CN103073285B - A kind of low-loss microwave dielectric ceramic with medium dielectric constant and its preparation technology - Google Patents
A kind of low-loss microwave dielectric ceramic with medium dielectric constant and its preparation technology Download PDFInfo
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Abstract
The present invention relates to a kind of low-loss microwave dielectric ceramic with medium dielectric constant and its preparation technology.XCaTiO3yLa of the present invention2O3·z Al2O3+awt%Al2O3It is into main point, Al2O3It is accessory ingredient, using suitable parameter, during successfully solving La substitutions Nd, sintering temperature is high and material Q relatively low technological difficulties, the invention has the advantages that following three advantages：1）La2O3Substitution Nd2O3This can be significantly reduced to；2）Improve Q × f0；3）Sintering temperature is reduced, the energy has been saved.
Description
Technical field
Microwave-medium ceramics formula the invention belongs to a kind of high quality factor and preparation method thereof, particularly a MTiO3-
LnAlO3It is composite perofskite microwave dielectric material and preparation method thereof.It is widely used in mobile phone, automobile telephone, TV to defend
In the systems such as star receiver, GPS, wireless local access and various radars.
Background technology
Microwave-medium ceramics are the core materials of microwave device.Due to microwave technology equipment to miniaturization with it is integrated, especially
It is that civilian high-volume, low price direction develop rapidly, be have developed large quantities of for various microwave frequency bands
Microwave dielectric ceramic materials.It is applied to the media ceramic of microwave circuit, it is necessary to meet following dielectric characterization requirement：1）Phase higher
To dielectric constant Er, the size of medium ceramic material relative dielectric constant is typically determined according to applying frequency.Applying frequency is 0.8
During ~ 4GHz (low side), Er ＞ 50；During 4 ~ 8GHz (middle-end), 30≤Er≤50；During 8 ~ 18GHz (middle-end), Er≤30；2）It is high
Quality factor q, to improve selecting frequency characteristic, typically require Q × f0≥5000；3）Frequency-temperature coefficient τ f close to zero are ensureing
Device has good temperature stability, and dielectric resonator device is typically all that the frequency of certain vibration mode of microwave-medium ceramics is made
It is its centre frequency.If τ f are big, showing the centre frequency of device will produce big drift, device because of the change of temperature
Part will be unable to high stable work.In microwave dielectric ceramic with medium dielectric constant system, MTiO3-LnAlO3(M:Sr,Ca;Ln:La,
Nd, Sm) CaTiO in system3-NdAlO3There is excellent microwave dielectric property, be widely used in microwave dielectric ceramic with medium dielectric constant material
Material, with respect to practicality microwave CaTiO3-NdAlO3Have the following disadvantages：1）CaTiO3-NdAlO3Based material sintering temperature is higher,
1600 DEG C could be densified ceramics；2）CaTiO3-NdAlO3System, Q × f0≤30000；3）As the price of rare earth element nd is continuous
Go up, do not meet the developing direction of microwave dielectric ceramic materials low price.
The content of the invention
The present invention is directed to drawbacks described above, and purpose caters to the miniaturization of tracking exchage microwave frequency, high frequency needs, it is intended to carry
There is microwave-medium ceramics formula of high quality factor and preparation method thereof for one, with CaTiO3-LnAlO3It is system right to study
As using Al2O3Be sintering aid, collaboration reduce ceramics sintering temperature, adjust oikocryst phase composition, comprehensive regulation material it is micro-
Ripple dielectric properties.
For this technical solution adopted by the present invention is：The present invention is with xCaTiO3yLa2O3·z Al2O3 + awt%
Al2O3It is into main point, Al2O3It is accessory ingredient, wherein 0.6≤x≤0.8,0. 1≤y≤0.2,0. 1≤z≤0.2,
0.04≤a≤0.16, wherein x, y, z are that mol ratio is added, a is added with mass percent, and awt% is to account for x CaTiO3·
yLa2O3·z Al2O3Mass percent.
