CN119822816B - A high-entropy superparaelectric BNT-KNN-SST ceramic material and its preparation method - Google Patents
A high-entropy superparaelectric BNT-KNN-SST ceramic material and its preparation methodInfo
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Abstract
本发明提供一种高熵超顺电BNT‑KNN‑SST陶瓷材料及其制备方法。所述陶瓷材料的化学组成通式为：(1‑x‑y)Bi0.5Na0.5TiO3‑xK0.5Na0.5NbO3‑ySr(Sc0.5Ta0.5)O3；其中，所述x、y为摩尔百分比，0.2≤x≤0.3、0≤y≤0.25。本发明所提供的技术方案通过多相共存协同调控、高熵工程设计、超顺电态调控和缺陷补偿等多重策略共同提高了陶瓷材料的综合性能指标。制备得到的BNT‑KNN‑SST基无铅储能陶瓷在中等电场下，储能密度可以达到8.0J/cm3以上，储能效率超过91％，最高可达到95.5％。另外，该材料还表现出极佳的高温稳定性(20‑240℃)和疲劳性能(＞106)。通过本发明所提供的BNT‑KNN‑SST基无铅储能陶瓷，首次在中等电场下同时实现了高储能密度、高效率以及优异的高温与疲劳稳定性，在储能设备、功率电子等领域具有重要的商业化应用前景。
The present invention provides a high-entropy superparaelectric BNT-KNN-SST ceramic material and a preparation method thereof. The general chemical composition formula of the ceramic material is: (1-x-y)Bi 0.5 Na 0.5 TiO 3 ‑xK 0.5 Na 0.5 NbO 3 ‑ySr(Sc 0.5 Ta 0.5 )O 3 ; wherein, the x and y are molar percentages, 0.2≤x≤0.3, 0≤y≤0.25. The technical solution provided by the present invention improves the comprehensive performance indicators of ceramic materials through multiple strategies such as multi-phase coexistence and coordinated regulation, high-entropy engineering design, superparaelectric state regulation and defect compensation. The prepared BNT-KNN-SST-based lead-free energy storage ceramics can achieve an energy storage density of more than 8.0 J/cm 3 under a medium electric field, and the energy storage efficiency exceeds 91%, and can reach up to 95.5%. In addition, the material also exhibits excellent high-temperature stability (20-240°C) and fatigue performance (>10 6 ). The BNT-KNN-SST-based lead-free energy storage ceramics provided by the present invention have achieved high energy storage density, high efficiency, and excellent high-temperature and fatigue stability for the first time under moderate electric fields, and have important commercial application prospects in the fields of energy storage equipment, power electronics, etc.
Description
Technical Field
The invention belongs to the technical field of energy storage, and particularly relates to a high-entropy supercis BNT-KNN-SST ceramic material and a preparation method thereof.
Background
Ceramic capacitors are attracting attention in the fields of renewable energy sources, smart grids, high-performance energy storage devices, and the like, due to their rapid charge-discharge capability and high power density. However, the existing energy storage ceramic materials generally have the technical problems of insufficient energy storage density, low energy efficiency and poor high temperature and fatigue resistance.
Heretofore, relatively high energy storage densities of dielectric ceramics have been achieved almost exclusively at high breakdown strength (BDS) (> 500 kV/cm). However, when the capacitor is operated under a high electric field (more than 500 kV/cm), a voltage transformation system compatible with the dielectric ceramic is additionally added, and additional risks are also added to the insulation performance of the system, so that the cost of the system is increased, and the safety of the system is reduced. Therefore, the method has important practical significance in exploring dielectric ceramics with high energy storage density and high energy storage efficiency under the condition of medium electric field (lower than 500 kV/cm).
The energy storage efficiency refers to the ratio of the recoverable energy in the discharging process to the total energy stored in the charging process, and directly reflects the efficiency of the piezoelectric material in the electric energy and mechanical energy conversion process. High energy storage efficiency means less energy is lost during conversion, which is critical for energy storage and conversion applications. However, in the prior art, there are few effective schemes for not only considering comprehensive performance but also further improving energy storage efficiency under the medium electric field intensity. For example "Realization of superior thermal stability and high-power density in BNT-based ceramics with excellent energy storage performance" discloses the introduction of NaTaO 3 (NT) into 0.7bi0.5na 0.5TiO3-0.3Sr0.7La0.2TiO3 (BNSLT) ceramics to increase the content of highly stable P4bm phase and thereby increase the energy storage density and energy storage efficiency, but the highest energy storage efficiency of ceramic materials in the paper is still less than 90%. Moreover, the energy storage density is reduced from 89% to 78% in the cyclic charge and discharge test, and the fatigue stability is insufficient. The inability to further increase energy storage efficiency and fatigue stability severely limits the wide application of energy storage ceramics in the field of practical industry.
