CN109734439A - A kind of medium dielectric constant microwave medium composite microwave medium ceramic material and preparation method thereof - Google Patents
A kind of medium dielectric constant microwave medium composite microwave medium ceramic material and preparation method thereof Download PDFInfo
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Abstract
The present invention relates to materials science fields, it is desirable to provide a kind of medium dielectric constant microwave medium composite microwave medium ceramic material.The chemical expression of the microwave dielectric ceramic materials is (1-x) Li2Ti0.75(Mg1/ 3Nb2/3)0.25O3+x BaTi4O9+ ywt%M；Wherein, 0.4≤x≤0.6, y are to account for Li2Ti0.75(Mg1/3Nb2/3)0.25O3And BaTi4O9The mass fraction of gross mass, 0.5≤y≤2, M are auxiliary agent, are LiF, MnCO3, CuO or GeO2One or more of mixing.Material dielectric constant of the invention is higher in 30 or so, Q × f value, and temperature coefficient of resonance frequency is small；It is able to satisfy demand of the microwave devices such as resonator, filter, GPS antenna to 30 or so microwave dielectric ceramic materials of dielectric constant.Preparation process of the present invention is simple, reproducible.
Description
Technical field
The invention belongs to materials science fields, and in particular to a kind of medium dielectric constant microwave medium composite microwave medium ceramic material and its
Preparation method.
Background technique
Microwave-medium ceramics are a kind of applied to microwave frequency band (300MHz~300GHz), and medium is played in circuit system
A series of ceramics of circuit functions such as isolation, Medium Wave Guide and dielectric resonance.With microwave dielectric ceramic materials preparation resonator,
The microwave devices such as filter, diectric antenna have become the core component of communication equipment.In recent years, with 4G/5G mobile communication, defend
The fast development of the technologies such as star communication, wireless network, GPS, bluetooth, microwave device is just towards miniaturization, height
Frequencyization and lightweight direction are developed, and to microwave dielectric ceramic materials, more stringent requirements are proposed: dielectric constant seriation, to meet
The demand of different communication frequency range device；The higher the better for Q × f value, to reduce the loss of microwave device；Frequency-temperature coefficient to the greatest extent may be used
Can be small, to reduce the influence of variation of the microwave device performance with external environment.
Currently, the microwave dielectric ceramic materials of existing seriation are developed in succession, however dielectric constant is in 25~35 intermediary
Electric constant microwave dielectric ceramic materials system is less, and the microwave devices such as resonator, filter are to the range dielectric constant
Microwave dielectric ceramic materials have strong demand.Ba(Zn,Ta)O3Ceramics have excellent microwave dielectric property: its dielectric constant
About 29, quality factor q × f are about 70000GHz, and frequency-temperature coefficient is close to zero, but Ta is expensive, the material manufacturing cost
It is high.Li L X etc. is in " Ceramics International " 9157-9161 pages of volume 7 " Crystal delivered of volume 42 in 2016
structure and microwave dielectric properties of the low dielectric loss
ZnZr1-xSnxNb2O8ZnZr is reported in a ceramics " text0.8Sn0.2Nb2O8The microwave dielectric property that ceramics are sintered at 1275 DEG C
Can: its permittivity εrIt is 27.37, quality factor q × f value is 76814GHz, but the frequency-temperature coefficient of the ceramics is very
Greatly, reach -55.09ppm/ DEG C.
Summary of the invention
The technical problem to be solved by the present invention is to overcome deficiency in the prior art, it is compound to provide a kind of medium dielectric constant microwave medium
Microwave dielectric ceramic materials and preparation method thereof.
In order to solve the technical problem, solution of the invention is:
A kind of medium dielectric constant microwave medium composite microwave medium ceramic material, the chemical expression of the microwave dielectric ceramic materials are provided
For (1-x) Li2Ti0.75(Mg1/3Nb2/3)0.25O3+x BaTi4O9+ ywt%M；Wherein, 0.4≤x≤0.6, y are that auxiliary agent M is accounted for
Li2Ti0.75(Mg1/3Nb2/3)0.25O3And BaTi4O9The mass fraction of gross mass, 0.5≤y≤2, M are auxiliary agent, are LiF, MnCO3、
CuO or GeO2One or more of mixing.
Invention further provides the preparation methods of the microwave dielectric ceramic materials, include the following steps:
(1) Li is pressed2Ti0.75(Mg1/3Nb2/3)0.25O3The molar ratio of each metallic element weighs raw material Li in chemical formula2CO3、
TiO2, MgO and Nb2O5, using wet ball grinding mixing 4h；After mixture is dried under the conditions of 880~920 DEG C 2~4h of pre-burning,
Li is made through ball milling again2Ti0.75(Mg1/3Nb2/3)0.25O3Powder；
(2) BaTi is pressed4O9The molar ratio of each metallic element weighs raw material BaCO in chemical formula3And TiO2, using wet process ball
Grind mixing 4h；After mixture is dried under the conditions of 1050~1100 DEG C 2~4h of pre-burning, then BaTi is made through ball milling4O9Powder；
(3) LiF, MnCO are taken3, CuO or GeO2One or more of mixing be used as auxiliary agent, with Li2Ti0.75(Mg1/ 3Nb2/3)0.25O3And BaTi4O9Ball milling mixing 2h is carried out, is then dried, mixed powder is made；Wherein, Li2Ti0.75(Mg1/ 3Nb2/3)0.25O3With BaTi4O9Molar ratio is (1-x): x, and auxiliary agent accounts for Li2Ti0.75(Mg1/3Nb2/3)0.25O3And BaTi4O9Gross mass
0.5~2wt%；
(4) polyvinyl alcohol water solution, the mass fraction of polyvinyl alcohol water solution are taken by 5~8wt% of mixed powder quality
It is 5%；After mixing by mixed powder and polyvinyl alcohol water solution, it is suppressed under 100MPa pressure, prepares cylinder
Shape green body；
(5) green body is obtained into medium dielectric constant microwave medium composite microwave medium ceramic material in 1200~1280 DEG C of heat preservation sintering 4h
Material.
