CN114591080A - Preparation method and application of dielectric ceramic material with high energy storage density - Google Patents
Preparation method and application of dielectric ceramic material with high energy storage density Download PDFInfo
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- 238000004146 energy storage Methods 0.000 title claims abstract description 21
- 229910010293 ceramic material Inorganic materials 0.000 title claims abstract description 17
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 238000000034 method Methods 0.000 claims abstract description 17
- 229910002902 BiFeO3 Inorganic materials 0.000 claims abstract description 15
- 238000000498 ball milling Methods 0.000 claims abstract description 15
- 238000001035 drying Methods 0.000 claims abstract description 13
- 239000000843 powder Substances 0.000 claims abstract description 12
- 229910002971 CaTiO3 Inorganic materials 0.000 claims abstract description 10
- 239000000919 ceramic Substances 0.000 claims abstract description 10
- 238000003825 pressing Methods 0.000 claims abstract description 10
- 230000008569 process Effects 0.000 claims abstract description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229910003237 Na0.5Bi0.5TiO3 Inorganic materials 0.000 claims abstract description 6
- 239000008187 granular material Substances 0.000 claims abstract description 5
- 238000005469 granulation Methods 0.000 claims abstract description 4
- 230000003179 granulation Effects 0.000 claims abstract description 4
- 238000002156 mixing Methods 0.000 claims abstract description 4
- 239000000203 mixture Substances 0.000 claims abstract description 3
- 239000002994 raw material Substances 0.000 claims abstract description 3
- 238000007873 sieving Methods 0.000 claims abstract description 3
- 238000005245 sintering Methods 0.000 claims description 7
- 239000003292 glue Substances 0.000 claims description 4
- 239000000463 material Substances 0.000 claims description 4
- 238000007599 discharging Methods 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 2
- 238000010438 heat treatment Methods 0.000 claims description 2
- 238000004321 preservation Methods 0.000 claims description 2
- 239000003989 dielectric material Substances 0.000 abstract description 4
- 239000008188 pellet Substances 0.000 abstract 1
- 239000006185 dispersion Substances 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 2
- 230000015556 catabolic process Effects 0.000 description 2
- 238000009792 diffusion process Methods 0.000 description 2
- 230000010287 polarization Effects 0.000 description 2
- 238000000634 powder X-ray diffraction Methods 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 238000001757 thermogravimetry curve Methods 0.000 description 2
- 230000007704 transition Effects 0.000 description 2
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 238000004626 scanning electron microscopy Methods 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
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- 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
- C04B35/46—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
- C04B35/475—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 bismuth titanates
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3231—Refractory metal oxides, their mixed metal oxides, or oxide-forming salts thereof
- C04B2235/3232—Titanium oxides or titanates, e.g. rutile or anatase
- C04B2235/3234—Titanates, not containing zirconia
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Abstract
The invention discloses a preparation method and application of a dielectric ceramic material with high energy storage density, which comprises the following steps: s1: mixing Na0.5Bi0.5TiO3、BiFeO3And CaTiO3Preparing according to a proportion, and then carrying out ball milling uniformly in an absolute ethyl alcohol atmosphere; s2: will S1The powder in the step (a) is placed in a drying box for drying; s3: will S2Pressing the raw materials into a cylinder with a certain size, placing the cylinder in a crucible, and then pre-burning the cylinder in a muffle furnace; s4: will S3Crushing the pre-sintered sample into powder, and performing secondary ball milling, and the step is S1Similarly, after ball milling is carried out uniformly, drying the mixture; s5: will S4Adding a proper amount of PVA into the dried powder for granulation, sieving with a 400-mesh sieve, and taking the granular material with a uniform lower layer; s6: will S5The pellets obtained in (1)Pressing into a green sheet (diameter of about 10mm, thickness of 1 mm). The invention provides CaTiO3Doping with Na0.5Bi0.5TiO3‑BiFeO3A preparation method and application of ceramics belong to the field of dielectric materials, and provide a preparation method with low cost and simple process.
