CN108585515B - Bismuth niobate-based glass ceramic material with high energy storage density and preparation method and application thereof - Google Patents
Bismuth niobate-based glass ceramic material with high energy storage density and preparation method and application thereof Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C10/00—Devitrified glass ceramics, i.e. glass ceramics having a crystalline phase dispersed in a glassy phase and constituting at least 50% by weight of the total composition
- C03C10/0009—Devitrified glass ceramics, i.e. glass ceramics having a crystalline phase dispersed in a glassy phase and constituting at least 50% by weight of the total composition containing silica as main constituent
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B19/00—Other methods of shaping glass
- C03B19/02—Other methods of shaping glass by casting molten glass, e.g. injection moulding
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B32/00—Thermal after-treatment of glass products not provided for in groups C03B19/00, C03B25/00 - C03B31/00 or C03B37/00, e.g. crystallisation, eliminating gas inclusions or other impurities; Hot-pressing vitrified, non-porous, shaped glass products
- C03B32/02—Thermal crystallisation, e.g. for crystallising glass bodies into glass-ceramic articles
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G4/00—Fixed capacitors; Processes of their manufacture
- H01G4/002—Details
- H01G4/018—Dielectrics
- H01G4/06—Solid dielectrics
- H01G4/08—Inorganic dielectrics
- H01G4/10—Metal-oxide dielectrics
- H01G4/105—Glass dielectric
Abstract
The invention relates to a bismuth niobate-based glass ceramic material with high energy storage density, a preparation method and application thereof, wherein the chemical composition of the bismuth niobate-based glass ceramic material conforms to a general formula of 25Bi2O3‑25Nb2O5‑50SiO2The main crystal phase is bismuth niobate; the preparation method adopts a high-temperature melting-controlled crystallization method. Compared with the prior art, the invention has the advantages of higher energy storage density, better temperature stability, simple preparation method, low cost, larger potential of subsequent research and application, and the like.
Description
Technical Field
The invention relates to the field of dielectric energy storage materials, in particular to a bismuth niobate-based glass ceramic material with high energy storage density and a preparation method thereof.
Background
In recent years, pulse counting has been widely used in the fields of electronic computers, televisions, communications, radars, remote control and measurement, automatic control, radio navigation, and measurement techniques, etc., as an important component in various electronic systems. Pulse technology refers to short-time energy release with power above a hundred Megawatts (MW) and pulse width less than 1 s. The pulse power device can be simplified in that low-power electric energy is stored in an energy storage device, such as a capacitor and the like, when the stored energy reaches a specified value, the stored energy is rapidly released in a very short time through the conversion of a charge-discharge circuit, so as to achieve the purpose of high-current and high-power output. The evaluation of the pulse power system mainly has two parameters, namely the size of reservoir energy and the speed of charge and discharge. Because the energy storage density of the currently practical energy storage material is lower, the pulse power system is too large in size, and the application of the technology is greatly limited. Therefore, it is a common knowledge of researchers to find stable energy storage materials with high energy storage density.
The glass ceramic energy storage material is prepared by adopting a high-temperature melting method, firstly melting raw materials with specific proportion to prepare glass molten slurry, and then quenching the obtained molten slurry to obtain the glass ceramic energy storage materialAmorphous bulk glass with uniform composition, and finally, preparing the non-porous glass-ceramic consisting of crystal phase particles with submicron or nanometer size and residual glass phase by a controllable crystallization method. In the controllable crystallization process, the effective control of the size, the shape and the content of crystal phase particles can be realized by adjusting the relative proportion of the metal oxide generating the ceramic phase and the glass phase network forming body and the control of the subsequent crystallization treatment process, thereby ensuring that the performance of the glass ceramic material has larger adjustability. The glass ceramic prepared by high-temperature melting and controllable crystallization has the characteristics of high density, high breakdown resistance and high energy storage density. In recent years, niobate glass ceramics are thermoelectric of high energy