CN112209713B - High-energy-storage and high-efficiency sodium niobate-based ceramic material and preparation method thereof - Google Patents
High-energy-storage and high-efficiency sodium niobate-based ceramic material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a sodium niobate-based ceramic material with high energy storage and high efficiency and a preparation method thereof, and the chemical composition formula is as follows: (1-x) NaNbO3-x mol% Bi (Mg0.5Sn0.5) O3 (0.03. ltoreq. x.ltoreq.0.09), wherein x is the molar ratio of Bi (Mg0.5Sn0.5) O3. The preparation method comprises the steps of preparing NaNbO3 based on Na2CO3 and Nb2O 5; preparing Bi (Mg0.5Sn0.5) O3 based on Bi2O3, MgO and SnO 2; mixing NaNbO3 and Bi (Mg0.5Sn0.5) O3 to obtain high-purity powder; adding zirconia balls and absolute ethyl alcohol, ball-milling for 5 hours, taking out, and drying in an oven at 100-110 ℃; adding 5 wt% of polyvinyl alcohol (PVA) for granulation; sieving with 60 and 120 mesh sieve; taking powder with the size of 60-120 meshes, pressing the powder into small cylinders with the diameter of 8mm and the thickness of 1.2mm by using a die, and discharging glue; and sintering the small cylinders after the glue is discharged at 1100-1250 ℃ for 2 hours respectively to obtain the required ceramic material. The solid solution ceramic material prepared by the invention has low sintering temperature (less than or equal to 1250 ℃), extremely high energy storage density and energy storage efficiency and great commercial application prospect.
Description
Technical Field
The invention relates to the field of energy storage materials, in particular to a sodium niobate-based ceramic material with high energy storage and high efficiency 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 cells). The solid-state capacitor is the energy storage mode preferentially selected by the pulse power technology by high power density (108W/kg), fast charge-discharge speed (nanosecond to microsecond) and long cycle life (50 ten thousand times), 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.
Dielectric capacitors for electrical energy storage have an ultra-high power density due to their ultra-fast charge/discharge rate, very suitable for pulsed power, compared to fuel cells and lithium ion batteriesAmong power sources, research is widely conducted. Generally, large saturation polarization (P)S) High breakdown strength (BDS) and low remanent polarization (P)r) Is crucial for achieving high energy storage densities. Currently, there are four representative dielectric materials for energy storage applications: linear Dielectrics (LDs), Ferroelectrics (FEs), relaxor ferroelectrics (REFs) and Antiferroelectrics (AFEs). LDs materials typically have a high BDS and a small PrBut low PmaxLimiting their use in high energy storage. At the same time, FEs have large PrAnd low WrecIt is difficult to optimally modify it, although the high polarization and dielectric of the FEs are desirable for energy storage properties. Has medium BDS and high PsNegligible PrLead element-based AFEs of (a) always achieve high energy storage densities. However, lead is a harmful element and seriously harms human health and environment, and the existing lead-free energy storage material has insufficient energy storage performance, so that the requirement of use cannot be met.
Disclosure of Invention
The invention aims to provide a sodium niobate-based ceramic material with high energy storage and high efficiency and a preparation method thereof, and aims to solve the problem that the existing lead-free energy storage material has poor energy storage performance and cannot meet the actual requirement.
In order to achieve the above object, in one aspect, the present invention provides a sodium niobate-based ceramic material with high energy storage and high efficiency, which has a chemical composition formula: (1-x) NaNbO3-xmol％Bi(Mg0.5Sn0.5)O3，0.03≤x≤0.09。
On the other hand, the invention also provides a preparation method of the sodium niobate-based ceramic material with high energy storage and high efficiency, which comprises the following steps:
based on Na2CO3And Nb2O5Preparation of NaNbO3；
Based on Bi2O3MgO and SnO2Preparation of Bi (Mg)0.5Sn0.5)O3；
Mixing NaNbO3And Bi (Mg)0.5Sn0.5)O3Proportioning to obtain high-purity powder;
adding zirconia balls and absolute ethyl alcohol, ball-milling for 5 hours, taking out, and drying in an oven at 100-110 ℃;
adding 5 wt% of polyvinyl alcohol for granulation;
sieving with 60 and 120 mesh sieve;
taking powder with the size of 60-120 meshes, pressing the powder into a cylinder with the diameter of 8mm and the thickness of 1.2mm by using a die, and removing glue;
and sintering the cylinders after glue discharging at 1100-1250 ℃ for 2 hours respectively to obtain the sodium niobate-based ceramic material with high energy storage and high efficiency.
