CN115536390A - Transparent dielectric energy storage ceramic material and preparation method and application thereof - Google Patents
Transparent dielectric energy storage ceramic material and preparation method and application thereof Download PDFInfo
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Abstract
The invention provides a sodium niobate-bismuth magnesium niobate-barium magnesium niobate-strontium titanate transparent medium energy storage ceramic material, which has the composition formula: 0.95[ 2 ], [0.90NaNbO ] 3 ‑0.10((1‑x)Bi(Mg 2/3 Nb 1/3 )O 3 ‑xBa(Mg 1/3 Nb 2/3 )O 3 )]‑0.05SrTiO 3 X is mole percentage, x is more than or equal to 0.10 and less than or equal to 0.25. Also provides a preparation method, which is to dry Na 2 CO 3 Raw material, bi 2 O 3 Raw material, baCO 3 Raw material SrCO 3 Raw material, nb 2 O 5 Raw material, tiO 2 The raw materials and MgO raw materials are weighed and mixed, and then are subjected to ball milling, presintering, secondary ball milling, tabletting and sintering, and then are subjected to polishing and surface metallization to prepare the magnesium-based alloy material. The preparation method is simple, good in repeatability, high in yield, and excellent in energy storage performance and certain in light transmittance. Strong practicability, easy routine batch production and capacity of being used simultaneouslyGu Chuneng performance and optical performance, is a lead-free transparent energy storage ceramic with excellent performance, and is expected to be used in the aspects of transparent pulse capacitors and the like.
Description
Technical Field
The invention belongs to the technical field of ceramic materials, and particularly relates to a sodium niobate-bismuth magnesium niobate-barium magnesium niobate-strontium titanate transparent medium energy storage ceramic material, and a preparation method and application thereof.
Background
The dielectric capacitor is widely applied to the fields of pulse power systems, electric automobiles, aerospace, defense technologies and the like as an extremely key electronic component. In recent years, with the development of miniaturization, light weight, safety and diversification of application fields of electronic components, inorganic electronic information materials advance toward high efficiency, high reliability, intellectualization and function integration, and further, higher requirements are provided for innovation of design and preparation technology of new materials, and multiple functional responses are realized in the same dielectric material, so that the inorganic electronic information materials become one of research hotspots of novel intelligent materials.
Sodium niobate ceramic is an important system of dielectric capacitor materials, and is considered as the material with the most commercial application potential due to the wide band gap (large breakdown electric field), no volatile K element (easy preparation) and low volume density (light weight), thereby causing wide attention of wide scientific and technological workers and enterprises. At present, regarding the research of sodium niobate-based ceramics, most researchers mainly focus on the aspects of improving and optimizing energy storage performance, on one hand, the large delta P (Pmax-Pr) is obtained by destroying the long-range order of ferroelectrics and enhancing the relaxation characteristic thereof through the local random field formed by doping A/B site ions and solid solution of two-phase and multi-phase components; on the other hand, the crystal grains with uniform distribution and fine size are obtained through the optimization of the preparation process, so that the breakdown field intensity (Eb) of the material is improved, and the energy storage characteristic of the material is improved.
Considering the development of high intelligence and high integration of materials and the development and application of transparent pulse capacitors, the design and preparation of new materials combining energy storage performance and optical transparency conform to the current material design concept, and especially play an extremely important role in the development of new-generation transparent pulse capacitors.
Disclosure of Invention
The technical problem to be solved by the invention is to provide a sodium niobate-bismuth magnesium niobate-barium magnesium niobate-strontium titanate transparent medium energy storage ceramic material, a preparation method and application thereof aiming at the defects of the prior art, wherein the preparation method is simple, good in repeatability, high in yield, and excellent in energy storage performance and certain in light transmittance. The material has strong practicability, is easy for routine batch production, can give consideration to energy storage performance and optical performance, is lead-free transparent energy storage ceramic with excellent performance, and is expected to be used in the aspects of transparent pulse capacitors and the like.
In order to solve the technical problems, the invention adopts the technical scheme that: a sodium niobate-bismuth magnesium niobate-barium magnesium niobate-strontium titanate transparent medium energy storage ceramic material has a composition formula as follows: 0.95[ 2 ], [0.90NaNbO ] 3 -0.10((1-x)Bi(Mg 2/3 Nb 1/3 )O 3 -xBa(Mg 1/3 Nb 2/3 )O 3 )]-0.05SrTiO 3 Wherein x is mole percentage, x is more than or equal to 0.10 and less than or equal to 0.25.
