CN107176792A - A kind of dielectric material of glass-ceramics and preparation method thereof - Google Patents
A kind of dielectric material of glass-ceramics and preparation method thereof Download PDFInfo
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- CN107176792A CN107176792A CN201710506230.9A CN201710506230A CN107176792A CN 107176792 A CN107176792 A CN 107176792A CN 201710506230 A CN201710506230 A CN 201710506230A CN 107176792 A CN107176792 A CN 107176792A
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- 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
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- 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
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B32/00—Thermal after-treatment of glass products not provided for in groups C03B19/00, C03B25/00 - C03B31/00 or C03B37/00, e.g. crystallisation, eliminating gas inclusions or other impurities; Hot-pressing vitrified, non-porous, shaped glass products
- C03B32/02—Thermal crystallisation, e.g. for crystallising glass bodies into glass-ceramic articles
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- 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
- C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
- C03C17/06—Surface treatment of glass, not in the form of fibres or filaments, by coating with metals
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Abstract
The invention discloses a kind of dielectric material of glass-ceramics and preparation method thereof, it is related to field of electronic materials, the dielectric substance includes following raw material：BaCO3、SrCO3、TiO2、SiO2、Al2O3、AlF3And Na2CO3；Its preparation method is that raw material first is made into powder；Powder is smelted into liquation to be poured into mould, sheet glass is obtained after annealed processing；Dominated crystallization processing is carried out to the sheet glass；Finally by material through screen-printing deposition adhesive property and the good middle temperature silver paste of electric conductivity, after sintering curing formation metal silver electrode at a temperature of 480 DEG C.The dielectric material of glass-ceramics of the present invention prepares simple and convenient, and energy consumption is low, with high-k, high breakdown strength and high energy storage density.
Description
Technical field
The present invention relates to field of electronic materials, and in particular to a kind of dielectric material of glass-ceramics and preparation method thereof.
Background technology
As energy crisis is realized and environmental consciousness is gradually stepped up, people begin attempt to exploitation and the profit of novel energy
With.As the important support means of new energy technology, energy storage technology has obtained various countries' great attention.Wherein capacitor has because of it
Specific power is high, charging rate is fast, resistance to circulation aging, suitable for HTHP occasion and it is environmentally safe the advantages of and enjoy
Concern.Current capacitor is applied on some visual plants, such as hybrid vehicle inverter, pulse-power apparatus.
But existing traditional impulse capacitor exist unfavorable factor such as energy storage density it is low and it is easy occur blast or discharge
Electric current is small, and discharge life is short etc., it is difficult to meet the demand that new technology further develops.Ceramic dielectric material is preparing high energy storage
There is some superiority in terms of density capacitor, but its maximum shortcoming is that anti-disruptive field intensity is difficult to rise again.Current capacitor element
Size it is less and less, it is necessary to anti-disruptive field intensity also more and more higher.Therefore, the dielectric with high energy storage density is developed
Material is extremely urgent.
Devitrified glass has advantage of both the high-k of ceramics and the high breakdown strength of glass concurrently, so that as system
The dielectric ideal material of standby high energy storage density.At present, research focuses primarily upon titanate devitrified glass and leaded niobates
Devitrified glass system, and be mostly the system based on silicate or silicon borate glass.But, due to titanate crystallite glass
The breakdown strength of glass is relatively low, and it is not high to ultimately result in energy storage density, and energy storage density deteriorates when applying high electric field；Leaded
Niobate microcrystalline glass containing more noxious material lead oxide in composition due to making its application receive a definite limitation, while at heat
It is unfavorable to the breakdown strength for improving material that substantial amounts of NaNbO3 is separated out during reason, and energy storage density is also not very high.In addition, two bodies
Be glass fusion temperature it is higher (more than 1500 DEG C), be unfavorable for reducing cost and energy-saving and emission-reduction.
The content of the invention
For problems of the prior art, the invention provides a kind of high-k, high breakdown strength and high storage
Dielectric material of glass-ceramics dielectric material of glass-ceramics of energy density and preparation method thereof.
In order to achieve the above object, the present invention is achieved through the following technical solutions：
A kind of dielectric material of glass-ceramics, including following raw material by weight are made：BaCO320-40 parts,
SrCO35-15 parts, TiO210-20 parts, SiO215-25 parts, Al2O310-20 parts, AlF31-10 parts and Na2CO36-12 parts；
Its key component mol ratio is BaO:SrO:TiO2:SiO2:Al2O3:Na2O=(0.20~0.40):(0.05~
0.15):(0.10~0.20):(0.15~0.25):(0.10~0.20):(0.06~0.12), adulterate AlF3Molal quantity account for
The 3~7% of component total mole number.
