CN101531461A - Dielectric material of glass-ceramics with high energy storage density and preparation method - Google Patents
Dielectric material of glass-ceramics with high energy storage density and preparation method Download PDFInfo
- Publication number
- CN101531461A CN101531461A CN200910082177A CN200910082177A CN101531461A CN 101531461 A CN101531461 A CN 101531461A CN 200910082177 A CN200910082177 A CN 200910082177A CN 200910082177 A CN200910082177 A CN 200910082177A CN 101531461 A CN101531461 A CN 101531461A
- Authority
- CN
- China
- Prior art keywords
- glass
- ceramics
- mole number
- energy storage
- storage density
- 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
Images
Abstract
The invention discloses a dielectric material of glass-ceramics with high energy storage density and a preparation method, belonging to the technical field of electronic materials and devices. The dielectric material mainly comprises BaO, SrO, TiO2, SiO2 and Al2O3, which is doped with AlF3 and MnO2; the mol numbers of the AlF3 and the MnO2 respectively account for 2-8% and 0.1-1% of the total mol number of the ingredients. The preparation method comprises the following steps: calcining and melting the raw materials after ball milling to prepare glass slices; carrying out controlled crystallization on the glass slices and obtaining ferroelectric glass-ceramics dielectric coated silver paste; sintering and solidifying the silver paste to form a metal silver electrode to prepare the dielectric material of glass-ceramics with high energy storage density. The ferroelectric glass-ceramics dielectric material prepared by the invention has compact structure and fine crystal grain and can be used for manufacturing various high-voltage capacitors with high energy storage density.
Description
Technical field
The invention belongs to electronic material and device technology field, particularly a kind of dielectric material of glass-ceramics with high energy storage density and preparation method thereof.
Background technology
The high energy storage density electrical condenser is widely used at modern industry and national defence field, as pulse power system, oil gas deep prospecting, hybrid vehicle, comprehensive full electric propulsion naval vessels etc., is playing the part of more and more important role in electric power, electronic system.The development of new technology is had higher requirement to its energy storage density and voltage-resistent characteristic.The core that improves the electrical condenser energy storage characteristic then is to develop the dielectric substance with high energy storage density.
At present, the dielectric substance of high energy storage density electrical condenser mainly contains three classes, and the first kind is barium titanate, the titanium dioxide dielectric ceramic of high-k; Second class is the organic film of high breaking down field strength, as polypropylene film, mylar (Mylar film), polyvinylidene fluoride film (pvdf membrane) etc.; The 3rd class is the composite dielectrics of pottery and polymkeric substance.Though the specific inductivity of barium titanate ferroelectric ceramics is high, be subjected to defective in the material (crystal boundary, hole etc.) and Temperature Influence very big, its breaking down field strength is lower in addition, and making with barium titanate ceramics is that the energy storage density of electrical condenser of dielectric medium preparation is lower usually.Polymeric film has breaking down field strength height, advantage such as shock-resistant, but its specific inductivity is low, is that the energy storage density of electrical condenser of dielectric materials preparation is common also lower with mylar (Mylar film).Pottery is common also not too high with the energy storage density of polymkeric substance composite dielectrics.Devitrified glass (is called glass-ceramic again, glass-ceramics) dielectric medium is a kind of novel high energy storage density material, be to adopt the preparation method of glass that oxide compound is melt into vitreous state, and then thermal treatment makes devitrification of glass at a certain temperature, and then obtain the complex body of glass and pottery.By the synergy of ferroelectric phase and glassy phase, ferroelectric glass-ceramic can obtain very high energy storage density.Yet, often be prone to dendritic brilliant tissue in the ferroelectric glass-ceramic material microstructure, and dielectric loss is higher relatively, very unfavorable to the anti-electrical property of devitrified glass.
Summary of the invention
The purpose of this invention is to provide a kind of dielectric material of glass-ceramics with high energy storage density and preparation method thereof.
A kind of dielectric material of glass-ceramics with high energy storage density is characterized in that, the main ingredient of dielectric material of glass-ceramics is BaO, SrO, TiO
2, SiO
2And Al
2O
3, it forms doped with Al F
3And MnO
2, the main ingredient mol ratio is BaO:SrO:TiO
2: SiO
2: Al
2O
3=(0.28～0.35): (0.05～0.10): (0.27～0.35): (0.20～0.25): (0.04～0.11), doped with Al F
3Mole number account for 2～8% of component total mole number, doped with Mn O
2Mole number account for 0.1～1% of component total mole number.
