CN116102352B - Antiferroelectric energy storage ceramic with high fatigue resistance, low electric field and high energy storage density and preparation method and application thereof - Google Patents
Antiferroelectric energy storage ceramic with high fatigue resistance, low electric field and high energy storage density and preparation method and application thereof Download PDFInfo
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- 239000000919 ceramic Substances 0.000 title claims abstract description 100
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- 238000002360 preparation method Methods 0.000 title claims abstract description 26
- 239000011159 matrix material Substances 0.000 claims abstract description 26
- 238000000034 method Methods 0.000 claims abstract description 19
- 239000013078 crystal Substances 0.000 claims abstract description 9
- 229910052761 rare earth metal Inorganic materials 0.000 claims abstract description 6
- 239000000126 substance Substances 0.000 claims abstract description 3
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- 235000015895 biscuits Nutrition 0.000 claims description 11
- 238000000498 ball milling Methods 0.000 claims description 9
- 238000005245 sintering Methods 0.000 claims description 9
- 239000013081 microcrystal Substances 0.000 claims description 7
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 6
- 229910052737 gold Inorganic materials 0.000 claims description 6
- 239000010931 gold Substances 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 6
- 229910010413 TiO 2 Inorganic materials 0.000 claims description 4
- 238000005498 polishing Methods 0.000 claims description 4
- 229910001404 rare earth metal oxide Inorganic materials 0.000 claims description 4
- 229910015902 Bi 2 O 3 Inorganic materials 0.000 claims description 3
- 229910017493 Nd 2 O 3 Inorganic materials 0.000 claims description 3
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 3
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- -1 rare earth ion Chemical group 0.000 description 3
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Abstract
An antiferroelectric energy-storage ceramic with high fatigue resistance, low electric field and high energy-storage density, a preparation method and application thereof. The application belongs to the field of energy storage material preparation. The application aims to solve the technical problem that the existing energy storage ceramic material cannot achieve the energy storage characteristics of excellent temperature stability, fatigue resistance, low electric field and high energy storage density. The chemical general formula of the energy storage ceramic is xNaNbO 3 ‑(1‑x)(Bi 0.5‑y R y Na 0.5 )TiO 3 zMe where 0.1.ltoreq.x.ltoreq.1, 0.05.ltoreq.y.ltoreq.0.25, 0.ltoreq.z.ltoreq.0.1, R is a rare earth ion and Me is a growth promoter. The method comprises the following steps: NN-BRNT fine crystals are taken as a matrix, and the radial ratio is adopted>5, adopting a template grain oriented growth technology, under the action of growth auxiliary agent, preparing edge [001]]Antiferroelectric energy-storage ceramic with high fatigue resistance, low electric field and high energy storage density and preferred orientation.
Description
Technical Field
The application belongs to the field of energy storage material preparation, and particularly relates to antiferroelectric energy storage ceramic with high fatigue resistance, low electric field and high energy storage density, and a preparation method and application thereof.
Background
The dielectric ceramic has the characteristics of high power density, short charge and discharge time and the like, has great advantages in the fields of various electric power and electronic systems, and particularly has irreplaceable application in the technical field of high-energy pulse power. With the rapid updating and iteration of electronic devices and power systems, the relatively low energy storage density of ceramics cannot meet the demands of the power devices and products for integration, light weight and miniaturization, and the development of dielectric energy storage ceramics with excellent energy storage characteristics of new generation has become a necessary trend. The energy storage density calculation formula of the dielectric ceramic is as follows:
wherein W is rec For effective energy storage density, P max And P r The saturated polarization and the residual polarization are respectively, E is an electric field, and P is the polarization.
NaNbO 3 Is a typical relaxation antiferroelectric material, has the characteristics of wide band gap (large breakdown electric field), no volatile potassium element (easy preparation) and low volume density (light weight), and has great application potential in the energy storage field. However, naNbO 3 Having a near rectangular hysteresis loop, residual polarization P r Large, it is difficult to achieve excellent energy storage characteristics.
