CN105418068B - A kind of niobate glass ceramics energy storage material and its preparation method and application - Google Patents
A kind of niobate glass ceramics energy storage material and its preparation method and application Download PDFInfo
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Abstract
The present invention relates to a kind of new niobate glass ceramics energy storage material and its preparation method and application, chemical composition is [(Ba1‑ xSrx)2NaNb5O15]0.6‑[SiO2]0.4, wherein 0≤x≤1.With BaCO3、SrCO3、NaCO3、Nb2O5、SiO2Powder is raw material, and the quality of each component has been weighed according to the chemical composition of design, and the fusing of crucible high temperature is added after ball milling mixing is uniform, high-temperature fusant Quick pouring is removed into destressing into the copper mould preheated in advance, is then cut into the thin slice that thickness is 1.0mm；Glass flake is put into annealing furnace and carries out Controlled Crystallization, by controlling component of glass raw material and optimization crystallization technique, the niobates glass ceramics of preparation has higher energy storage density and reliability.Compared with prior art, the inventive method is simple, and prepared glass ceramic material shows there is higher energy storage density and higher efficiency for charge-discharge by experimental test, is expected to be used as novel energy-storing capacitor material.
Description
Technical field
The invention belongs to field of dielectric energy storage material, more particularly, to a kind of new niobate glass ceramics energy storage material
Material and its preparation method and application.
Background technology
In order to meet the miniaturization of pulse power system and light-weighted requirement, the hair as the dielectric material of core component
Developable surface faces more challenges, and how further to improve the energy storage density of dielectric substance turns into the focus of research, the work of various countries' material
Person just tries to explore research with high-k, the low dielectric material for connecing electrical loss and high dielectric strength.Ferroelectric niobates glass
Glass ceramics are in recent years because its excellent dielectric properties in the field causes extensive concern.What is be widely studied at present is main
There are strontium barium niobate (SrxBa1-xNb2O6, x=0.25-0.75), lead meta-columbute (PbNb2O6), barium sodium niobate (BNN) (Ba2NaNb5O15)、
The systems such as potassium niobate (KNbO3), sodium niobate (NaNbO3).
In niobate glass ceramics system, the higher predominantly lead meta-columbute (PbNb of the energy storage density reported at present2O6)
Base glass ceramics system, Du Jun et al. are prepared for NaNbO using the method for controllable crystallization3-PbNb2O6-SiO2、(Pb,Sr)
Nb2O6-NaNbO3-SiO2Etc. system glass ceramics, by optimizing preparation technology, higher energy-storage property has been obtained
([Preparation and characterization of dielectric glass-ceramics in Na2O–PbO–
Nb2O5–SiO2system,Materials Letters 59(2005)2821-2826]).But these systems contain lead,
Facial pallor is volatile at high temperature, again harmful to environment.There is a document report, the AF45 glass of Schott AG's production has high resistance to hit
Wear voltage, measured in laboratory its it is breakdown voltage resistant reach 12MV/cm, the maximum energy storage density of AF45 glass reaches after tested
35J/cm3([Alkali-free glass as a high energy density dielectric material,
Materials Letters 63 (2009) 1245-1248]), but the composition of AF45 glass is excessively complicated, and the glass
Viscosity is too big, it is difficult to prepare under normal conditions.Zeng et al. effectively increases BaO-SrO-Nb by adulterating BaF22O5-B2O3
The dielectric constant of system glass ceramics, but the resistance to disruptive field intensity of the system only has 527Kv/cm, thus energy storage density is relatively low
([Effect of BaF2addition on crystallization kinetics and dielectric
properties of B2O3-Nb2O5-SrO-BaO glass-ceramics,J.Am.Ceram Soc,2011,94(2):
469]).This group, which uses early stage, is based on BaO-B2O3-Al2O3-SiO2As glass phase main component, ferroelectric niobates are prepared for
Glass ceramics ([Dielectric properties and charge-discharge behaviors in niobate
glass ceramics for energy-storage applications,Journal of Alloys and
Compounds 617 (2014) 418-422.]), still, because the composition of glass base is excessively complicated, not only preparation technology is more multiple
It is miscellaneous, and in Crystallization Process, it is easy to many impurities phases are formed, so as to influence the energy storage characteristic of glass ceramics.
