CN1113822C - Process for preparing microcrystal titanate glass medium - Google Patents
Process for preparing microcrystal titanate glass medium Download PDFInfo
- Publication number
- CN1113822C CN1113822C CN99124020A CN99124020A CN1113822C CN 1113822 C CN1113822 C CN 1113822C CN 99124020 A CN99124020 A CN 99124020A CN 99124020 A CN99124020 A CN 99124020A CN 1113822 C CN1113822 C CN 1113822C
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- glass
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- temperature
- mgo
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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
-
- 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
- C03C10/0036—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 SiO2, Al2O3 and a divalent metal oxide as main constituents
- C03C10/0045—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 SiO2, Al2O3 and a divalent metal oxide as main constituents containing SiO2, Al2O3 and MgO as main constituents
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Crystallography & Structural Chemistry (AREA)
- Dispersion Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Glass Compositions (AREA)
Abstract
The present invention provides a method for producing microwave dielectric materials with high frequency and low loss. The microwave dielectric material is microcrystalline glass with a MgO-Al2O3-SiO2-CeO2-TiO2 system, and the specific constituent range (by weight ratio) is as follows: 2 to 8W% of MgO, 10 to 19W% of Al2O3, 20 to 31W% of SiO2, 10 to 18W% of CeO2, and 30 to 50W% of TiO2. The temperature for melting glass is from 1480 to 1500 DEG C and is preserved for 3 hours, and the annealing temperature is 700 DEG C and is preserved for 1 hour. The crystallization temperature at the first stage is 10 DEG C higher or lower than 860 DEG C, and is 10 DEG C higher or lower than 1200 DEG C at the second stage. Under the frequency higher than 1GHz, microcrystalline glass produced with the method has the dielectric constant range from 15 to 20, and the dielectric loss is 9-6*10<-4>. Therefore, the microwave dielectric material has the advantages of applicability, high-frequency and low loss.
Description
The invention provides a kind of manufacture method of high-frequency low-consumption microwave dielectric material, belong to the microcrystal glass material field.A kind of method for preparing the titanate microcrystal glass material is provided or rather, this material frequency greater than the 1GHz condition under, specific inductivity is between 15～20, dielectric loss is between 6～9 * 10
-4
The present application people is once with regard to MgO-Al
2O
3-SiO
2-CeO
2-TiO
2System glass ceramics has proposed patent application (application number is 98110901.2) to Patent Office of the People's Republic of China, and the concrete compositing range of material (weight ratio) is:
MgO (5～10), Al
2O
3(18～25), SiO
2(28～35), CeO
2(13～19), TiO
2(18～27) with upper frequency, the specific inductivity of this material is greater than 9 less than 15 at 1GHZ, and dielectric loss is 6 * 10
-4Below.And enumerate German patent DE 2700333 contrivers and proposed MgO-Al
2O
3-SiO
2-LnO
2-TiO
2The system glass ceramics material.Concrete component is MgO (5～15), Al
2O
3(20～30), SiO
2(31～45), LnO
2(15～25), TiO
2(15～25), wherein LnO
2Be CeO
2, La
2O
3, Pr
2O
3, Nd
2O
3Four kinds of rare earth oxides.
The objective of the invention is, on the basis of contriver's original application patent (application number is 98110901.2), further improve the high-k components contents, promptly TiO
2Content bring up to greater than 30wt%, formation is with the titanate devitrified glass of rutile phase, α-Jin Qingshi phase and three kinds of principal crystalline phases of chevkinite phase, thereby make the specific inductivity of microcrystal glass material under frequency, bring up to 15～20, and dielectric loss remain on 6～9 * 10 greater than 1GHZ
-4
For achieving the above object, preparation method of the present invention is proposed.One of its feature is CeO
2Introducing, help TiO
2Separate out; Two of its feature is high-k component TiO
2Heavy dose of increasing forms the titanate glass system material, is principal crystalline phase with the rutile.
