CN1275901C - Low temperature sintered microwave dielectric ceramic with medium dielectric constant and its prepn process - Google Patents
Low temperature sintered microwave dielectric ceramic with medium dielectric constant and its prepn process Download PDFInfo
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- 238000000034 method Methods 0.000 title abstract description 7
- 239000000919 ceramic Substances 0.000 title abstract description 6
- 239000000463 material Substances 0.000 claims abstract description 41
- 238000005245 sintering Methods 0.000 claims abstract description 26
- 238000001354 calcination Methods 0.000 claims abstract description 17
- 238000000498 ball milling Methods 0.000 claims abstract description 15
- 239000000843 powder Substances 0.000 claims abstract description 10
- 238000005516 engineering process Methods 0.000 claims abstract description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 42
- 150000001875 compounds Chemical class 0.000 claims description 30
- 239000002253 acid Substances 0.000 claims description 21
- 230000001476 alcoholic effect Effects 0.000 claims description 21
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 14
- 238000012856 packing Methods 0.000 claims description 14
- 238000005096 rolling process Methods 0.000 claims description 13
- 229910010413 TiO 2 Inorganic materials 0.000 claims description 11
- 238000002156 mixing Methods 0.000 claims description 11
- 238000009766 low-temperature sintering Methods 0.000 claims description 10
- 238000002360 preparation method Methods 0.000 claims description 9
- 239000000203 mixture Substances 0.000 claims description 8
- 229910052797 bismuth Inorganic materials 0.000 claims description 7
- 238000009413 insulation Methods 0.000 claims description 7
- 239000005388 borosilicate glass Substances 0.000 claims description 5
- ZFZQOKHLXAVJIF-UHFFFAOYSA-N zinc;boric acid;dihydroxy(dioxido)silane Chemical compound [Zn+2].OB(O)O.O[Si](O)([O-])[O-] ZFZQOKHLXAVJIF-UHFFFAOYSA-N 0.000 claims description 5
- 239000002994 raw material Substances 0.000 claims description 4
- 239000000654 additive Substances 0.000 claims description 3
- 230000000996 additive effect Effects 0.000 claims description 3
- 239000000428 dust Substances 0.000 claims description 3
- 239000008188 pellet Substances 0.000 claims description 3
- 239000004615 ingredient Substances 0.000 claims description 2
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 abstract description 7
- 229910052709 silver Inorganic materials 0.000 abstract description 7
- 239000004332 silver Substances 0.000 abstract description 7
- 239000011521 glass Substances 0.000 abstract description 4
- 230000002349 favourable effect Effects 0.000 abstract description 2
- WMWLMWRWZQELOS-UHFFFAOYSA-N bismuth(iii) oxide Chemical compound O=[Bi]O[Bi]=O WMWLMWRWZQELOS-UHFFFAOYSA-N 0.000 abstract 4
- 229910007472 ZnO—B2O3—SiO2 Inorganic materials 0.000 abstract 2
- 229910007676 ZnO—SiO2 Inorganic materials 0.000 abstract 2
- 239000013078 crystal Substances 0.000 abstract 2
- 230000001105 regulatory effect Effects 0.000 abstract 2
- 229910002971 CaTiO3 Inorganic materials 0.000 abstract 1
- 238000003980 solgel method Methods 0.000 abstract 1
- 230000002195 synergetic effect Effects 0.000 abstract 1
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 13
- 239000012071 phase Substances 0.000 description 11
- 239000011787 zinc oxide Substances 0.000 description 6
- 238000011160 research Methods 0.000 description 5
- 238000005303 weighing Methods 0.000 description 4
- 239000010953 base metal Substances 0.000 description 3
- 229910010293 ceramic material Inorganic materials 0.000 description 3
- 239000010949 copper Substances 0.000 description 3
- 239000007791 liquid phase Substances 0.000 description 3
- 238000002844 melting Methods 0.000 description 3
- 230000008018 melting Effects 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 229910052745 lead Inorganic materials 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000002002 slurry Substances 0.000 description 2
- 229910052718 tin Inorganic materials 0.000 description 2
- 229910052725 zinc Inorganic materials 0.000 description 2
- 239000011701 zinc Substances 0.000 description 2
