CN115196960B - Sodium bismuth titanate based relaxation ferroelectric ceramic material with high energy storage density, high power density and high efficiency and preparation method thereof - Google Patents
Sodium bismuth titanate based relaxation ferroelectric ceramic material with high energy storage density, high power density and high efficiency and preparation method thereof Download PDFInfo
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Abstract
The invention provides a sodium bismuth titanate based relaxation ferroelectric ceramic material with high energy storage density, high power density and high efficiency and a preparation method thereof, belonging to the technical field of dielectric energy storage ceramic materials; its chemical composition is 0.5 (Bi) 0.5 Na 0.5 )TiO 3 ‑(0.5‑x)BaTiO 3 ‑xBaHfO 3 (x is more than or equal to 0.04 and less than or equal to 0.12). The method comprises the following steps: BNT is taken as a matrix, BT and BH are introduced by doping to synthesize a ternary solid solution, and then a solid phase reaction method is adopted to synthesize the ternary solid solution. The maximum breakdown field strength of the bismuth sodium titanate based relaxation ferroelectric ceramic material prepared by the invention reaches 800kV/cm, and the energy storage density can reach 12.7J/cm 3 The energy storage efficiency is stabilized to be above 84%, and the energy storage density reaches 89% under the electric field of 700 kV/cm. In addition, the preparation process is simple, low in cost and environment-friendly, and can realize large-scale production.
Description
Technical Field
The invention belongs to the field of dielectric energy storage ceramic materials, and particularly relates to a sodium bismuth titanate based relaxation ferroelectric ceramic material with high energy storage density, high power density and high efficiency and a preparation method thereof.
Background
In recent years, energy storage ceramics play an increasingly important role in the fields of pulse power and the like with the advantages of high power density, good temperature stability and the like, wherein lead-based capacitors become hot spots in the research field in the past due to extremely high breakdown field strength and energy storage density, but as the problems of environmental pollution and the like are increasingly serious, the development of lead-free ceramic capacitors has become a necessary trend. At present, the biggest constraint factors of the development of lead-free energy storage ceramics are small breakdown field intensity and low energy storage density, and the development trend of miniaturization and integration of current components is difficult to be complied with.
Among lead-free energy storage ceramics, bismuth sodium titanate systems are receiving a great deal of attention because of their high spontaneous polarization strength. However, the residual polarization intensity is large, the breakdown field intensity is low, the energy storage efficiency and the energy storage density are low, and the application range of the solar energy collector is limited. Aiming at the problems, at the present stage, the sodium bismuth titanate solid solution is mainly synthesized by doping and other modes, so that the energy storage density and the energy storage efficiency are improved, and the actual application requirements can be better met.
Disclosure of Invention
The invention aims to provide a bismuth sodium titanate-based relaxation ferroelectric ceramic material and a preparation method thereof, which have high energy storage density, high power density and high efficiency.
In order to solve the technical problems, the invention provides the following technical scheme:
in a first aspect, a sodium bismuth titanate based relaxor ferroelectric ceramic material having a chemical composition of 0.5 (Bi 0.5 Na 0.5 )TiO 3 -(0.5-x)BaTiO 3 -xBaHfO 3 (0.04≤x≤0.12)。
Preferably, 0.06.ltoreq.x.ltoreq.0.10, and x may be, for example, 0.06, 0.07, 0.08, 0.09, 0.10.
More preferably, x=0.08.
Under the preferable scheme x, the energy storage density can reach 12.7J/cm 3 The energy storage efficiency can reach 89%, and the maximum breakdown field strength can reach 800kV/cm. This is mainly due to the fact that by BaTiO 3 (BT) and BaHfO 3 Doping (BH) to obtain (Bi) 0.5 Na 0.5 )TiO 3 The (BNT) realizes the conversion from ferroelectric to relaxation ferroelectric at room temperature, the electric domain is changed from macroscopic scale to nanometer scale, the residual polarization is reduced, and the energy storage efficiency is improved. The grain size of the component is smaller, the density is higher, and the component has higher breakdown field intensity.
In a second aspect, there is provided a method for preparing the bismuth sodium titanate based relaxor ferroelectric ceramic material according to the first aspect, comprising: BNT is taken as a matrix, BT and BH are introduced by doping to synthesize a ternary solid solution, and then a solid phase reaction method is adopted to synthesize the ternary solid solution.
