CN105819846A - Cordierite type microwave medium ceramic material and preparation method thereof - Google Patents
Cordierite type microwave medium ceramic material and preparation method thereof 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
- C04B35/01—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
- C04B35/16—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 silicates other than clay
- C04B35/18—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 silicates other than clay rich in aluminium oxide
- C04B35/195—Alkaline earth aluminosilicates, e.g. cordierite or anorthite
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
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Abstract
The invention relates to a cordierite type microwave medium ceramic material and a preparation method thereof. The chemical formula of the microwave ceramic is Mg<2>Al<4>(Si<5-x>Ti<x>)O<18>, 0.05=<x=<0.40. The preparation method comprises the following steps: precisely weighing powder of oxides of each element in the chemical formula according to the chemical formula, mixing, evenly grinding, pre-burning, granulating, pressing granules into sheets, moulding, sintering to prepare ceramic, mechanically processing the ceramic to prepare a dielectric resonator in the late period, and carrying out a microwave test on the dielectric resonator. The disclosed microwave ceramic has a low dielectric constant, a high quality factor, and a temperature coefficient of resonance frequency, which is close to zero, and thus is suitable for being used as a substrate material of a microwave circuit.
Description
Technical field
The invention belongs to electronic information function ceramic material and device arts, be specifically related to
Altofrequency, low-k, high quality factor, low resonant frequency temperature drift coefficient feature
A kind of Mg2Al4(Si5-xTix)O18Microwave dielectric ceramic materials and preparation method thereof.
Background technology
Along with electronic technology is towards more miniaturization, integrated, the development in high frequency direction, letter
Electronics under the drive of breath technology is unprecedentedly universal and fast development makes communication frequency band
Contention the fiercest, all kinds of high-quality transmission of wireless signals make the components and parts must high frequency.
The electronic component producing applicable high-frequency microwave application becomes inevitable.Owing to this kind of electronic component works
Under microwave frequency band, thus the frequency response of microwave being had higher requirement, it is suitable to usually require that
Dielectric constant ensure the Sizes of device, higher quality factor reduce device transmission signal
During loss, low resonant frequency temperature drift coefficient guarantees that the working environment of device is by temperature
The restriction of degree change.That has reported at present is good in operating ambient temperature lower frequency temperature stability,
It is not a lot of that little and that dielectric constant less than 10 low dielectric microwave media ceramic kind is lost.
The present invention provides a kind of dielectric constant at the dielectric constant microwave ceramic medium of 6~about 7, has
Help supplement this series products, form system.
Summary of the invention
It is an object of the invention under prior art conditions, meet growing microwave and lead to
The development of letter technology is to low dielectric, low-loss, low resonant frequency temperature drift coefficient microwave material
Need, it is provided that a kind of silicates microwave dielectric ceramic materials, this ceramic dielectric constant
6~about 7, low-k, microwave property is excellent and near-zero frequency temperature coefficient.
The chemical formula of the cordierite type microwave dielectric material of the present invention is Mg2Al4(Si5-xTix)O18,
0.05≤x≤0.40;The DIELECTRIC CONSTANT ε of this microwave-medium ceramics systemrScope is 6.1~6.6,
Quality factor q f scope is 42,000~75,300GHZ, temperature coefficient of resonance frequency τfScope
For-24~+5ppm/ DEG C;
Make a general survey of this series compound, 0.05≤x≤0.40, this microwave dielectric ceramic materials thing phase
Mainly include single Mg2Al4(Si5-xTix)O18Cordierite solid solution phase, there is no rutile-type
TiO2Producing mutually, that nature exists in a large number is Mg2Al4Si5O18Cordierite type mineral, work as TiO2
With MgO, Al2O3And SiO2It is to have with cordierite according to generate after corresponding proportioning hybrid reaction
The Mg of same crystal structure Cccm (66)2Al4(Si5-xTix)O18。
It is a further object to provide the preparation method of above-mentioned microwave dielectric ceramic materials,
Specifically comprise the following steps that
(1). raw-material choose:
Purity (weight/mass percentage composition) is MgO, the purity (quality hundred of 99.70%~99.99%
Point content) it is the Al of 99.70%~99.99%2O3, purity (weight/mass percentage composition) be
The SiO of 99.70%~99.99%2It is 99.80%~99.99% with purity (weight/mass percentage composition)
TiO2;
(2). dispensing and batch mixing:
By MgO, Al2O3、SiO2、TiO2According to chemical formula Mg2Al4(Si5-xTix)O18Weigh former
Material, using dehydrated alcohol as abrasive media, is placed in grinding in ball grinder 18~24 hours, obtains
Thick compound;Then this compound is placed in 70 DEG C~90 DEG C of baking ovens and is dried to constant weight,
Obtain dry pack;
(3).Mg2Al4(Si5-xTix)O18Ceramic Material pre-burning:
Dry pack step (2) obtained first crosses 80 mesh standard sieves, after allowing granule be uniformly dispersed,
It is placed in box Muffle furnace 1250~1350 DEG C of pre-burnings 4 hours, makes mixed powder initial reaction
Generate Mg2Al4(Si5-xTix)O18Ceramic material, adds in the ceramic material that initial reaction generates again
Enter dehydrated alcohol, be placed in ball milling 18~taking-up after 24 hours in ball mill, be placed in 60~110 DEG C
Baking oven is dried to constant weight, obtain the Mg of particle diameter refinement2Al4(Si5-xTix)O18Ceramic material;
(4).Mg2Al4(Si5-xTix)O18The pelletize of ceramic material:
Mg after the particle diameter refinement that step 3 is obtained2Al4(Si5-xTix)O1880 mesh first crossed by ceramic material
Standard screen, after making granule be uniformly dispersed, adds binding agent mixing, after the refinement of every 40g particle diameter
Mg2Al4(Si5-xTix)O18Ceramic material adds 1.5ml~3ml binding agent, by the material after mixing
Insert in pressed powder forming machine, be pressed under 100~200Mpa pressure a diameter of 30~
40mm, thickness are the cylinder of 9~15mm;Crush after displaying 30 minutes, after crushing
Mg2Al4(Si5-xTix)O18Material granule crosses lamination standard screen successively, and this standard screen upper strata is 60
Mesh, lower floor is 120 mesh.Will be by 120 mesh standard sieves, the meticulous granule of particle diameter is as step
(6) bedding and padding, choose by 60 mesh sieves, but not by the granule of 120 mesh sieves as finally
Compressing material;
Described binding agent be mass concentration be the poly-vinyl alcohol solution of 5wt%~10wt%
(PVA);
(5).Mg2Al4(Si5-xTix)O18The compression molding of ceramic material:
The compressing material chosen in step (4) is inserted in pressed powder forming machine, 90~
Be pressed into a diameter of 15mm under 100Mpa pressure, thickness be 6~7mm cylinder;
(6).Mg2Al4(Si5-xTix)O18Ceramic material sinter porcelain into:
Cylinder step (5) being pressed into sinters 4 hours at a temperature of 1350~1450 DEG C, sintering
Time sample be placed on the aluminium oxide flat board being covered with bedding and padding, control less than 1000 DEG C programming rates
Being 4 DEG C/min, 1000 DEG C to sintering temperature programming rate is 2 DEG C/min, and sintering temperature arrives
The cooling rate of 1000 DEG C is 2 DEG C/min, closes temperature control system for less than 1000 DEG C and is naturally cooling to
Room temperature, finally obtains the Mg of given shape2Al4(Si5-xTix)O18Pottery;
(7). later stage machining:
The Mg that will sinter2Al4(Si5-xTix)O18Finished product is made in ceramic grinding polishing.
