBi2O3-(1+3x)TiO2And (3) powder.
6. The method of claim 4, wherein the ball milling is performed for 5 hours, the drying is performed at 120 ℃ for 6 hours, and the grinding is performed through a 40-mesh sieve.
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