A kind of preparation method of dielectric material of glass-ceramics with high energy storage density is characterized in that, this method steps is as follows,
(1) with purity greater than 99% BaCO
3, SrCO
3, TiO
2, SiO
2, Al
2O
3, AlF
3And MnO
2Be starting raw material, according to main ingredient BaO, SrO, TiO
2, SiO
2And Al
2O
3Mol ratio is BaO:SrO:TiO
2: SiO
2: Al
2O
3=(0.28～0.35): (0.05～0.10): (0.27～0.35): (0.20～0.25): (0.04～0.11), doped with Al F
3Mole number account for 2～8% of component total mole number, doped with Mn O
2Mole number account for 0.1～1% of component total mole number, prepare burden, then these raw materials are added ball-milling medium and ground 4～6 hours in planetary ball mills, the calcining of oven dry back, calcining temperature is 1400～1650 ℃, is incubated 2～6 hours high-temperature fusion;
(2) high-temperature fusant with step (1) is poured in the metal die, and obtaining thickness through cutting then is the glass flake of 0.2～1mm; Perhaps, the high-temperature fusant of step (1) is prepared the glass flake that thickness is 0.1～1mm through cold-rolling process; Perhaps, the high-temperature fusant of step (1) is carried out quick shrend, the glass particle that shrend is obtained adds ball-milling medium grinding 10～20 hours in planetary ball mill again, and air atmosphere is oven dry down, obtains the thin slice that thickness is 0.5～2mm through compression moulding then;
(3) glass flake with step (2) preparation carries out controlled crystallization, this crystallization process was divided into for two steps, at first impelled the principal crystalline phase nucleation in 1～2 hour 750～850 ℃ of temperature insulations, principal crystalline phase is a strontium-barium titanate, be incubated 1～3 hour then under 800～1100 ℃ of temperature and make nuclei growth, obtaining with the strontium-barium titanate with perovskite structure is the ferroelectric glass-ceramic dielectric of principal crystalline phase;
(4) the resulting glass-ceramic dielectric thin slice of step (3) is applied adhesive property and the good silver paste of conductivity through silk-screen printing technique, solidify to form the argent electrode at 500～550 ℃ of sintering temperatures, make the glass-ceramics with high energy storage density dielectric medium.
Described ball-milling medium is deionized water or dehydrated alcohol.
Described metal die material is steel or copper, and mould is circle or rectangle.
Beneficial effect of the present invention is: the present invention utilizes fluorochemical to reduce glass viscosity and manganese significantly and easily appraises at the current rate and stop 4 valency titaniums to be reduced into the characteristic of 3 valency titaniums, is doping agent with an amount of aluminum fluoride and Manganse Dioxide respectively, and preparation is based on BaO-SrO-TiO
2-SiO
2-Al
2O
3The microcrystal glass material of system.By being added in the heat of crystallization treating processes of aluminum fluoride, reduce glass viscosity, thereby elemental diffusion speed is accelerated greatly when heat of crystallization is handled, and effectively suppresses and stop the formation of dendritic strontium-barium titanate crystallite.Simultaneously, the introducing of Manganse Dioxide is played and is reduced dielectric loss significantly, improve the effectiveness of insulation resistance, under the comprehensive action of above-mentioned two kinds of doping agents, the densification of ferroelectric glass-ceramic dielectric structures, crystal grain trickle (less than 500nm) that the present invention is prepared, dielectric loss is compared the low order of magnitude of unadulterated sample, and anti-electrical property improves greatly.The dielectric material breaking down field strength (direct current) of gained surpasses 60kV/mm.The present invention can be used for the manufacturing of various high energy storage density high voltage capacitors.
