CN105601272A - Ultralow loss limit type Mgn+1TinO3n+1 microwave ceramic and making method thereof - Google Patents

Ultralow loss limit type Mgn+1TinO3n+1 microwave ceramic and making method thereof Download PDF

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CN105601272A
CN105601272A CN201610057795.9A CN201610057795A CN105601272A CN 105601272 A CN105601272 A CN 105601272A CN 201610057795 A CN201610057795 A CN 201610057795A CN 105601272 A CN105601272 A CN 105601272A
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microwave
1tino3n
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袁昌来
屈婧婧
黄先培
刘飞
刘笑
王殿辉
周昌荣
陈国华
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Guilin University of Electronic Technology
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Abstract

The invention discloses ultralow loss limit type Mgn+1TinO3n+1 microwave ceramic and a making method thereof. The chemical formula of the ceramic is: Mgn+1TinO3n+1, wherein n is equal to 2, 3, 4, 5, 6, 7, ... 50. According to the making method, Mgn+1TinO3n+1 powder is synthesized first, polyvinyl alcohol is added into the obtained powder, the mixture is mixed to be uniform and pressed into a cylindrical green body, the green body is sintered for 4 hours at the temperature of 1,340-1,380 DEG C to become ceramic, and then the ultralow loss limit type Mgn+1TinO3n+1 microwave ceramic can be obtained. Compared with MgTiO3 and Mg2TiO4 ceramic materials, the dielectric constant and temperature coefficient of resonance frequency of the Mgn+1TinO3n+1 series microwave ceramic do not change a lot, but the Q*f value is remarkably increased. The Mgn+1TinO3n+1 microwave ceramic (n=5) sintered for 4 hours at the temperature of 1,360 DEG C can obtain optimal microwave dielectric performance: Q*f is up to 382, 500 GHz (f0=7.534 GHz), epsilon r is up to 16.4, and tau f is up to -55.3 ppm/DEG C. It is predicated that the Mg6Ti5O16 ceramic material can be applied to a microwave circuit of large communication equipment in the high frequency field to serve as a main material of a dielectric substrate.