Wherein the Na is based on2CO3And Nb2O5Preparation of NaNbO3The method comprises the following specific steps:
mixing Na2CO3And Nb2O5Mixing;
adding zirconia balls and absolute ethyl alcohol, ball-milling for 4 hours, and quickly drying at 100-110 ℃;
removing zirconia balls by using a screen, and performing sealing preburning in an alumina crucible to obtain NaNbO3。
Removing zirconia balls by using a screen, and preburning in an alumina crucible to obtain NaNbO3The temperature of the heat preservation pipe is 900 ℃, the heat preservation time is 5 hours, and the heating rate is 5 ℃/min.
Wherein, the base is Bi2O3MgO and SnO2Preparation of Bi (Mg)0.5Sn0.5)O3The method comprises the following specific steps:
adding Bi2O3MgO and SnO2Mixing;
adding zirconia balls and absolute ethyl alcohol, ball-milling for 4 hours, and quickly drying at 100-110 ℃;
removing zirconia balls by using a screen, and performing sealing preburning in an alumina crucible to obtain Bi (Mg)0.5Sn0.5)O3。
The invention relates to a sodium niobate-based ceramic material with high energy storage and high efficiency and a preparation method thereof, wherein the chemical composition formula is as follows: (1-x) NaNbO3-xmol％Bi(Mg0.5Sn0.5)O3(0.03≤x≤0.09)；
Wherein X is Bi (Mg)0.5Sn0.5)O3In a molar ratio of (A) to (B), the preparation process comprising a Na-based2CO3And Nb2O5Preparation of NaNbO3(ii) a Based on Bi2O3MgO and SnO2Preparation of Bi (Mg)0.5Sn0.5)O3(ii) a Mixing NaNbO3And Bi (Mg)0.5Sn0.5)O3Proportioning to obtain high-purity powder; adding zirconia balls and absolute ethyl alcohol, ball-milling for 5 hours, taking out, and drying in an oven at 100-110 ℃; adding 5 wt% of polyvinyl alcohol for granulation; sieving with 60 and 120 mesh sieve; taking powder with the size of 60-120 meshes, pressing the powder into small cylinders with the diameter of 8mm and the thickness of 1.2mm by using a die, and discharging glue; and sintering the small cylinders after the glue is discharged at 1100-1250 ℃ for 2 hours respectively to obtain the required ceramic material. Performing wet ball milling in a certain ethanol solution by adopting a solid-phase synthesis method to obtain raw powder with fine particles and uniform particle size; the high-performance relaxation ferroelectric energy storage ceramic is prepared by adopting a heat treatment sintering process. The solid solution ceramic material prepared by the invention has lower sintering temperature (less than or equal to 1250 ℃) and excellent energy storage performance (extremely high energy storage density (W)rec) And energy storage efficiency (eta)), can solve the problem that the existing lead-free energy storage material has poor energy storage performance and cannot meet the actual requirement, and has great commercial application prospect.
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 a method for preparing a sodium niobate-based ceramic material with high energy storage and high efficiency according to the present invention;
FIG. 2 shows that the Na-base of the present invention2CO3And Nb2O5Preparation of NaNbO3A flow chart of (a);
FIG. 3 shows Bi-based compositions of the present invention2O3MgO and SnO2Preparation of Bi (Mg)0.5Sn0.5)O3A flow chart of (1);
figure 4 is a flow chart of the present invention for screening using 60 and 120 mesh screens.
Detailed Description
Reference will now be made in detail to embodiments of the present invention, examples of which are illustrated in the accompanying drawings, wherein like or similar reference numerals refer to the same or similar elements or elements having the same or similar function throughout. The embodiments described below with reference to the drawings are illustrative and intended to be illustrative of the invention and are not to be construed as limiting the invention.
In a first aspect, the present invention provides a sodium niobate-based ceramic material with high energy storage and high efficiency, which has a chemical composition formula:
(1-x)NaNbO3-xmol％Bi(Mg0.5Sn0.5)O3(0.03 ≦ x ≦ 0.09) where x is Bi (Mg)0.5Sn0.5)O3The molar ratio of x is more than or equal to 0.03 and less than or equal to 0.09.