Description of drawings
Fig. 1 is the SEM photo of the glass-ceramic dielectric of comparative example 1 preparation;
Fig. 2 is glass-ceramic dielectric (the doped with Mn O of embodiment 1 preparation
2Mole number account for the component total mole number 1%) XRD figure spectrum after heat of crystallization is handled;
Fig. 3 is glass-ceramic dielectric (the doped with Mn O of embodiment 1 preparation
2Mole number account for the component total mole number 1%) the SEM photo;
Fig. 4 is different MnO among the embodiment 1
2(doped with Mn O under the doping situation
2Mole number account for 0.1%, 0.2%, 0.5%, 1% o'clock of component total mole number respectively) the dielectric relative permittivity of glass-ceramics with high energy storage density, dielectric loss, the insulation resistivity of preparation;
Fig. 5 is comparative example 1 and 2, embodiment 1 (doped with Mn O
2Mole number account for the component total mole number 1%) in the weibull of the dielectric disruptive strength of glass-ceramics with high energy storage density distribute.
Embodiment
The invention will be further described below in conjunction with accompanying drawing:
Comparative example 1
A kind of dielectric material of glass-ceramics, the component of dielectric material of glass-ceramics are BaO, SrO, TiO
2, SiO
2And Al
2O
3, it forms not doped with Al F
3And MnO
2, the component mol ratio is BaO:SrO:TiO
2: SiO
2: Al
2O
3=0.2936:0.0734:0.305:0.212:0.086.
A kind of preparation method of dielectric material of glass-ceramics is as follows,
(1) with purity greater than 99% BaCO
3, SrCO
3, TiO
2, SiO
2And Al
2O
3Being starting raw material, is BaO:SrO:TiO according to the component mol ratio of dielectric material of glass-ceramics
2: SiO
2: Al
2O
3=0.2936:0.0734:0.305:0.212:0.086 batching adds these raw materials the ball-milling medium dehydrated alcohol then and ground 6 hours in planetary ball mill, oven dry back high-temperature fusion, and melt temperature is 1550 ℃, is incubated 6 hours;
(2) high-temperature fusant with step (1) is poured in the metal die (the metal die material is a copper, and mould is circular), and obtaining thickness through cutting then is the glass flake of 1mm;
(3) glass flake with step (2) preparation carries out controlled crystallization, this crystallization process was divided into for two steps, at first impelled the principal crystalline phase nucleation in 2 hours 750 ℃ of temperature insulations, principal crystalline phase is a strontium-barium titanate, insulation made nuclei growth in 2 hours under 1100 ℃ of temperature then, and obtaining with the strontium-barium titanate with perovskite structure is the ferroelectric glass-ceramic dielectric of principal crystalline phase;
(4) the resulting glass-ceramic dielectric thin slice of step (3) is applied adhesive property and the good silver paste of conductivity through silk-screen printing technique, solidify to form the argent electrode, make glass-ceramic dielectric at 500 ℃ of sintering temperatures.
The SEM photo of the glass-ceramic dielectric of this comparative example preparation as shown in Figure 1, therefrom the sample microtexture presents typical dendritic brilliant feature as can be seen.
Comparative example 2
A kind of dielectric material of glass-ceramics, the main ingredient of dielectric material of glass-ceramics are BaO, SrO, TiO
2, SiO
2And Al
2O
3, it forms doped with Al F
3, the main ingredient mol ratio is BaO:SrO:TiO
2: SiO
2: Al
2O
3=0.2936:0.0734:0.305:0.212:0.086, doped with Al F
3Mole number account for 4% of component total mole number.
A kind of preparation method of dielectric material of glass-ceramics is as follows,
(1) with purity greater than 99% BaCO
3, SrCO
3, TiO
2, SiO
2, Al
2O
3And AlF
3Be starting raw material, according to main ingredient BaO, SrO, TiO
2, SiO
2And Al
2O
3Mol ratio is BaO:SrO:TiO
2: SiO
2: Al
2O
3=0.2936:0.0734:0.305:0.212:0.086, doped with Al F
3Mole number account for 4% batching of component total mole number, then these raw materials are added the ball-milling medium dehydrated alcohol and ground 6 hours in planetary ball mills, oven dry is high-temperature fusion afterwards, melt temperature is 1550 ℃, is incubated 6 hours;
(2) high-temperature fusant with step (1) is poured in the metal die (the metal die material is a copper, and mould is circular), and obtaining thickness through cutting then is the glass flake of 1mm;
(3) glass flake with step (2) preparation carries out controlled crystallization, this crystallization process was divided into for two steps, at first impelled the principal crystalline phase nucleation in 2 hours 750 ℃ of temperature insulations, principal crystalline phase is a strontium-barium titanate, insulation made nuclei growth in 2 hours under 1100 ℃ of temperature then, and obtaining with the strontium-barium titanate with perovskite structure is the ferroelectric glass-ceramic dielectric of principal crystalline phase;
(4) the resulting glass-ceramic dielectric thin slice of step (3) is applied adhesive property and the good silver paste of conductivity through silk-screen printing technique, solidify to form the argent electrode, make glass-ceramic dielectric at 500 ℃ of sintering temperatures.
