CN102659406B - Nd2O3-TiO2 system microwave dielectric ceramic and preparation method of Nd2O3-TiO2 microwave dielectric ceramic - Google Patents
Nd2O3-TiO2 system microwave dielectric ceramic and preparation method of Nd2O3-TiO2 microwave dielectric ceramic Download PDFInfo
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- CN102659406B CN102659406B CN201210162971.7A CN201210162971A CN102659406B CN 102659406 B CN102659406 B CN 102659406B CN 201210162971 A CN201210162971 A CN 201210162971A CN 102659406 B CN102659406 B CN 102659406B
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- dielectric ceramic
- microwave dielectric
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- 239000000919 ceramic Substances 0.000 title claims abstract description 30
- 238000002360 preparation method Methods 0.000 title abstract description 6
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title abstract 7
- 239000000843 powder Substances 0.000 claims abstract description 17
- 239000000758 substrate Substances 0.000 claims abstract description 12
- 238000005469 granulation Methods 0.000 claims abstract description 8
- 230000003179 granulation Effects 0.000 claims abstract description 8
- 229910052692 Dysprosium Inorganic materials 0.000 claims abstract description 4
- 238000000498 ball milling Methods 0.000 claims description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 13
- 238000001816 cooling Methods 0.000 claims description 12
- 229910010413 TiO 2 Inorganic materials 0.000 claims description 9
- 238000000034 method Methods 0.000 claims description 8
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- 239000008188 pellet Substances 0.000 claims description 6
- 229910052573 porcelain Inorganic materials 0.000 claims description 6
- 238000003825 pressing Methods 0.000 claims description 6
- 238000002791 soaking Methods 0.000 claims description 6
- 238000005303 weighing Methods 0.000 claims description 6
- 239000003795 chemical substances by application Substances 0.000 claims description 5
- 238000009413 insulation Methods 0.000 claims 1
- 238000000227 grinding Methods 0.000 abstract description 7
- 239000002994 raw material Substances 0.000 abstract description 6
- 239000002019 doping agent Substances 0.000 abstract description 5
- 238000005245 sintering Methods 0.000 abstract description 5
- 229910052772 Samarium Inorganic materials 0.000 abstract description 3
- 229910052782 aluminium Inorganic materials 0.000 abstract description 3
- 229910052746 lanthanum Inorganic materials 0.000 abstract description 3
- 231100000252 nontoxic Toxicity 0.000 abstract description 2
- 230000003000 nontoxic effect Effects 0.000 abstract description 2
- PLDDOISOJJCEMH-UHFFFAOYSA-N neodymium(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Nd+3].[Nd+3] PLDDOISOJJCEMH-UHFFFAOYSA-N 0.000 abstract 6
- 239000007767 bonding agent Substances 0.000 abstract 1
- 238000004891 communication Methods 0.000 description 4
- 238000005498 polishing Methods 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 239000011230 binding agent Substances 0.000 description 3
- 239000002131 composite material Substances 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000010295 mobile communication Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 238000000748 compression moulding Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 229920001451 polypropylene glycol Polymers 0.000 description 1
- 238000005549 size reduction Methods 0.000 description 1
- 229910052718 tin Inorganic materials 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
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- Inorganic Insulating Materials (AREA)
Abstract
The invention relates to a neodymium sesquioxide (Nd2O3)-titanium dioxide (TiO2) system microwave dielectric ceramic and a preparation method of the Nd2O3-TiO2 microwave dielectric ceramic. Raw materials of the Nd2O3-TiO2 microwave dielectric ceramic consist of substrates and doping agents, wherein the substrates are Nd2O3 and TiO2, the doping agents are R2O3, R is Al, La, Sm or Dy, the raw materials are subjected to ball grinding and presintering treatment, then, the secondary ball grinding is carried out to obtain powder, bonding agents are then added, the grinding, the granulation, the tabletting and the forming are carried out, and then sintering is prformed to obtain the ceramic. The dielectric constant of the microwave dielectric ceramic prepared by the invention is 40 to 75, and the quality factor of the microwave dielectric ceramic is 7000 to 25000 and is relatively higher. The Nd2O3-TiO2 microwave dielectric ceramic conforms to the environment-friendly requirement and is non-toxic, and the environment pollution is avoided.