In the present invention, the pre-burning in the step (1) and step (2) is carried out in crucible.
In the present invention, in the step (4), diameter 10mm, the thickness 5mm of cylindric green body.
Inventive principle description:
Li2Ti0.75(Mg1/3Nb2/3)0.25O3With BaTiO3, it can be achieved that dielectric constant is adjusted, LiF and CuO are helped Ceramic Composite
Agent has low fusing point, can reduce the sintering temperature of composite microwave medium ceramic；MnCO3And GeO2Addition, can increase compound
Q × f value of ceramic systems.The medium dielectric constant microwave medium composite microwave medium ceramic that the present invention obtains, dielectric constant 26~32, Q × f
It is -10 < τ for 48000~86500GHz, temperature coefficient of resonance frequencyf+ 10ppm/ DEG C of <, it is able to satisfy resonator, filter etc.
The demand of microwave dielectric ceramic materials near microwave device centering dielectric constant especially dielectric constant 30.
Compared with prior art, beneficial effects of the present invention:
1, material dielectric constant of the present invention is higher in 30 or so, Q × f value, and temperature coefficient of resonance frequency is small；It is able to satisfy resonance
Demand of the microwave devices such as device, filter, GPS antenna to 30 or so microwave dielectric ceramic materials of dielectric constant.
2, preparation process of the present invention is simple, reproducible.
Specific embodiment
Embodiment below can make the technical staff of this professional skill field more fully understand the present invention, but not to appoint
Where formula limitation is of the invention:
Embodiment 1:
The preparation method of the medium dielectric constant microwave medium composite microwave medium ceramic material of the present embodiment, in accordance with the following steps:
Step (1): Li is pressed2Ti0.75(Mg1/3Nb2/3)0.25O3Chemical formula weighs raw material Li2CO3,TiO2, MgO and Nb2O5, adopt
It with wet ball grinding mixing 4h, is fitted into crucible after mixture is dried, in 880 DEG C of pre-burning 4h, then Li is made in ball milling2Ti0.75
(Mg1/3Nb2/3)0.25O3Powder；
Step (2): BaTi is pressed4O9Chemical formula weighs raw material BaCO3And TiO2, ball mill mixing 4h is carried out, using wet ball grinding
Mixing 4h is fitted into crucible after drying mixture, and in 1050 DEG C of pre-burning 4h, then BaTi is made in ball milling4O9Powder；
Step (3): Li is made in step (1)2Ti0.75(Mg1/3Nb2/3)0.25O3, step (2) be made BaTi4O9It is mixed with LiF
It closes, wherein Li2Ti0.75(Mg1/3Nb2/3)0.25O3With BaTi4O9Molar ratio is 0.6:0.4, and LiF accounts for Li2Ti0.75(Mg1/ 3Nb2/3)0.25O3And BaTi4O9The 0.5wt% of gross mass carries out dry, obtained mixed powder after ball milling mixing 2h；
Step (4): it is 5% polyvinyl alcohol water that mixed powder, which is made, with the mass fraction for accounting for its quality 5wt% in step (3)
It is uniformly mixed in solution, and is suppressed under 100MPa pressure, prepare the cylindric green body of diameter 10mm, thickness 5mm；
Step (5): by green body made from step (4) in 1250 DEG C of heat preservation sintering 4h, the medium dielectric constant microwave medium is obtained
Microwave dielectric ceramic materials.
It is according to medium dielectric constant microwave medium composite microwave medium ceramic material, chemical expression made from aforementioned formula and step
(1-x)Li2Ti0.75(Mg1/3Nb2/3)0.25O3+xBaTi4O9+ ywt%M,
Wherein x=0.4, y are that auxiliary agent M accounts for Li2Ti0.75(Mg1/3Nb2/3)0.25O3And BaTi4O9The mass fraction of gross mass, y
=0.5, M LiF.
Performance indexes are as follows: 1250 DEG C of sintering temperature, permittivity εr=27.6, quality factor q × f=
78000GHz, frequency-temperature coefficient τf=+2ppm/ DEG C.
Embodiment 2:
The preparation method of the medium dielectric constant microwave medium composite microwave medium ceramic material of the present embodiment, in accordance with the following steps:
Step (1): Li is pressed2Ti0.75(Mg1/3Nb2/3)0.25O3Chemical formula weighs raw material Li2CO3,TiO2, MgO and Nb2O5,
Using wet ball grinding mixing 4h, it is fitted into crucible after mixture is dried, in 900 DEG C of pre-burning 3h, then ball milling system
Obtain Li2Ti0.75(Mg1/3Nb2/3)0.25O3Powder；
Step (2): BaTi is pressed4O9Chemical formula weighs raw material BaCO3And TiO2, using wet ball grinding mixing 4h, by mixture
It is fitted into crucible after drying, in 1100 DEG C of pre-burning 2h, then BaTi is made in ball milling4O9Powder；
Step (3): Li is made in step (1)2Ti0.75(Mg1/3Nb2/3)0.25O3, step (2) be made BaTi4O9It is mixed with LiF
It closes, wherein Li2Ti0.75(Mg1/3Nb2/3)0.25O3With BaTi4O9Molar ratio is 0.4:0.6, and LiF accounts for Li2Ti0.75(Mg1/ 3Nb2/3)0.25O3And BaTi4O9The 2wt% of gross mass carries out dry, obtained mixed powder after ball milling mixing 2h；
Step (4): it is 5% polyvinyl alcohol water that mixed powder, which is made, with the mass fraction for accounting for its quality 7wt% in step (3)
It is uniformly mixed in solution, and is suppressed under 100MPa pressure, prepare the cylindric green body of diameter 10mm, thickness 5mm；
Step (5): by green body made from step (4) in 1200 DEG C of heat preservation sintering 4h, the medium dielectric constant microwave medium is obtained
Microwave dielectric ceramic materials.
