CN108383519A - A kind of microwave dielectric ceramic material and preparation method thereof - Google Patents
A kind of microwave dielectric ceramic material and preparation method thereof Download PDFInfo
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Abstract
The present invention provides a kind of microwave dielectric ceramic materials, are prepared by composite oxides and additive；The general formula of the composite oxides is xMg1.2Zn0.8SiO4‑yMg0.65Zn0.35Al2O4；Wherein, x+y=1,0.4≤x≤0.9,0.1≤y≤0.6.Compared with prior art, microwave dielectric ceramic material provided by the invention is prepared by the composite oxides and additive of specific general formula, is realized to microwave dielectric ceramic materials Mg2SiO4Be efficiently modified；The microwave dielectric ceramic material has low-k, high Q*f values and preferable sintering stability simultaneously, while can realize that temperature drift is continuously adjustable to meet various demands.The experimental results showed that the relative dielectric constant ε of microwave dielectric ceramic material provided by the inventionrIt is 7~8, quality factor q * f values >=180000GHz, temperature drift adjustable range is 10~+6ppm/ DEG C, and is sintered and stablizes, and has very outstanding application value and market potential.
Description
Technical field
The present invention relates to ceramic material technical fields, are to be related to a kind of microwave dielectric ceramic material more specifically
And preparation method thereof.
Background technology
Microwave-medium ceramics refer to being applied in microwave frequency band circuit as dielectric material and completing one or more functions
Ceramic material.It further expands to high-frequency range with the working frequency of communication equipment, after millimere-wave band, leads to
It is smaller and smaller to interrogate device size, reaches grade, thus, the critical issue of electronic component has no longer been miniaturization issues.But
It is that, with the raising of frequency, dielectric material loss significantly increases, and signal transmission delay time is longer, and problem of signal attenuation protrudes.
Both of these problems are related with dielectric constant and dielectric loss respectively.It is generally believed that signal delay time and dielectric constant at just
Than, and the quality of signal transmission then needs the high quality factor of material to ensure.The study found that permittivity εr≤ 10 material
When its quality factor is also higher, signal transmission rate and the signal quality received are significantly improved.And signal decaying with
The dielectric loss of material is directly related, and dielectric loss is bigger, and signal decaying is more severe.Therefore in order to ensure high-end microwave device
Under high frequency frequency of use obtain high speed and high quality transmission signal, need using low-k, low-dielectric loss it is micro-
Wave dielectric ceramic material.
To realize the development and application of low-k, low-dielectric-loss ceramic material, studying both at home and abroad at present more is
Magnesium silicate ceramic, magnesium silicate (Mg2SiO4) it is used as a kind of low dielectric microwave ceramic material, it is concerned in recent years.Magnesium silicate and quilt
Referred to as forsterite is a kind of nesosilicate compound collectively formed by Si-O tetrahedrons and Mg-O tetrahedrons, belongs to just
Crystallographic system is handed over, with Pmnb space groups, lattice parameter is：A=0.598nm, b=1.020nm, c=0.475nm.
It is that Ohsato et al. is studied and is found that Mg earliest2SiO4Ceramics have preferable dielectric properties, then,
Sugiyama also confirms the excellent microwave dielectric property of the ceramics under study for action：εr=6.8, Q*f=270000GHz, τf=-
70ppm/ DEG C, while having also indicated that its temperature stability is poor.In order to adjust the temperature coefficient of resonance frequency of magnesium silicate ceramic,
Ohsato et al. has studied in detail TiO2Additive amount is to ceramics τfThe influence of value, as a result, it has been found that, when additive amount is 24wt%,
The τ of gained ceramicsfIt is worth close to zero, but in sintering process, MgO-TiO2Between reaction product MgTi2O5Right
Mg2SiO4The dielectric properties of ceramics cause loss.Then, S.Q.Meng et al. passes through in Mg2SiO4Vanadic acid barium is added in ceramics
(Ba3(VO4)2) method adjust τfValue, as a result, it has been found that working as Mg2SiO4For 55wt% when, at 1175 DEG C be sintered after composite ceramics
Show preferable microwave dielectric property：εr=9.03, Q*f=52500GHz, τf=0.6ppm/ DEG C.
Although it follows that τ in the above systemfValue, which can be adjusted, is bordering on zero, but there is Q*f values and be substantially reduced or εrValue
Apparent the problem of rising, meanwhile, Mg2SiO4Ceramic post sintering stability is poor.
Invention content
In view of this, the purpose of the present invention is to provide a kind of microwave dielectric ceramic material and preparation method thereof, the present invention
The microwave dielectric ceramic material of offer has low-k, high Q*f values and preferable sintering stability, while energy simultaneously
Enough realize that temperature drift is continuously adjustable to meet various demands.
The present invention provides a kind of microwave dielectric ceramic materials, are prepared by composite oxides and additive；
The composite oxides have general formula shown in formula (I)：
xMg1.2Zn0.8SiO4-yMg0.65Zn0.35Al2O4Formula (I)；
In formula (I), x+y=1,0.4≤x≤0.9,0.1≤y≤0.6.
Preferably, the additive is in terms of the quality of composite oxides, including following components：
CaO 0.1wt%~1.5wt%；
MnO 0.1wt%~1.2wt%；
MBS sintering aids 0.1wt%~0.9wt%.