Description
Technical field
The present invention relates to a kind of middle high dielectric microwave-medium ceramics and preparation method, be mainly used in the microwave devices such as micro-wave communication, wave filter, dielectric resonator, vibrator, phase shifter, electrical condenser, relate in particular to a kind of novel Nd
2O
3-TiO
2Series microwave dielectric ceramic and preparation method thereof.
Background technology
Along with present mobile communication and satellite communications development, a large amount of utilizations of resonator, wave filter, polyrod antenna, so that the planner target tightening in the size reduction of microwave-medium ceramics and the raising of dielectric properties, this just requires microwave-medium ceramics to possess high-k, low dielectric loss, nearly zero temperature coefficient of resonance frequency.Middle high-permittivity microwave medium ceramics, its value are between 40 to 80, are mainly used in the mobile communication base station of microwave military radar, satellite communication and communication system of 2 ~ 8GHz.This type of ceramic development research helps the systematize of microwave-medium ceramics system, integration.Study at present many BaO-TiO
2System, (Zr, Sn) TiO
4System, BiNbO
4System etc., but because dielectric loss is large and the phase composite more complicated, also need further research.
Summary of the invention
Purpose of the present invention for improve existing in the loss of high dielectric microwave-medium ceramics large, the problem such as phase composite complexity and proposed a kind of Nd
2O
3-TiO
2Series microwave dielectric ceramic; Another object of the present invention also provides the preparation method of above-mentioned microwave-medium ceramics.
Technical scheme of the present invention is: a kind of Nd
2O
3-TiO
2Series microwave dielectric ceramic is characterized in that raw material is comprised of matrix and doping agent, and its mesostroma is Nd
2O
3And TiO
2, Nd
2O
3With TiO
2Mol ratio is 1: (2 ~ 5); Doping agent is R
2O
3, wherein R is Al, La, Sm or Dy, the doping of doping agent is the 2%-8% of raw material total mass; The specific inductivity of microwave-medium ceramics is 40～75, and quality factor are 7000～25000.
The present invention also provides above-mentioned Nd
2O
3-TiO
2The method of series microwave dielectric ceramic, its concrete steps are as follows:
A) with Nd
2O
3, TiO
2And R
2O
3Take by weighing raw material by proportioning, and ball milling, oven dry;
B) raw material of oven dry carries out preheating, and the powder furnace cooling after the calcining continues secondary ball milling after taking out, and oven dry obtains powder;
C) powder that obtains adds binding agent, grinds the granulation compression molding;
D) green compact of moulding sinter porcelain at 1250～1450 ° of C, and wherein temperature rise rate is at 2-4 ° of C/min, be incubated 3～6 hours furnace cooling then.
Preferred steps a) and step b) all take the planetary ball mill wet ball grinding; Rotational speed of ball-mill is 250 ~ 350 r/min, and Ball-milling Time is 6 ~ 10 hours, adds deionized water and agate ball, and material: water: the mass ratio of ball is 1: (1 ~ 2): (1 ~ 3).
Step b) calcined temperature of preheating is 900～1200 ° of C, and temperature rise rate is 2～4 ° of C/min, soaking time 2～3h.
Step c) binding agent described in is POLYPROPYLENE GLYCOL (PVA) or Xylo-Mucine (CMC); The adding quality of binding agent is 5%～10% of powder quality, and the powder after the grinding granulation is crossed 80 mesh sieves or 120 mesh sieves, and is dry-pressing formed.
Beneficial effect:
The invention provides a kind of novel microwave-medium ceramics system that is applicable to the 2-8GHz microwave frequency, specific inductivity is between 40-75, high quality factor Qf＞7000, and compared with the microwave-medium ceramics of identical specific inductivity, its quality factor is relatively high.The present invention meets environmental requirement, and is nontoxic, environmentally safe.
