CN104692792B - Low-temperature sintering temperature-stable stannate microwave dielectric ceramic materials - Google Patents
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Abstract
The present invention relates to a kind of low-temperature sintering temperature-stable stannate microwave dielectric ceramic materials, the thing of this ceramic material includes Li mutually2Mg3SnO6And Li2SnO3, wherein Li2Mg3SnO6Content be 35.1wt%～79.1wt%, remaining is Li2SnO3；The dielectric constant of this ceramic material is 14.2～14.7, and quality factor are 51300～78300GHz, and temperature coefficient of resonance frequency is 9.1～4.6ppm/ DEG C.The sintering temperature of low-temperature sintering temperature-stable stannate microwave dielectric ceramic materials of the present invention is 840～920 DEG C, overcome the shortcoming that ceramic material sintering temperature is high, temperature coefficient of resonance frequency is bigger than normal, ensure that the temperature stability of material, and it is raw materials used abundant, with low cost to prepare this ceramic material, be conducive to industrialized production, can be widely applied to the manufacture of the microwave devices such as LTCC system, gps antenna, wireless local area wave filter, multilayer dielectricity resonator.
Description
Technical field
The invention belongs to electronic information material and device arts thereof, be specifically related to a kind of microwave dielectric material, special
It it not a kind of low-temperature sintering temperature-stable stannate ceramics material.
Background technology
Microwave-medium ceramics refers to be applied in microwave frequency band (300MHz～300GHz) circuit as dielectric material
Complete 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).The resonance made of microwave-medium ceramics
The components and parts such as device, wave filter, Microwave integrated circuit substrate, at mobile communication, WLAN, military communication etc.
Modern communication technology is widely applied.Along with modern communications equipment is to miniaturization, integrated, high reliability
Developing with cost degradation direction, with LTCC, (Low temperature co-fired ceramic is called for short
LTCC) multi-layer structure design based on technology is to realize the important channel of components and parts miniaturization.LTCC technology is removed
Require that microwave dielectric material has outside good microwave dielectric property, also require that it can be with high conductivity, low melting point
Base metal Ag (960 DEG C) electrode matching co-firing.Additionally, improving constantly along with communication equipment running frequency, it is
System loss and caloric value increase therewith, and system stability is gradually deteriorated.The great number of issues brought for overcoming frequency to widen,
Need exploitation high q-factor and ε low, middle badlyr(10≤εr≤ 25) with nearly zero τfThe microwave dielectric material of value.
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.The low ε of above-mentioned novel high-frequencyr, high q-factor microwave
The subject matter that dielectric material exists is contradiction between high-performance and low-temperature sintering.
Monoclinic phase lithium stannate (Li2SnO3) have and Li2TiO3Similar structure, has good microwave dielectric property (εr
=12.82, Q × f=20800GHz, τf=+26.9ppm/ DEG C), its abundant raw material, with low cost, it is that one has very much
The low ε of development prospectr, high q-factor high frequency microwave dielectric material, but its sintering temperature high (1230 DEG C) and have bigger
Positive τfValue (+26.9ppm/ DEG C), thus limit its further commercialization.Therefore, reduce sintering temperature and improve it
τfValue is advantageously implemented Li2SnO3The actual application of base media ceramic.Pang etc. are by adding B2O3-CuO improves
Li2SnO3The sintering character of pottery, its microwave property εr=13.73, Q × f=36400GHz, τf=+27.4ppm/ DEG C.
Wu etc. have negative temperature coefficient of resonance frequency material by selection and regulate Li2SnO3Pottery temperature stability, i.e.
0.3Li3NbO4-0.7Li2SnO3Pottery, its εr=16, Q × f=75300GHz, τf=+3ppm/ DEG C, but its sintering temperature
Degree is 1200 DEG C, it is impossible to burn altogether with Ag.Liu etc. utilize ZnO and Li2SnO3Being combined can be by Li2SnO3Resonant frequency
Temperature coefficient regulates and controls to 0.27ppm/ DEG C, but its sintering temperature is more than 1300 DEG C, also cannot burn altogether with Ag.
More than research shows Li2SnO3Although sill resonant frequency has obtained Effective Regulation, but sintering temperature is the highest
Reach more than 1200 DEG C, it is impossible to burn altogether with silver electrode material, limit the application of material.
