CN101117285A - Ba(1-x)SrxTiO3-BaX6Ti6O19(X=Mg, Zn) diphasic composite micro-wave ceramic material and preparation method thereof - Google Patents
Ba(1-x)SrxTiO3-BaX6Ti6O19(X=Mg, Zn) diphasic composite micro-wave ceramic material and preparation method thereof Download PDFInfo
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- CN101117285A CN101117285A CNA2007100442134A CN200710044213A CN101117285A CN 101117285 A CN101117285 A CN 101117285A CN A2007100442134 A CNA2007100442134 A CN A2007100442134A CN 200710044213 A CN200710044213 A CN 200710044213A CN 101117285 A CN101117285 A CN 101117285A
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Abstract
The invention relates to the two-phase composite microwave ceramics material technical field with controllable permittivity with the seriation of composition components and the high adjustability in imposed DC electric field. The Ba(1-x)SrxTiO3-BaX6Ti6O19(X=Mg, Zn) two-phased composite microwave ceramics material of the invention comprises: Ba (1-x)SrxTiO3(x=0.3-0.6) 80.0wt percent to 20.0wt percent and BaX6Ti6O19 20.0wt percent to 80.0wt percent. Adopting traditional electronic ceramics preparation process, the invention selects a low dielectric microwave dielectric material BaX6Ti6O19(X=Mg, Zn) with a high dielectric property and a barium strontium titanate ferroelectric materials of a different Ba/Sr components to be in two-phase gradient composite. The composite material produced has an appropriate permittivity, an electric adjustable property and is applicable to adjustable microwave elements and electric adjustable medium function modules.
Description
Technical field
It is controlled and have a two-phase composite microwave ceramic material technical field of high tunable characteristic under the applying direct current electric field effect with the plural components seriation to the present invention relates to a kind of specific inductivity.
Background technology
The fast development of electronic devices and components industry has been researched and proposed new requirements at the higher level to the informational function stupalith, and the dielectric material that (1-4GHz) uses from the L-band to the S-band requires to have low-k, low-loss and suitable electric tunable characteristic.Passive adjustable microwave device is the active demand of modern information industry field institute as a kind of novel function electronic devices and components, and utilizing the electricity of ferroelectric material non-linear is one of important technology approach of realizing by passive adjustable microwave device, and simple BaTiO
3Base ferroelectric material system often has higher dielectric constant (ε
r＞2000), aspect the adjustable microwave device application, be difficult to satisfy the requirement of its space impedance matching and high power device use.For the traditional microwave ceramic material of routine, its functional performance is comparatively single, does not generally have the dielectric tunable characteristic, can not satisfy the design requirements of adjustable microwave device.Therefore, under the development trend of current electron device multifunction, function modoularization and compact in size, seek specific inductivity seriation (ε
r=50～2000), the novel microwave dielectric ceramic material system with dielectric tunable characteristic is an important developing direction.
Strontium-barium titanate (Ba
(1-x)Sr
xTiO
3) be a kind of typical perovskite structure ferroelectric material, excellent dielectric properties such as have high specific inductivity, low dielectric loss and nonlinear dielectric constant is adjustable under the DC electric field effect, and its Curie temperature can be with Ba/Sr than adjustable continuously in very wide scope.Therefore, the barium-strontium titanate ceramic material aspect microwave adjustable device (as phase shifter, wave filter, variable condenser and retarding line etc.) obtain increasingly extensive concern, especially aspect microwave phase shifter especially at present research focus.About the development research aspect of strontium-barium titanate dielectric material with adjustable and relevant adjustable microwave device thereof, main still with artificial representative such as Sengupta L.C., Drach W.C., Chiu L.H., Shamsaifar K. and Zhu Y.F., around Ba
(1-x)Sr
xTiO
3Ferroelectric material has obtained the dielectric material with adjustable system of a series of specific inductivity between 200～6000 by modes such as compound, doping vario-properties, has designed and developed adjustable microwave devices such as waveguide medium resonator, electric adjustable filter, oscillator.