The biggest constraint in the development of the current dielectric energy storage ceramics is that the dielectric energy storage ceramics need extremely high electric field (650 kV/cm) to realize higher energy storage density (W) rec >3J/cm 3 ) The dielectric material has high breakdown strength requirements, and simultaneously, the capacitor insulation system has high insulation strength requirements, so that the current development trend of miniaturization and integration of components is difficult to conform. In addition, in practical application, the capacitor is often required to bear higher working temperature and complex working environment, so that the comprehensive performances such as temperature stability, fatigue resistance and the like of the dielectric energy storage ceramic material are also not negligible. In summary, in order to better promote the practical development of the capacitor, development of antiferroelectric ceramic materials having excellent temperature stability, fatigue resistance, low electric field and high energy storage density is urgently required.
Disclosure of Invention
The application aims to solve the technical problems that the existing energy storage ceramic material cannot meet the requirements of excellent temperature stability, fatigue resistance and energy storage characteristics of low electric field and high energy storage density, cannot adapt to complex and harsh working environments and the current development trend of miniaturization and integration of components, and provides antiferroelectric energy storage ceramic with high fatigue resistance, low electric field and high energy storage density, and a preparation method and application thereof.
One of the purposes of the application is to provide an antiferroelectric energy storage ceramic with high fatigue resistance, low electric field and high energy storage density, wherein the chemical formula of the antiferroelectric energy storage ceramic with high fatigue resistance, low electric field and high energy storage density is xNaNbO 3 -(1-x)(Bi 0.5-y R y Na 0.5 )TiO 3 zMe where 0.1.ltoreq.x.ltoreq.1, 0.05.ltoreq.y.ltoreq.0.25, 0.ltoreq.z.ltoreq.0.1, R is a rare earth ion and Me is a growth promoter.
Further defined, the rare earth ion is La 3+ 、Pr 3+ 、Nd 3+ Or Sm 3+ 。
Further defined, the growth promoter is CuO, li 2 CO 3 、MnO 2 One or a mixture of two of them in any ratio.
The second purpose of the application is to provide a preparation method of antiferroelectric energy storage ceramic with high fatigue resistance, low electric field and high energy storage density, wherein the method of antiferroelectric energy storage ceramic with high fatigue resistance, low electric field and high energy storage density is carried out according to the following steps:
by xNaNbO 3 -(1-x)(Bi 0.5-y R y Na 0.5 )TiO 3 (x is more than or equal to 0.1 and less than or equal to 1, y is more than or equal to 0.05 and less than or equal to 0.25) fine crystals as a matrix, and the radial ratio is adopted>5 NaNbO 3 Flaky microcrystal is used as a template, the template grain directional growth technology is adopted, and the crystal growth promoter is used for preparing the crystal growth promoter [001]]Antiferroelectric energy-storage ceramic with high fatigue resistance, low electric field and high energy storage density and preferred orientation.
Further defined, the fine-grained matrix is with NaNbO 3 The molar ratio of the flaky microcrystals is 100 (1-10).
Further defined, naNbO 3 Flake crystallite size<50 μm, grain edge [001]]The direction is preferentially oriented.
Further defined, the fine-grain matrix preparation process is as follows: according to xNaNbO 3 -(1-x)(Bi 0.5-y R y Na 0.5 )TiO 3 Stoichiometric ratio of x is more than or equal to 0.1 and less than or equal to 1, y is more than or equal to 0.05 and less than or equal to 0.25, and Na is weighed 2 CO 3 、Nb 2 O 5 、Bi 2 O 3 、TiO 2 And rare earth oxide, ball milling and mixing, presintering for 2-8 h at 650-900 ℃ to obtain NN-BRNT fine crystal matrix.
