CN103708825A - High-tuning low-loss barium strontium titanate-zinc aluminate composite material and preparation method thereof - Google Patents

High-tuning low-loss barium strontium titanate-zinc aluminate composite material and preparation method thereof Download PDF

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Publication number
CN103708825A
CN103708825A CN201310703545.4A CN201310703545A CN103708825A CN 103708825 A CN103708825 A CN 103708825A CN 201310703545 A CN201310703545 A CN 201310703545A CN 103708825 A CN103708825 A CN 103708825A
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loss
matrix material
zinc aluminate
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梁瑞虹
董显林
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Shanghai Institute of Ceramics of CAS
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Shanghai Institute of Ceramics of CAS
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Abstract

The invention relates to a high-tuning low-loss barium strontium titanate-zinc aluminate composite material and a preparation method thereof. The chemical composition of the composite material is (1-y)Ba1-xSrxTiO3+yZnAl2O4, wherein x is more than or equal to 0.35 and less than or equal to 0.70, and y is more than or equal to 5wt% and less than or equal to 20.0wt%. The high-tuning low-loss barium strontium titanate-zinc aluminate composite material provided by the invention is compounded from barium strontium titanate (with a suitable Ba/Sr ratio) and the zinc aluminate at a suitable ratio, so that the material adjustability is greatly improved; furthermore, a dielectric constant and a dielectric loss of the material are reduced, and the high-adjustability (high-tuning) low-loss composite material can be obtained and can meet property requirements when being used a material of a phase shifter.

