CN103880288B - A kind of strontium barium niobate glass ceramic material of high-k high breakdown field strength and preparation method thereof - Google Patents
A kind of strontium barium niobate glass ceramic material of high-k high breakdown field strength and preparation method thereof Download PDFInfo
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- CN103880288B CN103880288B CN201410040185.9A CN201410040185A CN103880288B CN 103880288 B CN103880288 B CN 103880288B CN 201410040185 A CN201410040185 A CN 201410040185A CN 103880288 B CN103880288 B CN 103880288B
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- strontium barium
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- WOIHABYNKOEWFG-UHFFFAOYSA-N [Sr].[Ba] Chemical compound [Sr].[Ba] WOIHABYNKOEWFG-UHFFFAOYSA-N 0.000 title claims abstract description 61
- 239000006112 glass ceramic composition Substances 0.000 title claims abstract description 56
- 238000002360 preparation method Methods 0.000 title claims abstract description 25
- 230000015556 catabolic process Effects 0.000 title claims abstract description 21
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 69
- 239000011521 glass Substances 0.000 claims abstract description 64
- ZKATWMILCYLAPD-UHFFFAOYSA-N niobium pentoxide Chemical compound O=[Nb](=O)O[Nb](=O)=O ZKATWMILCYLAPD-UHFFFAOYSA-N 0.000 claims abstract description 46
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 35
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims abstract description 34
- AYJRCSIUFZENHW-UHFFFAOYSA-L barium carbonate Chemical compound [Ba+2].[O-]C([O-])=O AYJRCSIUFZENHW-UHFFFAOYSA-L 0.000 claims abstract description 34
- 239000000203 mixture Substances 0.000 claims abstract description 32
- 229910052905 tridymite Inorganic materials 0.000 claims abstract description 30
- 238000000137 annealing Methods 0.000 claims abstract description 29
- 229910052681 coesite Inorganic materials 0.000 claims abstract description 29
- 229910052906 cristobalite Inorganic materials 0.000 claims abstract description 29
- 229910052682 stishovite Inorganic materials 0.000 claims abstract description 29
- 229910001632 barium fluoride Inorganic materials 0.000 claims abstract description 28
- 238000002425 crystallisation Methods 0.000 claims abstract description 26
- 230000008025 crystallization Effects 0.000 claims abstract description 26
- 229910000019 calcium carbonate Inorganic materials 0.000 claims abstract description 17
- 238000000465 moulding Methods 0.000 claims abstract description 17
- 238000000034 method Methods 0.000 claims abstract description 11
- 229910000018 strontium carbonate Inorganic materials 0.000 claims abstract description 9
- LEDMRZGFZIAGGB-UHFFFAOYSA-L strontium carbonate Chemical compound [Sr+2].[O-]C([O-])=O LEDMRZGFZIAGGB-UHFFFAOYSA-L 0.000 claims abstract description 9
- 239000000463 material Substances 0.000 claims description 25
- 238000002844 melting Methods 0.000 claims description 18
- 230000008018 melting Effects 0.000 claims description 18
- 238000009413 insulation Methods 0.000 claims description 14
- 238000004455 differential thermal analysis Methods 0.000 claims description 8
- 239000002241 glass-ceramic Substances 0.000 abstract description 20
- 238000001816 cooling Methods 0.000 abstract description 2
- 238000007500 overflow downdraw method Methods 0.000 abstract description 2
- 239000013078 crystal Substances 0.000 description 11
- 238000004146 energy storage Methods 0.000 description 8
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 6
- 229910052788 barium Inorganic materials 0.000 description 6
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 description 6
- 229910052802 copper Inorganic materials 0.000 description 6
- 239000010949 copper Substances 0.000 description 6
- 239000000843 powder Substances 0.000 description 6
- 241000628997 Flos Species 0.000 description 5
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 4
- 238000004140 cleaning Methods 0.000 description 4
- 238000005520 cutting process Methods 0.000 description 4
- 239000002003 electrode paste Substances 0.000 description 4
- 238000005498 polishing Methods 0.000 description 4
- 229910052709 silver Inorganic materials 0.000 description 4
- 239000004332 silver Substances 0.000 description 4
- 239000011232 storage material Substances 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 3
- 230000005621 ferroelectricity Effects 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000005352 clarification Methods 0.000 description 2
- 239000010955 niobium Substances 0.000 description 2
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003990 capacitor Substances 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 239000003989 dielectric material Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 239000013081 microcrystal Substances 0.000 description 1
