CN109574656A - A kind of high energy storage bismuth-sodium titanate-strontium titanate base dielectric material and preparation method thereof - Google Patents

A kind of high energy storage bismuth-sodium titanate-strontium titanate base dielectric material and preparation method thereof Download PDF

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CN109574656A
CN109574656A CN201811533879.0A CN201811533879A CN109574656A CN 109574656 A CN109574656 A CN 109574656A CN 201811533879 A CN201811533879 A CN 201811533879A CN 109574656 A CN109574656 A CN 109574656A
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bismuth
energy storage
dielectric material
high energy
strontium titanate
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刘韩星
黄宁
郝华
谢鹃
曹明贺
尧中华
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Wuhan University of Technology WUT
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Abstract

The invention discloses a kind of high energy storage bismuth-sodium titanate based dielectric material, the chemical formula of the material is 0.5Bi0.5Na0.5TiO3‑0.5SrTiO3- x wt%MgO, wherein x=0.5~3.0, comprising the following steps: with SrCO3、TiO2、Bi2O3、Na2CO3, MgO be that raw material according to chemical formula dose ratio ingredient prepares ceramic powder, then ball milling, drying, granulation, and ceramic green is compressed into using tablet press machine；Again by green compact in Muffle furnace dumping, be sintered in Muffle furnace later, obtain ceramics sample.Preparation process of the present invention is simple, at low cost, pollution-free, and prepared energy-storing dielectric ceramic material has 1.61~2.17J/cm of high discharge energy-storage density3With higher 137~226kV/cm of breakdown strength.

Description

A kind of high energy storage bismuth-sodium titanate-strontium titanate base dielectric material and preparation method thereof
Technical field
The present invention relates to the technical field of ceramic material for being applied to electronic component, and in particular to a kind of high energy storage bismuth titanates Sodium-strontium titanate base dielectric material and preparation method thereof.
Background technique
The high power of pulse power system and miniaturization need to develop the energy storage dielectric haveing excellent performance as member Device, this is just needed, and the dielectric constant of material is big, dielectric loss is low and disruptive field intensity is high, to make the energy storage density of device High, energy storage efficiency height.For BNT base relaxation ferroelectric, directric relaxation behavior be all as caused by the thermal evolution process of PNRs, To make BNT possess higher polarizability, while the remanent polarization of BNT, coercive field strength are larger, can substantially meet storage The requirement of energy dielectric ceramics.But BNT haves the shortcomings that compressive resistance is not generally high, causes its energy-storage property bad.
Be all that the ST ceramics of perovskite structure possess higher breakdown strength, and have before scholar's studies have shown that cube The ST of phase can be completely dissolved into the BNT of tripartite's phase by way of solid solution, increase the dielectric constant of BNT, under Curie temperature Drop, and Jie Wen Feng broadens therewith.Also studies have found that ST can improve the breakdown voltage of BNT, so that it is close to further increase its energy storage Degree.In addition, can reduce its sintering temperature after thering is scholar to find MgO doping BNT, increase the consistency of system.
Summary of the invention
The technical problem to be solved by the present invention is to provide a kind of high energy storage in view of the deficiency of the prior art Bismuth-sodium titanate-strontium titanate base dielectric material and preparation method thereof, resulting energy-storing dielectric ceramic have the spy high pressure resistant, energy storage is high Point.
The present invention be solve the problems, such as it is set forth above used by technical solution are as follows:
A kind of high energy storage bismuth-sodium titanate-strontium titanate base dielectric material, chemical composition expression formula are 0.5Bi0.5Na0.5TiO3-0.5SrTiO3- x wt%MgO, wherein x=0.5~3.0.
The discharge energy-storage density of above-mentioned high energy storage bismuth-sodium titanate-strontium titanate base dielectric material is in 1.61~2.17J/cm3Model In enclosing, breakdown strength (i.e. maximum field intensity) is within the scope of 137~226kV/cm.
Preferably, above-mentioned high energy storage bismuth-sodium titanate-strontium titanate base dielectric material, chemical composition expression formula are 0.5Bi0.5Na0.5TiO3-0.5SrTiO3- x wt%MgO, x=1.5~3.0, discharge energy-storage density is in 1.90~2.17J/cm3 In range, breakdown strength is within the scope of 176.97~226.03kV/cm.
