CN104671773A - Low-dielectric-constant microwave dielectric ceramic material and preparation method thereof - Google Patents
Low-dielectric-constant microwave dielectric ceramic material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a low-dielectric-constant microwave dielectric ceramic material and a preparation method thereof. The ceramic material comprises 42wt%-95wt% of Li2Mg3SnO6 and Mg2SnO4 in balancing amount. The dielectric constant of the ceramic material is 7.8-8.8, the dielectric loss is 0.00,007-0.00,019, Q*f is 72,000-123,000GHz, and the temperature coefficient of resonant frequency is -40ppm/DEG C to -31ppm/DEG C. The ceramic material is prepared by a high-temperature solid-phase reaction method. The preparation method of the ceramic material is simple, the raw materials are abundant and low in cost, industrial production is facilitated, and the prepared ceramic material has stable performance, can be used as a material for manufacturing an electronic circuit substrate, a dielectric resonator, a filter, a high-frequency satellite microwave device substrate and a microstrip line, and has important application prospects and economic values in the fields of electronic circuit, microwave mobile communication, satellite communication and radar system.
Description
Technical field
The invention belongs to electronic information material and device arts thereof, be specifically related to a kind of low dielectric constant microwave dielectric ceramic material and preparation method thereof.
Background technology
Microwave-medium ceramics refers to the stupalith being applied to and completing one or more functions in microwave frequency band (300MHz ~ 300GHz) circuit as dielectric material.Ideal microwave media ceramic has suitable specific inductivity (ε
r), high quality factor (Q × f) and the temperature coefficient of resonance frequency (τ that goes to zero
f).With the components and parts such as resonator, wave filter, Microwave integrated circuit substrate that microwave-medium ceramics makes, be widely applied in the modern communication technologys such as mobile communication, WLAN (wireless local area network), military communication.In addition, along with improving constantly of signal equipment running frequency, system loss and thermal value increase thereupon, and system stability is deteriorated gradually.Widening for overcoming frequency the great number of issues brought, needing exploitation high q-factor and low, middle ε badly
r(10≤ε
r≤ 25) and nearly zero τ
fthe microwave dielectric material of value.Low ε
rcan reduce the coupling interaction loss between material and electrode, and improve signal transmission rate, low-dielectric loss is conducive to the alternative improving device operating frequencies, nearly zero τ
fcontribute to the frequency temperature stabilising characteristic improving device.
Traditional low ε
rpottery is mainly made up of glass-ceramic (devitrified glass), glass+ceramics (multiphase ceramic) etc.Although glass ceramic material can sinter at a lower temperature, due to the introducing of a large amount of low melting glass material, add the dielectric loss of material, be difficult to use in high frequency.For adapting to the needs of electronic devices and components to high frequency, high speed future development, novel low-k (ε
r<15), high q-factor microwave dielectric ceramic materials is more and more subject to the attention of domestic and international material scholar.The low ε of the typical case reported in recent years
r, high q-factor material system mainly comprises: M
2siO
4(M=Mg, Zn) base, Al
2o
3base, A
4m
2o
9(A=Co, Mg; B=Nb, Ta) and spinel structure M
2snO
4(M=Cu, Zn, Ni etc.) base microwave dielectric ceramics.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind ofly novel has microwave dielectric ceramic materials of low-k and excellent microwave dielectric property and preparation method thereof.
Solving the problems of the technologies described above adopted technical scheme is: the thing of this low dielectric constant microwave dielectric ceramic material comprises Li mutually
2mg
3snO
6and Mg
2snO
4, wherein Li
2mg
3snO
6content be 42wt% ~ 95wt%, all the other are Mg
2snO
4; The specific inductivity of this stupalith is 7.8 ~ 8.8, and dielectric loss is 0.00007 ~ 0.00019, Q × f is 72000 ~ 123000GHz, and temperature coefficient of resonance frequency is-40 ~-31ppm/ DEG C.
Li in above-mentioned stupalith
2mg
3snO
6content the best be 52wt%, all the other are Mg
2snO
4, its specific inductivity is 7.8, and dielectric loss is 0.00007, Q × f is 123000GHz, and temperature coefficient of resonance frequency is-32ppm/ DEG C.
