CN112919903A - Strontium bismuth titanate-based lead-free ceramic material for high-efficiency capacitor and preparation method thereof - Google Patents
Strontium bismuth titanate-based lead-free ceramic material for high-efficiency capacitor and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a strontium bismuth titanate-based lead-free ceramic material for a high-efficiency capacitor and a preparation method thereof, belonging to the field of electric energy storage materials. Adopts a solid-phase synthesis method to relax the ferroelectric material Sr0.7Bi0.2TiO3Based on that, a certain mole ratio of Nb to Ni aliovalent elements is doped in the B site of the perovskite structure to increase the charge disorder, so as to obtain a novel composite ceramic, the chemical formula of which is (1-x) Sr0.7Bi0.2TiO3‑xBi(Ni2/3Nb1/3)O3Wherein x is more than or equal to 0 and less than or equal to 0.15. The main performance parameter of the energy storage ceramic material obtained by the invention can restore the energy storage density WrecReaches 4.19 to 5.98J/cm3The energy storage efficiency eta is as high as 92.6-98.6%. The method has simple process flow, is suitable for industrial production, and simultaneously meets the current lead-free environment-friendly requirement.
Description
Technical Field
The invention relates to the technical field of functional materials and devices, in particular to a strontium bismuth titanate-based lead-free ceramic material for a high-efficiency capacitor and a preparation method thereof.
Background
At present, the main electrical energy storage devices are batteries, dielectric capacitors, electrochemical capacitors, and the like. These energy storage devices differ significantly in energy density and power density due to their different energy storage mechanisms and charging and discharging processes. In contrast to other energy storage devices, dielectric capacitors can discharge electric energy in a very short period of time (on the order of nanoseconds to microseconds) and generate a large pulse current or voltage, which also makes the dielectric capacitors have a great potential for use in pulsed power electronic systems. Also, unlike electrochemical capacitors and batteries, dielectric capacitors do not involve chemical reactions during charging and discharging, which makes dielectric capacitors have good thermal and chemical stability and can operate in high-voltage environments (hundreds to thousands of volts) for long periods of time.
The dielectric ceramic energy storage material in the dielectric capacitor has the characteristics of high power density, low cost, excellent thermal stability and the like, and is widely applied to high-power systems such as commerce, consumption, medical treatment, military and the like. At present, most of materials used for ceramic capacitors are lead-based ceramics, although the energy storage density is high, the systems contain a large amount of lead elements, which has great harm to human health and environment, and the development of lead-free materials to replace lead-containing system materials is a necessary trend. However, the lead-free dielectric ceramic capacitor has a limitation in that the energy storage density is low and cannot be compared with the energy storage performance of a lead-based ceramic capacitor, which makes it difficult to meet the development requirements of miniaturization, multifunction and integration of devices, thereby limiting its application in portable electronic devices. If the energy storage density of the lead-free dielectric ceramic capacitor can be effectively improved, the lead-free dielectric ceramic capacitor can be more widely applied to the field of energy storage.
The strontium bismuth titanate ceramic inherits the fine hysteresis loop of strontium titanate and uses Bi element to substituteThe method has the advantages that the traditional Pb element is replaced to realize the polarization enhancement effect, the damage to the environment is reduced, particularly, the dielectric property of the strontium bismuth titanate ceramic can be changed by adjusting the proportion of bismuth and strontium so as to meet different practical applications, and the method is considered to have great potential for energy storage application. However, the strontium bismuth titanate ceramic has a small amount of Bi element volatilization phenomenon in the sintering process, so that some oxygen vacancies are generated to cause lower breakdown strength, and the energy storage density of the strontium bismuth titanate ceramic is influenced, which also limits the application of the strontium bismuth titanate ceramic in a high energy storage density capacitor. The energy storage density of most of the strontium titanate bismuth-based ceramics is still low (<4J/cm3) There is a gap compared with the traditional lead-based ceramic material.
Disclosure of Invention
Aiming at the technical defects, the invention aims to provide a strontium bismuth titanate-based lead-free ceramic material for a high-efficiency capacitor and a preparation method thereof, wherein a solid-phase synthesis method is adopted to relax a ferroelectric material Sr0.7Bi0.2TiO3Based on that, a certain mole ratio of Nb to Ni aliovalent elements is doped in the B site of the perovskite structure to increase the charge disorder, so as to obtain a novel composite ceramic, the chemical formula of which is (1-x) Sr0.7Bi0.2TiO3-xBi(Ni2/3Nb1/3)O3Inducing the B site to form a polar nano micro area to obtain a fine electric hysteresis loop with low remanent polarization; the grain size is further reduced by a two-step sintering method, the compactness is improved, the breakdown strength is further improved, the research direction of doping modification is expanded, the sintering process is optimized, and the lead-free energy storage ceramic with application potential is prepared.
