CN1189411C - Formula and prepn. process of glass ceramics with low dielectric constant and low loss - Google Patents
Formula and prepn. process of glass ceramics with low dielectric constant and low loss Download PDFInfo
- Publication number
- CN1189411C CN1189411C CNB021241333A CN02124133A CN1189411C CN 1189411 C CN1189411 C CN 1189411C CN B021241333 A CNB021241333 A CN B021241333A CN 02124133 A CN02124133 A CN 02124133A CN 1189411 C CN1189411 C CN 1189411C
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- Prior art keywords
- glass
- low
- glass ceramics
- low dielectric
- zno
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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
- C03C10/0054—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 containing PbO, SnO2, B2O3
-
- 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
- C03C4/00—Compositions for glass with special properties
- C03C4/14—Compositions for glass with special properties for electro-conductive glass
Abstract
The present invention relates to a formula and preparation method of nucleated glass ceramics with low dielectric constants and low loss, which belongs to the technical field of ceramic materials. The glass ceramics with low dielectric constants and low loss are prepared from components of the following proportion: 10 to 40 wt% of Zno, 2 to 30 wt% of B2O3, 10 to 80 wt% of SiO2 and 0.5 to 10 wt% of Li2O. The nucleated glass ceramics has the advantages of low dielectric constants (epsi<5, 1MHz) and low dielectric loss (tan delta<0.001 1MHz).
Description
Technical field
The present invention relates to ZnO-B
2O
3-SiO
2-Li
2The composition range of O microcrystalline glass in series pottery and preparation technology etc.Belong to the stupalith field.
Background technology
Electronics and IT products high frequency trend makes that the application prospect of multilayer high-frequency chip inductor (HF-MLCI) in the message area that with the mobile communication product is representative is wide day by day.Because the restriction of magnetic media material, the operating frequency of the lamellar inductor that uses is confined to the element system that 500MHz is following, inductance value is lower at present.And the inductor components and parts of big inductance quantity, superpower and very high frequency(VHF), ultra-high frequency become at present the focus of research and development both at home and abroad with stupalith.According to document announcement, the dielectric material that is used for the chip inductor of high-frequency range should have two characteristics: (1) low-k (ε=4-5,1MHz) and low dielectric loss (tg δ≤0.001,1MHz), in the hope of reducing the subsidiary electric capacity (C of chip inductor
p) and inductance value (L), thereby improve self-resonant frequency (SRF); (2) low fever's (burning altogether with metal inner electrode Ag, Ag-Pd below 1000 ℃).The major advantage of lamellar inductor (MLCI) has: volume is little; The reliability height; Magnetic shielding is good; Be suitable for surface mounting (SMT) and automatic assembling etc.Many electronic products all be unable to do without lamellar inductor, as notebook, cell-phone, beeper, large-screen color TV movement etc.The application of lamellar inductor comprises: (1) and the synthetic LC wave filter of electric capacity; (2) conduct exchanges obstructing instrument in active device (as transistor); (3) be used for matching circuit; (4) as anti-electromagnetic interference (EMI) wave filter.Make multilayer chip inductor and mainly contain two kinds of materials: electrode materials and dielectric material.Electrode materials generally adopts argent (Ag) or silver-palladium alloy (Ag-Pd), if adopt argent, dielectric material requires sintering below 900 ℃; If dielectric material then adopts silver-colored palladium electrode at 1000 ℃ of following sintering.From present industrialized present situation, the chip inductor dielectric material mainly comprises and is applied to 300MHz with the ferrite dielectric material of lower frequency and the stupalith and the ferritic matrix material that are applied to the low-k in the high-frequency range (500MHz-2GHz).As seen, high performance dielectric material with and low fever's technology be the key of high-frequency chip inductor device industrialization development.The research to the low fever of low Jie's porcelain both at home and abroad concentrates on two individual system, promptly " devitrified glass " is and " glass+pottery " is, is difficult to high densification and makes problems such as the dielectric material loss is excessive but still exist " devitrified glass " based material sintering temperature to be difficult to be lower than 900 ℃ and " glass+pottery " based material.
Summary of the invention
The devitrified glass ceramics that the purpose of this invention is to provide a kind of low-temperature sintering, low-dielectric loss and low-k.