Chinese patent CN 104671665A disclose crown glass ceramics of low-dielectric loss and preparation method thereof, the glass
Glass ceramics into being grouped into：aBaO-bSrO-cNb2O5-dZnO-xSiO2-yB2O3- zREO, wherein, a, b, c, d, x, y, z are
Mol ratio between mol ratio expression composition, REO represent rare earth oxide；And meet：0≤a≤10.35,9.97≤b≤
20.70,20.19≤c≤20.70,14.80≤d≤15.50,14.56≤x≤15.00,27.51≤y≤28.10,0≤z≤
3.00.Selection raw material is formed according to the composition of glass ceramics, mixed in proportion, high-temperature fusion；Uniform glass precursor solution will be melted
It is quickly poured into the metal die of preheating, is cooled and shaped, stress relief annealing；Obtained sheet glass is subjected to controllable crystallization treatment i.e.
Can.The system principal crystalline phase is BaxSr1-xNbO3, glass is mutually ZnO-SiO2-B2O3, but because the system component is excessively multiple
It is miscellaneous, uneven components are easily caused in Sample Preparation Procedure, and in Crystallization Process, many impurities phases are easily generated, from
And cause the disruptive field intensity of the series of samples relatively low, and from the point of view of the breakdown strength of patent report, the breakdown strength of all samples
Not less than 200Kv/mm, well below the [(Ba involved by this patent1-xSrx)2NaNb5O15]0.6-[SiO2]0.4Breakdown it is strong
Angle value.
The content of the invention
It is an object of the present invention to overcome the above-mentioned drawbacks of the prior art and provide one kind improves glass ceramics
Dielectric constant while also improve new niobate glass ceramics energy storage material of resistance to disruptive field intensity and preparation method thereof
And application.
The purpose of the present invention can be achieved through the following technical solutions：
Niobate glass ceramics energy storage material, chemical composition are [(Ba1-xSrx)2NaNb5O15]0.6-[SiO2]0.4, wherein
0≤x≤1。
X span is preferably 0.1≤x≤0.5.
X span is most preferably 0.25.
The preparation method of new niobate glass ceramics energy storage material, using following steps：
(1) with analytically pure BaCO3、SrCO3、NaCO3、Nb2O5、B2O3、Al2O3、SiO2Powder is raw material, according to energy storage
The formula stock of the chemical composition of material；
(2) using absolute ethyl alcohol as dispersant, ball milling in ball grinder is placed in using agate ball and by said components, and will be mixed
Close uniform slurry drying；
(3) frit after drying is added into the fusing of crucible high temperature, then by high-temperature fusant Quick pouring to prior
In the copper mould of preheating, the clear glass block without crystallization is made, glass block is put into stress relief annealing in annealing furnace；
(4) clear glass block is thinly sliced using slicer；Glass flake is put into annealing furnace and carries out controlled analysis
Crystalline substance, the heating rate of annealing furnace is 3-5 DEG C/min, and recrystallization temperature is 800-1100 DEG C, soaking time 1-3h, that is, is prepared
Niobate glass ceramics energy storage material.
The time of ball mill mixing is 10~20h in step (2).
For step (3) during high temperature melting, the heating rate of glass furnace is 1-2 DEG C/min, and 3h is incubated at 800 DEG C, high
The temperature of temperature fusing is 1400~1600 DEG C, and time of high temperature melting is 2~5h, and copper mould is preheated to 500-650 DEG C in advance, excellent
Select 600 DEG C；Then glass block is put into destressing in annealing furnace, destressing holding temperature is 500-650 DEG C, preferably 600 DEG C；
Soaking time is 3-5h, and insulation terminates rear furnace cooling.
When step (4) carries out Controlled Crystallization, the heating rate of annealing furnace is 3-5 DEG C/min, recrystallization temperature 800-1100
DEG C, soaking time 2-3h, insulation terminates rear furnace cooling.
New niobate glass ceramics energy storage material can be applied in energy-storage capacitor Material Field.With prior art phase
Than the dielectric properties of glass ceramics of the present invention are the results by glass phase and crystalline phase performance synergy.The presence of glass phase makes
Obtaining devitrified glass has higher disruptive field intensity, and the composition of crystalline phase and content have important shadow to dielectric constant of material etc.