- 229910052726 zirconium Inorganic materials 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 229910000416 bismuth oxide Inorganic materials 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- TYIXMATWDRGMPF-UHFFFAOYSA-N dibismuth;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Bi+3].[Bi+3] TYIXMATWDRGMPF-UHFFFAOYSA-N 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 238000003411 electrode reaction Methods 0.000 description 1
- 229910052742 iron Inorganic materials 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
- 229910052758 niobium Inorganic materials 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 229910052573 porcelain Inorganic materials 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000006104 solid solution Substances 0.000 description 1
- 238000013517 stratification Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 238000009736 wetting Methods 0.000 description 1
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- Inorganic Insulating Materials (AREA)
- Compositions Of Oxide Ceramics (AREA)
Abstract
The present invention relates to low-temperature sintered microwave dielectric ceramics with medium dielectric constants and a preparing method thereof. Ca(Li<1/3>Nb<2/3>)O3 and CaTiO3 are used as main crystal phases, and Bi2O3, ZnO and ZnO-B2O3-SiO2 glass powder which is prepared by a sol-gel method are used as sintering aids. The present invention has the advantages that the sintering temperature of the materials are lowered by the synergistic effect of Bi2O3, ZnO and ZnO-B2O3-SiO2 glass powder, various microwave dielectric properties are synthetically regulated and controlled, a two-time calcining technology and a two-time ball milling technology are adopted, the method is favorable to fully synthesize main crystal phases, and the powder characteristics are improved. When sintered at about 900 DEG C, the low-temperature sintered microwave dielectric ceramics have good microwave dielectric properties: epsilon<r> is from 30 to 45, Q*f is from 6000 to 10000 GHz, and the frequency temperature coefficient can be regulated. The materials have stable technology and good reproducibility, and can be cofired with silver electrodes. The materials of the present invention can be used for designing and producing multilayer microwave frequency devices such as multilayer filters, diplexers, antennae, baluns, etc.
Description
Technical field
The present invention relates to a kind of medium dielectric constant microwave medium low-temperature sintering microwave medium pottery and preparation method thereof, belong to materials science field.
Background technology
Present mobile communication and WLAN (wireless local area network) are popularized rapidly in the world, and develop towards miniaturization, lightweight, high frequencyization, integrated, high reliability and low-cost direction.This also proposes higher requirement to the microwave circuit components and parts based on microwave-medium ceramics, and the miniaturization of microwave circuit components and parts, high frequencyization have become the main flow of technical development.
The approach that realizes the microwave device miniaturization mainly contains two: explore the multilayered structure design of high-permittivity microwave medium material and microwave device.The preparation of multiplayer microwave chip microwave device; need microwave dielectric ceramic materials to burn altogether with the metal of high conductivity; and consider that from economy and environment protection angle using lower silver (Ag), the copper base metals such as (Cu) of fusing point is ideal as electrode materials.At present, the microwave-medium ceramics sintering temperature of industrialization is all than higher, generally at 1200 ℃～1500 ℃, as BaTi
4O
9, Ba
2Ti
9O
20, (Zn, Sn) TiO
4, (Pb, Ca) (Fe, Nb, Zr) O
3, Ba (Ni
1/3Nb
2/3) O
3, (Pb, Ca) (Zr, Ti) O
3, their sintering temperature is higher than the fusing point of Ag (906 ℃), Cu (1064 ℃) far away.In order to realize burning altogether, must seek low-temp sintered material or existing material carry out low temperatureization with base metal.The low-temperature sintering microwave medium pottery be beneficial to components and parts multiple stratification, cut down the consumption of energy and electrodes in base metal burns altogether, thereby reduce production costs, mentioned the research schedule by Chinese scholars.