A kind of dielectric material of glass-ceramics with high energy storage density, the main ingredient of dielectric material of glass-ceramics are BaO, SrO, TiO
2, SiO
2And Al
2O
3, it forms doped with Al F
3And MnO
2, the main ingredient mol ratio is BaO:SrO:TiO
2: SiO
2: Al
2O
3=0.2936:0.0734:0.305:0.212:0.086, doped with Al F
3Mole number account for 4% of component (described component is made up of main ingredient and doping component) total mole number, doped with Mn O
2Mole number account for 1% of component (described component is made up of main ingredient and doping component) total mole number.
A kind of preparation method of dielectric material of glass-ceramics with high energy storage density is as follows,
(1) with purity greater than 99% BaCO
3, SrCO
3, TiO
2, SiO
2, Al
2O
3, AlF
3And MnO
2Be starting raw material, according to main ingredient BaO, SrO, TiO
2, SiO
2And Al
2O
3Mol ratio is BaO:SrO:TiO
2: SiO
2: Al
2O
3=0.2936:0.0734:0.305:0.212:0.086, doped with Al F
3Mole number account for 4% of component total mole number, doped with Mn O
2Mole number account for 1% of component total mole number, prepare burden, then these raw materials are added the ball-milling medium dehydrated alcohol and ground 6 hours in planetary ball mills, the calcining of oven dry back, calcining temperature is 1550 ℃, is incubated 6 hours high-temperature fusion;
(2) high-temperature fusant with step (1) is poured in the metal die (the metal die material is a copper, and mould is circular), and obtaining thickness through cutting then is the glass flake of 1mm;
(3) glass flake with step (2) preparation carries out controlled crystallization, this crystallization process was divided into for two steps, at first impelled the principal crystalline phase nucleation in 2 hours 750 ℃ of temperature insulations, principal crystalline phase is a strontium-barium titanate, insulation made nuclei growth in 2 hours under 1100 ℃ of temperature then, and obtaining with the strontium-barium titanate with perovskite structure is the ferroelectric glass-ceramic dielectric of principal crystalline phase;
(4) the resulting glass-ceramic dielectric thin slice of step (3) is applied adhesive property and the good silver paste of conductivity through silk-screen printing technique, solidify to form the argent electrode, make the glass-ceramics with high energy storage density dielectric medium at 500 ℃ of sintering temperatures.
Other conditions are constant, change doped with Mn O
2Molecular fraction, doped with Mn O
2Mole number account for 0.1%, 0.2% and 0.5% of component total mole number respectively, obtain doped with Mn O
2Mole number account for 0.1%, 0.2%, 0.5% o'clock glass-ceramics with high energy storage density dielectric medium of component total mole number respectively.
Step (3) gained ferroelectric glass-ceramic dielectric material phase analysis and microtexture as shown in Figures 2 and 3, Fig. 2 is glass-ceramic dielectric (doped with Mn O
2Mole number account for the component total mole number 1%) XRD figure spectrum after heat of crystallization is handled, therefrom the principal crystalline phase of this microcrystal glass material is a strontium-barium titanate as can be seen, other has a spot of BaAl
2Si
2O
8Fig. 3 is glass-ceramic dielectric (doped with Mn O
2Mole number account for the component total mole number 1%) the SEM photo, therefrom ferroelectric as can be seen crystallite size is even.
Doped with Mn O
2Mole number account for the component total mole number respectively 0.1%, 0.2%, 0.5%, 1% o'clock the dielectric relative permittivity of glass-ceramics with high energy storage density, dielectric loss, insulation resistivity as shown in Figure 4, test condition: specific inductivity and dielectric loss are that frequency 1kHz measures down; Insulation resistivity is measured down for the 100V direct current, and probe temperature is room temperature.The result shows: along with the increase of manganese dioxide doped amount, the sample insulation resistivity significantly improves, and dielectric loss descends, and relative permittivity decreases simultaneously.
