CN116639971A - Strontium zirconate doped copper sodium calcium cadmium titanate ceramic with high energy storage density and preparation method thereof - Google Patents
Strontium zirconate doped copper sodium calcium cadmium titanate ceramic with high energy storage density and preparation method thereof Download PDFInfo
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- 239000000919 ceramic Substances 0.000 title claims abstract description 90
- FFQALBCXGPYQGT-UHFFFAOYSA-N 2,4-difluoro-5-(trifluoromethyl)aniline Chemical compound NC1=CC(C(F)(F)F)=C(F)C=C1F FFQALBCXGPYQGT-UHFFFAOYSA-N 0.000 title claims abstract description 65
- 238000004146 energy storage Methods 0.000 title claims abstract description 58
- -1 copper sodium calcium cadmium Chemical compound 0.000 title claims abstract description 54
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 title claims abstract description 51
- 238000002360 preparation method Methods 0.000 title abstract description 15
- 239000011734 sodium Substances 0.000 claims abstract description 50
- 239000011575 calcium Substances 0.000 claims abstract description 42
- 239000010949 copper Substances 0.000 claims abstract description 40
- 238000000034 method Methods 0.000 claims abstract description 18
- 239000000126 substance Substances 0.000 claims abstract description 8
- 229910052712 strontium Inorganic materials 0.000 claims abstract description 5
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 claims abstract description 5
- 239000000843 powder Substances 0.000 claims description 37
- 238000010438 heat treatment Methods 0.000 claims description 23
- 238000005245 sintering Methods 0.000 claims description 13
- 238000000227 grinding Methods 0.000 claims description 12
- 238000000498 ball milling Methods 0.000 claims description 9
- 238000004321 preservation Methods 0.000 claims description 8
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 7
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 7
- 239000003292 glue Substances 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 5
- 238000003825 pressing Methods 0.000 claims description 4
- 239000002994 raw material Substances 0.000 claims description 4
- 229910010413 TiO 2 Inorganic materials 0.000 claims description 3
- 239000011230 binding agent Substances 0.000 claims description 3
- 239000011812 mixed powder Substances 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 238000000748 compression moulding Methods 0.000 claims description 2
- 230000015556 catabolic process Effects 0.000 abstract description 34
- 239000000463 material Substances 0.000 abstract description 10
- 239000013078 crystal Substances 0.000 abstract description 6
- 230000002159 abnormal effect Effects 0.000 abstract description 3
- 229910052726 zirconium Inorganic materials 0.000 abstract description 3
- 239000011232 storage material Substances 0.000 abstract description 2
- 230000002401 inhibitory effect Effects 0.000 abstract 1
- 238000009413 insulation Methods 0.000 abstract 1
- 229910010293 ceramic material Inorganic materials 0.000 description 22
- 230000000052 comparative effect Effects 0.000 description 12
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 8
- 229910052709 silver Inorganic materials 0.000 description 8
- 239000004332 silver Substances 0.000 description 8
- 238000012360 testing method Methods 0.000 description 8
- 244000137852 Petrea volubilis Species 0.000 description 7
- 230000001680 brushing effect Effects 0.000 description 7
- 238000005498 polishing Methods 0.000 description 7
- 238000005303 weighing Methods 0.000 description 7
- 239000003989 dielectric material Substances 0.000 description 6
- 239000003990 capacitor Substances 0.000 description 4
- 238000012986 modification Methods 0.000 description 4
- 230000004048 modification Effects 0.000 description 4
- 238000001237 Raman spectrum Methods 0.000 description 3
- 239000000853 adhesive Substances 0.000 description 3
- 230000001070 adhesive effect Effects 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- 238000007599 discharging Methods 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 230000004075 alteration Effects 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 230000033001 locomotion Effects 0.000 description 2
- 238000000465 moulding Methods 0.000 description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 206010063385 Intellectualisation Diseases 0.000 description 1
- 229910002661 O–Ti–O Inorganic materials 0.000 description 1
- 229910002655 O−Ti−O Inorganic materials 0.000 description 1
- 238000001069 Raman spectroscopy Methods 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 229910052793 cadmium Inorganic materials 0.000 description 1
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- HAUBPZADNMBYMB-UHFFFAOYSA-N calcium copper Chemical compound [Ca].[Cu] HAUBPZADNMBYMB-UHFFFAOYSA-N 0.000 description 1
