CN103848573B - A kind of high energy storage density high-temperature stability dielectric glass ceramic composite and preparation method thereof - Google Patents
A kind of high energy storage density high-temperature stability dielectric glass ceramic composite and preparation method thereof Download PDFInfo
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- CN103848573B CN103848573B CN201210519413.1A CN201210519413A CN103848573B CN 103848573 B CN103848573 B CN 103848573B CN 201210519413 A CN201210519413 A CN 201210519413A CN 103848573 B CN103848573 B CN 103848573B
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Abstract
A kind of high energy storage density high-temperature stability dielectric glass ceramic composite and preparation method thereof, this chemical constituent contained by dielectric glass ceramic composite is a PbO b BaO c Na2O‑d Nb2O5‑e SiO2‑fR2O3, wherein a, b, c, d, e, f represent the molar ratio between each component, respectively 0≤a≤7.1,6.2≤b≤17.1,15.5≤c≤17.1,29.7≤d≤34.3,31≤e≤38.5,0≤f≤3, and R is the one in La, Ce, Pr, Sm and Lu.This dielectric glass ceramic composite is prepared with the method for controlled crystallization by high-temperature fusion: first the fine powder after ball milling uses melted quickly cooling method but of accelerating prepare clear glass thin slice, it is then passed through controlled crystallization technique and prepares glass ceramics sheet, finally form and prepare metal electrode and obtain dielectric glass ceramic plate condenser.Dielectric glass ceramic prepared by the present invention is made up of mutually the amorphous glass of the fine and close high breakdown strength of nanoscale high-k ferroelectricity niobates phase and atresia, and the advantage having high energy storage density and high-temperature stability concurrently is used for manufacturing high pressure height energy-storage capacitor.
Description
Technical field
The present invention relates to a kind of high energy storage density high-temperature stability dielectric glass ceramic composite and preparation side thereof
Method.
Background technology
In modern society, along with acceleration and the increase of human's demand, the high pressure equipment such as pulse power of scientific and technological progress
System, cardiac pacemaker, hybrid-electric car, synchrotron radiation source etc. proposes new requirement to its energy-storage units:
The i.e. direction towards miniaturization with lightness is developed.In order to realize this urgent needs, there is high energy storage pressure, high
The capacitor of density plays important role, and determine the core of capacitor performance be develop possess high pressure,
The dielectric material of high energy storage density.
Due to dielectric energy storage density and its dielectric constant and square direct proportionality of electric field intensity, therefrom
Know that having the dielectric substance of high-k and high breakdown field strength characteristic concurrently will be provided with the speciality of high energy storage density.
For sintering pottery, it has high temperature resistant, wear-resistant, to be difficult to an aged deterioration feature, and its internal ferroelectricity
Crystal has the characteristic of high-k, is therefore widely used in manufacturing the electrolyte of high energy-storage capacitor.But by
In sintering ceramic dielectric internal itself exist hole, the microscopic appearance such as grain boundary defects so that ceramic condenser resistance to
Voltage capability is restricted.Compared with the former, glass ceramics dielectric material is a kind of well for producing high energy storage
The dielectric substance of capacitor.Glass ceramics dielectric material is to first pass through high-temperature fusion to prepare with the method quickly cooled down
Clear glass, then makes ferroelectric crystal granule forming core and crystallization by controlled crystallization technique, forms ferroelectric crystal
Grain is uniformly distributed in the novel dielectric composite material of one of glass basis.Due in this composite of glass ceramics
Ferroelectric crystal granule provides high-k, and atresia dense glass matrix has high voltage withstanding feature, makes
Obtain this dielectric glass ceramic and have the advantage of high-k and high breakdown field strength concurrently, and then make this composite dielectric material
Material possesses at a relatively high energy storage density.
For the capacitor used in the environment of high pressure, internal electrolyte can produce heat drastically under high voltages
Effect, although people take various measure and derive the heat that energy-storage capacitor distributes, but its internal temperature is still
Room temperature can be higher than.According to high-voltage capacitor industry standard, the capacitance of dielectric material needs-30 DEG C～80 DEG C of temperature
In the range of examine.Conventional sintering ceramic dielectric material, the pottery as given by patent documentation (CN 102101775A)
Medium, its electric capacity in-30 DEG C～80 DEG C of temperature ranges change between 9.3～-8.0 scope, its resistance to DC fields
It is confined to by force near 12kV/mm.It will be seen that its electric capacity of the ceramic medium material gone out given in this patent documentation
Value change in-30 DEG C～80 DEG C of temperature ranges is the biggest, and it pressure is still within relatively low level, no
It is well positioned to meet the demand of high-voltage capacitor.