- 229910052758 niobium Inorganic materials 0.000 description 1
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 description 1
- 230000006911 nucleation Effects 0.000 description 1
- 238000010899 nucleation Methods 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000010257 thawing Methods 0.000 description 1
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- Inorganic Insulating Materials (AREA)
- Glass Compositions (AREA)
- Compositions Of Oxide Ceramics (AREA)
Abstract
Strontium barium niobate glass ceramic material of a kind of high-k high breakdown field strength and preparation method thereof, by SrCO3, BaCO3, Nb2O5, CaCO3, SiO2、H3BO3And BaF2Mix homogeneously, melted uniform at 1,300 1400 DEG C, then molding, anneal rapidly, glass after being annealed；Glass after annealing is carried out under its crystallization temperature Crystallizing treatment, then furnace cooling, i.e. obtains strontium barium niobate glass ceramic material.It is easy that the present invention uses fusion method to prepare strontium barium niobate glass ceramic material method, and forming method is more.After being processed by strontium barium niobate glass ceramic material, it is carried out XRD, SEM and EDS test, it was demonstrated that strontium barium niobate glass ceramic material prepared by the present invention has high-k high breakdown field strength and the ferroelectric glass-ceramic of low dielectric loss.
Description
Technical field
The present invention relates to a kind of glass ceramic material and preparation method thereof, particularly a kind of high-k high breakdown field strength
Strontium barium niobate glass ceramic material and preparation method thereof.
Background technology
In recent years, along with developing rapidly of information technology and electronic science and technology, people are to can effectively reduce high pressure
The dielectric material demand with high energy storage density of capacitor volume is urgent, and electronic equipment is proposed higher use requirement, example
Such as lightness and miniaturization, high energy storage material the most just arises at the historic moment.Ferroelectric glass-ceramic is by the ferroelectric phase of high-k
With the functional material with ferroelectric properties of glass phase composition, it has concentrated glass and the advantage of pottery, internal crystallization structure ratio
Crystal in many ceramic materials will the most much, and the most all with densification, almost without pore, dielectric loss is the least, therefore
The glass ceramics utilizing devitrified glass method to prepare possesses the high breakdown strength of glass state material and the high dielectric of dielectric ceramic system
The double dominant of constant, becomes the focus of high energy-accumulating medium investigation of materials.
SBN glass ceramics is used as high energy storage material owing to possessing high disruptive field intensity.Glass basis is mostly at present
SiO2, it makes melt temperature be up to 1500 DEG C, H3BO3Addition melt temperature can be made to be greatly lowered.CaO drops when high temperature
The stickiness of low glass, promotes thawing and the clarification of glass, makes the crystallization tendency of glass increase.Therefore, CaO-SiO is selected2-B2O3
(CBS) system is as glass basis.The addition of glass reduces the porosity of material, increases the disruptive field intensity of material, but
Also reducing crystallization tendency, relatively low crystallization tendency can limit the application as energy storage material.Therefore, in order to improve glass
The crystallization tendency of glass pottery, introduces effective nucleator and goes the degree of crystallinity improving SBN glass ceramics to be necessary.
Summary of the invention
It is an object of the invention to provide a kind of high-k high breakdown field strength strontium barium niobate glass ceramic material and
Its preparation method, the method experimental implementation is simple, the reaction of raw material high uniformity, and the strontium barium niobate glass ceramic material tool prepared
There are disruptive field intensity height, dielectric constant high, and strontium barium niobate glass ceramic material porosity is little.
For achieving the above object, strontium barium niobate glass ceramic material of the present invention, is 12:12:24:2x:2x including mol ratio:
SrO, BaO, Nb of 3x:32O5、CaO、SiO2、B2O3And BaF2, and x=5～8.
The strontium barium niobate glass ceramic material of a kind of high-k high breakdown field strength is to be 12:12:24 by mol ratio:
The SrCO of 2x:2x:6x:33, BaCO3, Nb2O5, CaCO3, SiO2, H3BO3And BaF2Through melted, molding, annealing and Crystallizing treatment
Prepare.