It is according to medium dielectric constant microwave medium composite microwave medium ceramic material, chemical expression made from aforementioned formula and step
(1-x)Li2Ti0.75(Mg1/3Nb2/3)0.25O3+xBaTi4O9+ ywt%M,
Wherein x=0.6, y are that auxiliary agent M accounts for Li2Ti0.75(Mg1/3Nb2/3)0.25O3And BaTi4O9The mass fraction of gross mass, y
=2, M LiF.
Performance indexes are as follows: 1200 DEG C of sintering temperature, permittivity εr=31.2, quality factor q × f=
59000GHz, frequency-temperature coefficient τf=+8ppm/ DEG C.
Embodiment 3:
The preparation method of the medium dielectric constant microwave medium composite microwave medium ceramic material of the present embodiment, in accordance with the following steps:
Step (1): Li is pressed2Ti0.75(Mg1/3Nb2/3)0.25O3Chemical formula weighs raw material Li2CO3,TiO2, MgO and Nb2O5, adopt
It with wet ball grinding mixing 4h, is fitted into crucible after mixture is dried, in 920 DEG C of pre-burning 2h, then Li is made in ball milling2Ti0.75
(Mg1/3Nb2/3)0.25O3Powder；
Step (2): BaTi is pressed4O9Chemical formula weighs raw material BaCO3And TiO2, using wet ball grinding mixing 4h, by mixture
It is fitted into crucible after drying, in 1080 DEG C of pre-burning 3h, then BaTi is made in ball milling4O9Powder；
Step (3): Li is made in step (1)2Ti0.75(Mg1/3Nb2/3)0.25O3, step (2) be made BaTi4O9With LiF and
CuO is mixed, wherein Li2Ti0.75(Mg1/3Nb2/3)0.25O3With BaTi4O9Molar ratio is that 0.5:0.5, LiF and CuO are accounted for respectively
Li2Ti0.75(Mg1/3Nb2/3)0.25O3And BaTi4O9The 1.2wt% and 0.8wt% of gross mass carry out drying after ball milling mixing 2h,
Mixed powder is made；
Step (4): it is 5% polyvinyl alcohol water that mixed powder, which is made, with the mass fraction for accounting for its quality 8wt% in step (3)
It is uniformly mixed in solution, and is suppressed under 100MPa pressure, prepare the cylindric green body of diameter 10mm, thickness 5mm；
Step (5): by green body made from step (4) in 1200 DEG C of heat preservation sintering 4h, the medium dielectric constant microwave medium is obtained
Microwave dielectric ceramic materials.
It is according to medium dielectric constant microwave medium composite microwave medium ceramic material, chemical expression made from aforementioned formula and step
(1-x)Li2Ti0.75(Mg1/3Nb2/3)0.25O3+xBaTi4O9+ ywt%M,
Wherein x=0.5, y are that auxiliary agent M accounts for Li2Ti0.75(Mg1/3Nb2/3)0.25O3And BaTi4O9The mass fraction of gross mass, y
=2, M are LiF and CuO.
Performance indexes are as follows: 1200 DEG C of sintering temperature, permittivity εr=29.3, quality factor q × f=
61000GHz, frequency-temperature coefficient τf=+6ppm/ DEG C.
Embodiment 4:
The preparation method of the medium dielectric constant microwave medium composite microwave medium ceramic material of the present embodiment, in accordance with the following steps:
Step (1): Li is pressed2Ti0.75(Mg1/3Nb2/3)0.25O3Chemical formula weighs raw material Li2CO3,TiO2, MgO and Nb2O5, into
Row ball mill mixing 4h is fitted into crucible after drying mixture using wet ball grinding mixing 4h, in 900 DEG C of pre-burning 3h, then ball
Grind to obtain Li2Ti0.75(Mg1/3Nb2/3)0.25O3Powder；
Step (2): BaTi is pressed4O9Chemical formula weighs raw material BaCO3And TiO2, using wet ball grinding mixing 4h, by mixture
It is fitted into crucible after drying, in 1080 DEG C of pre-burning 3h, then BaTi is made in ball milling4O9Powder；
Step (3): Li is made in step (1)2Ti0.75(Mg1/3Nb2/3)0.25O3, step (2) be made BaTi4O9It is mixed with CuO
It closes, wherein Li2Ti0.75(Mg1/3Nb2/3)0.25O3With BaTi4O9Molar ratio is 0.45:0.55, and CuO accounts for Li2Ti0.75(Mg1/ 3Nb2/3)0.25O3And BaTi4O9The 2wt% of gross mass carries out dry, obtained mixed powder after ball milling mixing 2h；
Step (4): it is 5% polyvinyl alcohol water that mixed powder, which is made, with the mass fraction for accounting for its quality 6wt% in step (3)
It is uniformly mixed in solution, and is suppressed under 100MPa pressure, prepare the cylindric green body of diameter 10mm, thickness 5mm；
Step (5): by green body made from step (4) in 1200 DEG C of heat preservation sintering 4h, the medium dielectric constant microwave medium is obtained
Microwave dielectric ceramic materials.