Reduce sintering temperature three kinds of methods are arranged usually: 1. an amount of sintering aid-low melting point oxide and the low melting glass of admixture, carry out the liquid phase reactive sintering; 2. adopt chemical method to produce the high powder of surfactivity; 3. adopt the thin material of granularity as far as possible or select the lower material of intrinsic sintering sintering temperature for use.At present, aspect low-temperature sintering, mainly concentrate on the research of sintering aid selection and optimization aspect.In the mass transfer in liquid phase sintering process, because glass or oxide compound fusing form liquid phase, wetting parcel solid particulate promotes grain growth; Perhaps low melting point oxide enters the lattice replacement, forms substitutional solid solution, utilizes the vacant densification that can promote porcelain body.Some progress have been obtained in low temperature microwave medium ceramic material research, as at BaO-TiO
2-WO
3The middle SiO that adds
2, B
2O
3, ZnO-B
2O
3Deng sintering aid, sintering temperature can drop to 1000 ℃; (Zn, Sn) TiO
4Middle NiO, ZnO, the Fe of adding
2O
3Deng oxide compound, can make sintering temperature be reduced to 1400 ℃, add BaCuO simultaneously
2+ CuO can reach 97% density at 1000 ℃ of sintering.In addition, many scientific and technical personnel BiNbO low to intrinsic sintering temperature
4, Bi-Ca-Nb-O, Bi-Ca-Zn-Nb-O and leaded complex perovskite structure material, by adding CuO, V
2O
5Etc. the eutectoid point oxide compound, can make the sintering temperature of material be reduced to 920 ℃.At present, the material system of research is owing to the reason of material self character, have that sintering temperature height, material at low temperatureization and dielectric properties can not have both, slurry batching difficulty, mix silver, with problem such as silver electrode reaction, the low-temperature sintered microwave dielectric ceramic material of real industrialization is seldom.
Summary of the invention
The objective of the invention is to cater to the miniaturization of tracking exchage microwave frequency, high frequencyization needs, propose a kind of medium dielectric constant microwave medium low-temperature sintering microwave medium pottery and preparation method thereof, with Ca[(Li
1/3Nb
2/3)
1-xTi
x] O
3-δSystem is a research object, adopts Bi
2O
3, ZnO and ZBS be sintering aid, the collaborative sintering temperature that reduces pottery is adjusted principal crystalline phase and is formed, the microwave dielectric property of comprehensive regulation material obtains below 900 ℃ the low-temperature sintering microwave medium pottery that can burn altogether with silver electrode, and forms industrialization.
A kind of low-temperature sintering microwave medium material and preparation method that the present invention proposes comprise following content:
1. according to following component proportion ingredient:
Ca[(Li
1/3Nb
2/3)
1-xTi
x] O
3-8, x=0.1～0.5 wherein
With desired raw material CaCO
3, Li
2CO
3, Nb
2O
5, TiO
2The weight summation be 100%, the weight percent of additive is:
Bismuth oxide (Bi
2O
3): 2～6wt%
Zinc oxide (ZnO): 0～8wt%
Zinc borosilicate glass powder (ZBS): 5～15%
2. with above-mentioned CaCO
3, Li
2CO
3, Nb
2O
5, TiO
2By proportioning component batching; By compound and alcoholic acid weight ratio is 1: (1～1.5), add ethanol, mix 16～24h at rotating speed 300r/min rolling ball milling, 60～80 ℃ of oven dry are with the compound of the oven dry alumina crucible of packing into, at 800～950 ℃ of calcining 2～4h down, synthetic principal crystalline phase.
3. once the calcining material adds 2～6wt%Bi
2O
3, 0～8wt%ZnO, be 1 by compound and alcoholic acid weight ratio: (1～1.5), add ethanol, mix 16～24h, 60～80 ℃ of oven dry at rotating speed 300r/min rolling ball milling.With the compound alumina crucible of packing into of oven dry, at 700～850 ℃ of calcining 2～4h down.Calcining pellet abrasive dust is broken to median size 1 μ m, and is standby.
4. the secondary clacining material adds 5～15%ZBS, by compound and alcoholic acid weight ratio is 1: (1～1.5), add ethanol, mix 16～24h at rotating speed 300r/min rolling ball milling, be pressed into the knobble of diameter 25mm, thickness 10～15mm at 80～120Mpa, at 850～920 ℃ of following sintering, insulation 2～6h promptly obtains material of the present invention.