As a further limitation of the preparation of the fine-grained matrix according to the application, the rare earth oxide is La 2 O 3 、Pr 2 O 3 、Nd 2 O 3 、Sm 2 O 3 One of them.
As a further limitation of the preparation of the fine-grain matrix, the ball milling medium is absolute ethyl alcohol, and the ball milling time is 12-48 hours.
As a further limitation of the preparation of the fine-grained matrix according to the application, nb 2 O 5 、TiO 2 Particle diameter of powder<100nm。
As a further limitation of the preparation of the fine-grained matrix according to the application, the NN-BRNT fine-grained matrix has a particle size of <300nm.
Further limiting, the specific preparation method of the antiferroelectric energy storage ceramic with high fatigue resistance, low electric field and high energy storage density comprises the following steps:
step 1: fine-grain matrix, naNbO 3 Ball milling and mixing a flaky microcrystalline template, a growth aid, a solvent, a dispersing agent, an adhesive and a plasticizer, preparing a ceramic film by using a tape casting method, and sequentially performing lamination, hot water uniform pressure, cutting, glue discharging and cold isostatic pressing to obtain ceramic greenware with templates arranged in a fine crystal matrix in an oriented manner;
step 2: and wrapping the ceramic biscuit in Bai Jinpian, covering fine-grain matrixes on the upper surface and the lower surface of the ceramic biscuit, and sintering the ceramic biscuit at high temperature in an oxygen atmosphere to obtain the energy storage ceramic.
Further limited, the high temperature sintering temperature in the step 2 is 1000-1300 ℃ and the time is 1-15 h.
Further defined, the gas flow rate in step 2 is 0.1 to 2L/min.
The application further aims to provide an application of the antiferroelectric energy storage ceramic with high fatigue resistance, low electric field and high energy storage density in electronic devices.
The fourth object of the application is to provide an energy-storage ceramic electrode which is made of antiferroelectric energy-storage ceramic with high fatigue resistance, low electric field and high energy storage density.
The fifth purpose of the application is to provide a preparation method of an energy storage ceramic electrode, which comprises the following steps:
polishing the (001) surface of the energy-storage ceramic, sputtering a gold electrode on the upper surface and the lower surface of the energy-storage ceramic, uniformly coating silver paste on the surface of the gold electrode, and sintering the silver-permeation electrode at 650 ℃ for 30 minutes to obtain the energy-storage ceramic electrode.
Compared with the prior art, the application has the remarkable effects that:
the application is realized by the method that NaNbO 3 Is introduced into a new component (Bi) 0.5-y R y Na 0.5 ) Destroying the original ferroelectric long range order in the ceramic, and further at the A-site Bi 3+ The rare earth ion doping is introduced at the ion position to promote the formation of nano domains, so that the ceramic has a more slender electric hysteresis loop, the relaxation characteristic is enhanced, and meanwhile, the P is obviously reduced r The energy storage performance is optimized, a new feasible idea is provided for the design of the low-electric-field high-energy-storage ceramic material, and a reliable material is provided for the high-energy pulse power capacitor which needs to keep stability for a long time. The method has the specific advantages that:
(1) The application selects fine-grain matrix components as xNaNbO 3 -(1-x)(Bi 0.5-y R y Na 0.5 )TiO 3 Based on the synergistic effect of the component regulation strategy and the crystal orientation texture, the energy storage ceramic material with low electric field, high energy storage density and excellent temperature stability and fatigue resistance is prepared. Design of the introduction of perovskite New component (Bi 0.5-y R y Na 0.5 ) On one hand, the ceramic is guaranteed to be within a wide temperature range>200 ℃ has excellent energy storage property, on the other hand, a local random field is constructed, a ferroelectric domain with long-range order inside the ceramic is disturbed, a nano domain and a polar nano micro region are formed, the strain hysteresis generated by the inversion of the electric domain area along with an external electric field is greatly reduced, and an elongated electric hysteresis loop with low energy dissipation is realized.
