CN104961342B - A kind of devitrified glass insulating materials and preparation method thereof - Google Patents
A kind of devitrified glass insulating materials and preparation method thereof Download PDFInfo
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- CN104961342B CN104961342B CN201510317712.0A CN201510317712A CN104961342B CN 104961342 B CN104961342 B CN 104961342B CN 201510317712 A CN201510317712 A CN 201510317712A CN 104961342 B CN104961342 B CN 104961342B
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- insulating materials
- devitrified glass
- sintering aid
- glass insulating
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Abstract
The present invention relates to materials science field, it is desirable to provide a kind of devitrified glass insulating materials and preparation method thereof.The raw material of this kind of devitrified glass insulating materials is specific as follows by mass percentage：85~93% material of main part, 5~10% modifying agent, 2~5% sintering aid.The preparation method comprises the steps：Material of main part and modifying agent is taken to be mixed to prepare Iolite glass powder according to formula, again by obtained Iolite glass powder and sintering aid dispensing in proportion, it is granulated after ball milling mixing, pressurizes into base substrate, finally base substrate is sintered, that is, obtains the devitrified glass insulating materials of required preparation.Devitrified glass insulating materials synthesized by the present invention has excellent dielectric properties, can meet the application demands such as ultra-high-tension power transmission line insulation, microelectronic substrate.
Description
Technical field
The present invention is to belong to materials science field, more particularly to a kind of devitrified glass insulating materials and preparation method thereof.
Background technology
Cordierite is the MgO-Al of principal crystalline phase2O3-SiO2Microcrystalline glass in series has low thermal coefficient of expansion, high intensity, electric insulation
Functional, the features such as high-frequency loss is low, therefore in field extensive applications such as ultra-high-tension power transmission line insulation, microelectronics Packagings
Prospect.Studied in terms of being concentrated mainly on modified doping and process optimization at present, such as Wang JG exist《JapaneseJournal
of Applied Physics Part 1》" the Effect of CeO that the 8A phases page 5218 in 2007 deliver2on
microwavedielectric properties of MgO-Al2O3-SiO2In the texts of glass-ceramic " one, CeO is used2
The method of doping improves MgO-Al2O3-SiO2The quality factor of devitrified glass, reduce dielectric loss.Kirat G etc. exist
《Physica B-Condensed Materials》Volume 454 page 131 " Role of the Fe- delivered in 2014
substitution in dielectric behavior of the glass-ceramic cordierite
Mg2Al4Si5O18In the texts of system " one, it have studied Fe doping and cordierite mutually formed and the influence of dielectric properties.Ohsato H etc.
《Japanese Journal of Applied Physics》What 9 phase document number 09NF01 in 2011 were delivered
“Millimeter-wave dielectric properties of cordierite/indialite Glass
In the texts of Ceramics " one, the shadow of different crystallization temperatures and crystallization time to Iolite crystalline phase type, content and performance have studied
Ring.
However, MgO-Al2O3-SiO2Microcrystalline glass in series still suffers from crystallization and sintering temperature high (>=1100 DEG C), microstructure
Not fine and close, easy to form sub- warm transition state μ-Iolite, phase in version causes problems of crack.
The content of the invention
It is a primary object of the present invention to overcome deficiency of the prior art, there is provided one kind is by adding sintering aid and modification
Agent improves devitrified glass insulating materials of performance and preparation method thereof.In order to solve the above technical problems, the solution party of the present invention
Case is：
A kind of devitrified glass insulating materials is provided, the formula of its raw material by mass percentage is described in detail below：
Material of main part：85~93%；
Modifying agent：5~10%；
Sintering aid：2~5%；
The material of main part is by MgO, Al2O3And SiO2Composition, the modifying agent is by ZnO, B2O3、TiO2Composition, it is described to help
Burning agent is La2O3-B2O3；Wherein, every kind of oxide or compound account for formula gross mass in material of main part, modifying agent and sintering aid
Percentage be：
In the present invention, the sintering aid La2O3-B2O3In, each component and its mass content are respectively：
La2O3：40~50%；
H3BO3：50~60%.
