CN110304915A - A kind of microwave dielectric ceramic materials and preparation method thereof of high breakdown strength low-k - Google Patents
A kind of microwave dielectric ceramic materials and preparation method thereof of high breakdown strength low-k Download PDFInfo
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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- C04B35/46—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on titanium oxides or titanates
- C04B35/462—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on titanium oxides or titanates based on titanates
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- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
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- C04B2235/3284—Zinc oxides, zincates, cadmium oxides, cadmiates, mercury oxides, mercurates or oxide forming salts thereof
Abstract
The present invention provides a kind of microwave dielectric ceramic materials and preparation method thereof of high breakdown strength low-k, which basic composition is m wt%MgTiO3‑n wt%ZnNb2O6(MTZN), 94≤m≤99,1≤n≤6, m+n=100.The microwave dielectric ceramic materials have low-dielectric loss, higher breakdown strength and volume resistivity, properties simultaneously are as follows: 17 < ε of dielectric constantr≤ 17.5, product Q f > 23000GHz of quality factor and frequency, breakdown strength >=24kV/mm, volume resistivity >=2.2 × 108Ω•m。
Description
Technical field
Present invention relates particularly to a kind of microwave dielectric ceramic materials of high breakdown strength low-k, belong to media ceramic
Field.
Background technique
With the rapid development of modern communications technology, the 5th generation mechanics of communication will come into huge numbers of families.Early in 2014 5
The moon 13, Samsung has just announced, has taken the lead in having developed the first mobile transmission network based on 5G core technology, and table
The business promotion of 5G network will be carried out before the year two thousand twenty by showing.Communication apparatus constantly towards miniaturization, slimming, high frequency side
It marches forward, this whether made higher requirement antenna itself or its encapsulation technology.And ceramic antenna is in addition to meeting
It minimizes, is thinned, outside the requirement of high frequency, itself also has the advantages such as high reliablity, at low cost, leads in 5G radio-frequency front-end
The great development prospect in domain.It is necessary to meet following condition for the microwave dielectric material of function admirable: (1) suitable dielectric constant；(2) compared with
Low loss, generally requires Qf at least more than 2000；(3) higher breakdown strength and volume resistivity, part microwave-medium
Ceramics also require its breakdown strength and volume resistivity due to its use condition.Although 5G technology using extremely urgent,
But also seldom discovery can fully meet the material system of microwave dielectric properties requirement now.
A series of low dielectric constant microwave dielectric material (ε developed at presentr< 20), study the material of breakdown strength
Seldom.Main System mainly has: (1) MgTiO3Ceramics, dielectric constant are 17 or so, and microwave dielectric property is very excellent.
But it finds after tested, not high (breakdown strength is about 22kV/mm, and volume resistivity is about for breakdown strength and volume resistivity
3.3×107Ω m), this greatly hinders MgTiO3The development of ceramics.(1)Mg2TiO4Ceramics, dielectric constant 14 or so,
Equally there is excellent microwave dielectric property, but its breakdown strength is similarly very low (breakdown strength is about 20kV/mm), it is difficult to full
The demand in sufficient market.In addition to this, Mg2TiO4The sintering temperature of ceramics is higher, is higher than 1400 DEG C, also becomes its development of obstruction
A factor because sintering temperature is excessively high, sintering just become difficult to phenomena such as controlling, being easy to appear fried porcelain.How to guarantee
While its excellent microwave dielectric property, promoting its breakdown strength and volume resistivity just seems particularly significant.
Up to the present, it has not been found that having excellent microwave dielectric property (εr< 20, Qf > 2000GHz), high strike
Wear intensity (breakdown strength >=40kV/mm), high volume resistivity (volume resistivity >=1 × 1012Ω m) material system.With
The rapid development of microwave communication, to microwave-medium ceramics, more stringent requirements are proposed, and ceramics is needed to have good micro-wave dielectric
While performance, moreover it is possible to take into account the performances such as breakdown strength and volume resistivity.