The invention also provides a method for preparing the sodium niobate-bismuth magnesium niobate-barium magnesium niobate-strontium titanate transparent medium energy storage ceramic material, which comprises the following steps:
s1, drying materials: respectively adding Na 2 CO 3 Raw material, bi 2 O 3 Raw material, baCO 3 Raw material and SrCO 3 Drying the raw materials for 6h at 300 ℃ respectively;
nb to 2 O 5 Raw material, tiO 2 Respectively drying the raw material and the MgO raw material for 4 hours in strips at the temperature of 900 ℃;
the Na is 2 CO 3 The purity of the raw material is 99.8 percent, and the Bi is 2 O 3 The purity of the raw material is 99.8 percent, and the BaCO 3 The purity of the raw material is 99 percent, and the SrCO 3 Raw materialsHas a purity of 99%, and the Nb 2 O 5 The purity of (2) is 99.5%, and the purity of the MgO raw material is 98.5%;
s2, preparing materials: drying the dried Na in the S1 2 CO 3 Raw material, bi 2 O 3 Raw material, baCO 3 Raw material SrCO 3 Raw material, nb 2 O 5 Raw material, tiO 2 The raw material and MgO raw material are in accordance with 0.95[ 2 ], [0.90NaNbO ] 3 -0.10((1-x)Bi(Mg 2/3 Nb 1/3 )O 3 -x Ba(Mg 1/ 3 Nb 2/3 )O 3 )]-0.05SrTiO 3 Respectively weighing the above stoichiometric ratio, uniformly mixing to obtain a premix, adding agate balls and absolute ethyl alcohol, ball-milling for 6-10 h, separating the agate balls, drying at 80-100 ℃ for 12-24 h, and sieving with a 120-mesh sieve to obtain a raw material mixture;
s3, pre-burning: pre-burning the raw material mixture obtained in the step S2 for 2 to 4 hours at the temperature of 850 to 950 ℃, naturally cooling to room temperature, and grinding to obtain pre-burnt powder;
s4, secondary ball milling: adding agate balls and absolute ethyl alcohol into the pre-sintering powder obtained in the step S3, performing ball milling for 6-10 h, separating the agate balls, drying at the temperature of 80-100 ℃ for 12-24 h, and sieving with a 180-mesh sieve after grinding to obtain pre-sintering powder after ball milling;
s5, tabletting, namely adding 6% polyvinyl alcohol aqueous solution in mass percentage into the pre-sintered powder after the grinding balls obtained in the S4, granulating, sieving by a 40-mesh sieve to obtain spherical powder substances, and maintaining the pressure for 20-60S under the condition of the unidirectional pressure of 150-200 MPa to obtain a wafer-shaped ceramic blank;
s6, sintering: sintering the disk-shaped ceramic blank obtained in the step S5 to obtain a sintered ceramic blank; the sintering conditions are as follows: firstly, heating up to 550 ℃ from room temperature at a heating rate of 3 ℃/min, keeping the temperature for 3h, then heating up to 1230-1300 ℃ at a heating rate of 3-5 ℃/min, sintering for 2-4 h, and then cooling to room temperature at a cooling rate of 5 ℃/min;
s7, polishing: polishing the upper surface and the lower surface of the sintered ceramic blank obtained in the step S6 by using 600-mesh abrasive paper, polishing the upper surface and the lower surface by using 2000-mesh abrasive paper and carborundum until the thickness is 0.3-0.5 mm, putting the polished ceramic blank into deionized water, ultrasonically cleaning and drying the polished ceramic blank to obtain a polished ceramic blank;
s8, surface metallization: and (4) uniformly coating silver pastes with the thickness of 0.01-0.03 mm on the upper surface and the lower surface of the polished ceramic blank obtained in the step (S7), preserving the heat for 10min at the temperature of 850 ℃, and naturally cooling to room temperature to obtain the sodium niobate-bismuth magnesium niobate-barium magnesium niobate-strontium titanate transparent medium energy storage ceramic material.
The invention selects Na 2 CO 3 Raw material, bi 2 O 3 Raw Material, baCO 3 、SrCO 3 Raw material, nb 2 O 5 Raw material, tiO 2 The raw materials and MgO are directly synthesized to prepare a quaternary solid solution system of sodium niobate, bismuth magnesium niobate, barium magnesium niobate and strontium titanate, and the synthesized components have a pseudo-cubic phase structure with higher symmetry, so that the birefringence phenomenon of incident light between adjacent crystal grains is effectively avoided, the light scattering loss is reduced, and the light transmittance of the ceramic material is improved; the ball milling is carried out twice in the preparation process, so that the uniform mixing and full reaction of the initial raw materials are facilitated to form a uniform single-phase structure, the powder particles are refined, the size and the air holes of ceramic grains are reduced, the compactness of the ceramic grains is improved, incident light can easily pass through crystals, meanwhile, the light scattering of a crystal boundary is reduced, and the transparency of the ceramic is improved.
Preferably, the dosage ratio of the premix, the agate balls and the absolute ethyl alcohol in the S2 is 0.35g: 0.52mL.
Preferably, the dosage ratio of the agate balls to the absolute ethyl alcohol added into the pre-sintering powder of S4 is 0.30g: 0.40mL.
Preferably, the mass ratio of the 6% polyvinyl alcohol aqueous solution to the pre-sintered powder after ball grinding in the S5 is (25% -35%): 1.
the invention also provides application of the prepared sodium niobate-bismuth magnesium niobate-barium magnesium niobate-strontium titanate transparent medium energy storage ceramic material, which is characterized in that the sodium niobate-bismuth magnesium niobate-barium magnesium niobate-strontium titanate transparent medium energy storage ceramic material has light transmission and is used for preparing transparent pulse capacitors.
