CN104671773B - A kind of low dielectric constant microwave dielectric ceramic material and preparation method thereof - Google Patents
A kind of low dielectric constant microwave dielectric ceramic material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of low dielectric constant microwave dielectric ceramic material and preparation method thereof, the thing of this ceramic material includes Li mutually2Mg3SnO6And Mg2SnO4, wherein Li2Mg3SnO6Content be 42wt%～95wt%, remaining is Mg2SnO4；The dielectric constant of this ceramic material is 7.8～8.8, and dielectric loss is 0.00007～0.00019, and Q × f is 72000～123000GHz, and temperature coefficient of resonance frequency is 40～31ppm/ DEG C, uses high-temperature solid phase reaction method to be prepared from.Microwave dielectric ceramic materials preparation method of the present invention is simple, raw materials used abundant, with low cost, be conducive to industrialized production, obtained microwave-medium ceramics stable performance, important application prospect and economic worth can be had on electronic circuit, microwave mobile communication, satellite communication, radar system field as electronic circuit substrate, dielectric resonator, wave filter, high frequency satellite microwave device substrate and the manufacture materials'use of microstrip line.
Description
Technical field
The invention belongs to electronic information material and device arts thereof, be specifically related to a kind of dielectric constant microwave and be situated between
Ceramics and preparation method thereof.
Background technology
Microwave-medium ceramics refers to be applied in microwave frequency band (300MHz～300GHz) circuit as medium material
Expect the ceramic material of one or more functions.Ideal microwave media ceramic has suitable dielectric constant (εr)、
High quality factor (Q × f) and the temperature coefficient of resonance frequency (τ gone to zerof).With microwave-medium ceramics making
The components and parts such as resonator, wave filter, Microwave integrated circuit substrate, in mobile communication, WLAN, military affairs
The modern communication technologys such as communication are widely applied.Additionally, constantly carrying along with communication equipment running frequency
Height, system loss and caloric value increase therewith, and system stability is gradually deteriorated.Bring for overcoming frequency to widen
Great number of issues, needs exploitation high q-factor and ε low, middle badlyr(10≤εr≤ 25) and nearly zero τfThe microwave-medium material of value
Material.Low εrThe coupling interaction loss between material and electrode can be reduced, and improve signal transmission rate, low dielectric
Loss is conducive to improving the alternative of device operating frequencies, nearly zero τfThe frequency temperature being favorably improved device is steady
Determine characteristic.
Traditional low εrPottery is mainly by glass-ceramic (devitrified glass), glass+ceramics (multiphase ceramic) etc.
Composition.Although glass ceramic material can sinter at a lower temperature, but due to the introducing of a large amount of low-melting glass materials,
Add the dielectric loss of material, be difficult to use in high frequency.For adapting to electronic devices and components to high frequency, high speed direction
The needs of development, novel low-k (εr< 15), high q-factor microwave dielectric ceramic materials is increasingly by domestic
The attention of outer material scholar.The low ε of typical case reported in recent yearsr, high q-factor material system specifically include that M2SiO4
(M=Mg, Zn) base, Al2O3Base, A4M2O9(A=Co, Mg；B=Nb, Ta) and spinel structure
M2SnO4(M=Cu, Zn, Ni etc.) base microwave dielectric ceramics.
Summary of the invention
The technical problem to be solved is to provide a kind of novel low-k that has and is situated between with excellent microwave
Microwave dielectric ceramic materials of electrical property and preparation method thereof.
Solve above-mentioned technical problem and be the technical scheme is that the thing of this low dielectric constant microwave dielectric ceramic material
Include Li mutually2Mg3SnO6And Mg2SnO4, wherein Li2Mg3SnO6Content be 42wt%～95wt%, remaining is
Mg2SnO4；The dielectric constant of this ceramic material is 7.8～8.8, and dielectric loss is 0.00007～0.00019, Q × f
Being 72000～123000GHz, temperature coefficient of resonance frequency is-40～-31ppm/ DEG C.
Li in above-mentioned ceramic material2Mg3SnO6Content most preferably 52wt%, remaining is Mg2SnO4, its dielectric is normal
Number is 7.8, and dielectric loss is 0.00007, and 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
By the purity Li more than 99.9%2CO3Powder, MgO powder, SnO2Powder adds after mixing for 1:3:1 in molar ratio
Enter in ball grinder, with zirconia ball as abrading-ball, dehydrated alcohol as abrasive media, be sufficiently mixed ball milling 6～10 little
Time, 80～100 DEG C are dried.
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, with zirconia ball as abrading-ball, dehydrated alcohol as abrasive media, the most mixed
Closing ball milling 6～10 hours, 80～100 DEG C are dried.
4, pelletize, molding
In step 3 dried pre-burning powder add mass fraction be 5% polyvinyl alcohol water solution pelletize, cross 80～
160 mesh sieves, then it is pressed into cylindrical green body with powder compressing machine.
5, sintering
Cylindrical green body step 4 obtained sinters 2～10 hours at 1320～1400 DEG C, obtains low dielectric normal
Number microwave dielectric ceramic materials.
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, beneficially work
Industry metaplasia is produced, and obtained microwave-medium ceramics has low-k and excellent microwave dielectric property, can be as electricity
Sub-line base board, dielectric resonator, wave filter, high frequency satellite microwave device substrate and the manufacture materials'use of microstrip line,
Electronic circuit, microwave mobile communication, satellite communication, radar system field have important application prospect and economic valency
Value.
Accompanying drawing explanation
Fig. 1 is the X-ray diffractogram of the low dielectric constant microwave dielectric ceramic material of embodiment 1～7 preparation.