Description

A kind of ultra-low loss limit class Mgn+1TinO3n+1Microwave ceramics and preparation method thereof
Technical field
The present invention relates to information functional material, be specifically related to a kind of ultra-low loss limit class Mgn+1TinO3n+1Microwave ceramics materialMaterial.
Background technology
Because microwave signal has that frequency is high, wavelength is short, information capacity is large and the feature such as penetrability is strong, so that at heightIn the communication technology of speed development, microwave dielectric material, as indispensable a kind of new material, has become worldwideOne of study hotspot. Conventionally, the performance of evaluation microwave-medium ceramics mainly contains relative dielectric constant (εr), quality factor (Q) withProduct (Q × f:Q=1/tan, tan is dielectric loss) and the temperature coefficient of resonance frequency (τ of resonant frequencyf), three kinds of parameters are mutually auxiliaryCoordinate and restriction mutually. At present, the field relating to along with communication equipment constantly expands, in different microwave frequency ranges, allNeed to there is corresponding practical microwave dielectric material to match. So many traditional microwave dielectric materials no longer meet newlyThe high request of field to its dielectric properties, i.e. the development of novel microwave material and explore extremely urgent. Wherein, apply to high-end JieThe ultra-low loss limit class microwave dielectric ceramic materials of matter substrate also arises at the historic moment.
In recent years, mostly be low ε for the material of medium substraterHigh Q value microwave ceramics, the ε of these materialsrConventionally between 10 ~Between 25, have quite high Q × f value (100,000 ~ 200,000GHz), be also study the earliest and be able to practical simultaneouslyMicrowave-medium ceramics. This class material is mainly with multiple and perovskite A (B'B ") O3Series of solid solutions material is main, typically representativeThere is Ba (Mg, Ta) O3(BMT)、Ba(Zn,Ta)O3(BZT)、Ba(Mg,Nb)O3And Ba (Zn, Nb) O (BMN)3(BZN) withAnd compound, doping system taking them as matrix: BMT-Nd2O3，BZT-BaZrO3，BZT-B2O3-CuO，BZN-Sr(Zn1/ 3Nb2/3)O3Deng. But the sintering temperature of these materials is higher, not too easily meet the application of LCTT. And prolong in order to improve signalThe slow time, the Q value that these traditional materials are higher does not reach the standard of new demand yet; This forces researchers to developDevelop the low ε of novel ultrahigh Q-valuerMicrowave ceramic material. But, need to face, the exploitation of this class material is also in risingStep section, only has a small amount of research report.
In microwave ceramics system, if it is compound to adopt the perovskite structural material with opposite temperature coefficients to carry out, no matterBe form solid solution or formed multiphase system, the Q value of new material is normally at the Q of matrix value and the material Q compound with itBetween value, change. As (1-x) CaTiO3-xLaAlO3Q × f value of series is exactly at CaTiO3(Q × f ≈ 3600GHz) withLaAlO3Between (Q × f ≈ 68,000GHz), change. Want acquisition and there is the microwave-medium ceramics of higher Q value, and make its dielectricConstant remains in 10 ~ 20, has certain difficulty. But, Mgn+1TinO3n+1(1≤n≤∞) material be one notWrong selection, because Mgn+1TinO3n+1In compound, contain Ruddlesden-Popper (R-P) homology laminated perovskite structure,When hour this System forming multiphase structure of n value; Along with n value increases gradually, system changes into and has laminated perovskite structureWith pure MgTiO3The new compound coexisting; And in the time that n value further increases, system crystal structure is close to pure MgTiO3PhaseComposition; In the time that n value is infinity, though architecture approaches Mg:Ti ≈ 1:1, dephasign occurs once more. Wherein, thisThe existence of special R-P phase is also to make Mgn+1TinO3n+1The Q value of material is not simply at MgTiO3(Q×f≈166,Change 400GHz) and between the Q value of other phase, but occurred that a kind of stability of crystal structure and atom further arrange in orderThe Q value synergistic effect that the layer structure of row causes jointly.
