CN105254180B - A kind of K applied to energy storage2O‑Na2O‑Nb2O5‑SiO2‑B2O3System glass ceramic material and preparation method thereof - Google Patents

A kind of K applied to energy storage2O‑Na2O‑Nb2O5‑SiO2‑B2O3System glass ceramic material and preparation method thereof Download PDF

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CN105254180B
CN105254180B CN201510607884.1A CN201510607884A CN105254180B CN 105254180 B CN105254180 B CN 105254180B CN 201510607884 A CN201510607884 A CN 201510607884A CN 105254180 B CN105254180 B CN 105254180B
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蒲永平
郑晗煜
柳晓燕
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Shaanxi University of Science and Technology
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Abstract

The present invention relates to a kind of K applied to energy storage2O‑Na2O‑Nb2O5‑SiO2‑B2O3System glass ceramic material and preparation method thereof, be by mol ratio be 15：15：30：4：2：The K of (2~5)2CO3、Na2CO3、Nb2O5、SiO2、H3BO3And BaF2Made from blended melting, shaping, annealing and Crystallizing treatment.Possesses alkali metal oxide in raw material of the present invention, exist in glass system as network outer body, destroy glass network structure, therefore glass formula is simplified, not only reducing cost is also fundamentally reducing the species of precipitation dephasign, using fusion method, raw material high uniformity reacts, experimental implementation is simple, internal stress can be effectively eliminated after annealing, while makes crystalline phase growth more complete using segmentation insulation during Crystallizing treatment, crystallization is more thorough, and internal grain is thinner, the glass ceramics that homogenization degree is higher and energy storage density is higher beneficial to obtaining.