Description
Technical Field
The invention relates to the technical field of dielectric materials, in particular to a preparation method and application of a dielectric ceramic material with high energy storage density.
Background
The dielectric ceramic has the advantages of rapid charge and discharge, safety, easy miniaturization, adaptability to severe environment work and the like, and can be widely applied to the fields of pulse power technology, radar and the like. However, in practical applications, the dielectric ceramic contains lead element, which not only causes environmental pollution, but also damages human health. Therefore, it is important to find an environment-friendly lead-free dielectric ceramic material, but the low energy storage density is the biggest problem faced by the lead-free ceramic material at present. Among many nonlinear dielectric materials, a relaxor ferroelectric easily obtains excellent energy storage performance due to its large saturation polarization, small remanent polarization, and appropriate breakdown strength.
Thus, the present patent investigated CaTiO compounds having a paraelectric structure at room temperature3Doping with Na0.5Bi0.5TiO3-BiFeO3The ceramic also achieves excellent energy storage performance.
Disclosure of Invention
In order to make up for the disadvantages and shortcomings of the prior art, one of the objects of the present invention is to use CaTiO3With Na0.5Bi0.5TiO3-BiFeO3Successfully solid-dissolved together; the second purpose is to provide a preparation method with low cost and simple process; the third objective is to provide a dielectric ceramic material which has environmental protection and can obtain high energy storage density under high breakdown electric field.
The purpose of the invention is realized by the following technical scheme:
a preparation method and application of a dielectric ceramic material with high energy storage density comprise the following steps:
S1: mixing Na0.5Bi0.5TiO3、BiFeO3And CaTiO3Preparing according to a proportion, and then carrying out ball milling uniformly in an absolute ethyl alcohol atmosphere;
S2: will S1The powder in the step (a) is placed in a drying box for drying;
S3: will S2Pressing the raw materials into a cylinder with a certain size, placing the cylinder in a crucible, and then pre-burning the cylinder in a muffle furnace;
S4: will S3Crushing the pre-sintered sample into powder, and performing secondary ball milling, the step is S1Similarly, after ball milling is carried out uniformly, drying the mixture;
S5: will S4Adding a proper amount of PVA into the dried powder for granulation, sieving with a 400-mesh sieve, and taking the granular material with a uniform lower layer;
S6: will S5Pressing the obtained granules into green sheets (the diameter is about 10mm and the thickness is 1mm), placing the green sheets in a muffle furnace for removing glue, sintering, and finally cooling to room temperature along with the furnace to obtain samples.
Preferably, said S1In, Na0.5Bi0.5TiO3And BiFeO3In a ratio of 49: 1, NBT-BFO and CaTiO3The preparation proportion is 17: 3; the ratio of the material to the absolute ethyl alcohol to the balls is 1: 2: 1; the ball milling time was 30 hours.
Preferably, said S2The drying conditions were 70 ℃.
Preferably, said S3And the pre-sintering temperature is 850 ℃, the heating rate is 4 ℃/min, and the heat preservation time is 2 hours.
Preferably, said S4The ratio of the material, the absolute ethyl alcohol and the balls is 1: 2: 1; the ball milling time was 30 hours and the drying temperature was 70 ℃.
Preferably, said S5The amount of PVA used was about 60 drops per 20g of powder.
Preferably, said S6In the pressing process, 8MPa pressure is used for pressing the green sheet, the temperature is kept for 2 hours after the glue discharging process is carried out and the temperature is increased to 600 ℃ at the speed of 2 ℃/min, and the temperature is kept for 2 hours after the sintering process is carried out and the temperature is increased to 1110 ℃ at the speed of 4 ℃/min.
Preferably, the CaTiO prepared by the method3Doping with Na0.5Bi0.5TiO3-BiFeO3A ceramic.
Preferably, the CaTiO3Doping with Na0.5Bi0.5TiO3-BiFeO3The ceramic is applied to the fields of pulse, radar and the like which need to be charged and discharged quickly.
