CN102358930B - Low-loss high-dielectric adjustable titanic acid strontium barium substrate ceramic material and preparation method thereof - Google Patents
Low-loss high-dielectric adjustable titanic acid strontium barium substrate ceramic material and preparation method thereof Download PDFInfo
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Abstract
The utility model belongs to the technical field of electronic materials devices and in particular relates to a low-loss high-dielectric adjustable titanic acid strontium barium ceramic material and a preparation method thereof. The dielectric adjustable titanic acid strontium barium substrate ceramic material is in a single phase cube perovskite structure. The material comprises ingredients with following mass percentage of BaxSr1 to xTiO3 (x = 0.3 to 0.8) of 50 wt. % to 99.9 wt. % and ferrum (Fe) powder of 0.1 wt. % to 50 wt. %. The ferrum powder is added into the titanic acid strontium barium substrate ceramic material of different Ba/Sr ingredients. Thus, the low-loss high-dielectric adjustable titanic acid strontium barium substrate ceramic material is developed and obtained, and the ceramic material can be applied to adjustable parts and especially suitable for materials of microwave medium ceramic ferroelectric phase shifting devices of adjustable microwave parts.
Description
Technical field
The invention belongs to electronic material and device technology field, relate to a kind of low-loss, high adjustable dielectric barium strontium titanate stupalith and preparation method thereof, relate in particular to a kind of low-loss that has, specific inductivity changes greatly with applying direct current electric field, is suitable for the microwave-medium ceramics ferroelectric phase shifter material of adjustable microwave device.
Background technology
Ba
xSr
1-xTiO
3(BST) be BaTiO
3And SrTiO
3Unlimited Solid solution, potential using value is arranged, such as the little and capacious miniature capacitor of volume, tuning microwave device, ferroelectric phase shifter etc. in adjustable device.Barium strontium titanate material is generally considered the most promising ferroelectric phase shift material, aspect microwave adjustable device (such 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.1994, the American National military field engineering lab material L.C.Sengupta of section and u.s.a. military affairs research laboratory microwave and the W.C.Drach of photoelectricity section, in the report of survey of " strontium-barium titanate (BST) the phase shifter material electrology characteristic " submitted to mil, propose, make phase shifter if the BST ferroelectric material can replace Ferrite Material, Phased Array Radar Antenna will face a huge revolution.Yet the BST stupalith with high-k is difficult to application requiring satisfied and driving source internal impedance match and high-power component, and this has limited its application in the microwave adjustable device field greatly.
For solving above-mentioned technological difficulties, many investigators are the mode by ion doping mainly, so that dopant ion enters in the crystalline network of material, cause the change of material microstructure, effectively adjust and improve the correlated performance of material, reduce dielectric loss under specific inductivity and the microwave frequency band thereby reach, make it can be used for microwave adjustable device.Sengupta etc. are to the research of mixing of BST and various oxide compound, such as MgO, AI
2O
3, La
2O
3Deng, the result shows the dielectric loss that has reduced to a certain extent material that is added in of these oxide compounds, and has certain adjustable rate.Wherein the robot system such as Herner has been studied stoichiometric ratio and has been mixed 0.01mol%Bi
2O
3, Fe
2O
3, MnO
2BST pottery, contrast shows Fe
2O
3Adding significantly reduced dielectric loss and specific inductivity, yet the temperature dependent properties of specific inductivity and dielectric tunable characteristic but sharply descend.This seminar is carrying out MnCO in early days
3Doping Ba
0.4Sr
0.6TiO
3In the research, obtained low-loss microwave ceramic material, made great progress seeking to have low loss under the microwave condition.
This patent is chosen the Fe powder and is entered into the BST matrix as hotchpotch, relies on Fe simple substance at high temperature to be oxidized to the ion of different valence state, thereby can remedy the oxide compound (Fe of single valence iron
2O
3, Fe
3O
4) unfavorable factor of mixing, realize low-loss, low-k, high adjustable requirement.By literature search, up to the present not yet find to adopt the Fe powder that BST is mixed and the relevant report of dielectric properties aspect, also do not have the patent that duplicates with the present invention.