In addition, in some special applications, the capacitor needs to operate in a high temperature environment close to 200 ℃. To date, most of the reported energy storage ceramics have operating temperatures below 100-150 ℃, and thus it is seen that further improvement of the high temperature operating stability of dielectric energy storage ceramics is an urgent task.
In summary, exploring an energy storage ceramic material with high comprehensive energy storage performance, high temperature stability (200 ℃) and fatigue stability (the number of charge and discharge cycles exceeds 10 6 and the efficiency is always not lower than 90%) under the medium electric field intensity is a challenge, and is a technical problem to be solved by those skilled in the art. In view of this, the present invention has been made.
Disclosure of Invention
The invention aims to provide a high-entropy super-compliant electrical BNT-KNN-SST ceramic material. Aiming at the problems in the prior art, sr (Sc 0.5Ta0.5)O3 (SST)) is innovatively introduced into BNT-KNN-based ceramic, the comprehensive energy storage performance of the material is obviously improved through high-entropy engineering and super-cis-electric state regulation, and particularly, the high energy storage density, the high efficiency and the excellent high temperature and fatigue stability are realized under a medium electric field, so that the technical bottleneck of the existing energy storage ceramic system is broken through, and a brand new material solution is provided for commercial application of advanced energy storage equipment.
In order to achieve the purpose, the invention provides a high-entropy supercis electrical BNT-KNN-SST ceramic material, which has the specific chemical composition general formula:
(1-x-y)Bi0.5Na0.5TiO3-xK0.5Na0.5NbO3-ySr(Sc0.5Ta0.5)O3; Wherein, x and y are mole percentages, x is more than or equal to 0.2 and less than or equal to 0.3, and y is more than or equal to 0 and less than or equal to 0.25.
In a preferred embodiment of the present invention,
The energy storage density of 0.6Bi0.5Na0.5TiO3-0.2K0.5Na0.5NbO3-0.2Sr(Sc0.5Ta0.5)O3 under a medium electric field of 420kV/cm is more than 7J/cm 3, the energy storage efficiency eta is more than 95%, the temperature stability range is 20-240 ℃, and the fatigue resistance is more than 10 6.
In a preferred embodiment of the present invention,
The energy storage density of 0.55Bi0.5Na0.5TiO3-0.3K0.5Na0.5NbO3-0.15Sr(Sc0.5Ta0.5)O3 under a medium electric field of 500kV/cm is more than 8J/cm 3, the energy storage efficiency eta is more than 91%, the temperature stability range is 20-240 ℃, and the fatigue resistance is more than 10 6.
The invention further aims at providing a preparation method of the high-entropy super-compliant electrical BNT-KNN-SST ceramic material, which comprises the following steps:
s1, weighing Bi2O3、Na2CO3、TiO2、K2CO3、Nb2O5 and Sr 2CO3、Sc2O3、Ta2O5 according to a stoichiometric ratio;
s2, loading the weighed raw materials, ethanol and zirconia balls into a ball mill tank, and mixing and ball milling;
s3, separating out slurry after ball milling, and drying to constant weight to obtain dry powder;
S4, heating the dried powder to 750-850 ℃, preserving heat for 1-3 hours, cooling to room temperature, crushing and sieving to obtain presintered powder;
s5, adding 0.1-0.2wt% of manganese dioxide, ethanol and zirconia balls into the presintered powder, mixing, ball milling, separating out slurry after ball milling, drying to constant weight, granulating with a polyvinyl alcohol solution with the mass concentration of 4-6wt%, and filtering to obtain powder;
S6, pressing the filtered powder into ceramic green bodies, heating to 550-650 ℃ to discharge glue, heating to 1130-1180 ℃ at 3-7 ℃ per min after cold isostatic pressing, preserving heat for 1-3 hours, and cooling along with a furnace;
And S7, polishing the sample, coating high-temperature silver paste on both sides, and preserving heat to obtain the high-temperature silver paste.