- AOWKSNWVBZGMTJ-UHFFFAOYSA-N calcium titanate Chemical compound [Ca+2].[O-][Ti]([O-])=O AOWKSNWVBZGMTJ-UHFFFAOYSA-N 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 230000001939 inductive effect Effects 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 230000009022 nonlinear effect Effects 0.000 description 1
- 229910052574 oxide ceramic Inorganic materials 0.000 description 1
- 239000011224 oxide ceramic Substances 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
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Abstract
The application belongs to the technical field of energy storage materials, and discloses strontium zirconate doped copper sodium calcium cadmium titanate ceramic with high energy storage density and a preparation method thereof. The chemical general formula of the ceramic is Na 0.3 Ca 0.2 Cd 0.5 Cu 3 Ti 4 O 12 ‑xSrZrO 3 Wherein x is SrZrO 3 Take up Na 0.3 Ca 0.2 Cd 0.5 Cu 3 Ti 4 O 12 0 mass percent of (C)<x is less than or equal to 0.1. The method synthesizes the high dielectric constant material of copper sodium calcium cadmium titanate, adopts strontium zirconate doping to obtain Na 0.3 Ca 0.2 Cd 0.5 Cu 3 Ti 4 O 12 ‑xSrZrO 3 A ceramic; inhibiting abnormal growth of copper sodium calcium cadmium titanate crystal grains by utilizing strontium and zirconium ions, and enhancingThe insulation property of grain boundary and the density of material improve the breakdown field strength, and simultaneously have high dielectric constant and breakdown field strength, and the energy storage density can reach 1.15-2.23J/cm 3 。
Description
Technical Field
The application belongs to the technical field of energy storage materials, and particularly relates to strontium zirconate doped copper sodium calcium cadmium titanate ceramic with high energy storage density and a preparation method thereof.
Background
The development of information technology has placed demands on miniaturization and intellectualization of electronic components, and dielectric materials with high dielectric constants and energy storage densities are key to solving this problem. In recent years, researchers have reported a range of high dielectric constant ceramic materials, and the smaller breakdown field strength of these materials tends to result in a low energy storage density. Copper calcium titanate (CaCu) 3 Ti 4 O 12 CCTO) non-ferroelectric dielectric ceramic materials are members of the ACTO family, with ceramics having dielectric constants up to 10 4 The material has better temperature stability and no structural phase change at 100-600K, and is expected to be widely applied to high-density energy storage and high-dielectric capacitors.
The energy storage density of ACTO-type dielectrics can be expressed as:wherein ε is 0 、ε r 、E b The dielectric constant, the relative dielectric constant and the breakdown strength in vacuum, respectively. From the above formula, the energy density is proportional to the dielectric constant and the breakdown strength; in order to maximize the charge that can be accommodated by the capacitor, the dielectric material needs to have a high dielectric constant and breakdown field strength. Whereas studies have shown that the dielectric constant and breakdown strength of a single material can only be enhanced at the expense of each other. Therefore, designing and developing a dielectric material having both a high dielectric constant and a high breakdown field strength thereof is an effective way to achieve a high energy storage density of the dielectric material. Yang Zupei, et al, university of Shaanxi, 2020, by CdCu 3 Ti 4 O 12 Alumina is added in the ceramic, so that the breakdown field intensity of the ceramic is improved, and the optimal energy storage density is 1.52mJ/cm 3 (Z.Peng,J.Wang,X.Zhou,J.Zhu,X.Lei,P.Liang,X.Chao,Z.Yang,Grain engineering inducing high energy storage in CdCu 3 Ti 4 O 12 ceramics, ceramics International (2020) 14425-14430); 2022 he, heBy adding silica to CdCu 3 Ti 4 O 12 In the method, the breakdown field strength of the ceramic material is improved, and the maximum energy storage density reaches 1.77mJ/cm 3 (Z.Peng,J.Wang,F.Zhang,S.Xu,X.Lei,P.Liang,L.Wei,D.Wu,X.Chao,Z.Yang,High energy storage and colossal permittivity CdCu 3 Ti 4 O 12 oxide ceramics, ceramics International (2022) 4255-4260). These results indicate the benefit and potential application value of developing such studies.
At present, researchers are still continuously exploring new high-dielectric-constant ceramic materials, and the lower breakdown field intensity of the materials is also a key problem for preventing the energy storage density of the materials from being improved, so that the breakdown field intensity of the high-dielectric-constant ceramic materials is necessarily improved while the high-dielectric-constant ceramic materials are developed, and the aim of improving the energy storage density of the high-dielectric-constant ceramic materials is fulfilled.