Summary of the invention
The purpose of this invention is to provide and a kind ofly have specific inductivity and increase with the Fe add-on and reduce gradually, maintain simultaneously certain adjustable rate, this system has low loss under microwave frequency band, and can be used as adjustable microwave media ceramic ferroelectric phase shifter material.
To achieve these goals, the present invention adopts following technical scheme to realize:
The barium-strontium titanate-based microwave ceramic material that a kind of dielectric is adjustable, its structure are single-phase cubic perovskite structure, and described barium-strontium titanate-based microwave ceramic material comprises the feed composition of following mass percent:
Ba
xSr
1-xTiO
3(x＝0.3～0.8) 50wt.％～99.9wt.％；
Fe powder 0.1wt.%～50wt.%.
Preferably, described x=0.4.
Preferably, the mass percent of described Fe powder is 0.1wt.%～15wt.%.
The barium-strontium titanate-based microwave ceramic material that dielectric of the present invention is adjustable is Ba
xSr
1-xTiO
3(x=0.3～0.8) powder and Fe powder are composited.The present invention adds the Fe powder to the strontium-barium titanate microwave ceramic material and obtains the adjustable barium-strontium titanate-based microwave ceramic material of dielectric through electronic ceramic technology.
The preparation method of the barium-strontium titanate-based microwave ceramic material that dielectric of the present invention is adjustable comprises the steps:
(1) Ba
xSr
1-xTiO
3The preparation of (x=0.3～0.8) powder:
According to Ba
xSr
1-xTiO
3The stoichiometric ratio of middle Ba and Sr element takes by weighing main raw material BaTiO
3And SrTiO
3, with BaTiO
3And SrTiO
3Mixing and ball milling 20～24 hours is carried out pre-burning after the discharging oven dry under 1100 ℃～1200 ℃, obtain described Ba after grinding
xSr
1-xTiO
3(x=0.3～0.8) powder.
Better, described BaTiO
3And SrTiO
3Purity be 99.90%, come from Shandong state porcelain ceramic material company limited.
Better, during described ball milling, the mass ratio of the zirconia ball of adding and ball milling material is (1.2～1.5): 1; The dehydrated alcohol that adds or the mass ratio of deionized water and ball milling material are (1.5～3.0): 1.Raw material can be placed nylon ball grinder carry out during described ball milling.
Better, the time of described pre-burning is 1-4 hour, is preferably 4 hours.
Ba of the present invention
xSr
1-xTiO
3Traditional electronic ceramic powder preparation technology is adopted in the preparation of (x=0.3～0.8) powder, makes by solid reaction process.
(2) according to Ba
xSr
1-xTiO
3Take by weighing the Ba that step (1) obtains with the proportioning of Fe powder
xSr
1-xTiO
3Powder and Fe powder, ball milling and discharging oven dry, rear acquisition powder sieves.
The purity that Fe powder of the present invention can select AlfaAesar company to produce is 95% Fe powder.
Better, added zirconia ball and dehydrated alcohol or deionized water ball milling during described ball milling 20～24 hours; Wherein, 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.
Preferably, described sieve number of sieving is 200 orders.
(3) adopt binding agent that the powder that step (2) is obtained is carried out granulation, then compression moulding under 10～100MPa pressure obtains ceramic green.
Better, described binding agent is 8～10% polyvinyl alcohol (PVA) aqueous solution.
Ceramic green of the present invention can be pressed into by forming mould the block of desired size size.
(4) after ceramic green glues processing through row, 1320 ℃～1440 ℃ lower insulations 2～4 hours, obtain the adjustable barium-strontium titanate-based microwave ceramic material of described dielectric.