BaX
6Ti
6O
19(X=Mg Zn) is a class hexagonal structure (P6
3/ mmc) low-k (ε
r=20～40) microwave dielectric material has excellent microwave dielectric property.In recent years, people such as Jayanthi S. and Preethi T.M. has carried out synthetic preparation and Study on microwave dielectric property to such dielectric material.Yet, adopt BaX
6Ti
6O
19(X=Mg, Zn) the low dielectric microwave material of this class and high Jie Ba
(1-x)Sr
xTiO
3Ferroelectric material carries out organic compound, and the research that be intended to obtain the moderate and seriation of specific inductivity, has a composite microwave ceramic material of high dielectric tunable characteristic does not appear in the newspapers as yet.
Summary of the invention
Purpose of the present invention is exactly this technical barrier that solves desired moderate specific inductivity of present adjustable microwave dielectric material and high dielectric adjustable, and a kind of Ba is provided
(1-x)Sr
xTiO
3-BaX
6Ti
6O
19(X=Mg, Zn) two-phase composite microwave ceramic material, this composite microwave ceramic material had both had moderate specific inductivity and controlled with the plural components seriation, have again than high dielectric adjustable and low dielectric loss (high Q value), be applicable to designing and developing of adjustable microwave device and tunable medium functional module.
Another object of the present invention just provides above-mentioned Ba
(1-x)Sr
xTiO
3-BaX
6Ti
6O
19(X=Mg, Zn) preparation method of two-phase composite microwave ceramic material.
The present inventor finds to select for use the microwave dielectric material BaX of dielectric properties excellence through a large amount of experimental studies
6Ti
6O
19(X=Mg is Zn) with the Ba of different B a/Sr component
(1-x)Sr
xTiO
3It is compound that ferroelectric material carries out two phase gradients, obtains pure Ba
(1-x)Sr
xTiO
3-BaX
6Ti
6O
19(X=Mg, Zn) (x=0.3～0.6) two-phase composite material, and this composite microwave ceramic material has simultaneously than high dielectric adjustable, low dielectric loss (high Q value) and proper dielectric constant, is applicable to designing and developing of adjustable microwave device and tunable medium functional module.
The present invention is achieved through the following technical solutions:
A kind of Ba
(1-x)Sr
xTiO
3-BaX
6Ti
6O
19(its composition is for X=Mg, Zn) two-phase composite microwave ceramic material:
Ba
(1-x)Sr
xTiO
3(x＝0.3～0.6) 80.0wt％～20.0wt％
BaX
6Ti
6O
19 20.0wt％～80.0wt％。
Above-mentioned Ba
(1-x)Sr
xTiO
3-BaX
6Ti
6O
19(X=Mg, Zn) preparation method of two-phase composite microwave ceramic material comprises the steps:
A, take by weighing Ba by the set of dispense ratio
(1-x)Sr
xTiO
3(x=0.3～0.6) powder and BaX
6Ti
6O
19(X=Mg, Zn) powder add zirconia ball and dehydrated alcohol or deionized water, ball milling, and discharging oven dry back is crossed 200 mesh sieves and is obtained composite powder;
The polyvinyl alcohol (PVA) of b, employing 8～10% carries out granulation as binding agent to above-mentioned composite powder, is pressed into the ceramic green sheet of desired size size under 10～100MPa pressure;
C, with the ceramic green sheet through 550 ℃～600 ℃ row is sticking handle after, 1300 ℃～1500 ℃ insulations 2～4 hours, can obtain two-phase composite microwave ceramic material again.
Ba
(1-x)Sr
xTiO
3(x=0.3～0.6) powder adopts traditional electronic ceramic powder preparation method, and promptly solid reaction process is selected BaTiO for use
3And SrTiO
3Be main raw material, according to certain Ba/Sr molar ratio ingredient, confected materials placed nylon ball grinder, added zirconia ball and dehydrated alcohol or deionized water ball milling 20～24 hours, discharging oven dry back obtains after the grinding 1100 ℃ of pre-burnings 4 hours.
