CN112390645A - Barium titanate-based relaxor ferroelectric ceramic material with high energy storage density and high power density under high electric field and preparation method thereof - Google Patents
Barium titanate-based relaxor ferroelectric ceramic material with high energy storage density and high power density under high electric field and preparation method thereof Download PDFInfo
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- 238000004146 energy storage Methods 0.000 title claims abstract description 48
- 230000005684 electric field Effects 0.000 title claims abstract description 41
- 229910002113 barium titanate Inorganic materials 0.000 title claims abstract description 28
- JRPBQTZRNDNNOP-UHFFFAOYSA-N barium titanate Chemical compound [Ba+2].[Ba+2].[O-][Ti]([O-])([O-])[O-] JRPBQTZRNDNNOP-UHFFFAOYSA-N 0.000 title claims abstract description 28
- 229910002112 ferroelectric ceramic material Inorganic materials 0.000 title claims abstract description 26
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 229910010252 TiO3 Inorganic materials 0.000 claims abstract description 33
- 239000000463 material Substances 0.000 claims abstract description 29
- 238000000034 method Methods 0.000 claims abstract description 15
- 239000000126 substance Substances 0.000 claims abstract description 9
- 238000005245 sintering Methods 0.000 claims abstract description 8
- 239000000843 powder Substances 0.000 claims description 31
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 30
- 239000000919 ceramic Substances 0.000 claims description 30
- 238000000498 ball milling Methods 0.000 claims description 28
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 23
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 23
- 238000001035 drying Methods 0.000 claims description 15
- AYJRCSIUFZENHW-UHFFFAOYSA-L barium carbonate Chemical compound [Ba+2].[O-]C([O-])=O AYJRCSIUFZENHW-UHFFFAOYSA-L 0.000 claims description 14
- 239000000203 mixture Substances 0.000 claims description 14
- 238000003825 pressing Methods 0.000 claims description 14
- WMWLMWRWZQELOS-UHFFFAOYSA-N bismuth(III) oxide Inorganic materials O=[Bi]O[Bi]=O WMWLMWRWZQELOS-UHFFFAOYSA-N 0.000 claims description 13
- 238000001816 cooling Methods 0.000 claims description 13
- 238000000227 grinding Methods 0.000 claims description 12
- 238000002156 mixing Methods 0.000 claims description 12
- 229910000018 strontium carbonate Inorganic materials 0.000 claims description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 9
- 238000005498 polishing Methods 0.000 claims description 9
- 238000010438 heat treatment Methods 0.000 claims description 8
- MRELNEQAGSRDBK-UHFFFAOYSA-N lanthanum oxide Inorganic materials [O-2].[O-2].[O-2].[La+3].[La+3] MRELNEQAGSRDBK-UHFFFAOYSA-N 0.000 claims description 7
- LEDMRZGFZIAGGB-UHFFFAOYSA-L strontium carbonate Chemical compound [Sr+2].[O-]C([O-])=O LEDMRZGFZIAGGB-UHFFFAOYSA-L 0.000 claims description 7
- 238000007599 discharging Methods 0.000 claims description 6
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 5
- 239000011248 coating agent Substances 0.000 claims description 5
- 238000000576 coating method Methods 0.000 claims description 5
- 238000000465 moulding Methods 0.000 claims description 5
- 238000007873 sieving Methods 0.000 claims description 5
- 229910052709 silver Inorganic materials 0.000 claims description 5
- 239000004332 silver Substances 0.000 claims description 5
- 229910001220 stainless steel Inorganic materials 0.000 claims description 5
- 239000010935 stainless steel Substances 0.000 claims description 5
- 238000009461 vacuum packaging Methods 0.000 claims description 5
- 238000001354 calcination Methods 0.000 claims description 4
- 239000003292 glue Substances 0.000 claims description 3
- 238000004321 preservation Methods 0.000 claims description 3
- 239000007864 aqueous solution Substances 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 2
- 239000011230 binding agent Substances 0.000 claims 1
- 238000011049 filling Methods 0.000 claims 1
- 229910010293 ceramic material Inorganic materials 0.000 abstract description 2
- 238000006243 chemical reaction Methods 0.000 abstract description 2
- 230000007613 environmental effect Effects 0.000 abstract 1
- 238000003746 solid phase reaction Methods 0.000 abstract 1
- 239000010936 titanium Substances 0.000 description 31
- 239000002994 raw material Substances 0.000 description 9
- 239000000243 solution Substances 0.000 description 9
- 239000004570 mortar (masonry) Substances 0.000 description 6
- 230000010287 polarization Effects 0.000 description 6
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 5
- 150000001875 compounds Chemical class 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 239000002904 solvent Substances 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 3
- 239000012856 weighed raw material Substances 0.000 description 3
- 238000005303 weighing Methods 0.000 description 3
- 230000002269 spontaneous effect Effects 0.000 description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003990 capacitor Substances 0.000 description 1
- 239000003985 ceramic capacitor Substances 0.000 description 1
- 239000008358 core component Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000006073 displacement reaction Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 230000001939 inductive effect Effects 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000010295 mobile communication Methods 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000010532 solid phase synthesis reaction Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
