CN113024250B - Sb with high energy storage density and energy storage efficiency 5+ Strontium sodium silver tungsten bronze doped ferroelectric ceramic material and preparation method thereof - Google Patents
Sb with high energy storage density and energy storage efficiency 5+ Strontium sodium silver tungsten bronze doped ferroelectric ceramic material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses Sb with high energy storage density and energy storage efficiency 5+ Doped strontium sodium silver tungsten niobateA copper ferroelectric ceramic material and a preparation method thereof, the structural general formula of the ceramic material is Sr 2 Ag 0.2 Na 0.8 Nb 5‑x Sb x O 15 Wherein the value of x is 0.2-0.5. The invention is prepared by batching, ball milling, presintering, secondary ball milling, sieving, tabletting and sintering. The preparation method is simple, the cost is low, the repeatability is good, the yield is high, the obtained ceramic material has high energy storage density and high energy storage efficiency, and when x is 0.3, the effective energy storage density is 2.27J/cm 3 And the energy storage efficiency can reach 93.3 percent.
Description
Technical Field
The invention belongs to the technical field of tungsten bronze structure ceramic materials, and particularly relates to Sb with high energy storage density and high energy storage efficiency 5+ A strontium sodium silver tungsten bronze doped ferroelectric ceramic material and a preparation method thereof.
Background
With the rapid development of electronic information technology and the continuous consumption of non-renewable energy, the problems of energy crisis and environmental pollution become more severe, and the search and development of energy storage devices which are environment-friendly, excellent in performance and suitable for sustainable development are hot spots of research of scientists for over a decade. The ceramic energy storage capacitor has the advantages of high power density, high charging and discharging speed, strong mechanical property, high temperature resistance, corrosion resistance, long cycle life, environmental protection and the like, and is widely applied to advanced pulse power technologies, key medical devices and new energy automobiles. However, compared with devices such as batteries and electrochemical capacitors, energy storage ceramic capacitors have low energy storage density and low energy storage efficiency, and are difficult to meet the development requirements of lead-free, miniaturization, light weight and integration of present electronic devices, so that the development of energy storage ceramic materials with high energy storage density and high energy storage efficiency is urgent. However, the energy storage ceramic materials used at present have low energy storage density and most of them are lead-containing materials, so that the application is hindered. In recent years, lead-free ceramic materials have begun to replace lead-containing materials, most typically perovskite lead-free energy storage ceramic materials. The tungsten bronze structure ferroelectric is the second largest ferroelectric next to the perovskite structure, has moderate dielectric constant and very low dielectric loss, and is a promising energy storage material. How to obtain a ceramic energy storage capacitor with both high energy storage density and high energy storage efficiency in a lead-free tungsten bronze system becomes a hot point problem.
Disclosure of Invention
The invention aims to provide Sb with high energy storage density and high energy storage efficiency 5+ The strontium sodium silver tungsten bronze niobate-doped ferroelectric ceramic material and the preparation method with simple process, good repeatability and low cost are provided.
The structural formula of the ceramic material adopted for solving the technical problems is Sr 2 Ag 0.2 Na 0.8 Nb 5-x Sb x O 15 Wherein the value of x is 0.2-0.5, and preferably the value of x is 0.3.
Sb of the invention 5+ The preparation method of the strontium sodium silver tungsten bronze doped ferroelectric ceramic material comprises the following steps:
1. according to Sr 2 Ag 0.2 Na 0.8 Nb 5-x Sb x O 15 The purity of SrCO is more than 99.00 percent by weight respectively 3 、Ag 2 O、Na 2 CO 3 、Nb 2 O 5 、Sb 2 O 3 Fully mixing and ball-milling for 20-24 hours, and drying at 60-80 ℃ for 20-24 hours to obtain a raw material mixture;
2. pre-burning the raw material mixture for 5-8 hours at 1160-1200 ℃, and performing secondary ball milling, drying and sieving to obtain pre-burned powder;
3. after the pre-sintered powder is pressed into tablets, sintering is carried out for 3-5 hours at 1250-1300 ℃ to obtain Sb with high energy storage density and energy storage efficiency 5+ Doped strontium sodium silver tungsten bronze niobate ferroelectric ceramic material.