The preparation method of the strontium barium niobate glass ceramic material of a kind of high-k high breakdown field strength, including walking as follows
Rapid:
1) by SrCO3, BaCO3, Nb2O5, CaCO3, SiO2, H3BO3And BaF2According to 12SrO-12BaO-24Nb2O3-
2xCaO-2xSiO2-3xB2O3-3BaF2Mixed in molar ratio is uniform, obtains mixture；Wherein, x=5～8；
2) crucible is heated to 1100 DEG C with stove, is initially added into mixture, then proceed to be heated to 1300-1400 DEG C,
At 1300-1400 DEG C, insulation makes mixture melted uniformly, obtains mixed melting material；By the molding on mould of mixed melting material, then
Put in stove and anneal at 600-800 DEG C, glass after being annealed；
3) after annealing, glass is incubated under its crystallization temperature and carries out Crystallizing treatment, obtains strontium barium niobate glass ceramic material.
X=5,6,7 or 8 in described step 1).
Glass after annealing is determined by the described crystallization temperature in step 3) through DTA differential thermal analysis test.
As x=5, after annealing, the crystallization temperature of glass is 1035 DEG C；As x=6, after annealing, the crystallization temperature of glass is
973℃；As x=7, after annealing, the crystallization temperature of glass is 935 DEG C；As x=8, after annealing, the crystallization temperature of glass is 875
℃。
In described step 3), the Crystallizing treatment time is 3-6h.
Described step 2) in annealing time be 4-7h.
Compared with prior art, the beneficial effects of the present invention is:
Preparation method experimental implementation of the present invention is simple, and forming method is many；The strontium barium niobate glass ceramic material tool prepared
There is the porosity minimum, tests prove that, the Flos persicae shape that the strontium barium niobate glass ceramic material inner homogeneous that the present invention prepares generates
Tridymite crystal makes breakdown strength of material high；Meanwhile, the present invention goes back conservative control ferroelectricity Strontium Barium Niobate Crystal and glass content
Ratio, generate high-k high breakdown field strength and the ferroelectric glass-ceramic of low node loss.
Further, since add BaF in preparation process2As nucleator, BaF2Glass nucleation can be promoted, fluoride
Microcrystal is exactly the nuclearing centre of glass；Meanwhile, BaF2Nucleus formed temperature, less than crystal growth temperature, therefore, through BaF2
Coring, crystallization glassy grain tiny, and promote Strontium Barium Niobate Crystal precipitation.And, the present invention selects CaO-SiO2-B2O3
As glass basis, B2O3It is by H3BO3Add introduce, be mostly SiO with current glass basis2Melt temperature (up to
1500 DEG C) compare, H3BO3Happy and harmonious temperature can be made to be greatly lowered, and CaO is network modifying oxide, and Main Function is to weaken net
Network structure, beneficially glass are founded at a lower temperature and sinter, and reduce the stickiness of glass when high temperature, promote melting of glass
Change and clarification, make the crystallization tendency of glass increase.
Accompanying drawing explanation
Fig. 1 is X-ray diffraction (XRD) collection of illustrative plates of the strontium barium niobate glass ceramic material of the embodiment of the present invention 3 preparation；
Fig. 2 is the SEM figure of the strontium barium niobate glass ceramic material of the embodiment of the present invention 3 preparation；
Fig. 3 is the EDS figure of Flos persicae shape in strontium barium niobate glass ceramic material prepared by the embodiment of the present invention 3；
Fig. 4 is the EDS figure of Flos persicae shaped perimeters in strontium barium niobate glass ceramic material prepared by the embodiment of the present invention 3.
Detailed description of the invention
Embodiment 1:
In the present embodiment strontium barium niobate glass ceramic material include SrO that mol ratio is 12:12:24:10:10:15:3,
BaO、Nb2O5、CaO、SiO2、B2O3And BaF2。
The present embodiment strontium barium niobate glass ceramic material is to be the SrCO of 12:12:24:10:10:30:3 by mol ratio3,
BaCO3, Nb2O5, CaCO3, SiO2, H3BO3And BaF2Prepare through melted, molding, annealing and Crystallizing treatment.