The present invention uses the dielectric resonance post method test cylinder that Hakki and Coleman proposes
Under resonant frequency, microwave dielectric property [is referred to document: B.W.Hakki, and P.D.
Coleman, " Dielectric Resonator Method of Measuring Inductive
Capacities in the Millimeter Range, " IEEE Trans.Microw.Theory
Technol .Mtt-8,402 (1970)].
This microwave ceramics has low-k (6.1~6.6), belongs to low dielectric constant ceramic system.
This pottery is possible not only to obtain higher quality factor (Qf) 75,300GHz, minimum 49,000
GHZ.Temperature coefficient of resonance frequency nearly zero 0.2ppm/ DEG C, compare Mg2Al4Si5O18's
Qf (39,000GHz), temperature coefficient of resonance frequency (-32.1ppm/ DEG C) all has bigger performance to carry
Rise.This pottery is suitable as microwave circuit baseplate material.
Accompanying drawing explanation
Fig. 1 is the ceramic material XRD accompanying drawing spectrum that the embodiment of the present invention 1~8 prepares;
Fig. 2 is the ceramic dielectric constant accompanying drawing that the embodiment of the present invention 1~8 prepares;
Fig. 3 is the ceramic material quality factor accompanying drawing that the embodiment of the present invention 1~8 prepares;
Fig. 4 is the ceramic material resonant frequency temperature system that the embodiment of the present invention 1~8 prepares
Number accompanying drawing.
Detailed description of the invention
Example 1: preparation Mg2Al4(Si5-0.05Ti0.05)O18
Step (1). raw-material choose:
Purity (weight/mass percentage composition) is MgO, the purity (weight/mass percentage composition) of 99.99%
It is the Al of 99.99%2O3, purity (weight/mass percentage composition) be the SiO of 99.99%2And purity
(weight/mass percentage composition) is the TiO of 99.8%2;
Step (2). dispensing and batch mixing:
By MgO, Al2O3、SiO2、TiO2According to chemical formula Mg2Al4(Si5-xTix)O18For measuring,
Weigh 6.8854g MgO, 17.4012g Al successively2O3、25.3794g SiO2、0.3414g TiO2
Raw material, using dehydrated alcohol as abrasive media, is placed in grinding in ball grinder 24 hours, obtains
Aqueous compound;Then aqueous compound is placed in 90 DEG C of baking ovens and is dried to constant weight, obtain
The compound being dried;
Step (3) .Mg2Al4(Si5-0.05Ti0.05)O18Ceramic Material pre-burning:
Dry pack step (2) obtained first crosses 80 mesh standard sieves, after allowing granule be uniformly dispersed,
It is placed in box Muffle furnace 1250 DEG C of pre-burnings 4 hours, makes mixed powder initial reaction generate
Mg2Al4(Si5-0.05Ti0.05)O18Ceramic material;The ceramic material that initial reaction generates adds
Dehydrated alcohol, is placed in ball milling in ball mill and takes out after 24 hours, is placed in 90 DEG C of baking ovens drying
Do to constant weight, obtain the Mg of particle diameter refinement2Al4(Si5-0.05Ti0.05)O18Ceramic material;
Step (4) .Mg2Al4(Si5-0.05Ti0.05)O18The pelletize of ceramic material:
Mg after the particle diameter refinement that step (3) is obtained2Al4(Si5-0.05Ti0.05)O18Ceramic material first mistake
80 mesh standard sieves, after making granule be uniformly dispersed, are subsequently adding binding agent mixing, after mixing
Material insert in pressed powder forming machine, be pressed into a diameter of under 100~200Mpa pressure
30mm, thickness are the cylinder of 9mm;Crush after displaying 30 minutes, pelletize, will crushing
After Mg2Al4(Si5-0.05Ti0.05)O18Material granule crosses lamination standard screen successively, on this standard screen
Layer is 60 mesh, and lower floor is 120 mesh.The granule meticulous by 120 mesh standard sieve particle diameters is made
For the bedding and padding of step (6), choose by 60 mesh sieves, but do not made by the granule of 120 mesh sieves
For last compressing material;Obtain last compressing material;After every 40g particle diameter refinement
Mg2Al4(Si5-0.05Ti0.05)O18Ceramic material adds 3ml binding agent;
Described binding agent be mass concentration be the poly-vinyl alcohol solution (PVA) of 5wt%;
Step (5) .Mg2Al4(Si5-0.05Ti0.05)O18The compression molding of ceramic material:
The compressing material chosen in step (4) is inserted in pressed powder forming machine, 90~
Be pressed into a diameter of 15mm under 100Mpa pressure, thickness be 6~7mm cylinder;
Step (6) .Mg2Al4(Si5-0.05Ti0.05)O18Ceramic material sinter porcelain into:
Cylinder step (5) being pressed into sinters 4 hours at a temperature of 1450 DEG C, controls 1000 DEG C
Following programming rate is 4 DEG C/min, and 1000 DEG C to sintering temperature programming rate is 2 DEG C/min,
The cooling rate of sintering temperature to 1000 DEG C is 2 DEG C/min, closes temperature control system for less than 1000 DEG C
It is naturally cooling to room temperature, finally obtains the Mg of given shape2Al4(Si5-0.05Ti0.05)O18Pottery;
Step (7). later stage machining:
The Mg that will sinter2Al4(Si5-0.05Ti0.05)O18Finished product is made in ceramic grinding polishing.
