CN109608046A - A kind of close niobate energy storage glass ceramics of the glass structure of boracic and preparation method thereof - Google Patents
A kind of close niobate energy storage glass ceramics of the glass structure of boracic and preparation method thereof Download PDFInfo
- Publication number
- CN109608046A CN109608046A CN201910021958.1A CN201910021958A CN109608046A CN 109608046 A CN109608046 A CN 109608046A CN 201910021958 A CN201910021958 A CN 201910021958A CN 109608046 A CN109608046 A CN 109608046A
- Authority
- CN
- China
- Prior art keywords
- glass
- niobate
- energy storage
- ceramic material
- close
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 239000011521 glass Substances 0.000 title claims abstract description 61
- 238000004146 energy storage Methods 0.000 title claims abstract description 30
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 239000002241 glass-ceramic Substances 0.000 title claims description 16
- 239000006112 glass ceramic composition Substances 0.000 claims abstract description 28
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 22
- 239000013078 crystal Substances 0.000 claims abstract description 18
- ZKATWMILCYLAPD-UHFFFAOYSA-N niobium pentoxide Chemical compound O=[Nb](=O)O[Nb](=O)=O ZKATWMILCYLAPD-UHFFFAOYSA-N 0.000 claims abstract description 15
- BITYAPCSNKJESK-UHFFFAOYSA-N potassiosodium Chemical compound [Na].[K] BITYAPCSNKJESK-UHFFFAOYSA-N 0.000 claims abstract description 13
- 238000000137 annealing Methods 0.000 claims abstract description 12
- 239000000463 material Substances 0.000 claims abstract description 12
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 12
- 238000002425 crystallisation Methods 0.000 claims abstract description 11
- 230000008025 crystallization Effects 0.000 claims abstract description 11
- 238000002844 melting Methods 0.000 claims abstract description 11
- 230000008018 melting Effects 0.000 claims abstract description 11
- CDBYLPFSWZWCQE-UHFFFAOYSA-L sodium carbonate Substances [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims abstract description 11
- 229910000029 sodium carbonate Inorganic materials 0.000 claims abstract description 8
- 229910052681 coesite Inorganic materials 0.000 claims abstract description 6
- 229910052906 cristobalite Inorganic materials 0.000 claims abstract description 6
- 229910052682 stishovite Inorganic materials 0.000 claims abstract description 6
- 229910052905 tridymite Inorganic materials 0.000 claims abstract description 6
- 238000002156 mixing Methods 0.000 claims abstract 4
- 238000007669 thermal treatment Methods 0.000 claims abstract 2
- 239000000203 mixture Substances 0.000 claims description 10
- 238000004321 preservation Methods 0.000 claims description 10
- 239000011734 sodium Substances 0.000 claims description 7
- 238000010438 heat treatment Methods 0.000 claims description 6
- 238000000465 moulding Methods 0.000 claims description 6
- 239000010955 niobium Substances 0.000 claims description 6
- 229910052810 boron oxide Inorganic materials 0.000 claims description 3
- JKWMSGQKBLHBQQ-UHFFFAOYSA-N diboron trioxide Chemical compound O=BOB=O JKWMSGQKBLHBQQ-UHFFFAOYSA-N 0.000 claims description 3
- 238000007500 overflow downdraw method Methods 0.000 claims description 3
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 claims 6
- 229910000027 potassium carbonate Inorganic materials 0.000 claims 3
- UYLYBEXRJGPQSH-UHFFFAOYSA-N sodium;oxido(dioxo)niobium Chemical compound [Na+].[O-][Nb](=O)=O UYLYBEXRJGPQSH-UHFFFAOYSA-N 0.000 claims 2
- 230000015556 catabolic process Effects 0.000 abstract description 12
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 abstract description 2
- 229910052796 boron Inorganic materials 0.000 abstract description 2
- 238000001816 cooling Methods 0.000 abstract description 2
- 239000013081 microcrystal Substances 0.000 abstract 1
- 238000007493 shaping process Methods 0.000 abstract 1
- 238000000034 method Methods 0.000 description 10
- XZWYZXLIPXDOLR-UHFFFAOYSA-N metformin Chemical compound CN(C)C(=N)NC(N)=N XZWYZXLIPXDOLR-UHFFFAOYSA-N 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 2
- 229910003378 NaNbO3 Inorganic materials 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 229910010293 ceramic material Inorganic materials 0.000 description 2
- 229910052802 copper Inorganic materials 0.000 description 2
- 239000010949 copper Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 230000011218 segmentation Effects 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- XGCTUKUCGUNZDN-UHFFFAOYSA-N [B].O=O Chemical compound [B].O=O XGCTUKUCGUNZDN-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000006121 base glass Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 239000003989 dielectric material Substances 0.000 description 1