The present invention who adopts above-mentioned prescription and technology to form can burn with silver electrode below 900 ℃ altogether, has excellent microwave dielectric properties: ε
r=30～45, Qf=6000～10000GHz, resonant frequency is at 3～4GHz, and frequency-temperature coefficient is adjustable.This material is a kind of material that has development prospect, invested in plant production.The present invention has following characteristics:
1. adopt ZnO, Bi
2O
3, the collaborative sintering temperature that reduces of ZBS sintering aid, every microwave dielectric property of comprehensive coordination material, frequency-temperature coefficient effectively is controlled in the use range;
2. adopt secondary clacining and secondary ball milling process system, fully synthetic principal crystalline phase improves powder characteristics, is beneficial to the slurry preparation;
3. stable, the favorable reproducibility of material technology can burnt with silver electrode below 900 ℃ altogether, has dropped into the industrialization of multiplayer microwave ceramic filter and has produced.
Embodiment
Below in conjunction with embodiment the present invention is further described.
Embodiment 1:
According to x=0.2, CaCO in molar ratio in the principal crystalline phase expression formula
3: Li
2CO
3: Nb
2O
5: TiO
2=1.000: weighing in 0.1333: 0.2667: 0.2000 is 1: 1.2 by compound and alcoholic acid weight ratio, adds ethanol, is 300r/min rolling ball milling 24h at rotating speed, and 80 ℃ of oven dry, the alumina crucible of packing into is calcined 4h down at 905 ℃, synthetic principal crystalline phase; Once the calcining material adds 5wt%Bi
2O
3, be 1: 1.2 by compound and alcoholic acid weight ratio, add ethanol, at rotating speed 300r/min barreling batch mixing 24h, 80 ℃ of oven dry, the alumina crucible of packing into is calcined 2h down at 750 ℃; The secondary clacining material adds the ZBS of 8wt%, is 1: 1.2 by compound and alcoholic acid weight ratio, adds ethanol, at rotating speed 300r/min barreling batch mixing 24h, be pressed into the nahlock of diameter 25mm, thickness 12mm at 80Mpa, at 906 ℃ of following sintering, insulation 3.7h promptly obtains material of the present invention.Dielectric properties are: ε
r=37.77, Qf=9028GHz, resonant frequency f=3.4318GHz, frequency-temperature coefficient τ
f=3.89ppm/ ℃.
Embodiment 2:
According to x=0.22, CaCO in molar ratio in the principal crystalline phase expression formula
3: Li
2CO
3: Nb
2O
5: TiO
2=1.000: weighing in 0.1300: 0.2600: 0.2200 is 1: 1.2 by compound and alcoholic acid weight ratio, adds ethanol, is 300r/min rolling ball milling 24h at rotating speed, and 80 ℃ of oven dry, the alumina crucible of packing into is calcined 4h down at 905 ℃, synthetic principal crystalline phase; Once the calcining material adds 5wt%Bi
2O
3, be 1: 1.2 by compound and alcoholic acid weight ratio, add ethanol, at rotating speed 300r/min barreling batch mixing 24h, 80 ℃ of oven dry, the alumina crucible of packing into is calcined 2h down at 750 ℃; The secondary clacining material adds the ZBS of 8wt%, is 1: 1.2 by compound and alcoholic acid weight ratio, adds ethanol, at rotating speed 300r/min barreling batch mixing 24h, is pressed into the nahlock of diameter 25mm, thickness 12.4mm at 80Mpa.Become to burn under 906 ℃, insulation 3.7h promptly obtains material of the present invention.Dielectric properties are: ε
r=35.45, Qf=6944GHz, resonant frequency f=3.7997GHz, frequency-temperature coefficient τ
f=11.4ppm/ ℃.
