CN106565095A - A manganese dioxide-doped barium-strontium niobate based glass ceramic energy-storing material and a preparing method thereof - Google Patents
A manganese dioxide-doped barium-strontium niobate based glass ceramic energy-storing material and a preparing method thereof Download PDFInfo
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- CN106565095A CN106565095A CN201610862196.4A CN201610862196A CN106565095A CN 106565095 A CN106565095 A CN 106565095A CN 201610862196 A CN201610862196 A CN 201610862196A CN 106565095 A CN106565095 A CN 106565095A
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C10/00—Devitrified glass ceramics, i.e. glass ceramics having a crystalline phase dispersed in a glassy phase and constituting at least 50% by weight of the total composition
- C03C10/0036—Devitrified glass ceramics, i.e. glass ceramics having a crystalline phase dispersed in a glassy phase and constituting at least 50% by weight of the total composition containing SiO2, Al2O3 and a divalent metal oxide as main constituents
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C1/00—Ingredients generally applicable to manufacture of glasses, glazes, or vitreous enamels
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C4/00—Compositions for glass with special properties
- C03C4/16—Compositions for glass with special properties for dielectric glass
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Abstract
The invention relates to a manganese dioxide-doped barium-strontium niobate based glass ceramic energy-storing material and a preparing method thereof. BaCO3, SrCO3, Nb<2>O5, SiO2, Al<2>O3, B2O3 and MnO2 in a mole ratio of 20:20:20:30-35:5:1-5:0-0.5 (and 0 not included) are adopted as raw materials to prepare the glass ceramic energy-storing material. The raw materials are ball-milled, mixed, then dried and subjected to high-temperature melting, the high temperature melt is rapidly poured to a copper mold and molded, then stress relieving is performed, and controlled crystallization is performed after a product is cut into glass slices to obtain the glass ceramic energy-storing material. Compared with the prior art, a proper amount of the MnO2 is added, thus effectively reducing dielectric loss (0.004), obviously improving the microscopic structure, inhibiting crystal grain agglomeration, making the microstructure compact and uniform, and ensuring material performance stability. The theoretical energy storage density of the glass ceramic energy-storing material is 9.2 J/cm<3>, and the energy conversion efficiency is as high as 88.9%.
Description
Technical field
The invention belongs to field of dielectric energy storage material, more particularly, to a kind of manganese dioxide doped SrNb2 O6 bario glass
Ceramic energy storage material and preparation method thereof.
Background technology
In recent years, the important ingredient during pulse technique is as various electronic systems, is widely used to electrometer
Calculate it is mechanical, electrical depending on, communicate, radar, remote measuring and controlling, automatically control, the field such as radionavigation and e measurement technology.Pass judgment on a kind of pulse
The superiority of power system, mainly has three parameters, and one is the size of its storage energy；Two is the speed of its electric discharge, and three is which
Energy conversion efficiency.Therefore, the storage energy size of pulse power system, its energy conversion efficiency and efficiency for charge-discharge become and comment
Sentence the major parameter of pulse power system quality, this requires to apply the energy-storage capacitor material in pulse power system same
When possess higher energy storage density and energy conversion efficiency.In addition, for the energy-storage capacitor material in practical application, material
Dielectric loss size is also extremely important, relatively low dielectric loss, it is advantageously ensured that the recycling of energy-storage capacitor, extends device
Service life.
It is well known that the energy storage density of energy storage material is mainly relevant with the disruptive field intensity and dielectric constant of material itself, because
This, the material expected by high energy storage density must be that this material is provided simultaneously with higher disruptive field intensity and dielectric constant, so
And the material of high dielectric constant is usually associated with higher dielectric loss.Therefore various countries material worker just tries to explore research
High-k, low-dielectric loss and high withstand voltage intensity dielectric material.Ferroelectric glass-ceramic energy storage material is by controlling analysis
Brilliant temperature, the crystalline phase of high-k are separated out and are evenly distributed in glass basis in inside glass, compare this material
Ferroelectric ceramics energy storage material and macromolecule composite energy-storage material can have high-k and high breakdown field strength simultaneously.Therefore ferrum
Electric glass ceramics energy storage material is also to meet one of most advantageous material of capacitor material in pulse power system.