Fig. 5 is comparative example 1 and 2, embodiment 1 (doped with Mn O
2Mole number account for the component total mole number 1%) in the weibull of the dielectric disruptive strength of glass-ceramics with high energy storage density distribute.Disruptive strength is being that medium is measured with the transformer oil, and probe temperature is a room temperature.As can be seen from the figure the disruptive strength of the glass-ceramic dielectric of embodiment 1 preparation is significantly higher than the disruptive strength of the glass-ceramic dielectric of comparative example 1 and 2 preparations.
A kind of dielectric material of glass-ceramics with high energy storage density, the main ingredient of dielectric material of glass-ceramics are BaO, SrO, TiO
2, SiO
2And Al
2O
3, it forms doped with Al F
3And MnO
2, the main ingredient mol ratio is BaO:SrO:TiO
2: SiO
2: Al
2O
3=0.2800:0.0820:0.3150:0.2200:0.1060, doped with Al F
3Mole number account for 6% of component total mole number, doped with Mn O
2Mole number account for 0.4% of component total mole number.
A kind of preparation method of dielectric material of glass-ceramics with high energy storage density is as follows,
(1) with purity greater than 99% BaCO
3, SrCO
3, TiO
2, SiO
2, Al
2O
3, AlF
3And MnO
2Be starting raw material, according to main ingredient BaO, SrO, TiO
2, SiO
2And Al
2O
3Mol ratio is BaO:SrO:TiO
2: SiO
2: Al
2O
3=0.2800:0.0820:0.3150:0.2200:0.1060, doped with Al F
3Mole number account for 6% of component total mole number, doped with Mn O
2Mole number account for 0.4% of component total mole number, prepare burden, then these raw materials are added the ball-milling medium dehydrated alcohol and ground 5 hours in planetary ball mills, the calcining of oven dry back, calcining temperature is 1600 ℃, is incubated 5.5 hours high-temperature fusion;
(2) high-temperature fusant of step (1) is prepared the glass flake that thickness is 1mm through cold-rolling process;
(3) glass flake with step (2) preparation carries out controlled crystallization, this crystallization process was divided into for two steps, at first impelled the principal crystalline phase nucleation in 1.5 hours 800 ℃ of temperature insulations, principal crystalline phase is a strontium-barium titanate, insulation made nuclei growth in 3 hours under 1050 ℃ of temperature then, and obtaining with the strontium-barium titanate with perovskite structure is the ferroelectric glass-ceramic dielectric of principal crystalline phase;
(4) the resulting glass-ceramic dielectric thin slice of step (3) is applied adhesive property and the good silver paste of conductivity through silk-screen printing technique, solidify to form the argent electrode, make the glass-ceramics with high energy storage density dielectric medium at 550 ℃ of sintering temperatures.
The dielectric relative permittivity of the glass-ceramics with high energy storage density that present embodiment obtains, dielectric loss, insulation resistivity are close with embodiment 1 gained sample result.Test condition: specific inductivity and dielectric loss are measured down for frequency 1kHz; Insulation resistivity is measured down for the 100V direct current, and probe temperature is room temperature.
A kind of dielectric material of glass-ceramics with high energy storage density, the main ingredient of dielectric material of glass-ceramics are BaO, SrO, TiO
2, SiO
2And Al
2O
3, it forms doped with Al F
3And MnO
2, the main ingredient mol ratio is BaO:SrO:TiO
2: SiO
2: Al
2O
3=0.3301:0.0522:0.3150:0.2300:0.0800, doped with Al F
3Mole number account for 7% of component total mole number, doped with Mn O
2Mole number account for 0.6% of component total mole number.
