CN105622092A - Preparation method of high-energy storage density barium strontium titanate-zinc oxide multi-phase ceramic - Google Patents
Preparation method of high-energy storage density barium strontium titanate-zinc oxide multi-phase ceramic Download PDFInfo
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Abstract
The invention discloses a preparation method of high-energy storage density barium strontium titanate-zinc oxide multi-phase ceramic. The preparation method comprises the following steps: firstly, preparing raw materials of BaCO3, SrCO3 and TiO2 according to a chemical formula of Ba0.4Sr0.6TiO3, thus obtaining Ba0.4Sr0.6TiO3 powder; secondly, mixing the Ba0.4Sr0.6TiO3 powder with ZnO powder according to a mass ratio of (100-x):x, thus obtaining ceramic powder; finally, filling a die with the ceramic powder, and sintering at 1000 DEG C in a vacuum environment by utilizing a spark plasma sintering system, thus obtaining a ceramic sintering body; obtaining the high-energy storage density barium strontium titanate-zinc oxide multi-phase ceramic after thermal treatment. The high-energy storage density barium strontium titanate-zinc oxide multi-phase ceramic prepared by the preparation method disclosed by the invention is high in energy storage density, is capable of increasing the dielectric breakdown field strength to a large extent, can be used for components such as a high-density energy storage capacitor and has great application value in the fields of large power and pulse power.
Description
Technical field
The present invention relates to energy storage capacitor dielectric material technical field, particularly relate to the preparation method of a kind of high energy storage density complex phase dielectric ceramics.
Background technology
Dielectric capacitor, with the power density of its superelevation, is extremely applicable to being applied to the field that fluctuation of power is quick and unstable, and its energy storage mode is stored with the form of the enrichment charge voltage field between couple capacitors pole plate by electric energy. Compared with traditional fuel cell, lithium cell, the feature of dielectric medium energy storage capacitor is that fast response time, power density height, long service life, complete solid-state safe structure, use temperature scope are wide etc., has a very wide range of applications in high-power and Pulsed power device. Explore the dielectric materials with high-k, high dielectric breakdown field intensity and low-dielectric loss as energy storage capacitor dielectric material, it is the key improving energy storage density, realizing device miniaturization. In energy storage, lower dielectric loss, higher specific inductivity and breaking down field strength so that barium-strontium titanate ceramic is subject to extensive concern in energy storage field. But lower breaking down field strength constrains its performance, it is possible to realize the modification to barium strontium titanate medium material by compound two-phase.
Application number be 201310681668.2 Chinese patent disclose the preparation method of a kind of high energy storage density barium-strontium titanate ceramic, its step is as follows: (1) is by raw material BaCO3, SrCO3And TiO2By Ba1-xSrxTiO3Chemical formula is prepared burden, and grinding post-drying, sieves; (2), after powder obtained for step (1) being calcined 1��5 hour in 1100��1250 DEG C, sieve; (3) powder obtained for step (2) is loaded mould, utilize discharge plasma sintering system in vacuum environment 900��1050 DEG C sinter, obtained ceramic sintered bodies; (4) under air atmosphere, by described ceramic sintered bodies in 800��1100 DEG C of thermal treatments 1��5 hour, obtained described barium-strontium titanate ceramic. Pure Ba prepared by the method0.4Sr0.6TiO3The most high energy storage density of pottery can reach 1.20J/cm3��
Summary of the invention
It is an object of the invention to for the deficiencies in the prior art, it is provided that a kind of high energy storage density strontium-barium titanate-zinc oxide complex phase ceramic and its preparation method, the complex phase ceramic of preparation at room temperature energy storage density can reach 1.55J/cm3��
It is an object of the invention to be achieved through the following technical solutions: the preparation method of a kind of high energy storage density strontium-barium titanate-zinc oxide complex phase ceramic, comprises the following steps:
(1) by raw material BaCO3, SrCO3And TiO2By Ba0.4Sr0.6TiO3Chemical formula is prepared burden, and being ground to particle diameter is 100nm��500nm post-drying, sieves;
(2) powder 1150 DEG C calcining obtained for step (1), after 3 hours, is sieved, obtained Ba0.4Sr0.6TiO3Powder;
(3) Ba step (2) obtained0.4Sr0.6TiO3Powder and ZnO powder be (100-x) in mass ratio: x prepares burden, and grinding post-drying, sieves, obtained ceramic powder;
(4) ceramic powder obtained for step (3) is loaded mould, utilize discharge plasma sintering system in vacuum environment 1000 DEG C sinter, obtained ceramic sintered bodies;
(5) under air atmosphere, ceramic sintered bodies 1000 DEG C of thermal treatments that step (4) is obtained 3 hours, obtained described high energy storage density strontium-barium titanate-zinc oxide complex phase ceramic.