Preferably, the preparation method of the MBS sintering aids is specially：
By MgO, B2O3And SiO2After mixing, through ball milling, drying and cross the mesh of 280 mesh~320 successively and sieve, then 1450 DEG C~
0.5h~1h is melted at 1550 DEG C, finally through cold rolling, crushing and is crossed the mesh of 240 mesh~260 successively and is sieved, obtains MBS sintering aids.
Preferably, described MgO, B2O3And SiO2Mass ratio be (43~55)：(10~19)：(32~47).
The present invention also provides a kind of preparation methods of the microwave dielectric ceramic material described in above-mentioned technical proposal, including with
Lower step：
A) by MgO, ZnO and SiO2After mixing, first time milled processed is carried out, compound is obtained after calcining
Mg1.2Zn0.8SiO4；
B) by MgO, ZnO and Al2O3After mixing, second of milled processed is carried out, compound is obtained after calcining
Mg0.65Zn0.35Al2O4；
C) by above-mentioned Mg1.2Zn0.8SiO4And Mg0.65Zn0.35Al2O4It is x in molar ratio：Y is mixed, and additive is added, successively
It carries out third time milled processed, be granulated processing and compression moulding, obtain ceramic body；Wherein, x+y=1,0.4≤x≤0.9,
0.1≤y≤0.6；
D) the obtained ceramic bodies of step c) are sintered, obtain microwave dielectric ceramic material；
The step a) and step b) is limited without sequence.
Preferably, the process of first time milled processed described in step a) is specially：
The mesh sieve of 80 mesh~120 was dried after ball milling 8h~12h in pure water medium, obtains the powder after first time milled processed
Body；
The mean particle size D 50 of powder after the first time milled processed is 1.1 μm~1.3 μm.
Preferably, the temperature calcined described in step a) is 1200 DEG C~1300 DEG C, and the time is 3h~5h.
Preferably, the process of third time milled processed described in step c) is specially：
The mesh sieve of 80 mesh~120 was dried after ball milling 22h~26h in pure water medium, after obtaining third time milled processed
Powder；
The mean particle size D 50 of powder after the third time milled processed is 0.7 μm~0.9 μm.
Preferably, the process for processing being granulated described in step c) is specially：
Binder granulation is added in powder after third time milled processed, the mesh sieve of 180 mesh~220 is crushed after drying,
Powder after being granulated；
The binder is the polyvinyl alcohol water solution that mass concentration is 6%~10%；The dosage of the binder is the
1%~2% of powder quality after milled processed three times.
Preferably, the process being sintered described in step d) carries out in air atmosphere；The temperature of the sintering is 1350 DEG C
~1500 DEG C, the time is 5h~for 24 hours.
The present invention provides a kind of microwave dielectric ceramic materials, are prepared by composite oxides and additive；It is described multiple
The general formula for closing oxide is xMg1.2Zn0.8SiO4-yMg0.65Zn0.35Al2O4；Wherein, x+y=1,0.4≤x≤0.9,0.1≤y≤
0.6.Compared with prior art, microwave dielectric ceramic material provided by the invention by specific general formula composite oxides and additive
It is prepared, realizes to microwave dielectric ceramic materials Mg2SiO4Be efficiently modified；The microwave dielectric ceramic material has simultaneously
Low-k, high Q*f values and preferable sintering stability, while can realize that temperature drift is continuously adjustable to meet various need
It asks.The experimental results showed that the relative dielectric constant ε of microwave dielectric ceramic material provided by the inventionrIt is 7~8, quality factor q *
F values >=180000GHz, temperature drift adjustable range is -10~+6ppm/ DEG C, and is sintered and stablizes, and has very outstanding application value
And market potential.
In addition, preparation method sintering provided by the invention is convenient, sintering atmosphere is air atmosphere, suitable for large-scale industry
Change, there is very vast potential for future development.
Specific implementation mode
Below in conjunction with the embodiment of the present invention, technical scheme of the present invention is clearly and completely described, it is clear that institute
The embodiment of description is only a part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention,
Every other embodiment obtained by those of ordinary skill in the art without making creative efforts, belongs to this hair
The range of bright protection.
The present invention provides a kind of microwave dielectric ceramic materials, are prepared by composite oxides and additive；
The composite oxides have general formula shown in formula (I)：
xMg1.2Zn0.8SiO4-yMg0.65Zn0.35Al2O4Formula (I)；
In formula (I), x+y=1,0.4≤x≤0.9,0.1≤y≤0.6.