A kind of preparation method of dielectric material of glass-ceramics with high energy storage density is as follows,
(1) with purity greater than 99% BaCO
3, SrCO
3, TiO
2, SiO
2, Al
2O
3, AlF
3And MnO
2Be starting raw material, according to main ingredient BaO, SrO, TiO
2, SiO
2And Al
2O
3Mol ratio is BaO:SrO:TiO
2: SiO
2: Al
2O
3=0.3301:0.0522:0.3150:0.2300:0.0800, doped with Al F
3Mole number account for 7% of component total mole number, doped with Mn O
2Mole number account for 0.6% of component total mole number, prepare burden, then these raw materials are added the ball-milling medium dehydrated alcohol and ground 5 hours in planetary ball mills, the calcining of oven dry back, calcining temperature is 1500 ℃, is incubated 5 hours high-temperature fusion;
(2) high-temperature fusant with step (1) carries out quick shrend, and the glass particle that shrend is obtained adds ball-milling medium dehydrated alcohol grinding 20 hours in planetary ball mill again, and air atmosphere is oven dry down, obtains the thin slice that thickness is 1mm through compression moulding then;
(3) glass flake with step (2) preparation carries out controlled crystallization, this crystallization process was divided into for two steps, at first impelled the principal crystalline phase nucleation in 1 hour 760 ℃ of temperature insulations, principal crystalline phase is a strontium-barium titanate, insulation made nuclei growth in 3 hours under 1050 ℃ of temperature then, and obtaining with the barium titanate with perovskite structure is the ferroelectric glass-ceramic dielectric of principal crystalline phase;
(4) the resulting glass-ceramic dielectric thin slice of step (3) is applied adhesive property and the good silver paste of conductivity through silk-screen printing technique, solidify to form the argent electrode, make the glass-ceramics with high energy storage density dielectric medium at 530 ℃ of sintering temperatures.
The dielectric relative permittivity of the glass-ceramics with high energy storage density that present embodiment obtains, dielectric loss, insulation resistivity are close with embodiment 1 gained sample result.Test condition: specific inductivity and dielectric loss are measured down for frequency 1kHz; Insulation resistivity is measured down for the 100V direct current, and probe temperature is room temperature.
Claims (4)
1, a kind of dielectric material of glass-ceramics with high energy storage density is characterized in that, the main ingredient of dielectric material of glass-ceramics is BaO, SrO, TiO
2, SiO
2And Al
2O
3, it forms doped with Al F
3And MnO
2, the main ingredient mol ratio is BaO:SrO:TiO
2: SiO
2: Al
2O
3=(0.28～0.35): (0.05～0.10): (0.27～0.35): (0.20～0.25): (0.04～0.11), doped with Al F
3Mole number account for 2～8% of component total mole number, doped with Mn O
2Mole number account for 0.1～1% of component total mole number.
2, a kind of preparation method of dielectric material of glass-ceramics with high energy storage density is characterized in that, this method steps is as follows,
(1) with purity greater than 99% BaCO
3, SrCO
3, TiO
2, SiO
2, Al
2O
3, AlF
3And MnO
2Be starting raw material, according to main ingredient BaO, SrO, TiO
2, SiO
2And Al
2O
3Mol ratio is BaO:SrO:TiO
2: SiO
2: Al
2O
3=(0.28～0.35): (0.05～0.10): (0.27～0.35): (0.20～0.25): (0.04～0.11), doped with Al F
3Mole number account for 2～8% of component total mole number, doped with Mn O
2Mole number account for 0.1～1% of component total mole number, prepare burden, then these raw materials are added ball-milling medium and ground 4～6 hours in planetary ball mills, the calcining of oven dry back, calcining temperature is 1400～1650 ℃, is incubated 2～6 hours high-temperature fusion;
(2) high-temperature fusant with step (1) is poured in the metal die, and obtaining thickness through cutting then is the glass flake of 0.2～1mm; Perhaps, the high-temperature fusant of step (1) is prepared the glass flake that thickness is 0.1～1mm through cold-rolling process; Perhaps, the high-temperature fusant of step (1) is carried out quick shrend, the glass particle that shrend is obtained adds ball-milling medium grinding 10～20 hours in planetary ball mill again, and air atmosphere is oven dry down, obtains the thin slice that thickness is 0.5～2mm through compression moulding then;
(3) glass flake with step (2) preparation carries out controlled crystallization, this crystallization process was divided into for two steps, at first impelled the principal crystalline phase nucleation in 1～2 hour 750～850 ℃ of temperature insulations, principal crystalline phase is a strontium-barium titanate, be incubated 1～3 hour then under 800～1100 ℃ of temperature and make nuclei growth, obtaining with the strontium-barium titanate with perovskite structure is the ferroelectric glass-ceramic dielectric of principal crystalline phase;
(4) the resulting glass-ceramic dielectric thin slice of step (3) is applied adhesive property and the good silver paste of conductivity through silk-screen printing technique, solidify to form the argent electrode at 500～550 ℃ of sintering temperatures, make the glass-ceramics with high energy storage density dielectric medium.