Summary of the invention
The technical problem to be solved is the shortcoming overcoming above-mentioned ceramic material sintering temperature high, it is provided that a kind of
Sintering temperature low and have simultaneously excellent microwave dielectric property low-temperature sintering temperature-stable stannate microwave-medium pottery
Ceramic material.
Solve above-mentioned technical problem and be the technical scheme is that this low-temperature sintering temperature-stable stannate microwave is situated between
The thing of ceramics includes Li mutually2Mg3SnO6And Li2SnO3, wherein Li2Mg3SnO6Content be
35.1wt%～79.1wt%, remaining is Li2SnO3；The dielectric constant of this ceramic material is 14.2～14.7, quality because of
Number is 51300～78300GHz, and temperature coefficient of resonance frequency is-9.1～4.6ppm/ DEG C.
The thing of above-mentioned ceramic material middle Li mutually2Mg3SnO6Content most preferably 50.1wt%, remaining is Li2SnO3, its
Dielectric constant is 14.7, and quality factor are 78300GHz, and temperature coefficient of resonance frequency is-0.9ppm/ DEG C.
Ceramic material of the present invention is prepared by following step:
1, batch mixing
It is the Li of 98% by purity2CO3Powder and purity are the SnO of 99.5%2Powder adds after mixing for 1:1 in molar ratio
Enter in ball grinder, with zirconia ball as abrading-ball, dehydrated alcohol as ball-milling medium, be sufficiently mixed ball milling 6～12 little
Time, 80～100 DEG C are dried.
2, pre-burning
By dried for step 1 mixture pre-burning 2～6 hours at 700～900 DEG C, obtain Li2SnO3Pre-burning powder.
3, rerolling
According to (100-x) wt% (92wt%Li2SnO3-8wt%MgO)-xwt%LiF mass percent composition,
Wherein 1.0≤x≤6.0, obtain LiF powder and the step 2 that MgO powder that purity is 99.99%, purity are 99.6%
Li2SnO3Add in ball grinder after the mixing of pre-burning powder, with zirconia ball as abrading-ball, dehydrated alcohol be that ball milling is situated between
Matter, is sufficiently mixed ball milling 6～12 hours, and 60～80 DEG C are dried.
4, pelletize, molding
In the dried mixture of step 3 add mass fraction be 5% polyvinyl alcohol water solution pelletize, cross 80～
120 mesh sieves, then it is pressed into cylindrical green body with powder compressing machine.
5, sintering
Cylindrical green body step 4 obtained sinters 3～5 hours at 840～920 DEG C, obtains low-temperature sintering temperature
Stable type stannate microwave dielectric ceramic materials.
In above-mentioned steps 2, preferably by 700 DEG C of pre-burnings of dried for step 1 mixture 4 hours.
In above-mentioned steps 3, the value of preferably x is 2.0.
In above-mentioned steps 5, the cylindrical green body preferably step 4 obtained sinters 4 hours at 880 DEG C.
Low-temperature sintering temperature-stable stannate microwave dielectric ceramic materials sintering temperature of the present invention is low by (840～920
DEG C), good (dielectric constant is 14.2～14.7 to microwave property, and Q × f is 51300～78300GHz, resonant frequency temperature
Degree coefficient be-9.1～4.6ppm/ DEG C), overcome ceramic material sintering temperature height, temperature coefficient of resonance frequency bigger than normal
Shortcoming, it is ensured that the temperature stability of material, well enriches current high-frequency communication electronic circuit technology to work
The demand of the advanced low-k materials that environmental temperature stability is good and frequency selectivity is good, this pottery can be with silver simultaneously
Electrode burns altogether and meets LTCC material requirements.Microwave dielectric ceramic materials preparation method of the present invention is simple, raw materials used
Abundance, with low cost, suitable for mass production, can be widely applied to LTCC system, GPS days
The manufacture of the microwave devices such as line, wireless local area wave filter, multilayer dielectricity resonator.
Accompanying drawing explanation
Fig. 1 is the scanning electricity of the low-temperature sintering temperature-stable stannate microwave dielectric ceramic materials of embodiment 1 preparation
Mirror figure.
Fig. 2 is the X of the low-temperature sintering temperature-stable stannate microwave dielectric ceramic materials of embodiment 1～8 preparation
Ray powder diffraction pattern.
Fig. 3 be the low-temperature sintering temperature-stable stannate microwave dielectric ceramic materials of embodiment 1 preparation and Ag altogether
The X-ray diffractogram burnt.