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Abstract
The invention relates to a barium titanate-based relaxor ferroelectric ceramic material with high energy storage density and high power density under a high electric field and a preparation method thereof, belonging to the technical field of dielectric ceramic material preparation. The chemical formula of the material disclosed by the invention is 0.65 (Ba)0.985La0.03)Ti0.985O3‑0.35(Sr0.7Bi0.2)TiO3The material has the following properties: the material has high energy storage density under high electric field at room temperature, and the total energy storage density at room temperature under the electric field of 280kV/cm is 2.91J/cm3The effective energy storage density is 2.23J/cm3(ii) a Energy storage efficiency between 10 kV/cm and 280kV/cm>75 percent. The material is synthesized by adopting a solid-phase reaction method at a lower temperature, the preparation steps are simple and convenient, the equipment requirement is low, the reaction condition is simple and easy to control, the repeatability is good, the green environmental protection is realized, the relaxation phenomenon is obvious, and the sintering temperature is lowHaving a high dielectric constant.
Description
Technical Field
The invention belongs to the technical field of dielectric ceramic material preparation, and particularly relates to a barium titanate-based relaxor ferroelectric ceramic material with high energy storage density and high power density under a high electric field and a preparation method thereof.
Background
At present, capacitors with larger power density and higher energy storage density are being widely applied to the pulse fields of mobile communication, medical equipment, military and the like, and dielectric ceramic capacitors are increasingly becoming core components of pulse power supply systems by virtue of superior power density and energy storage density and miniaturization and integration characteristics thereof. Barium titanate, a typical ferroelectric ceramic, has a relatively high relative constant and saturation polarization, and is a potentially ideal matrix ceramic.
However, ferroelectric ceramics generally have some disadvantages, such as residual polarization, large coercive field, low effective energy storage density and energy storage efficiency, etc., which results in great limitations in practical applications. Therefore, the ferroelectric ceramics such as barium titanate are often converted into relaxor ferroelectric ceramics by doping modification and other methods to improve the energy storage efficiency, the effective energy storage density and the power density and enable the relaxor ferroelectric ceramics to bear higher external electric field, so that the relaxor ferroelectric ceramics can better meet the requirements of practical application.
Therefore, further intensive research into barium titanate-based relaxor ferroelectric ceramic materials having high energy storage density and energy storage efficiency and methods for preparing the same is required.
Disclosure of Invention
In view of the above, an object of the present invention is to provide a barium titanate-based relaxor ferroelectric ceramic material having high energy storage density and high power density under a high electric field; the second purpose of the invention is to provide a preparation method of barium titanate-based relaxor ferroelectric ceramic material with high energy storage density and high power density under high electric field.
In order to achieve the purpose, the invention provides the following technical scheme:
1. a barium titanate-based relaxor ferroelectric ceramic material having a high energy storage density and a high power density under a high electric field, the barium titanate-based relaxor ferroelectric ceramic material having a chemical formula of 0.65 (Ba)0.985La0.03)Ti0.985O3-0.35(Sr0.7Bi0.2)TiO3。
2. The preparation method of the barium titanate-based relaxor ferroelectric ceramic material comprises the following steps:
(1) mixing TiO according to the molar ratio of 3961:2561:980:1400:392、BaCO3、SrCO3、Bi2O3And La2O3Ball milling is carried out after mixing, and the mixture is obtained after drying and grinding and sieving by a 60-mesh sieve;
(2) briquetting the mixture in the step (1), presintering at 900-1000 ℃, preserving heat for 1-2 h, cooling to room temperature, and ball-milling again to obtain 0.65 (Ba)0.985La0.03)Ti0.985O3-0.35(Sr0.7Bi0.2)TiO3；
(3) Drying and grinding the material prepared in the step (1) to obtain powder, adding 1 drop of polyvinyl alcohol aqueous solution with the mass fraction of 8-10% into each gram of powder, uniformly mixing, and taking the powder after being sieved by a 60-mesh sieve;
(4) standing the powder obtained by the treatment in the step (3), pressing the powder into a cylindrical blank, and then calcining and discharging the gel to form a blank body;
(5) sintering the blank after the glue is removed in the step (4) at 1180-1200 ℃, and cooling to room temperature to obtain a ceramic wafer;
(6) and (3) sequentially polishing, polishing and drying the ceramic wafer obtained in the step (5), respectively coating silver paste on the upper surface and the lower surface of the ceramic wafer, heating to 600-800 ℃, then carrying out heat preservation treatment for 10-15 min, and cooling to room temperature to obtain the barium titanate-based relaxor ferroelectric ceramic material with high energy storage density and high power density under a high electric field.
