CN107793140A - A kind of temperature-stabilized microwave medium ceramic material and preparation method thereof - Google Patents
A kind of temperature-stabilized microwave medium ceramic material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of high-quality factor microwave medium ceramic material and preparation method thereof.The ceramic material structure expression is (1 y) Sr2Na6Al6Si6O24(XO4)2‑yTiO2, wherein one kind in 0.05≤y≤0.1, X S, Mo or W.The material is prepared by traditional high temperature solid phase synthesis, a small amount of dispersant is added during secondary ball milling, then the ultrasonic vibration under thermal environment, is made sample powder granule be not easy to reunite.Thus the material prepared sinters well at 1100 DEG C~1150 DEG C, and dielectric constant is 9.6~11.3, and its quality factor q f values are up to 64800 92000GHz, and temperature coefficient of resonance frequency is small.Present invention firstly discloses the Sr of blue party stone structure simultaneously2Na6Al6Si6O24(XO4)2(one kind in X S, Mo or W) ceramics have good microwave dielectric property.
Description
Technical field
The present invention relates to dielectric ceramic material, more particularly to for manufacturing ceramic substrate, the resonance that microwave frequency uses
Dielectric ceramic material of microwave device such as device and wave filter and preparation method thereof.
Background technology
In recent years, as microwave mobile communication technology constantly develops to high frequency and digitlization direction, to first device modularization
Requirement it is also more and more urgent.LTCC Technology (Low Temperature Co-fired Ceramics, LTCC) will
Ask microwave dielectric material must excellent performance, there is low sintering temperature (≤900 DEG C), and can be burnt altogether with Ag electrodes it is compatible,
This causes it to turn into one of major technique of electronic-component module.The burning of current commercialized microwave dielectric ceramic materials system
Junction temperature is generally greater than 1300 DEG C, it is impossible to directly burns to form multilayer ceramic capacitor altogether with low-melting-point metals such as Ag and Cu.
In order to meet LTCC technology demand, researcher both domestic and external system material in low sintering temperature has been carried out extensive exploration and
Research, the low Li bases of current intrinsic sintering temperature, V bases, Bi based compounds, borate salt system compound, phosphate system chemical combination
The material systems such as thing, tungstates system compound and tellurate system compound are the focus directions of research.These compounds
Crystal structure is with perovskite structure, spinel structure, and based on scheelite-type structure and garnet structure etc., but microwave dielectric property is joined
Difference is uneven, V bases, Bi bases, tungsten (molybdenum) base microwave medium ceramic material or the borate microwave-medium of wherein most article report
The synthesis microwave dielectric property of ceramic material is poor, is usually expressed as quality factor height but temperature coefficient of resonance frequency is excessive,
Or temperature coefficient of resonance frequency nearly zero but quality factor it is too low.This is due to three performance indications (ε of microwave dielectric ceramicr
With Qf and τf) between be the relation mutually restricted (see document：Restricting relation between microwave dielectric ceramic materials dielectric properties,
Zhu Jianhua, Liang Fei, Wang Xiaohong, Lv Wenzhong, electronic component and material, phase March the 3rd in 2005), meet three performance requirements and can
Low sintering single-phase microwave-medium ceramics are considerably less.Research to microwave-medium ceramics at present is largely to pass through many experiments
And the summary of experience drawn, but illustrate the relation of microstructure and dielectric properties without complete theory, and can not be
The microwave dielectric properties such as its temperature coefficient of resonance frequency and quality factor are predicted from the composition of compound and structure in theory.More
Importantly, the preparation technology of microwave dielectric ceramic materials is also one of principal element for influenceing material microwave dielectric properties, from
The microwave-medium ceramics having been commercialized integrate the preferable microwave dielectric ceramic materials of microwave dielectric property, its main system to recent
Preparation Method is by high temperature solid phase synthesis, because this method technology maturation, technique is simple, and production efficiency is high, relative to
Sol-gal process, hydro-thermal method etc. have more operability and economic value for the wet chemistry method of representative in industrial production, but high
Warm solid-phase synthesis its it is intrinsic the shortcomings that, such as energy consumption is big, particle is easily reunited after ball milling should cause the enough attention in the field.