The present invention uses the dielectric resonance cell method test cylinder that Hakki and Coleman proposes
Microwave dielectric property under resonant frequency.As initial group of the present invention, the microwave of this pottery is situated between
Electrical property is tested under 13.8GHZ resonant frequency: dielectric constant is 6.1, quality factor
Qf is 42,500GHZ, and temperature coefficient of resonance frequency is-24ppm/ DEG C, result see accompanying drawing 1~
4。
Example 2: preparation Mg2Al4(Si5-0.10Ti0.10)O18,
Step (1). raw-material choose:
Purity (weight/mass percentage composition) is MgO, the purity (weight/mass percentage composition) of 99.99%
It is the Al of 99.99%2O3, purity (weight/mass percentage composition) be the SiO of 99.99%2And purity
(weight/mass percentage composition) is the TiO of 99.8%2;
Step (2). dispensing and batch mixing:
By MgO, Al2O3、SiO2、TiO2According to chemical formula Mg2Al4(Si5-0.10Ti0.10)O18For
Metering, weighs 6.8738g MgO, 17.3719g Al successively2O3、25.0807g SiO2、0.6817g
TiO2Raw material, using dehydrated alcohol as abrasive media, is placed in grinding in ball grinder 24 hours,
Obtain aqueous compound;Then aqueous compound is placed in 90 DEG C of baking ovens and is dried to constant weight,
Obtain the compound being dried;
Step (3) .Mg2Al4(Si5-0.10Ti0.10)O18Ceramic Material pre-burning:
Dry pack step (2) obtained first crosses 80 mesh standard sieves, after allowing granule be uniformly dispersed,
It is placed in box Muffle furnace 1250 DEG C of pre-burnings 4 hours, makes mixed powder initial reaction generate
Mg2Al4(Si5-0.10Ti0.10)O18Ceramic material;The ceramic material that initial reaction generates adds
Dehydrated alcohol, is placed in ball milling in ball mill and takes out after 24 hours, is placed in 90 DEG C of baking ovens drying
Do to constant weight, obtain the Mg of particle diameter refinement2Al4(Si5-0.10Ti0.10)O18Ceramic material;
Step (4) .Mg2Al4(Si5-0.10Ti0.10)O18The pelletize of ceramic material:
Mg after the particle diameter refinement that step (3) is obtained2Al4(Si5-0.10Ti0.10)O18Ceramic material first mistake
80 mesh standard sieves, after making granule be uniformly dispersed, are subsequently adding binding agent mixing, after mixing
Material insert in pressed powder forming machine, be pressed into a diameter of under 100~200Mpa pressure
30mm, thickness are the cylinder of 9mm;Crush after displaying 30 minutes, pelletize, will crushing
After Mg2Al4(Si5-0.10Ti0.10)O18Material granule crosses lamination standard screen successively, on this standard screen
Layer is 60 mesh, and lower floor is 120 mesh.The granule meticulous by 120 mesh standard sieve particle diameters is made
For the bedding and padding of step (6), choose by 60 mesh sieves, but do not made by the granule of 120 mesh sieves
For last compressing material;Obtain last compressing material;After every 40g particle diameter refinement
Mg2Al4(Si5-0.10Ti0.10)O18Ceramic material adds 3ml binding agent;
Described binding agent be mass concentration be the poly-vinyl alcohol solution (PVA) of 5wt%;
Step (5) .Mg2Al4(Si5-0.10Ti0.10)O18The compression molding of ceramic material:
The compressing material chosen in step (4) is inserted in pressed powder forming machine, 90~
Be pressed into a diameter of 15mm under 100Mpa pressure, thickness be 6~7mm cylinder;
Step (6) .Mg2Al4(Si5-0.10Ti0.10)O18Ceramic material sinter porcelain into:
Cylinder step (5) being pressed into sinters 4 hours at a temperature of 1450 DEG C, controls 1000 DEG C
Following programming rate is 4 DEG C/min, and 1000 DEG C to sintering temperature programming rate is 2 DEG C/min,
The cooling rate of sintering temperature to 1000 DEG C is 2 DEG C/min, closes temperature control system for less than 1000 DEG C
It is naturally cooling to room temperature, finally obtains the Mg of given shape2Al4(Si5-0.10Ti0.10)O18Pottery;
Step (7). later stage machining:
The Mg that will sinter2Al4(Si5-0.10Ti0.10)O18Finished product is made in ceramic grinding polishing.
The present invention uses the dielectric resonance cell method test cylinder that Hakki and Coleman proposes
Microwave dielectric property under resonant frequency.Mg2Al4(Si5-0.10Ti0.10)O18The microwave dielectric property of pottery
Can test under 13.8GHZ resonant frequency and be: dielectric constant is 6.2, and quality factor q f is
49,000GHZ, temperature coefficient of resonance frequency is-19ppm/ DEG C, and result is shown in accompanying drawing 1~4.