Further, in step (1), (3), the method for grinding is: raw material is put into ball grinder, adds zirconia ball and deionized water carries out ball milling.
Further, in step (3), Ba0.4Sr0.6TiO3The mass ratio (100-x) of powder and Zinc oxide powder: x, x=0.5��3.0.
Further, in step (3), Ba0.4Sr0.6TiO3The mass ratio (100-x) of powder and Zinc oxide powder: x, x=0.5,1.0 or 3.0.
The present invention is by adopting discharge plasma sintering method, it is to increase the dielectric breakdown strength of complex phase ceramic, improves the specific inductivity of complex phase ceramic by adding zinc oxide, thus improves the energy storage density of complex phase ceramic.
Before preparation, raw material needs to be ground to certain fineness, during grinding, raw material can be put into ball grinder, adds and carries out ball milling in zirconia ball and deionized water.
The useful effect of the present invention is: the preparation method adopting the present invention, by Ba0.4Sr0.6TiO3Powder and Zinc oxide powder in mass ratio 99:1 proportioning time obtained complex phase ceramic at room temperature dielectric breakdown field intensity reach 260kV/cm, and adopt pure Ba prepared by discharge plasma sintering method0.4Sr0.6TiO3The dielectric breakdown field intensity of dielectric ceramics is only 230kV/cm, and dielectric breakdown field intensity improves 13%; Now, discharge plasma sintering temperature is 1000 DEG C, and adopts pure Ba prepared by discharge plasma sintering method0.4Sr0.6TiO3Dielectric ceramics sintering temperature is 1050 DEG C, and sintering temperature reduces more than 4%; Obtained complex phase ceramic at room temperature energy storage density reach 1.55J/cm3, and adopt pure Ba prepared by discharge plasma sintering method0.4Sr0.6TiO3The energy storage density of dielectric ceramics is only 1.28J/cm3Left and right, energy storage density improves more than 21%. High energy storage density strontium-barium titanate-zinc oxide complex phase ceramic prepared by the present invention, can be used for the components and parts such as high-density energy storage capacitor, has great using value in high-power and pulse power field.
Accompanying drawing explanation
Fig. 1 is the XRD diffracting spectrum of strontium-barium titanate-zinc oxide complex phase ceramic sample;
Fig. 2 is the section SEM photograph of strontium-barium titanate-zinc oxide complex phase ceramic sample, and magnification is 10k:(a) Ba0.4Sr0.6TiO3(comparative example 1); (b) 99.5wt.%Ba0.4Sr0.6TiO30.5wt.% zinc oxide (embodiment 1); (c) 99wt.%Ba0.4Sr0.6TiO31wt.% zinc oxide (embodiment 2); (d) 97wt.%Ba0.4Sr0.6TiO33wt.% zinc oxide (embodiment 3);
Fig. 3 is strontium-barium titanate-zinc oxide complex phase ceramic sample specific inductivity at different frequencies and dielectric loss variation with temperature curve: (a), (b) Ba0.4Sr0.6TiO3(comparative example 1); (c), (d) 99.5wt.%Ba0.4Sr0.6TiO30.5wt.% zinc oxide (embodiment 1); (e), (f) 99wt.%Ba0.4Sr0.6TiO31wt.% zinc oxide (embodiment 2); (g) (h) 97wt.%Ba0.4Sr0.6TiO33wt.% zinc oxide (embodiment 3);
Ferroelectric hysteresis loop under maximum electric field intensity during Fig. 4 barium-strontium titanate-based zinc oxide complex phase ceramic sample room temperature 60Hz: (a) Ba0.4Sr0.6TiO3(comparative example 1); (b) 99.5wt.%Ba0.4Sr0.6TiO30.5wt.% zinc oxide (embodiment 1); (c) 99wt.%Ba0.4Sr0.6TiO31wt.% zinc oxide (embodiment 2); (d) 97wt.%Ba0.4Sr0.6TiO33wt.% zinc oxide (embodiment 3).