(2) The application designs and regulates xNaNbO 3 -(1-x)(Bi 0.5-y R y Na 0.5 )TiO 3 The microstructure of the zMe energy storage ceramic allows the ceramic grains to preferentially orient in a dominant direction, resulting in a ceramic grain having a maximum polarization difference Δp (i.e., P max -P r ) The polarization difference delta P is about 2-3 times of that of the traditional unoriented ceramic, so that the effective energy storage density of the ceramic is greatly improved, and the accumulation of local stress in the overturning process can be slowed down by combining a nano domain and a polar nano micro-domain which are extremely easy to overturn along with an external electric field, the generation or the expansion and growth of microcracks are reduced, and the fatigue resistance of the ceramic is improved.
(3) xNaNbO prepared by the application 3 -(1-x)(Bi 0.5-y R y Na 0.5 )TiO 3 The zMe energy storage ceramic does not contain volatile potassium element and toxic lead element, has simple and stable process, is suitable for mass industrialized production, and can obviously reduce environmental pollution; at the same time, ceramic edge [001]]The degree of orientation of the direction is higher than 90%, in<Effective energy storage density W in low electric field of 250kV/cm rec Up to 5J/cm 3 The energy storage efficiency is higher than 80 percent, which is obviously better than the prior reported relaxation ferroelectric ceramic material (W rec <3J/cm 3 The electric field is 250-300 kV/cm).
(4) xNaNbO prepared by the application 3 -(1-x)(Bi 0.5-y R y Na 0.5 )TiO 3 zMe energy storage ceramics have excellent temperature stability and fatigue resistance, and the change rate of the effective energy storage density is less than 7% and the change rate of the energy storage efficiency is less than 2% in a wide temperature range up to 200 ℃; warp 10 6 After the number of circulation turns, the change rate of the effective energy storage density is less than 1%, and the change rate of the energy storage efficiency is less than 2%.
Drawings
FIG. 1 is an XRD pattern of antiferroelectric energy storage ceramic with high fatigue resistance, low electric field and high energy storage density obtained in the third step of example 1;
FIG. 2 is an SEM image of antiferroelectric energy-storage ceramic with high fatigue resistance, low electric field and high energy storage density obtained in the third step of example 1;
FIG. 3 is a graph showing the comparative hysteresis loop of the antiferroelectric energy storage ceramic electrode with high fatigue resistance, low electric field and high energy storage density prepared in example 1 and the conventional unoriented ceramic electrode of comparative example; (1) represents example 1, and (2) represents comparative example;
FIG. 4 is a graph showing the change of effective energy storage density with temperature of the antiferroelectric energy storage ceramic electrode with high fatigue resistance, low electric field and high energy storage density prepared in example 1;
fig. 5 is a graph showing the effective energy storage density and energy storage efficiency of the antiferroelectric energy storage ceramic electrode with high fatigue resistance, low electric field and high energy storage density prepared in example 1 after different cycles.
Detailed Description
The present application will be described in further detail with reference to the following examples in order to make the objects, technical solutions and advantages of the present application more apparent. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the scope of the application.
The experimental methods used in the following examples are conventional methods unless otherwise specified. The materials, reagents, methods and apparatus used, without any particular description, are those conventional in the art and are commercially available to those skilled in the art.
The terms "comprising," "including," "having," "containing," or any other variation thereof, as used in the following embodiments, are intended to cover a non-exclusive inclusion. For example, a composition, step, method, article, or apparatus that comprises a list of elements is not necessarily limited to only those elements but may include other elements not expressly listed or inherent to such composition, step, method, article, or apparatus.
