CN101265085B - Dielectric adjustable Ba[1-x]SrxTiO3-MgAl2O4 diphase composite microwave ceramic material and preparation method thereof - Google Patents

Dielectric adjustable Ba[1-x]SrxTiO3-MgAl2O4 diphase composite microwave ceramic material and preparation method thereof Download PDF

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CN101265085B
CN101265085B CN2008100363531A CN200810036353A CN101265085B CN 101265085 B CN101265085 B CN 101265085B CN 2008100363531 A CN2008100363531 A CN 2008100363531A CN 200810036353 A CN200810036353 A CN 200810036353A CN 101265085 B CN101265085 B CN 101265085B
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翟继卫
张景基
莫伟锋
丁西亚
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Tongji University
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Abstract

The invention belongs to the technology field of electronic materials and devices, and discloses a two-phase composite microwave ceramic material with adjustable dielectric property, Ba(1-x)SrxTiO3-MgAl2O4, and a production method thereof. The two-phase composite microwave ceramic material contains the following components according to mass percentage: 40.0-95.0 wt% of Ba(1-x)SrxTiO3 (x is in the range of 0.3-0.9) and 5.0-60.0 wt% of MgAl2O4. The inventive two-phase composite microwave ceramic material is characterized in adjustable dielectric property and low dielectric loss (high Q value) in microwave frequency band, and can be used for adjustable microwave devices.

Description

The Ba that dielectric is adjustable 1-xSr xTiO 3-MgAl 2O 4Two-phase composite microwave ceramic material and preparation method thereof
Technical field
The invention belongs to electronic material and device technology field, be specifically related to a kind of two-phase composite microwave ceramic material.
Background technology
Have high-k, low-dielectric loss, nonlinear dielectric constant is adjustable with and the adjustable calcium titanium ore structure Ba of Curie temperature 1-xSr xTiO 3Ferroelectric material aspect microwave adjustable device (like shifter, wave filter, VC and retarding line etc.) obtain increasingly extensive concern, especially aspect microwave phase shifter especially at present research focus.1994; American National military field engineering lab material L.C.Sengupta of portion and u.s.a. military affairs research laboratory microwave and the W.C.Drach of photoelectricity portion; In the report of survey of " strontium-barium titanate (BST) the shifter material electrology characteristic " submitted to mil, propose; Make shifter if the BST ferroelectric material can replace Ferrite Material, Phased Array Radar Antenna will face a huge revolution.But the BST stupalith with high-k is difficult to satisfy itself and the inner impedance matching of driving source, and it has bigger dielectric loss under microwave frequency band, this all big limitations its application in the microwave adjustable device field.Therefore, how to prepare both had moderate specific inductivity, low dielectric loss, the material that has high dielectric adjustable again is technological difficulties.
At present, most researchers mainly forms composite structure through adding non-ferroelectric microwave dielectric material, reduces dielectric loss under specific inductivity and the microwave frequency band thereby reach, and makes it can be used for microwave adjustable device.Sengupta etc. have carried out systematic research and have applied for related u. s. the compound of BST and non-ferroelectric material MgO; Though the specific inductivity of this matrix material and loss have obtained reduction to a certain extent; But along with the increase of MgO content, the temperature dependent properties of its specific inductivity and dielectric tunable characteristic but sharply descend.Dong Xianlin etc. are at BST stupalith and Mg 2SiO 4-MgO has also done certain research work in compound aspect, also is not well solved about specific inductivity and this contradiction of dielectric adjustable mutual restriction of BST material.This seminar is in early days at Ba 1-xSr xTiO 3-Mg 2TiO 4A few thing has been done in the composite ceramic material aspect, has obtained very big progress.Yet, Ba 1-xSr xTiO 3With MgAl with excellent microwave dielectric property 2O 4(ε r=8.75, Qf=68900GHz (loss tangent=0.00017 at 12.3GHz)) compound and Dielectric Properties is not seen relevant report as yet.
Summary of the invention
The purpose of this invention is to provide and a kind ofly have low-dielectric loss under dielectric tunable characteristic, the microwave frequency band (high Q value) and can be used for two-phase composite microwave ceramic material of adjustable microwave device and preparation method thereof.