The invention can be realized by the following technical scheme:
the chemical composition of the strontium titanate bismuth base lead-free ceramic material for the high-efficiency capacitor is (1-x) Sr0.7Bi0.2TiO3-xBi(Ni2/3Nb1/3)O3Wherein x is more than or equal to 0 and less than or equal to 0.15.
As a preferred embodiment, x is 0.12. This is mainly due to the fact that the component ceramic has a large activation energy and thus a large resistivity, which contributes to the improvement of the breakdown strength. At the same time, the dielectric loss of this component is very small at room temperature, which contributes to the energy storage efficiency of the ceramic.
The strontium bismuth titanate-based lead-free ceramic material for the high-efficiency capacitor is prepared into corresponding energy storage ceramic by using a solid-phase reaction method, and specifically comprises the following steps:
(1) selecting Bi with the purity of more than 98 percent2O3Powder and SrCO3Powder, TiO2Powder, NiO powder and Nb2O5The powder is used as a raw material and is Sr according to a general formula (1-x)0.7Bi0.2TiO3-xBi(Ni2/3Nb1/3)O3Weighing raw materials, wherein x is 0-0.15, adding absolute ethyl alcohol with the same mass as the powder, and uniformly mixing the raw materials and the absolute ethyl alcohol through a primary ball milling process to uniformly mix the powder to form slurry;
(2) placing the slurry in a constant-temperature oven at 90 ℃ for baking, removing absolute ethyl alcohol, and grinding in a mortar to obtain powder;
(3) placing the powder in a mold to be pre-pressed into a material block, pre-burning the material block under the closed condition at the temperature of 900-;
(4) crushing and grinding the pre-synthesized ceramic material block in a mortar to obtain ceramic powder, adding absolute ethyl alcohol with equal mass into the obtained powder, and carrying out secondary ball milling;
(5) drying the obtained slurry at 90 ℃, and performing granulation, sieving and compression molding to obtain a ceramic green body;
(6) carrying out gel removal treatment on the ceramic blank at the temperature of 600-650 ℃ for 5-10h, sintering the ceramic blank after gel removal at the sintering temperature of 1125-1150 ℃, at the heating rate of 2-4 ℃/min and at the heat preservation time of 2-6h, and cooling to room temperature to obtain the strontium bismuth titanate lead-free ceramic material for the high-efficiency capacitor.
Further, absolute ethyl alcohol and ZrO are adopted in the primary ball milling and the secondary ball milling2The ball is used as a ball milling medium, the rotating speed is 250-330r/min, the running direction is adjusted every half hour, and the ball milling time is 12-24 h.
Furthermore, the pre-sintering temperature is preferably 900-.
Furthermore, polyvinyl alcohol (PVA) with the concentration of 8% is used as a binder to be doped into the powder during granulation, the mass of the doped binder is 5-10% of the mass of the powder, the mass of the doped distilled water is 2.5-5% of the mass of the powder, and the powder is uniformly mixed in a mortar and then placed in a die to be pressed into powder blocks.
Furthermore, sieving with 80 mesh and 140 mesh sieve to obtain powder of the middle layer of 80 mesh and 140 mesh sieve.
Further, the pressure at the time of press molding was controlled to 200 MPa.
Furthermore, the heating rate is controlled to be 2-4 ℃/min during ordinary sintering, and the heat preservation time is controlled to be 2-6 h.
Further, the sintering of the ceramic blank after the glue removal in the sixth step is replaced by a two-step sintering method, which specifically comprises the following steps: heating to 950-1000 ℃ at a heating rate of 3-4 ℃/min, then rapidly heating to 1100-1150 ℃ at a heating rate of 8-10 ℃/min, rapidly cooling to 1025-1050 ℃ without heat preservation, and finally performing heat preservation for 10-40h at 1025-1050 ℃.