Summary of the invention
The technical problem to be solved by the present invention is to provide a kind of microwave Jie in view of the deficiency of the prior art
Ceramics, the material have low-k, higher breakdown strength and volume resistivity simultaneously.
The present invention be solve the problems, such as it is set forth above used by technical solution are as follows:
A kind of microwave dielectric ceramic materials of high breakdown strength low-k provided by the present invention, are a kind of solid solutions
Body, chemical composition can be expressed as m wt%MgTiO3- n wt%ZnNb2O6, wherein 94≤m≤99,1≤n≤6, m+n=100.
The microwave dielectric ceramic materials, 17 < ε of dielectric constantr≤ 17.5, product Qf > 23000GHz of quality factor and frequency, breakdown
Intensity >=24kV/mm, volume resistivity >=2.2 × 108Ω·m。
Preferably, in above-mentioned microwave dielectric ceramic materials, 94≤m≤97,3≤n≤6, m+n=100, and, dielectric constant
17 < εrProduct Qf > 23000GHz of < 17.5, quality factor and frequency, breakdown strength >=40kV/mm, volume resistivity >=
3.2×1011Ω·m。
The preparation method of the microwave dielectric ceramic materials of above-mentioned high breakdown strength low-k, key step are as follows:
5) MgO and TiO2It is mixed according to molar ratio 1.01-1.03:1, it is mixed with wet ball grinding method using dehydrated alcohol as solvent
Ball milling is closed, matrix material premix is obtained；After matrix material premix drying, in 1130 DEG C -1150 DEG C, air atmosphere
Middle pre-burning 2-4 hours, obtain MgTiO3Powder；
6) ZnO and Nb2O5It mixes according to molar ratio 1-1.01:1, using dehydrated alcohol as solvent, is mixed with wet ball grinding method equal
It is even, obtain doping premix；After doping premix drying, pre-burning 2-3 hours in 950 DEG C -1000 DEG C, air atmosphere,
Obtain ZnNb2O6Powder；
7) by step 2) MgTiO3Powder and ZnNb2O6Powder is m:n mixing in mass ratio, and using dehydrated alcohol as solvent,
It is mixed with wet ball-milling method；After drying, addition poly-vinyl alcohol solution makees binder granulation, is then sieved, is dry-pressing formed；
8) molded samples obtained by step 3) are sintered 2-4 hours under 1270 DEG C~1420 DEG C, air atmosphere after dumping,
Obtain the microwave dielectric ceramic materials that high strike wears intensity low-k.
Compared with prior art, the beneficial effects of the present invention are:
Firstly, the present invention provides a kind of new high breakdown strength dielectric constant microwave ceramic medium, with MgTiO3For base
Body mixes appropriate ZnNb2O6, not only there is excellent microwave dielectric property (εr≤ 17.5, Qf > 2000GHz), also while having
Standby higher breakdown strength and volume resistivity (breakdown strength >=40kV/mm, volume resistivity >=3.2 × 1011Ω·m).With
Existing microwave-medium ceramics are compared, and the present invention possesses higher breakdown strength and volume resistivity, and component is simple, non-volatile,
Nonhazardous, technical maturity are simple, and cost of material is cheap, have a good application prospect, and are able to satisfy the demand of existing market.
Secondly, once having scholar to prepare microwave-medium ceramics using sol-gal process, but manufacturing cycle is longer, price is more high
It is expensive, it is unfavorable for the industrialized production of microwave-medium ceramics.The present invention is with MgTiO3For matrix, appropriate ZnNb is mixed2O6, using solid
Prepared by phase method, have great advantages, and powder granule object soilless sticking, at low cost, yield is big, and preparation process is simple, this
A little advantages can be converted into big advantage in its industrialized production.