storage glass ceramic materials studied at home and abroad. The niobate microcrystalline glass is a composite material mainly composed of niobate crystals with tungsten bronze type structures and perovskite structures and a glass phase. In a niobate glass ceramic system, some scholars perform corresponding optimization and doping modification researches on the niobate glass ceramic system. Na reported by Guo-hua Chen et al2O-BaO-SrO-Nb2O5-B2O3-SiO2The glass ceramic reaches 4.0J/cm3The energy storage density of (1). Yi Zhou et al BaO-Na2O-Nb2O5-SiO2Is added with Gd2O3The results show that 1 mol% of Gd was added2O3Obviously improves the dielectric property of the glass ceramic, and the breakdown resistant field strength and the dielectric constant of the glass ceramic respectively reach 349 kV/mm and 56.16kV/mm3，SrCO3，Nb2O5，H3BO3As raw materials, the influence of different Sr/Ba ratios on the dielectric property of the glass ceramic is researched. M.P.Graca et al investigated the heat treatment on SiO2-Na2O-Nb2O5The influence of the electrical and dielectric properties of the glass-based ceramic was found to have a composition of 60SiO2-30Na2O-10Nb2O5The glass of the system is thermally treated at 650 ℃ for 4 hours, and the dielectric constant of the material is up to 48.19. The barium strontium niobate-based glass ceramic is prepared by Shyu and the like through an integral crystallization method, the SBN phase content is increased along with the increase of the sintering temperature, the calculated crystallization phase content is up to 40 percent, and the dielectric constant is highThe number is at most 180. (SrO, BaO) -Nb subsequently investigated2O5When the crystallization temperature of the system glass ceramic is lower than 1000 ℃, the dielectric constant of a sample is up to 351, the breakdown strength is up to 4.5kV/cm, and the residual polarization strength is 0.15 mu C/cm2. Subsequently, Zeng et al studied BaF2Additive pair SrO-BaO-Nb2O5-B2O3The influence of the crystallization kinetics and the dielectric property of the glass, and the dielectric constant of the microcrystalline glass of the system is found to be dependent on BaF2The increase in the amount of addition shows a change of increasing first and then decreasing, and the breakdown resistance tends to increase. When 5 mol% of BaF is added2Then, the microcrystalline glass ceramic with optimal performance is obtained, wherein the dielectric constant is 337, and the breakdown-resistant field strength is 527 kV/cm. Jun Luo et al are based on Na2O-PbO-Nb2O5-SiO2The glass ceramic system can successfully prepare the capacitor with a multilayer structure and excellent performance, and the energy storage density reaches 8J/cm3。
In the past research, oxides or oxycarbides of barium, potassium, sodium, strontium and other elements are mainly used as raw materials for the glass phase in glass ceramics, and the finally obtained glass ceramic crystal phase is mostly composed of these elements, niobium and oxygen, such as barium titanate (BaTiO)3) Strontium barium niobate (Sr)xBa1-xNb2O6) Barium strontium titanate (Sr)xBa1-xTiO3) Sodium niobate (NaNbO)3) In the background of years of research, the development of energy storage density approaches the bottleneck stage, and it is necessary to try to develop a new material system with high energy storage density.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provide a bismuth niobate-based glass ceramic material with high energy storage density, a preparation method and application thereof.
The purpose of the invention can be realized by the following technical scheme:
the chemical composition of the bismuth niobate-based glass ceramic material with high energy storage density conforms to the general formula of 25Bi2O3-25Nb2O5-50SiO2Main crystal phaseIs bismuth niobate.
The preparation method of the bismuth niobate-based glass ceramic material with high energy storage density comprises the following steps:
(1) with Bi2O3、Nb2O5And SiO2As a raw material, according to 25Bi2O3-25Nb2O5-50SiO2The materials are mixed according to the molar chemical ratio, and are melted at high temperature after being uniformly mixed by tumbling to obtain high-temperature glass melt;
(2) pouring the high-temperature glass molten slurry prepared in the step (1) into a preheated copper mold for molding, maintaining the preheating temperature to remove residual stress in the glass, preparing amorphous glass with uniform components, and slicing to obtain a glass sheet;
(3) and (3) performing controlled crystallization on the glass sheet prepared in the step (2) to obtain the bismuth niobate-based glass ceramic material with high energy storage density.
Preferably, the process conditions of the high-temperature melting in the step (1) are as follows: preserving the heat for 1-3 h at 1500-1600 ℃.
Preferably, the process conditions of the high-temperature melting in the step (1) are as follows: incubate at 1550 ℃ for 2 h.