The content of the invention
Based on above mentioned problem, it is an object of the invention to provide a kind of temperature-stabilized microwave medium ceramic material and preparation
The method of the microwave dielectric ceramic materials.The microwave dielectric ceramic materials have good heat endurance and low-loss, while can
Low-temperature sintering, and the host compound in material is compound of the report with good microwave dielectric property first.
For overcome the deficiencies in the prior art, technical scheme provided by the invention is：
A kind of temperature-stabilized microwave medium ceramic material, the chemical constitution formula of the ceramic material are：(1-y)
Sr2Na6Al6Si6O24(XO4)2-yTiO2, wherein 0.05≤y≤0.1, y are mol ratio, one kind in X S, Mo or W；The ceramics
The microwave dielectric property of material is：Dielectric constant is 9.6~11.3, and quality factor q f is 64800~92000GHz, resonant frequency
Temperature coefficient is -21.4ppm/ DEG C~13.9ppm/ DEG C.
Further, in described ceramic material, Sr2Na6Al6Si6O24(XO4)2Structure be blue party stone structure, its quality
Factor is 82000~97000GHz, and dielectric constant is 8.9~10.7, and temperature coefficient of resonance frequency is negative.
For another object of the present invention, the present invention also provides a kind of preparation of temperature-stabilized microwave medium ceramic material
Method, it is comprised the steps of：
(1) according to (1-y) Sr2Na6Al6Si6O24(XO4)2-yTiO2Middle Sr:Na:Al:Si:X:Ti mol ratio, which weighs, to be contained
The raw material of each element, wherein 0.05≤y≤0.1, y are mol ratio, X is positive hexad；Then the raw material weighed is carried out
Wet ball-milling, ball milling 2 hours, dried after ball milling and obtain raw mixture powder；By pressed by powder into blocks, at 1000 DEG C
Insulation 4 hours, obtains sample burning block；
(2) it is the grinding of sample burning block is broken, it is put into ball grinder, zirconia ball and deionized water is pre-loaded with ball grinder；
Put ball grinder into ball mill, the revolution rotating speed for setting ball mill is 280rpm per minute, and wet ball-milling stops after 2 hours；It is past
A small amount of dispersant is added in ball grinder, then in a manner of ball grinder rotation, rotating speed is that 300rpm per minute carries out ball milling 1 hour,
Sample powder is dried to obtain after ball milling；
(3) the sample powder of drying is put into the ball grinder equipped with the appropriate deionized water necessarily matched and alcohol mixeding liquid
It is interior, then the ball grinder is put into supersonic cleaning machine, water is housed, ball grinder is fixed in water, the height of water in supersonic cleaning machine
For ball grinder mid-height；The heating and thermal insulation program of supersonic cleaning machine is set, to the 40 DEG C and herein temperature of the water in heated wash machine
Degree insulation；Then ball grinder lid is closed, opens ultrasonic vibration, sample powder is in a sealed meter environment by ultrasonic vibration, supersonic frequency
Rate is 50kHz, ultrasonic vibration 30 minutes；Then remove ball grinder lid, heat supersonic cleaning machine reclaimed water temperature to 95 DEG C simultaneously
It is incubated the temperature, ultrasonic vibration 30 minutes, supersonic frequency 30kHz；
(4) dried after ultrasonic vibration terminates, obtain sample powder, be then granulated, sieve, the particle after sieving is pressed into
Type, 4 hours are then sintered at 1100 DEG C~1150 DEG C into porcelain, obtains temperature-stabilized microwave medium ceramic material.
Preferably, in described preparation method, positive hexad X is one kind in S, Mo or W.
Preferably, in described preparation method, the raw material containing each element is SrCO3、Na2CO3、Al2O3、SiO2、(NH4)2SO4、WO3、MoO3And TiO2。
Preferably, described dispersant is the mixture of Sodium Polyacrylate, calgon, sodium pyrophosphate and polyethylene glycol
Liquid, and the addition of the dispersant is the 0.1% of sample quality；Sodium Polyacrylate, calgon, sodium pyrophosphate and poly- second
The mass ratio of glycol is 3:1:1:1.
Preferably, in described preparation method, the deionized water and alcohol mixeding liquid in step (3) are by following proportioning group
Into：Deionized water weight：Ethanol weight=1：9.