The x is that 0.664, y is that 0.168, z is that 0.168, a is 0.12.
A kind of preparation technology of low-loss microwave dielectric ceramic with medium dielectric constant, comprises the following steps：
1）Calcium titanate, the pure lanthanum sesquioxide of analysis, spectroscopic pure alundum (Al2O3) are first pressed into xCaTiO3·yLa2O3·z
Al2O3Chemical formula dispensing mixes, in 1200-1280 DEG C of pre-burning 3.5-4.5h, synthesis principal component x CaTiO3·yLa2O3·z
Al2O3, wherein：0.6≤x≤0.8, 0. 1≤ y≤0.2, 0.1≤ z≤0.2, 0.04≤ a≤0.16；
2) the principal component x CaTiO that will synthesize3·yLa2O3·z Al2O3And accessory ingredient Al2O3Raw material presses x CaTiO3·
yLa2O3·z Al2O3 + awt% Al2O3Synthesis, wherein：0.6≤x≤0.8, 0. 1≤ y≤0.2, 0.1≤ z≤0.2,
0.04≤a≤0.16, awt% is to account for xCaTiO3·yLa2O3·z Al2O3Mass percent, obtained for preparing after mixing
The powder of low-loss microwave dielectric ceramic with medium dielectric constant, powder pressing into circle sheet, in 1420 DEG C of -1600 DEG C of sintering, is protected
Warm 5-7h.
1）In step, each material is placed in polyurethane ball-milling pot, adds zirconia ball and deionization water mill, wherein thing
Material：Deionized water：Zirconium ball weight ratio is 1:1.5:2 ~ 4.5, after mixing and ball milling in QM-BP planetary ball mills dry, after in case
1200-1280 DEG C of pre-burning 3.5-4.5h in formula stove, synthesis principal component xCaTiO3·yLa2O3·zAl2O3。
2）In step, the principal component x CaTiO that will synthesize3·yLa2O3·z Al2O3And awt% Al2O3Raw material presses porcelain
Material composition dispensing, is placed in polyurethane ball-milling pot, is dried after adding zirconia ball and deionization water mill, adds polyvinyl alcohol binder
Agent granulate, after be made circle sheet, 1420 DEG C -1600 DEG C sintering, be incubated 5-7h.
The present invention constituted using above-mentioned formula and preparation method, can obtain Er=44.2-45.1, and high quality factor is low humorous
The microwave-medium ceramics of vibration frequency coefficient τ f, performance indications can meet microwave dielectric ceramic materials requirement.
It is of the invention generally to use CaTiO with existing3-NdAlO3Medium dielectric constant microwave medium system compares, and successfully solves La substitution Nd mistakes
Cheng Zhong, sintering temperature is high and material Q relatively low technological difficulties, the invention has the advantages that following three advantages：1）La2O3Substitution
Nd2O3This can be significantly reduced to；2）Improve Q × f0；3）Sintering temperature is reduced, the energy has been saved.
Brief description of the drawings
Fig. 1,2,3 are the trial curve figure of each characterisitic parameter of the invention.
Specific embodiment
The present invention presses x CaTiO with calcium titanate, the pure lanthanum sesquioxide of analysis, spectroscopic pure alundum (Al2O3) first3·
yLa2O3·z Al2O3Chemical formula dispensing, is placed in polyurethane ball-milling pot, is dried after adding zirconia ball and deionization water mill, dries
After dry in batch-type furnace 1200-1280 DEG C of pre-burning 3.5-4.5h, synthesis principal component xCaTiO3·yLa2O3·zAl2O3。
The principal component x CaTiO that will synthesize3·yLa2O3·z Al2O3And awt% Al2O3Raw material presses porcelain composition dispensing,
It is placed in polyurethane ball-milling pot, is dried after adding zirconia ball and deionization water mill, adds 12wt% polyvinyl alcohol (PVA) bondings
Agent is granulated, and is then pressed into diameter 15mm, and the circle sheet of thickness 7.5mm, in 1420 DEG C of -1600 DEG C of sintering, is incubated 5-7h.