In the above step 2, the raw material mixture is preferably calcined at 1180 ℃ for 6 hours.
In the step 2, preferably, the tablet is pressed into a cylindrical blank by a powder tablet press, and then is subjected to cold isostatic pressing for 5-7 minutes under the pressure of 200-220 MPa.
In the above step 3, the sintering is preferably carried out at 1270 ℃ for 4 hours.
The invention has the following beneficial effects:
1. the invention selects in Sr 2 Ag 0.2 Na 0.8 Nb 5 O 15 System for carrying out Sb site 5+ By substitution of Sb 5+ The introduction of the ceramic material inhibits the growth of crystal grains, reduces the size of the crystal grains and the number of air holes, improves the density of the ceramic, and further improves the breakdown field strength of the ceramic material. In addition, Sb 5+ The introduction of the energy storage ceramic material enables the ceramic to be gradually changed into a relaxor ferroelectric from a normal ferroelectric, and the Curie temperature to move towards the room temperature, which is beneficial to obtaining a slender P-E curve, and finally the energy storage ceramic material with high energy storage density and high energy storage efficiency is obtained.
2. In the preparation process of the ceramic material, the advanced cold isostatic pressing technology is adopted, so that the waste of samples is avoided, the cost of a binder and a subsequent glue discharging process is saved, and the preparation period of the ceramic is shortened; meanwhile, the blank formed by utilizing the cold isostatic pressing has high density, uniform and consistent density and small internal stress of the blank, the defects of blank cracking, layering and the like are reduced, the quality of the ceramic is guaranteed, the foundation is laid for excellent experimental results, and the selected raw materials do not contain heavy metals such as lead and the like, and are environment-friendly.
Drawings
FIG. 1 shows a ferroelectric ceramic material of strontium sodium silver tungsten bronze niobate prepared in comparative example 1 and Sb prepared in examples 1 to 3 5+ XRD pattern of strontium sodium silver tungsten bronze doped material.
FIG. 2 is a graph of the dielectric constant and dielectric loss of the strontium sodium silver tungsten bronze niobate ferroelectric ceramic material prepared in comparative example 1 at different test frequencies.
FIG. 3 is Sb prepared in example 2 5+ And (3) a dielectric constant and dielectric loss diagram of the doped strontium sodium silver tungsten bronze niobate ferroelectric ceramic material at different test frequencies.
FIG. 4 shows a ferroelectric ceramic material of strontium sodium silver tungsten bronze niobate prepared in comparative example 1 and Sb prepared in examples 1 to 3 5+ A unipolar hysteresis loop diagram of the doped strontium sodium silver tungsten bronze niobate ferroelectric ceramic material under a critical breakdown electric field.
FIG. 5 shows a ferroelectric ceramic material of strontium sodium silver tungsten bronze niobate prepared in comparative example 1 and Sb prepared in examples 1 to 3 5+ And (3) a comparison graph of the effective energy storage density and the energy storage efficiency of the strontium sodium silver tungsten bronze doped ferroelectric ceramic material under a critical breakdown electric field.
Detailed Description
The invention will be further described in detail with reference to the following figures and examples, but the scope of the invention is not limited to these examples.
Example 1
1. According to Sr 2 Ag 0.2 Na 0.8 Nb 4.8 Sb 0.2 O 15 Respectively weighing SrCO with the purity of 99.95 percent 3 8.6190g of 99.7% pure Ag 2 O0.6782 g, 99.99% pure Na 2 CO 3 1.2371g of Nb with a purity of 99.99% 2 O 5 18.6150g of Sb with a purity of 99.99% 2 O 3 0.8506g, putting into a nylon pot, ball-milling for 24 hours by using a ball mill with the rotation speed of 401 r/min and the absolute ethyl alcohol as a ball-milling medium, drying for 24 hours at 80 ℃, and grinding for 30 minutes by using a mortar to obtain a raw material mixture.
2. Placing the raw material mixture into an alumina crucible, compacting by an agate rod, covering, placing into a resistance furnace, heating to 1180 ℃ at the heating rate of 3 ℃/min, preserving heat for 6 hours, naturally cooling to room temperature along with the furnace, discharging, grinding by a mortar for 30 minutes, performing secondary ball milling according to the method in the step 1, performing ball milling for 15 hours, placing into a drying oven, drying for 24 hours at the temperature of 80 ℃, grinding by the mortar for 10 minutes, and sieving by a 120-mesh sieve to obtain the pre-fired powder.