Example 3: preparation Mg2Al4(Si5-0.15Ti0.15)O18,
Step (1). raw-material choose:
Purity (weight/mass percentage composition) is MgO, the purity (weight/mass percentage composition) of 99.99%
It is the Al of 99.99%2O3, purity (weight/mass percentage composition) be the SiO of 99.99%2And purity
(weight/mass percentage composition) is the TiO of 99.8%2;
Step (2). dispensing and batch mixing:
By MgO, Al2O3、SiO2、TiO2According to chemical formula Mg2Al4(Si5-0.15Ti0.15)O18For
Metering, weighs 6.8622g MgO, 17.3427g Al successively2O3、24.7830g SiO2、1.0208g
TiO2Raw material, using dehydrated alcohol as abrasive media, is placed in grinding in ball grinder 24 hours,
Obtain aqueous compound;Then aqueous compound is placed in 90 DEG C of baking ovens and is dried to constant weight,
Obtain the compound being dried;
Step (3) .Mg2Al4(Si5-0.15Ti0.15)O18Ceramic Material pre-burning:
Dry pack step (2) obtained first crosses 80 mesh standard sieves, after allowing granule be uniformly dispersed,
It is placed in box Muffle furnace 1250 DEG C of pre-burnings 4 hours, makes mixed powder initial reaction generate
Mg2Al4(Si5-0.15Ti0.15)O18Ceramic material;The ceramic material that initial reaction generates adds
Dehydrated alcohol, is placed in ball milling in ball mill and takes out after 24 hours, is placed in 90 DEG C of baking ovens drying
Do to constant weight, obtain the Mg of particle diameter refinement2Al4(Si5-0.15Ti0.15)O18Ceramic material;
Step (4) .Mg2Al4(Si5-0.15Ti0.15)O18The pelletize of ceramic material:
Mg after the particle diameter refinement that step (3) is obtained2Al4(Si5-0.15Ti0.15)O18Ceramic material first mistake
80 mesh standard sieves, after making granule be uniformly dispersed, are subsequently adding binding agent mixing, after mixing
Material insert in pressed powder forming machine, be pressed into a diameter of under 100~200Mpa pressure
30mm, thickness are the cylinder of 9mm;Crush after displaying 30 minutes, pelletize, will crushing
After Mg2Al4(Si5-0.15Ti0.15)O18Material granule crosses lamination standard screen successively, on this standard screen
Layer is 60 mesh, and lower floor is 120 mesh.The granule meticulous by 120 mesh standard sieve particle diameters is made
For the bedding and padding of step (5), choose by 60 mesh sieves, but do not made by the granule of 120 mesh sieves
For last compressing material;Obtain last compressing material;After every 40g particle diameter refinement
Mg2Al4(Si5-0.15Ti0.15)O18Ceramic material adds 3ml binding agent;
Described binding agent be mass concentration be the poly-vinyl alcohol solution (PVA) of 5wt%;
Step (5) .Mg2Al4(Si5-0.15Ti0.15)O18The compression molding of ceramic material:
The compressing material chosen in step (4) is inserted in pressed powder forming machine, 90~
Be pressed into a diameter of 15mm under 100Mpa pressure, thickness be 6~7mm cylinder;
Step (6) .Mg2Al4(Si5-0.15Ti0.15)O18Ceramic material sinter porcelain into:
Cylinder step (5) being pressed into sinters 4 hours at a temperature of 1450 DEG C, controls 1000 DEG C
Following programming rate is 4 DEG C/min, and 1000 DEG C to sintering temperature programming rate is 2 DEG C/min,
The cooling rate of sintering temperature to 1000 DEG C is 2 DEG C/min, closes temperature control system for less than 1000 DEG C
It is naturally cooling to room temperature, finally obtains the Mg of given shape2Al4(Si5-0.15Ti0.15)O18Pottery;
Step (7). later stage machining:
The Mg that will sinter2Al4(Si5-0.15Ti0.15)O18Finished product is made in ceramic grinding polishing.
The present invention uses the dielectric resonance cell method test cylinder that Hakki and Coleman proposes
Microwave dielectric property under resonant frequency.As the matched group of the present invention,
Mg2Al4(Si5-0.15Ti0.15)O18The microwave dielectric property of pottery is surveyed under 13.8GHZ resonant frequency
Examination is: dielectric constant is 6.3, and quality factor q f is 59,000GHZ, resonant frequency temperature
Coefficient is-17ppm/ DEG C, and result is shown in accompanying drawing 1~4.
Example 4: preparation Mg2Al4(Si5-0.20Ti0.20)O18,
Step (1). raw-material choose:
Purity (weight/mass percentage composition) is MgO, the purity (weight/mass percentage composition) of 99.99%
It is the Al of 99.99%2O3, purity (weight/mass percentage composition) be the SiO of 99.99%2And purity
(weight/mass percentage composition) is the TiO of 99.8%2;
Step (2). dispensing and batch mixing:
By MgO, Al2O3、SiO2、TiO2According to chemical formula Mg2Al4(Si5-0.20Ti0.20)O18For
Metering, weighs 6.8507g MgO, 17.3135g Al successively2O3、24.4863g SiO2、1.3588g
TiO2Raw material, using dehydrated alcohol as abrasive media, is placed in grinding in ball grinder 24 hours,
Obtain aqueous compound;Then aqueous compound is placed in 90 DEG C of baking ovens and is dried to constant weight,
Obtain the compound being dried;
Step (3) .Mg2Al4(Si5-0.20Ti0.20)O18Ceramic Material pre-burning:
Dry pack step (2) obtained first crosses 80 mesh standard sieves, after allowing granule be uniformly dispersed,
It is placed in box Muffle furnace 1250 DEG C of pre-burnings 4 hours, makes mixed powder initial reaction generate
Mg2Al4(Si5-0.20Ti0.20)O18Ceramic material;The ceramic material that initial reaction generates adds
Dehydrated alcohol, is placed in ball milling in ball mill and takes out after 24 hours, is placed in 90 DEG C of baking ovens drying
Do to constant weight, obtain the Mg of particle diameter refinement2Al4(Si5-0.20Ti0.20)O18Ceramic material;
Step (4) .Mg2Al4(Si5-0.20Ti0.20)O18The pelletize of ceramic material:
Mg after the particle diameter refinement that step (3) is obtained2Al4(Si5-0.20Ti0.20)O18Ceramic material first mistake
80 mesh standard sieves, after making granule be uniformly dispersed, are subsequently adding binding agent mixing, after mixing
Material insert in pressed powder forming machine, be pressed into a diameter of under 100~200Mpa pressure
30mm, thickness are the cylinder of 9mm;Crush after displaying 30 minutes, pelletize, will crushing
After Mg2Al4(Si5-0.20Ti0.20)O18Material granule crosses lamination standard screen successively, on this standard screen
Layer is 60 mesh, and lower floor is 120 mesh.The granule meticulous by 120 mesh standard sieve particle diameters is made
For the bedding and padding of step (5), choose by 60 mesh sieves, but do not made by the granule of 120 mesh sieves
For last compressing material;Obtain last compressing material;After every 40g particle diameter refinement
Mg2Al4(Si5-0.20Ti0.20)O18Ceramic material adds 3ml binding agent;
Described binding agent be mass concentration be the poly-vinyl alcohol solution (PVA) of 5wt%;
Step (5) .Mg2Al4(Si5-0.20Ti0.20)O18The compression molding of ceramic material:
The compressing material chosen in step (4) is inserted in pressed powder forming machine, 90~
Be pressed into a diameter of 15mm under 100Mpa pressure, thickness be 6~7mm cylinder;
Step (6) .Mg2Al4(Si5-0.20Ti0.20)O18Ceramic material sinter porcelain into:
Cylinder step (5) being pressed into sinters 4 hours at a temperature of 1450 DEG C, controls 1000 DEG C
Following programming rate is 4 DEG C/min, and 1000 DEG C to sintering temperature programming rate is 2 DEG C/min,
The cooling rate of sintering temperature to 1000 DEG C is 2 DEG C/min, closes temperature control system for less than 1000 DEG C
It is naturally cooling to room temperature, finally obtains the Mg of given shape2Al4(Si5-0.20Ti0.20)O18Pottery;
Step (7). later stage machining:
The Mg that will sinter2Al4(Si5-0.20Ti0.20)O18Finished product is made in ceramic grinding polishing.