Compared with the prior art, the invention has the following advantages:
the ceramic material prepared by the invention has simple preparation method, good repeatability and high yield, and the obtained 0.95[0.90NaNbO ] 3 -0.10((1-x)Bi(Mg 2/3 Nb 1/3 )O 3 -xBa(Mg 1/3 Nb 2/3 )O 3 )]-0.05SrTiO 3 The transparent dielectric energy storage ceramic material has excellent energy storage performance and certain light transmittance. The material has strong practicability, is easy for routine batch production, can give consideration to energy storage performance and optical performance, is lead-free transparent energy storage ceramic with excellent performance, and is expected to be used in the aspects of transparent pulse capacitors and the like.
The present invention will be described in further detail with reference to the drawings and examples.
Drawings
FIG. 1 is an XRD pattern of ceramic samples prepared in examples 1-4 of the present invention.
FIG. 2 is an electron microscope photograph of ceramic samples prepared in examples 1 to 4 of the present invention.
FIG. 3 is a graph of breakdown field strength for ceramic samples made in examples 1-4 of the present invention.
FIG. 4 is a P-E curve of ceramic samples made in examples 1-4 of the present invention.
FIG. 5 is a photograph of 0.95[ 2 ], [0.90NaNbO ] obtained in example 3 of the present invention 3 -0.10(0.80Bi(Mg 2/3 Nb 1/3 )O 3 -0.20Ba(Mg 1/3 Nb 2/3 )O 3 )]-0.05SrTiO 3 Temperature stability picture of energy storage performance of ceramic sample.
FIG. 6 is 0.95[0.90NaNbO ] produced in example 3 of the present invention 3 -0.10(0.80Bi(Mg 2/3 Nb 1/3 )O 3 -0.20Ba(Mg 1/3 Nb 2/3 )O 3 )]-0.05SrTiO 3 Frequency stability picture of energy storage performance of ceramic sample.
FIG. 7 is 0.95[ 2 ], [0.90NaNbO ] prepared in example 3 of the present invention 3 -0.10(0.80Bi(Mg 2/3 Nb 1/3 )O 3 -0.20Ba(Mg 1/3 Nb 2/3 )O 3 )]-0.05SrTiO 3 And (5) testing the light transmittance of the ceramic sample.
Detailed Description
Example 1
The sodium niobate-bismuth magnesium niobate-barium magnesium niobate-strontium titanate transparent medium energy storage ceramic material of the embodiment has a composition formula as follows: 0.95[ 2 ], [0.90NaNbO ] 3 -0.10(0.90Bi(Mg 2/3 Nb 1/3 )O 3 -0.10Ba(Mg 1/3 Nb 2/3 )O 3 )]-0.05SrTiO 3 。
The embodiment also provides a method for preparing the sodium niobate-bismuth magnesium niobate-barium magnesium niobate-strontium titanate transparent medium energy storage ceramic material, which comprises the following steps:
s1, drying materials: respectively adding Na 2 CO 3 Raw material, bi 2 O 3 Raw Material, baCO 3 Raw material and SrCO 3 Drying the raw materials for 6h at 300 ℃ respectively;
mixing Nb with 2 O 5 Raw material, tiO 2 Respectively drying the raw material and the MgO raw material for 4 hours in strips at the temperature of 900 ℃;
the Na is 2 CO 3 The purity of the raw material is 99.8 percent, and the Bi is 2 O 3 The purity of the raw material is 99.8 percent, and the BaCO is 3 The purity of the raw material is 99 percent, and the SrCO 3 The purity of the raw material is 99 percent, and the Nb is 2 O 5 The purity of the MgO raw material is 99.5 percent, the purity of the MgO raw material is 98.5 percent, and the MgO raw material is purchased from chemical reagents of national medicine group, inc.;
s2, preparing materials: drying the dried Na in the S1 2 CO 3 Raw material, bi 2 O 3 Raw material, baCO 3 Raw material SrCO 3 Raw Material, nb 2 O 5 Raw material, tiO 2 The raw material and MgO raw material are in accordance with 0.95[ 2 ], [0.90NaNbO ] 3 -0.10(0.90Bi(Mg 2/3 Nb 1/3 )O 3 -0.10Ba(Mg 1/ 3 Nb 2/3 )O 3 )]-0.05SrTiO 3 The stoichiometric ratio of (A) is respectively weighed, namely the dried Na is weighed 2 CO 3 5.1089g raw material and Bi 2 O 3 2.2642g raw material, baCO 3 0.2131g raw material, srCO 3 Raw materials 0.8391g, nb 2 O 5 13.3748g raw material, tiO 2 Uniformly mixing 0.4586g of raw material and 0.2770g of MgO raw material to obtain a premix, adding agate balls and absolute ethyl alcohol, carrying out ball milling at the speed of 300r/min for 8 hours, separating the agate balls, drying at the temperature of 90 ℃ for 12 hours, and sieving with a 120-mesh sieve to obtain a raw material mixture; the dosage ratio of the premix, the agate balls and the absolute ethyl alcohol is 0.35g: 0.52mL;
s3, pre-burning: pre-burning the raw material mixture obtained in the step S2 for 3 hours at the temperature of 900 ℃, naturally cooling to room temperature, and grinding to obtain pre-burnt powder;
s4, secondary ball milling: adding agate balls and absolute ethyl alcohol into the pre-sintering powder obtained in the S3, carrying out ball milling for 8 hours, separating the agate balls, drying at the temperature of 90 ℃ for 20 hours, and sieving through a 180-mesh sieve after grinding to obtain the pre-sintering powder after ball milling; the dosage ratio of the agate balls to the absolute ethyl alcohol added into the pre-sintering powder is 0.30g: 0.40mL;