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 is not only
It is limited to these embodiments.
Embodiment 1
1, batch mixing
It is the Li of 98% by 20.875g (0.277mol) purity2CO3Powder and 41.937g (0.277mol) purity are
The SnO of 99.5%2Add after powder mixing in ball grinder, according to raw mixture and zirconia ball, the matter of dehydrated alcohol
Amount ratio is 1: 2: 2, addition zirconia ball and dehydrated alcohol, is 360 revs/min with planetary ball mill at rotating speed
Under be sufficiently mixed ball milling 8 hours, then at 80～100 DEG C be dried 12 hours.
2, pre-burning
By dried for step 1 mixture pre-burning 4 hours at 700 DEG C, obtain Li2SnO3Pre-burning powder.
3, rerolling
According to 98.0wt% (92wt%Li2SnO3-8wt%MgO)-2.0wt%LiF mass percent composition, will
LiF powder that MgO powder that 2.008g purity is 99.99%, 0.469g purity are 99.6%, 20.992g Li2SnO3In advance
Add in ball grinder after burning powder mixing, be 1 according to gained mixture with zirconia ball, the mass ratio of dehydrated alcohol:
2: 2, add zirconia ball and dehydrated alcohol, be sufficiently mixed under rotating speed is 360 revs/min with planetary ball mill
Ball milling 8 hours, is then dried 12 hours at 60～80 DEG C.
4, pelletize, molding
The polyvinyl alcohol water solution pelletize that 1.2g mass fraction is 5% is added in the dried mixture of step 3,
Cross 120 mesh sieves, then with powder compressing machine under 4MPa pressure, be compressed into a diameter of 11.5mm, thickness is
The cylindrical green body of 5.5mm.
5, sintering
Cylindrical green body step 4 obtained sinters 4 hours at 880 DEG C, obtains low-temperature sintering temperature-stable stannum
Hydrochlorate microwave dielectric ceramic materials.
Use Quantan200 (Holand) type environmental scanning electron microscope that gained ceramic material is characterized, result
See Fig. 1.As seen from Figure 1, prepared ceramic material uniform particle sizes, crystal grain is full, physically well develops, and pottery causes
Close property is good.
Embodiment 2
In the step 3 of embodiment 1, according to 99.0wt% (92wt%Li2SnO3-8wt%MgO)-1.0wt%LiF
Mass percent composition, be the LiF of 99.6% by MgO powder, the 0.233g purity that 2.008g purity is 99.99%
Powder, 20.992g Li2SnO3Add after the mixing of pre-burning powder in ball grinder, according to gained mixture and zirconia ball, nothing
The mass ratio of water-ethanol is 1: 2: 2, adds zirconia ball and dehydrated alcohol, is 360 with planetary ball mill at rotating speed
It is sufficiently mixed ball milling under rev/min 8 hours, is then dried 12 hours at 60～80 DEG C.Other steps and enforcement
Example 1 is identical, obtains low-temperature sintering temperature-stable stannate microwave dielectric ceramic materials.
Embodiment 3
In the step 3 of embodiment 1, according to 96.0wt% (92wt%Li2SnO3-8wt%MgO)-4.0wt%LiF
Mass percent composition, be the LiF of 99.6% by MgO powder, the 0.958g purity that 2.008g purity is 99.99%
Powder, 20.992g Li2SnO3Add after the mixing of pre-burning powder in ball grinder, according to gained mixture and zirconia ball, nothing
The mass ratio of water-ethanol is 1: 2: 2, adds zirconia ball and dehydrated alcohol, is 360 with planetary ball mill at rotating speed
It is sufficiently mixed ball milling under rev/min 8 hours, is then dried 12 hours at 60～80 DEG C.Other steps and enforcement
Example 1 is identical, obtains low-temperature sintering temperature-stable stannate microwave dielectric ceramic materials.
Embodiment 4
In the step 3 of embodiment 1, according to 94.0wt% (92wt%Li2SnO3-8wt%MgO)-6.0wt%LiF
Mass percent composition, be the LiF of 99.6% by MgO powder, the 1.468g purity that 2.008g purity is 99.99%
Powder, 20.992g Li2SnO3Add after the mixing of pre-burning powder in ball grinder, according to gained mixture and zirconia ball, nothing
The mass ratio of water-ethanol is 1: 2: 2, adds zirconia ball and dehydrated alcohol, is 360 with planetary ball mill at rotating speed
It is sufficiently mixed ball milling under rev/min 8 hours, is then dried 12 hours at 60～80 DEG C.Other steps and enforcement
Example 1 is identical, obtains low-temperature sintering temperature-stable stannate microwave dielectric ceramic materials.