The preparation method of above-mentioned low dielectric constant microwave dielectric ceramic material is made up of following step:
1, batch mixing
Purity is greater than the Li of 99.9%
2cO
3powder, MgO powder, SnO
2powder for adding in ball grinder after 1:3:1 mixing, take zirconia ball as abrading-ball in molar ratio, dehydrated alcohol is grinding medium, abundant mixing and ball milling 6 ~ 10 hours, 80 ~ 100 DEG C of dryings.
2, pre-burning
By dried for step 1 mixture 1000 ~ 1200 DEG C of pre-burnings 4 ~ 6 hours, obtain pre-burning powder.
3, rerolling
Pre-burning powder is added in ball grinder, take zirconia ball as abrading-ball, dehydrated alcohol is grinding medium, abundant mixing and ball milling 6 ~ 10 hours, 80 ~ 100 DEG C of dryings.
4, granulation, shaping
In the dried pre-burning powder of step 3, add the polyvinyl alcohol water solution granulation that massfraction is 5%, cross 80 ~ 160 mesh sieves, then be pressed into cylindrical green body with powder compressing machine.
5, sinter
Cylindrical green body step 4 obtained sinters 2 ~ 10 hours at 1320 ~ 1400 DEG C, obtains low dielectric constant microwave dielectric ceramic material.
In above-mentioned steps 2, preferably by dried for step 1 mixture 1000 DEG C of pre-burnings 4 hours.
In above-mentioned steps 5, cylindrical green body step 4 obtained sinters 6 hours at 1360 DEG C.
Microwave dielectric ceramic materials preparation method of the present invention is simple, raw materials used abundant, with low cost, be conducive to suitability for industrialized production, obtained microwave-medium ceramics has low-k and excellent microwave dielectric property, the manufactured materials that can be used as electronic circuit substrate, dielectric resonator, wave filter, high frequency satellite microwave device substrate and microstrip line uses, and electronic circuit, microwave mobile communication, satellite communications, radar system field have important application prospect and economic worth.
Accompanying drawing explanation
Fig. 1 is the X-ray diffractogram of low dielectric constant microwave dielectric ceramic material prepared by embodiment 1 ~ 7.
Embodiment
Below in conjunction with drawings and Examples, the present invention is described in more detail, but protection scope of the present invention is not limited only to these embodiments.
Embodiment 1
1, batch mixing
Get the Li that purity is greater than 99.9%
2cO
3powder 2.500g (0.033mol), MgO powder 4.012g (0.099mol), SnO
2powder 5.023g (0.033mol) mixes, and is in mass ratio to load in ball grinder at 1: 2: 2 by raw mixture and zirconia ball, dehydrated alcohol, 360 revs/min of abundant mixing and ball milling 8 hours, 80 ~ 100 DEG C of dryings 12 hours.
2, pre-burning
Be placed in alumina crucible by dried for step 1 mixture, be warming up to 1000 DEG C with the temperature rise rate of 2 DEG C/min, constant temperature pre-burning 4 hours, obtains pre-burning powder.
3, rerolling
Be load in ball grinder at 1: 2: 2 in mass ratio by pre-burning powder and zirconia ball, dehydrated alcohol, abundant mixing and ball milling 8 hours, 80 ~ 100 DEG C of dryings 12 hours.
4, granulation, shaping
The massfraction adding its quality 5% in the dried pre-burning powder of step 3 is the polyvinyl alcohol water solution granulation of 5%, crosses 120 mesh sieves, then under 4MPa pressure, is pressed into powder compressing machine that diameter is 11.5mm, thickness is the cylindrical green body of 5.5mm.
5, sinter
Cylindrical green body step 4 obtained sinters 6 hours at 1360 DEG C, obtains low dielectric constant microwave dielectric ceramic material.
Embodiment 2
In the step 5 of embodiment 1, cylindrical green body is sintered 6 hours at 1340 DEG C, and other steps are identical with embodiment 1, obtain low dielectric constant microwave dielectric ceramic material.
Embodiment 3
In the step 5 of embodiment 1, cylindrical green body is sintered 6 hours at 1320 DEG C, and other steps are identical with embodiment 1, obtain low dielectric constant microwave dielectric ceramic material.