In addition, prepare Sr2Na6Al6Si6O24(XO4)2(X is one kind in S, Mo or W as positive hexad) ceramics come
Its microwave dielectric property is tested, its preparation method is consistent with the above method, simply without addition TiO2。
Compared with prior art, it is an advantage of the invention that：1. technical scheme is used, to report first with good
The Sr of good microwave dielectric property2Na6Al6Si6O24(XO4)2For main body, TiO of the addition with positive temperature coefficient of resonance frequency2, lead to
Near-zero resonance frequency temperature coefficient can be obtained by crossing high temperature sintering, and the microwave-medium that the synthesis microwave dielectric property of temperature-stable is good is made pottery
Ceramic material.2. the technical solution adopted by the present invention, further perfect on traditional high temperature solid phase synthesis, by secondary ball
Appropriate, Suitable formulations ceramic powders dispersants are added during mill so that the sample powder particle after ball milling is not easy to reunite,
Then again by carrying out ultrasonic vibration, while the volatilization of water and alcohol mixeding liquid at high temperature to sample in high temperature water environment,
So that sample more preferably avoids molecule from reuniting in a liquid, and can the dispersant that is added of initial gross separation secondary ball milling, gained
The microwave-medium ceramics that are obtained through oversintering of sample it is finer and close, performance is more superior.
Embodiment
Such scheme is described further below in conjunction with specific embodiment.It should be understood that these embodiments are to be used to illustrate
The present invention and be not limited to limit the scope of the present invention.
Embodiment 1
(1) according to 0.95Sr2Na6Al6Si6O24(SO4)2-0.05TiO2Middle Sr:Na:Al:Si:S:Ti mol ratio weighs
Raw material containing each element (is respectively SrCO3、Na2CO3、Al2O3、SiO2、(NH4)2SO4、TiO2), the raw material that then will have been weighed
Carry out wet ball-milling, ball milling 2 hours；Drying obtains raw mixture powder after ball milling；By pressed by powder into blocks, 1000
4 hours are incubated at DEG C, obtains sample burning block；
(2) it is the grinding of sample burning block is broken, it is put into ball grinder, zirconia ball and deionized water is pre-loaded with ball grinder；
Put ball grinder into ball mill, the revolution rotating speed for setting ball mill is 280rpm per minute, and wet ball-milling stops after 2 hours；It is past
A small amount of dispersant is added in ball grinder, then in a manner of ball grinder rotation, rotating speed is that 300rpm per minute carries out ball milling 1 hour,
Sample powder is dried to obtain after ball milling；
(3) the sample powder of drying is put into the ball grinder equipped with the appropriate deionized water necessarily matched and alcohol mixeding liquid
It is interior, then the ball grinder is put into supersonic cleaning machine, water is housed, ball grinder is fixed in water, the height of water in supersonic cleaning machine
For ball grinder mid-height；The heating and thermal insulation program of supersonic cleaning machine is set, to the 40 DEG C and herein temperature of the water in heated wash machine
Degree insulation；Then ball grinder lid is closed, opens ultrasonic vibration, sample powder is in a sealed meter environment by ultrasonic vibration, supersonic frequency
Rate is 50kHz, ultrasonic vibration 30 minutes；Then remove ball grinder lid, heat supersonic cleaning machine reclaimed water temperature to 95 DEG C simultaneously
It is incubated the temperature, ultrasonic vibration 30 minutes, supersonic frequency 30kHz；
(4) dried after ultrasonic vibration terminates, obtain sample powder, be then granulated, sieve, the particle after sieving is pressed into
Type, 4 hours are then sintered at 1100 DEG C into porcelain, obtains temperature-stabilized microwave medium ceramic material.
Foregoing dispersant is the mixing thing liquid of Sodium Polyacrylate, calgon, sodium pyrophosphate and polyethylene glycol
Body, and the addition of the dispersant is the 0.1% of sample quality；Sodium Polyacrylate, calgon, sodium pyrophosphate and poly- second two
The mass ratio of alcohol is 3:1:1:1.Deionized water and alcohol mixeding liquid in abovementioned steps (3) are made up of following proportioning：Deionization
Water weight：Ethanol weight=1：9.
The microwave dielectric property of this group of ceramic material is：Dielectric constant is 9.6, quality factor 77400GHz, resonance frequency
Rate temperature coefficient is -17.8ppm/ DEG C.