Further, the dielectric substance is made including following raw material by weight：BaCO325-35 parts,
SrCO38-12 parts, TiO212-18 parts, SiO218-22 parts, Al2O312-18 parts, AlF31-5 parts and Na2CO38-10 parts；
Its key component mol ratio is BaO:SrO:TiO2:SiO2:Al2O3:Na2O=(0.25~0.35):(0.08~
0.12):(0.12~0.18):(0.18~0.22):(0.12~0.18):(0.08~0.10), adulterate AlF3Molal quantity account for
The 4~6% of component total mole number.
Further, the dielectric substance is made including following raw material by weight：BaCO330 parts, SrCO3
10 parts, TiO215 parts, SiO220 parts, Al2O315 parts, AlF33 parts and Na2CO39 parts；Its key component mol ratio is BaO:
SrO:TiO2:SiO2:Al2O3:Na2O=0.30:0.10:0.15:0.20:0.15:0.09, adulterate AlF3Molal quantity account for component
The 5% of total mole number.
A kind of preparation method of above-mentioned dielectric material of glass-ceramics, is followed the steps below：
(1) raw material is weighed by the weight, by raw material mixed grinding into powder；
(2) liquation is smelted into after powder is dried, melting heating rate is 60-80 DEG C/min；
(3) liquation is poured into preheated mold, preheating temperature is 560-620 DEG C, is moved back again after being poured
Fire processing, obtains sheet glass after cutting；
(4) dominated crystallization processing is carried out to the sheet glass, obtains dielectric material of glass-ceramics semi-finished product；
(5) it is the dielectric material of glass-ceramics semi-finished product are good by screen-printing deposition adhesive property and electric conductivity
Good middle temperature silver paste, after sintering curing formation metal silver electrode at a temperature of 480 DEG C.
Further, in step (1), the powder is by made from raw mill to particle diameter≤1mm by ball mill.
Further, in step (2), the temperature of the melting is 1420-1480 DEG C, and smelting time is 1-2h.
Further, in step (3), the annealing is that the sheet glass after pouring is placed in Muffle furnace, annealing
Temperature control is at 520-580 DEG C, and soaking time is 40-60min.
Further, in step (3), dominated crystallization processing be first be incubated at 760-780 DEG C 80-100min into
Core, is then incubated 80-100min at 860-880 DEG C.
The present invention has following beneficial effect：
(1) proportioning and its preparation technology of the invention by controlling raw material, regulates and controls BaO, SrO, TiO2、SiO2、Al2O3、
Na2O and AlF3Component molal quantity, and then obtain the crystallite glass of a kind of high-k, high breakdown strength and high energy storage density
Glass dielectric substance；The dielectric constant of this kind of glass-ceramic dielectric is up to more than 146, and breakdown strength is up to 880-
1460kV/cm is adjustable, available for various high energy storage densities and extra-high voltage capacitors equipment；
(2) dielectric material of glass-ceramics preparation method of the invention is simple and convenient, scientifically and rationally reduces material and exists
Required temperature when founding and being heat-treated, reduces the output of energy consumption, has reached effect and the purpose of energy-conserving and environment-protective, suitable to promote
Using.
Embodiment
The embodiment of the present invention is further described with reference to embodiment, following examples are only used for more
Technical scheme is clearly demonstrated, and can not be limited the scope of the invention with this.
Embodiment 1
A kind of dielectric material of glass-ceramics, weighs following raw material：BaCO320kg、SrCO35kg、TiO210kg、
SiO215kg、Al2O310kg、AlF31kg and Na2CO36kg；Its key component mol ratio is BaO:SrO:TiO2:SiO2:Al2O3:
Na2O=0.20:0.05:0.10:0.15:0.10:0.06, adulterate AlF3Molal quantity account for the 3% of component total mole number.