Embodiment
Embodiment 1
According to 2wt%Al
2O
3The Nd that mixes
2O
3-2TiO
2Prescription takes by weighing 26.5814gNd
2O
3, 12.6186gTiO
2, 0.8gAl
2O
3After, pellet water ratio with 1: 2: 1, add deionized water and agate ball, with planetary mills wet method ball milling 6 hours (250r/min), oven dry is by 900 ° of C of pre-burning, be incubated 2 hours (in air atmosphere), temperature rise rate is 2 ° of C/min, furnace cooling, powder after the pre-burning was carried out secondary ball milling 8 hours (other parameters are with a ball milling), add the tackiness agent of the 5wt%PVA of powder after the oven dry, granulation is ground, cross 80 purposes sieve, with powder pressing Cheng Houwei 6.5mm, diameter is the thin cylinder base substrate of 13mm, and pressure is 100MPa, sinters base substrate into porcelain at 1250 ° of C, temperature rise rate is 3 ° of C/min, soaking time is 3h,, furnace cooling then.Test result to this microwave-medium ceramics is as follows: with the sample surfaces polishing, adopt Agiligent 8722ET network analyzer, measure DIELECTRIC CONSTANT ε according to the Hakki-Coleman method
rAnd quality factor q, it is as follows to measure microwave dielectric property under the optimal sintering temperature: ε
r=43, Qf=7354GHz(7.705GHz)
Embodiment 2
According to 4wt%La
2O
3The Nd that mixes
2O
3-3TiO
2Prescription takes by weighing 22.4289gNd
2O
3, 15.9711gTiO
2, 1.6gLa
2O
3After, pellet water ratio with 1: 1: 2, add deionized water and agate ball, with planetary mills wet ball grinding 10 hours (250r/min), oven dry is by 1000 ° of C of pre-burning, be incubated 3 hours (in air atmosphere), temperature rise rate is 2.5 ° of C/min, furnace cooling, the powder after the pre-burning was carried out secondary ball milling 9 hours (1: 1: 2 pellet water ratio, 300r/min), the tackiness agent that adds 7wt%CMC after the oven dry, granulation is ground, and crosses 120 purposes sieve, with powder pressing Cheng Houwei 6.5mm, diameter is the thin cylinder base substrate of 13mm, pressure is 100MPa, sinter base substrate into porcelain at 1350 ° of C, temperature rise rate is 3.5 ° of C/min, and soaking time is 4h,, furnace cooling then.Test result to this microwave-medium ceramics is as follows: with the sample surfaces polishing, adopt Agiligent 8722ET network analyzer, measure DIELECTRIC CONSTANT ε according to the Hakki-Coleman method
rAnd quality factor q, it is as follows to measure microwave dielectric property under the optimal sintering temperature: ε
r=54, Qf=12488GHz(5.354GHz)
Embodiment 3
According to 6wt%Sm
2O
3The Nd that mixes
2O
3-4TiO
2Prescription takes by weighing 19.2877gNd
2O
3, 18.3123gTiO
2, 2.4gSm
2O
3After, pellet water ratio with 1: 1.5: 3, add deionized water and agate ball, with planetary mills wet ball grinding 9 hours (300r/min), oven dry is by 1100 ° of C of pre-burning, be incubated 3 hours (in air atmosphere), temperature rise rate is 3 ° of C/min, furnace cooling carried out secondary ball milling 7 hours with the powder after the pre-burning (250r/min, other parameters are with a ball milling), the tackiness agent that adds 8wt%CMC after the oven dry, granulation is ground, and crosses 120 purposes sieve, with powder pressing Cheng Houwei 6.5mm, diameter is the thin cylinder base substrate of 13mm, pressure is 100MPa, sinter base substrate into porcelain at 1400 ° of C, temperature rise rate is 4 ° of C/min, and soaking time is 5h,, furnace cooling then.