The present invention uses the dielectric resonance cell method test cylinder that Hakki and Coleman proposes
Microwave dielectric property under resonant frequency.As the matched group of the present invention, pure
Mg2Al4(Si5-0.20Ti0.20)O18The microwave dielectric property of pottery is surveyed under 13.0GHZ resonant frequency
Examination is: dielectric constant is 6.3, and quality factor q f is 74,000GHZ, resonant frequency temperature
Coefficient is-13ppm/ DEG C, and result is shown in accompanying drawing 1~4.
Example 5: preparation Mg2Al4(Si5-0.25Ti0.25)O18,
Step (1). raw-material choose:
Purity (weight/mass percentage composition) is MgO, the purity (weight/mass percentage composition) of 99.99%
It is the Al of 99.99%2O3, purity (weight/mass percentage composition) be the SiO of 99.99%2And purity
(weight/mass percentage composition) is the TiO of 99.8%2;
Step (2). dispensing and batch mixing:
By MgO, Al2O3、SiO2、TiO2According to chemical formula Mg2Al4(Si5-0.25Ti0.25)O18For
Metering, weighs 6.8392g MgO, 17.2845g Al successively2O3、24.1906g SiO2、1.6957g
TiO2Raw material, using dehydrated alcohol as abrasive media, is placed in grinding in ball grinder 24 hours,
Obtain aqueous compound;Then aqueous compound is placed in 90 DEG C of baking ovens and is dried to constant weight,
Obtain the compound being dried;
Step (3) .Mg2Al4(Si5-0.25Ti0.25)O188Ceramic Material pre-burning:
Dry pack step (2) obtained first crosses 80 mesh standard sieves, after allowing granule be uniformly dispersed,
It is placed in box Muffle furnace 1250 DEG C of pre-burnings 4 hours, makes mixed powder initial reaction generate
Mg2Al4(Si5-0.25Ti0.25)O18Ceramic material;The ceramic material that initial reaction generates adds
Dehydrated alcohol, is placed in ball milling in ball mill and takes out after 24 hours, is placed in 90 DEG C of baking ovens drying
Do to constant weight, obtain the Mg of particle diameter refinement2Al4(Si5-0.25Ti0.25)O18Ceramic material;
Step (4) .Mg2Al4(Si5-0.25Ti0.25)O18The pelletize of ceramic material:
Mg after the particle diameter refinement that step (3) is obtained2Al4(Si5-0.25Ti0.25)O18Ceramic material first mistake
80 mesh standard sieves, after making granule be uniformly dispersed, are subsequently adding binding agent mixing, after mixing
Material insert in pressed powder forming machine, be pressed into a diameter of under 100~200Mpa pressure
30mm, thickness are the cylinder of 9mm;Crush after displaying 30 minutes, pelletize, will crushing
After Mg2Al4(Si5-0.05Ti0.05)O18Material granule crosses lamination standard screen successively, on this standard screen
Layer is 60 mesh, and lower floor is 120 mesh.The granule meticulous by 120 mesh standard sieve particle diameters is made
For the bedding and padding of step (5), choose by 60 mesh sieves, but do not made by the granule of 120 mesh sieves
For last compressing material;Obtain last compressing material;After every 40g particle diameter refinement
Mg2Al4(Si5-0.05Ti0.05)O18Ceramic material adds 3ml binding agent;
Described binding agent be mass concentration be the poly-vinyl alcohol solution (PVA) of 5wt%;
Step (5) .Mg2Al4(Si5-0.25Ti0.25)O18The compression molding of ceramic material:
The compressing material chosen in step (4) is inserted in pressed powder forming machine, 90~
Be pressed into a diameter of 15mm under 100Mpa pressure, thickness be 6~7mm cylinder;
Step (6) .Mg2Al4(Si5-0.25Ti0.25)O18Ceramic material sinter porcelain into:
Cylinder step (5) being pressed into sinters 4 hours at a temperature of 1450 DEG C, controls 1000 DEG C
Following programming rate is 4 DEG C/min, and 1000 DEG C to sintering temperature programming rate is 2 DEG C/min,
The cooling rate of sintering temperature to 1000 DEG C is 2 DEG C/min, closes temperature control system for less than 1000 DEG C
It is naturally cooling to room temperature, finally obtains the Mg of given shape2Al4(Si5-0.25Ti0.25)O18Pottery;
Step (7). later stage machining:
The Mg that will sinter2Al4(Si5-0.25Ti0.25)O18Finished product is made in ceramic grinding polishing.