In a preferred embodiment, step S1, after weighing all the raw materials, further comprises drying all the raw materials in an environment of 110-130 ℃ for 2-4 hours in order to remove moisture in the raw materials and avoid cracking during sintering.
In a preferred embodiment, in step S2, the mass ratio of the raw material, ethanol and zirconia balls is 1:1:2.
In a preferred embodiment, in the step S2, the ball milling speed is 200-600r/min, and the ball milling time is 6-18 hours.
In a preferred embodiment, in the step S4, the temperature rising rate is 3-7 ℃ per minute, preferably, the temperature rising rate is 5 ℃ per minute, the temperature is raised to 800 ℃, and the temperature is kept for 2 hours.
In a preferred embodiment, in step S5, the mass ratio of the pre-sintered powder, ethanol and zirconia balls is 1:1:2.
In a preferred embodiment, in the step S5, the ball milling speed is 200-600r/min, and the ball milling time is 6-18 hours.
In a preferred embodiment, in step S5, the granulation is performed using a polyvinyl alcohol solution having a mass concentration of 4 to 6wt% as a conventional method known to those skilled in the art, and the number of mesh screens used for the filtration is 100 mesh, which will not be described herein.
In a preferred embodiment, in step S6, the ceramic green body has a diameter of 8-12mm and a thickness of 0.5-1.5mm, and the pressing pressure is 150-250MPa.
In a preferred embodiment, in step S6, the temperature rising rate during the adhesive discharging treatment is 0.5-1.5 ℃ per minute.
In a preferred embodiment, in step S7, the incubation conditions include incubation at 500-700℃for 5-15 minutes.
Compared with the prior art, the technical scheme of the invention has the following advantages:
the BNT-KNN based energy storage ceramic material is innovatively designed and modified by combining high-entropy ion doping with super-cis-electricity engineering. The method specifically comprises the following steps:
By adopting a high entropy strategy of the synergy of the A bit and the B bit, and introducing Sr 2+ to the A bit and Sc 3+ and Ta 5+ to the B bit, the local chemical disorder and lattice distortion of the system are obviously improved, the local polarization distortion is further induced, and the multi-phase coexisting super-cis-electric state structure is optimized. At the same time, KNN is introduced to realize The three phases of the battery are in coexistence, the highest dielectric constant temperature (Tm) is reduced, a room temperature super-smooth state is constructed, and the energy storage performance and the stability are obviously improved. The high-entropy structure remarkably reduces dielectric loss of the material, enhances energy storage performance, remarkably improves polarization-depolarization reversibility by multiphase coexistence, and reduces polarization hysteresis loss, thereby remarkably improving energy storage efficiency. In addition, the inherent defect vacancies of the material are effectively compensated by using the aliovalent ions (Sr 2+、Sc3 + and Ta 5 +), so that the fatigue resistance and the long-term stability are obviously improved.
The BNT-KNN-SST-based leadless energy storage ceramic prepared according to the formula and the preparation method can achieve the energy storage density of more than 8.0J/cm 3 under a medium electric field, and the energy storage efficiency is more than 91 percent and can reach 95.5 percent at most. Moreover, the material not only has excellent energy storage performance, but also has excellent high-temperature stability (20-240 ℃) and fatigue performance (> 10 6), and the comprehensive performance of the existing energy storage ceramic material under a medium electric field (300-500 kV/cm) is far better than that of the existing energy storage ceramic material.
Therefore, the technical scheme provided by the invention has important commercial application prospects in the fields of energy storage equipment, power electronics and the like.
Drawings
These and/or other aspects and advantages of the present invention will become more apparent and more readily appreciated from the following detailed description of the embodiments of the invention, taken in conjunction with the accompanying drawings, wherein:
FIG. 1 shows the single polarized P-E hysteresis loop and corresponding energy storage performance of the (0.8-x) BNT-0.2KNN-xSST ceramic prepared in example 1 of the present invention under E b;
FIG. 2 shows the fatigue resistance of the 0.6BNT-0.2KNN-0.2SST ceramic material prepared in example 1 of the present invention;
FIG. 3 shows the single polarized P-E hysteresis loop and corresponding energy storage performance of the (0.7-x) BNT-0.3KNN-xSST ceramic prepared in example 2 of the present invention under E b;
FIG. 4 shows the fatigue resistance of the 0.55BNT-0.3KNN-0.15SST ceramic material prepared in example 2 of the present invention;
FIG. 5 shows the high temperature stability of the 0.55BNT-0.3KNN-0.15SST ceramic material prepared in example 2 of the present invention;
FIG. 6 is a graph showing the comparison of dielectric temperature spectra of (0.7-x) BNT-0.3KNN-xSST ceramic material prepared in example 2 of the present invention at 10 kHz.