Compared with the prior art, the (1-x) Sr prepared by the invention0.7Bi0.2TiO3-xBi(Ni2/3Nb1/3)O3The ceramic is doped with Ni and Nb elements in the strontium bismuth titanate ceramic to improve the energy storage characteristic, and the design principle of the ceramic is as follows: the introduction of B-site aliovalent cations greatly improves the resistivity of the ceramic, further enhances the breakdown electric field of the strontium bismuth titanate ceramic, and on the other hand, the B-site cations break the long-range order of dipoles and introduce local random electric fields, so that the residual polarization is reduced and the larger polarization is maintained. And further, by optimizing the two-step sintering process, the grain size is reduced, and the breakdown field strength of the energy storage ceramic is further improved.
Compared with the prior art and energy storage materials, the invention has the following beneficial effects:
(1) the energy storage medium ceramic material provided by the invention realizes high energy storage density and high efficiency, and the releasable energy density is 4.19-5.98J/cm3The efficiency is 92.6-98.6%;
(2) the energy storage dielectric ceramic material provided by the invention has good temperature and frequency stability, and the releasable energy density exceeds 3J/cm under different temperatures and frequencies3Within the temperature range of 25-140 ℃, the change rate of the energy storage density is less than 9 percent, and within the frequency range of 1-200Hz, the change rate of the energy storage density is less than 7 percent;
(3) the energy storage medium ceramic material provided by the invention has excellent charge and discharge behaviors and high discharge power density of 215.94MW/cm3And ultra-short discharge time: (<50ns) and is expected to be applied to high-power pulse dielectric energy storage devices.
(4) The preparation method disclosed by the invention is simple in preparation process, low in preparation cost, good in repeatability, suitable for large-scale industrial production, and expected to be widely applied to pulse power systems such as high-power microwave weapons, laser weapons, electromagnetic emitters and hybrid electric vehicles.
Drawings
FIG. 1 is a scanning electron micrograph of a bismuth strontium titanate-based lead-free ceramic for a high performance capacitor prepared in example 5;
FIG. 2 is a graph showing the dielectric constant and dielectric loss versus temperature of the strontium bismuth titanate-based lead-free ceramic for a high performance capacitor prepared in example 3;
FIG. 3 is a hysteresis loop of a bismuth strontium titanate-based lead-free ceramic for a high efficiency capacitor prepared in example 5;
FIG. 4 is a graph showing the change of energy storage characteristics with electric field of the strontium bismuth titanate-based lead-free ceramic for a high efficiency capacitor prepared in example 5;
FIG. 5 is a graph showing the change of energy storage characteristics with temperature of the strontium bismuth titanate-based lead-free ceramic for a high efficiency capacitor prepared in example 5;
FIG. 6 is a graph showing the energy storage characteristics of the strontium bismuth titanate-based lead-free ceramic for a high efficiency capacitor prepared in example 5 as a function of frequency;
FIG. 7 shows the peak discharge current (I) of the strontium bismuth titanate-based lead-free ceramic for a high performance capacitor prepared in example 3max) Discharge current density (I)maxS) and discharge power density (P)D) Curve with electric field strength.
Detailed Description
The present invention will be further described with reference to the following examples. The following examples will assist those skilled in the art in further understanding the invention, but are not intended to limit the invention in any way. It should be noted that variations and modifications can be made by persons skilled in the art without departing from the spirit of the invention. All falling within the scope of the present invention.
Example 1
The chemical composition of the strontium titanate bismuth-based lead-free ceramic for the high-efficiency capacitor is (1-x) Sr0.7Bi0.2TiO3-xBi(Ni2/3Nb1/3)O3Wherein x is 0, the following steps are specifically adopted:
(1) selecting Bi with the purity of more than 98 percent2O3Powder and SrCO3Powder, TiO2The powder is taken as a raw material and is prepared according to the chemical formula Sr0.7Bi0.2TiO3Weighing raw materials, adding absolute ethyl alcohol with the same mass as that of the powder, and uniformly mixing the raw materials and the absolute ethyl alcohol through a primary ball milling process to uniformly mix the powder to form slurry. Wherein, anhydrous ethanol and ZrO are adopted in the primary ball milling2The ball is used as a ball milling medium, the rotating speed is 250r/min, the running direction is adjusted every half hour, and the ball milling time is 12 hours.