Detailed description of the invention
Fig. 1 is the XRD spectrum of the powder after being granulated in comparative example and embodiment 1-7；Wherein, with the n in chemical composition
Value respectively corresponds corresponding embodiment or comparative example；
Fig. 2 is the XRD spectrum of the microwave dielectric ceramic materials of comparative example and embodiment 1-7 preparation；Wherein, with chemical group
N value in respectively corresponds corresponding embodiment or comparative example；
Fig. 3 is the SEM image of the microwave dielectric ceramic materials of comparative example and embodiment 1-7 preparation；Wherein, a-h is successively
Respectively correspond comparative example, embodiment 1-7.
Specific embodiment
For a better understanding of the present invention, below with reference to the embodiment content that the present invention is furture elucidated, but the present invention is not
It is limited only to the following examples.
In following embodiments, raw material MgO, TiO2、ZnO、Nb2O5Purity be all larger than 99%.
In following embodiments, addition 5wt% poly-vinyl alcohol solution makees binder granulation；Dry-pressing formed pressure be 1~
20MPa.In general, raw material needed for one-pass molding is 0.26g, the piece of diameter 12mm, 1.1~1.3mm of thickness can be prepared as
Shape；Alternatively, raw material needed for one-pass molding is 2g, the column of diameter 12mm, 7~8mm of thickness can be prepared into.
In following embodiments, using the dielectric properties of the transverse electric field analysis sample of open type cell method microwave frequency, iron is used
Stations test its breakdown strength, test its volume resistivity with Keithley 6517A megger.
Comparative example 1
A kind of microwave dielectric ceramic materials, chemical composition can be expressed as MgTiO3.Its preparation process, specific as follows:
(1) by MgO and TiO21.02:1 is mixed in molar ratio, using dehydrated alcohol as medium, by its mixing ball milling 24 hours
After dry, then pre-burning 4 hours under 1150 DEG C, air atmosphere, obtain MgTiO3Powder；
(2) by above-mentioned MgTiO3Powder ball milling 24 hours, is granulated using dehydrated alcohol as medium after drying, dry-pressing formed, so
1000 DEG C first are warming up to 3.3 DEG C/min afterwards, then target firing temperature (target firing temperature 1270 is warming up to 2 DEG C/min
DEG C~1420 DEG C between, with 30 DEG C for spacing gradient, i.e., sintering temperature takes 1270,1300,1330,1360,1390,1420 respectively
DEG C, facilitate it is subsequent be compared, and then obtain optimal sintering temperature) be sintered 4 hours, obtain microwave dielectric ceramic materials pair
Compare sample.
The contrast sample combination bulk density is analyzed, and optimal sintering temperature is 1390 DEG C；Test its performance are as follows: dielectric
Constant εr=16.75, the product Qf=41170GHz of quality factor and frequency, breakdown strength 22kV/mm, volume resistivity
3.3×107Ω·m。
Embodiment 1
A kind of microwave dielectric ceramic materials of high breakdown strength low-k, chemical composition can be expressed as 99wt%
MgTiO3- 1wt%ZnNb2O6, i.e. m is 99, n 1.Its preparation process, specific as follows:
(1) by MgO and TiO21.02:1 is mixed in molar ratio, using dehydrated alcohol as medium, by its mixing ball milling 24 hours
After dry, then pre-burning 4 hours under 1150 DEG C, air atmosphere, obtain MgTiO3Powder；
(2) by ZnO and Nb2O51:1 is mixed in molar ratio, using dehydrated alcohol as medium, will be dried after mixing ball milling 24 hours
Dry, then pre-burning 3 hours under 1000 DEG C, air atmosphere, obtain ZnNb2O6Powder；
(3) by above-mentioned MgTiO3Powder and ZnNb2O6Powder mixing, m:n in mass ratio (embodiment 1 is 99:1) mixing, with
Dehydrated alcohol is medium, ball milling 24 hours, is granulated after drying, dry-pressing formed, is then first warming up to 1000 DEG C with 3.3 DEG C/min,
Again with 2 DEG C/min be warming up to target firing temperature (between 1270 DEG C~1420 DEG C, with 30 DEG C for spacing gradient, i.e. sintering temperature
Take 1270,1300,1330,1360,1390,1420 DEG C respectively, facilitate it is subsequent be compared, and then obtain optimal sintering temperature)
It is sintered 4 hours, obtains the microwave dielectric ceramic materials sample of high breakdown strength low-k.