Ring.Glass ceramics has higher disruptive field intensity, and the dielectric constant of material how is improved on the voltage endurance for keeping high
Deng the difficult point as research.The present invention uses and is based on SiO2As glass phase, with BaO (SrO)-Na2O-Nb2O5As ceramic phase,
Glass block is prepared by the method for fast melt-quenching, preparing ferroelectric niobates glass by the method for controllable crystallization after section makes pottery
Porcelain, by adjusting the ratio of glass phase and ceramic phase, using the macroscopic property of glass, using the crystallization technique of optimization, by spy
The glass for determining component carries out Crystallizing treatment under certain condition, originally uniform, fine and close flawless glass is mutually formed containing big
Measure the ferroelectric ceramics crystallite phase and the mutually equally distributed composite of glass of high-k.Component 6Na2O-18BaO-6SrO-
30Nb2O5-40SiO2Glass passes through the glass ceramics sample of 1000 DEG C of crystallizations after tested, and the dielectric constant of the sample is at room temperature
81, disruptive field intensity 1212Kv/cm, by calculating, its energy storage density reaches 5.27J/cm3。
Brief description of the drawings
Fig. 1 is the XRD spectrums that product is prepared in embodiment 1-5 after 1000 DEG C of crystallizations；
Fig. 2 is that XRD spectrum of the product after different temperatures crystallization is prepared in embodiment 2；
Fig. 3 is that product dielectric constant with temperature change curve after 1000 DEG C of crystallizations is prepared in embodiment 1-5；
Fig. 4 is that resistance to disruptive field intensity of the product after 1000 DEG C of crystallizations is prepared in embodiment 1-5；
Fig. 5 is that activation energy and disruptive field intensity of the product after 1000 DEG C of crystallizations is prepared in embodiment 1-5.
Embodiment
The present invention is described in detail with specific embodiment below in conjunction with the accompanying drawings.
Embodiment 1 (x=0)
The niobates glass ceramics 6Na of high energy storage density2O-24BaO-30Nb2O5-40SiO2
(1) with analytically pure BaCO3、NaCO3、Nb2O5、SiO2Powder is raw material, according to the chemical composition 6Na of design2O-
24BaO-30Nb2O5-40SiO2The quality of each component is weighed, sample gross mass is 80-100 grams.
(2) from absolute ethyl alcohol as dispersant, using agate ball, ball milling, rotating speed are in polytetrafluoroethylene (PTFE) ball grinder
50-60 turns/min, and well mixed slurry is dried.The time of ball milling is 20~30h, ratio of grinding media to material during ball milling for (1.0~
1.5)：1.
(3) frit after drying is added into the fusing of crucible high temperature, the temperature of high temperature furnace heating rate high temperature melting
For 1400 DEG C, the time of high temperature melting is 5h.Then by high-temperature fusant Quick pouring into the copper mould preheated in advance, nothing is made
The clear glass block of crystallization, glass block is put into stress relief annealing in annealing furnace.The temperature that copper mould preheats in advance is 500
℃；Then glass block is put into destressing in annealing furnace, destressing holding temperature is 500 DEG C；Soaking time is 5h；Insulation knot
The type of cooling is furnace cooling after beam.
(4) clear glass block is cut into the thin slice that thickness is 1.0mm using slicer；Glass flake is put into annealing furnace
Middle carry out Controlled Crystallization, the heating rate of annealing furnace is 3 DEG C/min, and recrystallization temperature is 1000 DEG C, and soaking time is 2 hours, is protected
It is furnace cooling that temperature, which terminates the rear type of cooling, finally gives niobates glass ceramics sample.
The XRD spectrum of ceramics sample obtained by the present embodiment is as shown in x=0 curves in Fig. 1, x in dielectric properties such as Fig. 3
Shown in=0 curve, resistance to sparking can be as shown in x=0 curves in Fig. 4, by the glass ceramics sample of 1000 DEG C of crystallizations through survey
Examination, the dielectric constant of the sample is 78, disruptive field intensity 1075kV/cm at room temperature, and by calculating, its energy storage density reaches
3.99J/cm3。
Embodiment 2 (x=0.25)
The niobates glass ceramics 6Na of high energy storage density2O-18BaO-6SrO-30Nb2O5-40SiO2
(1) with analytically pure BaCO3、SrCO3、NaCO3、Nb2O5、B2O3、Al2O3、SiO2Powder is raw material, according to design
Chemical composition 6Na2O-18BaO-6SrO-30Nb2O5-40SiO2The quality of each component is weighed, sample gross mass is 80-100
Gram.