Description

High tuning low-loss strontium-barium titanate-Zinc aluminate matrix material and preparation method thereof
Technical field
The present invention relates to a kind of strontium-barium titanate-Zinc aluminate (Ba 1-xsr xtiO 3/ ZnAl 2o 4) matrix material and preparation method thereof, belong to electrooptical material technical field, particularly phased array phase shifter Material Field.
Background technology
Phase shifter is the core component of phased array radar.Material as phase shifter is mainly ferrite and PIN diode at present, but they exist some larger shortcomings, for example: ferrite phase shifter (1) peak power is large, and transmission speed is restricted; (2) temperature-compensation circuit unavoidably causes the error in pointing of phased array antenna; (3) it is bulky that control circuit, compensating circuit not only make phase shifter itself, and cause phased array antenna reliability to reduce; (4) complex manufacturing technology, production cost is higher.PIN diode phase shifter is more cheap than ferrite phase shifter, but high insertion loss has limited its application.Therefore, ferrite phase shifter and PIN diode phase shifter are all difficult to meet the requirement of modern military technology to lightweight, miniaturization, high reliability and the high band of phased array antenna proposition of new generation.
The focus of phase shifter investigation of materials is in recent years to replace ferrite with ferroelectric material, this is that specific inductivity due to ferroelectric material can change under the effect of bias direct current electric field, cause that the phase place that sees through this material microwave changes, to reach the object of phased array radar.Twentieth century end of the nineties, the people such as US Naval Research Laboratory (NRL) J.L.Rao propose the thought of ferroelectric formula lens phase array system, adopt monoblock type phase-shifting unit, can effectively reduce phase shifter, the quantity of driving mechanism and controller (becomes m+n by original m * n, m wherein, n is respectively columns and the line number of phased array), the personnel of United States Army research laboratory did a statistics, use ferrite to prepare the radar array of Unit 1000, approximately 5,000,000 dollars of required expenses, and adopt ferroelectric material to replace ferrite, only need 200,000 dollars, material cost is only original 1/25.Volume is tending towards miniaturization and can integrated level be improved simultaneously, can make phased array radar be more convenient in airborne and On-Board System application.Ferroelectric material for phase shifter must have following performance:
(1) low specific inductivity: be conducive to the impedance matching of realization and circuit;
(2) low microwave dielectric loss: can reduce insertion loss, reduce the loss of energy in material;
(3) high adjustability: adjustability is to weigh the specific inductivity of ferroelectric material with the degree changing under bias field effect, can the be defined as: (DIELECTRIC CONSTANT ε of added electric field not 0dIELECTRIC CONSTANT ε under-bias field appthe DIELECTRIC CONSTANT ε of the added electric field of)/not 0.The ability that phase shifter changes phasing degree is mainly decided by adjustability, so high adjustability is very important for phase shifter material;
(4) good temperature stability: temperature stability can be used TCP ppmrepresent:
TCP ppm=(ε max-ε ref)/ε ref(T max-T ref)
ε max: specific inductivity maximum value within the scope of associated temperature;
ε ref: the specific inductivity of a certain reference point;
T max: the residing temperature of specific inductivity maximum value;
T ref: the temperature of reference point;
TCP ppmlower, temperature stability can be higher.The material that temperature stability is good can be applied to high Jie's substrate material, and can make the working temperature of material broaden;
(5) low Curie temperature: the Curie temperature of ferroelectric material refers to that material transfers the temperature of paraelectric state to from ferroelectric state.Low Curie temperature makes material in operating temperature range, can not occur to change mutually, also just without use heat protection in circuit.
The ferroelectric material for phase shifter (being also referred to as electrooptical material) of most study is strontium-barium titanate (BSTO) material at present.First it proposed in one piece of " Planar Microwave Electro-Optic Phase Shifter " article by name publishing in " Microwave Jounal " magazine in June, 1992 by people such as Richard W.Babbitt.But because BSTO material has high specific inductivity, high lossy microwave, thus need further material to be optimized, to meet the application requiring of phase shifter.The people such as United States Army laboratory Louise have improved BSTO and the compound Ferroelectric Composites obtaining of some metal oxide the performance of material greatly.Such as U.S. Patent No. 5,312, the BSTO-Al describing in 790 2o 3matrix material, U.S. Patent No. 5,486, the BSTO-ZrO describing in 491 2matrix material, U.S. Patent No. 5,635, BSTO-ZnO matrix material of describing in 433 etc.Wherein, U.S. Patent No. 5,645, the BSTO-MgO composite property of describing in 434 is best, has lower specific inductivity and lossy microwave.On this basis, the people such as Chiu have carried out again the modification of rare earth element to BSTO-MgO matrix material, and result is published in U.S. Patent No. 6,074, in 971.But at present the adjustability of material is still lower, such as U.S. Patent No. 6,074, the Ba describing in 971 0.55sr 0.45tiO 3-MgO matrix material only has 6.57% under electric field 2V/ μ m, and the adjustability of having added the matrix material of rare earth element is also no more than 8%, and this further carries out modification to material with regard to needs, to improve its adjustability.The BSTO-Mg being proposed by people such as Chiu equally 2siO 4material has just improved the specific inductivity adjustability of material greatly, be published in U.S. Patent No. 6,514, in 895B1, but the specific inductivity of material and microwave dielectric loss also increase thereupon, under 10GHz, the lossy microwave >0.02 of material, so be necessary material to carry out further exploratory development to optimize material property.