Preferably, anhydrous ethanol and zirconia balls are added during ball milling in the step (1), the ball milling time is not less than 24 hours, and the rotating speed during ball milling is 270-330 r/min.
Preferably, the standing time in the step (4) is 24-36 h.
Preferably, the specific method for pressing the cylindrical blank member in the step (4) is as follows: and (3) putting the standing powder into a stainless steel die with the diameter of 10-20 mm, pre-pressing and molding by using a single-shaft tablet press under the pressure of 4-8 MPa, and pressing the pre-pressed cylindrical blank under the pressure of 30-120 MPa by using a hydraulic press after vacuum packaging.
Preferably, the specific method for calcining and removing the glue in the step (4) is that the cylindrical blank is placed in a muffle furnace, heated to 600 ℃, and then kept for 2-4 hours.
Preferably, a crucible with a cover is used as a container during sintering in the step (5), and the same powder is used as a buried material; the time of the sintering treatment is 2 h.
Further preferably, the powder of the same kind is 0.65 (Ba) in the step (3) above0.985La0.03)Ti0.985O3-0.35(Sr0.7Bi0.2)TiO3And polyvinyl alcohol.
Further preferably, the mixture is polyvinyl alcohol with 0.65 (Ba)0.985La0.03)Ti0.985 O3-0.35(Sr0.7Bi0.2)TiO3Is 1: 1.
Preferably, the thickness of the ceramic wafer formed after the grinding and polishing in the step (6) is 0.15-0.2 mm.
Preferably, the TiO in step (1)2、BaCO3、SrCO3、Bi2O3And La2O3The purity of (A) is not less than 99%.
The invention has the beneficial effects that:
1. the invention discloses a barium titanate-based relaxor ferroelectric ceramic material with high energy storage density and high power density under high electric field, and the chemical formula is 0.65 (Ba)0.985La0.03)Ti0.985O3-0.35(Sr0.7Bi0.2)TiO3. The barium titanate-based relaxor ferroelectric ceramic material has the following properties: can resist high electric field at room temperature, has high energy storage density, and has total energy storage density of 2.91J/cm at room temperature under 280kV/cm electric field3The effective energy storage density is 2.23J/cm3(ii) a Energy storage efficiency between 10-280 kV/cm electric field>75 percent; the current peak value in the under-damped charging and discharging process under the electric field of 150kV/cm is 40.6A; the discharge current density is 574.66A/cm2The power density is 43.10MW/cm3。
2. The invention also discloses a preparation method of the barium titanate-based relaxor ferroelectric ceramic material with high energy storage density and high power density under high electric field, the material is prepared by adopting the traditional solid-phase synthesis method at lower temperature, the preparation method has the characteristics of simple operation and low requirement on equipment, the product has high dielectric constant, and meanwhile, the sintering temperature is relatively lower (below 1200 ℃), the reaction condition is easy to control, and the repeatability is good.
Additional advantages, objects, and features of the invention will be set forth in part in the description which follows and in part will become apparent to those having ordinary skill in the art upon examination of the following or may be learned from practice of the invention. The objectives and other advantages of the invention may be realized and attained by the means of the instrumentalities and combinations particularly pointed out hereinafter.