A kind of preparation method of above-mentioned dielectric material of glass-ceramics, is followed the steps below：
(1) first raw material is mixed and passes through ball mill grinding into particle diameter≤1mm powders；
(2) it is delivered to after powder is dried again in smelting furnace and is smelted into liquation, melting heating rate is 60 DEG C/min, melting
Temperature is 1420 DEG C, and smelting time is 1h；
(3) liquation is poured into preheated mold after, preheating temperature is 560 DEG C, and Muffle is placed in after being poured
Made annealing treatment in stove, and annealing temperature control, at 520 DEG C, soaking time is 40min, and sheet glass is obtained after cutting；
(4) dominated crystallization processing then is carried out to the sheet glass, is particularly first incubated 80min nucleation at 760 DEG C, so
80min is incubated at 860 DEG C afterwards, dielectric material of glass-ceramics semi-finished product are obtained after terminating；
(5) the dielectric material of glass-ceramics semi-finished product are finally passed through into screen-printing deposition adhesive property and electric conductivity
The good middle temperature silver paste of energy, crystallite glass of the invention is made after sintering curing formation metal silver electrode at a temperature of 480 DEG C
Glass dielectric substance.
Embodiment 2
A kind of dielectric material of glass-ceramics, weighs following raw material：BaCO325kg、SrCO38kg、TiO212kg、
SiO218kg、Al2O312kg、AlF31kg and Na2CO38kg；Its key component mol ratio is BaO:SrO:TiO2:SiO2:Al2O3:
Na2O=0.25:0.08:0.12:0.18:0.12:0.08, adulterate AlF3Molal quantity account for the 4% of component total mole number.
A kind of preparation method of above-mentioned dielectric material of glass-ceramics, is followed the steps below：
(1) first raw material is mixed and passes through ball mill grinding into particle diameter≤1mm powders；
(2) it is delivered to after powder is dried again in smelting furnace and is smelted into liquation, melting heating rate is 65 DEG C/min, melting
Temperature is 1460 DEG C, and smelting time is 1.2h；
(3) liquation is poured into preheated mold after, preheating temperature is 570 DEG C, and Muffle is placed in after being poured
Made annealing treatment in stove, and annealing temperature control, at 530 DEG C, soaking time is 45min, and sheet glass is obtained after cutting；
(4) dominated crystallization processing then is carried out to the sheet glass, is particularly first incubated 85min nucleation at 765 DEG C, so
85min is incubated at 865 DEG C afterwards, dielectric material of glass-ceramics semi-finished product are obtained after terminating；
(5) the dielectric material of glass-ceramics semi-finished product are finally passed through into screen-printing deposition adhesive property and electric conductivity
The good middle temperature silver paste of energy, crystallite glass of the invention is made after sintering curing formation metal silver electrode at a temperature of 480 DEG C
Glass dielectric substance.
Embodiment 3
A kind of dielectric material of glass-ceramics, weighs following raw material：BaCO330kg、SrCO310kg、TiO2 15kg、SiO2
20kg、Al2O3 15kg、AlF33kg and Na2CO39kg；Its key component mol ratio is BaO:SrO:TiO2:SiO2:Al2O3:
Na2O=0.30:0.10:0.15:0.20:0.15:0.09, adulterate AlF3Molal quantity account for the 5% of component total mole number.
A kind of preparation method of above-mentioned dielectric material of glass-ceramics, is followed the steps below：
(1) first raw material is mixed and passes through ball mill grinding into particle diameter≤1mm powders；
(2) it is delivered to after powder is dried again in smelting furnace and is smelted into liquation, melting heating rate is 70 DEG C/min, melting
Temperature is 1450 DEG C, and smelting time is 1.5h；
(3) liquation is poured into preheated mold after, preheating temperature is 590 DEG C, and Muffle is placed in after being poured
Made annealing treatment in stove, and annealing temperature control, at 550 DEG C, soaking time is 50min, and sheet glass is obtained after cutting；
(4) dominated crystallization processing then is carried out to the sheet glass, is particularly first incubated 90min nucleation at 770 DEG C, so
90min is incubated at 870 DEG C afterwards, dielectric material of glass-ceramics semi-finished product are obtained after terminating；
(5) the dielectric material of glass-ceramics semi-finished product are finally passed through into screen-printing deposition adhesive property and electric conductivity
The good middle temperature silver paste of energy, crystallite glass of the invention is made after sintering curing formation metal silver electrode at a temperature of 480 DEG C
Glass dielectric substance.
Embodiment 4
A kind of dielectric material of glass-ceramics, weighs following raw material：BaCO335kg、SrCO312kg、TiO218kg、
SiO222kg、Al2O318kg、AlF35kg and Na2CO310kg；Its key component mol ratio is BaO:SrO:TiO2:SiO2:
Al2O3:Na2O=0.35:0.12:0.18:0.22:0.18:0.10, adulterate AlF3Molal quantity account for the 6% of component total mole number.