When an equivalent, concentration, or other value or parameter is expressed as a range, preferred range, or a range bounded by a list of upper preferable values and lower preferable values, this is to be understood as specifically disclosing all ranges formed from any pair of any upper range limit or preferred value and any lower range limit or preferred value, regardless of whether ranges are separately disclosed. For example, when ranges of "1 to 5" are disclosed, the described ranges should be construed to include ranges of "1 to 4", "1 to 3", "1 to 2 and 4 to 5", "1 to 3 and 5", and the like. When a numerical range is described herein, unless otherwise indicated, the range is intended to include its endpoints and all integers and fractions within the range. In the description and claims of the application, the range limitations may be combined and/or interchanged, if not otherwise specified, including all the sub-ranges subsumed therein.
The indefinite articles "a" and "an" preceding an element or component of the application are not limited to the requirement (i.e. the number of occurrences) of the element or component. Thus, the use of "a" or "an" should be interpreted as including one or at least one, and the singular reference of an element or component includes the plural reference unless the amount clearly dictates otherwise.
Reference to "one embodiment" or "an embodiment" of the present application means that a particular feature, structure, or characteristic may be included in at least one implementation of the present application. The appearances of the phrase "in one embodiment" in various places in the specification are not necessarily all referring to the same embodiment, nor are separate or alternative embodiments mutually exclusive of other embodiments.
Example 1:
the preparation method of the antiferroelectric energy storage ceramic electrode with high fatigue resistance, low electric field and high energy storage density in the embodiment comprises the following steps:
the first step: preparation of xNaNbO 3 -(1-x)(Bi 0.5-y R y Na 0.5 )TiO 3 Fine-grained matrix
According to xNaNbO 3 -(1-x)(Bi 0.5-y R y Na 0.5 )TiO 3 (x＝0.76，y＝0.12，R＝Nd 3+ ) Stoichiometric ratio of fine-grain matrix to sheet-like microcrystal template Na 2 CO 3 、Nb 2 O 5 (particle size)<100nm)、Bi 2 O 3 、TiO 2 (particle size)<100 nm) and Nd 2 O 3 Absolute ethyl alcohol is used as a ball milling medium, ball milling and mixing are carried out for 24 hours, then drying is carried out, and the obtained dry powder is placed in a corundum crucible for presintering for 5 hours at 750 ℃ to obtain pure-phase particle size<300nAn NN-BRNT fine-grain matrix of m.
And a second step of: preparation of ceramic greenware with templates arranged in a highly directional manner in a fine-grained matrix
Select edge [001]NaNbO with preferential orientation direction 3 Flaky microcrystals (specific preparation process reference Advanced Powder Technology 2011,22,383-389;Ceramics International 2015,41,8377-8381) as templates (template size<50 μm radial ratio>5) 20g NN-BRNT fine-grain matrix, 0.9g NaNbO 3 Flaky microcrystal template and 0.02g of growth auxiliary MnO 2 10g of solvent (xylene-ethanol mixed solution with the mass ratio of 1:1), 0.5g of dispersing agent (herring oil), 1g of adhesive (polyvinyl butyral) and 1g of plasticizer (0.5 g of phthalate and 0.5g of polyethylene glycol), ball milling and mixing, preparing a ceramic film with the thickness of 70 mu m by using a tape casting method, and then sequentially laminating (the pressure of 20Mpa, the temperature of 80 ℃), hot water homogenizing (the pressure of 20Mpa, the temperature of 80 ℃), cutting, discharging glue (the temperature of 600 ℃ for 1 h) and cold isostatic pressing (the pressure of 200 Mpa) to obtain ceramic biscuit with templates arranged in a highly directional manner in a fine-grain matrix.
And a third step of: preparation of energy-storage ceramic along [001] preferred orientation
Wrapping the ceramic biscuit in Bai Jinpian, and covering the NN-BRNT fine-grain matrix prepared in the first step on the upper surface and the lower surface of the ceramic biscuit, wherein the mass ratio of the ceramic biscuit to the fine-grain matrix is 4:1, then placing the ceramic into a high temperature furnace, sintering in an oxygen atmosphere, wherein the gas flow rate is 0.2L/min, the sintering temperature is 1250 ℃, the heat preservation time is 4 hours, and in the sintering process, the template guides the matrix to grow directionally, so as to obtain NN-BRNT antiferroelectric energy storage ceramic with optimal orientation along [001], namely antiferroelectric energy storage ceramic with high fatigue resistance, low electric field and high energy storage density, and the degree of orientation of [001] is 95 percent according to XRD spectrum calculation.