3. The pre-sintered powder is put into a stainless steel die with the diameter of 11.5mm, the stainless steel die is pressed into a cylindrical blank with the thickness of 1.3mm by a powder tablet machine under the condition of no pressure, and the cylindrical blank is put into cold isostatic pressing for 5 minutes under the pressure of 200 MPa. Placing the cylindrical blank on a zirconium oxide plate, placing the zirconium oxide plate in an alumina closed sagger, heating to 1000 ℃ at a heating rate of 10 ℃/min, and heating to 12 ℃ at a heating rate of 3 ℃/minKeeping the temperature at 70 ℃ for 4 hours, and naturally cooling to room temperature along with the furnace to obtain Sb 5+ Doped strontium sodium silver tungsten bronze niobate ferroelectric ceramic material.
Example 2
In step 1 of this example, according to Sr 2 Ag 0.2 Na 0.8 Nb 4.7 Sb 0.3 O 15 Respectively weighing SrCO with the purity of 99.95 percent 3 8.6083g of 99.7% pure Ag 2 O0.6773 g, 99.99% pure Na 2 CO 3 1.2356g of Nb with a purity of 99.99% 2 O 5 18.2044g of Sb with the purity of 99.99% 2 O 3 1.2744g, other steps were carried out in the same manner as in example 1 to obtain Sb 5+ Doped strontium sodium silver tungsten bronze niobate ferroelectric ceramic material.
Example 3
In step 1 of this example, according to Sr 2 Ag 0.2 Na 0.8 Nb 4.5 Sb 0.5 O 15 Respectively weighing SrCO with the purity of 99.95 percent 3 8.5868g of Ag with a purity of 99.7% 2 O0.6756 g, 99.99% pure Na 2 CO 3 1.2325g of Nb with a purity of 99.99% 2 O 5 17.3864g of Sb with a purity of 99.99% 2 O 3 2.1187 g, the other steps were carried out in the same manner as in example 1 to obtain Sb 5+ Doped strontium sodium silver tungsten bronze niobate ferroelectric ceramic material.
Comparative example 1
According to Sr 2 Ag 0.2 Na 0.8 Nb 5 O 15 Respectively weighing SrCO with the purity of 99.95 percent 3 8.6407 g of 99.7% pure Ag 2 O0.6799 g, Na with purity of 99.99% 2 CO 3 1.2402g of Nb with a purity of 99.99% 2 O 5 19.4393g, the other steps are the same as the example 1, and the strontium sodium silver tungsten bronze niobate ferroelectric ceramic material is obtained.
Sb prepared in examples 1 to 3 5+ Strontium sodium silver tungsten bronze doped ferroelectric ceramic material and surface of strontium sodium silver tungsten bronze doped ferroelectric ceramic material prepared in comparative example 1Grinding, polishing, performing ultrasonic treatment, cleaning, respectively coating silver paste on the upper surface and the lower surface of the glass substrate, placing the glass substrate in a muffle furnace at 840 ℃ for 30 minutes, and naturally cooling to room temperature. The inventor adopts a SmartLab9 type ray diffractometer manufactured by Japan science, Inc., a 4294A, E4980A dielectric analyzer manufactured by Agilent technologies, Inc., and a ferroelectric tester manufactured by Radant in America to perform characterization tests on the structure and the performance, and calculates related performance parameters according to the following formula:
dielectric constant ε r ：ε r ＝4Ct/(πε 0 d)
Effective energy storage density W rec ：
Energy storage efficiency η:
in the formula: c is capacitance, t is thickness of ceramic plate, epsilon 0 Is the vacuum dielectric constant, d is the diameter of the ceramic wafer, P m At maximum polarization, P r W is the total storage energy density for remanent polarization. The results are shown in FIGS. 1 to 5.