In the present invention, the microwave dielectric ceramic material is prepared by composite oxides and additive.In the present invention
In, the composite oxides have general formula shown in formula (I)：
xMg1.2Zn0.8SiO4-yMg0.65Zn0.35Al2O4Formula (I)；
In formula (I), x+y=1,0.4≤x≤0.9,0.1≤y≤0.6；Preferably, 0.5 ＜ x≤0.9,0.1≤y ＜
0.5.In the preferred embodiment of the invention, the x is respectively 0.9,0.84,0.76,0.65,0.58 and 0.51, corresponding y points
It Wei 0.1,0.16,0.24,0.35,0.42 and 0.49；The composite oxides obtained from are respectively：
0.9Mg1.2Zn0.8SiO4-0.1Mg0.65Zn0.35Al2O4；
0.84Mg1.2Zn0.8SiO4-0.16Mg0.65Zn0.35Al2O4；
0.76Mg1.2Zn0.8SiO4-0.24Mg0.65Zn0.35Al2O4；
0.65Mg1.2Zn0.8SiO4-0.35Mg0.65Zn0.35Al2O4；
0.58Mg1.2Zn0.8SiO4-0.42Mg0.65Zn0.35Al2O4；
0.51Mg1.2Zn0.8SiO4-0.49Mg0.65Zn0.35Al2O4。
According to hybrid system modeling, the value of x and y is adjusted, compound Mg can be controlled1.2Zn0.8SiO4With
Mg0.65Zn0.35Al2O4Molar ratio, to realize that dielectric constant is low, and small range is controllable, relative dielectric constant εrFor 7~
8。
In the present invention, the additive preferably includes following components in terms of the quality of composite oxides：
CaO 0.1wt%~1.5wt%；
MnO 0.1wt%~1.2wt%；
MBS sintering aids 0.1wt%~0.9wt%；
More preferably：
CaO 0.2wt%~1.5wt%；
MnO 0.2wt%~1.2wt%；
MBS sintering aids 0.14wt%~0.9wt%.
In the present invention, by introducing additive, temperature drift adjustable range can be controlled to a certain extent, meets different items
Use demand under part.
In the present invention, the preparation method of the MBS sintering aids is preferably specially：
By MgO, B2O3And SiO2After mixing, through ball milling, drying and cross the mesh of 280 mesh~320 successively and sieve, then 1450 DEG C~
0.5h~1h is melted at 1550 DEG C, finally through cold rolling, crushing and is crossed the mesh of 240 mesh~260 successively and is sieved, obtains MBS sintering aids；
More preferably：
By MgO, B2O3And SiO2After mixing, successively through ball milling, drying and the sieve of 300 mesh excessively, then at 1450 DEG C~1550 DEG C
0.5h~1h is melted, finally obtains MBS sintering aids through cold rolling, crushing and the sieve of 250 mesh excessively successively.
In the present invention, described MgO, B2O3And SiO2Mass ratio be preferably (43~55)：(10~19)：(32~47),
More preferably (45~55)：(10~17)：(32~45).The present invention is to described MgO, B2O3And SiO2Source there is no special limit
System, using commercial goods well known to those skilled in the art.
In the present invention, the ball milling is preferably using the technical solution of planetary ball mill well known to those skilled in the art
It can；The process of the ball milling preferably uses ethyl alcohol as ball-milling medium；The time of the ball milling is preferably for 24 hours~26h.
In the present invention, the equipment of the drying preferably uses freeze drier well known to those skilled in the art；It is described
The dry time is preferably 30h~40h, more preferably 36h.
In the present invention, by introducing MBS sintering aids, sintering temperature is advantageously reduced to a certain extent, ensures sintering
Stability.
Microwave dielectric ceramic material provided by the invention is prepared by the composite oxides and additive of specific general formula, real
Show to microwave dielectric ceramic materials Mg2SiO4Be efficiently modified；The microwave dielectric ceramic material have simultaneously low-k,
High Q*f values and preferable sintering stability, while can realize that temperature drift is continuously adjustable to meet various demands.
The present invention also provides a kind of preparation methods of the microwave dielectric ceramic material described in above-mentioned technical proposal, including with
Lower step：
A) by MgO, ZnO and SiO2After mixing, first time milled processed is carried out, compound is obtained after calcining
Mg1.2Zn0.8SiO4；
B) by MgO, ZnO and Al2O3After mixing, second of milled processed is carried out, compound is obtained after calcining
Mg0.65Zn0.35Al2O4；
C) by above-mentioned Mg1.2Zn0.8SiO4And Mg0.65Zn0.35Al2O4It is x in molar ratio：Y is mixed, and additive is added, successively
It carries out third time milled processed, be granulated processing and compression moulding, obtain ceramic body；Wherein, x+y=1,0.4≤x≤0.9,
0.1≤y≤0.6；
D) the obtained ceramic bodies of step c) are sintered, obtain microwave dielectric ceramic material；
The step a) and step b) is limited without sequence.
The present invention is first by MgO, ZnO and SiO2After mixing, first time milled processed is carried out, compound is obtained after calcining
Mg1.2Zn0.8SiO4；Meanwhile by MgO, ZnO and Al2O3After mixing, second of milled processed is carried out, compound is obtained after calcining
Mg0.65Zn0.35Al2O4.In the present invention, described MgO, ZnO and SiO2By chemical formula Mg1.2Zn0.8SiO4Stoichiometric ratio it is mixed
It closes, specially：According to weight percent 27.87%：37.51%：34.62% weighs MgO, ZnO and SiO respectively2And it mixes.
In the present invention, the process of the first time milled processed is preferably specially：
The mesh sieve of 80 mesh~120 was dried after ball milling 8h~12h in pure water medium, obtains the powder after first time milled processed
Body；
More preferably：
Drying sieves with 100 mesh sieve after ball milling 8h~12h in pure water medium, obtains the powder after first time milled processed.
In the present invention, the mean particle size D 50 of the powder after the first time milled processed is preferably 1.1 μm~1.3 μm,
Ensure that the powder has preferable dispersing uniformity.
In the present invention, the temperature of the calcining is preferably 1200 DEG C~1300 DEG C；The time of the calcining is preferably 3h
~5h.
In the present invention, described MgO, ZnO and Al2O3By chemical formula Mg0.65Zn0.35Al2O4Stoichiometric ratio mixing, tool
Body is：According to weight percent 10.13%：11.02%：78.85% weighs MgO, ZnO and Al respectively2O3And it mixes.