Better, the temperature that described row glues is 500 ℃-550 ℃, soaking time is 5h.
Above-mentioned steps (2)-(4) can the success add the Fe powder to Ba
1-xSr
xTiO
3In (x=0.3～0.8).
The present invention adopts traditional electronic ceramic technology, select the Fe powder to add in the strontium-barium titanate ferroelectric material of different B a/Sr component, development obtains a kind of low-loss that has, high dielectric tunable characteristic, and the stupalith that can be used for adjustable device especially is suitable as the microwave-medium ceramics ferroelectric phase shifter material of adjustable microwave device.
The barium-strontium titanate-based microwave ceramic material that dielectric of the present invention is adjustable has following principal feature:
(1) adds Ba in the mode of Fe powder
1-xSr
xTiO
3In (x=0.3～0.8), there is not the generation of other dephasign.
(2) when the addition of iron powder between 0.1～1wt%, the Curie temperature after it is compound changes less, the adjustable rate of dielectric does not reduce rapidly, and is suitable with the adjustability of pure BST; When the addition of iron powder during greater than 1wt%, Curie temperature moves to the low temperature direction, and its adjustable rate still keeps within the specific limits;
(3) by adding the Fe powder to Ba
xSr
1-xTiO
3In (x=0.3～0.8), specific inductivity can be adjustable continuously between 100～1166, can obtain the material system of specific inductivity seriation, widened the range of application of material;
(4) under the applying direct current electric field effect (60kV/cm), described microwave ceramic material have higher dielectric tunable characteristic (〉=10%);
(5) this stupalith has low loss (tg δ＜0.01) under microwave frequency band.
(6) adopt traditional electronic ceramic technology, technique is simple, and cost is low, the side effect of material system environment-protecting asepsis, and excellent performance is applicable to exploitation and the design of adjustable microwave device.
Description of drawings
Fig. 1, (1-y) Ba
0.4Sr
0.6TiO
3The X-ray diffraction analysis collection of illustrative plates of-y Fe microwave ceramic material;
Fig. 2, (1-y) Ba
0.4Sr
0.6TiO
3The relation curve of-y Fe microwave ceramic material specific inductivity and temperature under f=10kHz;
Fig. 3, (1-y) Ba
0.4Sr
0.6TiO
3The relation curve of-y Fe microwave ceramic material specific inductivity and external dc field intensity under f=10kHz.
Embodiment
Further set forth the present invention below in conjunction with specific embodiment, should be understood that these embodiment only are used for explanation the present invention and are not used in restriction protection scope of the present invention.
Embodiment 1
Barium-strontium titanate-based microwave ceramic material (1-y) Ba that dielectric is adjustable
0.4Sr
0.6TiO
3The preparation of-yFe, wherein (1-y) Ba
0.4Sr
0.6TiO
3The component proportion of-yFe material is as shown in table 1.
Its preparation method specifically comprises the steps:
(1) according to Ba
0.4Sr
0.6TiO
3Stoichiometric ratio, take by weighing 28.015g BaTiO
3With 33.066g SrTiO
3Powder places nylon ball grinder, adds zirconia ball and dehydrated alcohol or deionized water, and (during ball milling, the mass ratio of the zirconia ball of adding and ball milling material was 1.5: 1 to ball milling in 24 hours; The dehydrated alcohol that adds or the mass ratio of deionized water and ball milling material are 3.0: 1), 1200 ℃ of pre-burnings 4 hours, obtain Ba after the grinding after the discharging oven dry
0.4Sr
0.6TiO
3Powder is stand-by.