Disclosure of Invention
Aiming at solving the problem that the prior art has lower breakdown field intensity and prevents the improvement of energy storage density, the application provides strontium zirconate doped copper sodium calcium cadmium titanate ceramic with high energy storage density and a preparation method thereof, and synthesizes the copper sodium calcium cadmium titanate (Na) with high dielectric constant which occupies Ca position by I/II-valence mixture 0.3 Ca 0.2 Cd 0.5 Cu 3 Ti 4 O 12 NCCCTO) ceramic material, thereby doping a second phase strontium zirconate (SrZrO) 3 ) The breakdown field intensity of the ceramic is improved, and finally the strontium zirconate doped sodium copper calcium cadmium titanate ceramic material with high energy storage density is prepared, the high dielectric constant of the ceramic is maintained while the breakdown field intensity of the ceramic is improved, the dielectric constant at 1kHz is 6100-8300, the breakdown field intensity is 56-82 kV/cm, and the energy storage density is 1.15-2.23J/cm 3 Thereby achieving a significant increase in energy storage density.
In order to achieve the above purpose, the technical scheme adopted by the application is as follows:
the first object of the application is to provide a strontium zirconate doped copper sodium calcium cadmium titanate ceramic with high energy storage density, wherein the chemical formula of the ceramic is Na 0.3 Ca 0.2 Cd 0.5 Cu 3 Ti 4 O 12 -xSrZrO 3 Wherein x is SrZrO 3 Take up Na 0.3 Ca 0.2 Cd 0.5 Cu 3 Ti 4 O 12 0 mass percent of (C)<x≤0.1。
Preferably, wherein, x is more than or equal to 0.02 and less than or equal to 0.08.
The second purpose of the application is to provide a preparation method of the strontium zirconate doped with copper sodium calcium cadmium titanate ceramic with high energy storage density, which comprises the following steps:
s1, selecting Na 2 CO 3 、CaCO 3 、CdO、CuO、TiO 2 、SrCO 3 And ZrO(s) 2 Is raw material powder, according to the composition general formula Na 0.3 Ca 0.2 Cd 0.5 Cu 3 Ti 4 O 12 And SrZrO 3 Batching, grinding to obtain uniformly mixed powder A and powder B respectively;
s2, sintering the powder A to obtain Na 0.3 Ca 0.2 Cd 0.5 Cu 3 Ti 4 O 12 Powder C; sintering the powder B to obtain SrZrO 3 Powder D; powder C and powder D are mixed according to a chemical formula Na 0.3 Ca 0.2 Cd 0.5 Cu 3 Ti 4 O 12 -xSrZrO 3 Mixing proportionally, grinding, adding binder, granulating, and press molding to obtain ceramic blank;
s3, firstly removing glue from the ceramic blank, and then heating and preserving heat to obtain the strontium zirconate doped copper sodium calcium cadmium titanate ceramic.
Preferably, in S1, the grinding mode is ball milling, and the time is 12-24 hours.
Preferably, in S2, the sintering temperature of the powder A is 850-950 ℃, the heat preservation time is 6-8 h, and the heating rate is 2-3 ℃/min.
Preferably, in S2, the sintering temperature of the powder B is 1100-1200 ℃, the heat preservation time is 3-4 h, and the heating rate is 3-4 ℃/min.
Preferably, in S2, the binder is polyvinyl alcohol, and the addition amount of the polyvinyl alcohol is 3-4wt% of the mass of the ground powder.
Preferably, in S2, the pressure intensity of the compression molding is 200-250 MPa; the size of the ceramic body is 1cm in diameter and 0.7-0.8 mm in thickness.
Preferably, in S3, the temperature of the adhesive discharge is 580-620 ℃, the heat preservation time is 2-3 h, the heating rate is 2-3 ℃/min, the heating temperature is increased to 1150 ℃, the heat preservation time is 6-8 h, and the heating rate is 3-5 ℃/min.
Compared with the prior art, the application has the beneficial effects that:
(1) The application synthesizes a novel high dielectric constant ceramic material of sodium, calcium and cadmium (Na) 0.3 Ca 0.2 Cd 0.5 Cu 3 Ti 4 O 12 ) By doping strontium zirconate (SrZrO 3 ) The abnormal growth of the copper sodium calcium cadmium titanate crystal grains is inhibited by utilizing strontium and zirconium ions, the insulativity of the crystal boundary and the compactness of the material are enhanced, the breakdown field intensity is obviously improved, and finally the strontium zirconate doped copper sodium calcium cadmium titanate (Na 0.3 Ca 0.2 Cd 0.5 Cu 3 Ti 4 O 12 -xSrZrO 3 ) The ceramic has high dielectric constant and breakdown field strength, and the energy storage density can reach 1.15-2.23J/cm 3 。
(2) The preparation method of the ceramic material is simple, low in cost and good in repeatability, and is suitable for industrial production, when x=0.05, the ceramic breakdown field strength is 82kV/cm, the dielectric constant is 7500 at 1kHz, and the energy storage density is 2.23J/cm 3 Has very important application value in the fields of high-density energy storage, high dielectric capacitors and the like.