The preparation method of the present embodiment strontium barium niobate glass ceramic material comprises the steps:
1) by SrCO3、BaCO3、Nb2O5、CaCO3、SiO2、H3BO3And BaF2Mix according to 12:12:24:10:10:30:3
Close uniformly, obtain mixture；
2) by silica crucible with stove heating from room temperature to 1100 DEG C time, be initially added into mixture, then proceed to be heated to
1350 DEG C, and at 1350 DEG C, insulation 30min makes mixture melted uniformly, obtains mixed melting material；By mixed melting material at copper
Molding on plate, then put into rapidly the 7h that anneals at 600 DEG C in stove, glass after being annealed；
3) it is ground into powder by glass after taking a small amount of annealing and does DTA differential thermal analysis test, the crystallization of glass after being annealed
Temperature is 1035 DEG C, and insulation 4h carries out Crystallizing treatment at such a temperature, and then furnace cooling is to room temperature, obtains the SrNb2 O6 of bulk
Barium glass ceramic material.
The strontium barium niobate glass ceramics cutting machine obtained by the present embodiment is switched to the thin slice that thickness is 0.1-0.2mm, thin
Sheet, after polishing, cleaning, uniformly coats silver electrode paste at thin slice tow sides, sinters 20 minutes in 600 DEG C, obtains glass to be measured
Glass ceramics sample.
Embodiment 2:
The present embodiment strontium barium niobate glass ceramic material include mol ratio be the SrO of 12:12:24:12:12:18:3, BaO,
Nb2O5、CaO、SiO2、B2O3And BaF2。
The present embodiment strontium barium niobate glass ceramic material is to be the SrCO of 12:12:24:12:12:36:3 by mol ratio3,
BaCO3, Nb2O5, CaCO3, SiO2, H3BO3And BaF2Prepare through melted, molding, annealing and Crystallizing treatment.
The preparation method of the present embodiment strontium barium niobate glass ceramic material comprises the steps:
1) by SrCO3, BaCO3, Nb2O5, CaCO3, SiO2, H3BO3And BaF2Mix according to 12:12:24:12:12:36:3
Close uniformly, obtain mixture；
2) by silica crucible when room temperature is heated to 1100 DEG C with stove, it is initially added into mixture, then proceedes to be heated to
1350 DEG C, and at 1350 DEG C, insulation 30min makes mixture melted uniformly, obtains mixed melting material；By mixed melting material at copper
Molding on plate, then put into rapidly the 7h that anneals at 600 DEG C in stove, glass after being annealed；
3) it is ground into powder by glass after taking a small amount of annealing and does DTA differential thermal analysis test, the crystallization of glass after being annealed
Temperature is 973 DEG C, and insulation 4h carries out Crystallizing treatment at such a temperature, then cools to room temperature with the furnace, obtains the SrNb2 O6 of bulk
Barium glass ceramic material.
The strontium barium niobate glass ceramics cutting machine obtained by the present embodiment is switched to the thin slice that thickness is 0.1-0.2mm, thin
Sheet, after polishing, cleaning, uniformly coats silver electrode paste at thin slice tow sides, sinters 20 minutes in 600 DEG C, obtains glass to be measured
Glass ceramics sample.
Embodiment 3:
The present embodiment strontium barium niobate glass ceramic material include mol ratio be the SrO of 12:12:24:14:14:21:3, BaO,
Nb2O5、CaO、SiO2、B2O3And BaF2。
The present embodiment strontium barium niobate glass ceramic material is to be the SrCO of 12:12:24:14:14:42:3 by mol ratio3,
BaCO3, Nb2O5, CaCO3, SiO2, H3BO3And BaF2Prepare through melted, molding, annealing and Crystallizing treatment.