It is according to medium dielectric constant microwave medium composite microwave medium ceramic material, chemical expression made from aforementioned formula and step
(1-x)Li2Ti0.75(Mg1/3Nb2/3)0.25O3+xBaTi4O9+ ywt%M,
Wherein x=0.55, y are that auxiliary agent M accounts for Li2Ti0.75(Mg1/3Nb2/3)0.25O3And BaTi4O9The mass fraction of gross mass,
Y=2, M CuO.
Performance indexes are as follows: 1200 DEG C of sintering temperature, permittivity εr=30.1, quality factor q × f=
48000GHz, frequency-temperature coefficient τf=+3ppm/ DEG C.
Embodiment 5:
The preparation method of the medium dielectric constant microwave medium composite microwave medium ceramic material of the present embodiment, in accordance with the following steps:
Step (1): Li is pressed2Ti0.75(Mg1/3Nb2/3)0.25O3Chemical formula weighs raw material Li2CO3,TiO2, MgO and Nb2O5, adopt
It with wet ball grinding mixing 4h, is fitted into crucible after mixture is dried, in 900 DEG C of pre-burning 3h, then Li is made in ball milling2Ti0.75
(Mg1/3Nb2/3)0.25O3Powder；
Step (2): BaTi is pressed4O9Chemical formula weighs raw material BaCO3And TiO2, using wet ball grinding mixing 4h, by mixture
It is fitted into crucible after drying, in 1080 DEG C of pre-burning 3h, then BaTi is made in ball milling4O9Powder；
Step (3): Li is made in step (1)2Ti0.75(Mg1/3Nb2/3)0.25O3, step (2) be made BaTi4O9It is mixed with CuO
It closes, wherein Li2Ti0.75(Mg1/3Nb2/3)0.25O3With BaTi4O9Molar ratio is 0.45:0.55, and CuO accounts for Li2Ti0.75(Mg1/ 3Nb2/3)0.25O3And BaTi4O9The 0.5wt% of gross mass carries out dry, obtained mixed powder after ball milling mixing 2h；
Step (4): it is 5% polyvinyl alcohol water that mixed powder, which is made, with the mass fraction for accounting for its quality 6wt% in step (3)
It is uniformly mixed in solution, and is suppressed under 100MPa pressure, prepare the cylindric green body of diameter 10mm, thickness 5mm；
Step (5): by green body made from step (4) in 1250 DEG C of heat preservation sintering 4h, the medium dielectric constant microwave medium is obtained
Microwave dielectric ceramic materials.
It is according to medium dielectric constant microwave medium composite microwave medium ceramic material, chemical expression made from aforementioned formula and step
(1-x)Li2Ti0.75(Mg1/3Nb2/3)0.25O3+xBaTi4O9+ ywt%M,
Wherein x=0.55, y are that auxiliary agent M accounts for Li2Ti0.75(Mg1/3Nb2/3)0.25O3And BaTi4O9The mass fraction of gross mass,
Y=0.5, M CuO.
Performance indexes are as follows: 1250 DEG C of sintering temperature, permittivity εr=30.3, quality factor q × f=
67500GHz, frequency-temperature coefficient τf=+1ppm/ DEG C.
Embodiment 6:
The preparation method of the medium dielectric constant microwave medium composite microwave medium ceramic material of the present embodiment, in accordance with the following steps:
Step (1): Li is pressed2Ti0.75(Mg1/3Nb2/3)0.25O3Chemical formula weighs raw material Li2CO3,TiO2, MgO and Nb2O5, adopt
It with wet ball grinding mixing 4h, is fitted into crucible after mixture is dried, in 900 DEG C of pre-burning 3h, then Li is made in ball milling2Ti0.75
(Mg1/3Nb2/3)0.25O3Powder；
Step (2): BaTi is pressed4O9Chemical formula weighs raw material BaCO3And TiO2, using wet ball grinding mixing 4h, by mixture
It is fitted into crucible after drying, in 1080 DEG C of pre-burning 3h, then BaTi is made in ball milling4O9Powder；
Step (3): Li is made in step (1)2Ti0.75(Mg1/3Nb2/3)0.25O3, step (2) be made BaTi4O9With MnCO3
It mixes, wherein Li2Ti0.75(Mg1/3Nb2/3)0.25O3With BaTi4O9Molar ratio is 0.48:0.52, MnCO3Account for Li2Ti0.75(Mg1/ 3Nb2/3)0.25O3And BaTi4O9The 0.5wt% of gross mass carries out dry, obtained mixed powder after ball milling mixing 2h；
Step (4): it is 5% polyvinyl alcohol water that mixed powder, which is made, with the mass fraction for accounting for its quality 6wt% in step (3)
It is uniformly mixed in solution, and is suppressed under 100MPa pressure, prepare the cylindric green body of diameter 10mm, thickness 5mm；
Step (5): by green body made from step (4) in 1280 DEG C of heat preservation sintering 4h, the medium dielectric constant microwave medium is obtained
Microwave dielectric ceramic materials.
It is according to medium dielectric constant microwave medium composite microwave medium ceramic material, chemical expression made from aforementioned formula and step
(1-x)Li2Ti0.75(Mg1/3Nb2/3)0.25O3+xBaTi4O9+ ywt%M,
Wherein x=0.52, y are that auxiliary agent M accounts for Li2Ti0.75(Mg1/3Nb2/3)0.25O3And BaTi4O9The mass fraction of gross mass,
Y=0.5, M MnCO3。
Performance indexes are as follows: 1280 DEG C of sintering temperature, permittivity εr=29.7, quality factor q × f=
72500GHz, frequency-temperature coefficient τf=-3ppm/ DEG C.