Summary of the invention
The object of this invention is to provide one and be applicable to high-end medium substrate, preparation technology is simple and to have utmost point low-loss lowDielectric Mgn+1TinO3n+1(n=2,3,4 ... 50) microwave ceramics, its Q × f value is almost close to existing dielectric basic theoryExplainable maximum limit category ~ 400,000GHz.
The technical scheme that realizes the object of the invention is:
A kind of ultra-low loss limit class Mgn+1TinO3n+1Microwave ceramics, its composition general formula is: Mgn+1TinO3n+1, in formula, n=2,3,4,5,6,7…50。
A kind of ultra-low loss limit class Mgn+1TinO3n+1The preparation method of microwave ceramics, comprises the steps:
(1) synthetic Mgn+1TinO3n+1Powder: design sample constituents: n=2,3,4,5,6,7 ... 50, and according to stoichiometric proportionRaw materials weighing powder MgO and TiO2, mix, 24 hours ball milling post-dryings of gained mixed powder are crossed to 100 mesh sieves, at 1100 DEG CBe incubated and within 2 hours, carry out pre-burning, the powder after pre-burning is carried out to secondary ball milling and after 12 hours, cross 200 sieves, obtain Mgn+1TinO3n+1CloseBecome powder.
(2) compressing: the Mg that step (1) is obtainedn+1TinO3n+1Synthetic powder adds 5wt% polyvinyl alcohol to mix allEven, fine grinding after drying is pressed into cylindrical base substrate on forming machine;
(3 sintering: the cylindrical base substrate of step (2) gained sintering at 1340 ~ 1380 DEG C of temperature is become to porcelain in 4 hours, obtain ultralowLoss limit class Mgn+1TinO3n+1Microwave ceramics.
The optimum sintering temperature of described cylindrical base substrate is 1360 DEG C.
Ultra-low loss limit class Mg prepared by the present inventionn+1TinO3n+1Microwave ceramics shows after performance test: with respect toMgTiO3(εr=17, Q × f ≈ 166,400GHz and τf≈-50ppm/ DEG C) and Mg2TiO4(εr=14.2，Q×f≈160,000GHz and τf≈-60ppm/ DEG C) ceramic microwave dielectric property, Mgn+1TinO3n+1(n=5) microwave ceramics can obtainHigher Q × f value ~ 382,500GHz (f0=7.534GHz), and DIELECTRIC CONSTANTSrBetween 14.9 ~ 16.4, and humorousVibration frequency temperature coefficient τfBe about-55ppm/ DEG C. Their εrAnd τfValue and MgTiO3、Mg2TiO4Compare change little, but Q× f value but has raising extremely significantly. Estimate further to regulate temperature coefficient (τf) close to 1 o'clock, Mgn+1TinO3n+1(n=5) microwave ceramics system is expected to be applied to as the main material of medium substrate the high-end large-scale communication equipment in each high frequency fieldIn microwave circuit.
Brief description of the drawings
Fig. 1 is MgTiO under room temperature3And Mgn+1TinO3n+1Series samples is at the XRD of 1360 DEG C of sintering 4h collection of illustrative plates;
Fig. 2 is Mgn+1TinO3n+1Dielectric constant (the ε of series samplesr) with the quality factor (graph of relation of Q × f) and n value.
Detailed description of the invention
Further illustrate substantive features of the present invention and marked improvement below by 10 embodiment, but the present invention absolutely not onlyBe limited to described embodiment.
Embodiment 1
Preparation Mg3Ti2O7Ceramics sample;
Its preparation method, comprises the steps:
(1) synthetic Mg3Ti2O7Powder: press raw material with MgO:TiO2=3:2 molar ratio mixes, gained mixed powder 24Hour ball milling post-drying is crossed 100 mesh sieves, and at 1100 DEG C, temperature retention time is carried out pre-burning for 2 hours, and the powder after pre-burning is carried out to twoInferior ball milling is crossed 200 sieves after 12 hours, obtain Mg3Ti2O7Synthetic powder.
(2) compressing: the Mg that step (1) is obtained3Ti2O7Porcelain adds 5wt% polyvinyl alcohol to mix evenly, after oven dryFine grinding is pressed into cylindrical base substrate on forming machine;
(3) sintering: the cylindrical base substrate of step (2) gained sintering at 1360 DEG C of temperature is become to porcelain in 4 hours, obtain ultra-low lossLimit class Mg3Ti2O7Microwave ceramics.