At present, SrNb2 O6 bario glass ceramics energy storage material be in terms of the high energy storage of high pressure using be considered as one kind have very much
The novel energy-storing material of future, is to prepare glass basis using high-temperature fusion, method for quick cooling, then through controllable crystallize legal system
It is standby to form.Although comparing with traditional ferroelectric ceramic material with macromolecule composite energy-storage material, the storage of SrNb2 O6 bario glass ceramics
Can material simultaneously there are some apparent advantages such as higher dielectric constant and higher disruptive field intensity, but due to its microcosmic
Crystal grain agglomeration is remained in structure, electric charge is easily collected on glass basis and crystalline phase interface, causes microstructure
It is uneven so that its resistance to disruptive field intensity is far below ideal value, and charge and discharge photoelectric transformation efficiency is low, and dielectric loss is high, and these are deposited
Problem affect application of this material in actual pulse system always.
Such issues that in order to solve, by many scholar's research have studied from material constitute and preparation method etc. in terms of change
Kind glass ceramics energy storage characteristic, such as Zhang.W.Q. et al. have studied the traditional temperature control crystallize of contrast and process and the process of microwave crystallize
Impact of the two methods to ferroelectric glass-ceramic energy storage material performance, it is found that microwave crystallize is processed can significantly improve material
Microstructure, reduces the generation of Dendritic TiC, but as the oneself factor of titanate glass energy storage material is limited, the storage of its material
Can density it is very low, be unfavorable for that (particular content refers to Journal of Alloys of volume 617 in 2014 for the practical application of the material
And Compounds pages 740 to 745).There are many scholars in addition by adding oxide to improve microstructure, improve
Energy storage density, such as Chen.G.H. et al. add a small amount of P in niobates glass ceramics energy storage material2O5, energy storage density reaches
9.1J/cm3But, (particular content refers to the 8th phase Material of volume 176 in 2016 to the dielectric loss up to 0.013 of the material
Letters pages 46 to 48)；Et al. Zheng.J. by adding rare earth oxide La2O3Adjust niobates glass ceramics energy storage material
The problems such as degree of crystallinity of the microscopic appearance and material of material, improve the energy storage density of material, although the dielectric loss of material is
Reduce, but still maintain 0.01 or so, (particular content refers to Ceramics of volume 42 in 2016 for obvious reduction
International pages 1827 to 1832).
The application and Chinese patent CN105399333A disclose SrNb2 O6 bario glass ceramics energy storage material and its preparation
Method is compared, and the application material is adding a certain amount of MnO2Afterwards, disruptive field intensity reaches 1470kV/cm, while energy storage density reaches
9.2J/cm is arrived3, it is most important that the dielectric loss of the application material is reduced to 0.004.
The content of the invention
The purpose of the present invention is exactly to provide a kind of high energy storage density, low to overcome defect that above-mentioned prior art is present
Dielectric loss, manganese dioxide doped SrNb2 O6 bario glass ceramics energy storage material of high-energy conversion efficiency and preparation method thereof.
The purpose of the present invention can be achieved through the following technical solutions：
Manganese dioxide doped SrNb2 O6 bario glass ceramics energy storage material, with BaCO3、SrCO3、Nb2O5、SiO2、Al2O3、
B2O3、MnO2For raw material, prepare for 20: 20: 20: 30-35: 5: 1-5: 0-0.5 (and not being 0) dispensing in molar ratio.
Preferably, the energy storage material is by BaCO3、SrCO3、Nb2O5、SiO2、Al2O3、B2O3、MnO2For raw material, in molar ratio
For 20: 20: 20: 33.5: 5: 1.5: 0.05-0.2 dispensing is prepared.