The Bi (Mg)0.5Sn0.5)O3Has the following advantages:
Bi(Mg0.5Sn0.5)O3the 6s of the medium Bi and the 2p orbital hybridization of O are favorable for obtaining high saturation polarization intensity; when Bi (Mg) is introduced0.5Sn0.5)O3When Bi is present3+And (Mg)0.5Sn0.5)3+Respectively enter into NaNbO3The A site and the B site of the ceramic break the long-range ordered structure of the ceramic, promote the formation of polar nano micro-regions and are beneficial to obtaining low residual polarization strength; high insulating property of MgO and SnO2The wide energy gap is beneficial to reducing dielectric loss and leakage current, and further higher breakdown strength is obtained; bi (Mg)0.5Sn0.5)O3The introduction of (A) can promote NaNbO3The sintering of the ceramic obviously reduces the pore content and the grain size, thereby obtaining high breakdown strength.
The ceramic has extremely high energy storage density and energy storage efficiency. At the same time, a very stable energy storage density can be maintained in the temperature range of 20-180 ℃. Thus, (1-x) NaNbO3-xmol％Bi(Mg0.5Sn0.5)O3The lead-free solid solution can be used as a high energy storage capacitor with a very promising prospect, and the problem that the existing lead-free energy storage material has poor energy storage performance and cannot meet the actual requirement is solved.
In a second aspect, referring to fig. 1, the present invention further provides a method for preparing a sodium niobate-based ceramic material with high energy storage and high efficiency, including:
s101 is based on Na2CO3And Nb2O5Preparation of NaNbO3；
Referring to fig. 2, the specific steps include:
s201 converting Na into2CO3And Nb2O5Mixing;
s202, adding zirconia balls and absolute ethyl alcohol, ball-milling for 4 hours, and quickly drying at 100-110 ℃;
the zirconia ceramic ball has high strength and toughness, good wear resistance, high temperature resistance, corrosion resistance, high rigidity, no magnetic conduction and electric insulation at normal temperature. As an abrasive, the absolute ethyl alcohol is added for wet ball milling, so that the grinding can be more complete, and the absolute ethyl alcohol is easy to remove by evaporation after grinding.
S203, removing zirconia balls by using a screen, and performing sealing pre-burning in an alumina crucible to obtain NaNbO3。
The temperature of the sealing pre-sintering is 900 ℃, the holding time is 5 hours, the heating rate is 5 ℃/min, and the sealing pre-sintering is used for reducing the volatilization of components and synthesizing a main crystal phase.
S102 is based on Bi2O3MgO and SnO2Preparation of Bi (Mg)0.5Sn0.5)O3；
Referring to fig. 3, the specific steps include:
s301 reacting Bi2O3MgO and SnO2Mixing;
s302, adding zirconia balls and absolute ethyl alcohol, ball-milling for 4 hours, and quickly drying at 100-110 ℃;
s303, removing zirconia balls by using a screen, and performing sealing pre-burning in an alumina crucible to obtain Bi (Mg)0.5Sn0.5)O3。
S103, reacting NaNbO3And Bi (Mg)0.5Sn0.5)O3Proportioning to obtain high-purity powder;
s104, adding zirconia balls and absolute ethyl alcohol, ball-milling for 5 hours, taking out, and drying in an oven at 100-110 ℃;
the mass ratio of the high-purity powder to the zirconia balls to the absolute ethyl alcohol is 1: 2: 1. previously prepared NaNbO3And preparing Bi (Mg)0.5Sn0.5)O3The same ratios may be used.
S105, adding 5 wt% of polyvinyl alcohol (PVA) for granulation;
s106, sieving by using a sieve with 60 and 120 meshes;
referring to fig. 4, the specific steps are:
s401, adopting a 60-mesh screen to carry out primary screening;
s402, adding the particles left on the 60-mesh screen into zirconia balls for re-grinding;
s403, sieving the reground particles again by using a 60-mesh sieve;
s404 the granules passing through the 60-mesh sieve are secondarily sieved using a 120-mesh sieve.
The large particles left on the 60-mesh screen are ground again, so that most of the large particles can be broken into smaller particles, the large particles can be used within the range of 60-120 meshes according to the use requirement, and the utilization rate of materials can be improved.
S107, taking powder with the size of 60-120 meshes, pressing the powder into a cylinder with the diameter of 8mm and the thickness of 1.2mm by using a die, and discharging glue;
the rubber discharging condition is that rubber is discharged for 5 hours at 550 ℃, and the heating rate is 1 ℃/min.