Description

A kind of K applied to energy storage2O-Na2O-Nb2O5-SiO2-B2O3System glass ceramics material Material and preparation method thereof
Technical field
The present invention relates to a kind of glass ceramic material and preparation method thereof, more particularly to a kind of K applied to energy storage2O- Na2O-Nb2O5-SiO2-B2O3System glass ceramic material and preparation method thereof.
Background technology
With the development of Pulse Power Techniques, people propose higher requirement for wherein energy-storage travelling wave tube energy storage density, Compared with other devices, the advantages that capacitor has that discharge power is big, and utilization ratio is high, and the energy storage density rising space is big, just by Gradually turn into the energy-storage travelling wave tube in pulse-power apparatus and be widely used.
According to linear dielectric energy storage density calculation formulaCan obtain the energy storage density of energy-storage travelling wave tube with The relative dielectric constant of its own is relevant with disruptive field intensity.Ferroelectric has high dielectric constant, and glass material is with very high Disruptive field intensity, therefore as the candidate of energy storage material be one of ideal chose using ferroelectric glass-ceramic.
Niobates glass ceramics is the hot research of energy storage glass ceramics at present, but surrounds strontium barium niobate glass powder mostly Or ceramics expansion research, but it is raw materials used complex in the preparation process of strontium barium niobate glass ceramics, raw material profit also be present With it is not high the defects of；And studied for potassium-sodium niobate glass ceramic material very few.Potassium-sodium niobate (i.e. (K, Na) NbO3) belong to allusion quotation Type perovskite crystal structure.The perovskite crystal structure of ABO3 types is that a kind of stable and widely used crystal formation is typical ferroelectricity Body, not only there is more research in terms of ferroelectricity, piezoelectricity, pyroelectricity, also there is more novel research in terms of photocatalysis, energy storage Pay close attention to temperature.With regard to Ca-Ti ore type (K, Na) NbO3For material, just there is its hotter research with opening in terms of piezoelectricity, PTC originally Hair prospect, a kind of potassium-sodium niobate glass ceramics with high breakdown field strength and high-k can not be also prepared at present.
The content of the invention
It is an object of the invention to overcome defect present in prior art, there is provided a kind of K applied to energy storage2O- Na2O-Nb2O5-SiO2-B2O3System glass ceramic material and preparation method thereof, the reaction of this method raw material high uniformity, utilization rate Height, and obtained glass ceramic material, there is high disruptive field intensity, high dielectric constant.
To achieve the above object, the technical scheme of glass ceramics use of the present invention is：
Be by mol ratio be 15：15：30：4：2：The K of (2~5)2CO3、Na2CO3、Nb2O5、SiO2、H3BO3And BaF2Through Made from mixed melting, shaping, annealing and Crystallizing treatment.
The technical scheme that the preparation method of glass ceramic material of the present invention uses is to comprise the following steps：
1) according to 15K2O-15Na2O-30Nb2O5-4SiO2-2B2O3- (2~5) BaF2Mol ratio weigh K2CO3, Na2CO3, Nb2O5, SiO2, H3BO3And BaF2And mix；
2) by the mixture heating in step 1) until forming well mixed melt；Melt is poured into mould molding, obtained Made annealing treatment to glass sample, then to glass sample；
3) glass sample by annealing is subjected to Crystallizing treatment, Crystallizing treatment be successively at 705~720 DEG C and 900~920 DEG C of insulations, insulation total time is 5h, obtains K2O-Na2O-Nb2O5-SiO2-B2O3System glass ceramic material.
Further, the heating-up temperature in step 2) is 1300~1400 DEG C.
Further, the annealing in step 2) is to be incubated 4~7h at 600~800 DEG C.
Further, the glass sample in step 3) contains two recrystallization temperatures, respectively 708 DEG C with 905 DEG C.
Further, the recrystallization temperature in step 3) is that glass sample tests determination through DSC differential thermal analyses.
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, simultaneously as forming glass needs network Body, network outer body and network intermediate three parts are formed, and in the raw material of target product potassium-sodium niobate to be prepared in itself Just possesses alkali metal oxide K2O-Na2O, exist in glass system as network outer body, destroy glass network structure, therefore Glass formula is simplified, not only reducing cost is also fundamentally reducing the species of precipitation dephasign.The present invention also rationally control The ratio of ferroelectricity potassium-sodium niobate crystal and glass content, generate the ferroelectricity glass of high-k high breakdown field strength and low-dielectric loss Glass ceramics, for dielectric constant up to 258, disruptive field intensity can be down to 0.004 up to 516kV/cm, dielectric loss, make energy storage density high, Up to 1.8J/cm3.Further, since BaF is added in preparation process2As nucleator, BaF2Glass can be promoted to be nucleated, be fluorinated The microcrystal of thing is exactly the nuclearing centre of glass；Meanwhile BaF2Nucleus form temperature, less than crystal growth temperature, therefore, warp BaF2Coring, the glassy grain of crystallization are tiny, and promote the precipitation of potassium niobate nano-crystal body.Moreover, present invention selection SiO2-B2O3 System is as glass basis, B2O3It is by H3BO3Addition introduce, be mostly SiO with current glass basis2Melting temperature (up to 1500 DEG C) are compared, H3BO3Melting temperature can be greatly lowered, make the melting of raw material be more easy to occur, be more easy to uniformly mixed Close.