Preferably, in the step (2), the high-temperature glass molten slurry prepared in the step (1) is poured into a copper mold preheated to 600 ℃ for molding, and the preheating temperature is kept for 6h to remove residual stress in the glass.
Preferably, the controlled crystallization conditions in step (3) are: heating to 700-900 ℃ at a heating rate of 2-4 ℃/min, and preserving heat for 4-8 h.
Preferably, the controlled crystallization conditions in step (3) are: heating to 700-900 ℃ at a heating rate of 3 ℃/min, and preserving heat for 6 h.
Preferably, the conditions for the optimally controlled crystallization in step (3) are: heating to 800 ℃ at the heating rate of 3 ℃/min, and keeping the temperature for 6 h.
The bismuth niobate-based glass ceramic material with high energy storage density can be used as an energy storage capacitor material.
The invention is based on 25Bi2O3-25Nb2O5-50SiO2(mol%) of the raw materials are mixed,by adjusting the crystallization temperature of the glass ceramic, the dielectric constant and the breakdown-resistant field strength are both maintained at a higher level. Particularly, when the crystallization temperature is 800 ℃, the energy storage density reaches the maximum value, and the theoretical energy storage density reaches 17.16J/cm3。
Compared with the prior art, the invention has the following advantages:
(1) the invention relates to a bismuth-containing bismuth with a molar composition ratio of 25Bi2O3-25Nb2O5-50SiO2Compared with the previous research on the glass ceramic, the glass ceramic taking bismuth niobate as the main crystal phase of the glass ceramic is obviously different from the common crystal phase of the glass ceramic, has higher energy storage density value, can be used for manufacturing a capacitor with high energy storage density, can continuously develop the research on the glass ceramic taking bismuth niobate as the main crystal phase on the basis, and has higher deep research value and practical application significance.
(2) The preparation method is simple, the temperature stability is good, the processability is good, and the crystallization temperature range is wide.
The invention is based on 25Bi2O3-25Nb2O5-50SiO2The glass ceramic with bismuth niobate as the main crystal phase is successfully separated out by proportioning (mol%), has high energy storage density, can be used for manufacturing high energy storage density capacitors, can be continuously researched on the basis, and has great deep research value and practical application significance.
Drawings
FIG. 1 shows 25Bi at different crystallization temperatures2O3-25Nb2O5-50SiO2(mol%) energy storage density of the glass ceramic energy storage material;
FIG. 2 shows 25Bi at different crystallization temperatures2O3-25Nb2O5-50SiO2(mol%) dielectric constant of the glass-ceramic energy storage material;
FIG. 3 shows 25Bi at different crystallization temperatures2O3-25Nb2O5-50SiO2(mol%) Wei of breakdown-resistant field strength of glass ceramic energy storage materialFill profile curve;
FIG. 4 shows 25Bi at different crystallization temperatures2O3-25Nb2O5-50SiO2(mol%) XRD spectrogram of the glass ceramic energy storage material;
FIGS. 5(a) to (e) show 25Bi contents at different crystallization temperatures in examples 1 to 52O3-25Nb2O5-50SiO2SEM image of (mol%) glass ceramic energy storage material.
Detailed Description
The chemical composition of the bismuth niobate-based glass ceramic material with high energy storage density conforms to the general formula of 25Bi2O3-25Nb2O5-50SiO2The main crystal phase is bismuth niobate.
The preparation method of the bismuth niobate-based glass ceramic material with high energy storage density comprises the following steps:
(1) with Bi2O3、Nb2O5And SiO2As a raw material, according to 25Bi2O3-25Nb2O5-50SiO2The materials are mixed according to the molar chemical ratio, and are melted at high temperature after being uniformly mixed by tumbling to obtain high-temperature glass melt;
(2) pouring the high-temperature glass molten slurry prepared in the step (1) into a preheated copper mold for molding, maintaining the preheating temperature to remove residual stress in the glass, preparing amorphous glass with uniform components, and slicing to obtain a glass sheet;
(3) and (3) performing controlled crystallization on the glass sheet prepared in the step (2) to obtain the bismuth niobate-based glass ceramic material with high energy storage density.
The preferable process conditions of the high-temperature melting in the step (1) are as follows: preserving the heat for 1-3 h at 1500-1600 ℃. Further preferably, the process conditions of the high-temperature melting in the step (1) are as follows: incubate at 1550 ℃ for 2 h.