1 gained finished product sample combination bulk density of embodiment is analyzed, and optimal sintering temperature is 1330 DEG C；Test its property
It can are as follows: permittivity εr=17.02, the product Qf=38265GHz of quality factor and frequency, breakdown strength 24kV/mm,
Volume resistivity 2.2 × 108Ω·m。
Embodiment 2
A kind of microwave dielectric ceramic materials of high breakdown strength low-k, chemical composition can be expressed as 98.5wt%
MgTiO3- 1.5wt%ZnNb2O6, i.e. m is 98.5, n 1.5.The main distinction of its preparation process and embodiment 1 is m:n not
Together.
2 gained finished product sample combination bulk density of embodiment is analyzed, and optimal sintering temperature is 1330 DEG C；Test its property
It can are as follows: permittivity εr=17.50, the product Qf=37265GHz of quality factor and frequency, breakdown strength 30kV/mm,
Volume resistivity 1.6 × 109Ω·m。
Embodiment 3
A kind of microwave dielectric ceramic materials of high breakdown strength low-k, chemical composition can be expressed as 98wt%
MgTiO3- 2wt%ZnNb2O6, i.e. m is 98, n 2.Its preparation process is that m:n is different from the main distinction of embodiment 1.
3 gained finished product sample combination bulk density of embodiment is analyzed, and optimal sintering temperature is 1330 DEG C；Test its property
It can are as follows: permittivity εr=17.04, the product Qf=35692GHz of quality factor and frequency, breakdown strength 36kV/mm,
Volume resistivity 4.4 × 1010Ω·m。
Embodiment 4
A kind of microwave dielectric ceramic materials of high breakdown strength low-k, chemical composition can be expressed as 97wt%
MgTiO3- 3wt%ZnNb2O6, i.e. m is 97, n 3.Its preparation process is that m:n is different from the main distinction of embodiment 1.
4 gained finished product sample combination bulk density of embodiment is analyzed, and optimal sintering temperature is 1330 DEG C；Test its property
It can are as follows: permittivity εr=17.14, the product Qf=31790GHz of quality factor and frequency, breakdown strength 40kV/mm,
Volume resistivity 1.2 × 1012Ω·m。
Embodiment 5
A kind of microwave dielectric ceramic materials of high breakdown strength low-k, chemical composition can be expressed as 96wt%
MgTiO3- 4wt%ZnNb2O6, i.e. m is 96, n 4.Its preparation process is that m:n is different from the main distinction of embodiment 1.
5 gained finished product sample combination bulk density of embodiment is analyzed, and optimal sintering temperature is 1330 DEG C；Test its property
It can are as follows: permittivity εr=17.23, the product Qf=30922GHz of quality factor and frequency, breakdown strength 45kV/mm,
Volume resistivity 1.1 × 1012Ω·m。。
Embodiment 6
A kind of microwave dielectric ceramic materials of high breakdown strength low-k, chemical composition can be expressed as 95wt%
MgTiO3- 5wt%ZnNb2O6, i.e. m is 95, n 5.Its preparation process is that m:n is different from the main distinction of embodiment 1.
6 gained finished product sample test its performance of embodiment are as follows: permittivity εr=17.06, quality factor and frequency multiply
Long-pending Qf=25047GHz, breakdown strength 50kV/mm, volume resistivity 5.5 × 1011Ω·m
Embodiment 7
A kind of microwave dielectric ceramic materials of high breakdown strength low-k, chemical composition can be expressed as 96wt%
MgTiO3- 4wt%ZnNb2O6, i.e. m is 96, n 4.Its preparation process is that m:n is different from the main distinction of embodiment 1.