Preparation method of the present invention only needs to carry out mixed melting, shaping, annealing and Crystallizing treatment to each raw material, you can obtains 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 shaping side Fado, internal stress can be effectively eliminated after annealing, while crystalline phase growth is allowed more using segmentation insulation during Crystallizing treatment Completely, crystallization is more thorough, and is made pottery beneficial to the glass that internal grain is thinner, homogenization degree is higher and energy storage density is higher is obtained Porcelain.
Brief description of the drawings
Fig. 1 is differential scanning calorimetry (DSC) curve of potassium-sodium niobate glass material of the present invention；
Fig. 2 is that the X- of potassium-sodium niobate glass ceramic material prepared by the embodiment of the present invention 1, embodiment 2 and embodiment 3 is penetrated Line diffraction (XRD) collection of illustrative plates；
Fig. 3 (a) is the SEM photograph of potassium-sodium niobate glass ceramic material prepared by the embodiment of the present invention 1, and Fig. 3 (b) is to implement The SEM photograph of potassium-sodium niobate glass ceramic material prepared by example 2, Fig. 3 (c) are potassium-sodium niobate glass prepared by the embodiment of the present invention 3 The SEM photograph of glass ceramic material.
Embodiment
The present invention's comprises the following steps that：
1) it is 15 by the amount ratio of material：15：30：4：2：(2~5), take K respectively2CO3、Na2CO3、Nb2O5、SiO2、 H3BO3 And BaF2And mixed, obtain mixture；
2) by silica crucible with stove from room temperature be heated to 900~1200 DEG C when, be initially added into mixture, then proceed to heat To 1300~1400 DEG C, and 20~40min is incubated, makes that mixture fully melts and bubble-free finally obtains mixed melting material；Room Mixed melting material is molded on copper coin mould under temperature, then is put into stove 4~7h of annealing at 600~800 DEG C rapidly, to eliminate Internal stress, obtain glass sample；
3) test of DSC differential scanning calorimetries is done by taking a small amount of glass sample produced by the present invention to smash, obtained It is respectively 708 DEG C and 905 DEG C to the first recrystallization temperature of glass sample and the second recrystallization temperature, referring to Fig. 1, illustrates to separate out Potassium-sodium niobate crystal under two exothermic peaks, it is necessary to all carry out insulation heat treatment.
Above-mentioned glass sample is continued, in 900~920 DEG C of insulations, be segmented at crystallization after 705~720 DEG C of insulations Reason, the total time of Crystallizing treatment is 5h, and then furnace cooling 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：1h is incubated in 708 DEG C and is incubated 4h in 905 DEG C.
The preparation method of the present embodiment glass ceramic material comprises the following steps：
1) the present embodiment potassium-sodium niobate glass ceramic material be by material amount ratio be 15：15：30：4：2：3, take K2CO3, Na2CO3, Nb2O5, SiO2, H3BO3And BaF2Mixing.
2) by silica crucible with stove heat from room temperature to 1100 DEG C when, be initially added into mixture, then proceed to be heated to 1350 DEG C, and being incubated 30min at 1350 DEG C makes mixture melting uniform, obtains mixed melting material；By mixed melting material in copper It is molded on plate, then is put into stove the 7h that annealed at 600 DEG C rapidly, glass after being annealed；
3) continue to be incubated 4h and then furnace cooling to room temperature at 905 DEG C after being incubated 1h at 708 DEG C, obtain K2O-Na2O- Nb2O5-SiO2-B2O3System glass ceramic material.
The potassium-sodium niobate glass ceramics that the present embodiment obtains is switched to the thin slice that thickness is 0.1~0.2mm with cutting machine, it is thin Piece uniformly coats silver electrode paste after polishing, cleaning, in thin slice tow sides, is incubated 20 minutes in 600 DEG C, obtains glass to be measured Glass ceramics sample.
Embodiment 2：
The Crystallizing treatment of glass sample in the present embodiment：4h is incubated in 708 DEG C and is incubated 1h in 905 DEG C, other conditions are same Embodiment one.
Embodiment 3：
The Crystallizing treatment of glass sample in the present embodiment：2h is incubated in 708 DEG C and is incubated 3h in 905 DEG C, other conditions are same Embodiment one.
Fig. 2 be to the X-ray diffraction analysis of three above embodiment, illustrate different Crystallizing treatments to its crystallization degree with The influence of crystallization purity.It can be seen that under the Crystallizing treatment of embodiment 1, due to the soaking time length under low temperature recrystallization temperature High temperature recrystallization temperature soaking time is short, thus is unfavorable for growing up for crystal grain, so glass mutually still largely exist, so as to miscellaneous peak compared with It is more.In example 2, holding time under high temperature, although being advantageous to the generation of principal crystalline phase, also help simultaneously other The growth of two-phase.Embodiment 3 obtains relatively optimal Crystallizing treatment and prepared, and the peak of principal crystalline phase is sharp, and dephasign is relatively fewer.