S108, sintering the cylinders after glue discharging at 1100-1250 ℃ for 2 hours respectively to obtain the required ceramic material.
Polishing the sintered sample to (0.15 +/-0.03) mm, coating high-temperature silver paste, sintering at 700 ℃, and then carrying out related electrical test analysis.
The results of the energy storage performance test of the materials obtained by selecting four different blending schemes of x 0.03, x 0.05, x 0.075 and x 0.09 at step S103 are shown in table 1, wherein W is 0.03, x is 0.05, and x is 0.09recRepresenting the energy storage density, η represents the energy storage efficiency:
TABLE 1
From table 1, it can be found that when x is 0.09, the ceramic has an extremely high energy storage density (4.93J/cm)3) And energy storage efficiency (81.4%). This indicates that (1-x) NaNbO3-xmol％Bi(Mg0.5Sn0.5)O3Ceramics may become a new lead-free candidate material for high energy storage applications.
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 (4)
1. A preparation method of a sodium niobate-based ceramic material with high energy storage and high efficiency is disclosed, wherein the chemical composition formula of the sodium niobate-based ceramic material is as follows: (1-x) NaNbO3-xmol％Bi(Mg0.5Sn0.5)O3And x is 0.09, characterized in that,
the method comprises the following steps:
based on Na2CO3And Nb2O5Preparation of NaNbO3；
Based on Bi2O3MgO and SnO2Preparation of Bi (Mg)0.5Sn0.5)O3；
Mixing NaNbO3And Bi (Mg)0.5Sn0.5)O3Proportioning to obtain high-purity powder;
adding zirconia balls and absolute ethyl alcohol, ball-milling for 5 hours, taking out, and drying in an oven at 100-110 ℃;
adding 5 wt% of polyvinyl alcohol for granulation;
sieving by using a sieve with 60 and 120 meshes, and comprises the following specific steps: sieving with 60 mesh sieve; adding the particles left on the 60-mesh screen into zirconia balls for re-grinding; sieving the reground particles again by using a 60-mesh sieve; the granules passing through the 60-mesh screen are secondarily screened by using a 120-mesh screen;
taking powder with the size of 60-120 meshes, pressing the powder into a cylinder with the diameter of 8mm and the thickness of 1.2mm by using a die, and discharging glue;
and sintering the cylinders after glue discharging at 1100-1250 ℃ for 2 hours respectively to obtain the sodium niobate-based ceramic material with high energy storage and high efficiency.
2. The method for preparing a sodium niobate-based ceramic material with high energy storage and high efficiency as claimed in claim 1,
the Na base2CO3And Nb2O5Preparation of NaNbO3The method comprises the following specific steps:
mixing Na2CO3And Nb2O5Mixing;
adding zirconia balls and absolute ethyl alcohol, ball-milling for 4 hours, and quickly drying at 100-110 ℃;
removing zirconia balls by using a screen, and performing sealing preburning in an alumina crucible to obtain NaNbO3。
3. The method for preparing a sodium niobate-based ceramic material with high energy storage and high efficiency as claimed in claim 2,
removing zirconia balls by using a screen, and performing sealing preburning in an alumina crucible to obtain NaNbO3The temperature of the mixture is 900 ℃, and the heat preservation time is 5 hoursThe temperature rise rate was 5 ℃/min.
4. The method for preparing a sodium niobate-based ceramic material with high energy storage and high efficiency as claimed in claim 1,
the base is based on Bi2O3MgO and SnO2Preparation of Bi (Mg)0.5Sn0.5)O3The method comprises the following specific steps:
adding Bi2O3MgO and SnO2Mixing;
adding zirconia balls and absolute ethyl alcohol, ball-milling for 4 hours, and quickly drying at 100-110 ℃;
removing zirconia balls by using a screen, and performing sealing preburning in an alumina crucible to obtain Bi (Mg)0.5Sn0.5)O3。
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Application publication date: 20210112 Assignee: Guilin Jingchao New Energy Co.,Ltd. Assignor: GUILIN University OF TECHNOLOGY Contract record no.: X2022450000026 Denomination of invention: A high energy storage and high efficiency sodium niobate based ceramic material and its preparation method Granted publication date: 20220510 License type: Common License Record date: 20221117 |