CN102358930A - 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 substrate 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, the potential using value is arranged, like the little and capacious miniature capacitor of volume, tuning microwave device, ferroelectric phase shifter etc. in adjustable device.The strontium-barium titanate material is generally believed it is the most promising ferroelectric phase shift 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.Yet the BST stupalith with high-k be difficult to satisfy the application requiring with driving source internal driving coupling and high-power component, this big limitations its application in the microwave adjustable device field.
For solving above-mentioned technological difficulties; Many investigators are the mode through ion doping mainly; Make dopant ion get in the crystalline network of material, cause the change of material microstructure, adjust and improve the correlated performance of material effectively; 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, like MgO, AI
2O
3, La
2O
3Deng, the result shows the dielectric loss that has reduced material to a certain extent that is added in of these oxide compounds, and has certain adjustable rate.Wherein 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, obtain low-loss microwave ceramic material, obtained very big 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) adulterated unfavorable factor, realize low-loss, low-k, high adjustable requirement.Through the document retrieval, up to the present find to adopt the Fe powder that BST is mixed as yet and the relevant report of dielectric properties aspect, there is not the patent that duplicates with the present invention yet.
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 certain adjustable rate simultaneously, 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 monophasic cubic perovskite structure, and said 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, said x=0.4.
Preferably, the mass percent of said 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, pre-burning is carried out in discharging oven dry back under 1100 ℃～1200 ℃, grind the back and obtain said Ba
xSr
1-xTiO
3(x=0.3～0.8) powder.
Preferable, said BaTiO
3And SrTiO
3Purity be 99.90%, come from Shandong state porcelain ceramic material ltd.
Preferable, during said ball milling, the mass ratio of the zirconia ball of adding and ball milling material is (1.2～1.5): 1; The absolute ethyl alcohol that adds or the mass ratio of deionized water and ball milling material are (1.5～3.0): 1.Can place nylon ball grinder to carry out raw material during said ball milling.
Preferable, the time of said 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 through 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, the back of sieving obtains powder.
The purity that Fe powder according to the invention can select for use AlfaAesar company to produce is 95% Fe powder.
Preferable, added zirconia ball and absolute ethyl alcohol or deionized water ball milling during said 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 absolute ethyl alcohol or deionized water and ball milling material is (1.5～3.0): 1.
Preferably, said sieve number of sieving is 200 orders.
(3) adopt sticker that the powder that step (2) is obtained is carried out granulation,, obtain ceramic green then in the moulding of 10～100MPa pressure pressed.
Preferable, said sticker is 8～10% Z 150PH (PVA) aqueous solution.
Ceramic green of the present invention can be pressed into the block of desired size size through forming mould.
(4) after ceramic green glued processing through row, insulation was 2～4 hours under 1320 ℃～1440 ℃, obtains the adjustable barium-strontium titanate-based microwave ceramic material of said dielectric.
Preferable, the temperature that said 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 for use 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 can be used for the stupalith of adjustable device, especially be 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 to 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 Tc 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%, Tc moves to the low temperature direction, and its adjustable rate still keeps within the specific limits;
(3) through 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), said 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, 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, (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 to the present invention is described 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 set of dispense of-yFe material is than 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 absolute ethyl 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 absolute ethyl alcohol that adds or the mass ratio of deionized water and ball milling material are 3.0: 1), discharging oven dry back obtains Ba 1200 ℃ of pre-burnings 4 hours after the grinding
0.4Sr
0.6TiO
3Powder is for use.
Get above-mentioned synthetic Ba according to set of dispense score another name in the table 1
0.4Sr
0.6TiO
3Powder, Fe powder are for use:
Table 1. (1-y) Ba
0.4Sr
0.6TiO
3-yFe stupalith set of dispense ratio
(2) with the Ba in above-mentioned each prescription
0.4Sr
0.6TiO
3Powder and Fe powder compound are put into nylon ball grinder respectively; Added zirconia ball and absolute ethyl alcohol ball milling 24 hours; Discharging oven dry back powder is crossed 200 mesh sieves, and again according to traditional electronic ceramic technology, Z 150PH (PVA) aqueous solution of employing 8% carries out granulation as sticker; Under 15MPa pressure, dry method all is pressed into diameter
Green sheet A1, B1, C1, D1, E1, and dry method is pressed into diameter respectively
12mm, 15mm, 18mm, 20mm; The right cylinder A2-A6 of thickness h=5-10mm, B2-B6, C2-C6, D2-D6, E2-E6; Then with A1-A6, B1-B6, C1-C6, D1-D6, E1-E6 respectively through 550 ℃ row is sticking handle 5 hours after, under air atmosphere, sintering temperature is controlled to be 1320-1440 ℃ again; Be incubated after 4-10 hour, obtain (1-y) Ba respectively
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 polishing both surfaces, quilt silver earlier, 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 the microwave property test after polishing, 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
3And the X-ray diffraction analysis collection of illustrative plates of Sample A, Sample E sample is as shown in Figure 1, can know that from Fig. 1 the complete solid solution of the adding of Fe powder and BST forms monophasic cubic perovskite structure, does not have other dephasign to occur; Structure through detecting the X-ray diffraction demonstration that can know Sample B, Sample C and Sample D sample is monophasic cubic perovskite structure, 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 are as shown in Figure 2, and the result shows the increase along with the Fe powder content, and Curie shifts at the peak low temperature and by broadening, 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 is as shown in Figure 3, and the result shows the increase along with the Fe powder content, and the adjustable rate of the dielectric of this stupalith still remains on more than 10%, and 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 set of dispense of-yFe material is than 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 absolute ethyl 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 absolute ethyl alcohol that adds or the mass ratio of deionized water and ball milling material are 1.5: 1), discharging oven dry back obtains Ba 1100 ℃ of pre-burnings 4 hours after the grinding
0.4Sr
0.6TiO
3Powder is for use.