Ceramic material of microcrystalline glass of the present invention is by ZnO, B
2O
3, SiO
2, Li
2Four kinds of one-tenth of O are grouped into.The proportioning of each composition is:
ZnO?10～40wt％ B
2O
3?2～30wt％ SiO
2?10～80wt％ Li
2O?0.5～10wt％
Its preparation process is:
1. the prescription scale gets chemical pure ZnO, B
2O
3, SiO
2, Li
2O ball milling 2～6 hours mixes after drying
In alumina crucible in 1400～1500 ℃ the insulation 1-3 hour, make its complete fusion and homogenizing
3. the melts in the crucible is quenched and obtained transparent glass cullet body in the distilled water
4. gained glass cullet body obtains the glass powder that median size is 0.5-1.5 μ m through wet ball grinding (using zirconium oxide balls), is
Ceramic material of microcrystalline glass of the present invention;
5, promptly get devitrified glass ceramics with under 850-900 ℃ temperature degree, being incubated 1-3 hour behind the ceramic material of microcrystalline glass powder compacting that makes.
The characteristics of ceramic material of microcrystalline glass of the present invention:
(1) the present invention adopts ZnO-B
2O
3-SiO
2-Li
2The glass ceramic material of O system preparation is at 850-900 ℃ of dense sintering, and sintered density reaches 98.5%, as shown in Figure 1;
(2) utilize the prepared devitrified glass ceramics of glass ceramic material of the present invention have low specific inductivity (ε＜5,1MHz) and dielectric loss (tan δ＜0.001,1MHz);
(3) ceramic material of microcrystalline glass of the present invention preparation can be well burns altogether with the silver and the silver-colored palladium electrode of low-resistivity.
(4) this material is applicable to and makes high-frequency multilayer chip inductor (MLCI), high frequency mixed unicircuit (HIC) ceramic substrate, electrode component and low temperature co-fired multilayer ceramic package casing (LTCC) etc.
Description of drawings
Fig. 1 is the sintered compact section.
Embodiment
Embodiment 1
Weighing ZnO (4wt%) by weight percentage, B
2O
3(15wt%), SiO
2(80wt%), Li
2O (1wt%).Through 3 hours batch mixings of ball milling evenly after, 70 ℃ of oven dry, the alumina crucible of packing into, fusion cast glass (1500 ℃ are incubated 2 hours) is quenched fused glass in the distilled water, obtains transparent glass cullet body.Through wet ball grinding (glass and proportion of ethanol are 1: 1,24 hours time), promptly obtaining median size of the present invention is the glass powder NO1 of 0.8 μ m with the glass cullet body.After granulation (ratio of powder and 5% polyvinyl butyral is 60/40) drying, dry-pressing formed at 1.5 tons pressure.The dry-pressing sheet is earlier 550 ℃ of binder removals (being incubated 4 hours), and (10 ℃ of rate of heating/min) also are incubated 2 hours, can obtain the devitrified glass ceramics of low-k and low-dielectric loss, and its performance is as shown in table 1 to be heated to 900 ℃ then rapidly.
Embodiment 2
Weighing ZnO (19.4wt%) by weight percentage, B
2O
3(4.2wt%), SiO
2(74.5wt%), Li
2O (1.9wt%).Through 3 hours batch mixings of ball milling evenly after, 70 ℃ of oven dry, the alumina crucible of packing into, fusion cast glass (1500 ℃ are incubated 2 hours) is quenched fused glass in the distilled water, obtains transparent glass cullet body.Through wet ball grinding (glass and proportion of ethanol are 1: 1,24 hours time), promptly obtaining median size of the present invention is the glass powder NO2 of 0.65 μ m with the glass cullet body.After granulation (ratio of powder and 5% polyvinyl butyral is 60/40) drying, dry-pressing formed at 1.5 tons pressure.The dry-pressing sheet is earlier 550 ℃ of binder removals (being incubated 4 hours), and (10 ℃ of rate of heating/min) also are incubated 2 hours, can obtain the devitrified glass ceramics of low-k and dielectric loss, and its performance is as shown in table 1 to be heated to 875 ℃ then rapidly.
Embodiment 3
Weighing ZnO (29wt%) by weight percentage, B
2O
3(20wt%), SiO
2(45wt%), Li
2O (6wt%).Through 3 hours batch mixings of ball milling evenly after, 70 ℃ of oven dry, the alumina crucible of packing into, fusion cast glass (1450 ℃ are incubated 2 hours) is quenched fused glass in the distilled water, obtains transparent glass cullet body.Through wet ball grinding (glass and proportion of ethanol are 1: 1,24 hours time), promptly obtaining median size of the present invention is the glass powder NO3 of 0.8 μ m with the glass cullet body.After granulation (ratio of powder and 5% polyvinyl butyral is 60/40) drying, dry-pressing formed at 1.5 tons pressure.The dry-pressing sheet is earlier 550 ℃ of binder removals (being incubated 4 hours), and (10 ℃ of rate of heating/min) also are incubated 2 hours, can obtain the devitrified glass ceramics of low-k and dielectric loss, and its performance is as shown in table 1 to be heated to 900 ℃ then rapidly.