A kind of preparation method of above-mentioned dielectric material of glass-ceramics, is followed the steps below：
(1) first raw material is mixed and passes through ball mill grinding into particle diameter≤1mm powders；
(2) it is delivered to after powder is dried again in smelting furnace and is smelted into liquation, melting heating rate is 75 DEG C/min, melting
Temperature is 1470 DEG C, and smelting time is 1.8h；
(3) liquation is poured into preheated mold after, preheating temperature is 610 DEG C, and Muffle is placed in after being poured
Made annealing treatment in stove, and annealing temperature control, at 570 DEG C, soaking time is 55min, and sheet glass is obtained after cutting；
(4) dominated crystallization processing then is carried out to the sheet glass, is particularly first incubated 95min nucleation at 775 DEG C, so
95min is incubated at 875 DEG C afterwards, dielectric material of glass-ceramics semi-finished product are obtained after terminating；
(5) the dielectric material of glass-ceramics semi-finished product are finally passed through into screen-printing deposition adhesive property and electric conductivity
The good middle temperature silver paste of energy, crystallite glass of the invention is made after sintering curing formation metal silver electrode at a temperature of 480 DEG C
Glass dielectric substance.
Embodiment 5
A kind of dielectric material of glass-ceramics, weighs following raw material：BaCO340kg、SrCO315kg、TiO220kg、
SiO225kg、Al2O320kg、AlF310kg and Na2CO312kg；Its key component mol ratio is BaO:SrO:TiO2:SiO2:
Al2O3:Na2O=0.40:0.15:0.20:0.25:0.20:0.12, adulterate AlF3Molal quantity account for the 7% of component total mole number.
A kind of preparation method of above-mentioned dielectric material of glass-ceramics, is followed the steps below：
(1) first raw material is mixed and passes through ball mill grinding into particle diameter≤1mm powders；
(2) it is delivered to after powder is dried again in smelting furnace and is smelted into liquation, melting heating rate is 80 DEG C/min, melting
Temperature is 1480 DEG C, and smelting time is 2h；
(3) liquation is poured into preheated mold after, preheating temperature is 620 DEG C, and Muffle is placed in after being poured
Made annealing treatment in stove, and annealing temperature control, at 580 DEG C, soaking time is 60min, and sheet glass is obtained after cutting；
(4) dominated crystallization processing then is carried out to the sheet glass, is particularly first incubated 100min nucleation at 780 DEG C,
Then 100min is incubated at 880 DEG C, dielectric material of glass-ceramics semi-finished product is obtained after terminating；
(5) the dielectric material of glass-ceramics semi-finished product are finally passed through into screen-printing deposition adhesive property and electric conductivity
The good middle temperature silver paste of energy, crystallite glass of the invention is made after sintering curing formation metal silver electrode at a temperature of 480 DEG C
Glass dielectric substance.
The preferred embodiments of the present invention are the foregoing is only, are not intended to limit the invention, although with reference to foregoing reality
Apply example the present invention is described in detail, for those skilled in the art, it still can be to foregoing each implementation
Technical scheme described in example is modified, or carries out equivalent substitution to which part technical characteristic.All essences in the present invention
God is with principle, and any modification, equivalent substitution and improvements made etc. should be included in the scope of the protection.
Claims (8)
1. a kind of dielectric material of glass-ceramics, it is characterised in that be made including following raw material by weight：BaCO320-
40 parts, SrCO35-15 parts, TiO210-20 parts, SiO215-25 parts, Al2O310-20 parts, AlF31-10 parts and Na2CO36-12 parts；
Its key component mol ratio is BaO:SrO:TiO2:SiO2:Al2O3:Na2O=(0.20~0.40):(0.05~0.15):
(0.10~0.20):(0.15~0.25):(0.10~0.20):(0.06~0.12), adulterate AlF3Molal quantity to account for component total
The 3~7% of molal quantity.
2. a kind of dielectric material of glass-ceramics according to claim 1, it is characterised in that including it is following by weight
Raw material be made：BaCO325-35 parts, SrCO38-12 parts, TiO212-18 parts, SiO218-22 parts, Al2O312-18 parts, AlF31-
5 parts and Na2CO38-10 parts；
Its key component mol ratio is BaO:SrO:TiO2:SiO2:Al2O3:Na2O=(0.25~0.35):(0.08~0.12):
(0.12~0.18):(0.18~0.22):(0.12~0.18):(0.08~0.10), adulterate AlF3Molal quantity to account for component total
The 4~6% of molal quantity.