The preparation method of manganese dioxide doped SrNb2 O6 bario glass ceramics energy storage material, using following steps：
(1) got the raw materials ready by formula；
(2) by the dispensing of step (1) Jing after barreling 22～26h of batch mixing, 120 DEG C of drying, and in 1500～1600 DEG C of high temperature
Fusing, is obtained molten glass liquid；
(3) high-temperature fusant obtained in step (2) is poured in the copper mould of 600～700 DEG C of preheatings, stress relief annealing 7
The clear glass for obtaining is cut into glass flake by～10h；
(4) glass flake for obtaining step (3) is warming up to 1100 DEG C with the programming rate of 2-4 DEG C/min, temperature retention time 2
～3h carries out Controlled Crystallization, then reaches 850 DEG C with the cooling rate of 2-4 DEG C/min, and furnace cooling is obtained two to room temperature afterwards
Oxidation additive Mn strontium barium niobate base glass ceramics energy storage material.
Preferably, the purity of each raw material in step (1) is more than 99.0wt%.
Preferably, the programming rate in step (4) is 3 DEG C/min, and cooling rate is 3 DEG C/min.
Add the SrNb2 O6 bario glass ceramics energy storage material of manganese dioxide, the Controlled Crystallization temperature control in preparation process
At 1100 DEG C, it is ensured that the joint behavior such as dielectric constant and disruptive field intensity of material is optimal, the material is controlled at 1100 DEG C in addition
After warm crystallize, 850 DEG C to be slow cooling to the cooling rate of 3 DEG C/min, it is to avoid material rapid cooling after high temperature crystallize is produced
Raw internal flaw, improves the performance of material
SrNb2 O6 bario glass ceramics energy storage material is prepared, the addition of manganese dioxide can not only be effectively improved the micro- of material
Structure is seen, material microstructure more dense uniform is made, it is ensured that material property is stablized, and can effectively strengthen breakdown potential
Pressure (1470.6kV/cm), improves solid density (9.2J/cm3) more importantly the dielectric loss of this material be reduced to
0.004, and the machining property of this material is excellent, can mechanical grinding be processed into the thin slice of less than 70 μm thickness, be
Follow-up miniaturized device processing provides possible, therefore this material with excellent electric property and machining property can be wide
It is general be applied to electronic computer, TV, communication, radar, remote measuring and controlling, automatically control, the neck such as radionavigation and e measurement technology
In the pulse technique of domain electronic system, and have great application prospect.
It is SrNb2 O6 bario glass ceramics that mol ratio carries out dispensing preparation disclose based on the present invention, by change titanium dioxide
Manganese mol ratio, the glass ceramics energy storage material of the function admirable of preparation, its microstructure are obviously improved, and crystal grain agglomeration is obvious
Reduce, resistance to disruptive field intensity is significantly improved, and dielectric loss is substantially reduced；When the addition of manganese dioxide is 0.05,25 DEG C of 100Hz
Dielectric constant under frequency has reached 95.8, and now resistance to disruptive field intensity reaches 1470.6kV/cm, and theoretical energy storage density reaches
9.2J/cm3, energy conversion efficiency 88.9%.
Compared with prior art, the invention has the characteristics that：
1) the appropriate MnO for adding2, dielectric loss (0.004) can be effectively reduced, it will be apparent that improve microstructure, be pressed down
The generation of combinations grain agglomeration, make dense micro-structure uniform, it is ensured that material property is stablized.Theoretical energy storage density reaches
9.2J/cm3, energy conversion efficiency is up to 88.9%.
2) preparation method is simple, without the need for complicated post-processing step, economical and practical, obtained SrNb2 O6 bario glass ceramics
The stable performance of energy storage material；
3) by the barium boro-alumino-silicate glass system SrNb2 O6 bario glass prepared by the material composition and preparation method of the present invention
Glass ceramic machinery processing characteristics is excellent, can mechanical grinding be processed into the thin slice of less than 70 μm thickness, be follow-up miniaturized device
Processing is provided may.
Description of the drawings
Fig. 1 is the SEM figures of the glass ceramics in embodiment 1～5；
Fig. 2 is the dielectric thermogram of the glass ceramics in embodiment 1～5；
Fig. 3 is the Weibull scattergrams of the resistance to disruptive field intensity of the glass ceramics in embodiment 1～5；
In figure, εrFor dielectric constant, tan δ are dielectric loss, EBDSFor resistance to disruptive field intensity.