Drawings
For the purposes of promoting a better understanding of the objects, aspects and advantages of the invention, reference will now be made to the following detailed description taken in conjunction with the accompanying drawings in which:
FIG. 1 is a room temperature hysteresis plot of the material prepared in example 1 at different electric field strengths;
FIG. 2 shows the variation of the total energy storage density, the effective energy storage density and the energy storage efficiency of the material prepared in example 1 with the electric field strength at room temperature;
FIG. 3 is an underdamped discharge curve for the material prepared in example 1;
FIG. 4 shows the peak current values at room temperature of the materials prepared in example 1(Imax) Current density (C)D) And power density (P)D) As a function of the electric field.
Detailed Description
The embodiments of the present invention are described below with reference to specific embodiments, and other advantages and effects of the present invention will be easily understood by those skilled in the art from the disclosure of the present specification. The invention is capable of other and different embodiments and of being practiced or of being carried out in various ways, and its several details are capable of modification in various respects, all without departing from the spirit and scope of the present invention. It should be noted that, in the following embodiments, features in the embodiments may be combined with each other without conflict.
Example 1
A compound of formula 0.65 (Ba) was prepared0.985La0.03)Ti0.985O3-0.35(Sr0.7Bi0.2)TiO3The barium titanate-based relaxor ferroelectric ceramic material with high energy storage density and high power density under high electric field comprises the following specific steps:
(1) weighing raw material TiO with the purity of more than 99 percent according to the molar ratio of 3961:2561:980:1400:392、BaCO3、SrCO3、Bi2O3、La2O3Bi2O3、SrCO3And TiO2Mixing the weighed raw materials, putting the mixture into a ball milling tank, adding ball milling solvents of absolute ethyl alcohol (the volume ratio of the absolute ethyl alcohol to the total volume of the added raw materials is 2:1) and zirconia balls (the volume ratio of the zirconia balls to the total volume of the added raw materials is 3:2, wherein the zirconia balls are composed of zirconia balls with the diameter of 10mm and the diameter of 5mm according to the number ratio of 1: 2), ball milling at the ball milling speed of 270r/min for 24 hours, and then putting the balls into an oven at 70 ℃ for drying to obtain a mixture;
(2) putting the mixture obtained in the step (1) into a mortar for grinding and briquetting, presintering in a muffle furnace at 900 ℃, preserving heat for 1 hour, naturally cooling to room temperature, and discharging; the same ball milling was performed again (the ball milling process was the same as in the step (1)), yielding 0.65 (Ba)0.985La0.03)Ti0.985O3-0.35(Sr0.7Bi0.2)TiO3；
(3) Drying the product obtained in the step (2), grinding and sieving the product in a mortar, adding 8 percent of polyvinyl alcohol (PVA) solution by mass percent (wherein the standard of adding PVA is that 0.65 (Ba) is added per 1g0.985La0.03)Ti0.985O3-0.35(Sr0.7Bi0.2)TiO3Adding 1 drop of PVA solution into the powder), uniformly mixing, and taking the powder after being screened by a 60-mesh sieve;
(4) standing the powder obtained by the treatment in the step (3) for 24 hours, putting the powder into a stainless steel mold with the diameter of 10mm, performing pre-pressing molding under the pressure of 4MPa by using a single-shaft tablet press, and pressing the pre-pressed cylindrical blank into a cylindrical blank under the pressure of 30MPa by using a hydraulic press after vacuum packaging;
(5) putting the cylindrical blank in the step (4) into a muffle furnace, heating to 600 ℃, preserving heat for 2 hours, and removing organic matters to obtain a rubber-removed blank;
(6) placing the blank subjected to the rubber removal in the step (5) into a crucible with a cover, and using the same powder (0.65 (Ba)0.985La0.03)Ti0.985O3-0.35(Sr0.7Bi0.2)TiO3And polyvinyl alcohol, wherein the volume of the polyvinyl alcohol is equal to 0.65 (Ba)0.985La0.03)Ti0.985 O3-0.35(Sr0.7Bi0.2)TiO3The volume ratio of (1: 1) is used as a buried material, the buried material is sintered at 1180 ℃, the temperature is kept for 2 hours, and the buried material is naturally cooled to room temperature along with a furnace to obtain a ceramic chip;
(7) polishing the ceramic wafer sintered in the step (6) to the thickness of 0.18mm, drying at 70 ℃, coating silver paste on the upper surface and the lower surface of the ceramic wafer, placing the ceramic wafer in a furnace, heating to 600 ℃, preserving heat for 10min, and naturally cooling to room temperature to obtain the ceramic wafer with the chemical formula of 0.65 (Ba) and high energy density and high power density under a high electric field0.985La0.03)Ti0.985O3-0.35(Sr0.7Bi0.2)TiO3The barium titanate-based relaxor ferroelectric ceramic material.