The two-phase composite microwave ceramic material that dielectric provided by the present invention is adjustable comprises following component by mass percent:
Ba 1-xSr xTiO 3，x＝0.3-0.9 40.0wt.％～95.0wt.％
MgAl 2O 4 5.0wt.％～60.0wt.％
Preferable, above-mentioned Ba 1-xSr xTiO 3In, x preferred 0.6.
The preparation method of two-phase composite microwave ceramic material provided by the present invention specifically comprises the steps:
(1) adopt solid reaction process to prepare Ba 1-xSr xTiO 3(x=0.3-0.9), obtain Ba after the grinding 1-xSr xTiO 3(x=0.3-0.9) powder.Be specially:
Adopt traditional electronic ceramic powder preparation technology,, select BaTiO for use through solid reaction process 3And SrTiO 3Be main raw material,, confected materials placed nylon ball grinder according to certain Ba/Sr molar ratio ingredient; Add zirconia ball, add absolute ethyl alcohol or deionized water, ball milling 20～24 hours; Discharging oven dry back obtains Ba 1100 ℃～1250 ℃ pre-burnings 4～8 hours after the grinding 1-xSr xTiO 3(x=0.3-0.9) powder.
(2) adopt solid reaction process to prepare MgAl 2O 4, obtain MgAl after the grinding 2O 4Powder.
According to the synthetic MgAl of following reaction equation 2O 4Powder:
MgO+Al 2O 3＝MgAl 2O 4
At first take by weighing the MgO (98.50%) and the Al of certain mole proportioning 2O 3(99.99%) compound places nylon ball grinder, adds zirconia ball, adds absolute ethyl alcohol or deionized water, ball milling 20～24 hours, and discharging oven dry back obtains MgAl 1250 ℃～1450 ℃ pre-burnings 4～8 hours after the grinding 2O 4Powder.
(3) take by weighing compound according to following set of dispense ratio, add zirconia ball, add absolute ethyl 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-xSr xTiO 3(x=0.3-0.9) powder 95.0wt.%～40.0wt.%
MgAl 2O 4Powder 5.0wt.%～60.0wt.%
(4) Z 150PH (PVA) of employing 8～10% carries out granulation as sticker to above-mentioned composite powder, under 10～100MPa pressure, is pressed into the ceramic green sheet of desired size size through the forming mould of different model.
(5) the ceramic green sheet through 550 ℃～600 ℃ row is sticking handle after, the ceramic plate that obtains is carried out 1400 ℃～1600 ℃ (being incubated 2～4 hours) sintering processes, can obtain said composite microwave ceramic material.
Wherein the mass ratio of zirconia ball and ball milling material is 1.2～1.5; The mass ratio of absolute ethyl alcohol or deionized water and ball milling material is 1.5～3.0.
The ball milling material is meant the summation of ball milling main raw material, is BaTiO in step 1 3And SrTiO 3, be MgO and Al in the step 2 2O 3, be Ba in the step 3 1-xSr xTiO 3(x=0.3-0.9) powder and MgAl 2O 4Powder.
The present invention adopts traditional electronic ceramic technology, selects microwave dielectric material magnesium aluminate (MgAl for use 2O 4) to carry out two phase gradients compound with the strontium-barium titanate ferroelectric material of different B a/Sr component, development obtains a kind of Ba that has low-dielectric loss under dielectric tunable characteristic, the microwave frequency band (high Q value) and can be used for the adjustable microwave device 1-xSr xTiO 3-MgAl 2O 4Two-phase composite microwave ceramic material, it has following principal feature:
(1) Tc of this composite ceramic material system can require the structure and the performance of adjustment material system according to the working temperature of the adjustable microwave device that is designed with Ba/Sr than adjustable continuously in very wide scope;
(2) pass through Ba 1-xSr xTiO 3(x=0.3-0.9), MgAl 2O 4The variation of two phase plural components content, the specific inductivity of composite ceramic material can be adjustable continuously between 15～2000, 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, said composite microwave ceramic material has higher dielectric tunable characteristic (>=10%), and under microwave frequency band, has higher Q value (>=200);
(4) its composition of this composite ceramic material is with Ba 1-xSr xTiO 3(x=0.3-0.9) and MgAl 2O 4The pure compound existence of two phase forms 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 spinoff 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 (1-x) Ba 0.4Sr 0.6TiO 3-xMgAl 2O 4The X-ray diffraction analysis collection of illustrative plates of two-phase composite microwave ceramic material.