Wherein, preferably, the following steps are adopted specifically:
s1 according to 0.5 (Bi 0.5 Na 0.5 )TiO 3 -(0.5-x)BaTiO 3 -xBaHfO 3 Stoichiometric ratio of Bi 2 O 3 、 Na 2 CO 3 、BaCO 3 、TiO 2 、HfO 2 Mixing with ethanol, ball milling, oven drying, grinding, calcining for one time, and cooling;
s2, dripping a binder into the sample obtained after calcining the S1, granulating, tabletting and then sintering;
s3, polishing the ceramic sheet obtained by sintering the S2, coating silver paste on the upper surface and the lower surface, and then feeding
And (3) performing secondary calcination and cooling to obtain the sodium bismuth titanate-based relaxor ferroelectric ceramic material with high energy storage density, high power density and high efficiency.
Wherein, preferably, the time of ball milling in S1 is 12-24h.
The dosage of the ethanol in the step S1 can be freely selected according to the volume of the adopted container and the grinding uniformity, so long as the grinding uniformity is facilitated, and the ethanol can be gradually evaporated in the subsequent treatment process.
Wherein, preferably, the conditions of the primary calcination in S1 include: the temperature is 600-900 ℃ and the time is 1-3h.
Wherein, preferably, the binder in S2 is one of PVA and PVB.
Preferably, the mass ratio of the binder to the sample obtained after S1 calcination is 1:5-15.
Wherein, preferably, the sintering conditions in S2 include: the temperature is 1100-1300 ℃ and the time is 1-3h.
Wherein, preferably, the conditions of the secondary calcination in S3 include: the temperature is 500-800 ℃ and the time is 0.5-3h.
The technical scheme of the invention has the following beneficial effects:
the invention introduces BaTiO by doping 3 (BT) and BaHfO 3 The (BH) synthesized bismuth sodium titanate based ternary solid solution provides a bismuth sodium titanate based relaxation ferroelectric ceramic material with high energy storage density, high power density and high efficiency, namely 0.5 (Bi) 0.5 Na 0.5 )TiO 3 -(0.5-x)BaTiO 3 -xBaHfO 3 (BNT-BT-BH) relaxor ferroelectric ceramic with energy storage density of 12.7J/cm 3 The energy storage efficiency can reach 89%, the maximum breakdown field strength can reach 800kV/cm, and the performance of most of reported energy storage ceramics is exceeded, so that the method can be widely applied to pulse power electronic systems such as mobile communication, medical treatment and health, national defense and military, and the like. The material has low cost, simple preparation method, environmental friendliness and long service life, can be produced in a large scale, is beneficial to promoting the related application, and is hopeful to replace other energy storage ceramics.
Drawings
FIG. 1 is an SEM image of a sodium bismuth titanate based relaxor ferroelectric ceramic prepared according to example 1;
FIG. 2 is a hysteresis loop of the sodium bismuth titanate based relaxor ferroelectric ceramic prepared in example 1;
FIG. 3 is a graph showing the change of the energy storage characteristics of the sodium bismuth titanate based relaxor ferroelectric ceramic prepared in example 1 with the electric field strength.
Detailed Description
In order to make the technical problems, technical solutions and advantages to be solved more apparent, the following detailed description will be given with reference to the accompanying drawings and specific embodiments.
Example 1:
preparation of 0.5 (Bi) by the present invention 0.5 Na 0.5 )TiO 3 -0.42BaTiO 3 -0.08BaHfO 3 . 2.9123 g Bi is weighed according to the chemical dose ratio 2 O 3 0.6624 g of Na 2 CO 3 4.9335 g BaCO 3 3.6740 g of TiO 2 0.8420 g of HfO 2 And pouring the mixture into a ball milling tank, adding ethanol, and ball milling for 24 hours. And (3) sequentially carrying out drying and grinding treatment on the ball-milled sample, and then placing the sample into a muffle furnace to be calcined for 2 hours at the temperature of 850 ℃. After cooling, the sample is poured into a mortar, a proper amount of PVA binder (the mass ratio of the binder to the sample is 1:10) is dripped into the mortar for grinding for 1h, and the mixture is uniformly ground and poured into
Pressed into tablets and then sintered in a muffle furnace at 1150 ℃ for 2 hours. After cooling, the ceramic sheet was polished to a thickness of 50 μm, coated with silver paste on the upper and lower surfaces, and then calcined at 550 ℃ for 1 hour. After cooling, thenThe sodium bismuth titanate based relaxation ferroelectric ceramic material with high energy storage density, high power density and high efficiency can be obtained.
Fig. 1 is an SEM picture of the sodium bismuth titanate based relaxor ferroelectric ceramic prepared in this embodiment, and it can be seen from the figure that the crystal grain size of the ceramic is about 1 μm, and the density is higher, which determines that the material has higher breakdown field strength, and further, has higher energy storage density.
Fig. 2 shows a unipolar ferroelectric hysteresis loop of the bismuth sodium titanate based relaxor ferroelectric ceramic prepared in this example at room temperature, and it can be seen from the figure that the ceramic hysteresis loop is elongated, and the maximum electric field strength can reach 800kV/cm.