Analyze Mg by XRD diffracting spectrum3Ti2O7Thing phase, determines its powder thing phase composition, surveys by vector network analysisTry its microwave dielectric property. Performance test shows: 1360 DEG C of sintering 4 hours, and its DIELECTRIC CONSTANTSrBe 15.8, resonant frequency temperatureDegree coefficient τfFor-58.1ppm/ DEG C, Q × f value is 211,600GHz (f0=7.843GHz)。
Embodiment 2
Preparation Mg4Ti3O10Ceramics sample;
Its preparation method, except pressing raw material with MgO:TiO2=4:3 molar ratio mixes and sintering temperature is outside 1340 DEG C, itsRemaining step is with embodiment 1.
Performance test shows: 1340 DEG C of sintering 4 hours, and its DIELECTRIC CONSTANTSrBe 15.4, temperature coefficient of resonance frequency τfFor-56.2ppm/ DEG C, Q × f value is 270,400GHz (f0=7.677GHz)。
Embodiment 3
Preparation Mg5Ti4O13Ceramics sample;
Its preparation method, except pressing raw material with MgO:TiO2Outside=5:4 molar ratio mixes, all the other steps are with embodiment 1.
Performance test shows: 1360 DEG C of sintering 4 hours, and its DIELECTRIC CONSTANTSrBe 16.4, temperature coefficient of resonance frequency τfFor-60.3ppm/ DEG C, Q × f value is 323,200GHz (f0=7.535GHz)。
Embodiment 4
Preparation Mg6Ti5O16Ceramics sample;
Its preparation method, except pressing raw material with MgO:TiO2Outside=6:5 molar ratio mixes, all the other steps are with embodiment 1.
Performance test shows: 1360 DEG C of sintering 4 hours, and its DIELECTRIC CONSTANTSrBe 16.4, temperature coefficient of resonance frequency τfFor-55.3ppm/ DEG C, Q × f value is 382,500GHz (f0=7.534GHz)。
Embodiment 5
Preparation Mg7Ti6O19Ceramics sample;
Its preparation method, except pressing raw material with MgO:TiO2Outside=7:6 molar ratio mixes, all the other steps are with embodiment 1.
Performance test shows: 1360 DEG C of sintering 4 hours, and its DIELECTRIC CONSTANTSrBe 16.5, temperature coefficient of resonance frequency τfFor-57.3ppm/ DEG C, Q × f value is 368,400GHz (f0=7.522GHz)。
Embodiment 6
Preparation Mg8Ti7O22Ceramics sample;
Its preparation method, except pressing raw material with MgO:TiO2Outside=8:7 molar ratio mixes, all the other steps are with embodiment 1.
Performance test shows: 1360 DEG C of sintering 4 hours, and its DIELECTRIC CONSTANTSrBe 17.1, temperature coefficient of resonance frequency τfFor-58.5ppm/ DEG C, Q × f value is 315,000GHz (f0=7.672GHz)。
Embodiment 7
Preparation Mg21Ti20O61Ceramics sample;
Its preparation method, except pressing raw material with MgO:TiO2=21:20 molar ratio mixes and sintering temperature is 1380 DEG COutward, all the other steps are with embodiment 1.
Performance test shows: 1380 DEG C of sintering 4 hours, and its DIELECTRIC CONSTANTSrBe 16.6, temperature coefficient of resonance frequency τfFor-61.1ppm/ DEG C, Q × f value is 250,100GHz (f0=7.592GHz)。
Embodiment 8
Preparation Mg31Ti30O91Ceramics sample;
Its preparation method, except pressing raw material with MgO:TiO2Outside=31:30 molar ratio mixes, the same embodiment of all the other steps1。
Performance test shows: 1360 DEG C of sintering 4 hours, and its DIELECTRIC CONSTANTSrBe 16.9, temperature coefficient of resonance frequency τfFor-60.7ppm/ DEG C, Q × f value is 237,300GHz (f0=7.652GHz)。
Embodiment 9
Preparation Mg41Ti40O121Ceramics sample;
Its preparation method, except pressing raw material with MgO:TiO2Outside=41:40 molar ratio mixes, the same embodiment of all the other steps1。
Performance test shows: 1360 DEG C of sintering 4 hours, and its DIELECTRIC CONSTANTSrBe 17.4, temperature coefficient of resonance frequency τfFor-62.1ppm/ DEG C, Q × f value is 186,500GHz (f0=7.501GHz)。
Embodiment 10
Preparation Mg51Ti50O151Ceramics sample;
Its preparation method, except pressing raw material with MgO:TiO2Outside=51:50 molar ratio mixes, all the other steps are with embodiment 1.
Performance test shows: 1360 DEG C of sintering 4 hours, and its DIELECTRIC CONSTANTSrBe 17.9, temperature coefficient of resonance frequency τfFor-59.1ppm/ DEG C, Q × f value is 166,300GHz (f0=7.420GHz)。
Contrast sample Microwave ceramics main component Sintering temperature εr τf(ppm/℃) Q×f (GHz)
Contrast sample 1 MgTiO3 1200℃ 17 -50 166,400
Contrast sample 2 Mg2TiO4 1500℃ 14.2 -60 160,000