Method for preparing a kind of described devitrified glass insulating materials is provided, specifically includes following step：
Step A：MgO, Al are taken according to formula2O3、SiO2、ZnO、H3BO3And TiO2Compound is configured to, that is, completes main body material
The mixing of material and modifying agent；
Wherein, B2O3With H3BO3Form introduces, B2O3With the H of introducing3BO3Mol ratio is 1:2；
Step B：After adding ethanol in the compound obtained to step A, ball milling mixing 2h, drying, aluminum oxide is then charged into
1~3h is founded at 1400~1500 DEG C in crucible, the glass water quenching melted is crushed, reuses planetary ball mill ball
Mill obtains Iolite glass powder；
Step C：La is taken according to formula2O3And H3BO3Batch mixing is configured to, ball milling 4h is carried out to batch mixing, is then placed in aluminum oxide
In crucible, 1~2h is heat-treated at 600~650 DEG C, that is, obtains sintering aid；
Wherein, La2O3And H3BO3When being prepared, B2O3With H3BO3Form introduces, B2O3With the H of introducing3BO3Mol ratio is
1:2；
Step D：By sintering aid made from Iolite glass powder made from step B and step C, dispensing, ball milling mix in proportion
After closing 18~24h, it is granulated, base substrate is prepared in extrusion forming；Base substrate is finally sintered into 1~4h at 850~950 DEG C, produced
To the devitrified glass insulating materials of required preparation.
In the present invention, the base substrate that base substrate made of extrusion forming is a diameter of 12mm in the step D, thickness is 6mm.
Compared with prior art, the beneficial effects of the invention are as follows：
Due to La2O3-B2O3Auxiliary agent softening point is relatively low, is melted in temperature-rise period, forms glass liquid phase, and it is blue or green to reduce α-violet
The crystallization and sintering temperature (≤950 DEG C) of stone devitrified glass, promote α-Iolite nucleus to be formed and grown up, reduce sub- warm transition state
The generation of μ-Iolite, devitrified glass deformation and problem of Cracking are avoided, promotes devitrified glass sintering densification, so as to improve it
Electromechanical properties.In addition, introduce TiO2To adjust the cordierite glass-ceramic coefficient of expansion and temperature coefficient, and nucleus can be used as
Agent, promote material crystallization.Synthesized devitrified glass insulating materials has excellent dielectric properties：Permittivity ε ≈ 5.1~
5.6 (1MHz), dielectric loss tan δ<0.8×10-3(1MHz), insulation resistivity ρ>3×1013Ω cm, low-expansion coefficient (4
~5 × 10-6K-1).Obtained devitrified glass insulating materials can meet that ultra-high-tension power transmission line insulation, microelectronic substrate etc. are applied
Demand.
Embodiment
The present invention is described in further detail with reference to embodiment：
The present invention is more fully understood in the professional and technical personnel that the following examples can make this professional, but not with any side
The formula limitation present invention.
Embodiment 1：
The percentage that every kind of oxide or compound account for gross mass in described cordierite body material and modifying agent is：
10%MgO, 35%Al2O3,45SiO2, 1.5%ZnO, 2%B2O3, 4%TiO2, 2.5%La2O3-B2O3；Described La2O3-B2O3
Each component and its mass content are respectively in sintering aid：45%La2O3And 55%H3BO3。
The preparation method of the glass ceramics composite insulating material, is followed the steps below successively：
(1) MgO, Al are weighed2O3、SiO2、ZnO、H3BO3And TiO2(B2O3With H3BO3Form introduces, B2O3With introducing
H3BO3Mol ratio is 1:2).Compound adds ethanol, ball milling mixing 2h, in 70 DEG C of drying, is fitted into alumina crucible in temperature
1500 DEG C are founded 2h, and the glass water quenching melted is crushed, and are reused planetary ball mill ball milling and are obtained glass powder.
(2) La is weighed2O3And H3BO3(B2O3With H3BO3Form introduces, B2O3With the H of introducing3BO3Mol ratio is 1:2)；Ball
Batch mixing 4h is ground, is then placed in alumina crucible and is heat-treated 2h at 600 DEG C, that is, obtain La2O3-B2O3Sintering aid.
(3) by La made from glass powder made from step (1) and step (2)2O3-B2O3Sintering aid dispensing in proportion, ball
Mill mixing 20h, is granulated, extrusion forming, prepares diameter 12mm, thickness 6mm base substrate；2h is sintered at 890 DEG C, produces the present invention
The devitrified glass insulating materials.
According to devitrified glass insulating materials made from aforementioned formula and step, material is without cracking and problem on deformation, Ge Xiangxing
Can index be：Permittivity ε=5.49 (1MHz), dielectric loss tan δ=0.78 × 10-3(1MHz), insulation resistivity ρ=
3.08×1013Ω cm, the coefficient of expansion=4.3 × 10-6K-1(20-300℃)。
Embodiment 2：
The percentage that every kind of oxide or compound account for gross mass in described cordierite body material and modifying agent is：
12%MgO, 25%Al2O3,48SiO2, 1%ZnO, 1%B2O3, 8%TiO2, 5%La2O3-B2O3；Described La2O3-B2O3Help burning
Each component and its mass content are respectively in agent：50%La2O3And 50%H3BO3。
The preparation method of the glass ceramics composite insulating material, is followed the steps below successively：
(1) MgO, Al are weighed2O3、SiO2、ZnO、H3BO3And TiO2(B2O3With H3BO3Form introduces, B2O3With introducing
H3BO3Mol ratio is 1:2).Compound adds ethanol, ball milling mixing 2h, in 80 DEG C of drying, is fitted into alumina crucible in temperature
1450 DEG C are founded 1h, and the glass water quenching melted is crushed, and are reused planetary ball mill ball milling and are obtained glass powder.