The preparation method of above-mentioned high energy storage bismuth-sodium titanate-strontium titanate base dielectric material, key step are as follows:
(1) with SrCO3、TiO2As raw material, according to SrTiO3Chemical composition expression formula in metallic element stoichiometry Than ingredient, ingredient A is obtained；With TiO2、Bi2O3、Na2CO3As raw material, according to Bi0.5Na0.5TiO3Chemical composition expression formula in The stoichiometric ratio ingredient of metallic element, obtains ingredient B；
(2) by the weighed ingredient A mixing and ball milling of step (1), drying, pre-burning, ST ceramic powder is obtained；Step (1) is claimed The ingredient B mixing and ball milling that takes, drying, pre-burning, obtain BNT ceramic powder；
(3) by the resulting BNT ceramic powder of step (2), ST ceramic powder and MgO according to chemical composition expression formula 0.5Bi0.5Na0.5TiO3-0.5SrTiO3The stoichiometric ratio ingredient of metallic element in-x wt%MgO, wherein x=0.5~3.0, Then common mixing and ball milling, and dry, obtain hybrid ceramic powder；
(4) the resulting hybrid ceramic powder of step (3) is uniformly mixed with binder, and grinds granulation, be sieved, dry-pressing at Type obtains ceramic green；
(5) it will be sintered 2~3 hours after ceramic green dumping that step (4) obtains being warming up to 1100~1200 DEG C, obtain High energy storage bismuth-sodium titanate-strontium titanate base dielectric material.
According to the above scheme, the pre-burning of ingredient A is to be warming up to 1100 with the heating rate of 1~3 DEG C/min in the step (2) ~1200 DEG C, keep the temperature 1~3 hour；The pre-burning of ingredient B is that 800~900 DEG C are warming up to the heating rate of 1~3 DEG C/min, is protected Temperature 1~3 hour.
According to the above scheme, the ball milling in step (2) and step (3) is to use zirconia ball and dehydrated alcohol as medium, is set It is carried out in ball grinder horizontal ball milling 20-24 hours；Drying in step (2) and step (3) is to keep the temperature 24 at 80~100 DEG C ~36 hours.
According to the above scheme, in step (4), the binder is polyvinyl alcohol water solution, and concentration is 4~5wt%, is added Enter 2~4% that amount is ceramic powder quality；The sieving was 60~120 meshes；The dry-pressing formed pressure size For 150~200MPa.
According to the above scheme, in step (5), the dumping is to be warming up to 600 with the heating rate of 0.5~1.5 DEG C/min DEG C heat preservation 1~3 hour, polyvinyl alcohol is discharged；The sintering is to be warming up at room temperature with the heating rate of 2~4 DEG C/min It 1000 DEG C, is then warming up at 1100~1200 DEG C with the heating rate of 1~3 DEG C/min and keeps the temperature 2~3 hours, it is naturally cold with furnace But.
Compared with prior art, the beneficial effects of the present invention are:
1, dielectric material of the present invention has good energy storage characteristic, by Bi0.5Na0.5TiO3Middle addition SrTiO3 0.5Bi is formd with MgO0.5Na0.5TiO3-0.5SrTiO3- x wt%MgO solid solution, wherein x=0.5~3.0, the system Breakdown strength (within the scope of 137~226kV/cm) and discharge energy-storage density are (in 1.61~2.17J/cm3In range) it is all significant It improves；Wherein, in x=2.0, breakdown strength increases to 226.03kV/cm, and discharge energy-storage density is up to 2.02J/cm3, in x= Energy storage density reaches 2.17J/cm when 3.03；
2, the selected pre-burning system of the present invention is not common first by pre-burning together after the mixing of all raw materials, but first Ingredient is distinguished according to the chemical composition of ST and BNT, then by the two pre-burning at different temperature respectively, this is because the pre-burning of ST Temperature range is 1100 DEG C~1500 DEG C, and the calcined temperature range of BNT is 800~900 DEG C, the calcined temperature of the two difference compared with Greatly.If direct mixing pre-burning will lead to the volatilization of Bi and Na, make ceramic generation if calcined temperature is higher than the calcined temperature of BNT Defect；If calcined temperature is lower than the calcined temperature of ST, the generation of ST is influenced, influence is synthetically produced on ceramics.Therefore it is of the invention Using pre-burning respectively, it is avoided that the above problem, obtains required ceramic material.
3, rare earth element and precious metal element are free of in the raw materials used in the present invention, cost is relatively low；And lead is free of in raw material, it is green Colour circle is protected；In the preparation process of dielectric material, sintering temperature is lower, is lower than 1300 DEG C, is conducive to energy-saving and emission-reduction.