Drawings
FIG. 1 is an XRD pattern of strontium zirconate doped copper sodium calcium cadmium titanate ceramics prepared in accordance with the present application and with examples 1-5 and comparative example 1;
FIG. 2 is a Raman spectrum diagram of strontium zirconate doped copper sodium calcium cadmium titanate ceramics prepared in examples 1-5 and comparative example 1 of the present application;
FIG. 3 is a graph showing the variation of dielectric constant with frequency of strontium zirconate doped copper sodium calcium cadmium titanate ceramics prepared in examples 1-5 and comparative example 1 of the present application;
FIG. 4 is a graph showing the nonlinear coefficient, breakdown field strength and energy storage density of strontium zirconate doped copper sodium calcium cadmium titanate ceramics prepared in examples 1-5 and comparative example 1 according to the present application.
Detailed Description
The technical solutions in the embodiments of the present application will be clearly and completely described below in conjunction with the data in the embodiments of the present application, and it is apparent that the described embodiments are only some embodiments of the present application, not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the application without making any inventive effort, are intended to be within the scope of the application.
It should be noted that the technical terms used in the present application are only for describing specific embodiments, and are not intended to limit the scope of the present application, and various raw materials, reagents, instruments and equipment used in the following embodiments of the present application may be purchased commercially or prepared by existing methods unless otherwise specifically described.
Strontium zirconate doped copper sodium calcium cadmium titanate ceramic with high energy storage density, wherein the chemical general formula of the ceramic is Na 0.3 Ca 0.2 Cd 0.5 Cu 3 Ti 4 O 12 -xSrZrO 3 Wherein 0 is<x is less than or equal to 0.1, preferably, 0.02 is less than or equal to 0.08.
By adding strontium zirconate, the abnormal growth of copper sodium calcium cadmium titanate crystal grains is inhibited by strontium and zirconium ions, the insulativity of crystal boundaries and the density of materials are enhanced, the breakdown field intensity is obviously improved, and finally, the strontium zirconate doped copper sodium calcium cadmium titanate ceramic has high dielectric constant and breakdown field intensity, and the aim of improving the energy storage density is achieved, wherein the dielectric constant of the ceramic material is 6100-8300 under 1kHz, the breakdown field intensity is 56-82 kV/cm, and the energy storage density is 1.15-2.23J/cm 3 。
The preparation method of the strontium zirconate doped copper sodium calcium cadmium titanate ceramic with high energy storage density comprises the following steps:
s1, selecting Na 2 CO 3 、CaCO 3 、CdO、CuO、TiO 2 、SrCO 3 And ZrO(s) 2 Is raw material powder, according to the composition general formula Na 0.3 Ca 0.2 Cd 0.5 Cu 3 Ti 4 O 12 And SrZrO 3 Proportioning, fully ball milling for 12-24 hours to respectively obtain evenly mixed powder A and powder B;
s2, heating the powder A to 850-950 ℃ at 2-3 ℃/min, and sintering in air atmosphere for 6-8 h to obtain Na 0.3 Ca 0.2 Cd 0.5 Cu 3 Ti 4 O 12 Powder C; heating the powder B to 1100-1200 ℃ at 3-4 ℃/min, and sintering for 3-4 h in air atmosphere to obtain SrZrO 3 Powder D; powder C and powder D are mixed according to a chemical formula Na 0.3 Ca 0.2 Cd 0.5 Cu 3 Ti 4 O 12 -xSrZrO 3 Mixing proportionally, grinding, adding polyvinyl alcohol accounting for 3-4wt% of the powder mass, granulating, and pressing under 200-250 MPa to obtain a ceramic blank with the diameter of 1cm and the thickness of 0.7-0.8 mm;
s3, heating the ceramic blank to 580-620 ℃ at 2-3 ℃/min, preserving heat for 2-3 h, discharging glue, heating to 1150 ℃ at 3-5 ℃/min, preserving heat for 6-8 h, and cooling along with a furnace to obtain the strontium zirconate doped copper sodium calcium cadmium titanate ceramic.
The present application will be further illustrated by the following examples.