Summary of the invention
It is an object of the invention to provide a kind of high energy storage density high-temperature stability dielectric glass ceramic composite wood
Material, this dielectric glass ceramic composite is suitable for high-voltage capacitor medium.
Another object of the present invention is to provide the preparation method of a kind of described dielectric glass ceramic composite.
For achieving the above object, the present invention is by the following technical solutions:
A kind of high energy storage density high-temperature stability dielectric glass ceramic composite, this dielectric glass ceramic is combined
Chemical constituent contained by material is a PbO-b BaO-c Na2O-d Nb2O5-e SiO2-fR2O3, wherein a, b, c,
D, e, f represent the molar ratio between each component, respectively 0≤a≤7.1,6.2≤b≤17.1,15.5≤c≤17.1,
29.7≤d≤34.3,31≤e≤38.5,0≤f≤3, R is the one in La, Ce, Pr, Sm and Lu.
The preparation method of a kind of described dielectric glass ceramic composite, comprises the following steps:
(1) with PbO, BaCO of analytical pure level3、Na2CO3、Nb2O5、SiO2And R2O3Powder be former
Material, in strict accordance with a PbO-b BaO-c Na2O-d Nb2O5-e SiO2-f R2O3Ratio dispensing mixing, will mixing
Powder adds ball-milling medium in planetary ball mill and grinds 12h, is then placed in platinum crucible by the raw material that ball milling is good
It is incubated 3h at 1500 DEG C；
(2) thickness will be prepared by the high-temperature fusant obtained by step (1) quickly through metallic roll calender
Be 0.3～1mm, the continuously adjustable transparent glass sheet of thickness；
Or, will by the high-temperature fusant Quick pouring obtained by step (1) to preheating metal die in, so
The thin glass sheet that thickness is 1～2mm is become by following process；
(3) controlled crystallization will be carried out by the sheet glass obtained by step (2), controlled crystallization employing two-step method:
First the powder stock mixed is slowly heated to 630 DEG C of insulation 3h, makes niobate crystal granule forming core, so
After continue to be heated to 900 DEG C of insulation 3h and make nuclei growth, separate out the ferroelectricity niobates phase of nano-scale, and uniformly
The glass ceramic composite material being distributed in glass basis.
Wherein, described ball-milling medium is deionized water or dehydrated alcohol.
The roller diameter of described metallic roll calender is 10～20cm, and rotating speed is 30～70r/min, roll material
For rustless steel.Described metal die is circular or rectangle, and material is steel or copper.
The dielectric glass ceramic composite of the present invention use silk-screen printing technique coating bonding good with electric conductivity
Good middle temperature silver paste, at a temperature of 550 DEG C, sintering curing obtains argent electrode, prepares dielectric glass ceramic and puts down
Parallel plate capacitor；Or by dielectric glass ceramic composite, through grinding and after surface finish, use magnetic control to spatter
The method penetrated, at plating metal on surface electrode, prepares dielectric glass ceramic plane-parallel capacitor.The target of magnetron sputtering
For metallic nickel.
It is an advantage of the current invention that:
The present invention, by first preparing glass, then prepares niobates nanometer ferroelectric particle by controlled crystallization and uniformly divides
The dielectric glass ceramic composite being distributed in nonporous glass matrix so that this dielectric glass ceramic composite is held concurrently
Tool high-k (＞ 301) and high breakdown strength (＞ 35kV/mm).
The dielectric glass ceramic composite of the present invention, comprises rare earth element in its component so that at-30 DEG C～85
Within the temperature range of DEG C, medium is that the electric capacity of glass ceramic composite material maintains the highest temperature stability
(＜ 4%).
The present invention is by converting kind and the content of glass ceramics composition middle rare earth, and the dielectric glass made is made pottery
Porcelain is while keeping high-k and high breakdown strength, and dielectric constant is in comparatively wide scope (301～504)
Adjustable.
Detailed description of the invention
Below by specific embodiment, the present invention will be further described.
