CN113929458A - High-efficiency high-energy-storage sodium niobate-based ceramic material and preparation method thereof - Google Patents
High-efficiency high-energy-storage sodium niobate-based ceramic material and preparation method thereof Download PDFInfo
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Abstract
The invention relates to the technical field of dielectric ceramic materials, and particularly discloses a high-efficiency high-energy-storage sodium niobate-based ceramic material and a preparation method thereof, wherein the material has a chemical composition formula as follows: (1-x) [0.9NaNbO3‑0.1Bi(Mg0.667Nb0.333)O3]‑xmol％(Bi0.5Na0.5)0.7Sr0.3TiO3(x is more than or equal to 0.05 and less than or equal to 0.4), performing wet ball milling by using an ethanol solution as a ball milling medium by adopting a solid phase reaction method to obtain raw powder with uniform particle size; the high-performance energy storage ceramic is prepared by adopting a traditional sintering process.
Description
Technical Field
The invention relates to the technical field of dielectric ceramic materials, in particular to a high-efficiency high-energy-storage sodium niobate-based ceramic material and a preparation method thereof.
Background
At present, the primary energy sources are mainly of the type electric (solid-state capacitors, supercapacitors, inductors, etc.), mechanical (motors, inertial energy storage) and chemical (lithium batteries, fuel electricity)A pool). In which the solid state capacitor is at its high power density (-10)8W/kg), fast charge and discharge speed<1 mus) and long cycle life (50 ten thousand times) become the preferred energy storage method for pulse power technology, but the energy storage density (W)rec) Is relatively low (10)-2-101Wh/kg), the requirements of integration, weight reduction and miniaturization of the pulse power device cannot be satisfied.
At present, most capacitors applied to high-power pulse power supplies are foil-type structure capacitors and metallized film capacitors. The former has the problems of low energy storage density, easy fault explosion and the like; the latter has the disadvantages of short service life, small discharge current, etc. Therefore, in order to meet the requirements of special properties such as high energy storage density, long charging and discharging service life, large output current and the like of an energy storage element in a high-power pulse power supply, designing and preparing the high-performance energy storage dielectric material has important significance.
Disclosure of Invention
The invention aims to provide a high-efficiency high-energy-storage sodium niobate-based ceramic material and a preparation method thereof, so that an energy storage element required in a high-power pulse power supply has high energy storage density, long charge-discharge service life and large output current.
In order to achieve the purpose, the high-efficiency high-energy-storage-rate sodium niobate-based ceramic material adopted by the invention has a chemical composition formula as follows:
(1-x)[0.9NaNbO3-0.1Bi(Mg0.667Nb0.333)O3]-xmol％(Bi0.5Na0.5)0.7Sr0.3TiO3(0.05≤x ≤0.4)。
the invention also provides a preparation method of the high-efficiency high-energy-storage-rate sodium niobate-based ceramic material, which comprises the following steps:
weighing high-purity Na2CO3、Nb2O5、Bi2O3MgO and Na2CO3、Bi2O3、SrCO3、TiO2Separately mixing to obtain powder;
putting the powder into a ball milling tank for wet ball milling, drying and sieving, pressing the powder into a column shape, and putting the column shape into an alumina crucible for sealing pre-sintering;
then 0.9NaNbO is added3-0.1Bi(Mg0.667Nb0.333)O3And (Bi)0.5Na0.5)0.7Sr0.3TiO3After proportioning, pouring the mixture into a ball milling tank for wet ball milling again, quickly drying the mixture in an oven at 100 ℃, sieving the mixture by using a screen, and pressing particles with the size of 60-120 meshes into round pieces by using a die;
carrying out sealing sintering on the wafer in a muffle furnace;
and polishing the sintered sample, coating high-temperature silver paste, sintering at high temperature and preserving heat to obtain the sodium niobate-based ceramic material.