Compared with the prior art, the invention provides a preparation method and application of a dielectric ceramic material with high energy storage density, and the dielectric ceramic material has the following beneficial effects:
the invention provides CaTiO3Doping with Na0.5Bi0.5TiO3-BiFeO3A preparation method and application of ceramics belong to the field of dielectric materials, and provide a preparation method with low cost and simple process. The CaTiO provided by the invention3Doping with Na0.5Bi0.5TiO3-BiFeO3The ceramic is in a three-side phase structure at room temperature, all samples have compact microstructures, the doped sample dielectric thermogram has frequency diffusion at room temperature, and the relaxor ferroelectric peak is shifted to be near the room temperature. In addition, doped CaTiO3The energy storage density of the sample reaches 1.15J/cm3。
Drawings
FIG. 1 is an X-ray powder diffractogram (XRD) of example 1(NBT-BFO), example 2 (NBT-BFO-CT);
FIG. 2 is a Scanning Electron Microscope (SEM) image of example 1 and example 2;
FIG. 3 is a dielectric thermogram of example 1 and example 2;
fig. 4 is hysteresis curves (P-E) of examples 1 and 2, and the energy storage densities thereof were calculated.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments.
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.
Example one
Preparation of 0.98Na0.5Bi0.5TiO3-0.02BiFeO3(NBT-BFO)
1) Mixing Na0.5Bi0.5TiO3And BiFeO3And (3) the ratio of 49: 1, preparing a sample by the steps of ball milling, presintering, secondary ball milling, granulation and tabletting, binder removal and sintering and the like;
2) covering the finished product obtained in the step 1) with a silver electrode, and carrying out electrical performance test.
In the examples, NBT-BFO was subjected to X-ray powder diffraction analysis, as shown in fig. 1, and exhibited a tripartite phase at room temperature; the NBT-BFO is subjected to a scanning electron microscope, and the sample is compact and has no obvious air holes as shown in figure 2 (a); performing a dielectric temperature spectrum test on the NBT-BFO, wherein the NBT-BFO has no frequency dispersion and dispersion phase transition at room temperature, and is a ferroelectric phase at room temperature, as shown in FIG. 3 (a); the NBT-BFO was subjected to a hysteresis loop test, and as shown in FIG. 4(a), the hysteresis loop exhibited a square shape and had a storage density of only 0.18J/cm3。
Example two
Preparation of 0.85(0.98 Na)0.5Bi0.5TiO3-0.02BiFeO3)-0.15CaTiO(NBT-BFO-CT)
1) NBT-BFO and CT were measured at 17: 3, the main preparation process is substantially the same as that of example 1.
In the examples, an X-ray powder diffraction analysis of NBT-BFO-CT was performed, which, as shown in fig. 1, appeared as a tripartite phase at room temperature, indicating successful solid dissolution of CT in NBT-BFO; scanning electron microscopy of NBT-BFO-CT as shown in FIG. 2(b), the microstructure is dense and pore-free; in the dielectric temperature spectrum test of NBT-BFO-CT, obvious frequency diffusion and dispersion phase transition occur, and the relaxor ferroelectric peak is shifted to room temperature, as shown in FIG. 3 (b); for NBT-BFO-CT test, the electrical hysteresis loop is shown in FIG. 4(b), compared with NBT-BFO, the shape becomes thin and the energy storage density is improved, and the energy storage density can reach 1.15J/cm3。
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (9)
1. A preparation method and application of a dielectric ceramic material with high energy storage density are characterized by comprising the following steps:
S1: mixing Na0.5Bi0.5TiO3、BiFeO3And CaTiO3Preparing according to a proportion, and then carrying out ball milling uniformly in an absolute ethyl alcohol atmosphere;
S2: will S1The powder in the step (a) is placed in a drying box for drying;
S3: will S2Pressing the raw materials into a cylinder with a certain size, placing the cylinder in a crucible, and then pre-burning the cylinder in a muffle furnace;
S4: will S3Crushing the pre-sintered sample into powder, and performing secondary ball milling, the step is S1Similarly, after ball milling is carried out uniformly, drying the mixture;
S5: will S4Adding a proper amount of PVA into the dried powder for granulation, sieving with a 400-mesh sieve, and taking the granular material with a uniform lower layer;
S6: will S5Pressing the obtained granules into green sheets (the diameter is about 10mm and the thickness is 1mm), placing the green sheets in a muffle furnace for removing glue, sintering, and finally cooling to room temperature along with the furnace to obtain samples.