Detailed description of the invention
Fig. 1 is the XRD diagram of high energy storage bismuth-sodium titanate-strontium titanate base dielectric material prepared by the embodiment of the present invention 1~5 Spectrum；
Fig. 2 is the SEM figure of high energy storage bismuth-sodium titanate-strontium titanate base dielectric material prepared by Examples 1 to 5；
Fig. 3 is that high energy storage bismuth-sodium titanate-strontium titanate base dielectric material prepared by Examples 1 to 5 is situated between under 1kHz frequency Electric constant variation with temperature figure (25~500 DEG C)；
Fig. 4 is high energy storage bismuth-sodium titanate-strontium titanate base dielectric material prepared by Examples 1 to 5 under 10Hz frequency P-E curve graph.
Specific embodiment
Technical solution in order to enable those skilled in the art to better understand the present invention, with reference to the accompanying drawing to the present invention make into One step detailed description.
The embodiment of the present invention provides a series of high energy storage bismuth-sodium titanate-strontium titanate base dielectric materials, chemical composition expression Formula is 0.5Bi0.5Na0.5TiO3-0.5SrTiO3- x wt%MgO, wherein x=0.5~3.0.
Embodiment 1
A kind of high energy storage bismuth-sodium titanate-strontium titanate base dielectric material, chemical composition expression formula are 0.5Bi0.5Na0.5TiO3-0.5SrTiO3- 0.5wt%MgO, preparation method specifically includes the following steps:
(1) according to composition expression formula, 0.5mol SrCO is weighed3、0.5mol TiO2As preparation SrTiO3Raw material A；Claim Take 0.5mol TiO2、0.125mol Bi2O3With 0.125mol Na2CO3As preparation Bi0.5Na0.5TiO3Raw material B；
(2) weighed raw material A is put into ball grinder, using zirconia ball and dehydrated alcohol as medium, in horizontal mill Upper ball milling 24 hours；Then dried at 100 DEG C and carry out pre-burning afterwards for 24 hours, calcined temperature be 1150 DEG C, burn-in process be with 2 DEG C/ The heating rate of min keeps the temperature 2h from room temperature to required calcined temperature, later with furnace natural cooling, obtains ST ceramic powder Body；
Weighed raw material B is put into ball grinder, using zirconia ball and dehydrated alcohol as medium, the ball in horizontal mill Mill 24 hours；It is then dried at 100 DEG C and carries out pre-burning afterwards for 24 hours, calcined temperature is 850 DEG C, and burn-in process is with 2 DEG C/min Heating rate keeps the temperature 2h from room temperature to required calcined temperature, later with furnace natural cooling, obtains BNT ceramic powder；
(3) by BNT ceramic powder, ST ceramic powder and MgO powder according to 0.5Bi0.5Na0.5TiO3-0.5SrTiO3- The chemical expression of 0.5wt%MgO mixes, and is put into ball grinder, using zirconia ball and dehydrated alcohol as medium, is placed in ball milling Ball milling 24 hours in tank then dry for 24 hours again through 100 DEG C, obtain hybrid ceramic powder；
(4) polyvinyl alcohol water solution that concentration is 5wt% is added in the hybrid ceramic powder obtained by step (3), wherein gathering The additional amount of vinyl alcohol aqueous solution is the 4% of ceramic powder quality, is then mixed, and is granulated, sieves with 100 mesh sieve, after taking sieving Uniformed powder particle, then with tablet press machine that its is dry-pressing formed, briquetting pressure 150MPa obtains the round pottery that diameter is 12mm Porcelain green compact；
(5) obtained ceramic green to 600 DEG C and is protected with the heating rate of 1 DEG C/min from room temperature in Muffle furnace Temperature 2 hours, with furnace natural cooling, polyvinyl alcohol is discharged；1000 are warming up to the heating rate of 3 DEG C/min in Muffle furnace again DEG C, 1200 DEG C then are warming up to the heating rate of 2 DEG C/min, and keep the temperature 2 hours, later with furnace natural cooling, obtain high storage It can bismuth-sodium titanate-strontium titanate base dielectric material.
High energy storage bismuth-sodium titanate prepared by embodiment 1-strontium titanate base dielectric material is carried out X-ray diffraction (XRD) to survey Examination, XRD spectrum is as shown in Figure 1, can be seen that the ceramic material shows pure perovskite structure by XRD spectrum, the second phase of nothing is in Cube phase structure.