Claims (3)

1. a ultra-low loss limit class Mgn+1TinO3n+1Microwave ceramics, is characterized in that, its composition general formula is: Mgn+ 1TinO3n+1, in formula, n=2,3,4,5,6,7 ... 50.
2. a ultra-low loss limit class Mgn+1TinO3n+1The preparation method of microwave ceramics, is characterized in that, comprises the steps:
(1) synthetic Mgn+1TinO3n+1Powder: design sample constituents: n=2,3,4,5,6,7 ... 50, and claim according to stoichiometric proportionContent of starting materials powder MgO and TiO2Mix, then mixed powder is incubated at 1100 DEG C to 2 hours synthetic Mgn+1TinO3n+1Powder;
(2) Mg step (1) being obtainedn+1TinO3n+1Synthetic powder, through secondary ball milling, adds polyvinyl alcohol to press on forming machineMake cylindrical base substrate;
(3) the cylindrical base substrate of step (2) gained sintering at 1340 ~ 1380 DEG C is become to porcelain in 4 hours, obtain the ultra-low loss limitClass Mgn+1TinO3n+1Microwave ceramics.
3. ultra-low loss limit class Mg according to claim 2n+1TinO3n+1The preparation method of microwave ceramics, its feature existsIn, the optimum sintering temperature of the described cylindrical base substrate of step (2) is 1360 DEG C.
CN201610057795.9A 2016-01-28 2016-01-28 Ultralow loss limit type Mgn+1TinO3n+1 microwave ceramic and making method thereof Pending CN105601272A (en)

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CN108033786A (en) * 2017-12-15 2018-05-15 无锡鑫圣慧龙纳米陶瓷技术有限公司 A kind of high q-factor magnesium titanium series microwave dielectric ceramic and preparation method thereof
CN108249913A (en) * 2018-01-25 2018-07-06 无锡鑫圣慧龙纳米陶瓷技术有限公司 A kind of temperature-stable ceramics as low-loss microwave medium and its preparation method and application
CN109320245A (en) * 2018-11-29 2019-02-12 无锡鑫圣慧龙纳米陶瓷技术有限公司 A kind of microwave-medium ceramics and preparation method thereof
CN115340374A (en) * 2022-08-16 2022-11-15 无锡市高宇晟新材料科技有限公司 MgTiO 3 Base composite microwave dielectric ceramic and preparation method and application thereof

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108033786A (en) * 2017-12-15 2018-05-15 无锡鑫圣慧龙纳米陶瓷技术有限公司 A kind of high q-factor magnesium titanium series microwave dielectric ceramic and preparation method thereof
CN108249913A (en) * 2018-01-25 2018-07-06 无锡鑫圣慧龙纳米陶瓷技术有限公司 A kind of temperature-stable ceramics as low-loss microwave medium and its preparation method and application
CN108249913B (en) * 2018-01-25 2020-10-16 无锡鑫圣慧龙纳米陶瓷技术有限公司 Temperature-stable low-loss microwave dielectric ceramic and preparation method and application thereof
CN109320245A (en) * 2018-11-29 2019-02-12 无锡鑫圣慧龙纳米陶瓷技术有限公司 A kind of microwave-medium ceramics and preparation method thereof
CN109320245B (en) * 2018-11-29 2021-04-27 无锡鑫圣慧龙纳米陶瓷技术有限公司 Microwave dielectric ceramic and preparation method thereof
CN115340374A (en) * 2022-08-16 2022-11-15 无锡市高宇晟新材料科技有限公司 MgTiO 3 Base composite microwave dielectric ceramic and preparation method and application thereof

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Application publication date: 20160525