The preparation method comprises the following steps of putting the powder into a ball milling tank for wet ball milling, drying and sieving, pressing the powder into a column shape, putting the column shape into an alumina crucible for sealing preburning, and specifically comprises the following steps:
according to the mass ratio of the powder, the zirconia balls and the absolute ethyl alcohol of 1: 2: 2, sequentially adding zirconia balls and absolute ethyl alcohol into a nylon tank, ball-milling for 4 hours, mixing and grinding, quickly drying at 100 ℃ to obtain powder, separating the powder from the zirconia balls by using a 60-mesh screen, and presintering the sieved powder in an alumina crucible to obtain powder.
Wherein, the step of pre-burning in the alumina crucible comprises the following steps:
the presintering temperature is 850 ℃, the heat preservation time is 4 hours, and the heating rate is 5 ℃/min.
Wherein, 0.9NaNbO is then added3-0.1Bi(Mg0.667Nb0.333)O3And (Bi)0.5Na0.5)0.7Sr0.3TiO3After proportioning, pouring the mixture into a ball milling tank for wet ball milling again, quickly drying the mixture in a drying oven at 100 ℃, sieving the mixture, and pressing particles with the size of 60-120 meshes into round pieces by using a die:
grinding the pre-sintered powder and mixing the powder with 0.9NaNbO in proportion3-0.1Bi(Mg0.667Nb0.333)O3And (Bi)0.5Na0.5)0.7Sr0.3TiO3And thirdly, mixing the powder, the zirconia balls and the absolute ethyl alcohol according to the mass ratio of 1: 2: 2 are sequentially put into a nylon tank for ball milling for 4 hours, then taken out and put into an oven to be dried at 100 ℃;
then adding 5 wt% of polyvinyl alcohol (PVA) for granulation, sieving by using a sieve of 60 meshes and a sieve of 120 meshes, and pressing the granules with the size of 60-120 meshes into round pieces with the diameter of 8mm and the thickness of 1mm by using a die.
Wherein, before the step of hermetically sintering the wafer in a muffle furnace:
the wafer was allowed to gel at 550 ℃ for 4 hours at a rate of 1 ℃/min.
The invention relates to a high-efficiency high-energy-storage sodium niobate-based ceramic material and a preparation method thereof.A solid-phase reaction method is adopted, and an ethanol solution is taken as a ball milling medium for wet ball milling to obtain raw powder with uniform particle size; the high-performance energy storage ceramic is prepared by adopting a traditional sintering process. The solid solution ceramic material prepared by the invention has lower sintering temperature and excellent energy storage performance, so that an energy storage element required in a high-power pulse power supply has high energy storage density, long charge-discharge service life and large output current.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
Fig. 1 is a flow chart of the steps of the preparation method of the high-efficiency high-energy-storage-rate sodium niobate-based ceramic material of the present invention.
FIG. 2 is a room temperature XRD pattern of (1-x) (0.9NN-0.1BMN) -xBNST ceramic (0.05. ltoreq. x. ltoreq.0.4) of the present invention.
Detailed Description
The invention introduces (Bi)0.5Na0.5)0.7Sr0.3TiO3With 0.9NaNbO3-0.1Bi(Mg0.667Nb0.333)O3A uniform solid solution is formed to improve the maximum polarization strength of the ceramic material, thereby obtaining a dielectric ceramic material with high energy storage density.
Introduced by the invention of (Bi)0.5Na0.5)0.7Sr0.3TiO3Has the following advantages:
(Bi0.5Na0.5)0.7Sr0.3TiO3hybridization of the 6s of middle Bi and the 2p orbital of O is beneficial to obtaining high saturation polarization.
When introducing (Bi)0.5Na0.5)0.7Sr0.3TiO3When is in contact with the substrate [ (Bi)0.5Na0.5)0.7Sr0.3]2+And Ti4+Respectively enter 0.9NaNbO3-0.1Bi(Mg0.667Nb0.333)O3The A site and the B site of the ceramic further destroy the long-range ferroelectric ordered structure of the ceramic, promote the formation of polar nano micro-regions and are beneficial to obtaining low residual polarization strength.
The high insulating property and wide band gap of MgO are beneficial to reducing dielectric loss and leakage current, and further higher breakdown strength is obtained.