High energy storage bismuth-sodium titanate-strontium titanate base media ceramic surface prepared by embodiment 1 is shot into SEM image, such as Shown in Fig. 2, amplification factor is 5000 times, and grain development is good, dense micro-structure, and crystal grain diameter is all between 2~3 μm.
High energy storage bismuth-sodium titanate-strontium titanate base media ceramic both ends prepared by embodiment 1 are polished and polished, silver-colored Electrode tests dielectric properties and energy-storage property.As shown in figure 3, the bismuth-sodium titanate-strontium titanate base media ceramic is in frequency 1kHz, 10kHz, 100kHz, 1MHz, dielectric constant is 3000 or more at 25 DEG C of temperature.
As shown in figure 4, maximum field intensity of the energy-storing dielectric ceramic under 10Hz frequency is 137.63kV/cm, it is maximum Polarization intensity is 32.10 μ C/cm2, according to formulaWithCalculating separately out should Charging energy-storing density, discharge energy-storage density and the energy storage efficiency of energy-storing dielectric ceramic are 1.73J/cm3、1.42J/cm3With 82.0%.
Embodiment 2
A kind of high energy storage bismuth-sodium titanate-strontium titanate base dielectric material, chemical composition expression formula are 0.5Bi0.5Na0.5TiO3-0.5SrTiO3- 1.0wt%MgO, preparation method specifically includes the following steps:
(1) according to composition expression formula, 0.5mol SrCO is weighed3、0.5mol TiO2As preparation SrTiO3Raw material A；Claim Take 0.5mol TiO2、0.125mol Bi2O3With 0.125mol Na2CO3As preparation Bi0.5Na0.5TiO3Raw material B；
(2) weighed raw material A is put into ball grinder, using zirconia ball and dehydrated alcohol as medium, in horizontal mill Upper ball milling 24 hours；Then dried at 100 DEG C and carry out pre-burning afterwards for 24 hours, calcined temperature be 1150 DEG C, burn-in process be with 2 DEG C/ The heating rate of min keeps the temperature 2h from room temperature to required calcined temperature, later with furnace natural cooling, obtains ST ceramic powder Body；
Weighed raw material B is put into ball grinder, using zirconia ball and dehydrated alcohol as medium, the ball in horizontal mill Mill 24 hours；It is then dried at 100 DEG C and carries out pre-burning afterwards for 24 hours, calcined temperature is 850 DEG C, and burn-in process is with 2 DEG C/min Heating rate keeps the temperature 2h from room temperature to required calcined temperature, later with furnace natural cooling, obtains BNT ceramic powder；
(3) by BNT ceramic powder, ST ceramic powder and MgO powder according to 0.5Bi0.5Na0.5TiO3-0.5SrTiO3- The chemical expression of 1.0wt%MgO mixes, and is put into ball grinder, using zirconia ball and dehydrated alcohol as medium, is placed in ball milling Ball milling 24 hours in tank then dry for 24 hours again through 100 DEG C, obtain hybrid ceramic powder；
(4) polyvinyl alcohol water solution that concentration is 5wt% is added in the hybrid ceramic powder obtained by step (3), wherein gathering The additional amount of vinyl alcohol aqueous solution is the 4% of ceramic powder quality, is then mixed, and is granulated, sieves with 100 mesh sieve, after taking sieving Uniformed powder particle, then with tablet press machine that its is dry-pressing formed, briquetting pressure 150MPa obtains the round pottery that diameter is 12mm Porcelain green compact；
(5) obtained ceramic green to 600 DEG C and is protected with the heating rate of 1 DEG C/min from room temperature in Muffle furnace Temperature 2 hours, with furnace natural cooling, polyvinyl alcohol is discharged；1000 are warming up to the heating rate of 3 DEG C/min in Muffle furnace again DEG C, 1200 DEG C then are warming up to the heating rate of 2 DEG C/min, and keep the temperature 2 hours, later with furnace natural cooling, obtain high storage It can bismuth-sodium titanate-strontium titanate base dielectric material.
High energy storage bismuth-sodium titanate prepared by embodiment 2-strontium titanate base dielectric material is carried out X-ray diffraction (XRD) to survey Examination, XRD spectrum is as shown in Figure 1, can be seen that the ceramic material shows pure perovskite structure by XRD spectrum, the second phase of nothing is in Cube phase structure.