Embodiment 4
In the step 5 of embodiment 1, cylindrical green body is sintered 6 hours at 1380 DEG C, and other steps are identical with embodiment 1, obtain low dielectric constant microwave dielectric ceramic material.
Embodiment 5
In the step 5 of embodiment 1, cylindrical green body is sintered 6 hours at 1400 DEG C, and other steps are identical with embodiment 1, obtain low dielectric constant microwave dielectric ceramic material.
Embodiment 6
In the step 5 of embodiment 1, cylindrical green body is sintered 2 hours at 1360 DEG C, and other steps are identical with embodiment 1, obtain low dielectric constant microwave dielectric ceramic material.
Embodiment 7
In the step 5 of embodiment 1, cylindrical green body is sintered 10 hours at 1360 DEG C, and other steps are identical with embodiment 1, obtain low dielectric constant microwave dielectric ceramic material.
The low dielectric constant microwave dielectric ceramic material that embodiment 1 ~ 7 is prepared by contriver adopts RagukuD/Max2550 type (Japan) X-ray diffractometer to characterize, and the results are shown in Figure 1.As seen from Figure 1, the thing phase composite of prepared low dielectric constant microwave dielectric ceramic material is Li
2mg
3snO
6and Mg
2snO
4, the mass percentage of each thing phase is in table 1.
The thing phase composite of table 1 microwave dielectric ceramic materials of the present invention
Li 2Mg 3SnO 6(wt%) | Mg 2SnO 4(wt%) | |
Embodiment 1 | 52 | 48 |
Embodiment 2 | 86 | 14 |
Embodiment 3 | 95 | 5 |
Embodiment 4 | 44 | 56 |
Embodiment 5 | 79 | 21 |
Embodiment 6 | 65 | 35 |
Embodiment 7 | 42 | 58 |
The stupalith grinding and polishing post-treatment that embodiment 1 ~ 7 is prepared by contriver becomes diameter to be the cylinder of 9 ~ 10mm, high 5mm, with vector network analyzer, closes chamber resonance method and coordinates high-low temperature incubator test ceramic microwave dielectric properties.The results are shown in Table 2.
The dielectric properties of table 2 microwave dielectric ceramic materials of the present invention and sintering characteristic
From table 2, microwave dielectric ceramic materials prepared by embodiment 1 ~ 7 has low-k, ultra-low loss and high Q × f value, temperature coefficient of resonance frequency is between-40 ~-31ppm/ DEG C, its sintering range wide (1320 ~ 1400 DEG C) and stable performance are a kind of novel microwave dielectric ceramic materials with low-k and excellent microwave dielectric property.
Claims (5)
1. a low dielectric constant microwave dielectric ceramic material, is characterized in that: the thing of this stupalith comprises Li mutually
2mg
3snO
6and Mg
2snO
4, wherein Li
2mg
3snO
6content be 42wt% ~ 95wt%, all the other are Mg
2snO
4; The specific inductivity of this stupalith is 7.8 ~ 8.8, and dielectric loss is 0.00007 ~ 0.00019, Q × f is 72000 ~ 123000GHz, and temperature coefficient of resonance frequency is-40 ~-31ppm/ DEG C.
2. low dielectric constant microwave dielectric ceramic material according to claim 1, is characterized in that: the thing of this stupalith comprises Li mutually
2mg
3snO
6and Mg
2snO
4, wherein Li
2mg
3snO
6content be 52wt%, all the other are Mg
2snO
4; The specific inductivity of this stupalith is 7.8, and dielectric loss is 0.00007, Q × f is 123000GHz, and temperature coefficient of resonance frequency is-32ppm/ DEG C.
3. a preparation method for low dielectric constant microwave dielectric ceramic material according to claim 1, is characterized in that it is made up of following step:
(1) batch mixing
Purity is greater than the Li of 99.9%
2cO
3powder, MgO powder, SnO
2powder for adding in ball grinder after 1:3:1 mixing, take zirconia ball as abrading-ball in molar ratio, dehydrated alcohol is grinding medium, abundant mixing and ball milling 6 ~ 10 hours, 80 ~ 100 DEG C of dryings;
(2) pre-burning
By step (1) dried mixture 1000 ~ 1200 DEG C of pre-burnings 4 ~ 6 hours, obtain pre-burning powder;
(3) rerolling
Pre-burning powder is added in ball grinder, take zirconia ball as abrading-ball, dehydrated alcohol is grinding medium, abundant mixing and ball milling 6 ~ 10 hours, 80 ~ 100 DEG C of dryings;
(4) granulation, shaping
In the dried pre-burning powder of step (3), add the polyvinyl alcohol water solution granulation that massfraction is 5%, cross 80 ~ 160 mesh sieves, then be pressed into cylindrical green body with powder compressing machine;
(5) sinter
Cylindrical green body step (4) obtained sinters 2 ~ 10 hours at 1320 ~ 1400 DEG C, obtains low dielectric constant microwave dielectric ceramic material.