Fig. 3 (a) to Fig. 3 (c) is the SEM photograph to glass ceramic material made from three above embodiment, embodiment 3 In generate potassium-sodium niobate crystal, and crystal grain quantity is big, is evenly distributed.And with reference to Fig. 2, the crystalline phase for further proving generation is Potassium-sodium niobate.From Fig. 3 (a) to the scanned photograph of embodiment 1 this it appears that crystallization is imperfect, because the sample is analysed in height The short period is incubated at brilliant temperature, and is found out from Fig. 3 (b), embodiment 2 is most complete due to the longer crystallization of soaking time at high temperature But stomata produces therewith.From Fig. 3 (c) as can be seen that still existing around the potassium-sodium niobate crystal grain generated in embodiment 3 small Particle, these molecules are glass phase, and glass is mutually filled uniformly between crystalline phase, shown inside potassium-sodium niobate glass ceramics Glass is uniformly distributed with ferroelectricity potassium-sodium niobate crystal, so as to effectively reduce the porosity and then reduce loss.Larger potassium-sodium niobate Crystal grain shows ferroelectric crystalline phases well-grown in glass ceramics, therefore has higher dielectric constant；Glass phase is (in Fig. 2 XRD The miscellaneous peak of diffraction maximum is provable) presence ensure that it has higher disruptive field intensity again.
Table one is potassium-sodium niobate glass ceramic material dielectric prepared by the embodiment of the present invention 1, embodiment 2 and embodiment 3 The performance test results, it is specific as follows：
The dielectric properties test data (1kHz) for the glass ceramics sample that the embodiment 1 of table one is prepared to embodiment 3
According to energy storage formula：Disruptive field intensity is to influence one of energy storage density factor the most significant, glass Glass ceramic material is because the presence dielectric constant of glass reduces, and disruptive field intensity increase, therefore, the present invention is by rationally controlling ferroelectricity niobium The ratio of sour potassium sodium crystal and glass content, generate the ferroelectric glass pottery of high-k high breakdown field strength and low-dielectric loss Porcelain.Also, sample is prepared using fusion method, simple process, forming method is more, and resistance to breakdown strength is high, is that to prepare high energy storage close Spend the important method of material.The potassium-sodium niobate glass ceramics of high-k high breakdown field strength prepared by the invention is expected to substitute and passed Ferroelectric ceramic material of uniting turns into one of energy storage material excellent 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 Flow is simple, and shaping can be controlled arbitrarily as needed, with short production cycle, be particularly suitable for industrialized production.In the present invention at crystallization Reason is that crystallization is more thorough in order to make crystalline phase growth more complete using segmentation insulation, and can also be obtained by later stage test, When two recrystallization temperatures simultaneously isothermal holding, obtained potassium-sodium niobate glass ceramics sample interior crystal grain is thinner, homogenize journey Du Genggao, energy storage density are higher.Potassium-sodium niobate glass ceramic material prepared by the present invention is that one kind has high-k high strike Wear the ferroelectric glass-ceramic of field strength and low dielectric loss.
Embodiment 4
The preparation method of the present embodiment glass ceramic material comprises the following steps：
1) the present embodiment potassium-sodium niobate glass ceramic material be by material amount ratio be 15：15：30：4：2：2, take K2CO3, Na2CO3, Nb2O5, SiO2, H3BO3And BaF2Mixing.
2) by silica crucible from room temperature with stove heat to 900 DEG C when, be initially added into mixture, then proceed to be heated to 1400 DEG C, and being incubated 20min at 1400 DEG C makes mixture melting uniform, obtains mixed melting material；By mixed melting material on copper coin Shaping, then the 4h of in 700 DEG C at annealing is put into stove rapidly, glass after being annealed；
3) continue to be incubated 2h at 910 DEG C after being incubated 3h at 710 DEG C and then cool to room temperature with the furnace, obtain K2O-Na2O- Nb2O5-SiO2-B2O3System glass ceramic material.
Embodiment 5
The preparation method of the present embodiment glass ceramic material comprises the following steps：
1) the present embodiment potassium-sodium niobate glass ceramic material be by material amount ratio be 15：15：30：4：2：4, take K2CO3, Na2CO3, Nb2O5, SiO2, H3BO3And BaF2Mixing.
2) by silica crucible from room temperature with stove heat to 1200 DEG C when, be initially added into mixture, then proceed to be heated to 1300 DEG C, and being incubated 40min at 1300 DEG C makes mixture melting uniform, obtains mixed melting material；By mixed melting material in copper It is molded on plate, then is put into stove the 5h that annealed at 800 DEG C rapidly, glass after being annealed；
3) continue to be incubated 2.5h at 900 DEG C after being incubated 2.5h at 720 DEG C and then cool to room temperature with the furnace, obtain K2O- Na2O-Nb2O5-SiO2-B2O3System glass ceramic material.
Embodiment 6
The preparation method of the present embodiment glass ceramic material comprises the following steps：
1) the present embodiment potassium-sodium niobate glass ceramic material be by material amount ratio be 15：15：30：4：2：5, take K2CO3, Na2CO3, Nb2O5, SiO2, H3BO3And BaF2Mixing.
2) by silica crucible from room temperature with stove heat to 1000 DEG C when, be initially added into mixture, then proceed to be heated to 1380 DEG C, and being incubated 25min at 1380 DEG C makes mixture melting uniform, obtains mixed melting material；By mixed melting material in copper It is molded on plate, then is put into stove the 6h that annealed at 650 DEG C rapidly, glass after being annealed；
3) continue to be incubated 1.5h at 920 DEG C after being incubated 3.5h at 705 DEG C and then cool to room temperature with the furnace, obtain K2O- Na2O-Nb2O5-SiO2-B2O3System glass ceramic material.
One embodiment of the present invention is the foregoing is only, is not all of or unique embodiment, this area leads to skill Art personnel are the present invention's by reading description of the invention any equivalent conversion for taking technical solution of the present invention Claim is covered.