s5, tabletting, namely adding 6% polyvinyl alcohol aqueous solution in percentage by mass into the pre-sintered powder after the grinding balls obtained in the S4, granulating, sieving by a 40-mesh sieve to obtain spherical powder substances, and maintaining the pressure for 40S under the condition of the unidirectional pressure of 180MPa to obtain a wafer-shaped ceramic blank; the mass ratio of the 6% polyvinyl alcohol aqueous solution to the pre-sintered powder after ball grinding is 30%:1;
s6, sintering: sintering the disk-shaped ceramic blank obtained in the step S5 to obtain a sintered ceramic blank; the sintering conditions are as follows: firstly, heating from room temperature to 550 ℃ at the heating rate of 3 ℃/min, preserving heat for 3h, then heating to 1250 ℃ at the heating rate of 4 ℃/min, sintering for 3h, and then cooling to room temperature at the cooling rate of 5 ℃/min;
s7, polishing: polishing the upper surface and the lower surface of the sintered ceramic blank obtained in the step S6 by using 600-mesh abrasive paper, polishing the upper surface and the lower surface by using 2000-mesh abrasive paper and carborundum until the thickness is 0.3mm, putting the ceramic blank into deionized water, ultrasonically cleaning and drying the ceramic blank to obtain a polished ceramic blank;
s8, surface metallization: and (4) uniformly coating silver pastes with the thickness of 0.03mm on the upper surface and the lower surface of the polished ceramic blank obtained in the step (S7), preserving the heat for 10min at the temperature of 850 ℃, and naturally cooling to room temperature to obtain the sodium niobate-bismuth magnesium niobate-barium magnesium niobate-strontium titanate transparent medium energy storage ceramic material.
Example 2
The sodium niobate-bismuth magnesium niobate-barium magnesium niobate-strontium titanate transparent medium energy storage ceramic material of the embodiment has a composition formula as follows: 0.95[ 2 ], [0.90NaNbO ] 3 -0.10(0.85Bi(Mg 2/3 Nb 1/3 )O 3 -0.15Ba(Mg 1/3 Nb 2/3 )O 3 )]-0.05SrTiO 3 。
The embodiment also provides a method for preparing the sodium niobate-bismuth magnesium niobate-barium magnesium niobate-strontium titanate transparent medium energy storage ceramic material, which comprises the following steps:
s1, drying materials: respectively adding Na 2 CO 3 Raw material, bi 2 O 3 Raw material, baCO 3 Raw material and SrCO 3 Drying the raw materials for 6h at 300 ℃ respectively;
mixing Nb with 2 O 5 Raw material, tiO 2 Respectively drying the raw material and the MgO raw material for 4 hours at the temperature of 900 ℃;
the Na is 2 CO 3 The purity of the raw material is 99.8 percent, and the Bi is 2 O 3 The purity of the raw material is 99.8 percent, and the BaCO is 3 The purity of the raw material is 99 percent, and the SrCO 3 The purity of the raw material is 99 percent, and the Nb is 2 O 5 The purity of the MgO raw material is 99.5 percent, the purity of the MgO raw material is 98.5 percent, and the MgO raw material is purchased from chemical reagents of national medicine group, inc.;
s2, preparing materials: drying the dried Na in the S1 2 CO 3 Raw material, bi 2 O 3 Raw Material, baCO 3 Raw material SrCO 3 Raw material, nb 2 O 5 Raw material, tiO 2 The raw material and MgO raw material were in accordance with 0.95[ 2 ], [0.90NaNbO ] 3 -0.10(0.85Bi(Mg 2/3 Nb 1/3 )O 3 -0.15Ba(Mg 1/ 3 Nb 2/3 )O 3 )]-0.05SrTiO 3 The stoichiometric ratio of (A) is respectively weighed, namely the dried Na is weighed 2 CO 3 5.1156g raw material and Bi 2 O 3 2.1412g raw material, baCO 3 0.3200g raw material, srCO 3 Raw materials 0.8401g, Nb 2 O 5 13.4161g raw material, tiO 2 Uniformly mixing 0.4592g of raw material and 0.2701g of MgO raw material to obtain a premix, adding agate balls and absolute ethyl alcohol, carrying out ball milling for 10 hours at the speed of 300r/min, separating the agate balls, drying for 24 hours at the temperature of 80 ℃, and sieving with a 120-mesh sieve to obtain a raw material mixture; the dosage ratio of the premix, the agate balls and the absolute ethyl alcohol is 0.35g: 0.52mL;
s3, pre-burning: pre-burning the raw material mixture obtained in the step S2 for 4 hours at the temperature of 850 ℃, naturally cooling to room temperature, and grinding to obtain pre-burnt powder;
s4, secondary ball milling: adding agate balls and absolute ethyl alcohol into the pre-sintering powder obtained in the step S3, carrying out ball milling for 6 hours, separating the agate balls, drying at the temperature of 80 ℃ for 24 hours, and sieving through a 180-mesh sieve after grinding to obtain the pre-sintering powder after ball milling; the dosage ratio of the agate balls to the absolute ethyl alcohol added into the pre-sintering powder is 0.30g: 0.40mL;