Specific embodiment
The present invention is described in detail with specific embodiment below in conjunction with the accompanying drawings.
Those skilled in the art can be by disclosed by this specification content understand easily the present invention other advantages and work(
Effect.The present invention can also be carried out or be applied, the every details in this specification by specific embodiments different in addition
Without departing from the spirit of the present invention various modifications and changes can also be carried out based on different viewpoints and application.
It should be clear that in the following example the not concrete process equipment for indicating or device adopt conventional equipment in the art or
Device.
In addition, it is to be understood that one or more method and steps mentioned in the present invention do not repel before and after the combination step
Can also there is additive method step or additive method step can also be inserted between the step of these specifically mention, unless separately
It is described；And, unless otherwise stated, the numbering of various method steps only differentiates the convenient tool of various method steps, Er Feiwei
Limit the ordering of various method steps or limit enforceable scope of the invention, its relativeness is altered or modified, in nothing
In the case of essence change technology contents, when being also considered as enforceable category of the invention.
As used throughout the specification, following abbreviations have following implications, unless clearly indicated otherwise in text：DEG C=
Degree Celsius；μm=micron；Mm=millimeters；Cm=centimetre；Mol=mole；H=hours；Min=minutes；Wt%=mass percentages
Than；Mol%=molar percentages.Various raw materials and reagent are purchased from commercial supplier, without being further purified, unless otherwise saying
It is bright.The raw material and reagent of moisture-sensitive is deposited in hermetically sealed bottle, and is directly used, without special handling.
Embodiment 1
High energy storage density, high-energy conversion efficiency, the manganese dioxide doped SrNb2 O6 bario glass pottery of low-dielectric loss
Ceramic material：
1) it is more than the BaCO of 99.0wt% with purity3、SrCO3、Nb2O5、SiO2、Al2O3、B2O3、MnO2For feed proportioning,
The molar percentage of above-mentioned each component is 20%, 20%, 20%, 33.5%, 5%, 1.5%, 0%, Jing after ball rolling batch mixing 20h,
Drying, in 1550 DEG C of high temperature meltings 2h；
2) by step 1) high-temperature fusant that obtains is poured in metal die, in 650 DEG C of temperature stress relief annealings 7h, then
It is cleaved to obtain the glass flake that thickness is 1.5mm or so；
3) by step 2) obtained in glass flake with the programming rate of 3 DEG C/min, at 1100 DEG C, temperature retention time 3h is controlled
Crystallize, reaches 850 DEG C with the cooling rate of 3 DEG C/min, and furnace cooling is obtained manganese dioxide doped strontium barium niobate to room temperature afterwards
Base glass ceramics energy storage material.
SEM is as shown in figure 1, can significantly to observe the component crystal grain agglomeration obvious；Dielectric properties such as Fig. 2 institutes
Show；Pressure performance test is as shown in Figure 3；Energy storage density is as shown in table 1.
Embodiment 2
High energy storage density, high-energy conversion efficiency, the manganese dioxide doped SrNb2 O6 bario glass pottery of low-dielectric loss
Ceramic material：
1) it is more than the BaCO of 99.0wt% with purity3、SrCO3、Nb2O5、SiO2、Al2O3、B2O3、MnO2For feed proportioning,
The molar percentage of above-mentioned each component be 20%, 20%, 20%, 33.5%, 5%, 1.5%, 0.05%, Jing balls rolling batch mixing 20h
Afterwards, dry, in 1550 DEG C of high temperature meltings 2h；
2) by step 1) high-temperature fusant that obtains is poured in metal die, in 650 DEG C of temperature stress relief annealings 7h, then
It is cleaved to obtain the glass flake that thickness is 1.5mm or so；
3) by step 2) obtained in glass flake with the programming rate of 3 DEG C/min, at 1100 DEG C, temperature retention time 3h is controlled
Crystallize, reaches 850 DEG C with the cooling rate of 3 DEG C/min, and furnace cooling is obtained manganese dioxide doped strontium barium niobate to room temperature afterwards
Base glass ceramics energy storage material.