(2) La is weighed2O3And H3BO3(B2O3With H3BO3Form introduces, B2O3With the H of introducing3BO3Mol ratio is 1:2)；Ball
Batch mixing 4h is ground, is then placed in alumina crucible and is heat-treated 1h at 650 DEG C, obtain La2O3-B2O3Sintering aid.
(3) by La made from glass powder made from step (1) and step (2)2O3-B2O3Sintering aid dispensing in proportion, ball
Mill mixing 18h, is granulated, extrusion forming, prepares diameter 12mm, thickness 6mm base substrate；1h is sintered at 850 DEG C, produces the present invention
The devitrified glass insulating materials.
According to devitrified glass insulating materials made from aforementioned formula and step, material is without cracking and problem on deformation, Ge Xiangxing
Can index be：Dielectric constant=5.61 (1MHz), dielectric loss tan δ=0.63 × 10-3(1MHz), insulation resistivity ρ=4.18
×1013Ω cm, the coefficient of expansion=4.6 × 10-6K-1(20-300℃)。
Embodiment 3：
The percentage that every kind of oxide or compound account for gross mass in described cordierite body material and modifying agent is：
15%MgO, 26%Al2O3,52SiO2, 2%ZnO, 1%B2O3, 2%TiO2, 2%La2O3-B2O3；Described La2O3-B2O3Help burning
Each component and its mass content are respectively in agent：40%La2O3And 60%H3BO3。
The preparation method of the glass ceramics composite insulating material, is followed the steps below successively：
(1) MgO, Al are weighed2O3、SiO2、ZnO、H3BO3And TiO2(B2O3With H3BO3Form introduces, B2O3With introducing
H3BO3Mol ratio is 1:2).Compound adds ethanol, ball milling mixing 2h, in 75 DEG C of drying, is fitted into alumina crucible in temperature
1450 DEG C are founded 3h, and the glass water quenching melted is crushed, and are reused planetary ball mill ball milling and are obtained glass powder.
(2) La is weighed2O3And H3BO3(B2O3With H3BO3Form introduces, B2O3With the H of introducing3BO3Mol ratio is 1:2)；Ball
Batch mixing 4h is ground, is then placed in alumina crucible and is heat-treated 1.5h at a temperature of 630 DEG C, obtain La2O3-B2O3Sintering aid.
(3) by La made from glass powder made from step (1) and step (2)2O3-B2O3Sintering aid dispensing in proportion, ball
Mill mixing 24h, is granulated, extrusion forming, prepares diameter 12mm, thickness 6mm base substrate；4h is sintered at 950 DEG C, produces the present invention
The devitrified glass insulating materials.
According to devitrified glass insulating materials made from aforementioned formula and step, material is without cracking and problem on deformation, Ge Xiangxing
Can index be：Dielectric constant=5.31 (1MHz), dielectric loss tan δ=0.71 × 10-3(1MHz), insulation resistivity ρ=2.20
×1013Ω cm, the coefficient of expansion=4.3 × 10-6K-1(20-300℃)。
Embodiment 4：
The percentage that every kind of oxide or compound account for gross mass in described cordierite body material and modifying agent is：
12%MgO, 32.5%Al2O3,45SiO2, 2ZnO, 1.5%B2O3, 5%TiO2, 2%La2O3-B2O3；Described La2O3-B2O3Help
Burning each component and its mass content in agent is respectively：45%La2O3And 55%H3BO3。
The preparation method of the glass ceramics composite insulating material, is followed the steps below successively：
(1) MgO, Al are weighed2O3、SiO2、ZnO、H3BO3And TiO2(B2O3With H3BO3Form introduces, B2O3With introducing
H3BO3Mol ratio is 1:2).Compound adds ethanol, ball milling mixing 2h, in 80 DEG C of drying, is fitted into alumina crucible in temperature
1400 DEG C are founded 2h, and the glass water quenching melted is crushed, and are reused planetary ball mill ball milling and are obtained glass powder.
(2) La is weighed2O3And H3BO3(B2O3With H3BO3Form introduces, B2O3With the H of introducing3BO3Mol ratio is 1:2)；Ball
Batch mixing 4h is ground, is then placed in alumina crucible and is heat-treated 2h at 600 DEG C, obtain La2O3-B2O3Sintering aid.