Fourth step: preparation of energy storage ceramic electrode
Firstly, sequentially polishing and polishing the (001) surface of the energy storage ceramic by using alumina abrasive powder with the particle diameters of 40 mu m, 20 mu m, 10 mu m, 5 mu m and 1 mu m, and then ultrasonically cleaning and drying in absolute ethyl alcohol to ensure that the upper surface and the lower surface of a sample are smooth and flat; and then sputtering gold electrodes (thickness is 200 nm) on the upper and lower surfaces of the sample, uniformly coating silver paste on the surface sputtered with the gold electrodes, and heating the silver-infiltrated electrode at 650 ℃ for 30min to obtain the NN-BRNT antiferroelectric energy storage ceramic electrode with excellent temperature stability, fatigue resistance, low electric field and high energy storage density.
Comparative example
The difference between this comparative example and example 1 is that: omitting NaNbO in the second step 3 And finally obtaining the traditional unoriented energy storage ceramic electrode by using the flaky microcrystal template. Other steps and parameters were the same as in example 1.
Detection test
FIG. 1 is an XRD pattern of antiferroelectric energy storage ceramic with high fatigue resistance, low electric field and high energy storage density obtained in the third step of example 1. As can be seen from the graph, the ceramic prepared by the method has a perovskite structure, has no impurity phase, and has a calculated texture degree of 95%.
Fig. 2 is an SEM image of antiferroelectric energy storage ceramics with high fatigue resistance, low electric field and high energy storage density obtained in the third step of example 1.
Fig. 3 is a graph showing the hysteresis loop comparison of the antiferroelectric energy storage ceramic electrode with high fatigue resistance, low electric field and high energy storage density prepared in example 1 and the conventional unoriented ceramic electrode of comparative example. As can be seen from FIG. 3, the NN-BRNT antiferroelectric energy storage ceramic of the present application has an elongated hysteresis loop. Moreover, compared with the traditional energy storage ceramic polarization difference delta P of the comparative example, the energy storage ceramic of the application is improved by 2 times by comparison of the curves (1) and (2), and the effective energy storage density of the ceramic is greatly improved. Effective energy storage Density W of the energy storage ceramic of example 1 at a low electric field of 250kV/cm rec Up to 5J/cm 3 The energy storage efficiency is higher than 80%, and the traditional unoriented energy storage ceramic of the comparative example has effective energy storage density W under the low electric field of 250kV/cm rec 2.9J/cm 3 . It can be seen that the energy storage ceramic of the application is significantly better than the presently reported relaxor ferroelectric ceramic materials.
Fig. 4 is a graph showing the change of effective energy storage density with temperature of the antiferroelectric energy storage ceramic electrode with high fatigue resistance, low electric field and high energy storage density prepared in example 1. As can be seen from the graph, the effective energy storage density of the energy storage ceramic of example 1 varies less than 7% and the energy storage efficiency varies less than 2% over a wide temperature range up to 200 ℃.
Fig. 5 is a graph showing the effective energy storage density and energy storage efficiency of the antiferroelectric energy storage ceramic electrode with high fatigue resistance, low electric field and high energy storage density prepared in example 1 after different cycles. As can be seen from the figure, the energy storage ceramic warp 10 of example 1 6 After the number of circulation turns, the change rate of the effective energy storage density is less than 1%, and the change rate of the energy storage efficiency is less than 2%.