Embodiment
The present invention is explained further below in conjunction with specific embodiment.
Embodiment 1
(1) by BaCO3, SrCO3And TiO2Raw material powder presses Ba respectively0.4Sr0.6TiO3Chemical formula weigh batching;
(2) chemical feedstocks that step (1) prepares being put into ball grinder, add ball milling 24 hours (particle diameter is 100nm��500nm) in zirconia ball and deionized water, after being dried in loft drier by the powder after ball milling, 120 orders sieve. After being calcined 3 hours by obtained powder 1150 DEG C, cross 120 order sieves, obtained Ba0.4Sr0.6TiO3Powder;
(3) Ba step (2) obtained0.4Sr0.6TiO3Powder and the clearly demarcated 99.5:0.5 in mass ratio of zinc oxide prepare burden, grinding post-drying, and 120 orders sieve, obtained ceramic powder;
(4) powder obtained for step (3) being loaded diameter is the graphite jig of 10mm, puts into discharge plasma sintering system 1000 DEG C, sintering 5 minutes under 30MPa mechanical pressure. Being 100 DEG C/min from room temperature to the temperature rise rate of 900 DEG C, from 900 DEG C to 980 DEG C, temperature rise rate is 40 DEG C/min, and 980 DEG C to 1000 DEG C temperature rise rates are 20 DEG C/min, 1000 DEG C of insulation 5min, after having sintered, sheds pressure and cold with stove.
SPS sintering theory: SPS utilizes DC pulse current directly to carry out energising pressure sintering, by regulating the power size of DC pulse current to control temperature rise rate. Whole sintering process both can carry out under vacuum conditions, also to carry out in protective atmosphere. Pulsed current directly acts on sample and mould, fast heating, and flash heat transfer, is rapidly heated, and significantly shortens sample sintering time
(5) thermal treatment 3 hours at 1000 DEG C in atmosphere after the graphite paper going ceramics sample obtained for step (4) at mill to adhere to. From room temperature to the temperature rise rate of 1000 DEG C be 5 DEG C/min, 1000 DEG C insulation 3h, cold with stove after having processed. And in air atmosphere, its thermal treatment at 1000 DEG C is obtained having the 99.5wt.%Ba of high energy storage density for 3 hours0.4Sr0.6TiO31.0wt.% zinc oxide complex phase ceramic.
Embodiment 2
(1) by BaCO3, SrCO3And TiO2Raw material powder presses Ba respectively0.4Sr0.6TiO3Chemical formula weigh batching;
(2) chemical feedstocks that step (1) prepares being put into ball grinder, add ball milling 24 hours (particle diameter is 100nm��500nm) in zirconia ball and deionized water, after being dried in loft drier by the powder after ball milling, 120 orders sieve. After being calcined 3 hours by obtained powder 1150 DEG C, cross 120 order sieves, obtained Ba0.4Sr0.6TiO3Powder;
(3) Ba step (2) obtained0.4Sr0.6TiO3Powder and the clearly demarcated 99:1 in mass ratio of zinc oxide prepare burden, grinding post-drying, and 120 orders sieve, obtained ceramic powder;
(4) powder obtained for step (3) being loaded diameter is the graphite jig of 10mm, puts into discharge plasma sintering system 1000 DEG C, sintering 5 minutes under 30MPa mechanical pressure. Being 100 DEG C/min from room temperature to the temperature rise rate of 900 DEG C, from 900 DEG C to 980 DEG C, temperature rise rate is 40 DEG C/min, and 980 DEG C to 1000 DEG C temperature rise rates are 20 DEG C/min, 1000 DEG C of insulation 5min, after having sintered, sheds pressure and cold with stove.