SEM is obviously improved as shown in figure 1, the component crystal grain agglomeration significantly can be observed, dense micro-structure
Uniformly；Dielectric properties are as shown in Fig. 2 pressure performance test is as shown in Figure 3；Energy storage density is as shown in table 1.The component is compared with embodiment
1, breakdown voltage improves a lot；
In the present embodiment, add appropriate MnO2Dielectric loss is substantially reduced to 0.007 afterwards, the microscopic appearance of glass ceramics
Have greatly improved, resistance to disruptive field intensity has obvious height, energy storage density reaches 9.2J/cm-3, this example is carried out in voltage
The charge-discharge test of 1000V/mm, energy conversion efficiency reach 88.9%.
Embodiment 3
High energy storage density, high-energy conversion efficiency, the manganese dioxide doped SrNb2 O6 bario glass pottery of low-dielectric loss
Ceramic material：
1) it is more than the BaCO of 99.0wt% with purity3、SrCO3、Nb2O5、SiO2、Al2O3、B2O3、MnO2For feed proportioning,
The molar percentage of above-mentioned each component be 20%, 20%, 20%, 33.5%, 5%, 1.5%, 0.1%, Jing balls rolling batch mixing 20h
Afterwards, dry, in 1550 DEG C of high temperature meltings 2h；
2) by step 1) high-temperature fusant that obtains is poured in metal die, in 650 DEG C of temperature stress relief annealings 7h, then
It is cleaved to obtain the glass flake that thickness is 1.5mm or so；
3) by step 2) obtained in glass flake with the programming rate of 3 DEG C/min, at 1100 DEG C, temperature retention time 3h is controlled
Crystallize, reaches 850 DEG C with the cooling rate of 3 DEG C/min, and furnace cooling is obtained manganese dioxide doped strontium barium niobate to room temperature afterwards
Base glass ceramics energy storage material.
SEM is as shown in figure 1, dielectric properties are as shown in Fig. 2 pressure performance test is as shown in Figure 3；Energy storage density such as 1 institute of table
Show.Compared with embodiment 1, breakdown voltage improves a lot the component；
In the present embodiment, add appropriate MnO2Dielectric loss is substantially reduced to 0.005 afterwards, the microscopic appearance of glass ceramics
Have greatly improved, resistance to disruptive field intensity has obvious height, energy storage density reaches 7.2J/cm-3。
Embodiment 4：
High energy storage density, high-energy conversion efficiency, the manganese dioxide doped SrNb2 O6 bario glass pottery of low-dielectric loss
Ceramic material：
1) it is more than the BaCO of 99.0wt% with purity3、SrCO3、Nb2O5、SiO2、Al2O3、B2O3、MnO2For feed proportioning,
The molar percentage of above-mentioned each component be 20%, 20%, 20%, 33.5%, 5%, 1.5%, 0.2%, Jing balls rolling batch mixing 20h
Afterwards, dry, in 1550 DEG C of high temperature meltings 2h；
2) by step 1) high-temperature fusant that obtains is poured in metal die, in 650 DEG C of temperature stress relief annealings 7h, then
It is cleaved to obtain the glass flake that thickness is 1.5mm or so；
3) by step 2) obtained in glass flake with the programming rate of 3 DEG C/min, at 1100 DEG C, temperature retention time 3h is controlled
Crystallize, reaches 850 DEG C with the cooling rate of 3 DEG C/min, and furnace cooling is obtained manganese dioxide doped strontium barium niobate to room temperature afterwards
Base glass ceramics energy storage material.