In the present invention, the process of second of milled processed is preferably specially：
The mesh sieve of 80 mesh~120 was dried after ball milling 10h~14h in pure water medium, after obtaining second of milled processed
Powder；
More preferably：
Drying sieves with 100 mesh sieve after ball milling 10h~14h in pure water medium, obtains the powder after second of milled processed.
In the present invention, the mean particle size D 50 of the powder after second of milled processed is preferably 0.9 μm~1.1 μm,
Ensure that the powder has preferable dispersing uniformity.
In the present invention, the temperature of the calcining is preferably 1250 DEG C~1350 DEG C；The time of the calcining is preferably 3h
~5h.
Obtain compound Mg1.2Zn0.8SiO4And compound Mg0.65Zn0.35Al2O4Afterwards, the present invention will be above-mentioned
Mg1.2Zn0.8SiO4And Mg0.65Zn0.35Al2O4It is x in molar ratio：Y is mixed, and additive is added, and is carried out at third time grinding successively
Reason is granulated processing and compression moulding, obtains ceramic body.
In the present invention, x+y=1,0.4≤x≤0.9,0.1≤y≤0.6；Preferably, 0.5 ＜ x≤0.9,0.1≤y ＜
0.5.In the preferred embodiment of the invention, the x is respectively 0.9,0.84,0.76,0.65,0.58 and 0.51, corresponding y points
It Wei 0.1,0.16,0.24,0.35,0.42 and 0.49；The composite oxides being further prepared are respectively：
0.9Mg1.2Zn0.8SiO4-0.1Mg0.65Zn0.35Al2O4；
0.84Mg1.2Zn0.8SiO4-0.16Mg0.65Zn0.35Al2O4；
0.76Mg1.2Zn0.8SiO4-0.24Mg0.65Zn0.35Al2O4；
0.65Mg1.2Zn0.8SiO4-0.35Mg0.65Zn0.35Al2O4；
0.58Mg1.2Zn0.8SiO4-0.42Mg0.65Zn0.35Al2O4；
0.51Mg1.2Zn0.8SiO4-0.49Mg0.65Zn0.35Al2O4。
According to hybrid system modeling, the value of x and y is adjusted, compound Mg can be controlled1.2Zn0.8SiO4With
Mg0.65Zn0.35Al2O4Molar ratio, to realize that dielectric constant is low, and small range is controllable, relative dielectric constant εrFor 7~
8。
In the present invention, the additive is with compound Mg1.2Zn0.8SiO4And compound Mg0.65Zn0.35Al2O4Mixing
The quality meter of powder, preferably includes following components：
CaO 0.1wt%~1.5wt%；
MnO 0.1wt%~1.2wt%；
MBS sintering aids 0.1wt%~0.9wt%；
More preferably：
CaO 0.2wt%~1.5wt%；
MnO 0.2wt%~1.2wt%；
MBS sintering aids 0.14wt%~0.9wt%.
In the present invention, by introducing additive, temperature drift adjustable range can be controlled to a certain extent, meets different items
Use demand under part.
In the present invention, the preparation method of the MBS sintering aids is preferably specially：
By MgO, B2O3And SiO2After mixing, through ball milling, drying and cross the mesh of 280 mesh~320 successively and sieve, then 1450 DEG C~
0.5h~1h is melted at 1550 DEG C, finally through cold rolling, crushing and is crossed the mesh of 240 mesh~260 successively and is sieved, obtains MBS sintering aids；
More preferably：
By MgO, B2O3And SiO2After mixing, successively through ball milling, drying and the sieve of 300 mesh excessively, then at 1450 DEG C~1550 DEG C
0.5h~1h is melted, finally obtains MBS sintering aids through cold rolling, crushing and the sieve of 250 mesh excessively successively.
In the present invention, described MgO, B2O3And SiO2Mass ratio be preferably (43~55)：(10~19)：(32~47),
More preferably (45~55)：(10~17)：(32~45).The present invention is to described MgO, B2O3And SiO2Source there is no special limit
System, using commercial goods well known to those skilled in the art.
In the present invention, the ball milling is preferably using the technical solution of planetary ball mill well known to those skilled in the art
It can；The process of the ball milling preferably uses ethyl alcohol as ball-milling medium；The time of the ball milling is preferably for 24 hours~26h.
In the present invention, the equipment of the drying preferably uses freeze drier well known to those skilled in the art；It is described
The dry time is preferably 30h~40h, more preferably 36h.
In the present invention, by introducing MBS sintering aids, sintering temperature is advantageously reduced to a certain extent, ensures sintering
Stability.
In the present invention, the process of the third time milled processed is preferably specially：
The mesh sieve of 80 mesh~120 was dried after ball milling 22h~26h in pure water medium, after obtaining third time milled processed
Powder；
More preferably：
Drying sieves with 100 mesh sieve after ball milling 22h~26h in pure water medium, obtains the powder after third time milled processed.
In the present invention, the mean particle size D 50 of the powder after the third time milled processed is preferably 0.7 μm~0.9 μm,
Ensure that the powder has preferable dispersing uniformity.
In the present invention, the process for being granulated processing is preferably specially：
Binder granulation is added in powder after third time milled processed, the mesh sieve of 180 mesh~220 is crushed after drying,
Powder after being granulated；
More preferably：
Binder granulation is added in powder after third time milled processed, 200 mesh sieve is crushed after drying, is granulated
Powder afterwards.