The present invention uses the dielectric resonance cell method test cylinder that Hakki and Coleman proposes
Microwave dielectric property under resonant frequency.As the matched group of the present invention,
Mg2Al4(Si5-0.25Ti0.25)O18The microwave dielectric property of pottery is surveyed under 15.0GHZ resonant frequency
Examination is: dielectric constant is 6.4, and quality factor q f is 68,500GHZ, resonant frequency temperature
Coefficient is-10ppm/ DEG C, and result is shown in accompanying drawing 1~4.
Example 6: preparation Mg2Al4(Si5-0.30Ti0.30)O18,
Step (1). raw-material choose:
Purity (weight/mass percentage composition) is MgO, the purity (weight/mass percentage composition) of 99.99%
It is the Al of 99.99%2O3, purity (weight/mass percentage composition) be the SiO of 99.99%2And purity
(weight/mass percentage composition) is the TiO of 99.8%2;
Step (2). dispensing and batch mixing:
By MgO, Al2O3、SiO2、TiO2According to chemical formula Mg2Al4(Si5-0.30Ti0.30)O18For
Metering, weighs 6.8278g MgO, 17.2556g Al successively2O3、23.8959g SiO2、2.0315g
TiO2Raw material, using dehydrated alcohol as abrasive media, is placed in grinding in ball grinder 24 hours,
Obtain aqueous compound;Then aqueous compound is placed in 90 DEG C of baking ovens and is dried to constant weight,
Obtain the compound being dried;
Step (3) .Mg2Al4(Si5-0.30Ti0.30)O18Ceramic Material pre-burning:
Dry pack step (2) obtained first crosses 80 mesh standard sieves, after allowing granule be uniformly dispersed,
It is placed in box Muffle furnace 1250 DEG C of pre-burnings 4 hours, makes mixed powder initial reaction generate
Mg2Al4(Si5-0.30Ti0.30)O18Ceramic material;The ceramic material that initial reaction generates adds
Dehydrated alcohol, is placed in ball milling in ball mill and takes out after 24 hours, is placed in 90 DEG C of baking ovens drying
Do to constant weight, obtain the Mg of particle diameter refinement2Al4(Si5-0.30Ti0.30)O18Ceramic material;
Step (4) .Mg2Al4(Si5-0.30Ti0.30)O18The pelletize of ceramic material:
Mg after the particle diameter refinement that step (3) is obtained2Al4(Si5-0.30Ti0.30)O18Ceramic material first mistake
80 mesh standard sieves, after making granule be uniformly dispersed, are subsequently adding binding agent mixing, after mixing
Material insert in pressed powder forming machine, be pressed into a diameter of under 100~200Mpa pressure
30mm, thickness are the cylinder of 9mm;Crush after displaying 30 minutes, pelletize, will crushing
After Mg2Al4(Si5-0.30Ti0.30)O18Material granule crosses lamination standard screen successively, on this standard screen
Layer is 60 mesh, and lower floor is 120 mesh.The granule meticulous by 120 mesh standard sieve particle diameters is made
For the bedding and padding of step (5), choose by 60 mesh sieves, but do not made by the granule of 120 mesh sieves
For last compressing material;Obtain last compressing material;After every 40g particle diameter refinement
Mg2Al4(Si5-0.30Ti0.30)O18Ceramic material adds 3ml binding agent;
Described binding agent be mass concentration be the poly-vinyl alcohol solution (PVA) of 5wt%;
Step (5) .Mg2Al4(Si5-0.30Ti0.30)O18The compression molding of ceramic material:
The compressing material chosen in step (4) is inserted in pressed powder forming machine, 90~
Be pressed into a diameter of 15mm under 100Mpa pressure, thickness be 6~7mm cylinder;
Step (6) .Mg2Al4(Si5-0.30Ti0.30)O18Ceramic material sinter porcelain into:
Cylinder step (5) being pressed into sinters 4 hours at a temperature of 1450 DEG C, controls 1000 DEG C
Following programming rate is 4 DEG C/min, and 1000 DEG C to sintering temperature programming rate is 2 DEG C/min,
The cooling rate of sintering temperature to 1000 DEG C is 2 DEG C/min, closes temperature control system for less than 1000 DEG C
It is naturally cooling to room temperature, finally obtains the Mg of given shape2Al4(Si5-0.30Ti0.30)O18Pottery;
Step (7). later stage machining:
The Mg that will sinter2Al4(Si5-0.30Ti0.30)O18Finished product is made in ceramic grinding polishing.
The present invention uses the dielectric resonance cell method test cylinder that Hakki and Coleman proposes
Microwave dielectric property under resonant frequency.As the matched group of the present invention, pure
Mg2Al4(Si5-0.30Ti0.30)O18The microwave dielectric property of pottery is surveyed under 17.2GHZ resonant frequency
Examination is: dielectric constant is 6.4, and quality factor q f is 75,000GHZ, resonant frequency temperature
Coefficient is-5ppm/ DEG C, and result is shown in accompanying drawing 1~4.