Embodiment 3:
According to x=0.25, CaCO in molar ratio in the principal crystalline phase expression formula
3: Li
2CO
3: Nb
2O
5: TiO
2=1.000: 0.125: 0.25: 0.25 batch weighing is 1: 1.2 by compound and alcoholic acid weight ratio, adds ethanol, is 300r/min rolling ball milling 24h at rotating speed, and 80 ℃ of oven dry, the alumina crucible of packing into is calcined 4h down at 870 ℃, synthetic principal crystalline phase; Once the calcining material adds 5.5wt%ZnO and 3.75wt%Bi
2O
3, be 1: 1.2 by compound and alcoholic acid weight ratio, add ethanol, at rotating speed 300r/min barreling batch mixing 24h, 80 ℃ of oven dry, the alumina crucible of packing into is calcined 2h down at 750 ℃; The secondary clacining material adds the ZBS of 8wt%, is 1: 1.2 by compound and alcoholic acid weight ratio, adds ethanol, at rotating speed 300r/min barreling batch mixing 24h, depresses to the knobble of diameter 25mm, thickness 13mm at the pressure of 80Mpa.Become to burn under 920 ℃, insulation 4h promptly obtains material of the present invention.Dielectric properties are: ε
r=38.66, Qf=6998, resonant frequency f=3.4357GHz, frequency-temperature coefficient τ
f=13.78ppm/ ℃.
Embodiment 4:
According to x=0.3, CaCO in molar ratio in the principal crystalline phase expression formula
3: Li
2CO
3: Nb
2O
5: TiO
2=1.000: weighing in 0.1167: 0.2333: 0.3000 is 1: 1.2 by compound and alcoholic acid weight ratio, adds ethanol, is 300r/min rolling ball milling 24h at rotating speed, and 80 ℃ of oven dry, the alumina crucible of packing into is calcined 4h down at 870 ℃, synthetic principal crystalline phase; Once the calcining material adds 5.5wt%ZnO and 3.75wt%Bi
2O
3, be 1: 1.2 by compound and alcoholic acid weight ratio, add ethanol, at rotating speed 300r/min barreling batch mixing 24h, 80 ℃ of oven dry, the alumina crucible of packing into is calcined 2h down at 780 ℃; The secondary clacining material adds the ZBS of 5wt%, by compound and alcoholic acid weight ratio is 1: 1.2, add ethanol, at rotating speed 300r/min barreling batch mixing 24h, oven dry depresses to the knobble of diameter 25mm, thickness 13mm at the pressure of 80Mpa, becomes to burn under 920 ℃, insulation 4h promptly obtains material of the present invention.Dielectric properties are: ε
r=38.49, Qf=8652, resonant frequency f=3.2893GHz, frequency-temperature coefficient τ
f=4.05ppm/ ℃.
Claims (3)
1, a kind of medium dielectric constant microwave medium low-temperature sintering microwave medium pottery is characterized in that its prescription composition formula is:
Ca[(Li
1/3Nb
2/3)
1-xTi
x] O
3-δ, x=0.1～0.5 wherein
With desired raw material CaCO
3, Li
2CO
3, Nb
2O
5, TiO
2The weight summation be 100%, the weight percent of additive is:
Bi
2O
3：2～6wt％
ZnO：0～8wt％
Zinc borosilicate glass powder: 5～15%.
2, a kind of preparation method of medium dielectric constant microwave medium low-temperature sintering microwave medium pottery is characterized in that preparation technology may further comprise the steps:
1. be Ca[(Li by the principal crystalline phase expression formula
1/3Nb
2/3)
1-xTi
x] O
3-δ, required each component mol ratio CaCO in x=0.1～0.5 wherein
3: Li
2CO
3: Nb
2O
5: TiO
2=1.000: (0.1500～0.0833): (0.3000～0.1667): (0.1000～0.5000) forms batching, by compound and alcoholic acid weight ratio is 1: (1～1.5), add ethanol, mix 16～24h at rotating speed 300r/min rolling ball milling, 60～80 ℃ of oven dry, with the compound alumina crucible of packing into of oven dry, at 800～950 ℃ of calcining 2～4h down, synthetic principal crystalline phase;
2. once the calcining material adds 2～6wt%Bi
2O
3, 0～8wt%ZnO, be 1 by compound and alcoholic acid weight ratio: (1～1.5), add ethanol, mix 16～24h, 60～80 ℃ of oven dry at rotating speed 300r/min rolling ball milling; With the compound alumina crucible of packing into of oven dry, at 700～850 ℃ of calcining 2～4h down; Calcining pellet abrasive dust is broken to median size 1 μ m, and is standby;
3. the secondary clacining material adds 5～15% zinc borosilicate glass powders, by compound and alcoholic acid weight ratio is 1: (1～1.5), add ethanol, mix 16～24h at rotating speed 300r/min rolling ball milling, be pressed into the knobble of diameter 25mm, thickness 10～15mm at 80～120MPa, at 850～920 ℃ of following sintering, insulation 2～6h promptly obtains material of the present invention.