BaX
6Ti
6O
19(X=Mg, Zn) powder can adopt solid reaction process equally, prepares according to following reaction equation:
BaTiO
3+5TiO
2+6MgO＝BaMg
6Ti
6O
19
BaTiO
3+5TiO
2+6ZnO＝BaZn
6Ti
6O
19
Concrete preparation method is: at first take by weighing BaTiO respectively by above-mentioned mole proportioning
3, TiO
2, MgO and BaTiO
3, TiO
2, the ZnO powder, mix the back and add zirconia ball and dehydrated alcohol or deionized water, ball milling, discharging oven dry back obtains BaX 1150 ℃～1300 ℃ pre-burnings 4～8 hours after the grinding
6Ti
6O
19(X=Mg, Zn) powder.
The preparation method of above-mentioned two kinds of powders is prior art.During the compound ball milling, the mass ratio of zirconia ball and ball milling material is preferably 1.2～1.5: 1; The mass ratio of dehydrated alcohol or deionized water and ball milling material is 1.5～3.0: 1.
Beneficial effect of the present invention: the present invention adopts traditional electronic ceramic technology, selects the low dielectric microwave dielectric material BaX of dielectric properties excellence for use
6Ti
6O
19(X=Mg, Zn) to carry out two phase gradients compound with the strontium-barium titanate ferroelectric material of different B a/Sr component, obtain unexpectedly a kind of specific inductivity moderate, have electric tunable characteristic and be applicable to the adjustable microwave device and the Ba of electric tunable medium functional module
(1-x)Sr
xTiO
3-BaX
6Ti
6O
19(X=Mg, Zn) two-phase composite microwave ceramic material.Specifically, this kind novel composite ceramic material has following principal feature:
(1) Curie temperature of this composite microwave ceramic material system can require to adjust the structure and the performance of material system according to the working temperature of designed adjustable microwave device with Ba/Sr than adjustable continuously in very wide scope;
(2) pass through Ba
(1-x)Sr
xTiO
3(x=0.3～0.6) and BaX
6Ti
6O
19(specific inductivity of composite microwave ceramic material can be adjustable continuously between 30～1500 for X=Mg, the Zn) variation of two-phase plural components content, can obtain the material system of specific inductivity seriation, widened the range of application of material;
(3) under the applying direct current electric field effect, described composite microwave ceramic material has higher dielectric tunable characteristic (T＞20%), is applicable to designing and developing of adjustable microwave device and electric tunable medium functional module;
(4) its composition of this composite ceramic material is with Ba
(1-x)Sr
xTiO
3(x=0.3～0.6) and BaX
6Ti
6O
19(X=Mg, Zn) the pure compound existence of two-phase form does not have the generation of other dephasign, has excellent dielectric properties;
(5) adopt traditional electronic ceramic technology, technology is simple, and cost is low, the side effect of material system environment-protecting asepsis, and excellent performance is applicable to the exploitation and the design of adjustable microwave device.
Description of drawings
Fig. 1 is Ba
(1-x)Sr
xTiO
3-BaX
6Ti
6O
19(X=Mg, Zn) the X-ray diffraction analysis collection of illustrative plates of two-phase composite microwave ceramic material.
Fig. 2 is Ba
(1-x)Sr
xTiO
3-BaX
6Ti
6O
19(X=Mg, Zn) relation curve of the specific inductivity of two-phase composite microwave ceramic material and loss and temperature.
Fig. 3 is Ba
(1-x)Sr
xTiO
3-BaX
6Ti
6O
19(X=Mg, Zn) relation curve of the specific inductivity of two-phase composite microwave ceramic material and external dc field intensity.
Embodiment
The preparation method of two-phase composite microwave ceramic material provided by the present invention specifically comprises the steps:
(1) adopts traditional electronic ceramic powder preparation technology,, select BaTiO for use by solid reaction process
3And SrTiO
3(99.9%, 100nm, Shandong state rises ceramic material company limited and provides) be main raw material, according to certain Ba/Sr molar ratio ingredient, confected materials is placed nylon ball grinder, added zirconia ball and dehydrated alcohol or deionized water ball milling 20～24 hours, discharging oven dry back obtains Ba 1100 ℃ of pre-burnings 4 hours after the grinding
(1-x)Sr
xTiO
3(x=0.3～0.6) powder.