Embodiment 7:
The preparation method of the medium dielectric constant microwave medium composite microwave medium ceramic material of the present embodiment, in accordance with the following steps:
Step (1): Li is pressed2Ti0.75(Mg1/3Nb2/3)0.25O3Chemical formula weighs raw material Li2CO3,TiO2, MgO and Nb2O5, adopt
It with wet ball grinding mixing 4h, is fitted into crucible after mixture is dried, in 900 DEG C of pre-burning 3h, then Li is made in ball milling2Ti0.75
(Mg1/3Nb2/3)0.25O3Powder；
Step (2): BaTi is pressed4O9Chemical formula weighs raw material BaCO3And TiO2, using wet ball grinding mixing 4h, by mixture
It is fitted into crucible after drying, in 1080 DEG C of pre-burning 3h, then BaTi is made in ball milling4O9Powder；
Step (3): Li is made in step (1)2Ti0.75(Mg1/3Nb2/3)0.25O3, step (2) be made BaTi4O9With MnCO3
It mixes, wherein Li2Ti0.75(Mg1/3Nb2/3)0.25O3With BaTi4O9Molar ratio is 0.48:0.52, MnCO3Account for Li2Ti0.75(Mg1/ 3Nb2/3)0.25O3And BaTi4O9The 2wt% of gross mass carries out dry, obtained mixed powder after ball milling mixing 2h；
Step (4): it is 5% polyvinyl alcohol water that mixed powder, which is made, with the mass fraction for accounting for its quality 6wt% in step (3)
It is uniformly mixed in solution, and is suppressed under 100MPa pressure, prepare the cylindric green body of diameter 10mm, thickness 5mm；
Step (5): by green body made from step (4) in 1280 DEG C of heat preservation sintering 4h, the medium dielectric constant microwave medium is obtained
Microwave dielectric ceramic materials.
It is according to medium dielectric constant microwave medium composite microwave medium ceramic material, chemical expression made from aforementioned formula and step
(1-x)Li2Ti0.75(Mg1/3Nb2/3)0.25O3+xBaTi4O9+ ywt%M,
Wherein x=0.52, y are that auxiliary agent M accounts for Li2Ti0.75(Mg1/3Nb2/3)0.25O3And BaTi4O9The mass fraction of gross mass,
Y=2, M MnCO3。
Performance indexes are as follows: 1280 DEG C of sintering temperature, permittivity εr=29.8, quality factor q × f=
70500GHz, frequency-temperature coefficient τf=-4ppm/ DEG C.
Embodiment 8:
The preparation method of the medium dielectric constant microwave medium composite microwave medium ceramic material of the present embodiment, in accordance with the following steps:
Step (1): Li is pressed2Ti0.75(Mg1/3Nb2/3)0.25O3Chemical formula weighs raw material Li2CO3,TiO2, MgO and Nb2O5, adopt
It with wet ball grinding mixing 4h, is fitted into crucible after mixture is dried, in 900 DEG C of pre-burning 3h, then Li is made in ball milling2Ti0.75
(Mg1/3Nb2/3)0.25O3Powder；
Step (2): BaTi is pressed4O9Chemical formula weighs raw material BaCO3And TiO2, using wet ball grinding mixing 4h, by mixture
It is fitted into crucible after drying, in 1080 DEG C of pre-burning 3h, then BaTi is made in ball milling4O9Powder；
Step (3): Li is made in step (1)2Ti0.75(Mg1/3Nb2/3)0.25O3, step (2) be made BaTi4O9With CuO,
MnCO3It mixes, wherein Li2Ti0.75(Mg1/3Nb2/3)0.25O3With BaTi4O9Molar ratio is 0.48:0.52, CuO and MnCO3It accounts for
Li2Ti0.75(Mg1/3Nb2/3)0.25O3And BaTi4O9The 0.8wt% and 1.2wt% of gross mass carry out drying after ball milling mixing 2h,
Mixed powder is made；
Step (4): it is 5% polyvinyl alcohol water that mixed powder, which is made, with the mass fraction for accounting for its quality 6wt% in step (3)
It is uniformly mixed in solution, and is suppressed under 100MPa pressure, prepare the cylindric green body of diameter 10mm, thickness 5mm；
Step (5): by green body made from step (4) in 1220 DEG C of heat preservation sintering 4h, the medium dielectric constant microwave medium is obtained
Microwave dielectric ceramic materials.
It is according to medium dielectric constant microwave medium composite microwave medium ceramic material, chemical expression made from aforementioned formula and step
(1-x)Li2Ti0.75(Mg1/3Nb2/3)0.25O3+xBaTi4O9+ ywt%M,
Wherein x=0.52, y are that auxiliary agent M accounts for Li2Ti0.75(Mg1/3Nb2/3)0.25O3And BaTi4O9The mass fraction of gross mass,
Y=2, M are CuO and MnCO3。
Performance indexes are as follows: 1220 DEG C of sintering temperature, permittivity εr=29.8, quality factor q × f=
68500GHz, frequency-temperature coefficient τf=+3ppm/ DEG C.