7 gained finished product sample test its performance of embodiment are as follows: permittivity εr=17.18, quality factor and frequency multiply
Long-pending Qf=23687GHz, breakdown strength 62kV/mm, volume resistivity 3.2 × 1011Ω·m。
The chemical composition and properties of 1 embodiment 1-6 of table and the microwave-medium ceramics of comparative example preparation
Fig. 1 is to be granulated the XRD spectrum of gained powder, i.e., the powder not being sintered also in embodiment preparation process.By scheming
1 it is found that in embodiment 1-7 be granulated gained powder without sintering when, all incorporation ZnNb2O6Granulation powder in can detect
ZnNb2O6Presence；And with ZnNb2O6Volume is continuously increased, ZnNb2O6Peak be more and more obvious, but be sintered after it is micro-
Biggish variation but has occurred in the crystal phase of wave medium ceramic material sample.As shown in Figure 2: passing through after high temperature sintering, embodiment
Fail to detect ZnNb in the microwave dielectric ceramic materials sample of 1-72O6The presence of crystal phase, and when volume continues growing, reach
When 4wt%, there is MgTi in ceramics2O5Second phase illustrates that high temperature sintering promotes ZnNb2O6Into MgTiO3Lattice, and and its
Form solid solution.This solid solution determines the dielectric properties of ceramics, and performance is with MgTiO3Based on, by ZnNb2O6And
MgTi2O5The influence of second phase, so the dielectric constant of ceramics is in 17 or so fluctuations；With ZnNb2O6Volume gradually increases, Q
F value gradually decreases, and is on the one hand because of ZnNb2O6Qf value be less than MgTiO3, on the other hand it is then because occurring in ceramics
Biggish MgTi is lost2O5Second phase.
As shown in Table 1: with ZnNb2O6The increase of content, dielectric constant have slight promotion.The reason is that ZnNb2O6Jie
Electric constant (25) is slightly above MgTiO3Dielectric constant, but volume is less, so being promoted to its dielectric constant smaller；And due to pottery
Porcelain dielectric constant is also influenced by factors such as its internal porosity and defects, therefore its dielectric constant is not with ZnNb2O6The increase of volume
And become larger, but fluctuated between 17~17.5.
It is also known by table 1: with ZnNb2O6The increase of content, Qf value gradually decrease.This is because ZnNb2O6Ceramics
Qf value be less than MgTiO3The Qf value of ceramics, so MgTiO3ZnNb is mixed in ceramics2O6Its performance can be deteriorated, cause it
Dielectric loss becomes larger.And in conjunction in XRD spectrum, work as ZnNb2O6When doping reaches 4wt%, there is MgTi2O5Phase, and
MgTi2O5Dielectric loss is higher, can further decrease the dielectric loss of MTZN ceramics.
It is also known by table 1: with ZnNb2O6The increase of content, breakdown strength continue to increase.Reason mainly includes two aspects that
First is that because ZnNb2O6Ceramics itself just have very high breakdown strength (~46kV/mm)；Another reason by Fig. 3 scanning figure
As can be seen that, ZnNb2O6Incorporation can constantly reduce MgTiO3The crystallite dimension of ceramics, and keep the size of crystal grain more uniform.And
And it is also found that with ZnNb2O6The increase of incorporation, MgTiO3Stomata inside ceramics is also tailing off.More uniform crystalline substance
Particle size and less stomata, can all make MgTiO3The internal structure of ceramics is more close, to improve MTZN ceramics
Breakdown strength.