s5, tabletting, namely adding 6% polyvinyl alcohol aqueous solution in percentage by mass into the pre-sintered powder after the grinding balls obtained in the S4, granulating, sieving by a 40-mesh sieve to obtain spherical powder substances, and maintaining the pressure for 60S under the condition of 150MPa of one-way pressure to obtain a wafer-shaped ceramic blank; the mass ratio of the 6% polyvinyl alcohol aqueous solution to the pre-sintered powder after ball grinding is 25%:1;
s6, sintering: sintering the disk-shaped ceramic blank obtained in the step S5 to obtain a sintered ceramic blank; the sintering conditions are as follows: firstly, heating from room temperature to 550 ℃ at the heating rate of 3 ℃/min, keeping the temperature for 3h, then heating to 1230 ℃ at the heating rate of 3 ℃/min, sintering for 4h, and then cooling to room temperature at the cooling rate of 5 ℃/min;
s7, polishing: polishing the upper surface and the lower surface of the sintered ceramic blank obtained in the step S6 by using 600-mesh abrasive paper, polishing the upper surface and the lower surface by using 2000-mesh abrasive paper and carborundum until the thickness is 0.5mm, putting the ceramic blank into deionized water, ultrasonically cleaning and drying the ceramic blank to obtain a polished ceramic blank;
s8, surface metallization: and (4) uniformly coating silver pastes with the thickness of 0.01mm on the upper surface and the lower surface of the polished ceramic blank obtained in the step (S7), preserving the heat for 10min at the temperature of 850 ℃, and naturally cooling to room temperature to obtain the sodium niobate-bismuth magnesium niobate-barium magnesium niobate-strontium titanate transparent medium energy storage ceramic material.
Example 3
The sodium niobate-bismuth magnesium niobate-barium magnesium niobate-strontium titanate transparent medium energy storage ceramic material of the embodiment has a composition formula as follows: 0.95[ 2 ], [0.90NaNbO ] 3 -0.10(0.80Bi(Mg 2/3 Nb 1/3 )O 3 -0.20Ba(Mg 1/3 Nb 2/3 )O 3 )]-0.05SrTiO 3 。
The embodiment also provides a method for preparing the sodium niobate-bismuth magnesium niobate-barium magnesium niobate-strontium titanate transparent medium energy storage ceramic material, which comprises the following steps:
s1, drying materials: respectively adding Na 2 CO 3 Raw material, bi 2 O 3 Raw material, baCO 3 Raw material and SrCO 3 Drying the raw materials respectively at 300 ℃ for 6h;
nb to 2 O 5 Raw Material, tiO 2 Respectively drying the raw material and the MgO raw material for 4 hours in strips at the temperature of 900 ℃;
the Na is 2 CO 3 The purity of the raw material is 99.8 percent, and the Bi is 2 O 3 The purity of the raw material is 99.8 percent, and the BaCO 3 The purity of the raw material is 99 percent, and the SrCO 3 The purity of the raw material is 99 percent, and the Nb is 2 O 5 The purity of the MgO raw material is 99.5 percent, the purity of the MgO raw material is 98.5 percent, and the MgO raw material is purchased from chemical reagents of national medicine group, inc.;
s2, preparing materials: drying the dried Na in the S1 2 CO 3 Raw material, bi 2 O 3 Raw material, baCO 3 Raw material SrCO 3 Raw material, nb 2 O 5 Raw Material, tiO 2 The raw material and MgO raw material are in accordance with 0.95[ 2 ], [0.90NaNbO ] 3 -0.10(0.8Bi(Mg 2/3 Nb 1/3 )O 3 -0.2Ba(Mg 1/3 Nb 2/3 )O 3 )]-0.05SrTiO 3 The stoichiometric ratio of (A) is respectively weighed, namely the dried Na is weighed 2 CO 3 5.1223g raw material and Bi 2 O 3 Feedstock 2.0179g, baCO 3 Feedstock 0.4273g、SrCO 3 0.8412g, nb 2 O 5 13.4575g raw material, tiO 2 Uniformly mixing 0.4598g raw material and 0.2631g MgO raw material to obtain a premix, adding agate balls and absolute ethyl alcohol, carrying out ball milling at the speed of 300r/min for 6h, separating the agate balls, drying at the temperature of 100 ℃ for 12h, and sieving with a 120-mesh sieve to obtain a raw material mixture; the dosage ratio of the premix, the agate balls and the absolute ethyl alcohol is 0.35g: 0.52mL;
s3, pre-burning: pre-burning the raw material mixture obtained in the step S2 for 2 hours at the temperature of 950 ℃, naturally cooling to room temperature, and grinding to obtain pre-burnt powder;
s4, secondary ball milling: adding agate balls and absolute ethyl alcohol into the pre-sintering powder obtained in the step S3, carrying out ball milling for 10 hours, separating the agate balls, drying at the temperature of 100 ℃ for 12 hours, and sieving through a 180-mesh sieve after grinding to obtain the pre-sintering powder after ball milling; the dosage ratio of the agate balls to the absolute ethyl alcohol added into the pre-sintering powder is 0.30g: 0.40mL;