(Bi0.5Na0.5)0.7Sr0.3TiO3Can promote the introduction of 0.9NaNbO3-0.1Bi(Mg0.667Nb0.333)O3The sintering of the ceramic obviously reduces the pore content and the grain size, thereby obtaining high breakdown strength.
The invention relates to a high-efficiency high-energy-storage-rate sodium niobate-based ceramic material and a preparation method thereof (1-x) [0.9NaNbO3-0.1Bi(Mg0.667Nb0.333)O3]-xmol％(Bi0.5Na0.5)0.7Sr0.3TiO3Wherein x is a molar ratio, and x is more than or equal to 0.05 and less than or equal to 0.4.
Referring to fig. 1 and fig. 2, the present invention provides a method for preparing a high-efficiency high-energy-storage-rate sodium niobate-based ceramic material, comprising: the method comprises the following steps:
s1: weighing high-purity Na2CO3、Nb2O5、Bi2O3MgO and Na2CO3、Bi2O3、SrCO3、 TiO2Separately mixing to obtain powder;
s2: putting the powder into a ball milling tank for wet ball milling, drying and sieving, pressing the powder into a column shape, and putting the column shape into an alumina crucible for sealing pre-sintering;
s3: then 0.9NaNbO is added3-0.1Bi(Mg0.667Nb0.333)O3And (Bi)0.5Na0.5)0.7Sr0.3TiO3After proportioning, pouring the mixture into a ball milling tank for wet ball milling again, quickly drying the mixture in a drying oven at 100 ℃, sieving the mixture, and pressing particles with the size of 60-120 meshes into round pieces by using a die;
s4: carrying out sealing sintering on the wafer in a muffle furnace;
s5: and polishing the sintered sample, coating high-temperature silver paste, sintering at high temperature and preserving heat to obtain the sodium niobate-based ceramic material.
The preparation method comprises the following steps of putting the powder into a ball milling tank for wet ball milling, drying and sieving, pressing the powder into a column shape, putting the column shape into an alumina crucible for sealing preburning, and specifically comprises the following steps:
according to the mass ratio of the powder, the zirconia balls and the absolute ethyl alcohol of 1: 2: 2, sequentially adding zirconia balls and absolute ethyl alcohol into a nylon tank, ball-milling for 4 hours, mixing and grinding, quickly drying at 100 ℃ to obtain powder, separating the powder from the zirconia balls by using a 60-mesh screen, and presintering the sieved powder in an alumina crucible to obtain powder.
The step of pre-burning in an alumina crucible comprises:
the presintering temperature is 850 ℃, the heat preservation time is 4 hours, and the heating rate is 5 ℃/min.
Then 0.9NaNbO is added3-0.1Bi(Mg0.667Nb0.333)O3And (Bi)0.5Na0.5)0.7Sr0.3TiO3After proportioning, pouring the mixture into a ball milling tank for wet ball milling again, quickly drying the mixture in an oven at 100 ℃,sieving is used, and 60-120 mesh granules are taken and pressed into round pieces by a mould:
grinding the pre-sintered powder and mixing the powder with 0.9NaNbO in proportion3-0.1Bi(Mg0.667Nb0.333)O3And (Bi)0.5Na0.5)0.7Sr0.3TiO3And thirdly, mixing the powder, the zirconia balls and the absolute ethyl alcohol according to the mass ratio of 1: 2: 2 are sequentially put into a nylon tank for ball milling for 4 hours, then taken out and put into an oven to be dried at 100 ℃;
then adding 5 wt% of polyvinyl alcohol (PVA) for granulation, sieving by using a sieve of 60 meshes and a sieve of 120 meshes, and pressing the granules with the size of 60-120 meshes into round pieces with the diameter of 8mm and the thickness of 1mm by using a die.
Before the step of hermetically sintering the wafer in a muffle furnace:
the wafer was allowed to gel at 550 ℃ for 4 hours at a rate of 1 ℃/min.