2. The method for preparing a dielectric ceramic material with high energy storage density and the application thereof as claimed in claim 1, wherein S is1In, Na0.5Bi0.5TiO3And BiFeO3In a ratio of 49: 1, NBT-BFO and CaTiO3The preparation proportion is 17: 3; the ratio of the material to the absolute ethyl alcohol to the balls is 1:2: 1; the ball milling time was 30 hours.
3. The method for preparing a dielectric ceramic material with high energy storage density and the application thereof as claimed in claim 1, wherein S is2The drying conditions were 70 ℃.
4. The method for preparing a dielectric ceramic material with high energy storage density and the application thereof as claimed in claim 1, wherein S is3And the pre-sintering temperature is 850 ℃, the heating rate is 4 ℃/min, and the heat preservation time is 2 hours.
5. The method for preparing a dielectric ceramic material with high energy storage density and the application thereof as claimed in claim 1, wherein S is4The ratio of the material, the absolute ethyl alcohol and the balls is 1: 2: 1; the ball milling time was 30 hours and the drying temperature was 70 ℃.
6. The method for preparing a dielectric ceramic material with high energy storage density and the application thereof as claimed in claim 1, wherein S is5The amount of PVA used was about 60 drops per 20g of powder.
7. The method for preparing a dielectric ceramic material with high energy storage density as claimed in claim 1, wherein S is selected from the group consisting of6In the pressing process, 8MPa pressure is used for pressing the green sheet, the temperature is kept for 2 hours after the glue discharging process is carried out and the temperature is increased to 600 ℃ at the speed of 2 ℃/min, and the temperature is kept for 2 hours after the sintering process is carried out and the temperature is increased to 1110 ℃ at the speed of 4 ℃/min.
8. CaTiO prepared according to the process of any one of claims 1 to 73Doping with Na0.5Bi0.5TiO3-BiFeO3And (3) ceramic.
9. The CaTiO of claim 83Doping with Na0.5Bi0.5TiO3-BiFeO3Ceramic is applied to the required fast speedPulse for charging and discharging, radar, and the like.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115448716A (en) * | 2022-09-16 | 2022-12-09 | 桂林理工大学 | Barium titanate-based energy storage ceramic material and preparation method thereof |
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| US20210126187A1 (en) * | 2018-05-08 | 2021-04-29 | Xaar Technology Limited | Electrical element comprising a multilayer thin film ceramic member, an electrical component comprising the same, and uses thereof |
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| CN104045340A (en) * | 2014-06-04 | 2014-09-17 | 同济大学 | Sodium bismuth titanate base and barium titanate base multilayer composite piezoelectric film and making method thereof |
| US20210126187A1 (en) * | 2018-05-08 | 2021-04-29 | Xaar Technology Limited | Electrical element comprising a multilayer thin film ceramic member, an electrical component comprising the same, and uses thereof |
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| Title |
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| PENGRONG REN: ""Compositionally driven relaxor to ferroelectric crossover in (1 - x)Na0.5Bi0.5TiO3–xBiFeO3 (0≤x ≤0.60)"，Pengrong Ren，《Journal of Materials Chemistry C》，第8613-9621页", 《JOURNAL OF MATERIALS CHEMISTRY C》 * |
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| CN115448716A (en) * | 2022-09-16 | 2022-12-09 | 桂林理工大学 | Barium titanate-based energy storage ceramic material and preparation method thereof |
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