(2) adopt solid reaction process, according to the synthetic Ba of following reaction equation
(1-x)Sr
xTiO
3-BaX
6Ti
6O
19(X=Mg, Zn) powder:
BaTiO
3+5TiO
2+6MgO＝BaMg
6Ti
6O
19
BaTiO
3+5TiO
2+6ZnO＝BaZn
6Ti
6O
19
At first take by weighing BaTiO respectively by above-mentioned mole proportioning
3, TiO
2(99.9%), MgO (99.9%) and BaTiO
3, TiO
2, ZnO (99.9%) powder, mix the back material and place nylon ball grinder, add zirconia ball and dehydrated alcohol or deionized water, ball milling 20～24 hours, discharging oven dry back obtains BaX 1150 ℃～1300 ℃ pre-burnings 4～8 hours after the grinding
6Ti
6O
19(X=Mg, Zn) powder.
(3) take by weighing compound according to following set of dispense ratio, add zirconia ball and dehydrated alcohol or deionized water, ball milling 20～24 hours, discharging oven dry back is crossed 200 mesh sieves and is obtained composite powder.
Ba
(1-x)Sr
xTiO
3(x＝0.3～0.6) 80.0wt％～20.0wt％
BaX
6Ti
6O
19(X＝Mg，Zn) 20.0wt％～80.0wt％
(4) polyvinyl alcohol (PVA) of employing 8～10% carries out granulation as binding agent to above-mentioned composite powder, under 10～100MPa pressure, is pressed into the ceramic green sheet of desired size size by the forming mould of different model.
(5) the ceramic green sheet through 550 ℃～600 ℃ row is sticking handle after, the pottery that obtains is carried out 1300 ℃～1500 ℃ (being incubated 2～4 hours) sintering processes, can obtain described two-phase composite microwave ceramic material.
Preparation Ba
(1-x)Sr
xTiO
3-BaX
6Ti
6O
19(x=0.50,0.45,0.40; X=Mg, Zn) two-phase composite microwave ceramic material:
According to Ba
0.5Sr
0.5TiO
3, Ba
0.55Sr
0.45TiO
3And Ba
0.6Sr
0.4TiO
3Stoichiometric ratio, take by weighing 46.6454gBaTiO respectively
3With 36.7034g SrTiO
3, 51.3099g BaTiO
3With 33.0331g SrTiO
3, 55.9744g BaTiO
3And 29.3627gSrTiO
3Powder places nylon ball grinder, adds zirconia ball and dehydrated alcohol, ball milling 24 hours, and discharging oven dry back obtains Ba 1100 ℃ of pre-burnings 4 hours after the grinding
0.5Sr
0.5TiO
3, Ba
0.55Sr
0.45TiO
3And Ba
0.6Sr
0.4TiO
3Powder is stand-by.In addition, take by weighing 16.3422g BaTiO respectively
3, 27.9930g TiO
2, 16.9429g MgO and 16.3422g BaTiO
3, 27.9930gTiO
2, 34.2222g ZnO powder places nylon ball grinder, adds zirconia ball and deionized water, ball milling 24 hours, discharging oven dry back obtains BaMg 1250 ℃ of pre-burnings 6 hours after the grinding
6Ti
6O
19And BaZn
6Ti
6O
19Powder is stand-by.