Example 2
A compound of formula 0.65 (Ba) was prepared0.985La0.03)Ti0.985O3-0.35(Sr0.7Bi0.2)TiO3The barium titanate-based relaxor ferroelectric ceramic material with high energy storage density and high power density under high electric field comprises the following specific steps:
(1) weighing raw material TiO with the purity of more than 99 percent according to the molar ratio of 3961:2561:980:1400:392、BaCO3、SrCO3、Bi2O3、La2O3Bi2O3、SrCO3And TiO2Mixing the weighed raw materials, putting the mixture into a ball milling tank, adding ball milling solvents of absolute ethyl alcohol (the volume ratio of the absolute ethyl alcohol to the total volume of the added raw materials is 2:1) and zirconia balls (the volume ratio of the zirconia balls to the total volume of the added raw materials is 3:2, wherein the zirconia balls are composed of zirconia balls with the diameter of 10mm and the diameter of 5mm according to the number ratio of 1: 2), ball milling at the ball milling speed of 300r/min for 24 hours, and then putting the balls into an oven at 70 ℃ for drying to obtain a mixture;
(2) putting the mixture obtained in the step (1) into a mortar for grinding and briquetting, presintering in a muffle furnace at 900 ℃, preserving heat for 2 hours, naturally cooling to room temperature, and discharging; the same ball milling was performed again (the ball milling process was the same as in the step (1)), yielding 0.65 (Ba)0.985La0.03)Ti0.985O3-0.35(Sr0.7Bi0.2)TiO3；
(3) Drying the product obtained in the step (2), grinding and sieving the product in a mortar, adding 9 percent of polyvinyl alcohol (PVA) solution by mass (wherein the standard of adding PVA is that 0.65 (Ba) is added per 1 g)0.985La0.03)Ti0.985O3-0.35(Sr0.7Bi0.2)TiO3Adding 1 drop of PVA solution into the powder), uniformly mixing, and taking the powder after being screened by a 60-mesh sieve;
(4) standing the powder obtained by the treatment in the step (3) for 30 hours, putting the powder into a stainless steel mold with the diameter of 15mm, performing pre-pressing molding under the pressure of 6MPa by using a single-shaft tablet press, and pressing the pre-pressed cylindrical blank into a cylindrical blank under the pressure of 80MPa by using a hydraulic press after vacuum packaging;
(5) putting the cylindrical blank in the step (4) into a muffle furnace, heating to 600 ℃, preserving heat for 3 hours, and removing organic matters to obtain a rubber-removed blank;
(6) placing the blank subjected to the rubber removal in the step (5) into a crucible with a cover, and using the same powder (0.65 (Ba)0.985La0.03)Ti0.985O3-0.35(Sr0.7Bi0.2)TiO3And polyvinyl alcohol, wherein the volume of the polyvinyl alcohol is equal to 0.65 (Ba)0.985La0.03)Ti0.985 O3-0.35(Sr0.7Bi0.2)TiO3The volume ratio of (1: 1) is used as a buried material, the buried material is sintered at 1180 ℃, the temperature is kept for 2 hours, and the buried material is naturally cooled to room temperature along with a furnace to obtain a ceramic chip;
(7) polishing the ceramic wafer sintered in the step (6) to the thickness of 0.18mm, drying at 70 ℃, coating silver paste on the upper surface and the lower surface of the ceramic wafer, placing the ceramic wafer in a furnace, heating to 800 ℃, preserving heat for 10min, and naturally cooling to room temperature to obtain the ceramic wafer with the chemical formula of 0.65 (Ba) and high energy density and high power density under a high electric field0.985La0.03)Ti0.985O3-0.35(Sr0.7Bi0.2)TiO3The barium titanate-based relaxor ferroelectric ceramic material.