Take by weighing respectively above-mentioned synthetic Ba according to component proportion in the table 1
0.4Sr
0.6TiO
3Powder, Fe powder are stand-by:
Table 1. (1-y) Ba
0.4Sr
0.6TiO
3-yFe stupalith component proportion
(2) with the Ba in above-mentioned each prescription
0.4Sr
0.6TiO
3Powder and Fe powder compound are put into respectively nylon ball grinder, added zirconia ball and dehydrated alcohol ball milling 24 hours, powder is crossed 200 mesh sieves after the discharging oven dry, again according to traditional electronic ceramic technology, polyvinyl alcohol (PVA) aqueous solution of employing 8% carries out granulation as binding agent, under 15MPa pressure, dry method all is pressed into diameter
Green sheet A1, B1, C1, D1, E1, and dry method is pressed into respectively diameter
12mm, 15mm, 18mm, 20mm, right cylinder A2-A6, the B2-B6 of thickness h=5-10mm, C2-C6, D2-D6, E2-E6, then with A1-A6, B1-B6, C1-C6, D1-D6, E1-E6 respectively through 550 ℃ row is sticking process 5 hours after, again under air atmosphere, sintering temperature is controlled to be 1320-1440 ℃, be incubated after 4-10 hour, obtain respectively (1-y) Ba
0.4Sr
0.6TiO
3-yFe microwave ceramics sample.With (1-y) Ba that makes
0.4Sr
0.6TiO
3-yFe pottery sheet sample all carries out first polishing both surfaces, quilt silver, carries out the test of material phase analysis and dielectric properties behind the silver ink firing, and the ceramic cylinder sample of gained all is used for microwave property after polishing tests, and the relevant dielectric properties of gained sample A-E are as shown in table 2.
Table 2. (1-y) Ba
0.4Sr
0.6TiO
3The relevant dielectric properties of-yFe stupalith
Sample A-Sample E prescription prepared (1-y) Ba among the embodiment 1
0.4Sr
0.6TiO
3-y Fe microwave ceramics sample, wherein pure Ba
0.4Sr
0.6TiO
3, and the X-ray diffraction analysis collection of illustrative plates of Sample A, Sample E sample is as shown in Figure 1, as can be known from Fig. 1, the complete solid solution of the adding of Fe powder and BST forms single-phase cubic perovskite structure, does not have other dephasign to occur; The structure of the X-ray diffraction of Sample B, Sample C and Sample D sample demonstration is single-phase cubic perovskite structure as can be known after testing, does not have other dephasign to occur; SampleA-Sample E prescription prepared (1-y) Ba among the embodiment 1
0.4Sr
0.6TiO
3The specific inductivity of-yFe microwave ceramic material and the relation curve of temperature as shown in Figure 2, the result shows the increase along with the Fe powder content, Curie shifts at the peak low temperature and broadened, specific inductivity significantly reduces; SampleA-Sample E prescription prepared (1-y) Ba among the embodiment 1
0.4Sr
0.6TiO
3The relation of the specific inductivity of-yFe stupalith and external dc field intensity as shown in Figure 3, the result shows the increase along with the Fe powder content, the adjustable rate of the dielectric of this stupalith still remains on more than 10%, the concrete outcome of its performance is as shown in table 2.
Embodiment 2
Barium-strontium titanate-based microwave ceramic material (1-y) Ba that dielectric is adjustable
0.4Sr
0.6TiO
3The preparation of-yFe, wherein (1-y) Ba
0.4Sr
0.6TiO
3The component proportion of-yFe material is as shown in table 3.
Its preparation method specifically comprises the steps:
(1) according to Ba
0.4Sr
0.6TiO
3Stoichiometric ratio, take by weighing 28.015g BaTiO
3With 33.066g SrTiO
3Powder places nylon ball grinder, adds zirconia ball and dehydrated alcohol or deionized water, and (during ball milling, the mass ratio of the zirconia ball of adding and ball milling material was 1.2: 1 to ball milling in 20 hours; The dehydrated alcohol that adds or the mass ratio of deionized water and ball milling material are 1.5: 1), 1100 ℃ of pre-burnings 4 hours, obtain Ba after the grinding after the discharging oven dry
0.4Sr
0.6TiO
3Powder is stand-by.