Example 1
A strontium zirconate doped copper sodium calcium cadmium titanate ceramic with high energy storage density comprises Na 0.3 Ca 0.2 Cd 0.5 Cu 3 Ti 4 O 12 -0.05SrZrO 3 。
The preparation method of the strontium zirconate doped copper sodium calcium cadmium titanate ceramic with high energy storage density comprises the following steps:
s1, according to the general formula Na 0.3 Ca 0.2 Cd 0.5 Cu 3 Ti 4 O 12 Weighing 0.31797g of Na 2 CO 3 、0.40036gCaCO 3 、1.2841gCdO、4.773gCuO、5.1096gTiO 2 Placing the powder into a ball milling tank, and then placing the ball milling tank into a ball mill for fully grinding for 16 hours to obtain powder A; according to the general formula SrZrO 3 1.4763gSrCO is weighed 3 、1.2322gZrO 2 Placing in a ball milling tank, and then placing the ball milling tank in a ball mill for sufficiently grinding for 16hObtaining powder B;
s2, heating the powder A to 900 ℃ at a speed of 3 ℃/min, and sintering for 7h in an air atmosphere to obtain Na 0.3 Ca 0.2 Cd 0.5 Cu 3 Ti 4 O 12 Powder C; heating the powder B to 1150 ℃ at a speed of 4 ℃/min, and sintering for 4 hours in an air atmosphere to obtain SrZrO 3 Powder D; powder D is pressed by Na 0.3 Ca 0.2 Cd 0.5 Cu 3 Ti 4 O 12 -0.05SrZrO 3 Adding the powder C in the mass percentage of the chemical formula, fully grinding for 18 hours, adding a polyvinyl alcohol adhesive accounting for 3wt% of the powder mass, granulating, and pressing at 220MPa to obtain a ceramic blank with the diameter of 1cm and the thickness of 0.8 mm;
s3, heating the ceramic blank to 600 ℃ at a speed of 2 ℃/min, preserving heat for 3 hours, discharging glue, heating to 1150 ℃ at a speed of 5 ℃/min, preserving heat for 8 hours, and cooling along with a furnace to obtain Na 0.3 Ca 0.2 Cd 0.5 Cu 3 Ti 4 O 12 -0.05SrZrO 3 And (3) ceramics.
Polishing the sintered ceramic sample to 200 μm with sand paper, brushing silver paste on the upper and lower surfaces of the ceramic, and testing electrical properties, wherein the dielectric constant of the ceramic material is 7500 at 1kHz, the breakdown field strength is 82kV/cm, and the energy density is 2.23J/cm 3 。
Example 2
A strontium zirconate doped copper sodium calcium cadmium titanate ceramic with high energy storage density comprises Na 0.3 Ca 0.2 Cd 0.5 Cu 3 Ti 4 O 12 -0.02SrZrO 3 。
The preparation method is the same as in example 1, except that: according to the general formula Na 0.3 Ca 0.2 Cd 0.5 Cu 3 Ti 4 O 12 Weighing 0.31797g of Na 2 CO 3 、0.40036gCaCO 3 、1.2841gCdO、4.773gCuO、5.1096gTiO 2 The method comprises the steps of carrying out a first treatment on the surface of the According to the general formula SrZrO 3 0.59025gSrCO is weighed 3 、0.49288gZrO 2 。
Polishing the sintered ceramic sample to 200 μm with sand paper, brushing silver paste on the upper and lower surfaces of the ceramic, and performing electrical property measurementThe ceramic material obtained was tested to have a dielectric constant of 8300 at 1kHz, a breakdown field strength of 56kV/cm and an energy density of 1.15J/cm 3 。
Example 3
A strontium zirconate doped copper sodium calcium cadmium titanate ceramic with high energy storage density comprises Na 0.3 Ca 0.2 Cd 0.5 Cu 3 Ti 4 O 12 -0.08SrZrO 3 。
The preparation method is the same as in example 1, except that: according to the general formula Na 0.3 Ca 0.2 Cd 0.5 Cu 3 Ti 4 O 12 Weighing 0.31797g of Na 2 CO 3 、0.40036gCaCO 3 、1.2841gCdO、4.773gCuO、5.1096gTiO 2 The method comprises the steps of carrying out a first treatment on the surface of the According to the general formula SrZrO 3 2.36208gSrCO is weighed 3 、1.97152gZrO 2 。
Polishing the sintered ceramic sample to 200 μm with sand paper, brushing silver paste on the upper and lower surfaces of the ceramic, and testing electrical properties, wherein the dielectric constant of the obtained ceramic material is 6600 at 1kHz, the breakdown field strength is 75kV/cm, and the energy density is 1.64J/cm 3 。