(2) Placing the slurry in a constant-temperature oven at 90 ℃ for baking, removing absolute ethyl alcohol, and grinding in a mortar to obtain powder;
(3) placing the powder in a mould to be pre-pressed into a material block, pre-sintering the material block at 900 ℃ under a closed condition, and keeping the temperature for 2 hours to obtain pre-synthesized ceramic powder;
(4) grinding the pre-synthesized ceramic material block in a mortar to obtain ceramic powder, adding absolute ethyl alcohol with equal mass into the obtained powder, and performing secondary ball milling, wherein the absolute ethyl alcohol and ZrO are still adopted in the process2The ball is used as a ball milling medium, the rotating speed is 250r/min, the running direction is adjusted every half hour, and the ball milling time is 12 hours.
(5) Drying the obtained slurry at 90 ℃, adding 8 wt% of polyvinyl alcohol (PVA) as a binder to be doped into the powder for granulation, crushing the powder blocks obtained by granulation, sieving the powder blocks by using 80-mesh and 140-mesh sieves, taking the powder blocks in the middle layers of the 80-mesh and 140-mesh sieves, and performing compression molding under the pressure of 200Mpa to obtain the ceramic green bodies. Wherein, in the granulation, the mass of the binder to be mixed is 5% of the mass of the powder, and the mass of the distilled water to be mixed is 2.5% of the mass of the powder.
(6) Placing the ceramic blank in a crucible, covering a cover with a gap, carrying out glue discharging treatment at 600 ℃ for 5h, then inverting the crucible on the ceramic blank subjected to glue discharging, carrying out closed sintering at the sintering temperature of 1125 ℃, at the heating rate of 2 ℃/min, keeping the temperature for 2h, and cooling to room temperature to obtain the strontium bismuth titanate-based lead-free ceramic for the high-efficiency capacitor.
The ceramic achieves 4.52J/cm charging energy density (total energy density, W) under 350kV/cm electric field through testing3Available energy storage density (available energy storage density, W)rec) Reaching 4.43J/cm3And the energy storage efficiency (eta) reaches 96.9 percent.
Example 2
The chemical composition of the strontium titanate bismuth-based lead-free ceramic for the high-efficiency capacitor is (1-x) Sr0.7Bi0.2TiO3-xBi(Ni2/3Nb1/3)O3Wherein x is 0.05, and the following steps are adopted:
(1) selecting Bi with the purity of more than 98 percent2O3Powder and SrCO3Powder, TiO2Powder, NiO powder and Nb2O5The powder is used as raw material and is Sr according to the chemical formula of 0.950.7Bi0.2TiO3-0.05Bi(Ni2/3Nb1/3)O3Weighing raw materials, adding absolute ethyl alcohol with the same mass as that of the powder, and uniformly mixing the raw materials and the absolute ethyl alcohol through a primary ball milling process to uniformly mix the powder to form slurry. Wherein, anhydrous ethanol and ZrO are adopted in the primary ball milling2The ball is used as a ball milling medium, the rotating speed is 290r/min, the running direction is adjusted every half hour, and the ball milling time is 18 h.
(2) Placing the slurry in a constant-temperature oven at 90 ℃ for baking, removing absolute ethyl alcohol, and grinding in a mortar to obtain powder;
(3) putting the powder into a die to be pre-pressed into a material block, pre-sintering the material block at 960 ℃ under a closed condition, and keeping the temperature for 3 hours to obtain pre-synthesized ceramic powder;
(4) grinding the pre-synthesized ceramic material block in a mortar to obtain ceramic powder, adding absolute ethyl alcohol with equal mass into the obtained powder, and performing secondary ball milling, wherein the absolute ethyl alcohol and ZrO are still adopted in the process2The ball is used as a ball milling medium, the rotating speed is 280r/min, the running direction is adjusted every half hour, and the ball milling time is 17 h.
(5) Drying the obtained slurry at 90 ℃, adding 8 wt% of polyvinyl alcohol (PVA) as a binder to be doped into the powder for granulation, crushing the powder blocks obtained by granulation, sieving the powder blocks by using 80-mesh and 140-mesh sieves, taking the powder blocks in the middle layers of the 80-mesh and 140-mesh sieves, and performing compression molding under the pressure of 200Mpa to obtain the ceramic green bodies. Wherein the mass of the binder incorporated at the time of granulation was 7% of the mass of the powder, and the mass of the distilled water incorporated was 4% of the mass of the powder.