Embodiment 1～4
The BaCO of the pure level of selection analysis3、Na2CO3、Nb2O5、SiO2、La2O3Powder be raw material, according to table
The molar ratio of 1 dispensing respectively, then well-mixed powder is added in planetary ball mill deionized water as
Ball-milling medium, grinds 12h.
Then the raw material stoving that ball milling is good is placed in Pt crucible and is incubated 3h at 1500 DEG C.Subsequently by obtained
It is the clear glass in the range of 0.3mm～1mm that high-temperature fusant suppresses thickness quickly through metallic roll calender
Sheet.Then sheet glass is moved rapidly in annealing furnace insulation 6h, carries out stress relief annealing, be then turned off annealing furnace,
Make sheet glass furnace cooling.
The sheet glass of preparation carries out controlled crystallization, and controlled crystallization uses two-step method: first by former for the powder that mixes
Material is slowly heated to 630 DEG C of insulation 3h, makes niobate crystal granule forming core, then proceedes to be heated to 900 DEG C of insulations
3h makes nuclei growth, separates out the ferroelectricity niobates phase of nano-scale, and the nanometer being uniformly distributed in glass basis
Dielectric glass ceramic composite.
By the dielectric glass ceramic idiosome of preparation, through grinding and after surface finish, the method for magnetron sputtering is used to exist
Plating metal on surface electrode, prepares easy glass ceramics plane-parallel capacitor and carries out performance test, test result such as table
Shown in 2.
By being analyzed comparing to result, it can be seen that along with La2O3The increase of addition, dielectric constant is notable
Improving, disruptive field intensity is the most more than 44.7kV/mm, especially at La2O3When content is 1mol%, disruptive field intensity
Reach peak 55.6/kV/mm.Capacitance shows extraordinary temperature stability.
Embodiment 5～8
The BaCO of the pure level of selection analysis3、Na2CO3、Nb2O5、SiO2、Sm2O3Powder be raw material, according to
The molar ratio of table 1 dispensing respectively, then adds well-mixed powder deionized water in planetary ball mill and makees
For ball-milling medium, grind 12h.
Then the raw material stoving that ball milling is good is placed in Pt crucible and is incubated 3h at 1500 DEG C.Subsequently by obtained
It is the clear glass in the range of 0.3mm～1mm that high-temperature fusant suppresses thickness quickly through metallic roll calender
Sheet.Then sheet glass is moved rapidly in annealing furnace insulation 6h, carries out stress relief annealing, be then turned off annealing furnace,
Make sheet glass furnace cooling.
The sheet glass of preparation carries out controlled crystallization, and controlled crystallization uses two-step method: first by former for the powder that mixes
Material is slowly heated to 630 DEG C of insulation 3h, makes niobate crystal granule forming core, then proceedes to be heated to 900 DEG C of insulations
3h makes nuclei growth, separates out the ferroelectricity niobates phase of nano-scale, and the nanometer being uniformly distributed in glass basis
Dielectric glass ceramic composite.
By the dielectric glass ceramic idiosome of preparation, through grinding and after surface finish, the method for magnetron sputtering is used to exist
Plating metal on surface electrode, prepares easy glass ceramics plane-parallel capacitor and does dielectric properties test, test result
As shown in table 2.
By being analyzed comparing to result, it can be seen that along with Sm2O3The increase of addition, dielectric constant is notable
Improving, disruptive field intensity shows downward trend after first rising, at Sm2O3When content is 1mol%, breakdown field
Reach by force peak 45.8/kV/mm.At examination temperature range (-30 DEG C～80 DEG C) capacitance along with the change of temperature
Change and control within 4%.
Embodiment 9～12
The BaCO of the pure level of selection analysis3、Na2CO3、Nb2O5、SiO2、Lu2O3Powder be raw material, according to table
The molar ratio of 1 dispensing respectively, then well-mixed powder is added in planetary ball mill deionized water as
Ball-milling medium, grinds 12h.
Then the raw material stoving that ball milling is good is placed in Pt crucible and is incubated 3h at 1500 DEG C.Subsequently by obtained
It is the clear glass in the range of 0.3mm～1mm that high-temperature fusant suppresses thickness quickly through metallic roll calender
Sheet.Then sheet glass is moved rapidly in annealing furnace insulation 6h, carries out stress relief annealing, be then turned off annealing furnace,
Make sheet glass furnace cooling.