Detailed Description
For a better understanding of the present invention, those skilled in the art will now make further details with reference to the drawings and the detailed description, but it should be understood that the scope of the invention is not limited by the detailed description.
The embodiment of the invention solves the technical problems that the existing ceramic capacitor is difficult to simultaneously realize high energy storage density, high energy efficiency and high temperature and fatigue stability under the medium electric field intensity by providing the high-entropy super-compliant electrical BNT-KNN-SST ceramic material and the preparation method thereof.
The technical scheme of the invention jointly realizes the optimization of the material performance through the following strategies, thereby solving the problems.
1. Multiphase coexisting cooperative regulation and control, namely, BNT and KNN are combinedThe polarization response and thermal stability of the material are optimized.
2. High entropy engineering design, namely constructing high entropy components at A site and B site of a perovskite structure by introducing Sr (Sc 0.5Ta0.5)O3 (SST), and remarkably enhancing local polarization diversity and distribution of a Polar Nano Region (PNRs).
3. And the super-cis-electric state regulation is carried out by inducing the room-temperature super-cis-electric state, so that the polarization hysteresis loss of the material is reduced, and the energy storage efficiency is improved.
4. And the defect compensation and the fatigue resistance enhancement are realized by effectively compensating inherent defect vacancies of the material by using aliovalent ions (Sr 2+、Sc3 + and Ta 5 +), so that the fatigue resistance and the long-term stability are obviously improved.
Through the successful application of the strategy, the BNT-KNN-SST ceramic material prepared by the method can simultaneously realize excellent comprehensive performance, excellent high-temperature stability and excellent fatigue resistance .0.6Bi0.5Na0.5TiO3-0.2K0.5Na0.5NbO3-0.2Sr(Sc0.5Ta0.5)O3 ceramic under a medium electric field of 420kV/cm, high energy storage density (Wrec >7J/cm 3) and high energy efficiency (η>95％);0.55Bi0.5Na0.5TiO3-0.3K0.5Na0.5NbO3-0.15Sr(Sc0.5Ta0.5)O3 ceramic under a medium electric field of 500kV/cm, and Wrec >8J/cm 3 and eta >91%. Moreover, the energy storage performance of the two ceramic materials is kept stable within the range of 20-240 ℃. After being subjected to an electric field cycle exceeding 10 6, the energy storage density and the efficiency of the material are not remarkably attenuated, and extremely strong fatigue resistance is shown.
The following describes the technical scheme of the application in detail through specific embodiments:
Unless otherwise indicated, the technical means used in the present invention are conventional means well known to those skilled in the art, and various raw materials, reagents, instruments, equipment, etc. used in the present invention are commercially available or can be prepared by existing methods. The reagents used in the invention are analytically pure unless otherwise specified.
Example 1
The preparation method of the high-entropy super-cis-electricity BNT-KNN-SST ceramic material comprises the following steps:
1. Raw materials are weighed, namely 6.051gBi2O3、1.835gNa2CO3、4.149gTiO2、0.598gK2CO3、2.301gNb2O5 g, 2.556g and Sr 2CO3、0.597gSc2O3、1.913gTa2O5 are weighed according to the design of stoichiometric ratio. All raw materials were previously dried at 120 ℃ for 3 hours.
2. And (3) mixing and ball milling, namely loading all the weighed raw materials, ethanol and zirconia balls into a ball milling tank according to the mass ratio of 1:1:2, and ball milling for 12 hours by a planetary ball mill at 400 r/min.
3. And (3) powder drying, namely separating ball materials from the ball-milled slurry, and drying to constant weight.
4. Presintering, namely placing the dried powder into an alumina crucible, heating to 800 ℃ in a muffle furnace at a temperature rising rate of 5 ℃ per min, preserving heat for 2 hours, and cooling to room temperature.
5. And (3) performing secondary ball milling and granulating, namely adding 0.15wt% of manganese dioxide into the presintered powder, repeating the ball milling process of the step (2), granulating by using 5wt% of polyvinyl alcohol solution after drying, and filtering by using a 100-mesh screen.