Detailed description of the invention
The present invention is described in more detail with embodiment below in conjunction with the accompanying drawings, but protection scope of the present invention not only limits
In these embodiments.
Embodiment 1
1, batch mixing
Take the purity Li more than 99.9%2CO3Powder 2.500g (0.033mol), MgO powder 4.012g (0.099mol),
SnO2Powder 5.023g (0.033mol) mix homogeneously, by raw mixture with zirconia ball, dehydrated alcohol by matter
Amount ratio is in 1: 2: 2 loading ball grinder, and 360 revs/min are sufficiently mixed ball milling 8 hours, and 80～100 DEG C are dried
12 hours.
2, pre-burning
Dried for step 1 mixture is placed in alumina crucible, is warming up to the heating rate of 2 DEG C/min
1000 DEG C, constant temperature pre-burning 4 hours, obtain pre-burning powder.
3, rerolling
It is in 1: 2: 2 loading ball grinder in mass ratio by pre-burning powder and zirconia ball, dehydrated alcohol, the most mixed
Closing ball milling 8 hours, 80～100 DEG C are dried 12 hours.
4, pelletize, molding
The polyvinyl alcohol water solution that mass fraction is 5% of its quality 5% is added in step 3 dried pre-burning powder
Pelletize, cross 120 mesh sieves, then with powder compressing machine be compressed under 4MPa pressure a diameter of 11.5mm,
Thickness is the cylindrical green body of 5.5mm.
5, sintering
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, other steps and reality
Execute example 1 identical, 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, other steps and reality
Execute example 1 identical, 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, other steps and reality
Execute example 1 identical, 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, other steps and reality
Execute example 1 identical, 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, other steps and reality
Execute example 1 identical, 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, other steps and reality
Execute example 1 identical, obtain low dielectric constant microwave dielectric ceramic material.
The low dielectric constant microwave dielectric ceramic material that embodiment 1～7 is prepared by inventor uses
RagukuD/Max2550 type (Japan) X-ray diffractometer characterizes, and result is shown in Fig. 1.As seen from Figure 1, institute
The thing phase composition of the low dielectric constant microwave dielectric ceramic material of preparation is Li2Mg3SnO6And Mg2SnO4, each thing phase
Weight/mass percentage composition be shown in Table 1.
The thing phase composition of table 1 microwave dielectric ceramic materials of the present invention
| Li2Mg3SnO6(wt%) | Mg2SnO4(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 |
Ceramic material grinding and polishing post-treatment prepared by embodiment 1～7 is become a diameter of 9～10mm, height by inventor
The cylinder of 5mm, with vector network analyzer, closes chamber the resonance method cooperation high-low temperature incubator test ceramic microwave dielectric
Performance.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, the microwave dielectric ceramic materials of embodiment 1～7 preparation has low-k, ultralow damage
Consumption and high Q × f value, temperature coefficient of resonance frequency between-40～-31ppm/ DEG C, its sintering range width (1320～
1400 DEG C) and stable performance, it is the microwave of a kind of novel microwave dielectric property with low-k and excellence
Medium ceramic material.
Claims (5)
1. a low dielectric constant microwave dielectric ceramic material, it is characterised in that: the thing of this ceramic material includes mutually
Li2Mg3SnO6And Mg2SnO4, wherein Li2Mg3SnO6Content be 42wt%～95wt%, remaining is Mg2SnO4；
The dielectric constant of this ceramic material is 7.8～8.8, and dielectric loss is 0.00007～0.00019, Q × f be 72000～
123000GHz, temperature coefficient of resonance frequency is-40～-31ppm/ DEG C.
Low dielectric constant microwave dielectric ceramic material the most according to claim 1, it is characterised in that: this pottery
The thing of material includes Li mutually2Mg3SnO6And Mg2SnO4, wherein Li2Mg3SnO6Content be 52wt%, remaining
For Mg2SnO4；The dielectric constant of this ceramic material is 7.8, and dielectric loss is 0.00007, and Q × f is 123000GHz,
Temperature coefficient of resonance frequency is-32ppm/ DEG C.
3. a preparation method for the low dielectric constant microwave dielectric ceramic material described in claim 1, its feature
It is that it is made up of following step:
(1) batch mixing
By the purity Li more than 99.9%2CO3Powder, MgO powder, SnO2Powder adds after mixing for 1:3:1 in molar ratio
Enter in ball grinder, with zirconia ball as abrading-ball, dehydrated alcohol as abrasive media, be sufficiently mixed ball milling 6～10 little
Time, 80～100 DEG C are dried；
(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, with zirconia ball as abrading-ball, dehydrated alcohol as abrasive media, the most mixed
Closing ball milling 6～10 hours, 80～100 DEG C are dried；
(4) pelletize, molding
Polyvinyl alcohol water solution pelletize, described polyvinyl alcohol water is added in step (3) dried mixture
In solution, the mass fraction of polyvinyl alcohol is 5%, crosses 80～160 mesh sieves, then is pressed into cylinder with powder compressing machine
Shape green compact；
(5) sintering
Cylindrical green body step (4) obtained sinters 2～10 hours at 1320～1400 DEG C, obtains low dielectric
Constant microwave dielectric ceramic materials.
The preparation method of low dielectric constant microwave dielectric ceramic material the most according to claim 3, its feature
It is: in described step (2), by step (1) dried mixture 1000 DEG C of pre-burnings 4 hours.
The preparation method of low dielectric constant microwave dielectric ceramic material the most according to claim 3, its feature
Being: in described step (5), cylindrical green body step (4) obtained sinters 6 hours at 1360 DEG C.
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| 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 |
| 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 |
| 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 |
| 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 |
| 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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