CN1079384C - Lead based micro-wave medium ceramic, and method for mfg. same - Google Patents
Lead based micro-wave medium ceramic, and method for mfg. same Download PDFInfo
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- CN1079384C CN1079384C CN99110272A CN99110272A CN1079384C CN 1079384 C CN1079384 C CN 1079384C CN 99110272 A CN99110272 A CN 99110272A CN 99110272 A CN99110272 A CN 99110272A CN 1079384 C CN1079384 C CN 1079384C
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Abstract
The present invention relates to lead-based microwave medium ceramics and a manufacturing method thereof. The lead-based microwave medium ceramics comprises the raw material proportioning of aPbO. bSrO. cBaO. dCaO. mMgO. nNb2O5. pTiO2. qSnO2, wherein a=0.6*[1-2(b+c+d)], m=n=a/3, p=b+d, q=c, 0 mol%<=b<=30 mol%, 0 mol%<=c<=30 mol%, 5 mol%<=d<=35 mol%, and 15 mol%<=b+c+d<=35 mol%. After being mixed for 24 hours by a wet type ball milling method, the raw materials are dried, and then a binding agent is added to the raw materials for granulation; then, press forming is carried out under the pressure of 98 to 147MPa, and sintering is carried out at 1200 to 1350 DEG C. The ceramics has the advantages of high dielectric constant, low dielectric loss and good temperature stability and can be used for manufacturing key elements in a microwave medium system.
Description
The present invention relates to plumbous oxide is the high-permittivity microwave medium ceramics and the manufacture method thereof of base-material.
Microwave-medium ceramics is the key components that is used for microwave communication systems such as dielectric resonator, wave filter and vibrator.In recent years, along with developing rapidly of mobile communication and satellite communication technology, the demand of the microwave-medium ceramics that microwave devices such as dielectric resonator and wave filter are used is just growing.
For microwave-medium ceramics, at first require it that low dielectric loss (high Q value is arranged, Qf＞3000GHz) and temperature coefficient of resonance frequency (f＜20ppm/ ℃ of the 20ppm/ ℃＜τ that approaches zero, for the lower material series of specific inductivity, f＜10ppm/ ℃ of requirement-10ppm/ ℃＜τ), simultaneously, require the high DIELECTRIC CONSTANT of trying one's best for the needs that satisfy device miniaturization.
On the other hand, though developed a series of microwave-medium ceramics at present, high specific inductivity class material (ε＞80) is less for number, even and the highest BaO-Nb of specific inductivity
2O
3-TiO
2Series, its specific inductivity is the highest also can only to be reached about 94.In general, its dielectric loss of the material that specific inductivity is big and temperature factor are also bigger.Therefore, 110 specific inductivity once was considered to " threshold " together that microwave-medium ceramics is difficult to go beyond.This has just limited the expansion of further miniaturization of microwave device and range of application widely.
It is good and the lead based micro-wave medium ceramic and the manufacture method thereof of high-k are as far as possible arranged to the purpose of this invention is to provide a kind of low-dielectric loss, temperature stability, can solve the problem that exists in the background technology.
In order to achieve the above object, the technical solution used in the present invention is:
1) proportioning raw materials (by mole per-cent) is:
APbObSrOcBaOdCaOmMgOnNb
2O
5PTiO
2QSnO
2, wherein, a, b, c, d, m, n, p and q are molar percentage, and a=0.6[1-2 (b+c+d)], m=n=a/3, p=b+d, q=c, 0mol%≤b≤30mol%, 0mol%≤c≤30mol%, 5mol%≤d≤35mol%, 15mol%≤b+c+d≤35mol%.
2) manufacture method
With purity is PbO, SrO, BaO, CaO, MgO, TiO more than 99.5%
2, SnO
2And Nb
2O
5Mix 24 hours (solvent is a distilled water) by said ratio with the wet ball-milling method, after the mixture oven dry, at 850～1110 ℃, give in the air atmosphere and burning 3～4 hours, then, giving polyvinyl alcohol (PVA) the binding agent granulation of burning interpolation 5wt% in the powder, press forming under the pressure of 98～147MPa, at 1200～1350 ℃, sintering is 2～3 hours in the air atmosphere at last.
The specific inductivity of existing non-plumbous series microwave dielectric ceramic generally is no more than 100, though and lead base composite perofskite pottery has very high specific inductivity, its dielectric loss and temperature factor are all too big, can not directly consider its microwave application.The present invention is conceived to the low-lossization and temperature factor control of lead base composite perofskite pottery, has found out above-mentioned high-permittivity microwave medium ceramics new system and prescription thereof at last.