Fig. 2 is (1-x) Ba 0.4Sr 0.6TiO 3-xMgAl 2O 4The relation curve of the specific inductivity of two-phase composite microwave ceramic material and loss and temperature.
Fig. 3 is (1-x) Ba 0.4Sr 0.6TiO 3-xMgAl 2O 4The relation curve of the specific inductivity of two-phase composite microwave ceramic material and loss and external dc field intensity.
Embodiment
Embodiment 1-5 prepares (1-x) Ba 0.4Sr 0.6TiO 3-xMgAl 2O 4Two-phase composite microwave ceramic material:
According to Ba 0.4Sr 0.6TiO 3Stoichiometric ratio, take by weighing 93.291g BaTiO 3With 110.110g SrTiO 3(99.90%, 100nm, Shandong state porcelain ceramic material ltd provides) powder places nylon ball grinder; Add zirconia ball and absolute ethyl alcohol or deionized water; Ball milling 24 hours, discharging oven dry back obtains Ba 1100 ℃～1250 ℃ pre-burnings 4 hours after the grinding 0.4Sr 0.6TiO 3Powder is for use.In addition, take by weighing 10.228g MgO and 25.493g Al respectively 2O 3Powder places nylon ball grinder, adds zirconia ball and absolute ethyl alcohol or deionized water, ball milling 24 hours, and discharging oven dry back obtains MgAl 1250 ℃～1450 ℃ pre-burnings 4 hours after the grinding 2O 4Powder is for use.
Take by weighing above-mentioned synthetic Ba respectively according to plural components proportioning in the table 1 0.4Sr 0.6TiO 3, MgAl 2O 4Powder for use:
Table 1. (1-x) Ba 0.4Sr 0.6TiO 3-xMgAl 2O 4The two-phase composite microwave ceramic material proportioning
Figure S2008100363531D00041
The compound of above-mentioned each prescription is put into nylon ball grinder; Added zirconia ball and absolute ethyl alcohol ball milling 24 hours; Discharging oven dry back powder is crossed 200 mesh sieves, and according to traditional electronic ceramic technology, the Z 150PH (PVA) of employing 8% carries out granulation as sticker; Under 10MPa pressure, dry method is pressed into diameter
Figure S2008100363531D00042
The right cylinder of green sheet and 10mm * 5mm, 15mm * 7mm, 18mm * 9mm, 25mm * 12mm, after the sticking processing of 550 ℃ rows, sample is under air atmosphere, and sintering temperature is 1500 ℃, is incubated after 4 hours, obtains (1-x) Ba 0.4Sr 0.6TiO 3-xMgAl 2O 4The two-phase composite microwave ceramic sample.The ceramics sample that makes is carried out polishing both surfaces, quilt silver earlier, carry out analysis of thing phase composition and dielectric properties test behind the silver ink firing, its relevant dielectric properties are seen table 2.
Table 2. (1-x) Ba 0.4Sr 0.6TiO 3-xMgAl 2O 4The relevant dielectric properties of two-phase composite microwave ceramic material
Figure S2008100363531D00043
Embodiment 1 #-5 #Prepared (1-x) Ba fills a prescription 0.4Sr 0.6TiO 3-xMgAl 2O 4The X-ray diffraction analysis collection of illustrative plates of two-phase composite microwave ceramic material is as shown in Figure 1, and the result shows with Ba 0.4Sr 0.6TiO 3And MgAl 2O 4Pure two phase forms coexistence does not have other dephasigns to generate; Embodiment 1 #-5 #Prepared (1-x) Ba fills a prescription 0.4Sr 0.6TiO 3-xMgAl 2O 4The relation curve of the specific inductivity of two-phase composite microwave ceramic material and loss and temperature is as shown in Figure 2, and the result shows along with MgAl 2O 4The increase of content, Curie shifts at the peak high temperature and by broadening, inhibition; Embodiment 1 #-5 #Prepared (1-x) Ba fills a prescription 0.4Sr 0.6TiO 3-xMgAl 2O 4The relation curve of the specific inductivity of two-phase composite microwave ceramic material and loss and external dc field intensity is as shown in Figure 3, and test result shows that interpolation is along with MgAl 2O 4The increase of content, modulation increases.