Example 3
A compound of formula 0.65 (Ba) was prepared0.985La0.03)Ti0.985O3-0.35(Sr0.7Bi0.2)TiO3The barium titanate-based relaxor ferroelectric ceramic material with high energy storage density and high power density under high electric field comprises the following specific steps:
(1) weighing raw material TiO with the purity of more than 99 percent according to the molar ratio of 3961:2561:980:1400:392、BaCO3、SrCO3、Bi2O3、La2O3Bi2O3、SrCO3And TiO2Mixing the weighed raw materials, putting the mixture into a ball milling tank, and simultaneously adding a ball milling solvent, namely absolute ethyl alcohol (absolute ethyl alcohol and absolute ethyl alcohol)The volume ratio of the total volume of the added raw materials is 2:1) and zirconia balls (the volume ratio of the zirconia balls to the total volume of the added raw materials is 3:2, wherein the zirconia balls comprise zirconia balls with the diameter of 10mm and the diameter of 5mm according to the number ratio of 1: 2), ball-milling is carried out at the ball-milling speed of 330r/min for 24 hours, and then the ball-milled zirconia balls are placed in an oven at 70 ℃ for drying to obtain a mixture;
(2) putting the mixture obtained in the step (1) into a mortar for grinding and briquetting, presintering in a muffle furnace at 1000 ℃, preserving heat for 1 hour, naturally cooling to room temperature, and discharging; the same ball milling was performed again (the ball milling process was the same as in the step (1)), yielding 0.65 (Ba)0.985La0.03)Ti0.985O3-0.35(Sr0.7Bi0.2)TiO3；
(3) Drying the product obtained in the step (2), grinding and sieving the product in a mortar, adding a polyvinyl alcohol (PVA) solution with the mass percent of 10% (wherein the standard of adding PVA is that 0.65 (Ba) is added per 1g0.985La0.03)Ti0.985O3-0.35(Sr0.7Bi0.2)TiO3Adding 1 drop of PVA solution into the powder), uniformly mixing, and taking the powder after being screened by a 60-mesh sieve;
(4) standing the powder obtained by the treatment in the step (3) for 36 hours, putting the powder into a stainless steel mold with the diameter of 20mm, performing pre-pressing molding under the pressure of 8MPa by using a single-shaft tablet press, performing vacuum packaging on the pre-pressed cylindrical blank, and pressing the cylindrical blank into a cylindrical blank under the pressure of 120MPa by using a hydraulic press;
(5) putting the cylindrical blank in the step (4) into a muffle furnace, heating to 600 ℃, preserving heat for 4 hours, and removing organic matters to obtain a de-gummed blank;
(6) placing the blank subjected to the rubber removal in the step (5) into a crucible with a cover, and using the same powder (0.65 (Ba)0.985La0.03)Ti0.985O3-0.35(Sr0.7Bi0.2)TiO3And polyvinyl alcohol, wherein the volume of the polyvinyl alcohol is equal to 0.65 (Ba)0.985La0.03)Ti0.985 O3-0.35(Sr0.7Bi0.2)TiO3In a volume ratio of 1:1) as a buried material, and firing at 1200 DEG CPerforming heat preservation for 2 hours, and naturally cooling to room temperature along with the furnace to obtain a ceramic wafer;
(7) polishing the ceramic wafer sintered in the step (6) to the thickness of 0.18mm, drying at 70 ℃, coating silver paste on the upper surface and the lower surface of the ceramic wafer, placing the ceramic wafer in a furnace, heating to 800 ℃, preserving heat for 15min, and naturally cooling to room temperature to obtain the ceramic wafer with the chemical formula of 0.65 (Ba) and high energy density and high power density under a high electric field0.985La0.03)Ti0.985O3-0.35(Sr0.7Bi0.2)TiO3The barium titanate-based relaxor ferroelectric ceramic material.
And (3) performance testing:
the underdamped discharge curve and the room temperature hysteresis loop of the material prepared in example 1 were respectively tested, and then the energy storage density and the energy storage efficiency were calculated from the hysteresis loop, and the current peak value, the current density and the power density were calculated from the underdamped discharge curve.
0.65 (Ba) prepared in example 10.985La0.03)Ti0.985O3-0.35(Sr0.7Bi0.2)TiO3The room temperature hysteresis loop of the material at different electric field strengths is shown in fig. 1. As can be seen from FIG. 1, the hysteresis loop is slender, and shows obvious characteristics of a relaxor ferroelectric, and the electric field strength can reach 280 kV/cm. Under the electric field, the maximum polarization is 22.72 mu C/cm2The residual polarization is 2.33 mu C/cm2。
0.65 (Ba) prepared in example 10.985La0.03)Ti0.985O3-0.35(Sr0.7Bi0.2)TiO3The changes of the total energy storage density, the effective energy storage density and the energy storage efficiency of the material at room temperature along with the electric field intensity are shown in figure 2. As can be seen from FIG. 2, the total energy storage density and the effective energy storage density increase with the increase of the electric field, and reach the maximum in the 280kV/cm electric field, which is 2.91J/cm respectively3And 2.23J/cm3. Under the electric field of not higher than 280kV/cm, the energy storage efficiency is always kept above 75%.