Embodiment 2
Embodiment 1 the step of in (1), according to 0.92Sr2Na6Al6Si6O24(SO4)2-0.08TiO2Middle Sr:Na:Al:
Si:S:Ti mol ratio weighs the raw material containing each element；Embodiment 1 the step of in (4), the particle after sieving is pressed into
Type, 4 hours are then sintered at 1125 DEG C into porcelain；Other step (containing raw material) same as Example 1, dispersants, deionized water
It is also identical with embodiment 1 with addition with the composition of alcohol mixeding liquid, obtain temperature-stabilized microwave medium ceramic material.
The microwave dielectric property of this group of ceramic material is：Dielectric constant is 10, quality factor 70000GHz, resonant frequency
Temperature coefficient is -8.5ppm/ DEG C.
Embodiment 3
Embodiment 1 the step of in (1), according to 0.9Sr2Na6Al6Si6O24(SO4)2-0.1TiO2Middle Sr:Na:Al:Si:
S:Ti mol ratio weighs the raw material containing each element；It is embodiment 1 the step of in (4), the particle after sieving is compressing, so
4 hours are sintered at 1150 DEG C afterwards into porcelain；Other step (containing raw material) same as Example 1, dispersant, deionized water and ethanol
The composition of mixed liquor is also identical with embodiment 1 with addition, obtains temperature-stabilized microwave medium ceramic material.
The microwave dielectric property of this group of ceramic material is：Dielectric constant is 10.2, quality factor 64800GHz, resonance frequency
Rate temperature coefficient is -2ppm/ DEG C.
Embodiment 4
Embodiment 1 the step of in (1), according to 0.95Sr2Na6Al6Si6O24(MoO4)2-0.05TiO2Middle Sr:Na:Al:
Si:Mo:It (is respectively SrCO that Ti mol ratio, which weighs the raw material containing each element,3、Na2CO3、Al2O3、SiO2、MoO3、TiO2)；Other
Step is same as Example 1, dispersant, and the composition of deionized water and alcohol mixeding liquid is also identical with embodiment 1 with addition, obtains
To temperature-stabilized microwave medium ceramic material.
The microwave dielectric property of this group of ceramic material is：Dielectric constant is 9.8, quality factor 92000GHz, resonance frequency
Rate temperature coefficient is -21.4ppm/ DEG C.
Embodiment 5
Embodiment 1 the step of in (1), according to 0.92Sr2Na6Al6Si6O24(MoO4)2-0.08TiO2Middle Sr:Na:Al:
Si:Mo:It (is respectively SrCO that Ti mol ratio, which weighs the raw material containing each element,3、Na2CO3、Al2O3、SiO2、MoO3、TiO2)；In reality
It is in the step of applying example 1 (4), the particle after sieving is compressing, 4 hours are then sintered at 1130 DEG C into porcelain；Other steps
Same as Example 1, dispersant, the composition of deionized water and alcohol mixeding liquid is also identical with embodiment 1 with addition, obtains temperature
Spend stable type microwave dielectric ceramic materials.
The microwave dielectric property of this group of ceramic material is：Dielectric constant is 10.5, quality factor 86000GHz, resonance frequency
Rate temperature coefficient is -9.7ppm/ DEG C.
Embodiment 6
Embodiment 1 the step of in (1), according to 0.9Sr2Na6Al6Si6O24(MoO4)2-0.1TiO2Middle Sr:Na:Al:Si:
Mo:It (is respectively SrCO that Ti mol ratio, which weighs the raw material containing each element,3、Na2CO3、Al2O3、SiO2、MoO3、TiO2)；Implementing
It is in the step of example 1 (4), the particle after sieving is compressing, 4 hours are then sintered at 1150 DEG C into porcelain；Other steps with
Embodiment 1 is identical, dispersant, and the composition of deionized water and alcohol mixeding liquid is also identical with embodiment 1 with addition, obtains temperature
Stable type microwave dielectric ceramic materials.
The microwave dielectric property of this group of ceramic material is：Dielectric constant is 11, quality factor 78700GHz, resonant frequency
Temperature coefficient is -2.8ppm/ DEG C.