Embodiment 6 preparation (1-x) Ba 0.7Sr 0.3TiO 3-xMgAl 2O 4Two-phase composite microwave ceramic material:
According to Ba 0.7Sr 0.3TiO 3Stoichiometric ratio, take by weighing 163.259g BaTiO 3With 55.055g SrTiO 3(99.90%, 100nm, Shandong state porcelain ceramic material ltd provides) powder places nylon ball grinder; Add zirconia ball and absolute ethyl alcohol or deionized water; Ball milling 24 hours, discharging oven dry back obtains Ba 1100 ℃～1250 ℃ pre-burnings 4 hours after the grinding 0.7Sr 0.3TiO 3Powder is for use.In addition, take by weighing 10.228g MgO and 25.493g Al respectively 2O 3Powder places nylon ball grinder, adds zirconia ball and absolute ethyl alcohol or deionized water, ball milling 24 hours, and discharging oven dry back obtains MgAl 1250 ℃～1450 ℃ pre-burnings 4 hours after the grinding 2O 4Powder is for use.
Take by weighing above-mentioned synthetic Ba respectively according to plural components proportioning in the table 3 0.7Sr 0.3TiO 3, MgAl 2O 4Powder for use:
Table 3. (1-x) Ba 0.7Sr 0.3TiO 3-xMgAl 2O 4The two-phase composite microwave ceramic material proportioning
Figure S2008100363531D00051
The compound of above-mentioned each prescription is put into nylon ball grinder; Added zirconia ball and absolute ethyl alcohol ball milling 24 hours; Discharging oven dry back powder is crossed 200 mesh sieves, and according to traditional electronic ceramic technology, the Z 150PH (PVA) of employing 8% carries out granulation as sticker; Under 10MPa pressure, dry method is pressed into diameter
Figure S2008100363531D00052
The right cylinder of green sheet and 10mm * 5mm, 15mm * 7mm, 18mm * 9mm, 25mm * 12mm, after the sticking processing of 550 ℃ rows, sample is under air atmosphere, and sintering temperature is 1500 ℃, is incubated after 4 hours, obtains (1-x) Ba 0.7Sr 0.3TiO 3-xMgAl 2O 4The two-phase composite microwave ceramic sample.
Embodiment 7 preparation (1-x) Ba 0.1Sr 0.9TiO 3-xMgAl 2O 4Two-phase composite microwave ceramic material:
According to Ba 0.1Sr 0.9TiO 3Stoichiometric ratio, take by weighing 23.323g BaTiO 3With 167.865g SrTiO 3(99.90%, 100nm, Shandong state porcelain ceramic material ltd provides) powder places nylon ball grinder; Add zirconia ball and absolute ethyl alcohol or deionized water; Ball milling 24 hours, discharging oven dry back obtains Ba 1100 ℃～1250 ℃ pre-burnings 4 hours after the grinding 0.1Sr 0.9TiO 3Powder is for use.In addition, take by weighing 10.228g MgO and 25.493g Al respectively 2O 3Powder places nylon ball grinder, adds zirconia ball and absolute ethyl alcohol or deionized water, ball milling 24 hours, and discharging oven dry back obtains MgAl 1250 ℃～1450 ℃ pre-burnings 4 hours after the grinding 2O 4Powder is for use.
Take by weighing above-mentioned synthetic Ba respectively according to plural components proportioning in the table 4 0.1Sr 0.9TiO 3, MgAl 2O 4Powder for use:
Table 4. (1-x) Ba 0.1Sr 0.9TiO 3-xMgAl 2O 4The two-phase composite microwave ceramic material proportioning
The compound of above-mentioned each prescription is put into nylon ball grinder; Added zirconia ball and absolute ethyl alcohol ball milling 24 hours; Discharging oven dry back powder is crossed 200 mesh sieves, and according to traditional electronic ceramic technology, the Z 150PH (PVA) of employing 8% carries out granulation as sticker; Under 10MPa pressure, dry method is pressed into diameter
Figure S2008100363531D00062
The right cylinder of green sheet and 10mm * 5mm, 15mm * 7mm, 18mm * 9mm, 25mm * 12mm, after the sticking processing of 550 ℃ rows, sample is under air atmosphere, and sintering temperature is 1500 ℃, is incubated after 4 hours, obtains (1-x) Ba 0.1Sr 0.9TiO 3-xMgAl 2O 4The two-phase composite microwave ceramic sample.The ceramics sample that makes is carried out polishing both surfaces, quilt silver earlier, carry out analysis of thing phase composition and dielectric properties test behind the silver ink firing.