SEM is as shown in figure 1, dielectric properties are as shown in Fig. 2 pressure performance test is as shown in Figure 3；Energy storage density such as 1 institute of table
Show.Compared with embodiment 1, breakdown voltage improves a lot the component；
In the present embodiment, add appropriate MnO2Dielectric loss is substantially reduced to 0.004 afterwards, the microscopic appearance of glass ceramics
Have greatly improved, resistance to disruptive field intensity has obvious height, energy storage density reaches 7.1J/cm-3。
Embodiment 5：
High energy storage density, high-energy conversion efficiency, the manganese dioxide doped SrNb2 O6 bario glass pottery of low-dielectric loss
Ceramic material：
1) it is more than the BaCO of 99.0wt% with purity3、SrCO3、Nb2O5、SiO2、Al2O3、B2O3、MnO2For feed proportioning,
The molar percentage of above-mentioned each component be 20%, 20%, 20%, 33.5%, 5%, 1.5%, 0.15%, Jing balls rolling batch mixing 20h
Afterwards, dry, in 1550 DEG C of high temperature meltings 2h；
2) by step 1) high-temperature fusant that obtains is poured in metal die, in 650 DEG C of temperature stress relief annealings 7h, then
It is cleaved to obtain the glass flake that thickness is 1.5mm or so；
3) by step 2) obtained in glass flake with the programming rate of 3 DEG C/min, at 1100 DEG C, temperature retention time 3h is controlled
Crystallize, reaches 850 DEG C with the cooling rate of 3 DEG C/min, and furnace cooling is obtained manganese dioxide doped strontium barium niobate to room temperature afterwards
Base glass ceramics energy storage material.
Table 1
。
Claims (6)
1. manganese dioxide doped SrNb2 O6 bario glass ceramics energy storage material, it is characterised in that the energy storage material is with BaCO3、
SrCO3、Nb2O5、SiO2、Al2O3、B2O3、MnO2For raw material, in molar ratio for 20: 20: 20: 30-35: 5: 1-5: 0-0.5 (and not
Prepare for 0) dispensing.
2. manganese dioxide doped SrNb2 O6 bario glass ceramics energy storage material according to claim 1, it is characterised in that should
Energy storage material is by BaCO3、SrCO3、Nb2O5、SiO2、Al2O3、B2O3、MnO2For raw material, it is 20: 20: 20: 33.5: 5 in molar ratio
: 1.5: 0.05-0.2 dispensing is prepared.
3. the preparation method of manganese dioxide doped SrNb2 O6 bario glass ceramics energy storage material as claimed in claim 1, which is special
Levy and be, the method adopts following steps：
(1) got the raw materials ready by formula；
(2) by the dispensing of step (1) Jing after barreling 22～26h of batch mixing, 120 DEG C of drying, and in 1500～1600 DEG C of high temperature meltings,
Prepared molten glass liquid；
(3) high-temperature fusant obtained in step (2) is poured in the copper moulds of 600～700 DEG C of preheatings, stress relief annealing 7～
The clear glass for obtaining is cut into glass flake by 10h；
(4) glass flake for obtaining step (3) is warming up to 1100 DEG C with the programming rate of 2-4 DEG C/min, 2～3h of temperature retention time
Controlled Crystallization being carried out, then 850 DEG C being reached with the cooling rate of 2-4 DEG C/min, furnace cooling is obtained titanium dioxide to room temperature afterwards
Additive Mn SrNb2 O6 bario glass ceramics energy storage material.
4. manganese dioxide doped SrNb2 O6 bario glass ceramics energy storage material according to claim 3, it is characterised in that step
Suddenly the purity of each raw material in (1) is more than 99.0wt%.
5. manganese dioxide doped SrNb2 O6 bario glass ceramics energy storage material according to claim 3, it is characterised in that step
Suddenly the programming rate in (4) is 3 DEG C/min.
6. manganese dioxide doped SrNb2 O6 bario glass ceramics energy storage material according to claim 3, it is characterised in that step
Suddenly the cooling rate in (4) is 3 DEG C/min.
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| CN107129155A (en) * | 2017-07-04 | 2017-09-05 | 合肥择浚电气设备有限公司 | A kind of preparation technology of dielectric material of glass-ceramics with high energy storage density |
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| CN103342466A (en) * | 2013-06-27 | 2013-10-09 | 桂林电子科技大学 | strontium barium niobate based glass-ceramic dielectric material and preparation method thereof |
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Application publication date: 20170419 |