Claims (5)

  1. A kind of 1. K applied to energy storage2O-Na2O-Nb2O5-SiO2-B2O3The preparation method of system glass ceramic material, its feature It is, comprises the following steps：
    1) according to 15K2O-15Na2O-30Nb2O5-4SiO2-2B2O3- (2~5) BaF2Mol ratio weigh K2CO3, Na2CO3, Nb2O5, SiO2, H3BO3And BaF2And mix；
    2) by the mixture heating in step 1) until forming well mixed melt；Melt is poured into mould molding, obtains glass Glass sample, then glass sample is made annealing treatment；
    3) glass sample by annealing is subjected to Crystallizing treatment, Crystallizing treatment be successively 705~720 DEG C and 900~ 920 DEG C of insulations, insulation total time is 5h, obtains K2O-Na2O-Nb2O5-SiO2-B2O3System glass ceramic material；
    Annealing in step 2) is to be incubated 4~7h at 600~800 DEG C.
  2. A kind of 2. K applied to energy storage according to claim 12O-Na2O-Nb2O5-SiO2-B2O3System glass ceramics material The preparation method of material, it is characterised in that：Heating-up temperature in step 2) is 1300~1400 DEG C.
  3. A kind of 3. K applied to energy storage according to claim 12O-Na2O-Nb2O5-SiO2-B2O3System glass ceramics material The preparation method of material, it is characterised in that：Glass sample in step 3) contains two recrystallization temperatures, respectively 708 DEG C and 905 ℃。
  4. A kind of 4. K applied to energy storage according to claim 12O-Na2O-Nb2O5-SiO2-B2O3System glass ceramics material The preparation method of material, it is characterised in that：Recrystallization temperature in step 3) is that glass sample tests determination through DSC differential thermal analyses.
  5. 5. utilize the obtained K for being applied to energy storage of preparation method described in claim 12O-Na2O-Nb2O5-SiO2-B2O3System glass Glass ceramic material, it is characterised in that：Be by mol ratio be 15：15：30：4：2：The K of (2~5)2CO3、Na2CO3、Nb2O5、SiO2、 H3BO3And BaF2Made from blended melting, shaping, annealing and Crystallizing treatment.
CN201510607884.1A 2015-09-22 2015-09-22 A kind of K applied to energy storage2O‑Na2O‑Nb2O5‑SiO2‑B2O3System glass ceramic material and preparation method thereof Active CN105254180B (en)

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CN105753472B (en) * 2016-01-26 2018-06-26 同济大学 The niobic acid barium potassium base glass ceramics energy storage material of high energy storage density and preparation and application
CN106865989B (en) * 2017-01-06 2019-10-01 陕西科技大学 A kind of the KNN base energy storage microcrystal glass material and preparation method of ultralow dielectric loss
CN108147812A (en) * 2018-01-15 2018-06-12 陕西科技大学 A kind of BT-KBT-NN based high energy storage densities ceramics and preparation method thereof
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
CN109608046B (en) * 2019-01-10 2021-06-01 陕西科技大学 Boron-containing niobate-based energy storage glass ceramic with compact glass structure and preparation method thereof
CN113461335B (en) * 2021-01-26 2023-01-31 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
CN113233770B (en) * 2021-01-26 2023-01-31 陕西科技大学 Containing Na 0.9 K 0.1 NbO 3 Crystalline phase high dielectric borate glass-ceramics, their preparation and use
CN114890674B (en) * 2022-06-02 2023-12-29 陕西科技大学 Needle-shaped high-dielectric energy storage microcrystalline glass and preparation method thereof

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CN102260044B (en) * 2011-04-30 2013-07-24 桂林电子科技大学 Energy storage niobate microcrystalline glass dielectric material and preparation method thereof
CN103880288B (en) * 2014-01-27 2016-08-17 陕西科技大学 A kind of strontium barium niobate glass ceramic material of high-k high breakdown field strength and preparation method thereof
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