Example 7: preparation Mg2Al4(Si5-0.35Ti0.35)O18,
Step (1). raw-material choose:
Purity (weight/mass percentage composition) is MgO, the purity (weight/mass percentage composition) of 99.99%
It is the Al of 99.99%2O3, purity (weight/mass percentage composition) be the SiO of 99.99%2And purity
(weight/mass percentage composition) is the TiO of 99.8%2;
Step (2). dispensing and batch mixing:
By MgO, Al2O3、SiO2、TiO2According to chemical formula Mg2Al4(Si5-0.35Ti0.35)O18For
Metering, weighs 6.8164g MgO, 17.2267g Al successively2O3、23.6022g SiO2、2.3661g
TiO2Raw material, using dehydrated alcohol as abrasive media, is placed in grinding in ball grinder 24 hours,
Obtain aqueous compound;Then aqueous compound is placed in 90 DEG C of baking ovens and is dried to constant weight,
Obtain the compound being dried;
Step (3) .Mg2Al4(Si5-0.35Ti0.35)O18Ceramic Material pre-burning:
Dry pack step (2) obtained first crosses 80 mesh standard sieves, after allowing granule be uniformly dispersed,
It is placed in box Muffle furnace 1250 DEG C of pre-burnings 4 hours, makes mixed powder initial reaction generate
Mg2Al4(Si5-0.35Ti0.35)O18Ceramic material;The ceramic material that initial reaction generates adds
Dehydrated alcohol, is placed in ball milling in ball mill and takes out after 24 hours, is placed in 90 DEG C of baking ovens drying
Do to constant weight, obtain the Mg of particle diameter refinement2Al4(Si5-0.35Ti0.35)O18Ceramic material;
Step (4) .Mg2Al4(Si5-0.35Ti0.35)O18The pelletize of ceramic material:
Mg after the particle diameter refinement that step (3) is obtained2Al4(Si5-0.35Ti0.35)O18Ceramic material first mistake
80 mesh standard sieves, after making granule be uniformly dispersed, are subsequently adding binding agent mixing, after mixing
Material insert in pressed powder forming machine, be pressed into a diameter of under 100~200Mpa pressure
30mm, thickness are the cylinder of 9mm;Crush after displaying 30 minutes, pelletize, will crushing
After Mg2Al4(Si5-0.35Ti0.35)O18Material granule crosses lamination standard screen successively, on this standard screen
Layer is 60 mesh, and lower floor is 120 mesh.The granule meticulous by 120 mesh standard sieve particle diameters is made
For the bedding and padding of step (5), choose by 60 mesh sieves, but do not made by the granule of 120 mesh sieves
For last compressing material;Obtain last compressing material;After every 40g particle diameter refinement
Mg2Al4(Si5-0.35Ti0.35)O18Ceramic material adds 3ml binding agent;
Described binding agent be mass concentration be the poly-vinyl alcohol solution (PVA) of 5wt%;
Step (5) .Mg2Al4(Si5-0.35Ti0.35)O18The compression molding of ceramic material:
The compressing material chosen in step (4) is inserted in pressed powder forming machine, 90~
Be pressed into a diameter of 15mm under 100Mpa pressure, thickness be 6~7mm cylinder;
Step (6) .Mg2Al4(Si5-0.35Ti0.35)O18Ceramic material sinter porcelain into:
Cylinder step (5) being pressed into sinters 4 hours at a temperature of 1450 DEG C, controls 1000 DEG C
Following programming rate is 4 DEG C/min, and 1000 DEG C to sintering temperature programming rate is 2 DEG C/min,
The cooling rate of sintering temperature to 1000 DEG C is 2 DEG C/min, closes temperature control system for less than 1000 DEG C
It is naturally cooling to room temperature, finally obtains the Mg of given shape2Al4(Si5-0.35Ti0.35)O18Pottery;
Step (7). later stage machining:
The Mg that will sinter2Al4(Si5-0.35Ti0.35)O18Finished product is made in ceramic grinding polishing.
The present invention uses the dielectric resonance cell method test cylinder that Hakki and Coleman proposes
Microwave dielectric property under resonant frequency.As the matched group of the present invention,
Mg2Al4(Si5-0.35Ti0.35)O18The microwave dielectric property of pottery is surveyed under 13.9GHZ resonant frequency
Examination is: dielectric constant is 6.5, and quality factor q f is 71,000GHZ, resonant frequency temperature
Coefficient is-0.3ppm/ DEG C, and result is shown in accompanying drawing 1~4.
Example 8: preparation Mg2Al4(Si5-0.40Ti0.40)O18,
Step (1). raw-material choose:
Purity (weight/mass percentage composition) is MgO, the purity (weight/mass percentage composition) of 99.99%
It is the Al of 99.99%2O3, purity (weight/mass percentage composition) be the SiO of 99.99%2And purity
(weight/mass percentage composition) is the TiO of 99.8%2;
Step (2). dispensing and batch mixing:
By MgO, Al2O3、SiO2、TiO2According to chemical formula Mg2Al4(Si5-0.40Ti0.40)O18For
Metering, weighs 6.8050g MgO, 17.1980g Al successively2O3、23.3094g SiO2、2.6996g
TiO2Raw material, using dehydrated alcohol as abrasive media, is placed in grinding in ball grinder 24 hours,
Obtain aqueous compound;Then aqueous compound is placed in 90 DEG C of baking ovens and is dried to constant weight,
Obtain the compound being dried;
Step (3) .Mg2Al4(Si5-0.40Ti0.40)O18Ceramic Material pre-burning:
Dry pack step (2) obtained first crosses 80 mesh standard sieves, after allowing granule be uniformly dispersed,
It is placed in box Muffle furnace 1250 DEG C of pre-burnings 4 hours, makes mixed powder initial reaction generate
Mg2Al4(Si5-0.40Ti0.40)O18Ceramic material;The ceramic material that initial reaction generates adds
Dehydrated alcohol, is placed in ball milling in ball mill and takes out after 24 hours, is placed in 90 DEG C of baking ovens drying
Do to constant weight, obtain the Mg of particle diameter refinement2Al4(Si5-0.40Ti0.40)O18Ceramic material;
Step (4) .Mg2Al4(Si5-0.40Ti0.40)O18The pelletize of ceramic material:
Mg after the particle diameter refinement that step (3) is obtained2Al4(Si5-0.40Ti0.40)O18Ceramic material first mistake
80 mesh standard sieves, after making granule be uniformly dispersed, are subsequently adding binding agent mixing, after mixing
Material insert in pressed powder forming machine, be pressed into a diameter of under 100~200Mpa pressure
30mm, thickness are the cylinder of 9mm;Crush after displaying 30 minutes, pelletize, will crushing
After Mg2Al4(Si5-0.40Ti0.40)O18Material granule crosses lamination standard screen successively, on this standard screen
Layer is 60 mesh, and lower floor is 120 mesh.The granule meticulous by 120 mesh standard sieve particle diameters is made
For the bedding and padding of step (5), choose by 60 mesh sieves, but do not made by the granule of 120 mesh sieves
For last compressing material;Obtain last compressing material;After every 40g particle diameter refinement
Mg2Al4(Si5-0.40Ti0.40)O18Ceramic material adds 3ml binding agent;
Described binding agent be mass concentration be the poly-vinyl alcohol solution (PVA) of 5wt%;
Step (5) .Mg2Al4(Si5-0.40Ti0.40)O18The compression molding of ceramic material:
The compressing material chosen in step (4) is inserted in pressed powder forming machine, 90~
Be pressed into a diameter of 15mm under 100Mpa pressure, thickness be 6~7mm cylinder;
Step (6) .Mg2Al4(Si5-0.40Ti0.40)O18Ceramic material sinter porcelain into:
Cylinder step (5) being pressed into sinters 4 hours at a temperature of 1450 DEG C, controls 1000 DEG C
Following programming rate is 4 DEG C/min, and 1000 DEG C to sintering temperature programming rate is 2 DEG C/min,
The cooling rate of sintering temperature to 1000 DEG C is 2 DEG C/min, closes temperature control system for less than 1000 DEG C
It is naturally cooling to room temperature, finally obtains the Mg of given shape2Al4(Si5-0.40Ti0.40)O18Pottery;
Step (7). later stage machining:
The Mg that will sinter2Al4(Si5-0.40Ti0.40)O18Finished product is made in ceramic grinding polishing.