3, the preparation method of a kind of dielectric material of glass-ceramics with high energy storage density according to claim 2 is characterized in that, described ball-milling medium is deionized water or dehydrated alcohol.
4, the preparation method of a kind of dielectric material of glass-ceramics with high energy storage density according to claim 2 is characterized in that, described metal die material is steel or copper, and mould is circle or rectangle.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200910082177XA CN101531461B (en) | 2009-04-16 | 2009-04-16 | Dielectric material of glass-ceramics with high energy storage density and preparation method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200910082177XA CN101531461B (en) | 2009-04-16 | 2009-04-16 | Dielectric material of glass-ceramics with high energy storage density and preparation method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101531461A true CN101531461A (en) | 2009-09-16 |
| CN101531461B CN101531461B (en) | 2011-06-29 |
Family
ID=41102345
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN200910082177XA Expired - Fee Related CN101531461B (en) | 2009-04-16 | 2009-04-16 | Dielectric material of glass-ceramics with high energy storage density and preparation method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101531461B (en) |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102260044A (en) * | 2011-04-30 | 2011-11-30 | 桂林电子科技大学 | Energy storage niobate microcrystalline glass dielectric material and preparation method thereof |
| CN102775069A (en) * | 2012-07-20 | 2012-11-14 | 同济大学 | Preparation method of barium strontium titanate based glass ceramic energy storage material |
| CN105271761A (en) * | 2015-11-10 | 2016-01-27 | 同济大学 | High-energy-density niobate-based glass ceramic energy storage material and preparation and application thereof |
| CN105776871A (en) * | 2016-03-04 | 2016-07-20 | 北京科技大学 | Method for regulating emission cross section of Nd3+/ Na2Ca2Si3O9 laser glass ceramic |
| CN107129155A (en) * | 2017-07-04 | 2017-09-05 | 合肥择浚电气设备有限公司 | A kind of preparation technology of dielectric material of glass-ceramics with high energy storage density |
| CN107176792A (en) * | 2017-06-28 | 2017-09-19 | 合肥博之泰电子科技有限公司 | A kind of dielectric material of glass-ceramics and preparation method thereof |
| CN111517645A (en) * | 2020-04-10 | 2020-08-11 | 广东健诚高科玻璃制品股份有限公司 | Jade glass, low-melting-point concentrated colorant for jade glass and dyeing method |
| CN114212985A (en) * | 2021-12-14 | 2022-03-22 | 华南理工大学 | Preparation method of microcrystalline glass based on defect-induced spatially selective crystallization |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH03232740A (en) * | 1990-02-08 | 1991-10-16 | Mitsubishi Electric Corp | Production of high-strength and readily processable glass ceramics |
| CN100360446C (en) * | 2005-11-23 | 2008-01-09 | 山东建筑工程学院材料科学研究所 | Process for preparing microcrystal glass ceramic by concrete sludge |
-
2009
- 2009-04-16 CN CN200910082177XA patent/CN101531461B/en not_active Expired - Fee Related
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102260044A (en) * | 2011-04-30 | 2011-11-30 | 桂林电子科技大学 | Energy storage niobate microcrystalline glass dielectric material and preparation method thereof |
| CN102775069A (en) * | 2012-07-20 | 2012-11-14 | 同济大学 | Preparation method of barium strontium titanate based glass ceramic energy storage material |
| CN102775069B (en) * | 2012-07-20 | 2015-02-18 | 同济大学 | Preparation method of barium strontium titanate based glass ceramic energy storage material |
| CN105271761A (en) * | 2015-11-10 | 2016-01-27 | 同济大学 | High-energy-density niobate-based glass ceramic energy storage material and preparation and application thereof |
| CN105776871A (en) * | 2016-03-04 | 2016-07-20 | 北京科技大学 | Method for regulating emission cross section of Nd3+/ Na2Ca2Si3O9 laser glass ceramic |
| CN105776871B (en) * | 2016-03-04 | 2019-10-18 | 北京科技大学 | A kind of Nd3+/Na2Ca2Si3O9 laser glass ceramics emission cross section regulation method |
| CN107176792A (en) * | 2017-06-28 | 2017-09-19 | 合肥博之泰电子科技有限公司 | A kind of dielectric material of glass-ceramics and preparation method thereof |
| CN107129155A (en) * | 2017-07-04 | 2017-09-05 | 合肥择浚电气设备有限公司 | A kind of preparation technology of dielectric material of glass-ceramics with high energy storage density |