- 238000004455 differential thermal analysis Methods 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 239000002003 electrode paste Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 229910002112 ferroelectric ceramic material Inorganic materials 0.000 description 1
- 238000000265 homogenisation Methods 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 239000003607 modifier 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
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052573 porcelain Inorganic materials 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- MUPJWXCPTRQOKY-UHFFFAOYSA-N sodium;niobium(5+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Na+].[Nb+5] MUPJWXCPTRQOKY-UHFFFAOYSA-N 0.000 description 1
- 239000011232 storage material Substances 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
Classifications
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B19/00—Other methods of shaping glass
- C03B19/02—Other methods of shaping glass by casting molten glass, e.g. injection moulding
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B25/00—Annealing glass products
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Crystallography & Structural Chemistry (AREA)
- Ceramic Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Dispersion Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Inorganic Insulating Materials (AREA)
- Glass Compositions (AREA)
Abstract
The present invention relates to a kind of containing the close niobate energy storage glass ceramic material of glass structure and preparation method thereof for adding boron, which is as glass phase and crystal phase through made from mixing, melting, cooling and shaping, annealing and crystallization and thermal treatment；Wherein, crystal phase is the K for being 7:1:8 by molar ratio2CO3、Na2CO3And Nb2O5；Glass phase is to be by molar ratiox: (1-x) (x=1,0.85,0.7,0.54,0.37,0) SiO2、H2BO3；Crystal phase and glass phase molar ratio are 4:1.Potassium-sodium niobate-based energy storage microcrystal glass material dielectric loss produced by the present invention is low；The H2BO3 that the present invention is added keeps glass network more fine and close, to obtain higher breakdown strength.Form the NaNbO of high dielectric constant3Phase finally obtains high energy storage density glass ceramic material.
Description
Technical field
The present invention relates to glass ceramic material field and preparation method thereof, in particular to a kind of glass structure of boracic is close
Niobate energy storage glass ceramic material and preparation method thereof.
Background technique
In recent years, the development of pulse technique and higher application demand propose the electrical breakdown withstand and energy-storage property of material
More harsh requirement, therefore the ferroelectric glass-ceramic material as the big branch of energy storage dielectric material one is increasingly by scientific research
The favor of worker.Ferroelectric glass-ceramic depends on the high breakdown field strength of its inner glass phase and good Jie of ferroelectric crystalline phases
The mutually coordinated matching of both electrical properties finally makes material have biggish energy storage density.
According to linear dielectric energy storage density calculation formula, can obtain the energy storage density of energy-storage travelling wave tube with
The relative dielectric constant of its own is related with disruptive field intensity, and wherein breakdown strength influences the size of energy storage density bigger.In order to
Make glass ceramic material energy storage density with higher, the glass phase composition for influencing glass ceramic material breakdown strength should be weighed
Point research.Glass structure mainly generates body, Network modifier and network intermediate composition by network.Breakdown strength and glass structure
Tightness degree have an important relationship, the electrical breakdown of glass ceramics mainly causes the long-range of a large amount of carriers to be transported with when applying external electric field
It moves related.And if remaining glass phase has a close glass structure, carrier long range motion if, can become difficult, to mention
High breakdown strength.Silica is that most important network generates body, and stable structure is used by a large amount of glass ceramics systems.Silicon oxygen
Key (106 kcal/mol) is smaller compared to boron oxygen key (119 kcal/mol) bond energy, it is contemplated that obtain glass more closely
Network structure, it is a kind of method that the bigger boron oxide of bond energy, which is added,.