The preparation method of the present embodiment strontium barium niobate glass ceramic material comprises the steps:
1) by SrCO3, BaCO3, Nb2O5, CaCO3, SiO2, H3BO3And BaF2According to 12:12:24:14:14:42:3's
Mixed in molar ratio is uniform, obtains mixture；
2) by silica crucible when room temperature is heated to 1100 DEG C with stove, it is initially added into mixture, then proceedes to be heated to
1350 DEG C, and at 1350 DEG C, insulation 30min makes mixture melted uniformly, obtains mixed melting material；By mixed melting material at copper
Molding on plate, then put into rapidly the 7h that anneals at 600 DEG C in stove, glass after being annealed；
3) it is ground into powder by glass after taking a small amount of annealing and does DTA differential thermal analysis test, the crystallization of glass after being annealed
Temperature is 935 DEG C, and insulation 4h carries out Crystallizing treatment at such a temperature, then cools to room temperature with the furnace, obtains the SrNb2 O6 of bulk
Barium glass ceramic material；
The strontium barium niobate glass ceramics cutting machine obtained by the present embodiment is switched to the thin slice that thickness is 0.1-0.2mm, thin
Sheet, after polishing, cleaning, uniformly coats silver electrode paste at thin slice tow sides, sinters 20 minutes in 600 DEG C, obtains glass to be measured
Glass ceramics sample.
As it is shown in figure 1, generate the purest Strontium Barium Niobate Crystal in this embodiment 3, and amount of crystals is big, has meanwhile
A small amount of SiO2Crystal separates out.As in Figure 2-4, the SEM photograph of the strontium barium niobate glass ceramics prepared by embodiment 3 and EDS
The Flos persicae shape that in photo, color is the deepest is SiO2, other are Strontium Barium Niobate Crystal.Flos persicae shape SiO2Uniformly generate, show niobium
Acid strontium barium glass pottery inner glass is uniformly distributed with ferroelectricity Strontium Barium Niobate Crystal, and fusion method prepares glass ceramics porosity pole
Little.
Embodiment 4:
The present embodiment strontium barium niobate glass ceramic material include mol ratio be the SrO of 12:12:24:16:16:24:3, BaO,
Nb2O5、CaO、SiO2、B2O3And BaF2。
The present embodiment strontium barium niobate glass ceramic material is to be the SrCO of 12:12:24:16:16:48:3 by mol ratio3,
BaCO3, Nb2O5, CaCO3, SiO2, H3BO3And BaF2Prepare through melted, molding, annealing and Crystallizing treatment.
The preparation method of the present embodiment strontium barium niobate glass ceramic material comprises the steps:
1) by SrCO3, BaCO3, Nb2O5, CaCO3, SiO2, H3BO3And BaF212:12:24:16:16:48:3 mole
Mix homogeneously, obtains mixture；
2) by silica crucible when room temperature is heated to 1100 DEG C with stove, it is initially added into mixture, then proceedes to be heated to
1350 DEG C, and at 1350 DEG C, insulation 30min makes mixture melted uniformly, obtains mixed melting material；By mixed melting material at copper
Molding on plate, then put into rapidly the 7h that anneals at 600 DEG C in stove, glass after being annealed；
3) by doing DTA differential thermal analysis test, the crystallization of glass after being annealed after glass is ground into powder after a small amount of annealing
Temperature is 875 DEG C, and insulation 4h carries out Crystallizing treatment at such a temperature, then cools to room temperature with the furnace, obtains the SrNb2 O6 of bulk
Barium glass ceramic material.
The strontium barium niobate glass ceramics cutting machine obtained by the present embodiment is switched to the thin slice that thickness is 0.1-0.2mm, thin
Sheet, after polishing, cleaning, uniformly coats silver electrode paste at thin slice tow sides, sinters 20 minutes in 600 DEG C, obtains glass to be measured
Glass ceramics sample.
Dielectric properties test data (1kHz) of the glass ceramics sample to be measured of table one preparation
According to energy storage formula:ε0For dielectric constant of air, εrDielectric for glass ceramics sample to be measured
Constant, EbFor disruptive field intensity；Disruptive field intensity is to affect energy storage density the most significantly one of factor, and glass ceramic material is because of glass
Existence dielectric constant reduce, disruptive field intensity increases, as it can be seen from table 1 the present invention is by conservative control ferroelectricity strontium barium niobate
Crystal and the ratio of glass content, generate high-k high breakdown field strength and the ferroelectric glass-ceramic of low dielectric loss.Molten
Melting legal system Preparation Method easy, forming method is more, and resistance to breakdown strength is high, is the important method preparing high energy storage density material.Should
The strontium barium niobate glass ceramics of the high-k high breakdown field strength of invention preparation is expected to substitute conventional iron electroceramics material to be become
Energy storage material is held concurrently one of excellent important candidate material technically and economically.