Example 4
A strontium zirconate doped copper sodium calcium cadmium titanate ceramic with high energy storage density comprises Na 0.3 Ca 0.2 Cd 0.5 Cu 3 Ti 4 O 12 -0.1SrZrO 3 。
The preparation method is the same as in example 1, except that: according to the general formula Na 0.3 Ca 0.2 Cd 0.5 Cu 3 Ti 4 O 12 Weighing 0.31797g of Na 2 CO 3 、0.40036gCaCO 3 、1.2841gCdO、4.773gCuO、5.1096gTiO 2 The method comprises the steps of carrying out a first treatment on the surface of the According to the general formula SrZrO 3 2.9526gSrCO is weighed 3 、2.4644gZrO 2 。
Polishing the sintered ceramic sample to 200 μm with sand paper, brushing silver paste on the upper and lower surfaces of the ceramic, and testing electrical properties, wherein the dielectric constant of the obtained ceramic material is 6100 at 1kHz, the breakdown field strength is 70kV/cm, and the energy density is 1.32J/cm 3 。
Example 5
A strontium zirconate doped copper sodium calcium cadmium titanate ceramic with high energy storage density comprises Na 0.3 Ca 0.2 Cd 0.5 Cu 3 Ti 4 O 12 -0.03SrZrO 3 。
The preparation method is the same as in example 1, except that: according to the general formula Na 0.3 Ca 0.2 Cd 0.5 Cu 3 Ti 4 O 12 Weighing 0.31797g of Na 2 CO 3 、0.40036gCaCO 3 、1.2841gCdO、4.773gCuO、5.1096gTiO 2 The method comprises the steps of carrying out a first treatment on the surface of the According to the general formula SrZrO 3 0.88578gSrCO is weighed 3 、0.73932gZrO 2 。
Polishing the sintered ceramic sample to 200 μm with sand paper, brushing silver paste on the upper and lower surfaces of the ceramic, and testing electrical properties, wherein the dielectric constant of the ceramic material is 7900 at 1kHz, the breakdown field strength is 62kV/cm, and the energy density is 1.34J/cm 3 。
Example 6
A strontium zirconate doped copper sodium calcium cadmium titanate ceramic with high energy storage density comprises Na 0.3 Ca 0.2 Cd 0.5 Cu 3 Ti 4 O 12 -0.07SrZrO 3 。
The preparation method is the same as in example 1, except that: according to the general formula Na 0.3 Ca 0.2 Cd 0.5 Cu 3 Ti 4 O 12 Weighing 0.31797g of Na 2 CO 3 、0.40036gCaCO 3 、1.2841gCdO、4.773gCuO、5.1096gTiO 2 The method comprises the steps of carrying out a first treatment on the surface of the According to the general formula SrZrO 3 2.06682gSrCO is weighed 3 、1.72508gZrO 2 。
Polishing the sintered ceramic sample to 200 μm with sand paper, brushing silver paste on the upper and lower surfaces of the ceramic, and performing electrical property test to obtain ceramic material with dielectric constant of 6800 at 1kHz, breakdown field strength of 78kV/cm, and energy density of 1.83J/cm 3 。
Comparative example 1
Copper sodium calcium cadmium titanate ceramic, composition Na of the ceramic 0.3 Ca 0.2 Cd 0.5 Cu 3 Ti 4 O 12 。
The preparation method of the copper sodium calcium cadmium titanate ceramic comprises the following steps:
s1, according to the general formula Na 0.3 Ca 0.2 Cd 0.5 Cu 3 Ti 4 O 12 Weighing 0.31797g of Na 2 CO 3 、0.40036gCaCO 3 、1.2841gCdO、4.773gCuO、5.1096gTiO 2 Placing the powder into a ball milling tank, and then placing the ball milling tank into a ball mill for fully grinding for 16 hours to obtain powder A;
s2, heating the powder A to 900 ℃ at a speed of 3 ℃/min, and sintering for 7h in an air atmosphere to obtain Na 0.3 Ca 0.2 Cd 0.5 Cu 3 Ti 4 O 12 Powder C; fully grinding for 18 hours, adding a polyvinyl alcohol adhesive with the powder mass of 3wt% for granulating, and pressing into a ceramic blank with the diameter of 1cm and the thickness of 0.8mm under 220 MPa;
s3, heating the ceramic blank to 600 ℃ at a speed of 2 ℃/min, preserving heat for 3 hours, discharging glue, heating to 1150 ℃ at a speed of 5 ℃/min, preserving heat for 8 hours, and cooling along with a furnace to obtain Na 0.3 Ca 0.2 Cd 0.5 Cu 3 Ti 4 O 12 And (3) ceramics.