Take by weighing above-mentioned synthetic Ba respectively according to plural components proportioning in the table 1
0.5Sr
0.5TiO
3, Ba
0.55Sr
0.45TiO
3, Ba
0.6Sr
0.4TiO
3, BaMg
6Ti
6O
19And BaZn
6Ti
6O
19Stand-by powder:
Table 1.Ba
(1-x)Sr
xTiO
3-BaX
6Ti
6O
19(x=0.50,0.45,0.40; X=Mg, Zn) composite microwave ceramic material proportioning
| |
1 # | 2 # | 3 # | 4 # | 5 # |
| Ba 0.5Sr 0.5TiO 3 | 8.0g | - | - | - | - |
| Ba 0.55Sr 0.45TiO 3 | - | 8.0g | - | - | - |
| Ba 0.6Sr 0.4TiO 3 | - | - | 12.0g | 8.0g | 10.0g |
| BaMg 6Ti 6O 19 | 12.0g | 12.0g | 8.0g | 12.0g | - |
| BaZn 6Ti 6O 19 | - | - | - | - | 10.0g |
The compound of above-mentioned each prescription is put into nylon ball grinder, added zirconia ball and dehydrated alcohol ball milling 24 hours, discharging oven dry back powder is crossed 200 mesh sieves, according to traditional electronic ceramic technology, the polyvinyl alcohol (PVA) of employing 8% carries out granulation as binding agent, under 10MPa pressure, dry method is pressed into diameter phi=10mm green sheet, after the sticking processing of 550 ℃ rows, sample is under air atmosphere, sintering temperature is in 1350 ℃～1450 ℃ scopes, is incubated after 4 hours, obtains Ba
(1-x)Sr
xTiO
3-BaX
6Ti
6O
19(x=0.50,0.45,0.40; X=Mg, Zn) two-phase composite microwave ceramic sample.
With the ceramics sample polishing both surfaces that makes, carried out analysis of thing phase composition and dielectric properties test behind silver, the silver ink firing.
Embodiment 1
#-5
#Prepared Ba fills a prescription
(1-x)Sr
xTiO
3-BaX
6Ti
6O
19(x=0.50,0.45,0.40; X=Mg, Zn) the X-ray diffraction analysis collection of illustrative plates of composite microwave ceramic material is as shown in Figure 1;
Embodiment 1
#-5
#Prepared Ba fills a prescription
(1-x)Sr
xTiO
3-BaX
6Ti
6O
19(x=0.50,0.45,0.40; X=Mg, Zn) relation curve of the specific inductivity of composite microwave ceramic material and loss and temperature is as shown in Figure 2;
Embodiment 1
#-5
#Prepared Ba fills a prescription
(1-x)Sr
xTiO
3-BaX
6Ti
6O
19(x-0.50,0.45,0.40; X=Mg, Zn) relation curve of the specific inductivity of composite microwave ceramic material and external dc field intensity as shown in Figure 3, wherein, 1
#40wt%Ba
0.5Sr
0.5TiO
3With 60wt%BaMg
6Ti
6O
19Compound; 2
#Be 40wt%Ba
0.55Sr
0.45TiO
3With 60wt%BaMg
6Ti
6O
19Compound; 3
#Be 60wt%Ba
0.6Sr
0.4TiO
3With 40wt%BaMg
6Ti
6O
19Compound; 4
#Be 40wt%Ba
0.6Sr
0.4TiO
3With 60wt%BaMg
6Ti
6O
19Compound; 5
#Be 50wt%Ba
0.6Sr
0.4TiO
3With 50wt%BaZn
6Ti
6O
19Compound.
Claims (4)
1. Ba
(1-x)Sr
xTiO
3-BaX
6Ti
6O
19(its composition is for X=Mg, Zn) two-phase composite microwave ceramic material:
Ba
(1-x)Sr
xTiO
3(x＝0.3～0.6)80.0wt％～20.0wt％
BaX
6Ti
6O
19 20.0wt％～80.0wt％。
2. the described Ba of claim 1
(1-x)Sr
xTiO
3-BaX
6Ti
6O
19(X=Mg, Zn) preparation method of two-phase composite microwave ceramic material comprises the steps:
A, take by weighing Ba by the set of dispense ratio
(1-x)Sr
xTiO
3(x=0.3～0.6) powder and BaX
6Ti
6O
19(X=Mg, Zn) powder add zirconia ball and dehydrated alcohol or deionized water, ball milling, and discharging oven dry back is crossed 200 mesh sieves and is obtained composite powder;
The polyvinyl alcohol of b, employing 8～10% carries out granulation as binding agent to above-mentioned composite powder, is pressed into the ceramic green sheet of desired size size under 10～100MPa pressure;
C, with the ceramic green sheet through 550 ℃～600 ℃ row is sticking handle after, again 1300 ℃～1500 ℃ insulations 2～4 hours.