Summary of the invention
It is an object of the invention to overcome defect existing in the prior art, it is close to provide a kind of plus boron glass structure
Niobate energy storage glass ceramic material and preparation method thereof, the reaction of this method raw material high uniformity, utilization rate is high, and obtained
Glass ceramic material has high disruptive field intensity, high dielectric constant.
To achieve the above object, glass ceramics of the present invention the technical solution adopted is that:
Crystal phase is the K for being 7:1:8 by molar ratio2CO3、Na2CO3And Nb2O5；Glass phase is to be by molar ratiox: (1-x) SiO2、
H2BO3；Crystal phase and glass phase molar ratio are that 4:1 is formulated through made from mixed melting, molding, annealing and Crystallizing treatment.
The preparation method of glass ceramic material of the present invention the technical solution adopted is that, include the following steps:
1) K for being 7:1:8 according to 4 molar ratios2CO3、Na2CO3And Nb2O5；Glass phase is the SiO for being 1:3 by molar ratio2、H2BO3；
Crystal phase is 4:1 with glass phase molar ratio and mixes；
2) silica crucible heating is added in the mixture in step 1) until forming uniformly mixed melt；Melt is poured into mold
Molding, obtains glass sample, then make annealing treatment to glass sample；
3) will by annealing glass sample carry out Crystallizing treatment, Crystallizing treatment be 950 DEG C heat preservation, heat preservation total time be
2h obtains K2O-Na2O-Nb2O5-SiO2-B2O3System glass ceramic material.
Further, the heating temperature in step 2 is 1450~1500 DEG C.
Further, the annealing in step 2 is in 500~600 DEG C of 8~11h of heat preservation.
Further, the glass sample crystallization temperature in step 3) is 950 DEG C or so.
Further, the crystallization temperature in step 3) is that glass matrix sample is determining through DSC differential thermal analysis test.
Compared with prior art, the beneficial effects of the present invention are:
The potassium-sodium niobate glass ceramic material porosity produced by the present invention is minimum, needs network to be formed simultaneously as forming glass
Body, network outer body and network intermediate three parts.B2O3Body is generated when for octahedral structure with more as glass network
Close structure.Therefore the present invention rationally controls B2O3The ratio of content generates more close network structure, and dielectric constant can
Up to 180, disruptive field intensity can be down to 0.073, increase energy storage density up to 460kV/cm, dielectric loss, up to 1.64J/cm3。
In addition, due to being during the preparation process multiform into NaNbO3Mutually there is embodiment more to joined Na2CO3, therefore these embodiments
Also more crystal phase can be obtained.
Preparation method of the present invention only needs to carry out mixed melting, molding, annealing and Crystallizing treatment to each raw material, can be obtained
Potassium-sodium niobate glass ceramic material, the present invention use fusion method, and the reaction of raw material high uniformity, experimental implementation is simple, and molding side
Fado can effectively eliminate internal stress after annealing, while allow crystal phase to grow more using segmentation heat preservation when Crystallizing treatment
Completely, crystallization is more thorough, and internal grain is thinner, homogenization degree is higher and the higher glass pottery of energy storage density conducive to obtaining
Porcelain.
Detailed description of the invention
Fig. 1 is niobium prepared by the embodiment of the present invention 1, embodiment 2, embodiment 3, embodiment 4, embodiment 5 and embodiment 6
X-ray diffraction (XRD) map of sour potassium sodium base glass ceramic material；
Fig. 2 is the dielectric constant and dielectric loss figure of potassium-sodium niobate-based glass ceramic material prepared by the present invention.