FIG. 3 is a graph showing the change of the energy storage characteristics of the bismuth sodium titanate-based relaxor ferroelectric ceramic prepared in the present example with the electric field strength, wherein the ceramic energy storage density can reach 12.7J/cm in an electric field of 800kV/cm 3 The method comprises the steps of carrying out a first treatment on the surface of the The energy storage efficiency can be stabilized to be above 84%, and the maximum energy storage efficiency can reach 89% under the electric field of 700kV/cm, and the data exceeds the vast majority of energy storage ceramic materials reported before.
Example 2:
preparation of 0.5 (Bi) by the present invention 0.5 Na 0.5 )TiO 3 -0.40BaTiO 3 -0.10BaHfO 3 . 2.9123 g Bi is weighed according to the chemical dose ratio 2 O 3 0.6624 g of Na 2 CO 3 4.9335 g BaCO 3 3.5942 g of TiO 2 1.0525 g of HfO 2 And pouring the mixture into a ball milling tank, adding ethanol, and ball milling for 24 hours. And (3) sequentially carrying out drying and grinding treatment on the ball-milled sample, and then placing the sample into a muffle furnace to be calcined for 2 hours at the temperature of 850 ℃. After cooling, the sample is poured into a mortar, a proper amount of PVA binder (the mass ratio of the binder to the sample is 1:10) is dripped into the mortar for grinding for 1h, and the mixture is uniformly ground and poured into
Pressed into tablets and then sintered in a muffle furnace at 1150 ℃ for 2 hours. After cooling, the ceramic sheet was polished to a thickness of 50 μm, coated with silver paste on the upper and lower surfaces, and then calcined at 550 ℃ for 1 hour.The sodium bismuth titanate based relaxation ferroelectric ceramic material with high energy storage density, high power density and high efficiency can be obtained after cooling.
Example 3:
preparation of 0.5 (Bi) by the present invention 0.5 Na 0.5 )TiO 3 -0.38BaTiO 3 -0.12BaHfO 3 . 2.9123 g Bi is weighed according to the chemical dose ratio 2 O 3 0.6624 g of Na 2 CO 3 4.9335 g BaCO 3 3.5143 g of TiO 2 1.2629 g of HfO 2 And pouring the mixture into a ball milling tank, adding ethanol, and ball milling for 24 hours. And (3) sequentially carrying out drying and grinding treatment on the ball-milled sample, and then placing the sample into a muffle furnace to be calcined for 2 hours at the temperature of 850 ℃. After cooling, the sample is poured into a mortar, a proper amount of PVA binder (the mass ratio of the binder to the sample is 1:10) is dripped into the mortar for grinding for 1h, and the mixture is uniformly ground and poured into
Pressed into tablets and then sintered in a muffle furnace at 1150 ℃ for 2 hours. After cooling, the ceramic sheet was polished to a thickness of 50 μm, coated with silver paste on the upper and lower surfaces, and then calcined at 550 ℃ for 1 hour. The sodium bismuth titanate based relaxation ferroelectric ceramic material with high energy storage density, high power density and high efficiency can be obtained after cooling.
While the foregoing is directed to the preferred embodiments of the present invention, it will be appreciated by those skilled in the art that various modifications and adaptations can be made without departing from the principles of the present invention, and such modifications and adaptations are intended to be comprehended within the scope of the present invention.
Claims (1)
1. A sodium bismuth titanate based relaxation ferroelectric ceramic material with high energy storage density, high power density and high efficiency is characterized in that the chemical composition is 0.5 (Bi 0.5 Na 0.5 )TiO 3 -0.42BaTiO 3 -0.08BaHfO 3 The preparation method comprises the following steps:
2.9123 g Bi is weighed according to the chemical dose ratio 2 O 3 0.6624 g of Na 2 CO 3 4.9335 g BaCO 3 3.6740 g of TiO 2 0.8420 g of HfO 2 Pouring the mixture into a ball milling tank, adding ethanol, ball milling for 24 hours, sequentially drying and grinding the ball-milled sample, then placing the sample into a muffle furnace, setting the temperature to 850 ℃ and calcining for 2 hours, cooling, pouring the sample into a mortar, dripping a proper amount of PVA binder, grinding for 1 hour, wherein the mass ratio of the binder to the sample is 1:10, grinding uniformly, pouring
Pressing into tablets, placing into a muffle furnace, setting the temperature to 1150 ℃ for sintering for 2 hours, cooling, polishing the thickness of the ceramic plate to 50 mu m, coating silver paste on the upper surface and the lower surface, calcining for 1 hour at 550 ℃, and cooling to obtain the sodium bismuth titanate based relaxation ferroelectric ceramic material with high energy storage density, high power density and high efficiency. />
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