(3) by La made from glass powder made from step (1) and step (2)2O3-B2O3Sintering aid dispensing in proportion, ball
Mill mixing 20h, is granulated, extrusion forming, prepares diameter 12mm, thickness 6mm base substrate；1h is sintered at 875 DEG C, produces the present invention
The devitrified glass insulating materials.
According to devitrified glass insulating materials made from aforementioned formula and step, material is without cracking and problem on deformation, Ge Xiangxing
Can index be：Dielectric constant=5.40 (1MHz), dielectric loss tan δ=0.63 × 10-3(1MHz), insulation resistivity ρ=4.28
×1013Ω cm, the coefficient of expansion=4.3 × 10-6K-1(20-300℃)。
Finally it should be noted that listed above is only specific embodiment of the invention.It is clear that the invention is not restricted to
Above example, there can also be many variations.One of ordinary skill in the art can directly lead from present disclosure
All deformations for going out or associating, are considered as protection scope of the present invention.
Claims (2)
1. a kind of devitrified glass insulating materials, it is characterised in that the formula of its raw material by mass percentage is described in detail below：
Material of main part：85~93%；
Modifying agent：5~10%；
Sintering aid：2~5%；
The material of main part is by MgO, Al2O3And SiO2Composition, the modifying agent is by ZnO, B2O3、TiO2Composition；The sintering aid
For La2O3-B2O3, each component and its mass content are respectively：
La2O3：40~50%；
H3BO3：50~60%；
Wherein, in material of main part, modifying agent and sintering aid every kind of oxide or compound account for formula gross mass percentage be：
The method for preparing the devitrified glass insulating materials, specifically includes following step：
Step A：MgO, Al are taken according to formula2O3、SiO2、ZnO、H3BO3And TiO2Be configured to compound, that is, complete material of main part and
The mixing of modifying agent；
Wherein, B2O3With H3BO3Form introduces, B2O3With the H of introducing3BO3Mol ratio is 1:2；
Step B：After adding ethanol in the compound obtained to step A, ball milling mixing 2h, drying, alumina crucible is then charged into
In found 1~3h at 1400~1500 DEG C, the glass water quenching melted is crushed, planetary ball mill ball milling is reused and obtains
To Iolite glass powder；
Step C：La is taken according to formula2O3And H3BO3Batch mixing is configured to, ball milling 4h is carried out to batch mixing, is then placed in alumina crucible
In, 1~2h is heat-treated at 600~650 DEG C, that is, obtains sintering aid；
Wherein, La2O3And H3BO3When being prepared, B2O3With H3BO3Form introduces, B2O3With the H of introducing3BO3Mol ratio is 1:2；
Step D：By the dispensing in proportion of sintering aid made from Iolite glass powder made from step B and step C, ball milling mixing 18
After~24h, it is granulated, base substrate is prepared in extrusion forming；Base substrate is finally sintered into 1~4h at 850~950 DEG C, that is, obtains institute
The devitrified glass insulating materials that need to be prepared.
2. devitrified glass insulating materials according to claim 1, it is characterised in that described to prepare devitrified glass insulating materials
Method in, in step D extrusion forming made of base substrate be a diameter of 12mm, thickness be 6mm base substrate.
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| US3450546A (en) * | 1966-05-26 | 1969-06-17 | Corning Glass Works | Transparent glass-ceramic articles and method for producing |
| CN1609025A (en) * | 2003-10-23 | 2005-04-27 | 浙江大学 | Dielectric material with low dielectric constant and low loss for microwave functional module and its prepn process |
| CN102167514A (en) * | 2011-01-20 | 2011-08-31 | 电子科技大学 | Microcrystalline glass ceramic material for substrate and preparation method of microcrystalline glass ceramic material |
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|---|---|---|---|---|
| JP2691263B2 (en) * | 1989-08-11 | 1997-12-17 | 株式会社オハラ | Transparent crystallized glass |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3450546A (en) * | 1966-05-26 | 1969-06-17 | Corning Glass Works | Transparent glass-ceramic articles and method for producing |
| CN1609025A (en) * | 2003-10-23 | 2005-04-27 | 浙江大学 | Dielectric material with low dielectric constant and low loss for microwave functional module and its prepn process |
| CN102167514A (en) * | 2011-01-20 | 2011-08-31 | 电子科技大学 | Microcrystalline glass ceramic material for substrate and preparation method of microcrystalline glass ceramic material |
Non-Patent Citations (1)
| Title |
|---|
| 低温共烧微波介质陶瓷及其器件的研究进展;杨辉等;《硅酸盐学报》;20080630;第36卷(第6期);第866-876页 * |
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