Take by weighing respectively above-mentioned synthetic Ba according to component proportion in the table 3
0.4Sr
0.6TiO
3Powder, Fe powder are stand-by:
Table 3. (1-y) Ba
0.4Sr
0.6TiO
3-yFe stupalith component proportion
(2) with the Ba in above-mentioned each prescription
0.4Sr
0.6TiO
3Powder and Fe powder compound are put into respectively nylon ball grinder, added zirconia ball and dehydrated alcohol ball milling 20 hours, powder is crossed 200 mesh sieves after the discharging oven dry, again according to traditional electronic ceramic technology, polyvinyl alcohol (PVA) aqueous solution of employing 10% carries out granulation as binding agent, under 10MPa, 20MPa, 35MPa, 50MPa, 100MPa pressure, dry method all is pressed into diameter respectively
The ceramic green sheet, simultaneously dry method is pressed into respectively diameter
12mm, 15mm, 18mm, 20mm, thickness h is respectively the ceramic green cylinder block of h=5mm, 7mm, 8mm, 9mm, 10mm, then respectively through 500-550 ℃ row is sticking process after after 5 hours, again under air atmosphere, sintering temperature is controlled to be 1350-1400 ℃, be incubated after 6-8 hour, obtain (1-y) Ba
0.4Sr
0.6TiO
3-yFe microwave ceramic material sample F-J.
The stupalith sheet sample F-J that makes is carried out first polishing both surfaces, quilt silver, carry out the test of material phase analysis and dielectric properties behind the silver ink firing; The stupalith cylindrical samples F-J that makes is used for the microwave property test after polishing, after testing as can be known:
Sample F among the embodiment 2-J prepared (1-y) Ba that fills a prescription
0.4Sr
0.6TiO
3The X-ray diffraction analysis collection of illustrative plates of-y Fe microwave ceramic material as can be known, the complete solid solution of the adding of Fe powder and BST forms single-phase cubic perovskite structure, does not have other dephasign to occur; Sample F among the embodiment 2-J prepared (1-y) Ba that fills a prescription
0.4Sr
0.6TiO
3The specific inductivity of-yFe microwave ceramic material and the relation curve of temperature as shown in Figure 2, the result shows the increase along with the Fe powder content, Curie shifts at the peak low temperature and broadened, specific inductivity significantly reduces; Sample F among the embodiment 2-J prepared (1-y) Ba that fills a prescription
0.4Sr
0.6TiO
3The relation of the specific inductivity of-yFe stupalith and external dc field intensity shows that along with the increase of Fe powder content, the adjustable rate of the dielectric of this stupalith presents the trend that reduces, but still remains on more than 10%.
Claims (5)
1. barium-strontium titanate-based microwave ceramic material that dielectric is adjustable, its structure is single-phase cubic perovskite structure, described barium-strontium titanate-based microwave ceramic material comprises the feed composition of following mass percent:
Ba
xSr
1-xTiO
3 50wt.%～99.9wt.%；
Fe powder 0.1wt.%～15wt.%;
X=0.3～0.8 wherein;
The barium-strontium titanate-based microwave ceramic material that described dielectric is adjustable adopts following steps to prepare:
1) Ba
xSr
1-xTiO
3The preparation of powder: according to Ba
xSr
1-xTiO
3The stoichiometric ratio of middle Ba and Sr element takes by weighing main raw material BaTiO
3And SrTiO
3, with BaTiO
3And SrTiO
3Mixing and ball milling 20～24 hours is carried out pre-burning after the discharging oven dry under 1100 ℃～1200 ℃, obtain described Ba after grinding
xSr
1-xTiO
3Powder;
2) according to Ba
xSr
1-xTiO
3Take by weighing the Ba that step 1) obtains with the proportioning of Fe powder
xSr
1-xTiO
3Powder and Fe powder, ball milling and discharging oven dry, the rear acquisition powder that sieves, described sieve number of sieving is 200 orders;
3) adopting binding agent to step 2) powder that obtains carries out granulation, and then compression moulding under 10～100MPa pressure obtains ceramic green, and described binding agent is 8～10% polyvinyl alcohol water solution;
4) after ceramic green glues processing through row, 1320 ℃～1440 ℃ lower insulations 2～4 hours, obtain described dielectric
Adjustable barium-strontium titanate-based microwave ceramic material.