Embodiment 5:
The present embodiment strontium barium niobate glass ceramic material include mol ratio be the SrO of 12:12:24:12:12:18:3, BaO,
Nb2O5、CaO、SiO2、B2O3And BaF2。
The present embodiment strontium barium niobate glass ceramic material is to be the SrCO of 12:12:24:12:12:36:3 by mol ratio3,
BaCO3, Nb2O5, CaCO3, SiO2, H3BO3And BaF2Prepare through melted, molding, annealing and Crystallizing treatment.
The preparation method of the present embodiment strontium barium niobate glass ceramic material comprises the steps:
1) by SrCO3, BaCO3, Nb2O5, CaCO3, SiO2, H3BO3And BaF2Mix according to 12:12:24:12:12:36:3
Close uniformly, obtain mixture；
2) by silica crucible when room temperature is heated to 1100 DEG C with stove, it is initially added into mixture, then proceedes to be heated to
1300 DEG C, and at 1300 DEG C, insulation 30min makes mixture melted uniformly, obtains mixed melting material；By mixed melting material at copper
Molding on plate, then put into rapidly the 6.5h that anneals at 680 DEG C in stove, glass after being annealed；
3) it is ground into powder by glass after taking a small amount of annealing and does DTA differential thermal analysis test, the crystallization of glass after being annealed
Temperature is 973 DEG C, and insulation 3h carries out Crystallizing treatment at such a temperature, then cools to room temperature with the furnace, obtains the SrNb2 O6 of bulk
Barium glass ceramic material.
Embodiment 6:
The present embodiment strontium barium niobate glass ceramic material include mol ratio be the SrO of 12:12:24:16:16:24:3, BaO,
Nb2O5、CaO、SiO2、B2O3And BaF2。
The present embodiment strontium barium niobate glass ceramic material is to be the SrCO of 12:12:24:16:16:48:3 by mol ratio3,
BaCO3, Nb2O5, CaCO3, SiO2, H3BO3And BaF2Prepare through melted, molding, annealing and Crystallizing treatment.
The preparation method of the present embodiment strontium barium niobate glass ceramic material comprises the steps:
1) by SrCO3, BaCO3, Nb2O5, CaCO3, SiO2, H3BO3And BaF212:12:24:16:16:48:3 mole
Mix homogeneously, obtains mixture；
2) by silica crucible when room temperature is heated to 1100 DEG C with stove, it is initially added into mixture, then proceedes to be heated to
1400 DEG C, and at 1400 DEG C, insulation 30min makes mixture melted uniformly, obtains mixed melting material；By mixed melting material at copper
Molding on plate, then put into rapidly the 4h that anneals at 800 DEG C in stove, glass after being annealed；
3) by doing DTA differential thermal analysis test, the crystallization of glass after being annealed after glass is ground into powder after a small amount of annealing
Temperature is 875 DEG C, and insulation 6h carries out Crystallizing treatment at such a temperature, then cools to room temperature with the furnace, obtains the SrNb2 O6 of bulk
Barium glass ceramic material.
The foregoing is only one embodiment of the present invention, be not all of or unique embodiment, this area leads to skill
The conversion of any equivalence that technical solution of the present invention is taked by art personnel by reading description of the invention, is the present invention's
Claim is contained.
Claims (7)
1. the strontium barium niobate glass ceramic material of a high-k high breakdown field strength, it is characterised in that: be 12 by mol ratio:
SrO, BaO, Nb of 12:24:2x:2x:3x:32O5、CaO、SiO2、B2O3And BaF2Composition, and x=5,6,7 or 8.
2. the strontium barium niobate glass ceramic material of a high-k high breakdown field strength, it is characterised in that: this strontium barium niobate glass
Glass ceramic material is to be the SrCO of 12:12:24:2x:2x:6x:3 by mol ratio3, BaCO3, Nb2O5, CaCO3, SiO2, H3BO3With
And BaF2Prepare through melted, molding, annealing and Crystallizing treatment；Wherein, x=5,6,7 or 8.