In the foregoing, the present application is merely preferred embodiments, which are based on different implementations of the overall concept of the application, and the protection scope of the application is not limited thereto, and any changes or substitutions easily come within the technical scope of the present application as those skilled in the art should not fall within the protection scope of the present application. Therefore, the protection scope of the present application should be subject to the protection scope of the claims.
Claims (6)
1. A preparation method of antiferroelectric energy storage ceramic with high fatigue resistance, low electric field and high energy storage density is characterized in that the antiferroelectric energy storage ceramic with high fatigue resistance, low electric field and high energy storage density has the chemical general formula ofxNaNbO 3 -(1-x)(Bi 0.5- y R y Na 0.5 )TiO 3 -zMe, wherein 0.76 is less than or equal tox＜1，0.05≤y≤0.25，0＜zLess than or equal to 0.1, R is rare earth ion, me is growth auxiliary agent, and rare earth ion is La 3+ 、Pr 3+ 、Nd 3+ Or Sm 3+ The growth auxiliary agent is CuO, li 2 CO 3 、MnO 2 One or two of the following components;
the preparation method comprises the following steps:
step 1: fine grain matrix, radial ratio>5 NaNbO 3 Ball milling and mixing a flaky microcrystalline template, a growth aid, a solvent, a dispersing agent, an adhesive and a plasticizer, preparing a ceramic film by using a tape casting method, and sequentially performing lamination, hot water uniform pressing, cutting, glue discharging and cold isostatic pressing to obtain the template in a fine crystalline matrixDirectionally arranged ceramic biscuit; fine-grain matrix and NaNbO 3 The molar ratio of the flaky microcrystals is 100:1-10, and NaNbO 3 Flake crystallite size<50. Mu m, grain edge [001]]A preferential orientation of the direction;
step 2: wrapping the ceramic biscuit in Bai Jinpian, covering fine-grain matrixes on the upper and lower surfaces of the ceramic biscuit, and sintering the ceramic biscuit at high temperature in an oxygen atmosphere to obtain antiferroelectric energy storage ceramic with high fatigue resistance, low electric field and high energy storage density along the preferred orientation of [001 ];
wherein, the preparation process of the fine crystal matrix is as follows: according toxNaNbO 3 -(1-x)(Bi 0.5-y R y Na 0.5 )TiO 3 Is to weigh Na 2 CO 3 、Nb 2 O 5 、Bi 2 O 3 、TiO 2 Ball-milling and mixing the rare earth oxide, and presintering for 2-8 hours at 650-900 ℃ to obtain an NN-BRNT fine crystal matrix;
the obtained antiferroelectric energy storage ceramic with high fatigue resistance, low electric field and high energy storage density<Effective energy storage density W in low electric field of 250kV/cm rec Up to 5J/cm 3 The energy storage efficiency is higher than 80%.
2. The method according to claim 1, wherein the rare earth oxide is La 2 O 3 、Pr 2 O 3 、Nd 2 O 3 、Sm 2 O 3 One of them.
3. The method according to claim 1, wherein the high temperature sintering in step 2 is performed at a temperature of 1000-1300 ℃ for a time of 1-15 hours at a gas flow rate of 0.1-2L/min.
4. The use of the antiferroelectric energy-storage ceramic of high fatigue resistance, low electric field and high energy storage density prepared by the method of claim 1 in electronic devices.
5. An energy storage ceramic electrode is characterized in that the energy storage ceramic electrode is made of antiferroelectric energy storage ceramic with high fatigue resistance, low electric field and high energy storage density, which is prepared by the method of claim 1.
6. The method for preparing the energy storage ceramic electrode according to claim 5, wherein the preparation method comprises the following steps:
polishing the (001) surface of the energy-storage ceramic, sputtering a gold electrode on the upper surface and the lower surface of the energy-storage ceramic, uniformly coating silver paste on the surface of the gold electrode, and sintering the silver-permeation electrode at 650 ℃ for 30 minutes to obtain the energy-storage ceramic electrode.
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