(5) thermal treatment 3 hours at 1000 DEG C in atmosphere after the graphite paper going ceramics sample obtained for step (4) at mill to adhere to. From room temperature to the temperature rise rate of 1000 DEG C be 5 DEG C/min, 1000 DEG C insulation 3h, cold with stove after having processed. And in air atmosphere, its thermal treatment at 1000 DEG C is obtained having the 99wt.%Ba of high energy storage density for 3 hours0.4Sr0.6TiO31wt.% zinc oxide complex phase ceramic.
Embodiment 3
(1) by BaCO3, SrCO3And TiO2Raw material powder presses Ba respectively0.4Sr0.6TiO3Chemical formula weigh batching;
(2) chemical feedstocks that step (1) prepares being put into ball grinder, add ball milling 24 hours (particle diameter is 100nm��500nm) in zirconia ball and deionized water, after being dried in loft drier by the powder after ball milling, 120 orders sieve. After being calcined 3 hours by obtained powder 1150 DEG C, cross 120 order sieves, obtained Ba0.4Sr0.6TiO3Powder;
(3) Ba step (2) obtained0.4Sr0.6TiO3Powder and the clearly demarcated 97:3 in mass ratio of zinc oxide prepare burden, grinding post-drying, and 120 orders sieve, obtained ceramic powder;
(4) powder obtained for step (3) being loaded diameter is the graphite jig of 10mm, puts into discharge plasma sintering system 1000 DEG C, sintering 5 minutes under 30MPa mechanical pressure. Being 100 DEG C/min from room temperature to the temperature rise rate of 900 DEG C, from 900 DEG C to 980 DEG C, temperature rise rate is 40 DEG C/min, and 980 DEG C to 1000 DEG C temperature rise rates are 20 DEG C/min, 1000 DEG C of insulation 5min, after having sintered, sheds pressure and cold with stove.
(5) thermal treatment 3 hours at 1000 DEG C in atmosphere after the graphite paper going ceramics sample obtained for step (4) at mill to adhere to. From room temperature to the temperature rise rate of 1000 DEG C be 5 DEG C/min, 1000 DEG C insulation 3h, cold with stove after having processed. And in air atmosphere, its thermal treatment at 1000 DEG C is obtained having the 97wt.%Ba of high energy storage density for 3 hours0.4Sr0.6TiO33wt.% zinc oxide complex phase ceramic.
Comparative example 1
Pure Ba is provided0.4Sr0.6TiO3The discharge plasma sintering preparation process of pottery:
(1) by BaCO3, SrCO3And TiO2Raw material powder presses Ba respectively0.4Sr0.6TiO3Chemical formula weigh batching;
(2) chemical feedstocks that step (1) prepares being put into ball grinder, add zirconia ball and deionized water ball milling 24 hours (particle diameter is 100nm��500nm), after being dried in loft drier by the powder after ball milling, 120 orders sieve. After calcining 3 hours at 1150 DEG C subsequently, 120 orders sieve again;
(3) powder obtained for step (2) being loaded diameter is the graphite jig of 10mm, puts into discharge plasma sintering system 1050 DEG C, sintering 5 minutes under 30MPa mechanical pressure. Being 100 DEG C/min from room temperature to the temperature rise rate of 950 DEG C, from 950 DEG C to 1030 DEG C, temperature rise rate is 40 DEG C/min, and 1030 DEG C to 1050 DEG C temperature rise rates are 20 DEG C/min, 1050 DEG C of insulation 5min, after having sintered, sheds pressure and cold with stove.