s5, tabletting, namely adding 6% polyvinyl alcohol aqueous solution in percentage by mass into the pre-sintered powder after the grinding balls obtained in the S4, granulating, sieving by a 40-mesh sieve to obtain spherical powder substances, and maintaining the pressure for 20S under the condition of the one-way pressure of 200MPa to obtain a wafer-shaped ceramic blank; the mass ratio of the 6% polyvinyl alcohol aqueous solution to the pre-sintered powder after ball grinding is 35%:1;
s6, sintering: sintering the disk-shaped ceramic blank obtained in the step S5 to obtain a sintered ceramic blank; the sintering conditions are as follows: firstly, heating from room temperature to 550 ℃ at the heating rate of 3 ℃/min, preserving heat for 3h, then heating to 1300 ℃ at the heating rate of 5 ℃/min, sintering for 2h, and then cooling to room temperature at the cooling rate of 5 ℃/min;
s7, polishing: polishing the upper surface and the lower surface of the sintered ceramic blank obtained in the step S6 by using 600-mesh abrasive paper, polishing the upper surface and the lower surface by using 2000-mesh abrasive paper and carborundum until the thickness is 0.5mm, putting the ceramic blank into deionized water, ultrasonically cleaning and drying the ceramic blank to obtain a polished ceramic blank;
s8, surface metallization: and (4) uniformly coating silver pastes with the thickness of 0.03mm on the upper surface and the lower surface of the polished ceramic blank obtained in the step (S7), preserving the heat for 10min at the temperature of 850 ℃, and naturally cooling to room temperature to obtain the sodium niobate-bismuth magnesium niobate-barium magnesium niobate-strontium titanate transparent medium energy storage ceramic material.
Example 4
The sodium niobate-bismuth magnesium niobate-barium magnesium niobate-strontium titanate transparent medium energy storage ceramic material of the embodiment has a composition formula as follows: 0.95[ 2 ], [0.90NaNbO ] 3 -0.10(0.75Bi(Mg 2/3 Nb 1/3 )O 3 -0.25Ba(Mg 1/3 Nb 2/3 )O 3 )]-0.05SrTiO 3 。
The embodiment also provides a method for preparing the sodium niobate-bismuth magnesium niobate-barium magnesium niobate-strontium titanate transparent medium energy storage ceramic material, which comprises the following steps:
s1, drying materials: respectively adding Na 2 CO 3 Raw material, bi 2 O 3 Raw Material, baCO 3 Raw material and SrCO 3 Drying the raw materials for 6h at 300 ℃ respectively;
mixing Nb with 2 O 5 Raw material, tiO 2 Respectively drying the raw material and the MgO raw material for 4 hours in strips at the temperature of 900 ℃;
the Na is 2 CO 3 The purity of the raw material is 99.8 percent, and the Bi is 2 O 3 The purity of the raw material is 99.8 percent, and the BaCO is 3 The purity of the raw material is 99 percent, and the SrCO 3 The purity of the raw material is 99 percent, and the Nb is 2 O 5 The purity of (2) is 99.5%, the purity of the MgO raw material is 98.5%, and the MgO raw material is purchased from national medicine group chemical reagent limited company;
s2, preparing materials: drying the dried Na in the S1 2 CO 3 Raw material, bi 2 O 3 Raw material, baCO 3 Raw material SrCO 3 Raw material, nb 2 O 5 Raw material, tiO 2 The raw material and MgO raw material are in accordance with 0.95[ 2 ], [0.90NaNbO ] 3 -0.10(0.75Bi(Mg 2/3 Nb 1/3 )O 3 -0.25Ba(Mg 1/ 3 Nb 2/3 )O 3 )]-0.05SrTiO 3 Respectively weighing the stoichiometric ratio of (A), namely weighing the dried Na 2 CO 3 5.1290g of raw material and Bi 2 O 3 Feedstock 1.8942g, baCO 3 0.5348g raw material, srCO 3 Raw materials 0.8423g, nb 2 O 5 13.4990g raw material, tiO 2 0.4604g of raw material and 0.2562g of MgO raw material are uniformly mixed to obtain a premix, agate balls and absolute ethyl alcohol are added, ball milling is carried out for 7h at the speed of 300r/min, after the agate balls are separated, drying is carried out for 15h at the temperature of 90 ℃, and after grinding, sieving is carried out by a 120-mesh sieve to obtain a raw material mixture; the dosage ratio of the premix, the agate balls and the absolute ethyl alcohol is 0.35g: 0.52mL;
s3, pre-burning: pre-burning the raw material mixture obtained in the step S2 at 880 ℃ for 2h, naturally cooling to room temperature, and grinding to obtain pre-burnt powder;
s4, secondary ball milling: adding agate balls and absolute ethyl alcohol into the pre-sintering powder obtained in the step S3, carrying out ball milling for 9 hours, separating the agate balls, drying at the temperature of 95 ℃ for 15 hours, and sieving with a 180-mesh sieve after grinding to obtain the pre-sintering powder after ball milling; the dosage ratio of the agate balls to the absolute ethyl alcohol added into the pre-sintering powder is 0.30g: 0.40mL;
s5, tabletting, namely adding 6 percent of polyvinyl alcohol aqueous solution into the pre-sintered powder after the grinding balls obtained in the S4, granulating, sieving by a 40-mesh sieve to obtain spherical powder substances, and maintaining the pressure for 30S under the condition of one-way pressure of 180MPa to obtain a wafer-shaped ceramic blank; the mass ratio of the 6% polyvinyl alcohol aqueous solution to the pre-sintered powder after ball grinding is 25%:1;