The sheet glass of preparation carries out controlled crystallization, and controlled crystallization uses two-step method: first by former for the powder that mixes
Material is slowly heated to 630 DEG C of insulation 3h, makes niobate crystal granule forming core, then proceedes to be heated to 900 DEG C of insulations
3h makes nuclei growth, separates out the ferroelectricity niobates phase of nano-scale, and the nanometer being uniformly distributed in glass basis
Dielectric glass ceramic composite.
By the dielectric glass ceramic idiosome of preparation, through grinding and after surface finish, the method for magnetron sputtering is used to exist
Plating metal on surface electrode, prepares easy glass ceramics plane-parallel capacitor and carries out dielectric properties test, test knot
Fruit is as shown in table 2.
It is analyzed comparing to result, it can be seen that along with Lu2O3The increase of addition, dielectric constant shows elder generation
The trend reduced after increase, disruptive field intensity is maintained at the level of ＞ 35.2kV/mm, at Lu2O3Content is 3mol%
Time reach peak 43.4kV/mm.At examination temperature range (-30 DEG C～80 DEG C) capacitance along with the change of temperature
Change can control within 4%.
Embodiment 13～17
PbO, BaCO of the pure level of selection analysis3、Na2CO3、Nb2O5、SiO2、La2O3、CeO2、Pr6O11、
Sm2O3、Lu2O3Powder be raw material, according to the molar ratio respectively dispensing of table 1, then by well-mixed powder
End adds dehydrated alcohol as ball-milling medium, grinding 12h in planetary ball mill.
Then the raw material stoving that ball milling is good is placed in Pt crucible and is incubated 3h at 1500 DEG C.Then by obtained
High-temperature fusant Quick pouring is in the metal die being preheated to 500 DEG C in advance, by sheet glass after melt tentatively solidifies
It is moved rapidly in annealing furnace insulation 6h, carries out stress relief annealing, be then turned off annealing furnace, make sheet glass cold with stove
But.
The sheet glass of preparation carries out controlled crystallization, and controlled crystallization uses two-step method: first will remove the glass of internal stress
Glass sheet is slowly heated to 630 DEG C of insulation 3h, makes niobate crystal granule forming core, then proceedes to be heated to 900 DEG C of guarantors
Temperature 3h makes nuclei growth, separates out the ferroelectricity niobates phase of nano-scale, and receiving of being uniformly distributed in glass basis
Rice dielectric glass ceramic composite.
Afterwards by the dielectric glass ceramic idiosome square-cut thin slice of preparation, after surface grinding and polishing, use silk screen
The middle temperature silver paste that typography coating bonding is good with electric conductivity, at a temperature of 550 DEG C, sintering curing obtains gold
Belong to silver electrode, prepare easy glass ceramics plane-parallel capacitor and carry out dielectric properties test, test result such as table
Shown in 2.
It will be seen that at 7.1PbO-6.2BaO-15.5Na2O-29.7Nb2O5-38.5SiO2In glass ceramics component
Add the La of 3mol%2O3、CeO2、Pr6O11、Sm2O3、Lu2O3, material all obtains dielectric constant ＞ 478,
Disruptive field intensity ＞ 41.7kV/mm, at examination temperature range (-30 DEG C～80 DEG C) capacitance along with the change ＜ 3.2 of temperature
The characteristic of %.
Table 1
Table 2
| Embodiment | Dielectric constant | Disruptive field intensity | Temperature characterisitic (-30 DEG C～85 DEG C) |
| 1 | 335 | 52.4 | -1.135～1.988 |
| 2 | 405 | 55.6 | -1.621～2.809 |
| 3 | 437 | 47.4 | -1.357～1.235 |
| 4 | 478 | 44.7 | -2.117～1.854 |
| 5 | 346 | 40.6 | -2.307～2.638 |
| 6 | 391 | 43.5 | -2.805～2.511 |
| 7 | 462 | 45.8 | -3.197～2.541 |
| 8 | 497 | 41.3 | -2.822～2.673 |
| 9 | 327 | 35.2 | -3.484～2.896 |
| 10 | 338 | 42.5 | -3.443～2.883 |
| 11 | 309 | 38.5 | -2.652～3.435 |
| 12 | 301 | 43.4 | -3.336～3.319 |
| 13 | 504 | 49.3 | -2.174～1.976 |
| 14 | 497 | 47.8 | -2.436～2.181 |
| 15 | 482 | 43.4 | -2.935～2.631 |
| 16 | 501 | 42.3 | -3.176～2.797 |
| 17 | 478 | 41.7 | -3.011～2.563 |
Claims (5)
1. a high energy storage density high-temperature stability dielectric glass ceramic composite, it is characterised in that contained
Chemical constituent be a PbO-b BaO-c Na2O-d Nb2O5-e SiO2-f R2O3, wherein a, b, c, d, e, f
Represent the molar ratio between each component, respectively 0≤a≤7.1,6.2≤b≤17.1,15.5≤c≤17.1,
29.7≤d≤34.3,31≤e≤38.5,0≤f≤3, R is the one in La, Ce, Pr, Sm and Lu.