Claims (8)

1. two-phase composite microwave ceramic material that dielectric is adjustable, form by following component by mass percent:
Ba 1-xSr xTiO 3，x＝0.3-0.9 40.0wt.％～95.0wt.％
MgAl 2O 4 5.0wt.％～60.0wt.％。
2. the adjustable two-phase composite microwave ceramic material of dielectric according to claim 1 is characterized in that said Ba 1-xSr xTiO 3In, x is 0.6.
3. the preparation method of the adjustable two-phase composite microwave ceramic material of the said dielectric of claim 1 comprises the steps:
A) adopt solid reaction process to prepare Ba 1-xSr xTiO 3Powder, wherein x=0.3-0.9;
B) adopt solid reaction process to prepare MgAl 2O 4Powder;
C) take by weighing the Ba that step a makes 1-xSr xTiO 3The MgAl that powder and b make 2O 4Powder adds zirconia ball, adds absolute ethyl alcohol or deionized water, and ball milling 20～24 hours obtains composite powder after the discharging oven dry, wherein, and Ba 1-xSr xTiO 3Powder and MgAl 2O 4Powder compares according to following set of dispense:
Ba 1-xSr xTiO 3Powder, x=0.3-0.9 95.0wt.%～40.0wt.%
MgAl 2O 4Powder 5.0wt.%～60.0wt.%;
D) Z 150PH of employing 8～10% carries out granulation as sticker to the composite powder that step c obtains, and under 10～100MPa pressure, is pressed into the ceramic green sheet through forming mould;
E) after the ceramic green sheet glues processing through row, carry out sintering processes, can obtain the adjustable two-phase composite microwave ceramic material of said dielectric.
4. like the preparation method of the adjustable two-phase composite microwave ceramic material of the said dielectric of claim 3, it is characterized in that among the said step c, the mass ratio of zirconia ball and ball milling material is 1.2～1.5, wherein the ball milling material is meant Ba 1-xSr xTiO 3Powder and MgAl 2O 4Powder.
5. like the preparation method of the adjustable two-phase composite microwave ceramic material of the said dielectric of claim 3, it is characterized in that among the said step c, the mass ratio of absolute ethyl alcohol or deionized water and ball milling material is 1.5～3.0, wherein the ball milling material is meant Ba 1-xSr xTiO 3Powder and MgAl 2O 4Powder.
6. like the preparation method of the adjustable two-phase composite microwave ceramic material of the said dielectric of claim 3, it is characterized in that the said solid reaction process of step a prepares Ba 1-xSr xTiO 3Powder comprises the steps:
Select BaTiO for use 3And SrTiO 3Be raw material, according to Ba 1-xSr xTiO 3The molar ratio ingredient of middle Ba/Sr places ball grinder with confected materials, adds zirconia ball, adds absolute ethyl alcohol or deionized water, ball milling 20～24 hours, and discharging oven dry back obtains Ba 1100 ℃～1250 ℃ pre-burnings 4～8 hours after the grinding 1-xSr xTiO 3Powder.
7. like the preparation method of the adjustable two-phase composite microwave ceramic material of the said dielectric of claim 3, it is characterized in that the said solid reaction process of step b prepares MgAl 2O 4Powder comprises the following steps:
Select MgO and Al for use 2O 3Be raw material, take by weighing MgO and Al 2O 3Compound places ball grinder, adds zirconia ball, adds absolute ethyl alcohol or deionized water, ball milling 20～24 hours, and discharging oven dry back obtains MgAl 1250 ℃～1450 ℃ pre-burnings 4～8 hours after the grinding 2O 4Powder.
8. like the preparation method of the adjustable two-phase composite microwave ceramic material of the said dielectric of arbitrary claim among the claim 3-7, it is characterized in that said Ba 1-xSr xTiO 3In, x is 0.6.
CN2008100363531A 2008-04-21 2008-04-21 Dielectric adjustable Ba[1-x]SrxTiO3-MgAl2O4 diphase composite microwave ceramic material and preparation method thereof Expired - Fee Related CN101265085B (en)

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