It is also known by table 1, with ZnNb2O6The increase of content, ceramic volume resistivity constantly increases, in x=3, body
Product resistivity has reached maximum (maximum value 1.2 × 1012Ω·m).The reason is that pure ZnNb2O6Ceramic volumetric resistivity is relatively high
(about 1.04 × 1013Ω m) after, with ZnNb2O6Volume continues growing, and the volume resistivity of MTZN ceramics starts
Existing downward trend.But due to ZnNb2O6Ceramic volume resistivity itself is relatively high, so the volume resistivity of MTZN ceramics declines
It must not be very much.
In addition, it has been observed that with ZnNb2O6Mass fraction is continuously increased, microwave dielectric ceramic materials color obtained by embodiment
From white to it is light blue excessively.In addition, with ZnNb2O6Mass fraction is continuously increased, and downward trend is also presented in sintering temperature.
The above is only a preferred embodiment of the present invention, it is noted that come for those of ordinary skill in the art
It says, without departing from the concept of the premise of the invention, several modifications and variations can also be made, these belong to of the invention
Protection scope.
Claims (8)
1. a kind of microwave dielectric ceramic materials of high breakdown strength low-k, it is characterised in that the microwave-medium ceramics material
The chemical composition of material is expressed as m wt%MgTiO3-n wt%ZnNb2O6, wherein 94≤m≤99,1≤n≤6, m+n=100.
2. a kind of microwave dielectric ceramic materials of high breakdown strength low-k according to claim 1, feature exist
In 17 < ε of dielectric constant of the microwave dielectric ceramic materialsr≤ 17.5, product Q f > 23000GHz of quality factor and frequency,
Breakdown strength >=24kV/mm, volume resistivity >=2.2 × 108Ω•m。
3. a kind of microwave dielectric ceramic materials of high breakdown strength low-k according to claim 1, feature exist
In the microwave dielectric ceramic materials, 94≤m≤97,3≤n≤6, m+n=100.
4. a kind of microwave dielectric ceramic materials of high breakdown strength low-k according to claim 3, feature exist
In the 17 < ε of dielectric constant of the microwave dielectric ceramic materialsrThe product Q f of < 17.5, quality factor and frequency >
23000GHz, breakdown strength >=40kV/mm, volume resistivity >=3.2 × 1011Ω•m。
5. a kind of preparation method of the microwave dielectric ceramic materials of high breakdown strength low-k, it is characterised in that key step
It is as follows:
MgO and TiO2According to molar ratio (1.01-1.03): 1 mixing and ball milling is uniform, obtains matrix material premix；Described matrix is former
After expecting premix drying, through pre-burning, MgTiO is obtained3Powder；
ZnO and Nb2O5According to molar ratio (1-1.01): 1 mixing and ball milling is uniform, obtains doping premix；The doping premix is dried
After dry, through pre-burning, ZnNb is obtained2O6Powder；
By MgTiO obtained by step 1)3ZnNb obtained by powder and step 22O6Powder is m:n mixing in mass ratio, and with wet type ball
Mill method mixes, and after drying, is granulated, is sieved, is dry-pressing formed, obtains molded samples；Wherein, 94≤m≤99,1≤n≤6, m+n=
100；
Molded samples obtained by step 3) are sintered 2-4 hours after dumping under 1270 DEG C ~ 1420 DEG C, air atmosphere to get arriving
The microwave dielectric ceramic materials of high breakdown strength low-k.
6. a kind of preparation side of the microwave dielectric ceramic materials of high breakdown strength low-k according to claim 6
Method, it is characterised in that after being dried in step 1), pre-burning 2-4 hours in 1130 DEG C -1150 DEG C, air atmosphere.
7. a kind of preparation side of the microwave dielectric ceramic materials of high breakdown strength low-k according to claim 6
Method, it is characterised in that after being dried in step 2, pre-burning 2-3 hours in 950 DEG C -1000 DEG C, air atmosphere.
8. a kind of preparation side of the microwave dielectric ceramic materials of high breakdown strength low-k according to claim 6
Method, it is characterised in that heating rate is 2-4 DEG C/min in step 4).
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