s6, sintering: sintering the disk-shaped ceramic blank obtained in the step S5 to obtain a sintered ceramic blank; the sintering conditions are as follows: firstly, heating from room temperature to 550 ℃ at the heating rate of 3 ℃/min, preserving heat for 3h, then heating to 1280 ℃ at the heating rate of 3 ℃/min, sintering for 3h, and then cooling to room temperature at the cooling rate of 5 ℃/min;
s7, polishing: polishing the upper surface and the lower surface of the sintered ceramic blank obtained in the step S6 by using 600-mesh abrasive paper, polishing the upper surface and the lower surface by using 2000-mesh abrasive paper and carborundum until the thickness is 0.4mm, putting the ceramic blank into deionized water, ultrasonically cleaning and drying the ceramic blank to obtain a polished ceramic blank;
s8, surface metallization: and (4) uniformly coating silver pastes with the thickness of 0.02mm on the upper surface and the lower surface of the polished ceramic blank obtained in the step (S7), preserving the heat for 10min at the temperature of 850 ℃, and naturally cooling to room temperature to obtain the sodium niobate-bismuth magnesium niobate-barium magnesium niobate-strontium titanate transparent medium energy storage ceramic material.
As can be seen from FIG. 1, the ceramic materials prepared in examples 1 to 4 are all pure perovskite structures. As can be seen from FIG. 2, the ceramic materials prepared in examples 1 to 4 have uniform grain size and dense particle distribution. As can be seen from FIGS. 3 and 4, the breakdown field strengths of the ceramic materials prepared in examples 1 to 4 reached 326Kv/cm,347Kv/cm,424Kv/cm and 372Kv/cm, respectively, where 0.95[0.90NaNbO ] prepared in example 3 3 -0.10(0.80Bi(Mg 2/3 Nb 1/3 )O 3 -0.20Ba(Mg 1/3 Nb 2/3 )O 3 )]-0.05SrTiO 3 The ceramic material has the best energy storage performance, and the maximum polarization intensity (Pmax) is 27.56 mu C/cm 2 Residual polarization intensity (Pr) of 0.92. Mu.C/cm 2 Energy storage Density (W) rec ) Reaching 4.49J/cm 3 The energy storage efficiency (eta) reaches 87 percent. As can be seen from FIGS. 5 and 6, 0.95[ 2 ] 0.90NaNbO prepared in example 3 3 -0.10(0.80Bi(Mg 2/3 Nb 1/3 )O 3 -0.20Ba(Mg 1/3 Nb 2/3 )O 3 )]-0.05SrTiO 3 The ceramic material has excellent energy storage performance, temperature stability and frequency stability, and the change value of the energy storage density Wrec in the temperature range of 25-175 DEG C<17% of the total weight of the composition, and the variation value is within the range of 1-300Hz<2 percent. As can be seen from fig. 7, the ceramic material prepared in example 3 exhibits a certain light transmittance, which can reach 50.60% in the near infrared region.
Meanwhile, the light transmittance of the ceramic materials prepared in example 1, example 2 and example 4 in the near infrared region is 48.90%, 47.80% and 49.80%, respectively
Therefore, the sodium niobate-bismuth magnesium niobate-barium magnesium niobate-strontium titanate transparent dielectric energy storage ceramic material prepared in the embodiments 1 to 4 has light transmittance, and can be used for preparing a transparent pulse capacitor, compared with the common methods of hot-pressing sintering, hot isostatic pressing sintering, vacuum sintering, microwave sintering and the like in the conventional transparent ceramic preparation, the preparation method adopts common normal-pressure sintering, no sintering aid is required to be added, the production process is simple, the cost is low, economy and energy conservation are realized, the purity of the obtained ceramic material is high, the capacitor prepared by the material overcomes the defect that the conventional pulse capacitor can not simultaneously meet the requirements of high light transmittance and high energy storage density, and the material has huge application potential and economic benefit in the fields of transparent electronic equipment, such as electronic readers, smart phones, touch screens and the like.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention in any way. Any simple modification, change and equivalent changes of the above embodiments according to the technical essence of the invention are still within the protection scope of the technical solution of the invention.
Claims (6)
1. The sodium niobate-bismuth magnesium niobate-barium magnesium niobate-strontium titanate transparent medium energy storage ceramic material is characterized by comprising the following components in percentage by weight: 0.95[ 2 ], [0.90NaNbO ] 3 -0.10((1-x)Bi(Mg 2/3 Nb 1/3 )O 3 -xBa(Mg 1/3 Nb 2/3 )O 3 )]-0.05SrTiO 3 Wherein x is mole percentage, and x is more than or equal to 0.10 and less than or equal to 0.25.