Embodiment 7
Embodiment 1 the step of in (1), according to 0.95Sr2Na6Al6Si6O24(WO4)2-0.05TiO2Middle Sr:Na:Al:
Si:W:It (is respectively SrCO that Ti mol ratio, which weighs the raw material containing each element,3、Na2CO3、Al2O3、SiO2、WO3、TiO2)；Other steps
The composition of rapid same as Example 1, dispersant, deionized water and alcohol mixeding liquid is also identical with embodiment 1 with addition, obtains
Temperature-stabilized microwave medium ceramic material.
The microwave dielectric property of this group of ceramic material is：Dielectric constant is 10.3, quality factor 81000GHz, resonance frequency
Rate temperature coefficient is -12.1ppm/ DEG C.
Embodiment 8
Embodiment 1 the step of in (1), according to 0.93Sr2Na6Al6Si6O24(WO4)2-0.07TiO2Middle Sr:Na:Al:
Si:W:It (is respectively SrCO that Ti mol ratio, which weighs the raw material containing each element,3、Na2CO3、Al2O3、SiO2、WO3、TiO2)；Implementing
It is in the step of example 1 (4), the particle after sieving is compressing, 4 hours are then sintered at 1120 DEG C into porcelain；Other steps with
Embodiment 1 is identical, dispersant, and the composition of deionized water and alcohol mixeding liquid is also identical with embodiment 1 with addition, obtains temperature
Stable type microwave dielectric ceramic materials.
The microwave dielectric property of this group of ceramic material is：Dielectric constant is 10.8, quality factor 75000GHz, resonance frequency
Rate temperature coefficient is -2.6ppm/ DEG C.
Embodiment 9
Embodiment 1 the step of in (1), according to 0.9Sr2Na6Al6Si6O24(WO4)2-0.1TiO2Middle Sr:Na:Al:Si:
W:It (is respectively SrCO that Ti mol ratio, which weighs the raw material containing each element,3、Na2CO3、Al2O3、SiO2、WO3、TiO2)；In embodiment 1
The step of (4) in, the particle after sieving is compressing, 4 hours are then sintered at 1140 DEG C into porcelain；Other steps are with implementing
Example 1 is identical, dispersant, and the composition of deionized water and alcohol mixeding liquid is also identical with embodiment 1 with addition, obtains temperature stabilization
Type microwave dielectric ceramic materials.
The microwave dielectric property of this group of ceramic material is：Dielectric constant is 11.3, quality factor 70200GHz, resonance frequency
Rate temperature coefficient is 7.7ppm/ DEG C.
Embodiment 10
Embodiment 1 the step of in (1), according to Sr2Na6Al6Si6O24(XO4)2Sr in (one kind in X S, Mo or W):
Na:Al:Si:X:Ti mol ratio weighs raw material (the raw material SrCO containing each element3、Na2CO3、Al2O3、SiO2、(NH4)2SO4、
MoO3、WO3、TiO2)；It is embodiment 1 the step of in (4), the particle after sieving is compressing, then sinter 4 at 1130 DEG C
Hour, other steps were same as Example 1, dispersant, composition and addition and the reality of deionized water and alcohol mixeding liquid into porcelain
It is also identical to apply example 1, obtains temperature-stabilized microwave medium ceramic material.
The microwave dielectric property of this group of ceramic material is respectively：Sr2Na6Al6Si6O24(SO4)2Dielectric constant：8.9, quality
Factor：82000GHz, temperature coefficient of resonance frequency：-23.7ppm/℃；Sr2Na6Al6Si6O24(MoO4)2Dielectric constant：10, product
Prime factor：97000GHz, temperature coefficient of resonance frequency：-29.6ppm/℃；Sr2Na6Al6Si6O24(WO4)2Dielectric constant：10.7,
Quality factor：86000GHz, temperature coefficient of resonance frequency：-17ppm/℃.
Above content is to combine specific preferred embodiment further description made for the present invention, it is impossible to is assert
The embodiment of the present invention is only limitted to this, for general technical staff of the technical field of the invention, is not taking off
On the premise of from present inventive concept, some simple deduction or replace can also be made, the present invention should be all considered as belonging to and be carried
The claim of friendship determines scope of patent protection.