The present invention uses the dielectric resonance cell method test cylinder that Hakki and Coleman proposes
Microwave dielectric property under resonant frequency.As the matched group of the present invention,
Mg2Al4(Si5-0.40Ti0.40)O18The microwave dielectric property of pottery is surveyed under 13.6GHZ resonant frequency
Examination is: dielectric constant is 6.6, and quality factor q f is 73,000GHZ, resonant frequency temperature
Coefficient is 5ppm/ DEG C, and result is shown in accompanying drawing 1~4.
Above-mentioned detailed description of the invention is used for explaining the present invention rather than limiting the invention,
In the protection domain of spirit and claims of the present invention, any amendment that the present invention is made
And change, both fall within protection scope of the present invention.
Claims (2)
1. a cordierite type microwave dielectric ceramic materials, it is characterised in that its chemical composition is
Mg2Al4(Si5‐xTix)O18, 0.05≤x≤0.40.
A kind of Mg the most according to claim 12Al4(Si5‐xTix)O18Microwave dielectric ceramic materials
Preparation method, it is characterised in that comprise the following steps:
(1). raw-material choose:
Purity (weight/mass percentage composition) is MgO, the purity (quality hundred of 99.70%~99.99%
Point content) it is the Al of 99.70%~99.99%2O3, purity (weight/mass percentage composition) be
The SiO of 99.70%~99.99%2It is 99.80%~99.99% with purity (weight/mass percentage composition)
TiO2;
(2). dispensing and batch mixing:
By MgO, Al2O3、SiO2、TiO2According to chemical formula Mg2Al4(Si5‐xTix)O18Weigh former
Material, using dehydrated alcohol as abrasive media, is placed in grinding in ball grinder 18~24 hours, obtains
Thick compound;Then this compound is placed in 70 DEG C~90 DEG C of baking ovens and is dried to constant weight,
Obtain dry pack;
(3).Mg2Al4(Si5‐xTix)O18Ceramic Material pre-burning:
Dry pack step (2) obtained first crosses 80 mesh standard sieves, after allowing granule be uniformly dispersed,
It is placed in box Muffle furnace 1250~1350 DEG C of pre-burnings 4 hours, makes mixed powder initial reaction
Generate Mg2Al4(Si5‐xTix)O18Ceramic material, adds in the ceramic material that initial reaction generates again
Enter dehydrated alcohol, be placed in ball milling 18~taking-up after 24 hours in ball mill, be placed in 60~110 DEG C
Baking oven is dried to constant weight, obtain the Mg of particle diameter refinement2Al4(Si5‐xTix)O18Ceramic material;
(4).Mg2Al4(Si5‐xTix)O18The pelletize of ceramic material:
Mg after the particle diameter refinement that step 3 is obtained2Al4(Si5‐xTix)O1880 mesh first crossed by ceramic material
Standard screen, after making granule be uniformly dispersed, adds binding agent mixing, after the refinement of every 40g particle diameter
Mg2Al4(Si5‐xTix)O18Ceramic material adds 1.5ml~3ml binding agent, by the material after mixing
Insert in pressed powder forming machine, be pressed under 100~200Mpa pressure a diameter of 30~
40mm, thickness are the cylinder of 9~15mm;Crush after displaying 30 minutes, after crushing
Mg2Al4(Si5‐xTix)O18Material granule crosses lamination standard screen successively, and this standard screen upper strata is
60 mesh, lower floor is 120 mesh.Will be by 120 mesh standard sieves, the granule conduct that particle diameter is meticulous
The bedding and padding of step (6), choose by 60 mesh sieves, but not by the granule conduct of 120 mesh sieves
Last compressing material;
Described binding agent be mass concentration be the poly-vinyl alcohol solution of 5wt%~10wt%
(PVA);
(5).Mg2Al4(Si5‐xTix)O18The compression molding of ceramic material:
The compressing material chosen in step (4) is inserted in pressed powder forming machine, 90~
Be pressed into a diameter of 15mm under 100Mpa pressure, thickness be 6~7mm cylinder;
(6).Mg2Al4(Si5‐xTix)O18Ceramic material sinter porcelain into:
Cylinder step (5) being pressed into sinters 4 hours at a temperature of 1350~1450 DEG C, sintering
Time sample be placed on the aluminium oxide flat board being covered with bedding and padding, control less than 1000 DEG C programming rates
Being 4 DEG C/min, 1000 DEG C to sintering temperature programming rate is 2 DEG C/min, and sintering temperature arrives
The cooling rate of 1000 DEG C is 2 DEG C/min, closes temperature control system for less than 1000 DEG C and is naturally cooling to
Room temperature, finally obtains the Mg of given shape2Al4(Si5‐xTix)O18Pottery;
(7). later stage machining:
The Mg that will sinter2Al4(Si5‐xTix)O18Finished product is made in ceramic grinding polishing.
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CN106380183A (en) * | 2016-09-22 | 2017-02-08 | 深圳方泰新材料技术有限公司 | Wireless-communication microwave ceramic dielectric resonator, and preparation method and application thereof |
CN108249906A (en) * | 2018-04-20 | 2018-07-06 | 电子科技大学 | A kind of high-quality factor microwave medium ceramic material and preparation method |
CN111423225A (en) * | 2020-05-12 | 2020-07-17 | 电子科技大学 | Cordierite microwave dielectric ceramic material and preparation method thereof |
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