0.65 (Ba) prepared in example 10.98Li0.04)Ti0.98O3-0.35(Sr0.7Bi0.2)TiO3The underdamped discharge curve of the material is shown in fig. 3, 0.65 (Ba) prepared in example 10.98Li0.04)Ti0.98O3-0.35(Sr0.7Bi0.2)TiO3Peak current (I) of material at room temperaturemax) Current density (C)D) And power density (P)D) The variation with electric field is shown in fig. 4. As can be seen from FIG. 4, the current becomes 0 after 4 attenuations, and under the electric field of 150kV/cm, the current peak value of one underdamping process is 40.6A, and the current density is 574.66A/cm2The power density is 43.10MW/cm3。
The same tests show that the chemical formula of the high energy storage density resistant to high electric field prepared in example 2 and example 3 is 0.65 (Ba)0.985La0.03)Ti0.985O3-0.35(Sr0.7Bi0.2)TiO3The barium titanate-based relaxor ferroelectric ceramic material of (a) has similar properties to the material prepared in example 1. The above test results show that the chemical formula of the material prepared by the preparation method of the present invention is 0.65 (Ba)0.985La0.03)Ti0.985O3-0.35(Sr0.7Bi0.2)TiO3Can resist high electric field and has high energy storage density at room temperature; and the high-energy storage density barium titanate-based relaxor ferroelectric ceramic material with high electric field strength has a total energy storage density of 2.91J/cm at room temperature under an electric field of 280kV/cm3The effective energy storage density is 2.23J/cm3(ii) a Energy storage efficiency between 10-280 kV/cm electric field>75%, the reason for this is: 12 coordinated Sr2+And Bi3+All radii of (A) are less than Ba2+Less 12-coordinate La3+Radius of (D) and Ba2+Of small difference in radius of La3+、Sr2+And Bi3+After being introduced, the titanium occupies the A site of the perovskite structure, the air gap of the oxygen octahedron is reduced, and therefore Ti at the B site4+The displacement distance of the ions is shortened, resulting in a decrease in spontaneous polarization of the crystal, thereby inducing ferroelectric-relaxative phase transition. When an external electric field is applied, the spontaneous polarization of the material is weakened, space charges are not easy to accumulate at the grain boundary, and the material is broken along the grain boundaryCracking does not easily occur, and thus the electric field strength resistance is improved.
Finally, the above embodiments are only intended to illustrate the technical solutions of the present invention and not to limit the present invention, and although the present invention has been described in detail with reference to the preferred embodiments, it will be understood by those skilled in the art that modifications or equivalent substitutions may be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions, and all of them should be covered by the claims of the present invention.
Claims (10)
1. A barium titanate-based relaxor ferroelectric ceramic material having high energy storage density and high power density under high electric field, characterized in that the chemical formula of the barium titanate-based relaxor ferroelectric ceramic material is 0.65 (Ba)0.985La0.03)Ti0.985O3-0.35(Sr0.7Bi0.2)TiO3。
2. The method for preparing a barium titanate-based relaxor ferroelectric ceramic material according to claim 1, comprising the steps of:
(1) mixing TiO according to the molar ratio of 3961:2561:980:1400:392、BaCO3、SrCO3、Bi2O3And La2O3Ball milling is carried out after mixing, and the mixture is obtained after drying and grinding and sieving by a 60-mesh sieve;
(2) briquetting the mixture in the step (1), presintering at 900-1000 ℃, preserving heat for 1-2 h, cooling to room temperature, and ball-milling again to obtain 0.65 (Ba)0.985La0.03)Ti0.985O3-0.35(Sr0.7Bi0.2)TiO3；
(3) Drying and grinding the material prepared in the step (2) to obtain powder, adding 1 drop of polyvinyl alcohol aqueous solution with the mass fraction of 8-10% into each gram of powder, uniformly mixing, and taking the powder after being sieved by a 60-mesh sieve;
(4) standing the powder obtained by the treatment in the step (3), pressing the powder into a cylindrical blank, and then calcining and discharging the gel to form a blank body;
(5) sintering the blank after the glue is removed in the step (4) at 1180-1200 ℃, and cooling to room temperature to obtain a ceramic wafer;
(6) and (3) sequentially polishing, polishing and drying the ceramic wafer obtained in the step (5), respectively coating silver paste on the upper surface and the lower surface of the ceramic wafer, heating to 600-800 ℃, then carrying out heat preservation treatment for 10-15 min, and cooling to room temperature to obtain the barium titanate-based relaxor ferroelectric ceramic material with high energy storage density and high power density under a high electric field.