In order to measure the dielectric properties of sample, cylindrical ceramic sample is polished on 1200 mesh silicon carbide papers first, so
Ultrasonic wave is used to be cleaned in alcohol afterwards.Using Ailment E5071B Network Analyzers, according to cavity method microwave frequency
Transverse electric field（TE011Mould）The dielectric properties of sample are analyzed, test frequency is in 4~5GHz.By measuring the humorous of dielectric resonator
Vibration frequency variation with temperature rate obtains the temperature coefficient of resonance frequency of sample, and the temperature range of measurement is -40 DEG C~85 DEG C.
Al2O3Addition effectively promote the densification of matrix, the sintering structure obtained in 1420 DEG C~1500 DEG C sintering ranges is caused
Close, stomata is few.As gradually rising for sintering temperature declines the stomata of matrix, the rising of temperature makes stomata disappear and crystal boundary shifting
Dynamic coordination is carried out, can acceleration of sintering matrix densification, raising system dielectric constant, the weak contact of fine and close sintering intrinsic silicon high
Ion is few, and sintered body loss is also smaller, and relevant each characterisitic parameter is shown in Fig. 1,2,3 referring to each experiment diagram.
The present invention uses parameters, the performance for obtaining such as following table：
| Numbering | x | Y | z | a | Best sintering temperature | Er: | Q*f0 | τf |
| 1 | 0.674 | 0.163 | 0.163 | 0 | 1600℃ | 45.1 | 37643 | +15.5 |
| 2 | 0.664 | 0.168 | 0.168 | 0 | 1600℃ | 44.4 | 38246 | +4.5 |
| 3 | 0.654 | 0.173 | 0.173 | 0 | 1600℃ | 44.2 | 40976 | -10.5 |
| 4 | 0.664 | 0.170 | 0.166 | 0 | 1600℃ | 44.5 | 37536 | +5.2 |
| 5 | 0.664 | 0.168 | 0.168 | 0.04 | 1540℃ | 44.2 | 43707 | 6.4 |
| 6 | 0.664 | 0.168 | 0.168 | 0.08 | 1480℃ | 44.4 | 45308 | 2.8 |
| 7 | 0.664 | 0.168 | 0.168 | 0.12 | 1450℃ | 44.5 | 46258 | 4.5 |
| 8 | 0.664 | 0.168 | 0.168 | 0.16 | 1420℃ | 44.3 | 43781 | 4.8 |
From table, as x increases, the Er increases of ceramics sample, quality factor q * f0Value is reduced, and τ f are to positive temperature system
The movement of number direction.The addition of x can adjust the τ f and Er of material, can be in Q*f0In value allowed band, τ f and Er are adjusted.Al
Being mixed after oikocryst is combined to reduces sintering warm area, when Al content increases, Q*f0Value first increases and lowers afterwards.Sintering temperature is progressively
Reduce.
As seen from table, in this implementation properties optimal components, x=0.664, y=0.168, z=0.168 a=0.12,
Component o'clock 1450 DEG C sintering have optimal microwave dielectric property：Er=44.5, Q*f0=46258GHz, τ f=4.8PPm.
Claims (5)
1. a kind of low-loss microwave dielectric ceramic with medium dielectric constant, it is characterised in that with xCaTiO3yLa2O3·z Al2O3 +
awt% Al2O3It is into main point, Al2O3It is accessory ingredient, wherein 0.6≤x≤0.8,0. 1≤y≤0.2,0. 1≤z≤
0.2,0.04≤a≤0.16, wherein x, y, z are that mol ratio is added, a is added with mass percent, and awt% is to account for x
CaTiO3·yLa2O3·z Al2O3Mass percent.
2. a kind of low-loss microwave dielectric ceramic with medium dielectric constant according to claim 1, it is characterised in that the x is
0.664th, y is that 0.168, z is that 0.168, a is 0.12.