(2) from absolute ethyl alcohol as dispersant, using agate ball, ball milling, rotating speed are in polytetrafluoroethylene (PTFE) ball grinder
50-60 turns/min, and well mixed slurry is dried.The time of ball milling is 20~30h, ratio of grinding media to material during ball milling for (1.0~
1.5)：1.
(3) frit after drying is added into the fusing of crucible high temperature, the temperature of high temperature furnace heating rate high temperature melting
For 1500 DEG C, the time of high temperature melting is 5h.Then by high-temperature fusant Quick pouring into the copper mould preheated in advance, nothing is made
The clear glass block of crystallization, glass block is put into stress relief annealing in annealing furnace.The temperature that copper mould preheats in advance is 600
℃；Then glass block is put into destressing in annealing furnace, destressing holding temperature is 600 DEG C；Soaking time is 4h；Insulation knot
The type of cooling is furnace cooling after beam.
(4) clear glass block is cut into the thin slice that thickness is 1.0mm using slicer；Glass flake is put into annealing furnace
Middle carry out Controlled Crystallization, the heating rate of annealing furnace is 4 DEG C/min, and recrystallization temperature is 1000 DEG C, and soaking time is 2 hours, is protected
It is furnace cooling that temperature, which terminates the rear type of cooling, finally gives niobates glass ceramics sample.
The XRD spectrum of ceramics sample obtained by the present embodiment is as shown in Fig. 2 curves, x=0.25 in dielectric properties such as Fig. 3
Shown in curve, resistance to sparking can be as shown in x=0.25 curves in Fig. 4, by the glass ceramics sample of 1000 DEG C of crystallizations through survey
Examination, the dielectric constant of the sample is 81, disruptive field intensity 1212kV/cm at room temperature, and by calculating, its energy storage density reaches
5.27J/cm3。
Embodiment 3 (x=0.50)
The niobates glass ceramics 6Na of high energy storage density2O-12BaO-12SrO-30Nb2O5-40SiO2
(1) with analytically pure BaCO3、SrCO3、NaCO3、Nb2O5、SiO2Powder is raw material, according to the chemical composition of design
6Na2O-12BaO-12SrO-30Nb2O5-40SiO2The quality of each component is weighed, sample gross mass is 80-100 grams.
(2) from absolute ethyl alcohol as dispersant, using agate ball, ball milling, rotating speed are in polytetrafluoroethylene (PTFE) ball grinder
50-60 turns/min, and well mixed slurry is dried.The time of ball milling is 20~30h, ratio of grinding media to material during ball milling for (1.0~
1.5)：1.
(3) frit after drying is added into the fusing of crucible high temperature, the temperature of high temperature furnace heating rate high temperature melting
For 1600 DEG C, the time of high temperature melting is 2h.Then by high-temperature fusant Quick pouring into the copper mould preheated in advance, nothing is made
The clear glass block of crystallization, glass block is put into stress relief annealing in annealing furnace.The temperature that copper mould preheats in advance is 650
℃；Then glass block is put into destressing in annealing furnace, destressing holding temperature is 650 DEG C, soaking time 3h；Insulation knot
The type of cooling is furnace cooling after beam.
(4) clear glass block is cut into the thin slice that thickness is 1.0mm using slicer；Glass flake is put into annealing furnace
Middle carry out Controlled Crystallization, the heating rate of annealing furnace is 5 DEG C/min, and recrystallization temperature is 1100 DEG C, and soaking time is 2 hours, is protected
It is furnace cooling that temperature, which terminates the rear type of cooling, finally gives niobates glass ceramics sample.
The XRD spectrum of ceramics sample obtained by the present embodiment is as shown in x=0.50 curves in Fig. 1, dielectric properties such as Fig. 3
Shown in middle x=0.50 curves, resistance to sparking can be as shown in x=0.50 curves in Fig. 4, by the glass ceramics of 1000 DEG C of crystallizations
After tested, the dielectric constant of the sample is 93, disruptive field intensity 963kV/cm to sample at room temperature, by calculating, its energy storage density
Reach 3.81J/cm3。
Embodiment 4 (x=0.75)
The niobates glass ceramics 6Na of high energy storage density2O-6BaO-18SrO-30Nb2O5-40SiO2
(1) with analytically pure BaCO3、SrCO3、NaCO3、Nb2O5、SiO2Powder is raw material, according to the chemical composition of design
6Na2O-6BaO-18SrO-30Nb2O5-40SiO2The quality of each component is weighed, sample gross mass is 80-100 grams.