Summary of the invention
Problem in the face of prior art exists, the object of this invention is to provide a kind of preparation technology simple, fills a prescription adjustable, has strontium-barium titanate-Zinc aluminate matrix material of low-dielectric loss, high adjustability, to meet the application requiring of phase shifter material.
At this, on the one hand, the invention provides a kind of high tuning low-loss strontium-barium titanate-Zinc aluminate matrix material, the chemical constitution of described matrix material is: (1-y) Ba 1-xsr xtiO 3+ y ZnAl 2o 4, 0.35≤x≤0.70 wherein, 5wt%≤y≤20.0wt%.Preferably, 10wt%≤y≤20.0wt%.
In the present invention, described matrix material specific inductivity under bias field 2.0kV/mm has 40～50% adjustability.
In the present invention, the dielectric loss of described matrix material is below 0.006.
The present invention is compound in suitable ratio to have strontium-barium titanate and the Zinc aluminate of suitable Ba/Sr ratio, greatly improved the adjustability of material, and material dielectric constant and dielectric loss are all reduced, obtain the low-loss matrix material of high adjustability (high tuning), can meet the performance requriements as phase shifter material.
On the other hand, the present invention also provides the preparation method of above-mentioned high tuning low-loss strontium-barium titanate-Zinc aluminate matrix material, comprising: by Ba 1-xsr xtiO 3powder and ZnAl 2o 4powder than mixing, makes described high tuning low-loss strontium-barium titanate-Zinc aluminate matrix material through wet ball grinding, oven dry, granulation, compression moulding, binder removal and sealed sintering by chemical constitution.
Preferably, in described wet ball grinding, the mass ratio of powder, ball-milling medium, water is 1:(1.5～2): (0.8～1), Ball-milling Time is 24～48 hours, described ball-milling medium is agate ball.
Preferably, the temperature of described binder removal is 650 ℃～800 ℃, and soaking time is 1～2 hour, and the heat-up rate of binder removal process is not higher than 3 ℃/h.By described binder removal, can get rid of the organic substance in biscuit.
Preferably, described sealed sintering be under air-proof condition in 1400 ℃～1450 ℃ insulations 2～4 hours, and in sinter surrounding, place Zinc aluminate grog in sintering process.By place Zinc aluminate grog in sinter surrounding in sintering process, can place Zinc aluminate volatilization.
Preferably, described Ba 1-xsr xtiO 3powder can be prepared by the following method: with pulverous BaCO 3, SrCO 3, TiO 2for raw material, by stoichiometric ratio proportioning, wet ball grinding 20～30 hours, pre-burning at 1100 ℃～1180 ℃ after discharging oven dry, is incubated 1～3 hour, obtains Ba 1-xsr xtiO 3powder.
Preferably, described ZnAl 2o 4powder can be prepared by the following method: with Powdered Al 2o 3with ZnO be raw material, according to stoichiometric ratio proportioning, wet ball grinding 12～24 hours, discharging dry after pre-burning at 1200 ℃～1250 ℃, be incubated 2～3 hours, obtain ZnAl 2o 4powder.
The present invention mainly selects suitable preparation technology by employing, suitable Ba/Sr ratio and appropriate BST and ZnAl 2o 4carry out compoundly, result shows ZnAl 2o 4the compound adjustability that greatly improves material, and material dielectric constant and dielectric loss are all reduced. the invention has the advantages that and adopt material compositing formula of the present invention and preparation technology can successfully obtain high adjustability matrix material.
Embodiment
Below provide embodiment and further illustrate the present invention, should be understood that following embodiment is only for the present invention is described, and unrestricted the present invention.
One aspect of the present invention provides a kind of high tuning low-loss strontium-barium titanate-Zinc aluminate matrix material, and the chemical constitution of described matrix material is: (1-y) Ba 1-xsr xtiO 3+ y ZnAl 2o 4, 0.35≤x≤0.70 wherein, 5wt%≤y≤20.0wt%.Preferably, 10wt%≤y≤20.0wt%.This matrix material specific inductivity under bias field 2.0kV/mm has 40～50% adjustability.Again, the dielectric loss of this matrix material is below 0.006.Therefore, strontium-barium titanate-Zinc aluminate composite-material formula of the present invention is adjustable, has low-dielectric loss, high adjustability, especially can meet the application requiring of phase shifter material.
As example, the preparation method of above-mentioned high tuning low-loss strontium-barium titanate-Zinc aluminate matrix material can comprise the following steps.
(1) with pulverous BaCO 3, SrCO 3, TiO 2for raw material, by stoichiometric ratio proportioning, wet ball grinding, rear pre-burning is dried in discharging, obtains Ba 1-xsr xtiO 3(BST) powder.Wherein, the processing condition of wet ball grinding can be: the mass ratio of powder, ball-milling medium, water is 1:(1.5～2): (0.8～1), Ball-milling Time is 20～30 hours, ball-milling medium is agate ball.The processing condition of pre-burning can be: at 1100 ℃～1180 ℃, be incubated 1～3 hour.
(2) with Powdered Al 2o 3with ZnO be raw material, according to stoichiometric ratio proportioning, wet ball grinding, discharging dry after pre-burning, obtain ZnAl 2o 4powder.Wherein, the processing condition of wet ball grinding can be: the mass ratio of powder, ball-milling medium, water is 1:(1.5～2): (0.8～1), Ball-milling Time is 12～24 hours, ball-milling medium is agate ball.The processing condition of pre-burning can be: at 1200 ℃～1250 ℃, be incubated 2～3 hours.