The present invention mainly adopts homemade industrial chemicals, and its devitrified glass consists of: (wt%)
MgO (2～8), Al
2O
3(10～19), SiO
2(20～31), CeO
2(10～18), TiO
2Compare with CN98110901.2 (30～50), TiO
2Content brings up to 30～50, the content of corresponding all the other compositions of minimizing from 18～27.Specific embodiment is: take by weighing raw materials such as magnesiumcarbonate, aluminium hydroxide, titanium dioxide, cerium oxide and quartz sand by proportioning, be mixed into glass batch.Admixtion is put into Platinum crucible, after 1480～1500 ℃ of fusions are incubated 3 hours, and castable.Send into annealing furnace, 700 ℃ of left and right sides insulation annealings 1 hour.Molded material divides the two-stage to heat-treat, and first section thermal treatment temp is 860 ± 10 ℃, and second section is 1200 ± 10 ℃, and soaking time was respectively 1.5 hours and 5 hours.
Characteristics of the present invention are to use the abundant and cheap industrial chemicals of raw material sources, only need control monovalent base metal content＜0.5% to get final product.
Two of characteristics are batchings, mix, and found, and manufacturing processedes such as crystallization all adopt conventional devitrified glass technology, and technology is simple, are easy to control.
Three of characteristics be can control effectively separate out high-k rutile mutually and the α-Jin Qingshi of low-dielectric loss mutually and the chevkinite phase, the serial devitrified glass of acquisition specific inductivity from 16～20.Salient features is as shown in table 1.
Further specify substantive distinguishing features of the present invention and obvious improvement below in conjunction with embodiment.Be noted that the present invention is confined to following each embodiment by no means.
Table 1 devitrified glass performance provided by the invention
Technical parameter product properties density of the present invention (g/cm
3)～3.1 specific inductivity (＞1GHz) 15～20 dielectric losses (＞1GHz)＜6～9 * 10
-4
Embodiment 1:
Glass is formed (wt%): SiO
2MgO Al
2O
3TiO
2CeO
2
31 2 19 30 18
With quartz sand, magnesiumcarbonate, aluminium hydroxide, cerium oxide and titanium dioxide is raw material, by said components weighing, mixing, then at 1510 ℃, fusion insulation 3 hours, the glass that melts casts in and is cooled to pristine glass in the mould fast, is cooled to room temperature in 1 hour in 700 ℃ of annealing.Glass after the die for molding rises to 860 ℃ from room temperature, handles through insulation in 1.5 hours, is warming up to 1200 ℃ of insulations 5 hours again, be cooled to room temperature the high frequency low loss devitrified glass microwave dielectric material.Specific inductivity is 15, dielectric loss＜6 * 10
-4, other performance is as shown in table 1.
Embodiment 2:
Glass is formed (wt%): SiO
2MgO Al
2O
3TiO
2CeO
2
25 3.5 16 40 14.5
With quartz sand, magnesiumcarbonate, aluminium hydroxide, cerium oxide and titanium dioxide is raw material, by said components weighing, mixing, then at 1500 ℃, fusion insulation 3 hours, the glass that melts casts in and is cooled to pristine glass in the mould fast, is cooled to room temperature in 1 hour in 700 ℃ of annealing.Glass after the die for molding rises to 860 ℃ from room temperature, handles through insulation in 1.5 hours, is warming up to 1200 ℃ of insulations 5 hours again, be cooled to room temperature the high frequency low loss devitrified glass microwave dielectric material.Specific inductivity is 18.5, dielectric loss＜7 * 10
-4, other performance is as shown in table 1.
Embodiment 3:
Glass is formed (wt%): SiO
2MgO Al
2O
3TiO
2CeO
2
20 8 12 50 10
With quartz sand, magnesiumcarbonate, aluminium hydroxide, cerium oxide and titanium dioxide is raw material, by said components weighing, mixing, then at 1480 ℃, fusion insulation 3 hours, the glass that melts casts in and is cooled to pristine glass in the mould fast, is cooled to room temperature in 1 hour in 700 ℃ of annealing.Glass after the die for molding rises to 860 ℃ from room temperature, handles through insulation in 1.5 hours, is warming up to 1200 ℃ of insulations 5 hours again, be cooled to room temperature the high frequency low loss devitrified glass microwave dielectric material.Specific inductivity is 20 ,/dielectric loss＜9 * 10
-4, other performance is as shown in table 1.