Embodiment 5
In the step 5 of embodiment 1, cylindrical green body is sintered 4 hours at 840 DEG C, other steps and enforcement
Example 1 is identical, obtains low-temperature sintering temperature-stable stannate microwave dielectric ceramic materials.
Embodiment 6
In the step 5 of embodiment 1, cylindrical green body is sintered 4 hours at 860 DEG C, other steps and enforcement
Example 1 is identical, obtains low-temperature sintering temperature-stable stannate microwave dielectric ceramic materials.
Embodiment 7
In the step 5 of embodiment 1, cylindrical green body is sintered 4 hours at 900 DEG C, other steps and enforcement
Example 1 is identical, obtains low-temperature sintering temperature-stable stannate microwave dielectric ceramic materials.
Embodiment 8
In the step 5 of embodiment 1, cylindrical green body is sintered 4 hours at 920 DEG C, other steps and enforcement
Example 1 is identical, obtains low-temperature sintering temperature-stable stannate microwave dielectric ceramic materials.
Use the low-temperature sintering temperature that embodiment 1～8 is obtained by RagukuD/Max2550 (Japan) type X-ray diffractometer
Degree stable type stannate microwave dielectric ceramic materials characterizes, and result is shown in Fig. 2.From Figure 2 it can be seen that prepared pottery
The thing phase composition of ceramic material is Li2Mg3SnO6And Li2SnO3, the weight/mass percentage composition of each thing phase is shown in Table 1.
The thing phase composition of table 1 microwave dielectric ceramic materials of the present invention
| Li2Mg3SnO6(wt%) | Li2SnO3(wt%) | |
| Embodiment 1 | 50.1 | 49.9 |
| Embodiment 2 | 37.7 | 62.3 |
| Embodiment 3 | 54.7 | 45.3 |
| Embodiment 4 | 79.1 | 20.9 |
| Embodiment 5 | 36.0 | 64.0 |
| Embodiment 6 | 40.5 | 59.5 |
| Embodiment 7 | 39.8 | 60.2 |
| Embodiment 8 | 35.1 | 64.9 |
Ceramic material grinding and polishing post-treatment prepared by embodiment 1～8 is become a diameter of 9～10mm, height by inventor
The cylinder of 5mm, uses and closes chamber the resonance method, with ZVB20 vector network analyzer (by Luo De Schwarz company of Germany
Produce) coordinate high-low temperature incubator, the low-temperature sintering temperature-stable stannate microwave-medium pottery to embodiment 1～8 preparation
Ceramic material carries out microwave dielectric property test, the results are shown in Table 2.
The microwave dielectric property of table 2 microwave dielectric ceramic materials of the present invention
From table 1, the low-temperature sintering temperature-stable stannate microwave-medium of the embodiment of the present invention 1～8 preparation
The sintering temperature of ceramic material is 840～920 DEG C, and relative density reaches 96.5%～97.5%, resonant frequency temperature
Coefficient | τf|≤10, there is the microwave dielectric property of excellence simultaneously.The low-temperature sintering temperature-stable stannate of the present invention
The sintering temperature of microwave dielectric ceramic materials compares the 0.3Li of report3NbO4-0.7Li2SnO3Composite ceramics,
0.7Li2SnO3The sintering temperature of-0.3ZnO composite ceramics significantly reduces, and microwave dielectric property is suitable；With
Li2SnO3-1wt% (B2O3-CuO) ceramic phase ratio, though sintering temperature difference is little, but Q × f value is high more than 2 times,
Temperature stability significantly improves.
In order to prove beneficial effects of the present invention, inventor is simultaneously introduced during the rerolling of embodiment 1
Li2SnO3Pre-burning powder, the Ag powder of MgO, LiF three's gross mass 10%, other steps are same as in Example 1,
Gained ceramic material uses RagukuD/Max2550 (Japan) type X-ray diffractometer to characterize, and result is shown in Fig. 3.
As seen from Figure 3, the thing phase composition of gained ceramic material is Li2Mg3SnO6、Li2SnO3, Ag, illustrate that the present invention is low
There is not chemical reaction in temperature sintering temperature stable type stannate microwave dielectric ceramic materials and Ag, can be applicable to low
Temperature common burning porcelain system.