Preferably, in the step (2), the high-temperature glass molten slurry prepared in the step (1) is poured into a copper mold preheated to 600 ℃ for molding, and the preheating temperature is kept for 6h to remove residual stress in the glass.
The preferable conditions for controlled crystallization in step (3) are: heating to 700-900 ℃ at a heating rate of 2-4 ℃/min, and preserving heat for 4-8 h. Further preferred conditions for controlled crystallization in step (3) are: heating to 700-900 ℃ at a heating rate of 3 ℃/min, and preserving heat for 6 h. Further preferred conditions for the optimally controlled crystallization in step (3) are: heating to 800 ℃ at the heating rate of 3 ℃/min, and keeping the temperature for 6 h.
The invention is described in detail below with reference to the figures and specific embodiments.
Example 1
The preparation method of the bismuth niobate-based glass ceramic energy storage material with high energy storage density comprises the following steps:
(1) with a purity of more than 99 wt.% of Bi2O3，Nb2O5，SiO2The raw materials are mixed, the mol percentage of each component is 25 percent, 25 percent and 50 percent, the mixture is ball milled and mixed for 24 hours, and after being dried for 6 hours at 120 ℃, the mixture is melted for 2 hours at 1550 ℃; (the ball milling takes absolute ethyl alcohol as a medium, and the ball-to-material ratio is 1.5: 1).
(2) Pouring the high-temperature melt obtained in the step (1) into a square copper mold, performing stress relief annealing at the temperature of 600 ℃ for 6 hours, and then cutting to obtain a glass sheet with the thickness of 1.0-1.5 mm;
(3) and (3) putting the glass sheets prepared in the step (2) into a square crucible in equal quantity, heating to 700 ℃ at a heating speed of 3 ℃/min, and then preserving heat for 6h to obtain the glass ceramic.
The energy storage density of the sample prepared in this example is shown in FIG. 1, and is 13.41J/cm3The material can be applied to energy storage capacitor materials. The dielectric properties are shown in FIG. 2, 67; the pressure resistance test is shown in FIG. 3, which is 2126 kV/cm; XRD is shown in figure 4, wherein the precipitated crystal phase is alpha-BiNbO4SEM is shown in FIG. 5 (a). The microscopic appearance of the glass ceramic is found to be very compact by SEM, and after crystallization, the ceramic phase and the residual glass phase form a structure without gaps, so that the glass ceramic has higher breakdown field strength.
Example 2
The preparation method of the bismuth niobate-based glass ceramic energy storage material with high energy storage density comprises the following steps
(1) In a purity of greater than 99 wt%Bi2O3，Nb2O5，SiO2The raw materials are mixed, the mol percentage of each component is 25 percent, 25 percent and 50 percent, the mixture is ball milled and mixed for 24 hours, and after being dried for 6 hours at 120 ℃, the mixture is melted for 2 hours at 1550 ℃; (the ball milling takes absolute ethyl alcohol as a medium, and the ball-to-material ratio is 1.5: 1).
(2) Pouring the high-temperature melt obtained in the step (1) into a square copper mold, performing stress relief annealing at the temperature of 600 ℃ for 6 hours, and then cutting to obtain a glass sheet with the thickness of 1.0-1.5 mm;
(3) and (3) putting an equal number of the glass sheets prepared in the step (2) into a square crucible, heating to 750 ℃ at a heating speed of 3 ℃/min, and preserving heat for 6h to obtain the glass ceramic.
The energy storage density of the sample prepared in this example is shown in FIG. 1, and is 15.13J/cm3The material can be applied to energy storage capacitor materials. The dielectric properties are shown in FIG. 2, 84; the withstand voltage performance test is 2017kV/cm as shown in FIG. 3; XRD is shown in figure 4, wherein the precipitated crystal phase is alpha-BiNbO4SEM is shown in FIG. 5 (b). The microscopic appearance of the glass ceramic is found to be very compact by SEM, and after crystallization, the ceramic phase and the glass phase form a structure without gaps, so that the glass ceramic has higher breakdown field strength.