Test result to this microwave-medium ceramics is as follows: with the sample surfaces polishing, adopt Agiligent 8722ET network analyzer, measure DIELECTRIC CONSTANT ε according to the Hakki-Coleman method
rAnd quality factor q, it is as follows to measure microwave dielectric property under the optimal sintering temperature: ε
r=63, Qf=18756GHz(6.687GHz)
Embodiment 4
According to 8wt%Dy
2O
3The Nd that mixes
2O
3-5TiO
2Prescription takes by weighing 16.8283gNd
2O
3, 19.9717gTiO
2, 3.2gDy
2O
3After, pellet water ratio with 1: 2: 2, add deionized water and agate ball, with planetary mills wet method ball milling 8 hours (350r/min), oven dry is by 1200 ° of C of pre-burning, be incubated 2 hours (in air atmosphere), temperature rise rate is 4 ° of C/min, furnace cooling, powder after the pre-burning was carried out secondary ball milling 10 hours (parameter is with a ball milling), add the tackiness agent of 10wt%PVA after the oven dry, granulation is ground, cross 80 purposes sieve, with powder pressing Cheng Houwei 6.5mm, diameter is the thin cylinder base substrate of 13mm, and pressure is 100MPa, sinters base substrate into porcelain at 1450 ° of C, temperature rise rate is 3 ° of C/min, soaking time is 6h,, furnace cooling then.
Test result to this microwave-medium ceramics is as follows: with the sample surfaces polishing, adopt Agiligent 8722ET network analyzer, measure DIELECTRIC CONSTANT ε according to the Hakki-Coleman method
rAnd quality factor q, it is as follows to measure microwave dielectric property under the optimal sintering temperature: ε
r=76, Qf=22465GHz(5.413GHz).
Claims (1)
1. Nd
2O
3-TiO
2Series microwave dielectric ceramic is characterized in that: according to 8wt%Dy
2O
3The Nd that mixes
2O
3-5TiO
2Prescription takes by weighing 16.8283gNd
2O
3, 19.9717gTiO
2, 3.2gDy
2O
3After, with the pellet water ratio of 1:2:2, add deionized water and agate ball, use ball milling of planetary mills wet method 8 hours, rotational speed of ball-mill is 350r/min, oven dry is by 1200 ℃ of pre-burnings, and insulation is 2 hours in air atmosphere, and temperature rise rate is 4 ℃/min, furnace cooling, powder after the pre-burning was carried out secondary ball milling 10 hours, and parameter adds the 10wt%PVA tackiness agent with a ball milling after the oven dry, granulation is ground, cross 80 purposes sieve, with powder pressing Cheng Houwei 6.5mm, diameter is the thin cylinder base substrate of 13mm, and pressure is 100MPa, sinter base substrate into porcelain at 1450 ℃, temperature rise rate is 3 ℃/min, and soaking time is 6h, then furnace cooling.
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|---|---|---|---|
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| CN201210162971.7A CN102659406B (en) | 2012-05-23 | 2012-05-23 | Nd2O3-TiO2 system microwave dielectric ceramic and preparation method of Nd2O3-TiO2 microwave dielectric ceramic |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101182199A (en) * | 2007-11-12 | 2008-05-21 | 南京工业大学 | Y2O3-TiO2 series microwave dielectric ceramic and preparation method thereof |
| CN102153342A (en) * | 2010-12-27 | 2011-08-17 | 南京工业大学 | Composite doped modified Y2Ti2O7 microwave medium ceramic material |
| CN102295457A (en) * | 2011-01-17 | 2011-12-28 | 南京工业大学 | Low-loss Sm2O3-TiO2 microwave medium ceramic and preparation method thereof |
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| JPS5851363B2 (en) * | 1981-12-29 | 1983-11-16 | 日本電気株式会社 | Porcelain dielectric material for temperature compensation |
| JP2004345914A (en) * | 2003-05-23 | 2004-12-09 | Murata Mfg Co Ltd | Dielectric glass ceramic composition and multilayer circuit board |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101182199A (en) * | 2007-11-12 | 2008-05-21 | 南京工业大学 | Y2O3-TiO2 series microwave dielectric ceramic and preparation method thereof |
| CN102153342A (en) * | 2010-12-27 | 2011-08-17 | 南京工业大学 | Composite doped modified Y2Ti2O7 microwave medium ceramic material |
| CN102295457A (en) * | 2011-01-17 | 2011-12-28 | 南京工业大学 | Low-loss Sm2O3-TiO2 microwave medium ceramic and preparation method thereof |
Non-Patent Citations (2)
| Title |
|---|
| JP昭57-154714A 1982.09.24 |
| JP特开2004-345914A 2004.12.09 |
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