(2) from absolute ethyl alcohol as dispersant, using agate ball, ball milling, rotating speed are in polytetrafluoroethylene (PTFE) ball grinder
50-60 turns/min, and well mixed slurry is dried.The time of ball milling is 20~30h, ratio of grinding media to material during ball milling for (1.0~
1.5)：1.
(3) frit after drying is added into the fusing of crucible high temperature, the temperature of high temperature furnace heating rate high temperature melting
For 1600 DEG C, the time of high temperature melting is 5h.Then by high-temperature fusant Quick pouring into the copper mould preheated in advance, nothing is made
The clear glass block of crystallization, glass block is put into stress relief annealing in annealing furnace.The temperature that copper mould preheats in advance is 650
DEG C, glass block is then put into destressing in annealing furnace, destressing holding temperature is 600 DEG C；Soaking time is 5h；Insulation knot
The type of cooling is furnace cooling after beam.
(4) clear glass block is cut into the thin slice that thickness is 1.0mm using slicer；Glass flake is put into annealing furnace
Middle carry out Controlled Crystallization, the heating rate of annealing furnace is 5 DEG C/min, and recrystallization temperature is 1000 DEG C, and soaking time is 2 hours, is protected
It is furnace cooling that temperature, which terminates the rear type of cooling, finally gives niobates glass ceramics sample.
The XRD spectrum of ceramics sample obtained by the present embodiment is as shown in x=0.75 curves in Fig. 1, dielectric properties such as Fig. 3
Shown in middle x=0.75 curves, resistance to sparking can be as shown in x=0.75 curves in Fig. 4, by the glass ceramics of 1000 DEG C of crystallizations
After tested, the dielectric constant of the sample is 72, disruptive field intensity 820kV/cm to sample at room temperature, by calculating, its energy storage density
Reach 2.14J/cm3。
Embodiment 5 (x=1)
The niobates glass ceramics 6Na of high energy storage density2O-24SrO-30Nb2O5-40SiO2
(1) with analytically pure SrCO3、NaCO3、Nb2O5、SiO2Powder is raw material, according to the chemical composition 6Na of design2O-
24SrO-30Nb2O5-40SiO2The quality of each component is weighed, sample gross mass is 80-100 grams.
(2) from absolute ethyl alcohol as dispersant, using agate ball, ball milling, rotating speed are in polytetrafluoroethylene (PTFE) ball grinder
50-60 turns/min, and well mixed slurry is dried.The time of ball milling is 20~30h, ratio of grinding media to material during ball milling for (1.0~
1.5)：1.
(3) frit after drying is added into the fusing of crucible high temperature, the temperature of high temperature furnace heating rate high temperature melting
For 1500 DEG C, the time of high temperature melting is 4h.Then by high-temperature fusant Quick pouring into the copper mould preheated in advance, nothing is made
The clear glass block of crystallization, glass block is put into stress relief annealing in annealing furnace.The temperature that copper mould preheats in advance is 500
℃；Then glass block is put into destressing in annealing furnace, destressing holding temperature is 650 DEG C；Soaking time is 4h；Insulation knot
The type of cooling is furnace cooling after beam.
(4) clear glass block is cut into the thin slice that thickness is 1.0mm using slicer；Glass flake is put into annealing furnace
Middle carry out Controlled Crystallization, the heating rate of annealing furnace is 4 DEG C/min, and recrystallization temperature is 1100 DEG C, and soaking time is 2 hours, is protected
It is furnace cooling that temperature, which terminates the rear type of cooling, finally gives niobates glass ceramics sample.