In the present invention, the binder is preferably the polyvinyl alcohol water solution that mass concentration is 6%~10%, more preferably
The polyvinyl alcohol water solution for being 8% for mass concentration.The present invention is not particularly limited the source of the binder, using ability
Commercial goods known to field technique personnel.
In the present invention, the dosage of the binder be preferably the powder quality after third time milled processed 1%~
2%, more preferably 1.5% of the powder quality after third time milled processed.
In the present invention, the pressure of the compression moulding is preferably 30MPa~40MPa.The present invention is to the compression moulding
Equipment be not particularly limited, using the equipment well known to those skilled in the art for compression moulding ceramic body.
After obtaining the ceramic body, obtained ceramic body is sintered by the present invention, obtains microwave dielectric ceramic material
Material.In the present invention, the process of the sintering carries out preferably in air atmosphere.In the present invention, the temperature of the sintering is excellent
It is selected as 1350 DEG C~1500 DEG C；The time of the sintering is preferably 5h~for 24 hours, and more preferably 16h~for 24 hours.
The present invention provides a kind of microwave dielectric ceramic materials, are prepared by composite oxides and additive；It is described multiple
The general formula for closing oxide is xMg1.2Zn0.8SiO4-yMg0.65Zn0.35Al2O4；Wherein, x+y=1,0.4≤x≤0.9,0.1≤y≤
0.6.Compared with prior art, microwave dielectric ceramic material provided by the invention by specific general formula composite oxides and additive
It is prepared, realizes to microwave dielectric ceramic materials Mg2SiO4Be efficiently modified；The microwave dielectric ceramic material has simultaneously
Low-k, high Q*f values and preferable sintering stability, while can realize that temperature drift is continuously adjustable to meet various need
It asks.The experimental results showed that the relative dielectric constant ε of microwave dielectric ceramic material provided by the inventionrIt is 7~8, quality factor q *
F values >=180000GHz, temperature drift adjustable range is -10~+6ppm/ DEG C, and is sintered and stablizes, and has very outstanding application value
And market potential.
In addition, preparation method sintering provided by the invention is convenient, sintering atmosphere is air atmosphere, suitable for large-scale industry
Change, there is very vast potential for future development.
In order to further illustrate the present invention, it is described in detail below by following embodiment.Following embodiment of the present invention
Used in pharmaceutical raw material be commercial goods.
Embodiment 1
(1) according to weight percent 27.87%：37.51%：34.62% weighs MgO, ZnO and SiO respectively2And mix,
Pure water is added and is used as ball-milling medium, after ball milling 10h drying sieve with 100 mesh sieve net, at 1200 DEG C, calcining 4h, obtains compound A：
Mg1.2Zn0.8SiO4；
According to weight percent 10.13%：11.02%：78.85% weighs MgO, ZnO and Al respectively2O3And mix, it is added
Pure water as ball-milling medium, after ball milling 12h drying sieve with 100 mesh sieve net, 3h is calcined at 1300 DEG C, obtains compound B：
Mg0.65Zn0.35Al2O4；
According to mass percent 55%：13%：32% weighs MgO, B respectively2O3And SiO2And mix, ethyl alcohol conduct is added
Ball-milling medium, planetary ball mill for 24 hours after, be put into freeze drier drying 36h after cross 300 mesh screens, place into silica crucible and exist
After 1500 DEG C of melting 0.5h, rapid cold-rolling mill of crossing obtains tablet, and above-mentioned tablet was then ground 250 mesh screens,
Obtain MBS sintering aids.
(2) above compound A and compound B is pressed into x：Y=90：10 molar ratio mixing, obtains mixed powder；Then
Additive is added, and (additive is made of CaO, MnO and above-mentioned MBS sintering aids, the matter of the relatively above-mentioned mixed powder weight of each component
Measuring percentage is respectively：CaO is 0.2wt%,
MnO is 0.3wt%, and MBS sintering aids are 0.9wt%), drying sieves with 100 mesh sieve after ball milling 22h in pure water medium
Net, the binder (the PVA aqueous solutions that mass concentration is 8%) that powder gross mass 1.5% is then added are granulated, grounds travel after drying
200 mesh of broken mistake sieves, then the compression moulding under 30MPa pressure, obtains ceramic green.
(3) above-mentioned ceramic green in air atmosphere is warming up to 1350 DEG C, keeps the temperature 16h, obtains microwave dielectric ceramic.
The dielectricity for the microwave dielectric ceramic that embodiment 1 provides is measured using closed resonator method combination Network Analyzer
Can, relative dielectric constant is calculated according to Hakki-Coleman principles, and temperature drift test temperature is 25-85 DEG C；The microwave dielectric ceramic
Relative dielectric constant be 7.1, Q*f values be 280000GHz, temperature drift is -9.3ppm/ DEG C.