Wherein, SrO, CaO and TiO
2Effect be to reduce dielectric loss and temperature coefficient of resonance frequency.And SnO
2By forming BaSnO with BaO
3, can further reduce dielectric loss, improve the Qf value.SrO, BaO, CaO, TiO
2And SnO
2Content can not be too low, can not be too high.If b+c+d＜15mol%, the temperature coefficient of resonance frequency of material is too high; Behind b+c+d＞35mol%, can cause problems such as material hard-to-sinter and dielectric loss increase.
Embodiment:
At first, with purity be PbO, SrO, BaO, CaO, MgO, TiO more than 99.5%
2, SnO
2And Nb
2O
5Mix 24 hours (solvent is a distilled water) with the wet ball-milling method according to a certain percentage, the oven dry back is given in 850～1110 ℃, air atmosphere and being burnt 3 hours.Then, after in giving the burning powder, adding PVA and granulation, be formed in the ceramic body of preparing diameter 12mm, thickness 3～8mm under the pressure of 98～147MPa by uniaxial tension, at last in 1200～1350 ℃, air atmosphere sintering 3 hours to prepare required microwave-medium ceramics.
Carried out material phase analysis with the ceramic sample of powder method of X-ray diffraction after, and carried out the evaluation of microwave dielectric property with the cylindrical dielectric resonator method at 3GHz sintering.
Below listed the microwave dielectric property of material and the relation of composition among the embodiment, as shown in table 1.
As known from Table 1, in ceramic systems of the present invention, along with PbO, MgO and Nb
2O
5The minimizing of content (a, m, n), DIELECTRIC CONSTANT are tending towards reducing and Qf value (Q is that quality factor are the inverse of dielectric loss, and f is a resonant frequency) is tending towards increasing, while temperature coefficient of resonance frequency τ
fBe tending towards reducing.When b+c+d＜15mol%, temperature coefficient of resonance frequency and dielectric loss are all excessive; And during b+c+d＞35mol%, material will become be difficult to sintering, its Qf value also will be less than 3000GHz.Therefore, basal component scope of the present invention is decided to be a=0.6[1-2 (b+c+d)], m=n=a/3, p=b+d, q=c, 0mol%≤b≤30mol%, 0mol%≤c≤30mol%, 5mol%≤d≤35mol%, 15mol%≤b+c+d≤35mol%.
In all the components of embodiment, in the 11 composition, PbO=24mol%, SrO=2.5mol%, BaO=2.5mol%, CaO=25mol%, MgO=8mol%, Nb
2O
5=8mol%, TiO
2=27.5mol%, SnO
2Microwave dielectric property overall target the best of the one-tenth branch of=2.5mol%: ε=150, Qf=3600GHz, τ
f=14ppm/ ℃.
[table 1]
| PbO mol％ | SrO mol％ | BaO mol％ | CaO mol％ | MgO mol％ | Nb 2O 5 Mol％ | TiO 2 mol％ | SnO 2 mol％ | ε | Qf GHz | τ fppm/℃ |
| 42 | 0 | 10 | 5 | 14 | 14 | 5 | 10 | 200 | 3100 | 20 |
| 42 | 2.5 | 2.5 | 10 | 14 | 14 | 12.5 | 2.5 | 198 | 3000 | 20 |
| 36 | 0 | 10 | 10 | 12 | 12 | 10 | 10 | 196 | 3050 | 18 |
| 30 | 2.5 | 2.5 | 20 | 10 | 10 | 22.5 | 2.5 | 185 | 3200 | 18 |
| 30 | 20 | 0 | 5 | 10 | 10 | 25 | 0 | 200 | 3100 | 19 |
| 30 | 10 | 10 | 5 | 10 | 10 | 15 | 10 | 196 | 3500 | 17 |
| 30 | 0 | 20 | 5 | 10 | 10 | 5 | 20 | 190 | 3900 | 16 |
| 24 | 5 | 5 | 20 | 8 | 8 | 25 | 5 | 165 | 3400 | 17 |
| 24 | 2.5 | 7.5 | 20 | 8 | 8 | 22.5 | 7.5 | 160 | 350 | 15 |
| 24 | 5 | 10 | 15 | 8 | 8 | 20 | 10 | 145 | 3600 | 15 |
| 24 | 2.5 | 2.5 | 25 | 8 | 8 | 27.5 | 2.5 | 150 | 3600 | 14 |
| 24 | 0 | 5 | 25 | 8 | 8 | 25 | 5 | 135 | 4200 | 16 |
| 24 | 5 | 0 | 25 | 8 | 8 | 30 | 0 | 140 | 3800 | 18 |
| 18 | 5 | 5 | 25 | 6 | 6 | 30 | 5 | 120 | 3200 | 18 |
| 18 | 10 | 15 | 10 | 6 | 6 | 20 | 15 | 142 | 3400 | 17 |
| 18 | 5 | 20 | 10 | 6 | 6 | 15 | 20 | 122 | 3500 | 16 |
| 18 | 30 | 0 | 5 | 6 | 6 | 35 | 0 | 200 | 3600 | 20 |
| 18 | 0 | 30 | 5 | 6 | 6 | 5 | 30 | 196 | 4000 | 19 |
| 18 | 0 | 0 | 35 | 6 | 6 | 35 | 0 | 110 | 3000 | 20 |