(4) thermal treatment 3 hours at 1000 DEG C in atmosphere after the graphite paper going ceramics sample obtained for step (3) at mill to adhere to. From room temperature to the temperature rise rate of 1000 DEG C be 5 DEG C/min, 1000 DEG C insulation 2h, cold with stove after having processed, obtain Ba0.4Sr0.6TiO3Pottery.
Cylindrical dielectric ceramics sample sand paper embodiment 1��3 and comparative example 1 prepared is milled to 0.20mm thickness, and after gold electrode is sprayed on surface, the ferroelectric hysteresis loop under utilizing ferroelectric analyser to measure its 60Hz frequency, utilizes integration to calculate its energy storage density.
Table 1
Table 1 shows (100-x) wt.%Ba utilizing the preparation method of the present invention to obtain0.4Sr0.6TiO3Xwt.% zinc oxide (x=0.5,1,3) complex phase ceramic and the Ba utilizing discharge plasma sintering method to prepare0.4Sr0.6TiO3The dielectric breakdown strength of pottery under room temperature, 60Hz frequency and energy storage density, as shown in Table 1, high energy storage density strontium-barium titanate-zinc oxide complex phase ceramic that the present invention obtains at room temperature most high energy storage density be 1.55J/cm3, and utilize pure Ba prepared by discharge plasma sintering method0.4Sr0.6TiO3Under the room temperature of pottery, energy storage density is only 1.28J/cm3��
By Fig. 2,3,4 is provable, add zinc oxide mutually after, breaking down field strength, the energy storage density of composite ceramics significantly improve. Compared to pure barium-strontium titanate ceramic, with the addition of massfraction be 0.5%, 1.0%, 3% zinc oxide mutually after, breaking down field strength increases to 240kV/cm, 260kV/cm, 260kV/cm from 230kV/cm. Therefore its energy storage density also corresponding raising, reaches when addition is 1.0% and is up to 1.55J/cm3, purer barium-strontium titanate ceramic improves 21%.
Claims (4)
1. the preparation method of high energy storage density strontium-barium titanate-zinc oxide complex phase ceramic, it is characterised in that, comprise the following steps:
(1) by raw material BaCO3, SrCO3And TiO2By Ba0.4Sr0.6TiO3Chemical formula is prepared burden, and being ground to particle diameter is 100nm��500nm post-drying, sieves;
(2) powder 1150 DEG C calcining obtained for step (1), after 3 hours, is sieved, obtained Ba0.4Sr0.6TiO3Powder;
(3) Ba step (2) obtained0.4Sr0.6TiO3Powder and ZnO powder be (100-x) in mass ratio: x prepares burden, and grinding post-drying, sieves, obtained ceramic powder;
(4) ceramic powder obtained for step (3) is loaded mould, utilize discharge plasma sintering system in vacuum environment 1000 DEG C sinter, obtained ceramic sintered bodies;
(5) under air atmosphere, ceramic sintered bodies 1000 DEG C of thermal treatments that step (4) is obtained 3 hours, obtained described high energy storage density strontium-barium titanate-zinc oxide complex phase ceramic.
2. preparation method as claimed in claim 1, it is characterised in that, in step (1), (3), the method for grinding is: raw material is put into ball grinder, adds zirconia ball and deionized water carries out ball milling.
3. preparation method as claimed in claim 1, it is characterised in that, in step (3), Ba0.4Sr0.6TiO3The mass ratio (100-x) of powder and ZnO powder: x, x=0.5��3.0.
4. preparation method as claimed in claim 3, it is characterised in that, in step (3), Ba0.4Sr0.6TiO3The mass ratio (100-x) of powder and ZnO powder: x, x=0.5,1.0 or 3.0.
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| CN106542821A (en) * | 2016-10-18 | 2017-03-29 | 陕西科技大学 | A kind of Bi2O3‑B2O3ZnO glass adds Ba0.4Sr0.6TiO3Base energy storage ceramic and preparation method thereof |
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