Claims (7)
1. a kind of temperature-stabilized microwave medium ceramic material, it is characterised in that the chemical constitution formula of the ceramic material is：(1-
y)Sr2Na6Al6Si6O24(XO4)2-yTiO2, wherein 0.05≤y≤0.1, y are mol ratio, one kind in X S, Mo or W；The pottery
The microwave dielectric property of ceramic material is：Dielectric constant is 9.6~11.3, and quality factor q f is 64800~92000GHz, and resonance is frequently
Rate temperature coefficient is -21.4ppm/ DEG C~13.9ppm/ DEG C.
2. temperature-stabilized microwave medium ceramic material according to claim 1, it is characterised in that described ceramic material
In, Sr2Na6Al6Si6O24(XO4)2Structure be blue party stone structure, and its quality factor is 82000~97000GHz, and dielectric is normal
Number is 8.9~10.7, and temperature coefficient of resonance frequency is negative.
A kind of 3. preparation method of the temperature-stabilized microwave medium ceramic material described in claim 1, it is characterised in that it by
Following steps form：
(1) according to (1-y) Sr2Na6Al6Si6O24(XO4)2-yTiO2Middle Sr:Na:Al:Si:X:Ti mol ratio is weighed containing each member
The raw material of element, wherein 0.05≤y≤0.1, y are mol ratio, X is positive hexad；Then the raw material weighed is subjected to wet type
Ball milling, ball milling 2 hours；Drying obtains raw mixture powder after ball milling, by pressed by powder into blocks, is incubated at 1000 DEG C
4 hours, obtain sample burning block；
(2) it is the grinding of sample burning block is broken, it is put into ball grinder, zirconia ball and deionized water is pre-loaded with ball grinder；By ball
Grinding jar puts ball mill into, and the revolution rotating speed for setting ball mill is 280rpm per minute, and wet ball-milling stops after 2 hours；Toward ball milling
A small amount of dispersant is added in tank, then in a manner of ball grinder rotation, rotating speed is that 300rpm per minute carries out ball milling 1 hour, ball milling
After dry to obtain sample powder；
(3) the sample powder of drying is put into the ball grinder equipped with the appropriate deionized water necessarily matched and alcohol mixeding liquid,
The ball grinder is put into supersonic cleaning machine again, water is housed in supersonic cleaning machine, ball grinder is fixed in water, and the height of water is ball
Grinding jar mid-height；The heating and thermal insulation program of supersonic cleaning machine is set, the water in heated wash machine is protected to 40 DEG C and in this temperature
Temperature；Then ball grinder lid is closed, opens ultrasonic vibration, sample powder is in a sealed meter environment by ultrasonic vibration, supersonic frequency
50kHz, ultrasonic vibration 30 minutes；Then ball grinder lid is removed, the temperature of heating supersonic cleaning machine reclaimed water to 95 DEG C and is incubated
The temperature, ultrasonic vibration 30 minutes, supersonic frequency 30kHz；
(4) dried after ultrasonic vibration terminates, obtain sample powder, be then granulated, sieve, the particle after sieving is compressing,
Then 4 hours are sintered at 1100 DEG C~1150 DEG C into porcelain, obtains temperature-stabilized microwave medium ceramic material.
4. the preparation method of temperature-stabilized microwave medium ceramic material according to claim 3, it is characterised in that described
Preparation method in, positive hexad X is one kind in S, Mo or W.
5. the preparation method of temperature-stabilized microwave medium ceramic material according to claim 3, it is characterised in that described
Preparation method in, the raw material containing each element is SrCO3、Na2CO3、Al2O3、SiO2、(NH4)2SO4、WO3、MoO3And TiO2。
6. the preparation method of temperature-stabilized microwave medium ceramic material according to claim 3, it is characterised in that described
Dispersant be Sodium Polyacrylate, calgon, the mixture liquid of sodium pyrophosphate and polyethylene glycol, and the dispersant adds
Dosage is the 0.1% of sample quality；Sodium Polyacrylate, calgon, the mass ratio of sodium pyrophosphate and polyethylene glycol are 3:1:
1:1。
7. the preparation method of temperature-stabilized microwave medium ceramic material according to claim 3, it is characterised in that described
Deionized water and alcohol mixeding liquid in step (3) are made up of following proportioning：Deionized water weight：Ethanol weight=1：9.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111384524A (en) * | 2018-12-31 | 2020-07-07 | 深圳市大富科技股份有限公司 | Dielectric filter, method for preparing dielectric filter and communication equipment |
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