3, the preparation method of a kind of medium dielectric constant microwave medium low-temperature sintering microwave medium pottery according to claim 2 is characterized in that:
1. raw material is pressed following proportion ingredient:
Ca[(Li
1/3Nb
2/3)
1-xTi
x] O
3-δ, wherein x=0.2, i.e. Ca[(Li
1/3Nb
2/3)
0.8Ti
0.2] O
3-δ
The mol ratio CaCO of each required component
3: Li
2CO
3: Nb
2O
5: TiO
2=1.000: 0.1333: 0.2667: 0.2000
With desired raw material CaCO
3, Li
2CO
3, Nb
2O
5And TiO
2The weight summation be 100%, the weight percent of additive is:
Bi
2O
3：5wt％
Zinc borosilicate glass powder: 8wt%
2. with above-mentioned Li
2CO
3, Nb
2O
5, CaCO
3, TiO
2Proportioning is 1: 1.2 by compound and alcoholic acid weight ratio, adds ethanol, and at rotating speed 300r/min rolling ball milling mixings 24h, 80 ℃ of oven dry with the compound of the oven dry alumina crucible of packing into, at 905 ℃ of calcining 4h down, are synthesized principal crystalline phase;
3. once the calcining material adds 5wt%Bi
2O
3, be 1: 1.2 by compound and alcoholic acid weight ratio, add ethanol, in rotating speed 300r/min rolling ball milling mixing 24h, 80 ℃ of oven dry; With the compound alumina crucible of packing into of oven dry, at 750 ℃ of calcining 2h down; Calcining pellet abrasive dust is broken to median size 1 μ m, and is standby;
4. the secondary clacining material adds 8% zinc borosilicate glass powder, by compound and alcoholic acid weight ratio is 1: (1～1.2), add ethanol, at rotating speed 300r/min rolling ball milling mixing 24h, be pressed into the knobble of diameter 25mm, thickness 12mm at 80MPa, at 906 ℃ of following sintering, insulation 3.7h promptly obtains material of the present invention.
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|---|---|---|---|
| CN 200310104221 CN1275901C (en) | 2003-10-23 | 2003-10-23 | Low temperature sintered microwave dielectric ceramic with medium dielectric constant and its prepn process |
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|---|---|---|---|
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| CN1275901C true CN1275901C (en) | 2006-09-20 |
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| CN1317226C (en) * | 2005-09-09 | 2007-05-23 | 华中科技大学 | Low dielectric constant microwave dielectric ceramic material |
| CN100378031C (en) * | 2006-03-09 | 2008-04-02 | 中国科学院上海硅酸盐研究所 | Low temperature sintered microwave dielectric ceramics and its preparing method |
| CN100393666C (en) * | 2006-08-01 | 2008-06-11 | 浙江大学 | Environmental protection low temperature sintered microwave medium ceramic material and its preparation method |
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| TW201119974A (en) * | 2009-10-16 | 2011-06-16 | Nippon Chemical Ind | Composition for forming dielectric ceramic and dielectric ceramic material |
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| CN104177060B (en) * | 2014-07-14 | 2016-03-16 | 浙江大学 | A kind of glass-ceramic composite insulating material and preparation method thereof |
| CN107021757B (en) * | 2017-05-27 | 2020-01-10 | 电子科技大学 | Microwave dielectric ceramic material and preparation method thereof |
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2003
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