(6) Placing the ceramic blank in a crucible, covering a cover with a gap, carrying out glue discharging treatment for 7h at 620 ℃, then inverting the crucible on the ceramic blank subjected to glue discharging, carrying out closed sintering at the sintering temperature of 1130 ℃, at the heating rate of 3 ℃/min, keeping the temperature for 4h, and cooling to room temperature to obtain the strontium bismuth titanate-based lead-free ceramic for the high-efficiency capacitor.
The ceramic achieves 4.83J/cm charging energy density (total energy density, W) under 370kV/cm electric field through testing3Available energy storage density (available energy storage density, W)rec) Reaching 4.61J/cm3And the energy storage efficiency (eta) reaches 95.3 percent.
Example 3
The chemical composition of the strontium titanate bismuth-based lead-free ceramic for the high-efficiency capacitor is (1-x) Sr0.7Bi0.2TiO3-xBi(Ni2/3Nb1/3)O3Wherein x is 0.12, and the following steps are adopted:
(1) selecting Bi with the purity of more than 98 percent2O3Powder and SrCO3Powder, TiO2Powder, NiO powder and Nb2O5The powder is used as raw material and is prepared according to the chemical formula0.88Sr0.7Bi0.2TiO3-0.12Bi(Ni2/3Nb1/3)O3Weighing raw materials, adding absolute ethyl alcohol with the same mass as that of the powder, and uniformly mixing the raw materials and the absolute ethyl alcohol through a primary ball milling process to uniformly mix the powder to form slurry. Wherein, anhydrous ethanol and ZrO are adopted in the primary ball milling2The ball is used as a ball milling medium, the rotating speed is 330r/min, the running direction is adjusted every half hour, and the ball milling time is 24 hours.
(2) Placing the slurry in a constant-temperature oven at 90 ℃ for baking, removing absolute ethyl alcohol, and grinding in a mortar to obtain powder;
(3) putting the powder into a die to be pre-pressed into a material block, pre-sintering the material block at 1000 ℃ under a closed condition, and keeping the temperature for 4 hours to obtain pre-synthesized ceramic powder;
(4) grinding the pre-synthesized ceramic material block in a mortar to obtain ceramic powder, adding absolute ethyl alcohol with equal mass into the obtained powder, and performing secondary ball milling, wherein the absolute ethyl alcohol and ZrO are still adopted in the process2The ball is used as a ball milling medium, the rotating speed is 330r/min, the running direction is adjusted every half hour, and the ball milling time is 24 hours.
(5) Drying the obtained slurry at 90 ℃, adding 8 wt% of polyvinyl alcohol (PVA) as a binder to be doped into the powder for granulation, crushing the powder blocks obtained by granulation, sieving the powder blocks by using 80-mesh and 140-mesh sieves, taking the powder blocks in the middle layers of the 80-mesh and 140-mesh sieves, and performing compression molding under the pressure of 200Mpa to obtain the ceramic green bodies. Wherein the mass of the binder incorporated at the time of granulation was 10% of the mass of the powder, and the mass of the distilled water incorporated was 5% of the mass of the powder.
(6) Placing the ceramic blank in a crucible, covering a cover with a gap, carrying out glue discharging treatment at 650 ℃ for 10h, then inverting the crucible on the ceramic blank subjected to glue discharging, carrying out closed sintering at 1150 ℃, wherein the temperature rising rate is 4 ℃/min, the heat preservation time is 6h, and cooling to room temperature to obtain the strontium bismuth titanate-based lead-free ceramic for the high-efficiency capacitor.
The ceramic achieves 5.24J/cm charging energy density (total energy density, W) under 480kV/cm electric field through testing3Usable energy storage densityDegree (available energy storage density, W)rec) Reaches 5.09J/cm3And the energy storage efficiency (eta) reaches 97.1 percent. The dielectric test of this example is shown in fig. 2, and the dielectric constant does not change significantly with frequency, and the dielectric loss is small. As shown in FIG. 7, which is a graph of the maximum current, the current density and the power density in the charge and discharge test of this example, it can be seen that the ceramic material can obtain a higher current density of 1199.68A/cm2And simultaneously has higher power density of 215.94MW/cm3。
Example 4
The chemical composition of the strontium titanate bismuth-based lead-free ceramic for the high-efficiency capacitor is (1-x) Sr0.7Bi0.2TiO3-xBi(Ni2/3Nb1/3)O3Wherein x is 0.15, and the following steps are adopted:
(1) selecting Bi with the purity of more than 98 percent2O3Powder and SrCO3Powder, TiO2Powder, NiO powder and Nb2O5The powder is used as raw material and has a chemical formula of 0.85Sr0.7Bi0.2TiO3-0.15Bi(Ni2/3Nb1/3)O3Weighing raw materials, adding absolute ethyl alcohol with the same mass as that of the powder, and uniformly mixing the raw materials and the absolute ethyl alcohol through a primary ball milling process to uniformly mix the powder to form slurry. Wherein, anhydrous ethanol and ZrO are adopted in the primary ball milling2The ball is used as a ball milling medium, the rotating speed is 330r/min, the running direction is adjusted every half hour, and the ball milling time is 20 h.