Polishing the sintered ceramic sample to 200 μm with sand paper, brushing silver paste on the upper and lower surfaces of the ceramic, and testing electrical properties, wherein the dielectric constant of the ceramic material is 13800 at 1kHz, the breakdown field strength is 5.7kV/cm, and the energy density is 0.019J/cm 3 。
Silver electrodes were prepared on the surfaces of the ceramic samples prepared in examples 1 to 5 and comparative example 1 described above for electrical property test. The inventors used SmartLab SE type ray diffractometer (japan), rani shao confocal laser raman spectrometer (uk), 4294A type precision impedance analyzer (united states) manufactured by agilent technologies, inc. In the united states, and the gehley 4200 test system (united states) to characterize the crystal structure, microscopic morphology, and electrical properties of ceramic materials, and calculated the relevant performance parameters using the following formulas.
Dielectric constant: epsilon r ＝Cd/ε 0 A and C are the capacitance, and the capacitance is the capacitance,d is the thickness of the sample, ε 0 Is vacuum dielectric constant (8.85×10) - 12 F/m), A is the area of the electrode.
Nonlinear coefficient:U 1 ，U 2 respectively is I 1 ＝0.1mA，I 2 Corresponding voltage when=1ma.
Energy storage density: the energy storage density of the linear dielectric material is determined by the dielectric constant and the breakdown field strength, and the energy storage densityWherein ε is 0 、ε r Respectively the dielectric constant in vacuum (8.85×10) -12 F/m) and relative dielectric constant; breakdown field strength: />U 2 Taking the voltage when the current is 1mA, and d is the thickness of the ceramic sample.
FIG. 1 is an XRD pattern of strontium zirconate doped copper sodium calcium cadmium titanate ceramics prepared in accordance with the present application and with examples 1-5 and comparative example 1. As can be seen from FIG. 1, the strontium zirconate doped copper sodium calcium cadmium titanate ceramics prepared in comparative example 1 and example 1, example 2 and example 5 are both of a single perovskite structure, and no obvious second phase is generated. While as the doping amount of strontium zirconate increases, peaks of strontium zirconate appear as in examples 3 and 4.
FIG. 2 is a Raman spectrum diagram of strontium zirconate doped copper sodium calcium cadmium titanate ceramics prepared in examples 1-5 and comparative example 1 of the present application. As shown in FIG. 2, 441cm -1 ，507cm -1 ，572cm -1 A corresponding to ACTO ceramics respectively g (1)，A g (2) And F g (3) And (5) molding. General A g (1) And A g (2) The mould corresponds to TiO 6 And F is a rotational movement of g (3) The reverse stretch atomic motion from O-Ti-O, furthermore, the Raman spectrum of example 4 was at 454cm -1 ，607cm -1 The characteristic mode of strontium zirconate occurs and the doping amount corresponding to strontium zirconate is also maximum because of implementationThe strontium zirconate in example 4 has the greatest doping level and thus exhibits distinct characteristic peaks.
FIG. 3 shows the dielectric constants of strontium zirconate doped copper sodium calcium cadmium titanate ceramics prepared in examples 1 to 5 and comparative example 1 according to the present application as a function of frequency. As shown in FIG. 3, the dielectric constant of the strontium zirconate doped copper sodium calcium cadmium titanate is reduced from 13800 to 6100-8300 at 1kHz, but the dielectric constant is 10 2 -10 6 Stability in the Hz range is improved.
FIG. 4 is a graph showing the nonlinear coefficient, breakdown field strength and energy storage density of strontium zirconate doped copper sodium calcium cadmium titanate ceramics prepared in examples 1-5 and comparative example 1 according to the present application. From fig. 4, it can be seen that the strontium zirconate doped material improves the nonlinear properties of the copper sodium calcium cadmium titanate ceramic material such as nonlinear coefficient, breakdown field strength and the like, which is obviously beneficial to the improvement of energy storage density. The undoped copper sodium calcium cadmium titanate of comparative example 1 had an energy storage density of only 0.019J/cm 3 The method comprises the steps of carrying out a first treatment on the surface of the And the energy density of examples 1 to 5 after doping with strontium zirconate is 1.15 to 2.23J/cm 3 In particular example 1, na 0.3 Ca 0.2 Cd 0.5 Cu 3 Ti 4 O 12 -0.05SrZrO 3 The energy density of the ceramic reaches 2.23J/cm 3 Is obviously higher than the energy storage density of the similar ceramic materials. Therefore, the strontium zirconate doped copper sodium calcium cadmium titanate ceramic has the advantages of high energy storage density, simple process, low cost and good repeatability, and has very important application prospects in the fields of high-density energy storage, high-dielectric capacitors and the like.
