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
- Authority
- CN
- China
- Prior art keywords
- glass
- low
- glass ceramics
- low dielectric
- zno
- 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.)
- Expired - Fee Related
Links
- 239000002241 glass-ceramic Substances 0.000 title claims abstract description 15
- 229910010293 ceramic material Inorganic materials 0.000 claims abstract description 8
- 238000002360 preparation method Methods 0.000 claims abstract description 7
- 239000011521 glass Substances 0.000 claims description 42
- 239000006063 cullet Substances 0.000 claims description 12
- 239000000843 powder Substances 0.000 claims description 12
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 10
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 6
- 238000000498 ball milling Methods 0.000 claims description 6
- 239000012153 distilled water Substances 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 6
- 230000004927 fusion Effects 0.000 claims description 6
- 238000000227 grinding Methods 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 238000009413 insulation Methods 0.000 claims description 2
- 239000000155 melt Substances 0.000 claims description 2
- 239000000126 substance Substances 0.000 claims description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 abstract 2
- FUJCRWPEOMXPAD-UHFFFAOYSA-N Li2O Inorganic materials [Li+].[Li+].[O-2] FUJCRWPEOMXPAD-UHFFFAOYSA-N 0.000 abstract 1
- 229910052681 coesite Inorganic materials 0.000 abstract 1
- 229910052906 cristobalite Inorganic materials 0.000 abstract 1
- XUCJHNOBJLKZNU-UHFFFAOYSA-M dilithium;hydroxide Chemical compound [Li+].[Li+].[OH-] XUCJHNOBJLKZNU-UHFFFAOYSA-M 0.000 abstract 1
- 238000009472 formulation Methods 0.000 abstract 1
- 239000000377 silicon dioxide Substances 0.000 abstract 1
- 235000012239 silicon dioxide Nutrition 0.000 abstract 1
- 229910052682 stishovite Inorganic materials 0.000 abstract 1
- 229910052905 tridymite Inorganic materials 0.000 abstract 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 8
- 239000003989 dielectric material Substances 0.000 description 8
- 238000003825 pressing Methods 0.000 description 8
- 239000000463 material Substances 0.000 description 5
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 4
- 239000011230 binding agent Substances 0.000 description 4
- 238000005469 granulation Methods 0.000 description 4
- 230000003179 granulation Effects 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- 238000002156 mixing Methods 0.000 description 4
- 238000012856 packing Methods 0.000 description 4
- 229920002037 poly(vinyl butyral) polymer Polymers 0.000 description 4
- 238000005245 sintering Methods 0.000 description 4
- 238000005303 weighing Methods 0.000 description 4
- 206010037660 Pyrexia Diseases 0.000 description 3
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000000919 ceramic Substances 0.000 description 2
- 239000007772 electrode material Substances 0.000 description 2
- 239000006112 glass ceramic composition Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 229910052763 palladium Inorganic materials 0.000 description 2
- 229910052709 silver Inorganic materials 0.000 description 2
- 229910001252 Pd alloy Inorganic materials 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000009766 low-temperature sintering Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000010295 mobile communication Methods 0.000 description 1
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 1
- SWELZOZIOHGSPA-UHFFFAOYSA-N palladium silver Chemical compound [Pd].[Ag] SWELZOZIOHGSPA-UHFFFAOYSA-N 0.000 description 1
- 229910052573 porcelain Inorganic materials 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 229910001928 zirconium oxide Inorganic materials 0.000 description 1
- 229910000859 α-Fe Inorganic materials 0.000 description 1
Images
Classifications
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Ceramic Engineering (AREA)
- Crystallography & Structural Chemistry (AREA)
- Dispersion Chemistry (AREA)
- Glass Compositions (AREA)
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 |
Applications Claiming Priority (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 |
Publications (2)
Publication Number | Publication Date |
---|---|
CN1389416A CN1389416A (en) | 2003-01-08 |
CN1189411C true CN1189411C (en) | 2005-02-16 |
Family
ID=4745343
Family Applications (1)
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 |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN1189411C (en) |
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
Also Published As
Publication number | Publication date |
---|---|
CN1389416A (en) | 2003-01-08 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
CN101318815B (en) | Bismuth-based molybdenum-based microwave dielectric ceramic material sintered at ultra low temperature and manufacture of the same | |
CN102173587A (en) | Microcrystalline glass material for electronic substrate and preparation method thereof | |
CN101870584A (en) | Molybdenum-based ultralow-temperature sintering microwave medium ceramic materials and preparation method thereof | |
CN101367651B (en) | High-frequency low-temperature sintered ceramics dielectric material and method of manufacturing obtained electrical condenser | |
CN1872753A (en) | Ceramic material of microcrystalline glass, and preparation method | |
CN1909748A (en) | Rare earth electrode slurry of rare earth thick film circuit based on metal plate and its preparation technology | |
CN114315162B (en) | Leadless borosilicate glass-based ceramic composite material and preparation method thereof | |
CN102167514A (en) | Glass ceramic material for substrate and preparation method thereof | |
CN102718473B (en) | Bismuth-base microwave dielectric ceramic sintered at low temperature and preparation method thereof | |
CN103467099A (en) | LTCC material and preparation method thereof | |
CN1189410C (en) | Formula and prepn process of glass ceramics for HF chip inductor | |
CN1189411C (en) | Formula and prepn. process of glass ceramics with low dielectric constant and low loss | |
JP3737773B2 (en) | Dielectric ceramic composition | |
CN1267376C (en) | Composite material of glass ceramics cosintered by low temp | |
CN1219716C (en) | Dielectric ceramic composition | |
JP3737774B2 (en) | Dielectric ceramic composition | |
CN103232241A (en) | Ultralow-temperature-sintered composite microwave dielectric ceramic material and preparation method thereof | |
CN104016670B (en) | A kind of low-temperature sintering temperature-stabilized microwave medium ceramic material and preparation method thereof | |
CN103319177B (en) | Microwave dielectric ceramic Ba3WTiO8 with low-temperature sintering characteristic and preparation method thereof | |
CN101289312B (en) | Low sintering temperature and low loss microwave ceramic medium and preparation process thereof | |
CN103539449A (en) | Microwave dielectric ceramic BiNbW2O10 capable of being sintered at low temperature and preparation method thereof | |
CN1304894A (en) | Process for preparing cordierite-base microcrystal glass-ceramics medium material used for multi-layer inductor | |
CN1323969C (en) | Glass ceramic composition, electronic component therewith and laminated LC composite component | |
CN1317213C (en) | Dielectric material with low dielectric constant and low loss for microwave functional module and its prepn process | |
CN106810078A (en) | A kind of devitrified glass series microwave dielectric material of sintered at ultra low temperature and preparation method thereof |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
C10 | Entry into substantive examination | ||
SE01 | Entry into force of request for substantive examination | ||
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 | ||
C19 | Lapse of patent right due to non-payment of the annual fee | ||
CF01 | Termination of patent right due to non-payment of annual fee |