2. A method for preparing the sodium niobate-bismuth magnesium niobate-barium magnesium niobate-strontium titanate transparent medium energy storage ceramic material of claim 1, which comprises the following steps:
s1, drying materials: respectively adding Na 2 CO 3 Raw material, bi 2 O 3 Raw material, baCO 3 Raw material and SrCO 3 Drying the raw materials respectively at 300 ℃ for 6h;
mixing Nb with 2 O 5 Raw Material, tiO 2 Respectively drying the raw material and the MgO raw material for 4 hours in strips at the temperature of 900 ℃;
the Na is 2 CO 3 The purity of the raw material is 99.8 percent, and the Bi is 2 O 3 The purity of the raw material is 99.8 percent, and the BaCO is 3 The purity of the raw material is 99 percent, and the SrCO 3 The purity of the raw material is 99 percent, and the Nb is 2 O 5 The purity of the MgO raw material is 99.5 percent, and the purity of the MgO raw material is 98.5 percent;
s2, preparing materials: drying the dried Na in the S1 2 CO 3 Raw material, bi 2 O 3 Raw material, baCO 3 Raw material SrCO 3 Raw material, nb 2 O 5 Raw material, tiO 2 The raw material and MgO raw material are in accordance with 0.95[ 2 ], [0.90NaNbO ] 3 -0.10((1-x)Bi(Mg 2/3 Nb 1/3 )O 3 -x Ba(Mg 1/3 Nb 2/3 )O 3 )]-0.05SrTiO 3 The chemical metering ratios are respectively weighed and uniformly mixed to obtain premix, agate balls and absolute ethyl alcohol are added, ball milling is carried out for 6-10 h, after the agate balls are separated, drying is carried out for 12-24 h at the temperature of 80-100 ℃, and after grinding, a 120-mesh sieve is sieved to obtain a raw material mixture;
s3, pre-burning: pre-burning the raw material mixture obtained in the step S2 for 2 to 4 hours at the temperature of 850 to 950 ℃, naturally cooling to room temperature, and grinding to obtain pre-burnt powder;
s4, secondary ball milling: adding agate balls and absolute ethyl alcohol into the pre-sintering powder obtained in the step S3, performing ball milling for 6-10 h, separating the agate balls, drying at the temperature of 80-100 ℃ for 12-24 h, and sieving with a 180-mesh sieve after grinding to obtain pre-sintering powder after ball milling;
s5, tabletting, namely adding 6% polyvinyl alcohol aqueous solution in mass percentage into the pre-sintered powder after the grinding balls obtained in the S4, granulating, sieving by a 40-mesh sieve to obtain spherical powder substances, and maintaining the pressure for 20-60S under the condition of the unidirectional pressure of 150-200 MPa to obtain a wafer-shaped ceramic blank;
s6, sintering: sintering the disk-shaped ceramic blank obtained in the step S5 to obtain a sintered ceramic blank; the sintering conditions are as follows: firstly, heating up to 550 ℃ from room temperature at a heating rate of 3 ℃/min, keeping the temperature for 3h, then heating up to 1230-1300 ℃ at a heating rate of 3-5 ℃/min, sintering for 2-4 h, and then cooling to room temperature at a cooling rate of 5 ℃/min;
s7, polishing: polishing the upper surface and the lower surface of the sintered ceramic body obtained in the step S6 by using 600-mesh abrasive paper, polishing the upper surface and the lower surface by using 2000-mesh abrasive paper and diamond grains until the thickness of the sintered ceramic body is 0.3-0.5 mm, putting the sintered ceramic body into deionized water, ultrasonically cleaning and drying the polished ceramic body to obtain a polished ceramic body;
s8, surface metallization: and (4) uniformly coating silver pastes with the thickness of 0.01-0.03 mm on the upper surface and the lower surface of the polished ceramic blank obtained in the step (S7), preserving the heat for 10min at the temperature of 850 ℃, and naturally cooling to room temperature to obtain the sodium niobate-bismuth magnesium niobate-barium magnesium niobate-strontium titanate transparent medium energy storage ceramic material.
3. The method according to claim 2, wherein the premix, the agate balls and the absolute ethyl alcohol in the S2 are used in a ratio of 0.35g: 0.52mL.
4. The method according to claim 2, characterized in that the amount ratio of the agate balls to the absolute ethyl alcohol added to the pre-sintering powder of S4 is 0.30g: 0.40mL.
5. The method according to claim 2, wherein the mass ratio of the 6% polyvinyl alcohol aqueous solution to the pre-sintered powder after ball milling in S5 is (25-35%): 1.
6. the application of the sodium niobate-bismuth magnesium niobate-barium magnesium niobate-strontium titanate transparent medium energy storage ceramic material prepared according to any one of claims 2 to 5, wherein the sodium niobate-bismuth magnesium niobate-barium magnesium niobate-strontium titanate transparent medium energy storage ceramic material has light transmittance and is used for preparing transparent pulse capacitors.
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