Embodiment 2
(1) according to weight percent 27.87%：37.51%：34.62% weighs MgO, ZnO and SiO respectively2And mix,
Pure water is added and is used as ball-milling medium, after ball milling 9h drying sieve with 100 mesh sieve net, at 1250 DEG C, calcining 3h, obtains compound A：
Mg1.2Zn0.8SiO4；
According to weight percent 10.13%：11.02%：78.85% weighs MgO, ZnO and Al respectively2O3And mix, it is added
Pure water as ball-milling medium, after ball milling 12h drying sieve with 100 mesh sieve net, 3h is calcined at 1300 DEG C, obtains compound B：
Mg0.65Zn0.35Al2O4；
According to mass percent 55%：13%：32% weighs MgO, B respectively2O3And SiO2And mix, ethyl alcohol conduct is added
Ball-milling medium, planetary ball mill for 24 hours after, be put into freeze drier drying 36h after cross 300 mesh screens, place into silica crucible and exist
After 1500 DEG C of melting 0.5h, rapid cold-rolling mill of crossing obtains tablet, and above-mentioned tablet was then ground 250 mesh screens,
Obtain MBS sintering aids.
(2) above compound A and compound B is pressed into x：Y=84：16 molar ratio mixing, obtains mixed powder；Then
Additive is added, and (additive is made of CaO, MnO and above-mentioned MBS sintering aids, the matter of the relatively above-mentioned mixed powder weight of each component
Measuring percentage is respectively：CaO is 0.3wt%, and MnO 0.5wt%, MBS sintering aids are 0.75wt%), the ball in pure water medium
Drying sieves with 100 mesh sieve net after mill 22h, and then (PVA that mass concentration is 8% is water-soluble for the binder of addition powder gross mass 1.5%
Liquid) it is granulated, 200 mesh sieve, then the compression moulding under 30MPa pressure were ground after drying, obtained ceramic green.
(3) above-mentioned ceramic green in air atmosphere is warming up to 1400 DEG C, keeps the temperature 16h, obtains microwave dielectric ceramic.
The dielectricity for the microwave dielectric ceramic that embodiment 2 provides is measured using closed resonator method combination Network Analyzer
Can, relative dielectric constant is calculated according to Hakki-Coleman principles, and temperature drift test temperature is 25-85 DEG C；The microwave dielectric ceramic
Relative dielectric constant be 7.3, Q*f values be 250000GHz, temperature drift is -6.5ppm/ DEG C.
Embodiment 3
(1) according to weight percent 27.87%：37.51%：34.62% weighs MgO, ZnO and SiO respectively2And mix,
Pure water is added and is used as ball-milling medium, after ball milling 10h drying sieve with 100 mesh sieve net, at 1300 DEG C, calcining 4h, obtains compound A：
Mg1.2Zn0.8SiO4；
According to weight percent 10.13%：11.02%：78.85% weighs MgO, ZnO and Al respectively2O3And mix, it is added
Pure water as ball-milling medium, after ball milling 10h drying sieve with 100 mesh sieve net, 4h is calcined at 1350 DEG C, obtains compound B：
Mg0.65Zn0.35Al2O4；
According to mass percent 50%：17%：33% weighs MgO, B respectively2O3And SiO2And mix, ethyl alcohol conduct is added
Ball-milling medium, planetary ball mill for 24 hours after, be put into freeze drier drying 36h after cross 300 mesh screens, place into silica crucible and exist
After 1450 DEG C of melting 1h, rapid cold-rolling mill of crossing obtains tablet, and above-mentioned tablet was then ground 250 mesh screens, is obtained
To MBS sintering aids.
(2) above compound A and compound B is pressed into x：Y=76：24 molar ratio mixing, obtains mixed powder；Then
Additive is added, and (additive is made of CaO, MnO and above-mentioned MBS sintering aids, the matter of the relatively above-mentioned mixed powder weight of each component
Measuring percentage is respectively：CaO is 0.8wt%, and MnO 0.2wt%, MBS sintering aids are 0.7wt%), the ball milling in pure water medium
Drying sieves with 100 mesh sieve net afterwards for 24 hours, and then (PVA that mass concentration is 8% is water-soluble for the binder of addition powder gross mass 1.5%
Liquid) it is granulated, 200 mesh sieve, then the compression moulding under 30MPa pressure were ground after drying, obtained ceramic green.
(3) above-mentioned ceramic green in air atmosphere is warming up to 1500 DEG C, keeps the temperature 18h, obtains microwave dielectric ceramic.
The dielectricity for the microwave dielectric ceramic that embodiment 3 provides is measured using closed resonator method combination Network Analyzer
Can, relative dielectric constant is calculated according to Hakki-Coleman principles, and temperature drift test temperature is 25-85 DEG C；The microwave dielectric ceramic
Relative dielectric constant be 7.4, Q*f values be 270000GHz, temperature drift is -4.3ppm/ DEG C.
Embodiment 4
(1) according to weight percent 27.87%：37.51%：34.62% weighs MgO, ZnO and SiO respectively2And mix,
Pure water is added and is used as ball-milling medium, after ball milling 8h drying sieve with 100 mesh sieve net, at 1250 DEG C, calcining 3h, obtains compound A：
Mg1.2Zn0.8SiO4；
According to weight percent 10.13%：11.02%：78.85% weighs MgO, ZnO and Al respectively2O3And mix, it is added
Pure water as ball-milling medium, after ball milling 14h drying sieve with 100 mesh sieve net, 3h is calcined at 1250 DEG C, obtains compound B：
Mg0.65Zn0.35Al2O4；
According to mass percent 45%：10%：45% weighs MgO, B respectively2O3And SiO2And mix, ethyl alcohol conduct is added
Ball-milling medium, planetary ball mill for 24 hours after, be put into freeze drier drying 36h after cross 300 mesh screens, place into silica crucible and exist
After 1550 DEG C of melting 0.5h, rapid cold-rolling mill of crossing obtains tablet, and above-mentioned tablet was then ground 250 mesh screens,
Obtain MBS sintering aids.