(2) Placing the slurry in a constant-temperature oven at 90 ℃ for baking, removing absolute ethyl alcohol, and grinding in a mortar to obtain powder;
(3) putting the powder into a die to be pre-pressed into a material block, pre-sintering the material block at 960 ℃ under a closed condition, and keeping the temperature for 4 hours to obtain pre-synthesized ceramic powder;
(4) grinding the pre-synthesized ceramic material block in a mortar to obtain ceramic powder, adding absolute ethyl alcohol with equal mass into the obtained powder, and performing secondary ball milling, wherein the absolute ethyl alcohol and ZrO are still adopted in the process2The ball is used as a ball milling medium, the rotating speed is 330r/min, and the ball is adjusted to be transported once every half hourTurning the direction, the ball milling time is 24 h.
(5) Drying the obtained slurry at 90 ℃, adding 8 wt% of polyvinyl alcohol (PVA) as a binder to be doped into the powder for granulation, crushing the powder blocks obtained by granulation, sieving the powder blocks by using 80-mesh and 140-mesh sieves, taking the powder blocks in the middle layers of the 80-mesh and 140-mesh sieves, and performing compression molding under the pressure of 200Mpa to obtain the ceramic green bodies. Wherein, in the granulation, the mass of the mixed binder is 5-10% of the mass of the powder, and the mass of the mixed distilled water is 2.5-5% of the mass of the powder.
(6) Placing the ceramic blank in a crucible, covering a cover with a gap, carrying out glue discharging treatment at 600 ℃ for 7h, then inverting the crucible on the ceramic blank subjected to glue discharging, carrying out closed sintering at the sintering temperature of 1125 ℃, at the heating rate of 3 ℃/min, keeping the temperature for 4h, and cooling to room temperature to obtain the strontium bismuth titanate-based lead-free ceramic for the high-efficiency capacitor.
The ceramic achieves 4.52J/cm charging energy density (total energy density, W) under 400kV/cm electric field through testing3Available energy storage density (available energy storage density, W)rec) Reaching 4.19J/cm3And the energy storage efficiency (eta) reaches 92.6 percent.
Example 5
The chemical composition of the strontium titanate bismuth-based lead-free ceramic for the high-efficiency capacitor is (1-x) Sr0.7Bi0.2TiO3-xBi(Ni2/3Nb1/3)O3Wherein x is 0.12, a two-step sintering method is used, and the following steps are specifically adopted:
(1) selecting Bi with the purity of more than 98 percent2O3Powder and SrCO3Powder, TiO2Powder, NiO powder and Nb2O5The powder is used as raw material and has a chemical formula of 0.88Sr0.7Bi0.2TiO3-0.12Bi(Ni2/3Nb1/3)O3Weighing raw materials, adding absolute ethyl alcohol with the same mass as that of the powder, and uniformly mixing the raw materials and the absolute ethyl alcohol through a primary ball milling process to uniformly mix the powder to form slurry. Wherein, anhydrous ethanol and ZrO are adopted in the primary ball milling2The ball is used as a ball milling medium, the rotating speed is 330r/min, the running direction is adjusted every half hour, and the ball milling time is 12 h.
(2) Placing the slurry in a constant-temperature oven at 90 ℃ for baking, removing absolute ethyl alcohol, and grinding in a mortar to obtain powder;
(3) putting the powder into a die to be pre-pressed into a material block, pre-sintering the material block at 900 ℃ under a closed condition, and keeping the temperature for 4 hours to obtain pre-synthesized ceramic powder;
(4) grinding the pre-synthesized ceramic material block in a mortar to obtain ceramic powder, adding absolute ethyl alcohol with equal mass into the obtained powder, and performing secondary ball milling, wherein the absolute ethyl alcohol and ZrO are still adopted in the process2The ball is used as a ball milling medium, the rotating speed is 330r/min, the running direction is adjusted every half hour, and the ball milling time is 12 h.