3. the preparation method of the strontium barium niobate glass ceramic material of a high-k high breakdown field strength, it is characterised in that bag
Include following steps:
1) by SrCO3, BaCO3, Nb2O5, CaCO3, SiO2, H3BO3And BaF2According to 12SrO-12BaO-24Nb2O3-2xCaO-
2xSiO2-3xB2O3-3BaF2Mixed in molar ratio is uniform, obtains mixture；Wherein, x=5,6,7 or 8；
2) crucible is heated to 1100 DEG C with stove, is initially added into mixture, then proceed to be heated to 1300-1400 DEG C, at 1300-
At 1400 DEG C, insulation makes mixture melted uniformly, obtains mixed melting material；By the molding on mould of mixed melting material, place into stove
In at 600-800 DEG C anneal, glass after being annealed；
3) after annealing, glass is incubated under its crystallization temperature and carries out Crystallizing treatment, obtains strontium barium niobate glass ceramic material.
The preparation side of the strontium barium niobate glass ceramic material of high-k high breakdown field strength the most according to claim 3
Method, it is characterised in that: described step 3) in crystallization temperature by glass after annealing through DTA differential thermal analysis test determine.
The preparation side of the strontium barium niobate glass ceramic material of high-k high breakdown field strength the most according to claim 4
Method, it is characterised in that: as x=5, after annealing, the crystallization temperature of glass is 1035 DEG C；As x=6, the crystallization of glass after annealing
Temperature is 973 DEG C；As x=7, after annealing, the crystallization temperature of glass is 935 DEG C；As x=8, the crystallization temperature of glass after annealing
Degree is 875 DEG C.
The preparation side of the strontium barium niobate glass ceramic material of high-k high breakdown field strength the most according to claim 3
Method, it is characterised in that: described step 3) in the Crystallizing treatment time be 3-6h.
The preparation side of the strontium barium niobate glass ceramic material of high-k high breakdown field strength the most according to claim 3
Method, it is characterised in that: described step 2) in annealing time be 4-7h.
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| CN105236745A (en) * | 2015-08-27 | 2016-01-13 | 陕西科技大学 | Ferromagnetic Fe3O4 nano micro-crystal glass and preparation method thereof |
| CN105110647A (en) * | 2015-08-27 | 2015-12-02 | 陕西科技大学 | Ferromagnetic Sr2FeSi2O7 microcrystal glass and preparation method thereof |
| CN105254180B (en) * | 2015-09-22 | 2018-01-02 | 陕西科技大学 | A kind of K applied to energy storage2O‑Na2O‑Nb2O5‑SiO2‑B2O3System glass ceramic material and preparation method thereof |
| CN105399333A (en) * | 2015-11-10 | 2016-03-16 | 同济大学 | Strontium barium niobate-based glass ceramic energy storage material and preparation method thereof |
| CN105712634B (en) * | 2016-01-19 | 2018-12-18 | 同济大学 | Lanthanum oxide doping strontium barium niobate base glass ceramics energy storage material and preparation method thereof |
| CN106865988A (en) * | 2017-02-25 | 2017-06-20 | 郑州坤博科技有限公司 | A kind of energy storage high breakdown field strength microcrystal glass material high and preparation method thereof |
| CN109020232B (en) * | 2018-10-31 | 2021-08-17 | 成都光明光电有限责任公司 | Glass ceramics |
| CN110981479B (en) * | 2020-01-10 | 2022-03-01 | 陕西科技大学 | High-breakdown ferroelectric ceramic and preparation method thereof |
| CN111362578B (en) * | 2020-03-09 | 2022-06-21 | 广东四维新材料有限公司 | Microcrystalline glass ceramic for 6G communication filter and preparation method thereof |
| CN116081952A (en) * | 2023-03-03 | 2023-05-09 | 电子科技大学 | High-hardness boron niobate energy storage microcrystalline glass and preparation method thereof |
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| CN103102079A (en) * | 2011-11-10 | 2013-05-15 | 北京有色金属研究总院 | Glass ceramic dielectric with high breakdown strength and preparation method thereof |
| CN103342466B (en) * | 2013-06-27 | 2015-05-20 | 桂林电子科技大学 | Strontium barium niobate based glass-ceramic dielectric material and preparation method thereof |
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