3. a kind of preparation technology of low-loss microwave dielectric ceramic with medium dielectric constant, it is characterised in that comprise the following steps：
1）Calcium titanate, the pure lanthanum sesquioxide of analysis, spectroscopic pure alundum (Al2O3) are first pressed into xCaTiO3·yLa2O3·z Al2O3Change
Formula dispensing mixes, in 1200-1280 DEG C of pre-burning 3.5-4.5h, synthesis principal component x CaTiO3·yLa2O3·z Al2O3, its
In：0.6≤x≤0.8, 0. 1≤ y≤0.2, 0.1≤ z≤0.2, 0.04≤ a≤0.16；
2) the principal component x CaTiO that will synthesize3·yLa2O3·z Al2O3And accessory ingredient Al2O3Raw material presses x CaTiO3·
yLa2O3·z Al2O3 + awt% Al2O3Synthesis, wherein：0.6≤x≤0.8, 0. 1≤ y≤0.2, 0.1≤ z≤0.2,
0.04≤a≤0.16, awt% is to account for xCaTiO3·yLa2O3·z Al2O3Mass percent, obtained for preparing after mixing
The powder of low-loss microwave dielectric ceramic with medium dielectric constant, powder pressing into circle sheet, in 1420 DEG C of -1600 DEG C of sintering, is protected
Warm 5-7h.
4. a kind of preparation technology of low-loss microwave dielectric ceramic with medium dielectric constant according to claim 3, its feature exists
In 1）In step, each material is placed in polyurethane ball-milling pot, adds zirconia ball and deionization water mill, wherein material：Go
Ionized water：Zirconium ball weight ratio is 1:1.5:2 ~ 4.5, after mixing and ball milling in QM-BP planetary ball mills dry, after in batch-type furnace
1200-1280 DEG C of pre-burning 3.5-4.5h, synthesis principal component xCaTiO3·yLa2O3·zAl2O3。
5. a kind of preparation technology of low-loss microwave dielectric ceramic with medium dielectric constant according to claim 3, its feature exists
In,
2）In step, the principal component x CaTiO that will synthesize3·yLa2O3·z Al2O3And awt% Al2O3Raw material is constituted by porcelain
Dispensing, is placed in polyurethane ball-milling pot, is dried after adding zirconia ball and deionization water mill, adds poly (vinyl alcohol) binder to make
Grain, after be made circle sheet, 1420 DEG C -1600 DEG C sintering, be incubated 5-7h.
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| CN110723968A (en) * | 2019-11-06 | 2020-01-24 | 苏州博恩希普新材料科技有限公司 | Microwave dielectric ceramic with high dielectric constant and preparation method thereof |
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| JP2001114553A (en) * | 1999-10-18 | 2001-04-24 | Ngk Spark Plug Co Ltd | Microwave dielectric substance ceramic composition |
| US6377440B1 (en) * | 2000-09-12 | 2002-04-23 | Paratek Microwave, Inc. | Dielectric varactors with offset two-layer electrodes |
| CN101830697A (en) * | 2010-05-10 | 2010-09-15 | 嘉兴佳利电子有限公司 | Medium-temperature sintered high-Q medium microwave ceramics and preparation method thereof |
| CN102531571A (en) * | 2012-02-23 | 2012-07-04 | 华中科技大学 | High-Q-value medium-dielectric-constant microwave dielectric ceramic and preparation method thereof |
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| JP2001114553A (en) * | 1999-10-18 | 2001-04-24 | Ngk Spark Plug Co Ltd | Microwave dielectric substance ceramic composition |
| US6377440B1 (en) * | 2000-09-12 | 2002-04-23 | Paratek Microwave, Inc. | Dielectric varactors with offset two-layer electrodes |
| CN101830697A (en) * | 2010-05-10 | 2010-09-15 | 嘉兴佳利电子有限公司 | Medium-temperature sintered high-Q medium microwave ceramics and preparation method thereof |
| CN102531571A (en) * | 2012-02-23 | 2012-07-04 | 华中科技大学 | High-Q-value medium-dielectric-constant microwave dielectric ceramic and preparation method thereof |
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