Specific embodiment
The specific steps of the present invention are as follows:
1) K for being 7:1:8 according to molar ratio2CO3、Na2CO3And Nb2O5；Glass phase is to be by molar ratiox: (1-x) SiO2、
H2BO3；Crystal phase is 4:1 with glass phase molar ratio and mixes, and obtains mixture；
2) when silica crucible being heated to 1000 ~ 1200 DEG C from room temperature with furnace, it is initially added into mixture, then proceedes to be heated to
1450~1500 DEG C, and 50~60min is kept the temperature, make that mixture sufficiently melts and bubble-free finally obtains mixed melting material；Room temperature
It is lower to form mixed melting material on copper sheet mold, then annealing 8~11h in 500~600 DEG C at is put into furnace rapidly, to eliminate
Internal stress obtains glass sample；
Above-mentioned glass sample is kept the temperature at 950 DEG C, carries out segmentation Crystallizing treatment, the total time of Crystallizing treatment is 4h, then with furnace
It is cooled to room temperature, obtains K2O-Na2O-Nb2O5-SiO2-B2O3System glass ceramic material.
The present invention is described in further details below in conjunction with specific embodiment:
Embodiment 1:
The Crystallizing treatment of glass sample in the present embodiment: in 950 DEG C of heat preservation 4h.
The preparation method of the present embodiment glass ceramic material includes the following steps:
1) the present embodiment molar ratio is the K of 7:1:82CO3、Na2CO3And Nb2O5；Glass phase is the SiO for being 1:0 by molar ratio2、
H2BO3；Crystal phase is that 4:1 is mixed with glass phase molar ratio.
2) by silica crucible with stove heating from room temperature to 1100 DEG C when, be initially added into mixture, then proceed to be heated to
1500 DEG C, and keeping the temperature 60min at 1500 DEG C keeps mixture melting uniform, obtains mixed melting material；By mixed melting material in copper
It is formed on plate, then is put into furnace at 500 DEG C the 11h that anneals, the glass matrix after being annealed rapidly；
3) in 950 DEG C of heat preservation 4h, then furnace cooling obtains K to room temperature2O-Na2O-Nb2O5-SiO2-B2O3System glass ceramics
Material.
The potassium-sodium niobate glass ceramics that the present embodiment obtains is switched to the thin slice with a thickness of 0.1~0.2mm with cutting machine, it is thin
After piece is polished, cleaned, silver electrode paste is uniformly coated in thin slice tow sides, 20 minutes is kept the temperature in 600 DEG C, obtains glass to be measured
Glass ceramics sample.
Embodiment 2:
The glass phase of glass sample is the SiO for being 0.85:0.15 by molar ratio in the present embodiment2、H2BO3, and add at 1500 DEG C
Material melting and heat preservation 60min, other conditions are the same as embodiment 1.
Embodiment 3:
The formula of glass sample is the SiO of 0.7:0.3 in the present embodiment2、H2BO3, other conditions are the same as embodiment 1.
Embodiment 4:
The SiO that the formula of glass sample is 0.54: 0.46 in the present embodiment2、H2BO3, other conditions are the same as embodiment 1.
Embodiment 5:
The formula of glass sample is the SiO of 0.37:0.63 in the present embodiment2、H2BO3, other conditions are the same as embodiment 1.
Embodiment 6:
The formula of glass sample is the SiO of 0:1 in the present embodiment2、H2BO3, other conditions are the same as embodiment 1.