High energy storage bismuth-sodium titanate-strontium titanate base media ceramic surface prepared by embodiment 2 is shot into SEM image, such as Shown in Fig. 2, amplification factor is 5000 times, and grain development is good, dense micro-structure, and crystal grain diameter is all between 2~3 μm.
High energy storage bismuth-sodium titanate-strontium titanate base media ceramic both ends prepared by embodiment 2 are polished and polished, silver-colored Electrode tests dielectric properties and energy-storage property.As shown in figure 3, the bismuth-sodium titanate-strontium titanate base media ceramic is in frequency 1kHz, 10kHz, 100kHz, 1MHz, dielectric constant is 2500 or more at 25 DEG C of temperature.
As shown in figure 4, maximum field intensity of the energy-storing dielectric ceramic under 10Hz frequency is 137.62kV/cm, it is maximum Polarization intensity is 39.12 μ C/cm2, according to formulaWithCalculating separately out should Charging energy-storing density, discharge energy-storage density and the energy storage efficiency of energy-storing dielectric ceramic are 2.22J/cm3、1.61J/cm3With 72.6%.
Embodiment 3
A kind of high energy storage bismuth-sodium titanate-strontium titanate base dielectric material, chemical composition expression formula are 0.5Bi0.5Na0.5TiO3-0.5SrTiO3- 1.5wt%MgO, preparation method specifically includes the following steps:
(1) according to composition expression formula, 0.5mol SrCO is weighed3、0.5mol TiO2As preparation SrTiO3Raw material A；Claim Take 0.5mol TiO2、0.125mol Bi2O3With 0.125mol Na2CO3As preparation Bi0.5Na0.5TiO3Raw material B；
(2) weighed raw material A is put into ball grinder, using zirconia ball and dehydrated alcohol as medium, in horizontal mill Upper ball milling 24 hours；Then dried at 100 DEG C and carry out pre-burning afterwards for 24 hours, calcined temperature be 1150 DEG C, burn-in process be with 2 DEG C/ The heating rate of min keeps the temperature 2h from room temperature to required calcined temperature, later with furnace natural cooling, obtains ST ceramic powder Body；
Weighed raw material B is put into ball grinder, using zirconia ball and dehydrated alcohol as medium, the ball in horizontal mill Mill 24 hours；It is then dried at 100 DEG C and carries out pre-burning afterwards for 24 hours, calcined temperature is 850 DEG C, and burn-in process is with 2 DEG C/min Heating rate keeps the temperature 2h from room temperature to required calcined temperature, later with furnace natural cooling, obtains BNT ceramic powder；
(3) by BNT ceramic powder, ST ceramic powder and MgO powder according to 0.5Bi0.5Na0.5TiO3-0.5SrTiO3- The chemical expression of 1.5wt%MgO mixes, and is put into ball grinder, using zirconia ball and dehydrated alcohol as medium, is placed in ball milling Ball milling 24 hours in tank then dry for 24 hours again through 100 DEG C, obtain hybrid ceramic powder；
(4) polyvinyl alcohol water solution that concentration is 5wt% is added in the hybrid ceramic powder obtained by step (3), wherein gathering The additional amount of vinyl alcohol aqueous solution is the 4% of ceramic powder quality, is then mixed, and is granulated, sieves with 100 mesh sieve, after taking sieving Uniformed powder particle, then with tablet press machine that its is dry-pressing formed, briquetting pressure 150MPa obtains the round pottery that diameter is 12mm Porcelain green compact；
(5) obtained ceramic green to 600 DEG C and is protected with the heating rate of 1 DEG C/min from room temperature in Muffle furnace Temperature 2 hours, with furnace natural cooling, polyvinyl alcohol is discharged；1000 are warming up to the heating rate of 3 DEG C/min in Muffle furnace again DEG C, 1200 DEG C then are warming up to the heating rate of 2 DEG C/min, and keep the temperature 2 hours, later with furnace natural cooling, obtain high storage It can bismuth-sodium titanate-strontium titanate base dielectric material.
High energy storage bismuth-sodium titanate prepared by embodiment 3-strontium titanate base dielectric material is carried out X-ray diffraction (XRD) to survey Examination, XRD spectrum is as shown in Figure 1, can be seen that the ceramic material shows pure perovskite structure by XRD spectrum, the second phase of nothing is in Cube phase structure.