Embodiment 9:
The preparation method of the medium dielectric constant microwave medium composite microwave medium ceramic material of the present embodiment, in accordance with the following steps:
Step (1): Li is pressed2Ti0.75(Mg1/3Nb2/3)0.25O3Chemical formula weighs raw material Li2CO3,TiO2, MgO and Nb2O5, adopt
It with wet ball grinding mixing 4h, is fitted into crucible after mixture is dried, in 900 DEG C of pre-burning 3h, then Li is made in ball milling2Ti0.75
(Mg1/3Nb2/3)0.25O3Powder；
Step (2): BaTi is pressed4O9Chemical formula weighs raw material BaCO3And TiO2, using wet ball grinding mixing 4h, by mixture
It is fitted into crucible after drying, in 1080 DEG C of pre-burning 3h, then BaTi is made in ball milling4O9Powder；
Step (3): Li is made in step (1)2Ti0.75(Mg1/3Nb2/3)0.25O3, step (2) be made BaTi4O9With GeO2It is mixed
It closes, wherein Li2Ti0.75(Mg1/3Nb2/3)0.25O3With BaTi4O9Molar ratio is 0.4:0.6, GeO2Account for Li2Ti0.75(Mg1/ 3Nb2/3)0.25O3And BaTi4O9The 0.5wt% of gross mass carries out dry, obtained mixed powder after ball milling mixing 2h；
Step (4): it is 5% polyvinyl alcohol water that mixed powder, which is made, with the mass fraction for accounting for its quality 8wt% in step (3)
It is uniformly mixed in solution, and is suppressed under 100MPa pressure, prepare the cylindric green body of diameter 10mm, thickness 5mm；
Step (5): by green body made from step (4) in 1280 DEG C of heat preservation sintering 4h, the medium dielectric constant microwave medium is obtained
Microwave dielectric ceramic materials.
It is according to medium dielectric constant microwave medium composite microwave medium ceramic material, chemical expression made from aforementioned formula and step
(1-x)Li2Ti0.75(Mg1/3Nb2/3)0.25O3+xBaTi4O9+ ywt%M,
Wherein x=0.6, y are that auxiliary agent M accounts for Li2Ti0.75(Mg1/3Nb2/3)0.25O3And BaTi4O9The mass fraction of gross mass, y
=0.5, M GeO2。
Performance indexes are as follows: 1280 DEG C of sintering temperature, permittivity εr=27.8, quality factor q × f=
81500GHz, frequency-temperature coefficient τf=+5ppm/ DEG C.
Embodiment 10:
The preparation method of the medium dielectric constant microwave medium composite microwave medium ceramic material of the present embodiment, in accordance with the following steps:
Step (1): Li is pressed2Ti0.75(Mg1/3Nb2/3)0.25O3Chemical formula weighs raw material Li2CO3,TiO2, MgO and Nb2O5, adopt
It with wet ball grinding mixing 4h, is fitted into crucible after mixture is dried, in 900 DEG C of pre-burning 3h, then Li is made in ball milling2Ti0.75
(Mg1/3Nb2/3)0.25O3Powder；
Step (2): BaTi is pressed4O9Chemical formula weighs raw material BaCO3And TiO2, using wet ball grinding mixing 4h, by mixture
It is fitted into crucible after drying, in 1080 DEG C of pre-burning 3h, then BaTi is made in ball milling4O9Powder；
Step (3): Li is made in step (1)2Ti0.75(Mg1/3Nb2/3)0.25O3, step (2) be made BaTi4O9With GeO2It is mixed
It closes, wherein Li2Ti0.75(Mg1/3Nb2/3)0.25O3With BaTi4O9Molar ratio is 0.4:0.6, GeO2Account for Li2Ti0.75(Mg1/ 3Nb2/3)0.25O3And BaTi4O9The 2wt% of gross mass carries out dry, obtained mixed powder after ball milling mixing 2h；
Step (4): it is 5% polyvinyl alcohol water that mixed powder, which is made, with the mass fraction for accounting for its quality 6wt% in step (3)
It is uniformly mixed in solution, and is suppressed under 100MPa pressure, prepare the cylindric green body of diameter 10mm, thickness 5mm；
Step (5): by green body made from step (4) in 1280 DEG C of heat preservation sintering 4h, the medium dielectric constant microwave medium is obtained
Microwave dielectric ceramic materials.
It is according to medium dielectric constant microwave medium composite microwave medium ceramic material, chemical expression made from aforementioned formula and step
(1-x)Li2Ti0.75(Mg1/3Nb2/3)0.25O3+xBaTi4O9+ ywt%M,
Wherein x=0.6, y are that auxiliary agent M accounts for Li2Ti0.75(Mg1/3Nb2/3)0.25O3And BaTi4O9The mass fraction of gross mass, y
=2, M GeO2。
Performance indexes are as follows: 1280 DEG C of sintering temperature, permittivity εr=27.6, quality factor q × f=
86500GHz, frequency-temperature coefficient τf=+4ppm/ DEG C.
Embodiment 11:
The preparation method of the medium dielectric constant microwave medium composite microwave medium ceramic material of the present embodiment, in accordance with the following steps:
Step (1): Li is pressed2Ti0.75(Mg1/3Nb2/3)0.25O3Chemical formula weighs raw material Li2CO3,TiO2, MgO and Nb2O5, adopt
It with wet ball grinding mixing 4h, is fitted into crucible after mixture is dried, in 900 DEG C of pre-burning 3h, then Li is made in ball milling2Ti0.75
(Mg1/3Nb2/3)0.25O3Powder；
Step (2): BaTi is pressed4O9Chemical formula weighs raw material BaCO3And TiO2, using wet ball grinding mixing 4h, by mixture
It is fitted into crucible after drying, in 1080 DEG C of pre-burning 3h, then BaTi is made in ball milling4O9Powder；
Step (3): Li is made in step (1)2Ti0.75(Mg1/3Nb2/3)0.25O3, step (2) be made BaTi4O9With LiF,
GeO2It mixes, wherein Li2Ti0.75(Mg1/3Nb2/3)0.25O3With BaTi4O9Molar ratio is 0.4:0.6, LiF and GeO2It accounts for respectively
Li2Ti0.75(Mg1/3Nb2/3)0.25O3And BaTi4O9The 1wt% and 1wt% of gross mass carry out drying after ball milling mixing 2h, are made
Mixed powder；
Step (4): it is 5% polyvinyl alcohol water that mixed powder, which is made, with the mass fraction for accounting for its quality 6wt% in step (3)
It is uniformly mixed in solution, and is suppressed under 100MPa pressure, prepare the cylindric green body of diameter 10mm, thickness 5mm；
Step (5): by green body made from step (4) in 1200 DEG C of heat preservation sintering 4h, the medium dielectric constant microwave medium is obtained
Microwave dielectric ceramic materials.