Fig. 1 be to the X-ray diffraction analysis of above six embodiments, illustrate different experiments formula to its crystallization degree with
The influence of object phase.It can be seen that 950oUnder the crystallization temperature of C, 6 kinds of embodiments have high crystallization degree, and crystal phase is mainly
NaNbO3。
It is potassium-sodium niobate glass ceramic material Jie that Fig. 2, which is to the table one of glass ceramic material made from above six embodiments,
Electric performance test is as a result, specific as follows:
The performance test data of the glass ceramics sample of one embodiment 1 to embodiment 4 of table preparation
| Embodiment | 1 | 2 | 3 | 4 | 5 | 6 |
| Dielectric constant | 150 | 75 | 100 | 73 | 70 | 72 |
| Disruptive field intensity (kV/cm) | 425 | 460 | 400 | 415 | 375 | 350 |
| Dielectric loss | 0.060 | 0.074 | 0.045 | 0.027 | 0.025 | 0.028 |
| Energy storage density (J/cm3) | 1.34 | 1.43 | 1.18 | 1.05 | 0.89 | 0.73 |
According to energy storage formula:, disruptive field intensity is to influence one of energy storage density factor the most significant, glass pottery
Ceramic material is because glass is there are dielectric constant reduction, and disruptive field intensity increases, and therefore, the present invention is by rationally controlling antiferroelectric niobic acid
The content of sodium crystal generates the ferroelectric glass-ceramic of high dielectric constant high breakdown field strength and low-dielectric loss.Also, using melting
Method prepares sample, and simple process, forming method is more, and it is the important method for preparing high energy storage density material that resistance to breakdown strength is high.
The high dielectric constant of invention preparation and the potassium-sodium niobate glass ceramics of high breakdown field strength are expected to substitute traditional ferroelectric ceramic material
As energy storage material excellent one of important candidate material simultaneous technically and economically.
The present invention prepares potassium-sodium niobate glass ceramic material using fusion method, the advantage is that preparation method simplicity, technique
Process is simple, and molding can be controlled arbitrarily as needed, with short production cycle, is particularly suitable for industrialized production.In the present invention at crystallization
Reason is to make crystal phase growth more complete using 4h soaking time, and crystallization is more thorough, and can also be obtained by later period test
It arrives, when the potassium-sodium niobate-based glass ceramics sample interior crystal content in higher crystallization peak isothermal holding, obtained is higher, energy storage is close
Du Genggao.Potassium-sodium niobate-based glass ceramic material prepared by the present invention is a kind of with high dielectric constant high breakdown field strength and low
The ferroelectric glass-ceramic of dielectric loss.
It the foregoing is merely one embodiment of the present invention, is not all of or unique embodiment, art technology
Any equivalent transformation that personnel take technical solution of the present invention by reading description of the invention, is power of the invention
Benefit requires to be covered.
Claims (7)
1. a kind of close niobate energy storage glass ceramics of the glass structure of boracic and preparation method thereof, it is characterised in that: packet
Including crystal phase and glass phase, the crystal phase includes potassium-sodium niobate and sodium niobate, and the glass phase is only silica or boron oxide, and
Silica and boron oxide mixing.
2. a kind of close niobate energy storage glass ceramic material of the glass structure of boracic according to claim 1,
Be characterized in that: the crystal phase is by Na2CO3、K2CO3、Nb2O57:1:8 in molar ratio, SiO2、H2BO3In molar ratiox: (1-x),x=1
~ 0, crystal phase and glass are comparably 4:1, and proportion mixing handles to obtain through fusion method.
3. a kind of close niobate energy storage glass ceramic material of the glass structure of boracic according to claim 1,
Be characterized in that: the content of the glass phase is 20% of integral molar quantity in glass ceramic material.
4. a kind of preparation method of the close niobate energy storage glass ceramic material of the glass structure of boracic, which is characterized in that
Include the following steps:
Na2CO3、K2CO3、Nb2O5、SiO2And H2BO3It mixing in molar ratio, heating melting mixture, internal stress is eliminated in annealing, into
Row crystallization and thermal treatment obtains the Na containing potassium-sodium niobate and sodium niobate phase2O-K2O-Nb2O5-SiO2-B2O3System stored energy glass ceramics
Material.
5. a kind of system of the close niobate energy storage glass ceramic material of the glass structure of boracic according to claim 4
Preparation Method, which is characterized in that specific steps include:
1) Na is weighed according to molar ratio set in claim 22CO3、K2CO3、Nb2O5、SiO2And H2BO3And it mixes；
2) by the mixture heating in step 1) until forming uniformly mixed melt；Melt is poured into mold molding, obtains glass
Glass sample, then glass sample is made annealing treatment；
3) will by annealing glass sample carry out Crystallizing treatment, Crystallizing treatment be 950 DEG C heat preservation, heat preservation total time be
4h obtains Na2O-K2O-Nb2O5-SiO2-B2O3System glass ceramic material.