6. Tabletting and shaping, namely pressing the granulated powder into ceramic green bodies with the diameter of 10mm and the thickness of 1mm under 200 MPa.
7. Sintering, namely heating the green body to 600 ℃ at 1 ℃ per minute, discharging glue, cold isostatic pressing (150 MPA for 2 minutes), then embedding the green body into ceramic powder with the same component, heating to 1160 ℃ at 5 ℃ per minute, preserving heat for 2 hours, and cooling along with a furnace.
8. Polishing and electrode coating, namely polishing a sample, adopting screen printing to coat high-temperature silver paste on both sides, and preserving heat for 10 minutes at 600 ℃. The BNT-KNN-SST-based lead-free energy storage ceramic with the general formula 0.6Bi0.5Na0.5TiO3-0.2K0.5Na0.5NbO3-0.2Sr(Sc0.5Ta0.5)O3 can be obtained.
The performance of the ceramic material obtained by the preparation method is tested, the result is that the energy storage density of ：0.6Bi0.5Na0.5TiO3-0.2K0.5Na0.5NbO3-0.2Sr(Sc0.5Ta0.5)O3 under the electric field of 420kV/cm is 7.02J/cm 3, the energy storage efficiency is 95.5% (see figure 1), and the temperature stability range is 20-240 ℃. In the fatigue stability test, the test result is shown in fig. 2, and it can be seen from the graph that the energy storage efficiency of the prepared 0.6BNT-0.2KNN-0.2SST ceramic material after up to 10 6 cycles is always over 90%.
Example 2
Compared with the embodiment 1, the high-entropy super-cis-electric BNT-KNN-SST ceramic material is different in the following components:
0.55Bi0.5Na0.5TiO3-0.3K0.5Na0.5NbO3-0.15Sr(Sc0.5Ta0.5)O3, And the sintering temperature is raised to 1150 ℃ at 5 ℃ per minute. The rest of the preparation process is exactly the same as in example 1.
The performance of the ceramic material obtained by the preparation method is tested, and the result is that the energy storage density of ：0.55Bi0.5Na0.5TiO3-0.3K0.5Na0.5NbO3-0.15Sr(Sc0.5Ta0.5)O3 under the electric field of 500kV/cm is 8.15J/cm 3, and the energy storage efficiency is 91.3% (see figure 3). In the fatigue stability test, the test result is shown in fig. 4, and it can be seen from the graph that the energy storage efficiency of the prepared 0.55BNT-0.3KNN-0.15SST ceramic material always exceeds 93% after up to 10 6 cycles, and no decline trend still exists. In the temperature stability test, the test results are shown in FIG. 5, and the temperature stability range is 20-240 ℃. As can be seen from fig. 6, tm of the 0.55BNT-0.3KNN-0.15SST ceramic material is reduced to room temperature (< 25 ℃), that is, a super-homeotropic state at room temperature is realized, and successful construction of the room temperature super-homeotropic state is a main reason for significantly improving energy storage performance and stability.
The foregoing descriptions of specific exemplary embodiments of the present invention are presented for purposes of illustration and description. It is not intended to limit the invention to the precise form disclosed, and obviously many modifications and variations are possible in light of the above teaching. The exemplary embodiments were chosen and described in order to explain the specific principles of the invention and its practical application to thereby enable one skilled in the art to make and utilize the invention in various exemplary embodiments and with various modifications as are suited to the particular use contemplated. It is intended that the scope of the invention be defined by the claims and their equivalents.
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| CN102234195A (en) * | 2010-04-23 | 2011-11-09 | 四川师范大学 | Potassium-sodium niobate and sodium lithium bismuth titanate-system lead-free piezoelectric ceramic composition |
| CN111170735A (en) * | 2020-01-14 | 2020-05-19 | 西安工业大学 | A kind of ceramic material with high electrical energy storage efficiency and preparation method thereof |
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| JP6327914B2 (en) * | 2014-04-11 | 2018-05-23 | 日本特殊陶業株式会社 | Lead-free piezoelectric ceramic composition, piezoelectric element using the same, and lead-free piezoelectric ceramic composition manufacturing method |
| CN117383930B (en) * | 2023-10-31 | 2025-11-07 | 陕西师范大学 | Bismuth sodium titanate-based lead-free energy storage ceramic material with high ferroelectric stability and temperature stability and preparation method thereof |
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