2. the preparation method of the adjustable barium-strontium titanate-based microwave ceramic material of dielectric as claimed in claim 1 comprises the steps:
(1) Ba
xSr
1-xTiO
3The preparation of powder: according to Ba
xSr
1-xTiO
3The stoichiometric ratio of middle Ba and Sr element takes by weighing main raw material BaTiO
3And SrTiO
3, with BaTiO
3And SrTiO
3Mixing and ball milling 20～24 hours is carried out pre-burning after the discharging oven dry under 1100 ℃～1200 ℃, obtain described Ba after grinding
xSr
1-xTiO
3Powder;
(2) according to Ba
xSr
1-xTiO
3Take by weighing the Ba that step (1) obtains with the proportioning of Fe powder
xSr
1-xTiO
3Powder and Fe powder, ball milling and discharging oven dry, the rear acquisition powder that sieves, described sieve number of sieving is 200 orders;
(3) adopt binding agent that the powder that step (2) is obtained is carried out granulation, then compression moulding under 10～100MPa pressure obtains ceramic green, and described binding agent is 8～10% polyvinyl alcohol water solution;
(4) after ceramic green glues processing through row, 1320 ℃～1440 ℃ lower insulations 2～4 hours, obtain the adjustable barium-strontium titanate-based microwave ceramic material of described dielectric.
3. preparation method as claimed in claim 2 is characterized in that, in step (1) and the step (2), during described ball milling, the mass ratio of the zirconia ball of adding and ball milling material is (1.2～1.5): 1; The dehydrated alcohol that adds or the mass ratio of deionized water and ball milling material are (1.5～3.0): 1.
4. preparation method as claimed in claim 2 is characterized in that, in the step (4), the temperature range that described row glues is 500 ℃-550 ℃.
5. the as claimed in claim 1 adjustable application of barium-strontium titanate-based microwave ceramic material in ferroelectric phase shifter, miniature capacitor, tuning microwave device, wave filter, variable condenser and retarding line of dielectric.
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| CN101337811A (en) * | 2008-08-11 | 2009-01-07 | 同济大学 | Composite microwave ceramic materials with dielectric adjustable and method for preparing same |
| CN101665353A (en) * | 2009-09-08 | 2010-03-10 | 同济大学 | Dielectric tunable barium-strontium titanate-based composite tungstate microwave dielectric material and preparation thereof |
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|---|---|---|---|---|
| CN101337811A (en) * | 2008-08-11 | 2009-01-07 | 同济大学 | Composite microwave ceramic materials with dielectric adjustable and method for preparing same |
| CN101665353A (en) * | 2009-09-08 | 2010-03-10 | 同济大学 | Dielectric tunable barium-strontium titanate-based composite tungstate microwave dielectric material and preparation thereof |
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| Title |
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| Structural and dielectric properties of the system Ba1-xSrxFe0.01Ti0.99O3;laishram Radhapiyari,et al;《MATERIALS LETTERS》;20031231;第57卷;第1824-1829页 * |
| 周歧刚等.Mn-Mg共掺杂对钛酸锶钡薄膜介电性能的影响.《无机材料学报》.2007,第22卷(第3期),第519-523页. |
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| 杂质分布设计对钛酸锶钡薄膜结构和性能的影响;周歧刚等;《物理学报》;20071130;第56卷(第11期);第6666-6673页 * |
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