The sintered samples were polished to 0.12 ± 0.02 mm.
Polishing a sintered sample, coating high-temperature silver paste, sintering at high temperature and preserving heat to obtain the sodium niobate-based ceramic material, wherein the method comprises the following steps:
the high-temperature sintering and heat preservation method specifically comprises the following steps: sintering for 2 hours at 1180-1210 ℃.
The method specifically comprises the following steps: high-purity powder with the purity of more than or equal to 99 percent is mixed according to Na2CO3、Nb2O5、Bi2O3、MgO、SrCO3And TiO2Preparing (1-x) (0.9NN-0.1BMN) -xBNST as a raw material, wherein the mass ratio of the powder, the zirconia balls and the absolute ethyl alcohol is 1: 2: 1, sequentially adding zirconia balls and absolute ethyl alcohol into a nylon tank, ball-milling for 4 hours, mixing and grinding, then quickly drying at 100 ℃, separating the zirconia balls by using a screen, placing the sieved powder into an alumina crucible for presintering (reducing volatilization of low-melting-point oxides), wherein the presintering temperature is 850 ℃, the heat preservation time is 4 hours, the temperature rise rate is 5 ℃/min,
grinding the pre-sintered powder by an agate mortar, and mixing the powder with 0.9NaNbO according to a certain proportion3-0.1Bi(Mg0.667Nb0.333)O3And (Bi)0.5Na0.5)0.7Sr0.3TiO3And thirdly, mixing the powder, the zirconia balls and the absolute ethyl alcohol according to the mass ratio of 1: 2: 2 are sequentially put into a nylon tank for ball milling for 4 hours, and then are taken out and put into an oven to be dried at 100 ℃. And adding 5 wt% of polyvinyl alcohol (PVA) into the dried powder for granulation, sieving by using a sieve of 60 meshes and 120 meshes, pressing the granules of 60 meshes to 120 meshes into a wafer with the diameter of 8mm and the thickness of 1mm by using a mould, and carrying out gel discharge at 550 ℃ for 4 hours at the temperature rise rate of 1 ℃/min. And finally, sintering the wafers after the glue is discharged at 1180-1210 ℃ for 2 hours respectively to obtain the required ceramic material.
Table 1 lists 4 specific examples of the various constituents that make up the invention and their energy storage properties (the methods of preparation are described above).
Table 1:
the invention adopts a solid phase reaction method, and takes ethanol solution as a ball milling medium to carry out wet ball milling to obtain raw powder with uniform particle size; the high-performance energy storage ceramic is prepared by adopting a traditional sintering process. The solid solution ceramic material prepared by the invention has lower sintering temperature (less than or equal to 1210 ℃) and excellent energy storage performance [ W [rec＞4.00J/cm3And eta > 80.00%]And has great commercial application prospect.
The invention designs a sodium niobate-based ceramic material, namely lead-free relaxation ferroelectric ceramic, (1-x) [0.9NaNbO3-0.1Bi(Mg0.667Nb0.333)O3]-xmol％(Bi0.5Na0.5)0.7Sr0.3TiO3Wherein x is a molar ratio, and x is more than or equal to 0.05 and less than or equal to 0.4. The results show that the ceramic has extremely high energy storage density (7.72J/cm) when x is 0.43) And storeEnergy efficiency (83.80%). At the same time, a very stable energy storage density can be maintained in the temperature range of 20-160 ℃. Therefore, 0.6(0.9NN-0.1BMN) -0.4BNST lead-free solid solution is expected to be a promising high energy storage capacitor.