6. a kind of system of the close niobate energy storage glass ceramic material of the glass structure of boracic according to claim 5
Preparation Method, it is characterised in that: the heating temperature in step 2 is 1450~1500 DEG C.
7. a kind of system of the close niobate energy storage glass ceramic material of the glass structure of boracic according to claim 5
Preparation Method, it is characterised in that: the condition of the annealing in step 2 is in 500~600 DEG C of 8~11h of heat preservation.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910021958.1A CN109608046B (en) | 2019-01-10 | 2019-01-10 | Boron-containing niobate-based energy storage glass ceramic with compact glass structure and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910021958.1A CN109608046B (en) | 2019-01-10 | 2019-01-10 | Boron-containing niobate-based energy storage glass ceramic with compact glass structure and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN109608046A true CN109608046A (en) | 2019-04-12 |
| CN109608046B CN109608046B (en) | 2021-06-01 |
Family
ID=66018485
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201910021958.1A Active CN109608046B (en) | 2019-01-10 | 2019-01-10 | Boron-containing niobate-based energy storage glass ceramic with compact glass structure and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN109608046B (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113233770A (en) * | 2021-01-26 | 2021-08-10 | 陕西科技大学 | Containing Na0.9K0.1NbO3Crystalline phase high dielectric borate glass ceramics, preparation and application thereof |
| CN113461335A (en) * | 2021-01-26 | 2021-10-01 | 陕西科技大学 | Borate glass ceramic with low dielectric loss and high energy storage density and compact structure, and preparation method and application 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 |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20070203011A1 (en) * | 2006-02-01 | 2007-08-30 | Gudgel Katherine A | Translucent piezoelectric glass ceramic |
| CN102046551A (en) * | 2008-05-27 | 2011-05-04 | 默克专利股份有限公司 | Glass-ceramic discs for use in pigments |
| CN105254180A (en) * | 2015-09-22 | 2016-01-20 | 陕西科技大学 | K2O-Na2O-Nb2O5-SiO2-B2O3 system glass ceramic material used for energy storage, and preparation method thereof |
| CN108794003A (en) * | 2018-07-17 | 2018-11-13 | 华南理工大学 | A kind of biological glass ceramic and preparation method thereof of doping potassium-sodium niobate |
| CN108840570A (en) * | 2018-07-18 | 2018-11-20 | 陕西科技大学 | Containing NaNbO3The Na of phase2O-K2O-Nb2O5-SiO2Low-dielectric loss energy storage glass ceramics |
-
2019
- 2019-01-10 CN CN201910021958.1A patent/CN109608046B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20070203011A1 (en) * | 2006-02-01 | 2007-08-30 | Gudgel Katherine A | Translucent piezoelectric glass ceramic |
| CN102046551A (en) * | 2008-05-27 | 2011-05-04 | 默克专利股份有限公司 | Glass-ceramic discs for use in pigments |
| CN105254180A (en) * | 2015-09-22 | 2016-01-20 | 陕西科技大学 | K2O-Na2O-Nb2O5-SiO2-B2O3 system glass ceramic material used for energy storage, and preparation method thereof |
| CN108794003A (en) * | 2018-07-17 | 2018-11-13 | 华南理工大学 | A kind of biological glass ceramic and preparation method thereof of doping potassium-sodium niobate |
| CN108840570A (en) * | 2018-07-18 | 2018-11-20 | 陕西科技大学 | Containing NaNbO3The Na of phase2O-K2O-Nb2O5-SiO2Low-dielectric loss energy storage glass ceramics |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113233770A (en) * | 2021-01-26 | 2021-08-10 | 陕西科技大学 | Containing Na0.9K0.1NbO3Crystalline phase high dielectric borate glass ceramics, preparation and application thereof |
| CN113461335A (en) * | 2021-01-26 | 2021-10-01 | 陕西科技大学 | Borate glass ceramic with low dielectric loss and high energy storage density and compact structure, and preparation method and application 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 |
Also Published As