4. the preparation method of low dielectric constant microwave dielectric ceramic material according to claim 3, is characterized in that: in described step (2), by step (1) dried mixture 1000 DEG C of pre-burnings 4 hours.
5. the preparation method of low dielectric constant microwave dielectric ceramic material according to claim 3, is characterized in that: in described step (5), and cylindrical green body step (4) obtained sinters 6 hours at 1360 DEG C.
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Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN106187158A (en) * | 2016-07-19 | 2016-12-07 | 桂林理工大学 | High quality factor temperature-stable ultralow dielectric microwave dielectric ceramic Li2mgSnO4 |
CN106187156A (en) * | 2016-07-19 | 2016-12-07 | 桂林理工大学 | High quality factor temperature-stable dielectric constant microwave dielectric ceramic Li2baSnO4 |
CN106587968A (en) * | 2016-11-08 | 2017-04-26 | 桂林理工大学 | Microwave dielectric ceramic material with low dielectric constant and preparation method thereof |
CN110357618A (en) * | 2019-06-20 | 2019-10-22 | 安徽理工大学 | Low-temperature sintering temperature-stable zirconates microwave dielectric ceramic materials and preparation method thereof |
CN113264761A (en) * | 2021-06-07 | 2021-08-17 | 安徽理工大学 | Low-temperature sintering temperature-stable stannate microwave dielectric ceramic and preparation method thereof |
Citations (1)
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CN103232242A (en) * | 2013-04-22 | 2013-08-07 | 江苏大学 | BMN (bismuth magnesium niobate)-based microwave dielectric ceramic material and preparation method thereof |
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2015
- 2015-02-09 CN CN201510066715.1A patent/CN104671773B/en active Active
Patent Citations (1)
Publication number | Priority date | Publication date | Assignee | Title |
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CN103232242A (en) * | 2013-04-22 | 2013-08-07 | 江苏大学 | BMN (bismuth magnesium niobate)-based microwave dielectric ceramic material and preparation method thereof |
Non-Patent Citations (1)
Title |
---|
C. W. LIU ET AL.: ""Phase formation, microstructure and microwave dielectric properties of Li2SnO3-MO (M=Mg, Zn,) ceramics"", 《J ELECTROCERAM》 * |
Cited By (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN106187158A (en) * | 2016-07-19 | 2016-12-07 | 桂林理工大学 | High quality factor temperature-stable ultralow dielectric microwave dielectric ceramic Li2mgSnO4 |
CN106187156A (en) * | 2016-07-19 | 2016-12-07 | 桂林理工大学 | High quality factor temperature-stable dielectric constant microwave dielectric ceramic Li2baSnO4 |
CN106587968A (en) * | 2016-11-08 | 2017-04-26 | 桂林理工大学 | Microwave dielectric ceramic material with low dielectric constant and preparation method thereof |
CN110357618A (en) * | 2019-06-20 | 2019-10-22 | 安徽理工大学 | Low-temperature sintering temperature-stable zirconates microwave dielectric ceramic materials and preparation method thereof |
CN110357618B (en) * | 2019-06-20 | 2021-08-24 | 安徽理工大学 | Low-temperature sintering temperature-stable zirconate microwave dielectric ceramic material and preparation method thereof |
CN113264761A (en) * | 2021-06-07 | 2021-08-17 | 安徽理工大学 | Low-temperature sintering temperature-stable stannate microwave dielectric ceramic and preparation method thereof |
CN113264761B (en) * | 2021-06-07 | 2022-07-08 | 安徽理工大学 | Low-temperature sintering temperature-stable stannate microwave dielectric ceramic and preparation method thereof |
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