3. The preparation method of claim 2, wherein absolute ethyl alcohol and zirconia balls are added during ball milling in the step (1), the ball milling time is not less than 24 hours, and the rotation speed during ball milling is 270-330 r/min.
4. The preparation method according to claim 2, wherein the standing time in the step (4) is 24-36 h.
5. The manufacturing method according to claim 2, wherein the specific method of pressing into the cylindrical blank member in the step (4) is: and (3) putting the standing powder into a stainless steel die with the diameter of 10-20 mm, pre-pressing and molding by using a single-shaft tablet press under the pressure of 4-8 MPa, and pressing the pre-pressed cylindrical blank under the pressure of 30-120 MPa by using a hydraulic press after vacuum packaging.
6. The preparation method according to claim 2, wherein the specific method for calcining and removing the binder in the step (4) is to place the cylindrical blank in a muffle furnace, heat the cylindrical blank to 600 ℃, and then keep the cylindrical blank at the temperature for 2-4 hours.
7. The preparation method according to claim 2, wherein the crucible with a cover is used as a container during the sintering in the step (5), and the same kind of powder is used as a filling material; the time of the sintering treatment is 2 h.
8. According to claim 7The process for preparing the same is characterized in that the powder of the same kind is 0.65 (Ba) in the step (3) of claim 20.985La0.03)Ti0.985O3-0.35(Sr0.7Bi0.2)TiO3And polyvinyl alcohol.
9. The preparation method according to claim 2, wherein the thickness of the ceramic sheet formed after the grinding and polishing in the step (6) is 0.15-0.2 mm.
10. The method according to claim 2, wherein the TiO in the step (1)2、BaCO3、SrCO3、Bi2O3And La2O3The purity of (A) is not less than 99%.
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| CN114292104A (en) * | 2021-12-28 | 2022-04-08 | 摩比天线技术（深圳）有限公司 | Energy storage ceramic material for pulse capacitor and preparation method thereof |
| CN114433067A (en) * | 2022-01-11 | 2022-05-06 | 陕西科技大学 | Photocatalyst with high built-in electric field and preparation method thereof |
| CN114573338A (en) * | 2022-02-25 | 2022-06-03 | 东莞市普隆电子有限公司 | Preparation method and application of high-energy-storage-density dielectric ceramic |
| CN114671681A (en) * | 2022-04-11 | 2022-06-28 | 北京科技大学 | Barium titanate-based relaxor ferroelectric ceramic material with high energy storage density, high power density and high efficiency and preparation method thereof |
| CN115108826A (en) * | 2022-07-28 | 2022-09-27 | 哈尔滨工业大学 | Relaxor ferroelectric ceramic material with low electric field driving, high energy storage density and ultra-fast discharge rate and preparation method thereof |
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| CN114292104A (en) * | 2021-12-28 | 2022-04-08 | 摩比天线技术（深圳）有限公司 | Energy storage ceramic material for pulse capacitor and preparation method thereof |
| CN114433067A (en) * | 2022-01-11 | 2022-05-06 | 陕西科技大学 | Photocatalyst with high built-in electric field and preparation method thereof |
| CN114433067B (en) * | 2022-01-11 | 2023-07-25 | 陕西科技大学 | Photocatalyst with high built-in electric field and preparation method thereof |
| CN114573338A (en) * | 2022-02-25 | 2022-06-03 | 东莞市普隆电子有限公司 | Preparation method and application of high-energy-storage-density dielectric ceramic |
| CN114573338B (en) * | 2022-02-25 | 2023-12-26 | 东莞市普隆电子有限公司 | Preparation method and application of dielectric ceramic with high energy storage density |
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| CN115108826A (en) * | 2022-07-28 | 2022-09-27 | 哈尔滨工业大学 | Relaxor ferroelectric ceramic material with low electric field driving, high energy storage density and ultra-fast discharge rate and preparation method thereof |
| CN115108826B (en) * | 2022-07-28 | 2023-06-06 | 哈尔滨工业大学 | Relaxation ferroelectric ceramic material with low electric field driving high energy storage density and ultrafast discharge rate and preparation method thereof |
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