As can be seen from FIG. 1, a small amount of Na appears in the ceramic materials prepared in comparative example 1 and example 1 0.5 Sr 0.25 Nb 5 O 15 The second phase, the ceramic material prepared in examples 2 and 3, is a pure tungsten bronze structure. As can be seen from FIGS. 2 to 3, in comparative example 1, Sb was not doped 5+ The ceramic material of (1) is typically a ferroelectric, example 2 is doped with Sb 5+ The relaxivity of the ceramic material of (a) is enhanced and a relaxor ferroelectric is developed. And with Sb 5+ The curie temperature gradually moves to the room temperature by increasing the doping amount, that is, the relaxor ferroelectric phase is adjusted to be near the room temperature. As can be seen in FIG. 4, with Sb 5+ The doped amount is increased, the breakdown field strength of the ceramic material prepared in the embodiment 1 is obviously improved from 160 kV/cm to 220kV/cm in the comparative example 1, and the energy storage density is greatly improved due to the improvement of the breakdown field strength; example 2 the ceramic material was at maximum polarization (P) compared to example 1 max ) Residual polarization (P) while remaining substantially constant r ) The breakdown field strength is obviously reduced and slightly improved, so that the ceramic material obtains higher effective energy storage density and high energy storage efficiency; ceramic material of example 3 with respect to ceramic material P of example 2 max The energy storage density is slightly reduced. As can be seen from FIG. 5, the ceramic material prepared in comparative example 1 had an effective energy storage density of 0.92J/cm 3 Energy storage efficiency of 79.5%, via Sb 5+ The B site doping is adopted, the energy storage density and the energy storage efficiency of the ceramic material prepared in the embodiments 1 to 3 are obviously improved, and the energy storage density is about 1.91 to 2.27J/cm 3 The energy storage efficiency is about 88.6% -93.3%, especially when Sb is used 5+ When the doping amount of (2) is 0.3, the effective energy storage density of the ceramic is as high as 2.27J/cm 3 And the energy storage efficiency is as high as 93.3%. Therefore, the tungsten bronze structure ceramic material disclosed by the invention has high energy storage density and high energy storage efficiency, and is expected to become a candidate material of an energy storage ceramic capacitor.
Claims (4)
1. Sb with high energy storage density and energy storage efficiency 5+ The strontium sodium silver tungsten bronze doped ferroelectric ceramic material is characterized in that: the structural general formula of the ceramic material is Sr 2 Ag 0.2 Na 0.8 Nb x5- Sb x O 15 WhereinxThe value of (a) is 0.2-0.5;
the preparation method of the ceramic material comprises the following steps:
(1) according to Sr 2 Ag 0.2 Na 0.8 Nb x5- Sb x O 15 Respectively weighing SrCO with the purity of more than 99.00 percent 3 、Ag 2 O、Na 2 CO 3 、Nb 2 O 5 、Sb 2 O 3 Uniformly mixing all the weighed raw materials, putting the mixture into a nylon tank, fully mixing and ball-milling for 20-24 hours by taking zirconium balls as grinding balls and absolute ethyl alcohol as a ball-milling medium, and drying for 20-24 hours at 60-80 ℃ to obtain a raw material mixture;
(2) pre-burning the raw material mixture for 5-8 hours at 1160-1200 ℃, and performing secondary ball milling, drying and sieving to obtain pre-burned powder;
(3) pressing the pre-sintered powder into a cylindrical blank by using a powder tablet press, then carrying out cold isostatic pressing for 5-7 minutes under the pressure of 200-220 MPa, and sintering for 3-5 hours at 1250-1300 ℃ to obtain Sb with high energy storage density and energy storage efficiency 5+ Doped strontium sodium silver tungsten bronze niobate ferroelectric ceramic material.
2. The high energy storage density and energy storage efficiency Sb of claim 1 5+ The strontium sodium silver tungsten bronze doped ferroelectric ceramic material is characterized in that:xis 0.3.
3. Sb having high energy storage density and energy storage efficiency according to claim 1 5+ The strontium sodium silver tungsten bronze doped ferroelectric ceramic material is characterized in that: in step (2), the raw material mixture is prefired at 1180 ℃ for 6 hours.
4. The high energy storage density and energy storage efficiency Sb of claim 1 5+ The strontium sodium silver tungsten bronze doped ferroelectric ceramic material is characterized in that: in step (3), sintering was carried out at 1270 ℃ for 4 hours.
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