(2) above compound A and compound B is pressed into x：Y=65：35 molar ratio mixing, obtains mixed powder；Then
Additive is added, and (additive is made of CaO, MnO and above-mentioned MBS sintering aids, the matter of the relatively above-mentioned mixed powder weight of each component
Measuring percentage is respectively：CaO is 1.2wt%, and MnO 1.2wt%, MBS sintering aids are 0.34wt%), the ball in pure water medium
Drying sieves with 100 mesh sieve net to mill afterwards for 24 hours, and then (PVA that mass concentration is 8% is water-soluble for the binder of addition powder gross mass 1.5%
Liquid) it is granulated, 200 mesh sieve, then the compression moulding under 30MPa pressure were ground after drying, obtained ceramic green.
(3) above-mentioned ceramic green in air atmosphere is warming up to 1500 DEG C, keeps the temperature 20h, obtains microwave dielectric ceramic.
The dielectricity for the microwave dielectric ceramic that embodiment 4 provides is measured using closed resonator method combination Network Analyzer
Can, relative dielectric constant is calculated according to Hakki-Coleman principles, and temperature drift test temperature is 25-85 DEG C；The microwave dielectric ceramic
Relative dielectric constant be 7.7, Q*f values be 190000GHz, temperature drift is 5.6ppm/ DEG C.
Embodiment 5
(1) according to weight percent 27.87%：37.51%：34.62% weighs MgO, ZnO and SiO respectively2And mix,
Pure water is added and is used as ball-milling medium, after ball milling 12h drying sieve with 100 mesh sieve net, at 1200 DEG C, calcining 3h, obtains compound A：
Mg1.2Zn0.8SiO4；
According to weight percent 10.13%：11.02%：78.85% weighs MgO, ZnO and Al respectively2O3And mix, it is added
Pure water as ball-milling medium, after ball milling 13h drying sieve with 100 mesh sieve net, 3h is calcined at 1250 DEG C, obtains compound B：
Mg0.65Zn0.35Al2O4；
According to mass percent 45%：10%：45% weighs MgO, B respectively2O3And SiO2And mix, ethyl alcohol conduct is added
Ball-milling medium, planetary ball mill for 24 hours after, be put into freeze drier drying 36h after cross 300 mesh screens, place into silica crucible and exist
After 1550 DEG C of melting 0.8h, rapid cold-rolling mill of crossing obtains tablet, and above-mentioned tablet was then ground 250 mesh screens,
Obtain MBS sintering aids.
(2) above compound A and compound B is pressed into x：Y=58：42 molar ratio mixing, obtains mixed powder；Then
Additive is added, and (additive is made of CaO, MnO and above-mentioned MBS sintering aids, the matter of the relatively above-mentioned mixed powder weight of each component
Measuring percentage is respectively：CaO is 0.3wt%, and MnO 0.6wt%, MBS sintering aids are 0.28wt%), the ball in pure water medium
Drying sieves with 100 mesh sieve net after mill 22h, and then (PVA that mass concentration is 8% is water-soluble for the binder of addition powder gross mass 1.5%
Liquid) it is granulated, 200 mesh sieve, then the compression moulding under 40MPa pressure were ground after drying, obtained ceramic green.
(3) above-mentioned ceramic green is warming up to 1500 DEG C in air atmosphere, heat preservation for 24 hours, obtains microwave dielectric ceramic.
The dielectricity for the microwave dielectric ceramic that embodiment 5 provides is measured using closed resonator method combination Network Analyzer
Can, relative dielectric constant is calculated according to Hakki-Coleman principles, and temperature drift test temperature is 25-85 DEG C；The microwave dielectric ceramic
Relative dielectric constant be 7.8, Q*f values be 230000GHz, temperature drift is -2.6ppm/ DEG C.
Embodiment 6
(1) according to weight percent 27.87%：37.51%：34.62% weighs MgO, ZnO and SiO respectively2And mix,
Pure water is added and is used as ball-milling medium, after ball milling 10h drying sieve with 100 mesh sieve net, at 1250 DEG C, calcining 3h, obtains compound A：
Mg1.2Zn0.8SiO4；
According to weight percent 10.13%：11.02%：78.85% weighs MgO, ZnO and Al respectively2O3And mix, it is added
Pure water as ball-milling medium, after ball milling 12h drying sieve with 100 mesh sieve net, 3h is calcined at 1250 DEG C, obtains compound B：
Mg0.65Zn0.35Al2O4；
According to mass percent 55%：13%：32% weighs MgO, B respectively2O3And SiO2And mix, ethyl alcohol conduct is added
Ball-milling medium after planetary ball mill 26h, crosses 300 mesh screens after being put into freeze drier drying 36h, places into silica crucible and exist
After 1550 DEG C of melting 1h, rapid cold-rolling mill of crossing obtains tablet, and above-mentioned tablet was then ground 250 mesh screens, is obtained
To MBS sintering aids.