| CN111517645A (en) * | 2020-04-10 | 2020-08-11 | 广东健诚高科玻璃制品股份有限公司 | Jade glass, low-melting-point concentrated colorant for jade glass and dyeing method |
| CN114212985A (en) * | 2021-12-14 | 2022-03-22 | 华南理工大学 | Preparation method of microcrystalline glass based on defect-induced spatially selective crystallization |
Also Published As
| Publication number | Publication date |
|---|---|
| CN101531461B (en) | 2011-06-29 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101531461B (en) | Dielectric material of glass-ceramics with high energy storage density and preparation method | |
| CN102260044B (en) | Energy storage niobate microcrystalline glass dielectric material and preparation method thereof | |
| CN102060521B (en) | Hexagonal type barium titanate powder, producing method thereof, dielectric ceramic composition and electronic component | |
| CN105753472B (en) | The niobic acid barium potassium base glass ceramics energy storage material of high energy storage density and preparation and application | |
| CN101026035A (en) | Dielectric ceramic composition and the production method | |
| EP1860080A1 (en) | Dielectric porcelain composition and method for production thereof | |
| CN102050484B (en) | Hexagonal type barium titanate powder, producing method thereof, dielectric ceramic composition and electronic component | |
| CN105418068B (en) | A kind of niobate glass ceramics energy storage material and its preparation method and application | |
| JP2000044341A (en) | Dielectric ceramic composition | |
| CN105271761A (en) | High-energy-density niobate-based glass ceramic energy storage material and preparation and application thereof | |
| CN105712634B (en) | Lanthanum oxide doping strontium barium niobate base glass ceramics energy storage material and preparation method thereof | |
| CN110240409A (en) | Lead bariun niobate sodium base glass ceramic material of high energy storage density and preparation method thereof | |
| JP4613826B2 (en) | Ceramic substrate composition, ceramic substrate, method for producing ceramic substrate, and glass composition | |
| CN1790568B (en) | Dielectric ceramic composition, electronic component, and method for manufacturing the same | |
| CN108585515B (en) | Bismuth niobate-based glass ceramic material with high energy storage density and preparation method and application thereof | |
| CN106630642B (en) | A kind of barium strontium niobate sodium base glass ceramics energy storage material and the preparation method and application thereof | |
| CN104803605A (en) | Rare-earth-doped barium-strontium-titanate-based glass ceramic energy storage material and preparation method thereof | |
| CN106186704B (en) | A kind of strontium barium niobate potassium base glass ceramics energy storage material and the preparation method and application thereof | |
| CN103102079A (en) | Glass ceramic dielectric with high breakdown strength and preparation method thereof | |
| CN105541115A (en) | Titanic acid and niobic acid compound glass ceramic as well as preparation method and application thereof | |
| CN106565095A (en) | A manganese dioxide-doped barium-strontium niobate based glass ceramic energy-storing material and a preparing method thereof | |
| JP2004026543A (en) | Dielectric porcelain composition and laminated ceramic component using the same | |
| JPH0737427A (en) | Dielectric ceramic composition | |
| KR100509633B1 (en) | Dielectric ceramic composition with reinforced insulation glass frit and reinforced insulation glass frit | |
| CN102531579A (en) | Ceramic dielectric material and manufacture method thereof and ceramic capacitor and manufacture method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| EE01 | Entry into force of recordation of patent licensing contract |
Application publication date: 20090916 Assignee: Beijing Yuanliu Hongyuan Electronic Technology Co., Ltd. Assignor: Tsinghua University Contract record no.: 2013990000664 Denomination of invention: Dielectric material of glass-ceramics with high energy storage density and preparation method Granted publication date: 20110629 License type: Exclusive License Record date: 20131012 |
|
| LICC | Enforcement, change and cancellation of record of contracts on the licence for exploitation of a patent or utility model | ||
| C17 | Cessation of patent right | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20110629 Termination date: 20140416 |