It should be noted that, when the numerical ranges are referred to in the present application, it should be understood that two endpoints of each numerical range and any numerical value between the two endpoints are optional, and because the adopted step method is the same as the embodiment, in order to prevent redundancy, the present application describes a preferred embodiment. While preferred embodiments of the present application have been described, additional variations and modifications in those embodiments may occur to those skilled in the art once they learn of the basic inventive concepts. It is therefore intended that the following claims be interpreted as including the preferred embodiments and all such alterations and modifications as fall within the scope of the application.
It will be apparent to those skilled in the art that various modifications and variations can be made to the present application without departing from the spirit or scope of the application. Thus, it is intended that the present application also include such modifications and alterations insofar as they come within the scope of the appended claims or the equivalents thereof.
Claims (9)
1. A strontium zirconate doped copper sodium calcium cadmium titanate ceramic with high energy storage density is characterized in that the chemical general formula of the ceramic is Na 0.3 Ca 0.2 Cd 0.5 Cu 3 Ti 4 O 12 -xSrZrO 3 Wherein x is SrZrO 3 Take up Na 0.3 Ca 0.2 Cd 0.5 Cu 3 Ti 4 O 12 0 mass percent of (C)<x≤0.1。
2. The high energy storage density strontium zirconate doped copper sodium calcium cadmium titanate ceramic according to claim 1 wherein x is greater than or equal to 0.02 and less than or equal to 0.08.
3. A method for preparing the high energy storage density strontium zirconate doped copper sodium calcium cadmium titanate ceramic according to claim 1 or 2, comprising the steps of:
s1, selecting Na 2 CO 3 、CaCO 3 、CdO、CuO、TiO 2 、SrCO 3 And ZrO(s) 2 Is raw material powder, according to the composition general formula Na 0.3 Ca 0.2 Cd 0.5 Cu 3 Ti 4 O 12 And SrZrO 3 Batching, grinding to obtain uniformly mixed powder A and powder B respectively;
s2, sintering the powder A to obtain Na 0.3 Ca 0.2 Cd 0.5 Cu 3 Ti 4 O 12 Powder C; sintering the powder B to obtain SrZrO 3 Powder D; powder C and powder D are mixed according to a chemical formula Na 0.3 Ca 0.2 Cd 0.5 Cu 3 Ti 4 O 12 -xSrZrO 3 Proportionally mixing, grinding, and adding adhesiveGranulating and pressing to obtain a ceramic blank;
s3, firstly removing glue from the ceramic blank, and then heating and preserving heat to obtain the strontium zirconate doped copper sodium calcium cadmium titanate ceramic.
4. The method for preparing the strontium zirconate-doped copper sodium calcium cadmium titanate ceramic with high energy storage density according to claim 3, wherein in the step S1, the grinding mode is ball milling, and the time is 12-24 hours.
5. The method for preparing the strontium zirconate doped with copper sodium calcium cadmium titanate ceramic with high energy storage density according to claim 3, wherein in S2, the sintering temperature of the powder A is 850-950 ℃, the heat preservation time is 6-8 h, and the heating rate is 2-3 ℃/min.
6. The method for preparing the strontium zirconate doped with copper sodium calcium cadmium titanate ceramic with high energy storage density according to claim 3, wherein in S2, the sintering temperature of the powder B is 1100-1200 ℃, the heat preservation time is 3-4 h, and the heating rate is 3-4 ℃/min.
7. The method for preparing the strontium zirconate doped with copper sodium calcium cadmium titanate ceramic with high energy storage density according to claim 3, wherein in S2, the binder is polyvinyl alcohol, and the addition amount of the polyvinyl alcohol is 3-4wt% of the mass of the ground powder.
8. The method for preparing the strontium zirconate-doped copper sodium calcium cadmium titanate ceramic with high energy storage density according to claim 3, wherein in S2, the pressure of the compression molding is 200-250 MPa; the size of the ceramic body is 1cm in diameter and 0.7-0.8 mm in thickness.
9. The method for preparing the strontium zirconate doped with copper sodium calcium cadmium titanate ceramic with high energy storage density according to claim 3, wherein in S3, the temperature of the discharged glue is 580-620 ℃, the heat preservation time is 2-3 h, the heating rate is 2-3 ℃/min, the heating temperature is increased to 1150 ℃, the heat preservation time is 6-8 h, and the heating rate is 3-5 ℃/min.
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