(2) above compound A and compound B is pressed into x：Y=51：49 molar ratio mixing, obtains mixed powder；Then
Additive is added, and (additive is made of CaO, MnO and above-mentioned MBS sintering aids, the matter of the relatively above-mentioned mixed powder weight of each component
Measuring percentage is respectively：CaO is 1.5wt%, and MnO 0.4wt%, MBS sintering aids are 0.14wt%), the ball in pure water medium
Drying sieves with 100 mesh sieve net after mill 22h, and then (PVA that mass concentration is 8% is water-soluble for the binder of addition powder gross mass 1.5%
Liquid) it is granulated, 200 mesh sieve, then the compression moulding under 40MPa pressure were ground after drying, obtained ceramic green.
(3) above-mentioned ceramic green is warming up to 1500 DEG C in air atmosphere, heat preservation for 24 hours, obtains microwave dielectric ceramic.
The dielectricity for the microwave dielectric ceramic that embodiment 6 provides is measured using closed resonator method combination Network Analyzer
Can, relative dielectric constant is calculated according to Hakki-Coleman principles, and temperature drift test temperature is 25-85 DEG C；The microwave dielectric ceramic
Relative dielectric constant be 7.9, Q*f values be 210000GHz, temperature drift is 3.4ppm/ DEG C.
In conclusion the relative dielectric constant ε for the microwave dielectric ceramic that the embodiment of the present invention 1~6 providesrIt is 7~8, product
Prime factor Q*f values >=180000GHz, temperature drift adjustable range is -10~+6ppm/ DEG C, and is sintered and stablizes, and is had very outstanding
Application value and market potential.
The above description of the disclosed embodiments, enables those skilled in the art to implement or use the present invention.It is right
A variety of modifications of these embodiments will be apparent to those skilled in the art, and as defined herein one
As principle can realize in other embodiments without departing from the spirit or scope of the present invention.Therefore, the present invention will
It will not be intended to be limited to the embodiments shown herein, and be to fit to consistent with the principles and novel features disclosed herein
Widest range.
Claims (10)
1. a kind of microwave dielectric ceramic material, is prepared by composite oxides and additive；
The composite oxides have general formula shown in formula (I)：
xMg1.2Zn0.8SiO4-yMg0.65Zn0.35Al2O4Formula (I)；
In formula (I), x+y=1,0.4≤x≤0.9,0.1≤y≤0.6.
2. microwave dielectric ceramic material according to claim 1, which is characterized in that the additive is with composite oxides
Quality meter, including following components：
CaO 0.1wt%~1.5wt%；
MnO 0.1wt%~1.2wt%；
MBS sintering aids 0.1wt%~0.9wt%.
3. microwave dielectric ceramic material according to claim 2, which is characterized in that the preparation method of the MBS sintering aids
Specially：
By MgO, B2O3And SiO2After mixing, through ball milling, drying and crosses the mesh of 280 mesh~320 successively and sieve, then 1450 DEG C~1550
0.5h~1h is melted at DEG C, finally through cold rolling, crushing and is crossed the mesh of 240 mesh~260 successively and is sieved, obtains MBS sintering aids.
4. microwave dielectric ceramic material according to claim 3, which is characterized in that described MgO, B2O3And SiO2Quality
Than for (43~55)：(10~19)：(32~47).
5. a kind of preparation method of Claims 1 to 4 any one of them microwave dielectric ceramic material, includes the following steps：
A) by MgO, ZnO and SiO2After mixing, first time milled processed is carried out, compound Mg is obtained after calcining1.2Zn0.8SiO4；
B) by MgO, ZnO and Al2O3After mixing, second of milled processed is carried out, compound is obtained after calcining
Mg0.65Zn0.35Al2O4；
C) by above-mentioned Mg1.2Zn0.8SiO4And Mg0.65Zn0.35Al2O4It is x in molar ratio：Y is mixed, and additive is added, carries out successively
Third time milled processed is granulated processing and compression moulding, obtains ceramic body；Wherein, x+y=1,0.4≤x≤0.9,0.1≤y
≤0.6；
D) the obtained ceramic bodies of step c) are sintered, obtain microwave dielectric ceramic material；
The step a) and step b) is limited without sequence.
6. preparation method according to claim 5, which is characterized in that the process of first time milled processed described in step a)
Specially：
The mesh sieve of 80 mesh~120 was dried after ball milling 8h~12h in pure water medium, obtains the powder after first time milled processed；
The mean particle size D 50 of powder after the first time milled processed is 1.1 μm~1.3 μm.
7. preparation method according to claim 5, which is characterized in that the temperature calcined described in step a) be 1200 DEG C~
1300 DEG C, the time is 3h~5h.
8. preparation method according to claim 5, which is characterized in that the process of third time milled processed described in step c)
Specially：
The mesh sieve of 80 mesh~120 was dried after ball milling 22h~26h in pure water medium, obtains the powder after third time milled processed；
The mean particle size D 50 of powder after the third time milled processed is 0.7 μm~0.9 μm.
9. preparation method according to claim 5, which is characterized in that the process for being granulated processing described in step c) is specific
For：
Binder granulation is added in powder after third time milled processed, the mesh sieve of 180 mesh~220 is crushed after drying, is obtained
Powder after granulation；
The binder is the polyvinyl alcohol water solution that mass concentration is 6%~10%；The dosage of the binder is third time
1%~2% of powder quality after milled processed.
10. preparation method according to claim 5, which is characterized in that the process being sintered described in step d) is in air gas
It is carried out in atmosphere；The temperature of the sintering is 1350 DEG C~1500 DEG C, and the time is 5h~for 24 hours.
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