| Publication number | Publication date |
|---|---|
| CN109608046B (en) | 2021-06-01 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN108840570A (en) | Containing NaNbO3The Na of phase2O-K2O-Nb2O5-SiO2Low-dielectric loss energy storage glass ceramics | |
| CN105254180B (en) | A kind of K applied to energy storage2O‑Na2O‑Nb2O5‑SiO2‑B2O3System glass ceramic material and preparation method thereof | |
| CN109626828A (en) | Containing NaNbO3The Na of phase2O-Nb2O5-SiO2High dielectric constant energy storage glass ceramics and preparation method | |
| CN109608046A (en) | A kind of close niobate energy storage glass ceramics of the glass structure of boracic and preparation method thereof | |
| CN103880288B (en) | A kind of strontium barium niobate glass ceramic material of high-k high breakdown field strength and preparation method thereof | |
| CN106865989B (en) | A kind of the KNN base energy storage microcrystal glass material and preparation method of ultralow dielectric loss | |
| CN105418068B (en) | A kind of niobate glass ceramics energy storage material and its preparation method and application | |
| CN112225460B (en) | Alkali metal oxide substituted niobate glass ceramic with low dielectric loss and high energy storage density, preparation method and application | |
| CN110668680A (en) | Production process of high borosilicate glass tube | |
| CN114031297B (en) | Cordierite-based porous glass ceramic and preparation method thereof | |
| CN105967526A (en) | Formula of glass-ceramic plate and preparation technology | |
| CN114933418A (en) | Low dielectric constant and low dielectric loss glass fiber composition, glass fiber and application thereof | |
| CN111777333B (en) | Zirconium titanate/sapphirine complex phase microcrystalline glass material and preparation method thereof | |
| CN110372204B (en) | High-temperature and high-pressure resistant window glass and preparation method and application thereof | |
| CN112159110B (en) | Energy storage glass ceramic capable of adjusting ferroelectricity by controlling crystallization power, preparation method and application | |
| CN113233770B (en) | Containing Na 0.9 K 0.1 NbO 3 Crystalline phase high dielectric borate glass-ceramics, their preparation and use | |
| CN116161869A (en) | Preparation method of microwave dielectric material | |
| CN101412586A (en) | Infrared transmitting multi-component oxyhalide tellurite nucleated glass and preparation thereof | |
| CN107417097B (en) | A kind of preparation method of high-fracture toughness chalcogenide glass | |
| CN109704584B (en) | SrNb-containing steel6O16Phase titanate and niobate compounded glass ceramic with low dielectric loss and preparation method thereof | |
| CN110803868A (en) | Diopside reinforced mica-based machinable glass ceramic and preparation method thereof | |
| CN109942195B (en) | Glass ceramic with high dielectric constant and low dielectric loss and preparation method thereof | |
| CN113233772B (en) | Glass ceramic for realizing high dielectric constant and high breakdown performance by regulating and controlling glass network structure and preparation method thereof | |
| CN113461335B (en) | Borate glass ceramic with low dielectric loss and high energy storage density and compact structure, and preparation method and application thereof | |
| CN113755045B (en) | Infrared radiation coating and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20240222 Address after: 518000 1002, Building A, Zhiyun Industrial Park, No. 13, Huaxing Road, Henglang Community, Longhua District, Shenzhen, Guangdong Province Patentee after: Shenzhen Wanzhida Technology Co.,Ltd. Country or region after: China Address before: 710021 Shaanxi province Xi'an Weiyang university campus of Shaanxi University of Science and Technology Patentee before: SHAANXI University OF SCIENCE & TECHNOLOGY Country or region before: China |
|
| TR01 | Transfer of patent right |