Get above-mentioned synthetic Ba according to set of dispense score another name in the table 3
0.4Sr
0.6TiO
3Powder, Fe powder are for use:
Table 3. (1-y) Ba
0.4Sr
0.6TiO
3-yFe stupalith set of dispense ratio
(2) with the Ba in above-mentioned each prescription
0.4Sr
0.6TiO
3Powder and Fe powder compound are put into nylon ball grinder respectively; Added zirconia ball and absolute ethyl alcohol ball milling 20 hours; Discharging oven dry back powder is crossed 200 mesh sieves, and again according to traditional electronic ceramic technology, Z 150PH (PVA) aqueous solution of employing 10% carries out granulation as sticker; 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 diameter respectively
12mm, 15mm, 18mm, 20mm; Thickness h is respectively the ceramic green cylinder block of h=5mm, 7mm, 8mm, 9mm, 10mm; Pass through 500-550 ℃ sticking the processing after back 5 hours of row then respectively, under air atmosphere, sintering temperature is controlled to be 1350-1400 ℃ again; 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 polishing both surfaces, quilt silver earlier, carry out the test of material phase analysis and dielectric properties behind the silver ink firing; The stupalith right cylinder sample F-J that makes is used for the microwave property test after polishing, can knows through detecting:
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 can know that the complete solid solution of the adding of Fe powder and BST forms monophasic 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 are as shown in Figure 2, and the result shows the increase along with the Fe powder content, and Curie shifts at the peak low temperature and by broadening, 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 (7)
1. barium-strontium titanate-based microwave ceramic material that dielectric is adjustable, its structure is monophasic cubic perovskite structure, said 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.%～50wt.%;
X=0.3～0.8 wherein.
2. the preparation method of the barium-strontium titanate-based microwave ceramic material that dielectric as claimed in claim 1 is adjustable 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, pre-burning is carried out in discharging oven dry back under 1100 ℃～1200 ℃, grind the back and obtain said BaxSr1-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 back of sieving obtains powder;
(3) adopt sticker that the powder that step (2) is obtained is carried out granulation,, obtain ceramic green then in the moulding of 10～100MPa pressure pressed;
(4) after ceramic green glued processing through row, insulation was 2～4 hours under 1320 ℃～1440 ℃, obtains the adjustable barium-strontium titanate-based microwave ceramic material of said dielectric.
3. preparation method as claimed in claim 2 is characterized in that, in step (1) and the step (2), during said ball milling, the mass ratio of the zirconia ball of adding and ball milling material is (1.2～1.5): 1; The absolute ethyl 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 (2), said sieve number of sieving is 200 orders.
5. preparation method as claimed in claim 2 is characterized in that, in the step (3), said sticker is 8～10% polyvinyl alcohol water solution.
6. preparation method as claimed in claim 2 is characterized in that, in the step (4), the TR that said row glues is 500 ℃-550 ℃.
7. the adjustable application of barium-strontium titanate-based microwave ceramic material in ferroelectric phase shifter, miniature capacitor, tuning microwave device, wave filter, VC and retarding line of dielectric according to claim 1.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107935588A (en) * | 2017-11-22 | 2018-04-20 | 信维通信（江苏）有限公司 | Microwave-tuned device barium strontium titanate medium material |
| 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 |
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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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2011
- 2011-06-30 CN CN 201110183011 patent/CN102358930B/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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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 |
|---|
| LAISHRAM RADHAPIYARI,ET AL: "Structural and dielectric properties of the system Ba1-xSrxFe0.01Ti0.99O3", 《MATERIALS LETTERS》 * |
| 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》 * |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107935588A (en) * | 2017-11-22 | 2018-04-20 | 信维通信（江苏）有限公司 | Microwave-tuned device barium strontium titanate medium material |
| 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 |
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