High energy storage bismuth-sodium titanate-strontium titanate base media ceramic surface prepared by embodiment 3 is shot into SEM image, such as Shown in Fig. 2, amplification factor is 5000 times, and grain development is good, dense micro-structure, and crystal grain diameter is all between 2~3 μm.
High energy storage bismuth-sodium titanate-strontium titanate base media ceramic both ends prepared by embodiment 3 are polished and polished, silver-colored Electrode tests dielectric properties and energy-storage property.As shown in figure 3, the bismuth-sodium titanate-strontium titanate base media ceramic is in frequency 1kHz, 10kHz, 100kHz, 1MHz, dielectric constant is 2500 or more at 25 DEG C of temperature.
As shown in figure 4, maximum field intensity of the energy-storing dielectric ceramic under 10Hz frequency is 176.97kV/cm, it is maximum Polarization intensity is 42.57 μ C/cm2, according to formulaWithCalculating separately out should Charging energy-storing density, discharge energy-storage density and the energy storage efficiency of energy-storing dielectric ceramic are 3.69J/cm3、1.90J/cm3With 51.5%.
Embodiment 4
This example provides a kind of preparation method of high energy storage bismuth-sodium titanate-strontium titanate base dielectric material, chemical composition table It is 0.5Bi up to formula0.5Na0.5TiO3-0.5SrTiO3- 2.0wt%MgO, preparation method difference from example 1 is that: By BNT ceramic powder, ST ceramic powder and MgO powder according to 0.5Bi0.5Na0.5TiO3-0.5SrTiO3- 2.0wt%MgO's Chemical expression mixing, is put into ball grinder, using zirconia ball and dehydrated alcohol as medium, it is small to be placed in ball milling 24 in ball grinder When, it is then dried for 24 hours through 100 DEG C again, obtains hybrid ceramic powder.
High energy storage bismuth-sodium titanate prepared by embodiment 4-strontium titanate base dielectric material is carried out X-ray diffraction (XRD) to survey Examination, XRD spectrum is as shown in Figure 1, can be seen that the ceramic material shows pure perovskite structure by XRD spectrum, the second phase of nothing is in Cube phase structure.
High energy storage bismuth-sodium titanate-strontium titanate base media ceramic surface prepared by embodiment 4 is shot into SEM image, such as Shown in Fig. 2, amplification factor is 5000 times, and grain development is good, dense micro-structure, and crystal grain diameter is all between 2~3 μm.
High energy storage bismuth-sodium titanate-strontium titanate base media ceramic both ends prepared by embodiment 4 are polished and polished, silver-colored Electrode tests dielectric properties and energy-storage property.As shown in figure 3, the bismuth-sodium titanate-strontium titanate base media ceramic is in frequency 1kHz, 10kHz, 100kHz, 1MHz, dielectric constant is 2000 or more at 25 DEG C of temperature.
As shown in figure 4, maximum field intensity of the energy-storing dielectric ceramic under 10Hz frequency is 226.03kV/cm, it is maximum Polarization intensity is 42.9 μ C/cm2, according to formulaWithCalculate separately out the storage Charging energy-storing density, discharge energy-storage density and the energy storage efficiency of energy media ceramic are 4.23J/cm3、2.02J/cm3With 47.7%.
Embodiment 5
This example provides a kind of preparation method of high energy storage bismuth-sodium titanate-strontium titanate base dielectric material, chemical composition table It is 0.5Bi up to formula0.5Na0.5TiO3-0.5SrTiO3- 3.0wt%MgO, preparation method difference from example 1 is that: By BNT ceramic powder, ST ceramic powder and MgO powder according to 0.5Bi0.5Na0.5TiO3-0.5SrTiO3- 3.0wt%MgO's Chemical expression mixing, is put into ball grinder, using zirconia ball and dehydrated alcohol as medium, it is small to be placed in ball milling 24 in ball grinder When, it is then dried for 24 hours through 100 DEG C again, obtains hybrid ceramic powder.
High energy storage bismuth-sodium titanate prepared by embodiment 5-strontium titanate base dielectric material is carried out X-ray diffraction (XRD) to survey Examination, XRD spectrum is as shown in Figure 1, can be seen that the ceramic material shows pure perovskite structure by XRD spectrum, the second phase of nothing is in Cube phase structure.
High energy storage bismuth-sodium titanate-strontium titanate base media ceramic surface prepared by embodiment 5 is shot into SEM image, such as Shown in Fig. 2, amplification factor is 5000 times, and grain development is good, dense micro-structure, and crystal grain diameter is all between 2~3 μm.