(3) according to forming design, by the ZnAl of BST powder and different amounts 2o 4sphere of powder body mixing wet ball grinding, oven dry, granulation, compression moulding.Wherein, the processing condition of wet ball grinding can be: the mass ratio of ball-milling medium, water is 1:(1.5～2): (0.8～1), ball-milling medium is agate, Ball-milling Time is 24～48 hours.Bake out temperature can be between 80～100 ℃.During granulation, can add 7wt%PVA.The pressure of compression moulding can be 100MPa.
(4) binder removal in 650 ℃～800 ℃ temperature ranges, is incubated 1～2 hour, gets rid of the organic substance in biscuit.The heat-up rate of binder removal process is preferably not higher than 3 ℃/h.
(5) sintering in 1400 ℃～1450 ℃ temperature ranges, is incubated and within 2～4 hours, makes strontium-barium titanate-Zinc aluminate matrix material.During sintering, must be sealed sintering, in order to prevent Zinc aluminate volatilization, can place appropriate Zinc aluminate grog in sample surrounding simultaneously.
Dielectric properties test:
Strontium-barium titanate-Zinc aluminate matrix material after burning till is processed through fine grinding, after ultrasonic cleaning, by silver electrode, for dielectric properties, tests.Known after tested, strontium-barium titanate-Zinc aluminate matrix material of the present invention specific inductivity under bias field 2.0kV/mm has 40～50% adjustability.Again, dielectric loss is below 0.006.
Compared with prior art, the present invention has following beneficial effect:
The present invention mainly selects suitable preparation technology by employing, suitable Ba/Sr ratio and appropriate BST and ZnAl 2o 4carry out compoundly, result shows ZnAl 2o 4the compound adjustability that greatly improves material, and material dielectric constant and dielectric loss are all reduced. the invention has the advantages that and adopt material compositing formula of the present invention and preparation technology can successfully obtain high adjustability matrix material, can be used as phase shifter material.
Further exemplify embodiment below to describe the present invention in detail.Should understand equally; following examples are only used to further illustrate the present invention; can not be interpreted as limiting the scope of the invention, some nonessential improvement that those skilled in the art's foregoing according to the present invention is made and adjustment all belong to protection scope of the present invention.The processing parameter that following example is concrete etc. is only also an example in OK range, and those skilled in the art can be done in suitable scope and be selected by explanation herein, and do not really want to be defined in the below concrete numerical value of example.
Embodiment 1
With pulverous BaCO 3, SrCO 3, TiO 2for raw material, by stoichiometric ratio proportioning, wet ball grinding 24h, pre-burning at 1150 ℃ after discharging oven dry, insulation 2h, obtains Ba 1-xsr xtiO 3(x=0.45) powder;
With Powdered Al 2o 3with ZnO be raw material, according to stoichiometric ratio proportioning, wet ball grinding 12h, discharging dry after pre-burning at 1200 ℃, insulation 3h, obtains ZnAl 2o 4powder;
By Ba 1-xsr xtiO 3(x=0.45) powder and ZnAl 2o 4powder is according to (1-y) Ba 1-xsr xtiO 3+ y ZnAl 2o 4(x=0.45, y=10wt%) proportioning, after wet ball grinding 24h, discharging, dries, briquetting, then add 7wt%PVA granulating and forming, under the pressure of 100MPa by pressed by powder moulding; Binder removal in 650 ℃ of temperature ranges, insulation 1-2 hour, gets rid of the organic substance in biscuit, and the heat-up rate of binder removal process is not higher than 3 ℃/h; At 1420 ℃ of sintering, insulation 3h.Sample after burning till is processed through fine grinding, after ultrasonic cleaning, by silver electrode, for dielectric properties, tests.Component described in the present embodiment is carried out to performance test, and electric property is in Table 1.
Embodiment 2
According to (1-y) Ba 1-xsr xtiO 3+ y ZnAl 2o 4(x=0.45, y=15wt%) proportioning, concrete technology route is identical with embodiment 1, BST and ZnAl 2o 4mix dry-pressing formed after, binder removals in 650 ℃ of temperature ranges. insulation 1-2 hour, at 1440 ℃ of sintering, insulation 3h.Described in the present embodiment, component electric property is in Table 1.
Embodiment 3
According to (1-y) Ba 1-xsr xtiO 3+ y ZnAl 2o 4(x=0.45, y=20wt%) proportioning, concrete technology route is identical with embodiment 1, BST and ZnAl 2o 4mix dry-pressing formed after, binder removals in 650 ℃ of temperature ranges. insulation 1-2 hour, at 1440 ℃ of sintering, insulation 3h.Described in the present embodiment, component electric property is in Table 1.
Comparative example 1
With pulverous BaCO 3, SrCO 3, TiO 2for raw material, by stoichiometric ratio proportioning, wet ball grinding 24h, pre-burning at 1150 ℃ after discharging oven dry, insulation 2h, obtains Ba 1-xsr xtiO 3(x=0.45) powder.This comparative example gained Ba 1- xsr xtiO 3(x=0.45) powder electric property is in Table 1.
(1-y) Ba of table 1 different composite amount 0.55sr 0.45tiO 3+ y ZnAl 2o 4the electric property of matrix material
From above result, strontium-barium titanate-Zinc aluminate matrix material of the present invention is compared to the strontium-barium titanate of compound Zinc aluminate not, and adjustability significantly improves, and dielectric loss significantly reduces.For example, at (1-y) Ba 1-xsr xtiO 3+ y ZnAl 2o 4in the situation of (x=0.45, y=20wt%), adjustability is up to 46.4%, and dielectric loss is only 0.0056, and specific inductivity is only 2362.Therefore, strontium-barium titanate-Zinc aluminate matrix material of the present invention meets the performance requriements for phase shifter, can be used as phase shifter material.
Industrial applicability: strontium-barium titanate-Zinc aluminate matrix material of the present invention specific inductivity under bias field 2.0kV/mm has 40～50% adjustability, dielectric loss is below 0.006, be the low-loss ferroelectric material of a kind of high tuning, can be applied to the fields such as phase shifter.And preparation method's technique of the present invention is simple, the cycle is short, cost is low, is applicable to large-scale production, can meet the needs of practical application.