3. the described Ba of claim 2
(1-x)Sr
xTiO
3-BaX
6Ti
6O
19(X=Mg, the Zn) preparation method of two-phase composite microwave ceramic material is characterized in that: Ba
(1-x)Sr
xTiO
3(x=0.3～0.6) powder and BaX
6Ti
6O
19(X=Mg, Zn) powder adopts solid reaction process to make.
4. the described Ba of claim 2
(1-x)Sr
xTiO
3-BaX
6Ti
6O
19(X=Mg, the Zn) preparation method of two-phase composite microwave ceramic material is characterized in that: during the compound ball milling, the mass ratio of zirconia ball and ball milling material is 1.2～1.5: 1; The mass ratio of dehydrated alcohol or deionized water and ball milling material is 1.5～3.0: 1.
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|---|---|---|---|
| CNB2007100442134A CN100480212C (en) | 2007-07-26 | 2007-07-26 | Ba1-XSrXTiO3-BaX6Ti6O19(X=Mg, zn) two-phase composite microwave ceramic material and its preparation method |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101372417B (en) * | 2008-09-25 | 2011-08-10 | 中国科学院青海盐湖研究所 | High specific saturation magnetization and high coercitive force strontium ferrite magnetic powder and preparation thereof |
| CN103288348A (en) * | 2013-05-17 | 2013-09-11 | 同济大学 | High-energy-density barium strontium titanate based glass ceramic energy storage material as well as preparation and application thereof |
| CN103316651A (en) * | 2013-06-25 | 2013-09-25 | 桂林理工大学 | Visible-light-responded photocatalyst BaTi6Mg6O19 and preparation method thereof |
| CN109626984A (en) * | 2019-01-30 | 2019-04-16 | 浙江大学 | A kind of high dielectric of existing fringing field is adjustable zirconium doping barium ferrite and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1181010C (en) * | 2003-05-23 | 2004-12-22 | 华中科技大学 | Composite microwave tuning strontium barium titanate ceramics |
| CN1927765A (en) * | 2006-09-22 | 2007-03-14 | 中国科学院上海硅酸盐研究所 | Preparation method for non-homogeneous phase precipitation of strontium barium titanate-magnesium oxide composite material |
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2007
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101372417B (en) * | 2008-09-25 | 2011-08-10 | 中国科学院青海盐湖研究所 | High specific saturation magnetization and high coercitive force strontium ferrite magnetic powder and preparation thereof |
| CN103288348A (en) * | 2013-05-17 | 2013-09-11 | 同济大学 | High-energy-density barium strontium titanate based glass ceramic energy storage material as well as preparation and application thereof |
| CN103288348B (en) * | 2013-05-17 | 2015-07-29 | 同济大学 | The barium-strontium titanate-based glass-ceramic energy storage material of high energy storage density and Synthesis and applications |
| CN103316651A (en) * | 2013-06-25 | 2013-09-25 | 桂林理工大学 | Visible-light-responded photocatalyst BaTi6Mg6O19 and preparation method thereof |
| CN109626984A (en) * | 2019-01-30 | 2019-04-16 | 浙江大学 | A kind of high dielectric of existing fringing field is adjustable zirconium doping barium ferrite and preparation method thereof |
| CN109626984B (en) * | 2019-01-30 | 2020-11-27 | 浙江大学 | Low-electric-field high-dielectric adjustable zirconium-doped barium ferrite and preparation method thereof |
| CN112062551A (en) * | 2020-08-06 | 2020-12-11 | 同济大学 | Bismuth ferrite-based piezoelectric ceramic material with high depolarization temperature and high piezoelectric performance and preparation method thereof |
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| Publication number | Publication date |
|---|---|
| CN100480212C (en) | 2009-04-22 |
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