High energy storage bismuth-sodium titanate-strontium titanate base media ceramic both ends prepared by embodiment 5 are polished and polished, silver-colored Electrode tests dielectric properties and energy-storage property.As shown in figure 3, the bismuth-sodium titanate-strontium titanate base media ceramic is in frequency 1kHz, 10kHz, 100kHz, 1MHz, dielectric constant is 2000 or more at 25 DEG C of temperature.
As shown in figure 4, maximum field intensity of the energy-storing dielectric ceramic under 10Hz frequency is 196.66kV/cm, it is maximum Polarization intensity is 47.58 μ C/cm2, according to formulaWithCalculating separately out should Charging energy-storing density, discharge energy-storage density and the energy storage efficiency of energy-storing dielectric ceramic are 4.66J/cm3、2.17J/cm3With 46.6%.
High energy storage bismuth-sodium titanate-strontium titanate base dielectric material prepared by each embodiment is specifically listed in table 1 in 10Hz The energy-storage property of 25 DEG C of lower room temperature.
Table 1
Table 1 and Fig. 4 it is found that with MgO incorporation x increase, bismuth-sodium titanate-strontium titanate base media ceramic maximum field Intensity and discharge energy-storage density gradually increase, and energy storage efficiency is gradually reduced；MgO incorporation x=0.5~3.0, the system hit Intensity (within the scope of 137~226kV/cm) and discharge energy-storage density are worn (in 1.61~2.17J/cm3In range) both relative to BNT-ST ceramics (breakdown strength 110kV/cm, energy storage density 1.06J/cm undoped with MgO3) significantly improve；Especially in x= When 2.0, breakdown strength increases to 226.03kV/cm, and discharge energy-storage density is up to 2.02J/cm3, the energy storage density in x=3.0 Reach 2.17J/cm3。
Embodiment 6
The present embodiment difference from example 1 is that: the pre-burning of ingredient A is with 3 DEG C/min in the step (2) Heating rate is warming up to 1200 DEG C, keeps the temperature 2 hours；The pre-burning of ingredient B is that 800 DEG C are warming up to the heating rate of 3 DEG C/min, is protected Temperature 2 hours.
Embodiment 7
The present embodiment difference from example 1 is that: the ball milling in step (2) and step (3) is to use zirconia ball With dehydrated alcohol as medium, it is placed in ball grinder and carries out horizontal ball milling 20 hours；Drying in step (2) and step (3) is 30 hours are kept the temperature at 80 DEG C.
Embodiment 8
The present embodiment difference from example 1 is that: according to the above scheme, in step (4), the binder is poly- Vinyl alcohol aqueous solution, concentration 4wt%, additional amount are the 2% of ceramic powder quality；The sieving was 60 meshes；Institute The dry-pressing formed pressure size stated is 200MPa.
Embodiment 9
The present embodiment difference from example 1 is that: in step (5), the dumping is with the liter of 0.5 DEG C/min Warm rate is warming up to 600 DEG C and keeps the temperature 2 hours, polyvinyl alcohol is discharged；The sintering is fast with the heating of 2 DEG C/min at room temperature Rate is warming up to 1000 DEG C, is then warming up at 1100 DEG C with the heating rate of 2 DEG C/min and keeps the temperature 3 hours, with furnace natural cooling.
By above to the detailed description of the embodiment of the present invention, it will be appreciated that, the present invention provides a kind of high energy storage bismuth titanates Sodium-strontium titanate base dielectric material and preparation method thereof solves the problems, such as that ceramics are not high intolerant to breakdown and discharge energy-storage density, Prepared 0.5Bi0.5Na0.5TiO3-0.5SrTiO3- x wt%MgO (x=0.5~3.0) media ceramic disruptive field intensity increases Greatly, so that discharge energy-storage density is improved, up to 1.61~2.17J/cm3。
It is understood that the principle that embodiment of above is intended to be merely illustrative of the present and the exemplary implementation that uses Mode, however the present invention is not limited thereto.For those skilled in the art, essence of the invention is not being departed from In the case where mind and essence, various changes and modifications can be made therein, these variations and modifications are also considered as protection scope of the present invention.

Claims (9)

1. a kind of high energy storage bismuth-sodium titanate-strontium titanate base dielectric material, it is characterised in that its chemical composition expression formula is 0.5Bi0.5Na0.5TiO3-0.5SrTiO3- x wt%MgO, wherein x=0.5~3.0.