Claims (5)
1. a low-temperature sintering temperature-stable stannate microwave dielectric ceramic materials, it is characterised in that: this pottery
The thing of material includes Li mutually2Mg3SnO6And Li2SnO3, wherein Li2Mg3SnO6Content be 35.1wt%～
79.1wt%, remaining is Li2SnO3；The dielectric constant of this ceramic material is 14.2～14.7, quality factor be 51300～
78300GHz, temperature coefficient of resonance frequency is-9.1～4.6ppm/ DEG C, and it is prepared by following step:
(1) batch mixing
It is the Li of 98% by purity2CO3Powder and purity are the SnO of 99.5%2Powder adds after mixing for 1:1 in molar ratio
Enter in ball grinder, with zirconia ball as abrading-ball, dehydrated alcohol as ball-milling medium, be sufficiently mixed ball milling 6～12 little
Time, 80～100 DEG C are dried；
(2) pre-burning
By step (1) dried mixture pre-burning 2～6 hours at 700～900 DEG C, obtain Li2SnO3In advance
Burn powder；
(3) rerolling
According to (100-x) wt% (92wt%Li2SnO3-8wt%MgO)-xwt%LiF mass percent composition,
Wherein 1.0≤x≤6.0, by LiF powder and step (2) that MgO powder that purity is 99.99%, purity are 99.6%
The Li obtained2SnO3Adding in ball grinder after the mixing of pre-burning powder, with zirconia ball as abrading-ball, dehydrated alcohol is as ball
Grinding media, is sufficiently mixed ball milling 6～12 hours, and 60～80 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 80～120 mesh sieves, then is pressed into cylinder with powder compressing machine
Shape green compact；
(5) sintering
Cylindrical green body step (4) obtained sinters 3～5 hours at 840～920 DEG C, obtains low-temperature sintering
Temperature-stable stannate microwave dielectric ceramic materials.
Low-temperature sintering temperature-stable stannate microwave dielectric ceramic materials the most according to claim 1, its
It is characterised by: in described step (2), by 700 DEG C of pre-burnings of step (1) dried mixture 4 hours.
Low-temperature sintering temperature-stable stannate microwave dielectric ceramic materials the most according to claim 1, its
It is characterised by: in described step (3), x=2.0.
Low-temperature sintering temperature-stable stannate microwave dielectric ceramic materials the most according to claim 1, its
Being characterised by: in described step (5), cylindrical green body step (4) obtained sinters 4 hours at 880 DEG C.
Low-temperature sintering temperature-stable stannate microwave dielectric ceramic materials the most according to claim 1, its
It is characterised by: the thing of this ceramic material includes Li mutually2Mg3SnO6And Li2SnO3, wherein Li2Mg3SnO6Contain
Amount is 50.1wt%, and remaining is Li2SnO3；The dielectric constant of this ceramic material is 14.7, and quality factor are 78300GHz,
Temperature coefficient of resonance frequency is-0.9ppm/ DEG C, and it is prepared by following step:
(1) batch mixing
It is the Li of 98% by purity2CO3Powder and purity are the SnO of 99.5%2Powder adds after mixing for 1:1 in molar ratio
Enter in ball grinder, with zirconia ball as abrading-ball, dehydrated alcohol as ball-milling medium, be sufficiently mixed ball milling 6～12 little
Time, 80～100 DEG C are dried；
(2) pre-burning
By step (1) dried mixture pre-burning 4 hours at 700 DEG C, obtain Li2SnO3Pre-burning powder；
(3) rerolling
By (100-x) wt% (92wt%Li2SnO3-8wt%MgO)-xwt%LiF mass percent composition,
Wherein x=2.0, obtains LiF powder and the step (2) that MgO powder that purity is 99.99%, purity are 99.6%
Li2SnO3Add in ball grinder after the mixing of pre-burning powder, with zirconia ball as abrading-ball, dehydrated alcohol as ball-milling medium,
Being sufficiently mixed ball milling 6～12 hours, 60～80 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 80～120 mesh sieves, then is pressed into cylinder with powder compressing machine
Shape green compact；
(5) sintering
Cylindrical green body step (4) obtained sinters 4 hours at 880 DEG C, obtains low-temperature sintering temperature stabilization
Type stannate microwave dielectric ceramic materials.
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