Example 3
The preparation method of the bismuth niobate-based glass ceramic energy storage material with high energy storage density comprises the following steps:
(1) with a purity of more than 99 wt.% of Bi2O3，Nb2O5，SiO2The raw materials are mixed, the mol percentage of each component is 25 percent, 25 percent and 50 percent, the mixture is ball milled and mixed for 24 hours, and after being dried for 6 hours at 120 ℃, the mixture is melted for 2 hours at 1550 ℃; (the ball milling takes absolute ethyl alcohol as a medium, and the ball-to-material ratio is 1.5: 1).
(2) Pouring the high-temperature melt obtained in the step (1) into a square copper mold, performing stress relief annealing at the temperature of 600 ℃ for 6 hours, and then cutting to obtain a glass sheet with the thickness of 1.0-1.5 mm;
(3) and (3) putting the glass sheets prepared in the step (2) into a square crucible in equal quantity, heating to 800 ℃ at a heating speed of 3 ℃/min, and then preserving heat for 6h to obtain the glass ceramic.
The energy storage density of the sample prepared in this example is shown in FIG. 1, and is 17.16J/cm3The material can be applied to energy storage capacitor materials. The dielectric properties are shown in FIG. 2, 121; the voltage endurance test is 1790kV/cm as shown in FIG. 3; XRD is shown in figure 4, wherein the precipitated crystal phase is beta-BiNbO4SEM is shown in FIG. 5 (c). The microscopic appearance of the glass ceramic is found to be very compact by SEM, and after crystallization, the ceramic phase and the glass phase form a structure without gaps, so that the glass ceramic has higher breakdown field strength.
Example 4
The preparation method of the bismuth niobate-based glass ceramic energy storage material with high energy storage density comprises the following steps:
(1) with a purity of more than 99 wt.% of Bi2O3，Nb2O5，SiO2The raw materials are mixed, the mol percentage of each component is 25 percent, 25 percent and 50 percent, the mixture is ball milled and mixed for 24 hours, and after being dried for 6 hours at 120 ℃, the mixture is melted for 2 hours at 1550 ℃; (the ball milling takes absolute ethyl alcohol as a medium, and the ball-to-material ratio is 1.5: 1).
(2) Pouring the high-temperature melt obtained in the step (1) into a square copper mold, performing stress relief annealing at the temperature of 600 ℃ for 6 hours, and then cutting to obtain a glass sheet with the thickness of 1.0-1.5 mm;
(3) and (3) putting an equal number of the glass sheets prepared in the step (2) into a square crucible, heating to 850 ℃ at a heating speed of 3 ℃/min, and preserving heat for 6h to obtain the glass ceramic.
The energy storage density of the sample prepared in this example is shown in FIG. 1, and is 9.54J/cm3The material can be applied to energy storage capacitor materials. The dielectric properties are shown in FIG. 2, which is 89; the withstand voltage performance test is 1556kV/cm as shown in FIG. 3; XRD is shown in figure 4, wherein the precipitated crystal phase is beta-BiNbO4SEM is shown in FIG. 5 (d). The microscopic appearance of the glass ceramic is found to be very compact by SEM, and after crystallization, the ceramic phase and the glass phase form a structure without gaps, so that the glass ceramic has higher breakdown field strength.
Example 5
The preparation method of the bismuth niobate-based glass ceramic energy storage material with high energy storage density comprises the following steps:
(1) with a purity of more than 99 wt.% of Bi2O3，Nb2O5，SiO2The raw materials are mixed, the mol percentage of each component is 25 percent, 25 percent and 50 percent, the mixture is ball milled and mixed for 24 hours, and after being dried for 6 hours at 120 ℃, the mixture is melted for 2 hours at 1550 ℃; (the ball milling takes absolute ethyl alcohol as a medium, and the ball-to-material ratio is 1.5: 1).
(2) Pouring the high-temperature melt obtained in the step (1) into a square copper mold, performing stress relief annealing at the temperature of 600 ℃ for 6 hours, and then cutting to obtain a glass sheet with the thickness of 1.0-1.5 mm;
(3) and (3) putting an equal number of the glass sheets prepared in the step (2) into a square crucible, heating to 900 ℃ at a heating rate of 3 ℃/min, and preserving heat for 6h to obtain the glass ceramic.