Claims (4)
1. the manufacture method of a high-frequency low-consumption microwave dielectric material, this material belongs to titanate devitrified glass system, it is characterized in that:
(1) weight percentage of each component is:
SiO
2 MgO Al
2O
3 TiO
2 CeO
2
20～31 2～8 12～19 30～50 10～18
(2) the glass smelting temperature is 1480～1500 ℃, is incubated 3 hours, and annealing temperature is 700 ℃, is incubated 1 hour;
(3) two-stage crystallization, first section crystallization temperature is 860 ± 10 ℃, second section crystallization temperature is 1200 ± 10 ℃.Soaking time was respectively 1.5 hours and 5 hours;
(4) this devitrified glass is made of rutile phase, α-Jin Qingshi phase and three kinds of main crystalline phases of chevkinite phase;
(5) improve TiO2 content, then increase the rutile phasor, improve specific inductivity.
2. manufacture method of glass-ceramic according to claim 1 is characterized in that:
(1) glass composition (wt%) is: SiO
2MgO Al
2O
3TiO
2CeO
2
31 2 19 30 18
(2) glass melting temperature is 1500 ℃, is incubated 3 hours
(3) first sections crystallization temperatures are 860 ℃, are incubated 1.5 hours; Second section crystallization temperature is 1200 ℃, is incubated 5 hours.
3. manufacture method of glass-ceramic according to claim 1 is characterized in that:
(1) glass composition (wt%) is: SiO
2MgO Al
2O
3TiO
2CeO
2
20 8 12 50 10
(2) glass melting temperature is 1480 ℃, is incubated 3 hours;
(3) first sections crystallization temperatures are 860 ℃, are incubated 1.5 hours; Second section crystallization temperature is 1200 ℃, is incubated 5 hours.
4. manufacture method of glass-ceramic according to claim 1, the bar that makes, sheet material, the material of sheet material and other geometrical shapies.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN99124020A CN1113822C (en) | 1999-11-17 | 1999-11-17 | Process for preparing microcrystal titanate glass medium |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN99124020A CN1113822C (en) | 1999-11-17 | 1999-11-17 | Process for preparing microcrystal titanate glass medium |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1250754A CN1250754A (en) | 2000-04-19 |
| CN1113822C true CN1113822C (en) | 2003-07-09 |
Family
ID=5283118
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN99124020A Expired - Fee Related CN1113822C (en) | 1999-11-17 | 1999-11-17 | Process for preparing microcrystal titanate glass medium |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1113822C (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP2782881B1 (en) * | 2011-11-24 | 2020-03-11 | Schott Ag | Glass-ceramic as dielectric in the high-frequency range |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1317213C (en) * | 2003-10-23 | 2007-05-23 | 浙江大学 | Dielectric material with low dielectric constant and low loss for microwave functional module and its prepn process |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4304603A (en) * | 1980-08-11 | 1981-12-08 | Corning Glass Works | Glass-ceramic compositions designed for radomes |
| US5013605A (en) * | 1988-08-11 | 1991-05-07 | Gritz David N | Cordierite-type glass-ceramic with controlled coloration |
| CN1202469A (en) * | 1998-06-16 | 1998-12-23 | 中国科学院上海硅酸盐研究所 | Process for producing high frequency low loss devitrified glass material |
-
1999
- 1999-11-17 CN CN99124020A patent/CN1113822C/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4304603A (en) * | 1980-08-11 | 1981-12-08 | Corning Glass Works | Glass-ceramic compositions designed for radomes |
| US5013605A (en) * | 1988-08-11 | 1991-05-07 | Gritz David N | Cordierite-type glass-ceramic with controlled coloration |
| CN1202469A (en) * | 1998-06-16 | 1998-12-23 | 中国科学院上海硅酸盐研究所 | Process for producing high frequency low loss devitrified glass material |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP2782881B1 (en) * | 2011-11-24 | 2020-03-11 | Schott Ag | Glass-ceramic as dielectric in the high-frequency range |
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| Publication number | Publication date |
|---|---|
| CN1250754A (en) | 2000-04-19 |
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