(5) Drying the obtained slurry at 90 ℃, adding 8 wt% of polyvinyl alcohol (PVA) as a binder to be doped into the powder for granulation, crushing the powder blocks obtained by granulation, sieving the powder blocks by using 80-mesh and 140-mesh sieves, taking the powder blocks in the middle layers of the 80-mesh and 140-mesh sieves, and performing compression molding under the pressure of 200Mpa to obtain the ceramic green bodies. Wherein the mass of the binder incorporated at the time of granulation was 5% of the mass of the powder, and the mass of the distilled water incorporated was 3% of the mass of the powder.
(6) Placing the ceramic blank in a crucible, covering a cover with a gap, carrying out glue discharging treatment for 7h at 600 ℃, then inverting the crucible on the ceramic blank subjected to glue discharging, carrying out two-step sintering, heating to 950 ℃ at a heating rate of 3 ℃/min during sintering, then rapidly heating to 1100 ℃ at a heating rate of 8 ℃/min, rapidly cooling to 1025 ℃ without heat preservation, and finally carrying out heat preservation for 40h at 1025 ℃. And cooling to room temperature to obtain the strontium bismuth titanate-based lead-free ceramic for the high-efficiency capacitor.
The test shows that the scanning electron microscope picture of the energy storage dielectric is shown in figure 1, the ceramic material is compact, the grain size is small and uniform, and the average grain size is 0.49 μm at room temperature. The measured unipolar hysteresis loop of the energy storage dielectric is shown in fig. 3, where the hysteresis loop is relatively long and thin with relatively low losses. As shown in FIG. 4, the effective energy storage density reaches 5.98J/cm at 580kV/cm3And the energy storage efficiency reaches 98.6 percent. As shown in fig. 5, is a reservoir of this embodimentThe recoverable energy storage density of the ceramic material is in a range of 3.12 to 3.42J/cm according to the relationship graph of the recoverable energy storage density of the dielectric medium under 420kV/cm and different temperatures and the efficiency with the temperature3The change rate is less than 9%, and the efficiency is kept above 96%. As shown in FIG. 6, the recoverable energy storage density and efficiency of the energy storage dielectric of this embodiment are plotted as a function of frequency at 420kV/cm, and it can be seen that the recoverable energy storage density of the ceramic material varies from 3.02 to 3.20J/cm3The change rate is less than 7%, and the efficiency is kept above 95%.
Example 6; wherein the steps (1) to (5) are the same as in example 5; (6) placing the ceramic blank in a crucible, covering a cover with a gap, carrying out glue discharging treatment for 7h at 600 ℃, then inverting the crucible on the ceramic blank subjected to glue discharging, carrying out two-step sintering, heating to 1000 ℃ at a heating rate of 4 ℃/min during sintering, then rapidly heating to 1150 ℃ at a heating rate of 10 ℃/min, rapidly cooling to 1050 ℃ without heat preservation, and finally carrying out heat preservation for 10h at 1050 ℃; and cooling to room temperature to obtain the strontium bismuth titanate-based lead-free ceramic for the high-efficiency capacitor.
Example 7; wherein the steps (1) to (5) are the same as in example 5; (6) placing the ceramic blank in a crucible, covering a cover with a gap, carrying out glue discharging treatment for 7h at 650 ℃, then inverting the crucible on the ceramic blank subjected to glue discharging, carrying out two-step sintering, heating to 980 ℃ at a heating rate of 4 ℃/min during sintering, then rapidly heating to 1130 ℃ at a heating rate of 9 ℃/min, rapidly cooling to 1030 ℃ without heat preservation, and finally carrying out heat preservation for 30h at 1030 ℃; and cooling to room temperature to obtain the strontium bismuth titanate-based lead-free ceramic for the high-efficiency capacitor.
Claims (9)
1. The strontium bismuth titanate-based lead-free ceramic material for high-efficiency capacitor is characterized in that the chemical composition of the ceramic is (1-x) Sr0.7Bi0.2TiO3-xBi(Ni2/3Nb1/3)O3Wherein x is more than or equal to 0 and less than or equal to 0.15.