It is according to medium dielectric constant microwave medium composite microwave medium ceramic material, chemical expression made from aforementioned formula and step
(1-x)Li2Ti0.75(Mg1/3Nb2/3)0.25O3+xBaTi4O9+ ywt%M
Wherein x=0.6, y are that auxiliary agent M accounts for Li2Ti0.75(Mg1/3Nb2/3)0.25O3And BaTi4O9The mass fraction of gross mass, y
=2, M are LiF and GeO2。
Performance indexes are as follows: 1200 DEG C of sintering temperature, permittivity εr=27.3, quality factor q × f=
78500GHz, frequency-temperature coefficient τf=+4ppm/ DEG C.
Embodiment 12:
The preparation method of the medium dielectric constant microwave medium composite microwave medium ceramic material of the present embodiment, in accordance with the following steps:
Step (1): Li is pressed2Ti0.75(Mg1/3Nb2/3)0.25O3Chemical formula weighs raw material Li2CO3,TiO2, MgO and Nb2O5, adopt
It with wet ball grinding mixing 4h, is fitted into crucible after mixture is dried, in 900 DEG C of pre-burning 3h, then Li is made in ball milling2Ti0.75
(Mg1/3Nb2/3)0.25O3Powder；
Step (2): BaTi is pressed4O9Chemical formula weighs raw material BaCO3And TiO2, using wet ball grinding mixing 4h, by mixture
It is fitted into crucible after drying, in 1080 DEG C of pre-burning 3h, then BaTi is made in ball milling4O9Powder；
Step (3): Li is made in step (1)2Ti0.75(Mg1/3Nb2/3)0.25O3, step (2) be made BaTi4O9With LiF,
MnCO3And GeO2It mixes, wherein Li2Ti0.75(Mg1/3Nb2/3)0.25O3With BaTi4O9Molar ratio is 0.45:0.55, LiF, MnCO3
And GeO2Li is accounted for respectively2Ti0.75(Mg1/3Nb2/3)0.25O3And BaTi4O91wt%, 0.5wt% and 0.5wt% of gross mass are carried out
It is dry after ball milling mixing 2h, mixed powder is made；
Step (4): it is 5% polyvinyl alcohol water that mixed powder, which is made, with the mass fraction for accounting for its quality 6wt% in step (3)
It is uniformly mixed in solution, and is suppressed under 100MPa pressure, prepare the cylindric green body of diameter 10mm, thickness 5mm；
Step (5): by green body made from step (4) in 1200 DEG C of heat preservation sintering 4h, the medium dielectric constant microwave medium is obtained
Microwave dielectric ceramic materials.
It is according to medium dielectric constant microwave medium composite microwave medium ceramic material, chemical expression made from aforementioned formula and step
(1-x)Li2Ti0.75(Mg1/3Nb2/3)0.25O3+xBaTi4O9+ ywt%M
Wherein x=0.55, y are that auxiliary agent M accounts for Li2Ti0.75(Mg1/3Nb2/3)0.25O3And BaTi4O9The mass fraction of gross mass,
Y=2, M LiF, MnCO3And GeO2。
Performance indexes are as follows: 1200 DEG C of sintering temperature, permittivity εr=30.2, quality factor q × f=
77500GHz, frequency-temperature coefficient τf=+2ppm/ DEG C.
Embodiment 13:
The preparation method of the medium dielectric constant microwave medium composite microwave medium ceramic material of the present embodiment, in accordance with the following steps:
Step (1): Li is pressed2Ti0.75(Mg1/3Nb2/3)0.25O3Chemical formula weighs raw material Li2CO3,TiO2, MgO and Nb2O5, adopt
It with wet ball grinding mixing 4h, is fitted into crucible after mixture is dried, in 910 DEG C of pre-burning 3h, then Li is made in ball milling2Ti0.75
(Mg1/3Nb2/3)0.25O3Powder；
Step (2): BaTi is pressed4O9Chemical formula weighs raw material BaCO3And TiO2, using wet ball grinding mixing 4h, by mixture
It is fitted into crucible after drying, in 1075 DEG C of pre-burning 2h, then BaTi is made in ball milling4O9Powder；
Step (3): Li is made in step (1)2Ti0.75(Mg1/3Nb2/3)0.25O3, step (2) be made BaTi4O9With LiF,
MnCO3And GeO2It mixes, wherein Li2Ti0.75(Mg1/3Nb2/3)0.25O3With BaTi4O9Molar ratio is 0.5:0.5, LiF, MnCO3With
GeO2Li is accounted for respectively2Ti0.75(Mg1/3Nb2/3)0.25O3And BaTi4O90.7wt%, 0.5wt% and 0.5wt% of gross mass are carried out
It is dry after ball milling mixing 2h, mixed powder is made；
Step (4): it is 5% polyvinyl alcohol water that mixed powder, which is made, with the mass fraction for accounting for its quality 6wt% in step (3)
It is uniformly mixed in solution, and is suppressed under 100MPa pressure, prepare the cylindric green body of diameter 10mm, thickness 5mm；
Step (5): by green body made from step (4) in 1230 DEG C of heat preservation sintering 4h, the medium dielectric constant microwave medium is obtained
Microwave dielectric ceramic materials.