The present invention compares the useful effect that has with background technology:
The invention provides dielectric constant up to 110～200, with having simultaneously the microwave-medium ceramics of low-loss with less temperature coefficient of resonance frequency, the dielectric constant of particularly having broken through microwave-medium ceramics is generally less than 110 " threshold ". And utilize low-dielectric loss provided by the invention, temperature stability good and the microwave-medium ceramics of high-k is arranged, can make the further miniaturization of the microwave devices such as dielectric resonator and wave filter become possibility. Simultaneously, pottery provided by the invention also can be applicable to high-frequency ceramic capacitor or temperature compensating ceramic capacit etc. Therefore, the present invention has a great popularizing value industrial.
Claims (3)
1. lead based micro-wave medium ceramic, it is characterized in that: proportioning raw materials is aPbObSrOcBaOdCaOmMgOnNb
2O
5PTiO
2QSnO
2, wherein, a, b, c, d, m, n, p and q are molar percentage, and a=0.6[1-2 (b+c+d)], m=n=a/3, p=b+d, q=c, 0mol%≤b≤30mol%, 0mol%≤c≤30mol%, 5mol%≤d≤35mol%, 15mol%≤b+c+d≤35mol%.
2. manufacture method of making the described lead based micro-wave medium ceramic of claim 1 is characterized in that: with purity is PbO, SrO, BaO, CaO, MgO, TiO more than 99.5%
2, SnO
2And Nb
2O
5Mixed 24 hours with the wet ball-milling method by said ratio, solvent is a distilled water, after the mixture oven dry, at 850～1110 ℃, give in the air atmosphere and burning 3～4 hours, then, giving the polyvinyl alcohol adhesive granulation of burning interpolation 5wt% in the powder, press forming under the pressure of 98～147MPa, at last at 1200～1350 ℃, sintering is 2～3 hours in the air atmosphere.
3. the manufacture method of lead based micro-wave medium ceramic according to claim 2 is characterized in that: its proportioning raw materials PbO=24mol%, SrO=2.5mol%, BaO=2.5mol%, CaO=25mol%, MgO=8mol%, Nb
2O
5=8mol%, TiO
2=27.5mol%, SnO
2=2.5mol%.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN99110272A CN1079384C (en) | 1999-07-28 | 1999-07-28 | Lead based micro-wave medium ceramic, and method for mfg. same |
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|---|---|---|---|
| CN99110272A CN1079384C (en) | 1999-07-28 | 1999-07-28 | Lead based micro-wave medium ceramic, and method for mfg. same |
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|---|---|
| CN1242347A CN1242347A (en) | 2000-01-26 |
| CN1079384C true CN1079384C (en) | 2002-02-20 |
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| CN99110272A Expired - Fee Related CN1079384C (en) | 1999-07-28 | 1999-07-28 | Lead based micro-wave medium ceramic, and method for mfg. same |
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| KR101161614B1 (en) * | 2006-11-30 | 2012-07-03 | 한국세라믹기술원 | Glass-free microwave dielectric ceramics and the manufacturing method thereof |
| CN100453504C (en) * | 2007-01-26 | 2009-01-21 | 武汉理工大学 | Temperature stability capacitance ceramic and manufacturing method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN87101816A (en) * | 1986-03-12 | 1987-10-28 | 松下电器产业株式会社 | Stack capacitor element with ceramic dielectric |
| CN1163874A (en) * | 1996-03-26 | 1997-11-05 | 株式会社村田制作所 | Dielectric ceramics composition |
-
1999
- 1999-07-28 CN CN99110272A patent/CN1079384C/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN87101816A (en) * | 1986-03-12 | 1987-10-28 | 松下电器产业株式会社 | Stack capacitor element with ceramic dielectric |
| CN1163874A (en) * | 1996-03-26 | 1997-11-05 | 株式会社村田制作所 | Dielectric ceramics composition |
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