The energy storage density of the sample prepared in this example is shown in FIG. 1, and is 3.62J/cm3The material can be applied to energy storage capacitor materials. The dielectric properties are as shown in FIG. 2, 45; the voltage resistance test is shown in FIG. 3 and is 1348 kV/cm; XRD is shown in figure 4, wherein the precipitated crystal phase is beta-BiNbO4SEM is shown in FIG. 5 (e). The microscopic appearance of the glass ceramic is found to be very compact by SEM, and after crystallization, the ceramic phase and the glass phase form a structure without gaps, so that the glass ceramic has higher breakdown field strength.
The embodiments described above are intended to facilitate the understanding and use of the invention by those skilled in the art. It will be readily apparent to those skilled in the art that various modifications to these embodiments may be made, and the generic principles described herein may be applied to other embodiments without the use of the inventive faculty. Therefore, the present invention is not limited to the above embodiments, and those skilled in the art should make improvements and modifications within the scope of the present invention based on the disclosure of the present invention.
Claims (7)
1. The bismuth niobate-based glass ceramic material with high energy storage density is characterized in that the bismuth niobate-based glass ceramic material is used as an energy storage capacitor material, and the chemical composition of the bismuth niobate-based glass ceramic material is measured by molar ratioIs 25Bi2O3-25Nb2O5-50SiO2The main crystal phase is bismuth niobate, and the theoretical energy storage density of the material reaches 17.16J/cm3；
The preparation method of the bismuth niobate-based glass ceramic material with high energy storage density comprises the following steps:
(1) with Bi2O3、Nb2O5And SiO2As a raw material, according to 25Bi2O3-25Nb2O5-50SiO2The materials are mixed according to the molar chemical ratio, and are melted at high temperature after being uniformly mixed by tumbling to obtain high-temperature glass melt;
(2) pouring the high-temperature glass molten slurry prepared in the step (1) into a preheated copper mold for molding and maintaining to remove residual stress in the glass, preparing amorphous glass with uniform components, and slicing to obtain a glass sheet;
(3) performing controlled crystallization on the glass sheet prepared in the step (2) to obtain the bismuth niobate-based glass ceramic material with high energy storage density;
the controlled crystallization conditions in the step (3) are as follows: heating to 700-900 ℃ at a heating rate of 3 ℃/min, and preserving heat for 6 h.
2. The method for preparing the bismuth niobate-based glass ceramic material with high energy storage density according to claim 1, comprising the following steps:
(1) with Bi2O3、Nb2O5And SiO2As a raw material, according to 25Bi2O3-25Nb2O5-50SiO2The materials are mixed according to the molar chemical ratio, and are melted at high temperature after being uniformly mixed by tumbling to obtain high-temperature glass melt;
(2) pouring the high-temperature glass molten slurry prepared in the step (1) into a preheated copper mold for molding and maintaining to remove residual stress in the glass, preparing amorphous glass with uniform components, and slicing to obtain a glass sheet;
(3) and (3) performing controlled crystallization on the glass sheet prepared in the step (2) to obtain the bismuth niobate-based glass ceramic material with high energy storage density.
3. The preparation method of the bismuth niobate-based glass ceramic material with high energy storage density as claimed in claim 2, wherein the process conditions of the high-temperature melting in the step (1) are as follows: preserving the heat for 1-3 h at 1500-1600 ℃.
4. The preparation method of the bismuth niobate-based glass ceramic material with high energy storage density as claimed in claim 3, wherein the process conditions of the high-temperature melting in the step (1) are as follows: incubate at 1550 ℃ for 2 h.
5. The method for preparing the bismuth niobate-based glass ceramic material with high energy storage density as claimed in claim 2, wherein in the step (2), the high-temperature glass melt slurry prepared in the step (1) is poured into a copper mold preheated to 600 ℃ for molding and is kept for 6h to remove the residual stress in the glass.
6. The preparation method of the bismuth niobate-based glass ceramic material with high energy storage density as claimed in claim 2, wherein the controlled crystallization conditions in the step (3) are as follows: heating to 800 ℃ at the heating rate of 3 ℃/min, and keeping the temperature for 6 h.
7. The use of bismuth niobate-based glass ceramic materials with high energy storage density according to claim 1 as energy storage capacitor materials.
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| BISMUTH NIOBATE-BASED GLASS-CERAMICS FOR DIELECTRICALLY LOADED MICROWAVE ANTENNAS;MEHDI MIRSANEH等;《Functional Materials Letters》;20080630;第1卷(第1期);第25-30页 * |
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