2. the preparation method of the dielectric glass ceramic composite described in a claim 1, it is characterised in that
Comprise the following steps:
(1) with PbO, BaCO of analytical pure level3、Na2CO3、Nb2O5、SiO2And R2O3Powder be former
Material, in strict accordance with a PbO-b BaO-c Na2O-d Nb2O5-e SiO2-f R2O3Ratio dispensing mixing, will mixing
Powder adds ball-milling medium in planetary ball mill and grinds 12h, is then placed in platinum crucible by the raw material that ball milling is good
It is incubated 3h at 1500 DEG C；
(2) thickness will be prepared by the high-temperature fusant obtained by step (1) quickly through metallic roll calender
Be 0.3～1mm, the continuously adjustable transparent glass sheet of thickness；
Or, will by the high-temperature fusant Quick pouring obtained by step (1) to preheating metal die in, so
The thin glass sheet that thickness is 1～2mm is become by following process；
(3) controlled crystallization will be carried out by the sheet glass obtained by step (2), controlled crystallization employing two-step method:
First the powder stock mixed is slowly heated to 630 DEG C of insulation 3h, makes niobate crystal granule forming core, so
After continue to be heated to 900 DEG C of insulation 3h and make nuclei growth, separate out the ferroelectricity niobates phase of nano-scale, and uniformly
The nanometer dielectric glass ceramic composite being distributed in glass basis.
The preparation method of dielectric glass ceramic composite the most according to claim 2, it is characterised in that
Described ball-milling medium is deionized water or dehydrated alcohol.
The preparation method of dielectric glass ceramic composite the most according to claim 2, it is characterised in that
The roller diameter of described metallic roll calender is 10～20cm, and rotating speed is 30～70r/min, and roll material is not
Rust steel.
The preparation method of dielectric glass ceramic composite the most according to claim 2, it is characterised in that
Described metal die is circular or rectangle, and material is steel or copper.
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| RU2616648C1 (en) * | 2015-12-29 | 2017-04-18 | Акционерное общество "Научно-исследовательский и технологический институт оптического материаловедения Всероссийского научного центра "Государственный оптический институт им. С.И. Вавилова" (АО "НИТИОМ ВНЦ "ГОИ им. С.И. Вавилова") | Method for production of glass-ceramic material with rare earth elements niobates nanoscale crystals |
| CN105753472B (en) * | 2016-01-26 | 2018-06-26 | 同济大学 | The niobic acid barium potassium base glass ceramics energy storage material of high energy storage density and preparation and application |
| CN108395106B (en) * | 2018-04-23 | 2021-03-26 | 同济大学 | Barium niobate lead sodium based glass ceramic material with high energy storage density and preparation method thereof |
| CN110240409B (en) * | 2019-05-30 | 2021-10-08 | 同济大学 | Barium niobate lead sodium based glass ceramic material with high energy storage density and preparation method thereof |
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| CN1249286A (en) * | 1998-09-28 | 2000-04-05 | 株式会社村田制作所 | Dielectric ceramic composition and stacked ceramic capacitor |
| CN101226827A (en) * | 2007-12-28 | 2008-07-23 | 天津大学 | Ultra-high dielectric constant multilayer ceramic capacitor medium and preparation method thereof |
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| CN1249286A (en) * | 1998-09-28 | 2000-04-05 | 株式会社村田制作所 | Dielectric ceramic composition and stacked ceramic capacitor |
| CN101226827A (en) * | 2007-12-28 | 2008-07-23 | 天津大学 | Ultra-high dielectric constant multilayer ceramic capacitor medium and preparation method thereof |
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