Claims (10)

1. high tuning low-loss strontium-barium titanate-Zinc aluminate matrix material, is characterized in that, the chemical constitution of described matrix material is: (1-y) Ba 1-xsr xtiO 3+ y ZnAl 2o 4, 0.35≤x≤0.70 wherein, 5wt%≤y≤20.0wt%.
2. high tuning low-loss strontium-barium titanate-Zinc aluminate matrix material according to claim 1, is characterized in that 10wt%≤y≤20.0wt%.
3. high tuning low-loss strontium-barium titanate-Zinc aluminate matrix material according to claim 1 and 2, is characterized in that, described matrix material specific inductivity under bias field 2.0kV/mm has 40～50% adjustability.
4. according to the high tuning low-loss strontium-barium titanate-Zinc aluminate matrix material described in any one in claims 1 to 3, it is characterized in that, the dielectric loss of described matrix material is below 0.006.
5. a preparation method for the high tuning low-loss strontium-barium titanate-Zinc aluminate matrix material described in any one in claim 1 to 4, is characterized in that, comprising: by Ba 1-xsr xtiO 3powder and ZnAl 2o 4powder than mixing, makes described high tuning low-loss strontium-barium titanate-Zinc aluminate matrix material through wet ball grinding, oven dry, granulation, compression moulding, binder removal and sealed sintering by chemical constitution.
6. preparation method according to claim 5, is characterized in that, in described wet ball grinding, the mass ratio of powder, ball-milling medium, water is 1:(1.5～2): (0.8～1), Ball-milling Time is 24～48 hours, described ball-milling medium is agate ball.
7. according to the preparation method described in claim 5 or 6, it is characterized in that, the temperature of described binder removal is 650 ℃～800 ℃, and soaking time is 1～2 hour, and the heat-up rate of binder removal process is not higher than 3 ℃/h.
8. according to the preparation method described in any one in claim 5 to 7, it is characterized in that, described sealed sintering be under air-proof condition in 1400 ℃～1450 ℃ insulations 2～4 hours, and in sinter surrounding, place Zinc aluminate grog in sintering process.
9. according to the preparation method described in any one in claim 5 to 8, it is characterized in that, also comprise described Ba 1-xsr xtiO 3the preparation process of powder: with pulverous BaCO 3, SrCO 3, TiO 2for raw material, by stoichiometric ratio proportioning, wet ball grinding 20～30 hours, pre-burning at 1100 ℃～1180 ℃ after discharging oven dry, is incubated 1～3 hour, obtains Ba 1-xsr xtiO 3powder.
10. according to the preparation method described in any one in claim 5 to 9, it is characterized in that, also comprise described ZnAl 2o 4the preparation process of powder: with Powdered Al 2o 3with ZnO be raw material, according to stoichiometric ratio proportioning, wet ball grinding 12～24 hours, discharging dry after pre-burning at 1200 ℃～1250 ℃, be incubated 2～3 hours, obtain ZnAl 2o 4powder.
CN201310703545.4A 2013-12-19 2013-12-19 High-tuning low-loss barium strontium titanate-zinc aluminate composite material and preparation method thereof Pending CN103708825A (en)

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CN110386816A (en) * 2019-07-23 2019-10-29 山东理工大学 A kind of high adjustable compound gallic acid zinc ceramic material of rate low-loss barium strontium titanate
CN110386815A (en) * 2019-07-23 2019-10-29 山东理工大学 A kind of compound zinc aluminate ceramic material of barium strontium titanate that can be practical with higher adjustable rate low-loss

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Application publication date: 20140409