3. a kind of dielectric material of glass-ceramics according to claim 2, it is characterised in that including it is following by weight
Raw material be made：BaCO330 parts, SrCO310 parts, TiO215 parts, SiO220 parts, Al2O315 parts, AlF33 parts and Na2CO39 parts；Its
Key component mol ratio is BaO:SrO:TiO2:SiO2:Al2O3:Na2O=0.30:0.10:0.15:0.20:0.15:0.09, mix
Miscellaneous AlF3Molal quantity account for the 5% of component total mole number.
4. a kind of preparation method of dielectric material of glass-ceramics as described in claim 1-3 any one, it is characterised in that
Comprise the following steps：
(1) raw material is weighed by the weight, by raw material mixed grinding into powder；
(2) liquation is smelted into after powder is dried, melting heating rate is 60-80 DEG C/min；
(3) liquation is poured into preheated mold, preheating temperature is 560-620 DEG C, is carried out again at annealing after being poured
Reason, obtains sheet glass after cutting；
(4) dominated crystallization processing is carried out to the sheet glass, obtains dielectric material of glass-ceramics semi-finished product；
(5) it is that the dielectric material of glass-ceramics semi-finished product are good by screen-printing deposition adhesive property and electric conductivity
Middle temperature silver paste, after sintering curing formation metal silver electrode at a temperature of 480 DEG C.
5. the preparation method of a kind of dielectric material of glass-ceramics according to claim 4, it is characterised in that in step
(1) in, the powder is by made from raw mill to particle diameter≤1mm by ball mill.
6. the preparation method of a kind of dielectric material of glass-ceramics according to claim 4, it is characterised in that in step
(2) in, the temperature of the melting is 1420-1480 DEG C, and smelting time is 1-2h.
7. the preparation method of a kind of dielectric material of glass-ceramics according to claim 4, it is characterised in that in step
(3) in, the annealing is that the sheet glass after pouring is placed in Muffle furnace, and annealing temperature is controlled at 520-580 DEG C, insulation
Time is 40-60min.
8. the preparation method of a kind of dielectric material of glass-ceramics according to claim 4, it is characterised in that in step
(3) in, the dominated crystallization processing is first to be incubated 80-100min nucleation at 760-780 DEG C, is then incubated 80- at 860-880 DEG C
100min。
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110828168A (en) * | 2019-12-06 | 2020-02-21 | 电子科技大学 | Multilayer microcrystalline glass capacitor and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2005061403A1 (en) * | 2003-12-19 | 2005-07-07 | Murata Manufacturing Co., Ltd. | Ferroelectric glass composition and process for producing the same |
| CN101531461A (en) * | 2009-04-16 | 2009-09-16 | 清华大学 | Dielectric material of glass-ceramics with high energy storage density and preparation method |
| CN102775069A (en) * | 2012-07-20 | 2012-11-14 | 同济大学 | Preparation method of barium strontium titanate based glass ceramic energy storage material |
| CN105541115A (en) * | 2016-02-03 | 2016-05-04 | 同济大学 | Titanic acid and niobic acid compound glass ceramic as well as preparation method and application thereof |
-
2017
- 2017-06-28 CN CN201710506230.9A patent/CN107176792A/en not_active Withdrawn
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2005061403A1 (en) * | 2003-12-19 | 2005-07-07 | Murata Manufacturing Co., Ltd. | Ferroelectric glass composition and process for producing the same |
| CN101531461A (en) * | 2009-04-16 | 2009-09-16 | 清华大学 | Dielectric material of glass-ceramics with high energy storage density and preparation method |
| CN102775069A (en) * | 2012-07-20 | 2012-11-14 | 同济大学 | Preparation method of barium strontium titanate based glass ceramic energy storage material |
| CN105541115A (en) * | 2016-02-03 | 2016-05-04 | 同济大学 | Titanic acid and niobic acid compound glass ceramic as well as preparation method and application thereof |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110828168A (en) * | 2019-12-06 | 2020-02-21 | 电子科技大学 | Multilayer microcrystalline glass capacitor and preparation method thereof |
| CN110828168B (en) * | 2019-12-06 | 2021-09-24 | 电子科技大学 | Multilayer microcrystalline glass capacitor and preparation method thereof |
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Application publication date: 20170919 |