2. high energy storage bismuth-sodium titanate-strontium titanate base dielectric material according to claim 1, it is characterised in that its electric discharge storage Energy density is in 1.61~2.17J/cm3In range, breakdown strength is within the scope of 137~226kV/cm.
3. high energy storage bismuth-sodium titanate-strontium titanate base dielectric material according to claim 1, it is characterised in that its chemical group It is 0.5Bi at expression formula0.5Na0.5TiO3-0.5SrTiO3- x wt%MgO, wherein x=1.5~3.0, discharge energy-storage density exist 1.90~2.17J/cm3In range, breakdown strength is within the scope of 176.97~226.03kV/cm.
4. a kind of preparation method of high energy storage bismuth-sodium titanate-strontium titanate base dielectric material, it is characterised in that key step is as follows:
(1) with SrCO3、TiO2As raw material, according to SrTiO3Chemical composition expression formula in the stoichiometric ratio of metallic element match Material, obtains ingredient A；With TiO2、Bi2O3、Na2CO3As raw material, according to Bi0.5Na0.5TiO3Chemical composition expression formula in metal The stoichiometric ratio ingredient of element, obtains ingredient B；
(2) by the weighed ingredient A mixing and ball milling of step (1), drying, pre-burning, ST ceramic powder is obtained；Step (1) is weighed Ingredient B mixing and ball milling, drying, pre-burning, obtain BNT ceramic powder；
(3) by the resulting BNT ceramic powder of step (2), ST ceramic powder and MgO according to chemical composition expression formula 0.5Bi0.5Na0.5TiO3-0.5SrTiO3The stoichiometric ratio ingredient of metallic element in-x wt%MgO, wherein x=0.5~3.0, Then common mixing and ball milling, and dry, obtain hybrid ceramic powder；
(4) the resulting hybrid ceramic powder of step (3) is uniformly mixed with binder, and grinds granulation, be sieved, dry-pressing formed To ceramic green；
(5) it will be sintered 2~3 hours after ceramic green dumping that step (4) obtains being warming up to 1100~1200 DEG C, obtain high storage It can bismuth-sodium titanate-strontium titanate base dielectric material.
5. a kind of preparation method of high energy storage bismuth-sodium titanate-strontium titanate base dielectric material according to claim 4, feature The pre-burning for being ingredient A in the step (2) is that 1100~1200 DEG C are warming up to the heating rate of 1~3 DEG C/min, keeps the temperature 1- 3 hours；The pre-burning of ingredient B is that 800~900 DEG C are warming up to the heating rate of 1~3 DEG C/min, when keeping the temperature 1-3.
6. a kind of preparation method of high energy storage bismuth-sodium titanate-strontium titanate base dielectric material according to claim 4, feature It is that the ball milling in step (2) and step (3) is to use zirconia ball and dehydrated alcohol as medium, is placed in ball grinder and crouches Formula ball milling 20-24 hours；Drying in step (2) and step (3) is to keep the temperature 24~36 hours at 80~100 DEG C.
7. a kind of preparation method of high energy storage bismuth-sodium titanate-strontium titanate base dielectric material according to claim 4, feature It is in step (4), the binder is polyvinyl alcohol water solution, and concentration is 4~5wt%, and additional amount is ceramic powder The 2~4% of quality；The sieving was 60~120 meshes；The dry-pressing formed pressure size is 150~200MPa.
8. a kind of preparation method of high energy storage bismuth-sodium titanate-strontium titanate base dielectric material according to claim 4, feature It is in step (5), the dumping is to be warming up to 600 DEG C with the heating rate of 0.5~1.5 DEG C/min to keep the temperature 1~3 hour, Polyvinyl alcohol is discharged.
9. a kind of preparation method of high energy storage bismuth-sodium titanate-strontium titanate base dielectric material according to claim 4, feature It is in step (5), the sintering is to be warming up to 1000 DEG C at room temperature with the heating rate of 2~4 DEG C/min, then with 1~3 DEG C/heating rate of min is warming up at 1100~1200 DEG C and keeps the temperature 2~3 hours, with furnace natural cooling.
CN201811533879.0A 2018-12-14 2018-12-14 A kind of high energy storage bismuth-sodium titanate-strontium titanate base dielectric material and preparation method thereof Pending CN109574656A (en)

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