Embodiment 4
Weighing ZnO (30wt%) by weight percentage, B
2O
3(25wt%), SiO
2(42wt%), Li
2O (3wt%).Through 3 hours batch mixings of ball milling evenly after, 70 ℃ of oven dry, the alumina crucible of packing into, fusion cast glass (1450 ℃ are incubated 2 hours) is quenched fused glass in the distilled water, obtains transparent glass cullet body.Through wet ball grinding (glass and proportion of ethanol are 1: 1,24 hours time), can obtain median size of the present invention is the glass powder NO4 of 0.8 μ m with the glass cullet body.After granulation (ratio of powder and 5% polyvinyl butyral is 60/40) drying, dry-pressing formed at 1.5 tons pressure.The dry-pressing sheet is earlier 550 ℃ of binder removals (being incubated 4 hours), and (10 ℃ of rate of heating/min) also are incubated 2 hours, can obtain the devitrified glass ceramics of low-k and dielectric loss, and its performance is as shown in table 1 to be heated to 900 ℃ then rapidly.
The performance of sintered sample in each example of table 1
The loss of sample shrinking percentage relative density K dielectric
(％) (％) (1MHz) (×10
-3，1MHz)
NO1 18.0 98.3 4.27 1.03
NO2 18.5 98.2 3.96 0.95
NO3 18.5 97.6 4.46 1.11
NO4 18.6 97.1 4.53 1.12
Claims (2)
1, a kind of low dielectric constant and low loss devitrified glass ceramics is characterized in that by ZnO, B
2O
3, SiO
2, Li
2Four kinds of one-tenth of O are grouped into, and the proportioning of each minute is:
ZnO 10～40wt％ B
2O
3 2～30wt％ SiO
2 10～80wt％ Li
2O 0.5～10wt％
2, according to the preparation method of the low dielectric constant and low loss devitrified glass ceramics of claim 1 record, it is characterized in that forming by the following step:
(1) gets chemical pure ZnO, B by the prescription scale
2O
3, SiO
2, Li
2O ball milling 2～6 hours mixes after drying
(2) in alumina crucible in 1400～1500 ℃ the insulation 1-3 hour, make its complete fusion and homogenizing
(3) melts in the crucible is quenched obtained transparent glass cullet body in the distilled water
(4) gained glass cullet body obtains the glass powder that median size is 0.5-1.5 μ m through wet ball grinding, is ceramic material of microcrystalline glass of the present invention;
(5) promptly get devitrified glass ceramics with under 850-900 ℃ temperature degree, being incubated 1-3 hour behind the ceramic material of microcrystalline glass powder compacting that makes.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB021241333A CN1189411C (en) | 2002-07-12 | 2002-07-12 | Formula and prepn. process of glass ceramics with low dielectric constant and low loss |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB021241333A CN1189411C (en) | 2002-07-12 | 2002-07-12 | Formula and prepn. process of glass ceramics with low dielectric constant and low loss |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1389416A CN1389416A (en) | 2003-01-08 |
| CN1189411C true CN1189411C (en) | 2005-02-16 |
Family
ID=4745343
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB021241333A Expired - Fee Related CN1189411C (en) | 2002-07-12 | 2002-07-12 | Formula and prepn. process of glass ceramics with low dielectric constant and low loss |
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Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2004238247A (en) * | 2003-02-05 | 2004-08-26 | Sumitomo Metal Mining Co Ltd | Glass ceramic composition and thick film glass paste composition |
| CN102603192B (en) * | 2012-02-29 | 2014-04-16 | 深圳光启创新技术有限公司 | Porous glass ceramic material, preparation method and prepared metamaterial substrate |
| CN106810078B (en) * | 2016-12-29 | 2019-07-16 | 中国科学院上海硅酸盐研究所 | A kind of devitrified glass series microwave dielectric material of sintered at ultra low temperature and preparation method thereof |
-
2002
- 2002-07-12 CN CNB021241333A patent/CN1189411C/en not_active Expired - Fee Related
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| Publication number | Publication date |
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