While the invention has been described with reference to a preferred embodiment, it will be understood by those skilled in the art that various changes in form and detail may be made therein without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (6)
1. A high-efficiency high-energy-storage-rate sodium niobate-based ceramic material is characterized by comprising the following chemical composition formula:
(1-x)[0.9NaNbO3-0.1Bi(Mg0.667Nb0.333)O3]-xmol％(Bi0.5Na0.5)0.7Sr0.3TiO3(0.05≤x≤0.4)。
2. the preparation method of the high-efficiency high-energy-storage-rate sodium niobate-based ceramic material as claimed in claim 1, comprising the steps of:
weighing high-purity Na2CO3、Nb2O5、Bi2O3MgO and Na2CO3、Bi2O3、SrCO3、TiO2Separately mixing to obtain powder;
putting the powder into a ball milling tank for wet ball milling, drying and sieving, pressing the powder into a column shape, and putting the column shape into an alumina crucible for sealing pre-sintering;
then 0.9NaNbO is added3-0.1Bi(Mg0.667Nb0.333)O3And (Bi)0.5Na0.5)0.7Sr0.3TiO3After proportioning, pouring the mixture into a ball milling tank for wet ball milling again, quickly drying the mixture in a drying oven at 100 ℃, sieving the mixture, and pressing particles with the size of 60-120 meshes into round pieces by using a die;
carrying out sealing sintering on the wafer in a muffle furnace;
and polishing the sintered sample, coating high-temperature silver paste, sintering at high temperature and preserving heat to obtain the sodium niobate-based ceramic material.
3. The preparation method of the sodium niobate-based ceramic material with high efficiency and high energy storage rate as claimed in claim 2, wherein the powder is put into a ball milling tank for wet ball milling, drying and sieving, and the powder is pressed into a column shape and put into an alumina crucible for sealing pre-sintering, and the method specifically comprises the following steps:
according to the mass ratio of the powder, the zirconia balls and the absolute ethyl alcohol of 1: 2: 2, sequentially adding zirconia balls and absolute ethyl alcohol into a nylon tank, ball-milling for 4 hours, mixing and grinding, quickly drying at 100 ℃ to obtain powder, separating the powder from the zirconia balls by using a 60-mesh screen, and presintering the sieved powder in an alumina crucible to obtain powder.
4. The method for preparing the sodium niobate-based ceramic material with high efficiency and high energy storage rate as claimed in claim 3, wherein the step of pre-sintering in an alumina crucible comprises:
the presintering temperature is 850 ℃, the heat preservation time is 4 hours, and the heating rate is 5 ℃/min.
5. The method for preparing the high-efficiency high-energy-storage-rate sodium niobate-based ceramic material according to claim 4, wherein 0.9NaNbO is added later3-0.1Bi(Mg0.667Nb0.333)O3And (Bi)0.5Na0.5)0.7Sr0.3TiO3After proportioning, pouring the mixture into a ball milling tank for wet ball milling again, quickly drying the mixture in a drying oven at 100 ℃, sieving the mixture by using a screen, and pressing particles with the size of 60-120 meshes into round pieces by using a die:
grinding the pre-sintered powder and mixing the powder with 0.9NaNbO in proportion3-0.1Bi(Mg0.667Nb0.333)O3And (Bi)0.5Na0.5)0.7Sr0.3TiO3Again according to the powder, zirconia balls and aluminaThe mass ratio of the water to the ethanol is 1: 2: 2 are sequentially put into a nylon tank for ball milling for 4 hours, then taken out and put into an oven to be dried at 100 ℃;
then adding 5 wt% of polyvinyl alcohol (PVA) for granulation, sieving by using a sieve of 60 meshes and a sieve of 120 meshes, and pressing the granules with the size of 60-120 meshes into round pieces with the diameter of 8mm and the thickness of 1mm by using a die.
6. The method for preparing the high-efficiency high-energy-storage-rate sodium niobate-based ceramic material according to claim 5, wherein before the step of hermetically sintering the wafer in a muffle furnace:
the wafer was allowed to gel at 550 ℃ for 4 hours at a rate of 1 ℃/min.
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| CN115368132A (en) * | 2022-07-21 | 2022-11-22 | 桂林理工大学 | Barium titanate-based ceramic material and preparation method thereof |
| CN116789449A (en) * | 2022-03-28 | 2023-09-22 | 中国科学院上海硅酸盐研究所 | High-energy-storage sodium niobate-based ferroelectric ceramic material with excellent temperature stability, and preparation method and application thereof |
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