2. The strontium bismuth titanate-based lead-free ceramic material for high efficiency capacitors as claimed in claim 1, wherein x is 0.12.
3. The strontium bismuth titanate-based lead-free ceramic material for high-efficiency capacitors as claimed in claim 1, wherein when x is 0. ltoreq. x.ltoreq.0.15, the lead-free relaxed ceramic material with high-efficiency energy storage property has a released energy density of 4.19-5.98J/cm at 350kV/cm or higher3The high energy storage efficiency is more than 92 percent, and the high energy storage efficiency has good temperature/frequency/fatigue stability and simultaneously has large discharge density of 1.60J/cm3And an ultra-short discharge time of 40 ns.
4. The preparation method of the strontium bismuth titanate-based lead-free ceramic material for the high efficiency capacitor according to claim 1, wherein the corresponding energy storage ceramic is prepared by a solid phase reaction method, and the method specifically comprises the following steps:
the method comprises the following steps: selecting Bi with the purity of more than 98 percent2O3Powder and SrCO3Powder, TiO2Powder, NiO powder and Nb2O5The powder is used as a raw material and is Sr according to a general formula (1-x)0.7Bi0.2TiO3-xBi(Ni2/3Nb1/3)O3Weighing raw materials, wherein x is more than or equal to 0 and less than or equal to 0.15, adding absolute ethyl alcohol with the same mass as the powder, and uniformly mixing the raw materials and the absolute ethyl alcohol through a primary ball milling process to uniformly mix the powder to form slurry;
step two: placing the slurry in a constant-temperature oven at 90 ℃ for baking, removing absolute ethyl alcohol, and grinding in a mortar to obtain powder;
step three: placing the powder in a mold to be pre-pressed into a material block, pre-burning the material block under the closed condition at the temperature of 900-;
step four: crushing and grinding the pre-synthesized ceramic material block in a mortar to obtain ceramic powder, adding absolute ethyl alcohol with equal mass into the obtained powder, and carrying out secondary ball milling;
step five: drying the obtained slurry at 90 ℃, and performing granulation, sieving and compression molding to obtain a ceramic green body;
step six: carrying out gel removal treatment on the ceramic green body at the temperature of 600-650 ℃ for 5-10h, sintering the ceramic green body after gel removal at the sintering temperature of 1125-1150 ℃, at the heating rate of 2-4 ℃/min and at the heat preservation time of 2-6h, and cooling to room temperature to obtain the strontium bismuth titanate-based lead-free ceramic material for the high-efficiency capacitor.
5. The method for preparing the strontium bismuth titanate-based lead-free ceramic material for the high efficiency capacitor as claimed in claim 4, wherein the anhydrous ethanol and ZrO are adopted in the primary ball milling and the secondary ball milling2The ball is used as a ball milling medium, the rotating speed is 250-330r/min, the running direction is adjusted every half hour, and the ball milling time is 12-24 h.
6. The method for preparing a strontium bismuth titanate-based lead-free ceramic material for a high-efficiency capacitor according to claim 4, wherein polyvinyl alcohol with a mass concentration of 8% is used as a binder to be mixed into the powder during granulation, the mass of the mixed binder is 5-10% of the mass of the powder, the mass of the mixed distilled water is 2.5-5% of the mass of the powder, and the powder is uniformly mixed in a mortar, placed in a mold and pressed into a powder block.
7. The method for preparing the strontium bismuth titanate-based lead-free ceramic material for the high efficiency capacitor as claimed in claim 4, wherein the powder of the intermediate layer of 80 mesh and 140 mesh is obtained by sieving with 80 mesh and 140 mesh sieves.
8. The method for preparing a bismuth strontium titanate-based lead-free ceramic material for a high efficiency capacitor as claimed in claim 4, wherein the pressure during compression molding is controlled to 200 MPa.
9. The method for preparing the bismuth strontium titanate-based lead-free ceramic material for the high efficiency capacitor according to claim 4, wherein the method comprises the following steps: in the sixth step, sintering the ceramic blank after binder removal is replaced by a two-step sintering method, which specifically comprises the following steps: heating to 950-1000 ℃ at a heating rate of 3-4 ℃/min, then rapidly heating to 1100-1150 ℃ at a heating rate of 8-10 ℃/min, rapidly cooling to 1025-1050 ℃ without heat preservation, and finally performing heat preservation for 10-40h at 1025-1050 ℃.
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