The XRD spectrum of ceramics sample obtained by the present embodiment is as shown in x=1 curves in Fig. 1, x in dielectric properties such as Fig. 3
=0.75 curve is shown, resistance to sparking can pass through as shown in x=1 curves in Fig. 4 by the glass ceramics sample of 1000 DEG C of crystallizations
Test, the dielectric constant of the sample is 65, disruptive field intensity 713kV/cm at room temperature, and by calculating, its energy storage density reaches
1.46J/cm3。
Table 1 is that energy storage density of the product after 1000 DEG C of crystallizations is prepared in embodiment 1-5
。
Claims (8)
1. a kind of niobate glass ceramics energy storage material, it is characterised in that the chemical composition of the energy storage material is [(Ba1- xSrx)2NaNb5O15]0.6-[SiO2]0.4, wherein 0≤x≤1, the energy storage material is prepared using following methods：
(1) with analytically pure BaCO3、SrCO3、NaCO3、Nb2O5、SiO2Powder is raw material, according to the chemical composition of energy storage material
Formula stock；
(2) using absolute ethyl alcohol as dispersant, ball milling in ball grinder is placed in using agate ball and by said components, and will mix equal
Even slurry drying；
(3) frit after drying is added into the fusing of crucible high temperature, then by high-temperature fusant Quick pouring to prior preheating
Copper mould in, be made the clear glass block without crystallization, glass block is put into stress relief annealing in annealing furnace, in high temperature melting
During change, the heating rate of glass furnace is 1-2 DEG C/min, 3h is incubated at 800 DEG C, the temperature of high temperature melting is 1400~1600
DEG C, the time of high temperature melting is 2~5h；
(4) clear glass block is thinly sliced using slicer；Glass flake is put into annealing furnace and carries out Controlled Crystallization, is moved back
The heating rate of stove is 3-5 DEG C/min, and recrystallization temperature is 800-1100 DEG C, soaking time 1-3h, that is, niobic acid is prepared
Based glass ceramics energy storage material.
2. a kind of niobate glass ceramics energy storage material according to claim 1, it is characterised in that x value is
0.25。
A kind of 3. preparation method of niobate glass ceramics energy storage material as claimed in claim 1, it is characterised in that the party
Method uses following steps：
(1) with analytically pure BaCO3、SrCO3、NaCO3、Nb2O5、SiO2Powder is raw material, according to the chemical composition of energy storage material
Formula stock；
(2) using absolute ethyl alcohol as dispersant, ball milling in ball grinder is placed in using agate ball and by said components, and will mix equal
Even slurry drying；
(3) frit after drying is added into the fusing of crucible high temperature, then by high-temperature fusant Quick pouring to prior preheating
Copper mould in, be made the clear glass block without crystallization, glass block is put into stress relief annealing in annealing furnace, in high temperature melting
During change, the heating rate of glass furnace is 1-2 DEG C/min, 3h is incubated at 800 DEG C, the temperature of high temperature melting is 1400~1600
DEG C, the time of high temperature melting is 2~5h；
(4) clear glass block is thinly sliced using slicer；Glass flake is put into annealing furnace and carries out Controlled Crystallization, is moved back
The heating rate of stove is 3-5 DEG C/min, and recrystallization temperature is 800-1100 DEG C, soaking time 1-3h, that is, niobic acid is prepared
Based glass ceramics energy storage material.
A kind of 4. preparation method of niobate glass ceramics energy storage material according to claim 3, it is characterised in that step
Suddenly the time of ball mill mixing is 10~20h in (2).
A kind of 5. preparation method of niobate glass ceramics energy storage material according to claim 3, it is characterised in that step
Suddenly the copper mould in (3) is preheated to 500-650 DEG C in advance；Then glass block is put into destressing in annealing furnace, destressing is protected
Temperature is 500-650 DEG C；Soaking time is 3-5h, and insulation terminates rear furnace cooling.
A kind of 6. preparation method of niobate glass ceramics energy storage material according to claim 3, it is characterised in that step
Suddenly the copper mould in (3) is preheated to 600 DEG C in advance, and destressing holding temperature is 600 DEG C.
A kind of 7. preparation method of niobate glass ceramics energy storage material according to claim 3, it is characterised in that step
Suddenly when (4) carry out Controlled Crystallization, the heating rate of annealing furnace is 3-5 DEG C/min, and recrystallization temperature is 800-1100 DEG C, soaking time
For 2-3h, insulation terminates rear furnace cooling.
A kind of 8. application of the niobate glass ceramics energy storage material as energy-storage capacitor material as claimed in claim 1.
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| CN108840570B (en) * | 2018-07-18 | 2021-04-27 | 陕西科技大学 | Containing NaNbO3Na of phase2O-K2O-Nb2O5-SiO2Low dielectric loss energy storage glass ceramic |
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| CN114685050A (en) * | 2022-04-28 | 2022-07-01 | 电子科技大学 | High-energy-storage-efficiency silicon niobate microcrystalline glass material and preparation method thereof |
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| "高储能密度铌酸盐铁电玻璃陶瓷制备及性能研究";张文俊;《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》;20130415(第4期);第B015-90页 * |
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