It is according to medium dielectric constant microwave medium composite microwave medium ceramic material, chemical expression made from aforementioned formula and step
(1-x)Li2Ti0.75(Mg1/3Nb2/3)0.25O3+xBaTi4O9+ ywt%M
Wherein x=0.5, y are that auxiliary agent M accounts for Li2Ti0.75(Mg1/3Nb2/3)0.25O3And BaTi4O9The mass fraction of gross mass, y
=1.7, M LiF, MnCO3And GeO2。
Performance indexes are as follows: 1230 DEG C of sintering temperature, permittivity εr=30.4, quality factor q × f=
79000GHz, frequency-temperature coefficient τf=+3ppm/ DEG C.
Embodiment 14:
The preparation method of the medium dielectric constant microwave medium composite microwave medium ceramic material of the present embodiment, in accordance with the following steps:
Step (1): Li is pressed2Ti0.75(Mg1/3Nb2/3)0.25O3Chemical formula weighs raw material Li2CO3,TiO2, MgO and Nb2O5, adopt
It with wet ball grinding mixing 4h, is fitted into crucible after mixture is dried, in 890 DEG C of pre-burning 4h, then Li is made in ball milling2Ti0.75
(Mg1/3Nb2/3)0.25O3Powder；
Step (2): BaTi is pressed4O9Chemical formula weighs raw material BaCO3And TiO2, using wet ball grinding mixing 4h, by mixture
It is fitted into crucible after drying, in 1100 DEG C of pre-burning 2h, then BaTi is made in ball milling4O9Powder；
Step (3): Li is made in step (1)2Ti0.75(Mg1/3Nb2/3)0.25O3, step (2) be made BaTi4O9With CuO and
MnCO3It mixes, wherein Li2Ti0.75(Mg1/3Nb2/3)0.25O3With BaTi4O9Molar ratio is 0.55:0.45, CuO and MnCO3It accounts for respectively
Li2Ti0.75(Mg1/3Nb2/3)0.25O3And BaTi4O9The 0.75wt% and 0.75wt% of gross mass are done after carrying out ball milling mixing 2h
It is dry, mixed powder is made；
Step (4): it is 5% polyvinyl alcohol water that mixed powder, which is made, with the mass fraction for accounting for its quality 6wt% in step (3)
It is uniformly mixed in solution, and is suppressed under 100MPa pressure, prepare the cylindric green body of diameter 10mm, thickness 5mm；
Step (5): by green body made from step (4) in 1240 DEG C of heat preservation sintering 4h, the medium dielectric constant microwave medium is obtained
Microwave dielectric ceramic materials.
It is according to medium dielectric constant microwave medium composite microwave medium ceramic material, chemical expression made from aforementioned formula and step
(1-x)Li2Ti0.75(Mg1/3Nb2/3)0.25O3+xBaTi4O9+ ywt%M
Wherein x=0.45, y are that auxiliary agent M accounts for Li2Ti0.75(Mg1/3Nb2/3)0.25O3And BaTi4O9The mass fraction of gross mass,
Y=1.5, M are CuO and MnCO3。
Performance indexes are as follows: 1240 DEG C of sintering temperature, permittivity εr=29.7, quality factor q × f=
69800GHz, frequency-temperature coefficient τf=+2ppm/ DEG C.
Claims (4)
1. a kind of medium dielectric constant microwave medium composite microwave medium ceramic material, which is characterized in that the chemistry of the microwave dielectric ceramic materials
Expression formula is (1-x) Li2Ti0.75(Mg1/3Nb2/3)0.25O3+x BaTi4O9+ ywt%M；Wherein, 0.4≤x≤0.6, y are to account for
Li2Ti0.75(Mg1/3Nb2/3)0.25O3And BaTi4O9The mass fraction of gross mass, 0.5≤y≤2, M are auxiliary agent, are LiF, MnCO3、
CuO or GeO2One or more of mixing.
2. the preparation method of microwave dielectric ceramic materials described in claim 1, which comprises the steps of:
(1) Li is pressed2Ti0.75(Mg1/3Nb2/3)0.25O3The molar ratio of each metallic element weighs raw material Li in chemical formula2CO3、TiO2、
MgO and Nb2O5, using wet ball grinding mixing 4h；After mixture is dried under the conditions of 880~920 DEG C 2~4h of pre-burning, then through ball
Grind to obtain Li2Ti0.75(Mg1/3Nb2/3)0.25O3Powder；
(2) BaTi is pressed4O9The molar ratio of each metallic element weighs raw material BaCO in chemical formula3And TiO2, mixed using wet ball grinding
Expect 4h；After mixture is dried under the conditions of 1050~1100 DEG C 2~4h of pre-burning, then BaTi is made through ball milling4O9Powder；
(3) LiF, MnCO are taken3, CuO or GeO2One or more of mixing be used as auxiliary agent, with Li2Ti0.75(Mg1/3Nb2/3)0.25O3And BaTi4O9Ball milling mixing 2h is carried out, is then dried, mixed powder is made；Wherein, Li2Ti0.75(Mg1/3Nb2/3)0.25O3
With BaTi4O9Molar ratio is (1-x): x, and auxiliary agent accounts for Li2Ti0.75(Mg1/3Nb2/3)0.25O3And BaTi4O9The 0.5 of gross mass~
2wt%；
(4) polyvinyl alcohol water solution is taken by 5~8wt% of mixed powder quality, the mass fraction of polyvinyl alcohol water solution is
5%；After mixing by mixed powder and polyvinyl alcohol water solution, it is suppressed, is prepared cylindric under 100MPa pressure
Green body；
(5) green body is obtained into medium dielectric constant microwave medium composite microwave medium ceramic material in 1200~1280 DEG C of heat preservation sintering 4h.
3. according to the method described in claim 2, it is characterized in that, the pre-burning in the step (1) and step (2) is in crucible
Middle progress.
4. according to the method described in claim 2, it is characterized in that, in the step (4), the diameter 10mm of cylindric green body,
Thickness 5mm.
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